NiDI Nickel Development Institute Nickel Alloys for Electronics A Nickel Development Institute Reference Book Series N° 11 002 1988 NiDI Nickel Development Institute Nickel Development Institute (NiDI) is the market development and applications research organization of the primary nickel industry. NiDl was incorporated and organized in 1984. Its headquarters are in Toronto, Canada. NiDI's objective is sustained growth in the consumption of nickel. Through a network of a dedicated permanent staff and key international consultants and project contractors, NiDl carries out market development activities, market exploration, and applications-oriented technical research relevant to the achievement of its objective around the world. It provides technical service to nickel consumers and others concerned with nickel, nickel alloys and their uses. NiDI's principal marketing efforts are directed toward the United States, Western Europe, Japan and the newly industrializing nations in Latin America, the Pacific rim and the Indian subcontinent … those countries having the greatest current consumption of nickel and those having the greatest potential for growth. NiDI's information services are available to designers, specifiers, and educators as well as to nickel users. Enquiries are welcomed from architects, engineers, specification writers, and others responsible for selection of materials for manufacturing and construction. NiDl cooperates with colleges and universities by furnishing relevant information and material for engineering, materials science, and industrial design education. The material presented herein has been prepared for the general information of the reader and should not be used or relied upon for specific applications without first securing competent advice. While the material is believed to be technically correct, NiDl, its members, staff, and consultants do not represent or warrant its suitability for any general or specific use and assume no liability or responsibility of any kind in connection with the information herein. Drawings and/or photographs of equipment, machinery, and products are for illustrative purposes only, and their inclusion does not constitute or imply any endorsement of the items or of the companies that manufacture or distribute them. Foreword Reliability, freedom from maintenance costs, longer service and minimum production rejects have become increasingly important to designers and manufacturers of electronic and electrical equipment. In civilian communications and computers, military equipment and industrial controls, nickel alloys provide the combinations of characteristics and properties that warrant their review whenever new designs or design modifications are being considered. Nickel Alloys for Electronics is intended to provide information that will be directly applicable to engineers and designers in evaluating and applying the nickel alloys that are most useful to the electronics industry. The Nickel Development Institute (NiDI) gratefully acknowledges the cooperation of the many companies who have contributed information and background data. The materials included in this reference book are based on generic alloys that have industry specifications and Unified Numbering System (UNS) numbers. Proprietary alloys and manufacturers thereof are not included. Table of Contents Page No. Semiconductor Packaging, Lead Frame and Glass Sealing Alloys 42 Alloy (K94100)................................................................................................ 1 F 15 Alloy (K94610) ............................................................................................ 7 426 Alloy (K94760)............................................................................................ 10 46 Alloy (K94600).............................................................................................. 13 52 Alloy (N14052).............................................................................................. 16 Reference Data on Non-Metallic Materials................................................................. 19 Minimum Expansion Alloy Invar (K93600)................................................................................................... 20 Nickel Beryllium (N03360) ........................................................................................... 23 Nickel Nickel 200, 201, 205, 233, 270/290 (N02200, N02201, N02205, N02233, N02270/N02290)................................ 25 Copper-Base Connector and Spring Alloys Copper Alloy C72500........................................................................................ 29 Copper Alloy C76200........................................................................................ 33 Copper Alloy C77000 ....................................................................................... 37 Spinodal Alloy Copper Alloy C72900........................................................................................ 40 Stainless Steel Alloys AISI 301 and 304..................................................................... 46 Nickel Electroplating ..................................................................................................... 49 Standards and Specifications ...................................................................................... 62 Note—Numbers in parentheses are UNS (Unified Numbering System) Numbers; Copper Development Association (CDA) and UNS Numbers for Copper-Base Alloys are identical. 42 Alloy* Superior bend properties at the temper used for lead frames Nickel and iron-nickel alloys were the original commercial semiconductor packaging metals. 42 Alloy lead frames continue to be used widely for highreliability ceramic Cer-DIP and plasticpackaged devices where these advantages are important: Important in making conventional 90° as well as J-bends. Closest possible match to thermal expansion of alumina, beryllia and vitreous glass Worldwide availability There are no patents on 42 Alloy and it is made everywhere semiconductor devices are manufactured and packaged. Extremely important in avoiding cracks and breaks in soldered joints (Fig. 3). Intrinsically superior strength and stiffness Plateability The much higher yield strength and modulus of elasticity of 42 Alloy is important in minimizing bent leads, especially in automatic insertion (Fig. 1). 42 Alloy strip can be plated, striped or spot-plated with nickel, copper or lead-tin solder as well as gold or silver. Weldability High softening and stress relaxation temperatures Iron-nickel alloys are welded readily by spot, projection, seam, stitch, flash and other resistance and fusion processes. Alloy 42 is also adaptable to ultrasonic and thermocompression bonding and electron-beam and laser welding. Strength and stiffness are maintained completely during exposure to soldering, burn-in and other manufacturing steps where exposure to elevated temperatures is possible (Fig. 2). Cladding Higher hardness at temper used Composite strip can be produced by cladding or inlaying 42 Alloy with copper, aluminum, gold or silver to obtain combinations of the best properties of two or more alloys or metals, and to reduce costs. This is reflected in improved lead frame strip surface. No intermetallic compounds that can be harmful to solderability These characteristics add up to the use of 42 Alloy wherever resistance to heat, moisture or aggressive environments is encountered, and where long life and high reliability are called for. Properties of 42 Alloy are shown in Table 1. High strength levels are developed through cold work alone. *UNS K94100 1 Thermal Management in Semiconductor Devices and Printed Circuit Board Assemblies Limiting junction and average die temperatures in microelectronic devices and assemblies require consideration of the chip and board designs, component densities and external cooling systems. These design factors plus the bulk thermal conductivity of the ceramic or epoxy package usually have more effect than the thermal conductivity of the lead frame material alone. Thermal test boards and systems are now widely used to test new device and board designs and should be used to determine whether the difference between the thermal conductivity of a 42 Alloy lead frame and a copper-base frame is significant. The high reliability and the superior mechanical properties of 42 Alloy should not be overlooked simply because the thermal conductivity of the material is not as high as the copper-base alloys. 2 Fig 1 Comparative yield strength levels of 42 Alloy vs C19400 at several tempers 3 Fig 2 Stress relaxation of high-strength lead-frame alloys as measured by resistance to softening [strip thickness 0.254 mm (0.010 in.)] 4 Fig 3 Linear thermal expansion of 42 Alloy, 99.5% beryllia and 94% alumina vs temperature 5 Table 1 Properties of 42 Alloy Chemical Composition, % Nickel 41.5 Cobalt nominal 0.50 maximum Chromium 0.25 maximum Manganese 0.80 maximum Silicon 0.30 maximum Carbon 0.05 maximum Aluminum 0.10 maximum Phosphorus 0.025 maximum 0.025 maximum Sulfur Iron Balance Comparative Thermal Expansion Coefficient (Instantaneous) 42 Alloy (ASTM F 30 and Mil-I-23011) 4.0 to 4.7 × 10–6cm/cm/°C 6.7 to 7.4 × 10–6cm/cm/°C 10.5 × 10–6cm/cm/°C 2.2 to 2.6 × 10–6in./in./°F 3.7 to 4.1 × 10–6in./in./°F 5.8 × 10–6in./in./°F Alumina, 94% Al2O3 7.2 4.0 96% Al2O3 7.5 4.1 99.5% Al2O3 7.6 4.2 Beryllia, 99.5% BeO 7.8 4.3 30-300 °C (86-572 °F) 30-450 °C (86-842 °F) 30-700 °C (86-1292 °F) Ceramics - Typical, 25-700 °C (77-1292 °F) Vitreous Glass-Typical, 25-300 °C (77-572 °F) 8.0 4.45 C19400 Copper-base Lead Frame Alloy-Typical 20-300 °C (68-572 °F) 16.9 9.3 Density 8.11g/cc 0.293 Ib/in.3 Melting Point 1425 °C 2597 °F 20-100 °C (68-212 °F) 14.7 W/(m • °K) 100.8 Btu • in./h • ft2 • °F Electrical Resistivity 20 °C (66 °F) 63 microhm • cm 380 ohm • cmil/ft Curie Temperature 375 °C 707 °F Physical Properties Thermal Conductivity Mechanical Properties (Half-hard Temper) Tensile Strength Yield Strength, 0.2% offset Elongation, % in 2 in.(5.08 cm) Hardness (Vickers equivalent) Modulus of Elasticity Poisson's Ratio 790 MPa 720 MPa 115,000 psi 105,000 psi 5 170 144,000 MPa 21,000,000 psi 0.25 NOTE: By controlling the processing variables, the mill can effect changes in the above mechanical properties. It is suggested that you consult your supplier to discuss the range of possibilities available. 6 F 15 Alloy* ASTM F 15 Alloy is a nickel-cobaltiron alloy specifically designed to match the expansion of borosilicate glass (Fig. 4). The balance of nickel with cobalt in this alloy results in the following special characteristics and attributes: Very low and uniform thermal expansion properties High reliability under thermal shock Excellent deep drawing and freedom from earing Low outgassing Resists attack by mercury The properties of F 15 are shown in Table 2. *UNS K94610 7 Fig 4 Linear thermal expansion of F 15 Alloy and hard glass vs temperature 8 Table 2 Properties of F 15 Alloy Chemical Composition, % Nickel 29 nominal Cobalt 17 nominal Manganese 0.50 Silicon 0.20 maximum Carbon 0.06 maximum Balance maximum Iron maximum Aluminum, Magnesium, Zirconium and Titanium may be 0.10% each, maximum, but, total cannot exceed 0.20% Thermal Expansion Coefficient 30-400 °C (86-752 °F) 4.60 to 5.20 × 10–6cm/cm/°C 2.6 to 2.9 × 10–6in./in./°F 30-450 °C (86-842 °F) 5.10 to 5.50 × 10 cm/cm/°C 2.8 to 3.1 × 10–6in./in./°F Density 8.35 g/cc 0.302 lb/in.3 Melting Point 1450 °C 2642 °F 30 °C (86°F) 16.6W/(m • °K) 114.5 Btu • in./h • ft2 • °F 300 °C (632 °F) 20.3 W/(m • °K) 141 Btu • in./h • ft2 • °F 49 microhm • cm 294 ohm • cmil/ft 435 °C 815 °F Tensile Strength 790 MPa 115,000 psi Yield Strength, 0.2% offset 720 MPa –6 Physical Properties Thermal Conductivity Electrical Resistivity 20 °C (68 °F) Curie Temperature Mechanical Properties (Half-hard) 105,000 psi Elongation, % in 2 in.(5.08cm) 5 Hardness (Vickers equivalent) 210 Modulus of Elasticity 137,000 MPa Poisson's Ratio 20,000,000 psi 0.30 NOTE: By controlling the processing variables, the mill can effect changes in the above mechanical properties. It is suggested that you consult your supplier to discuss the range of possibilities available. 9 426 Alloy* 426 Alloy (ASTM F 31) was developed to match the thermal expansion characteristics of potash-soda-lead glass such as Corning 0120 (Fig. 5). An advantage of this glass-to-metal sealing alloy is that a tight green oxide film is formed by wet hydrogen annealing at 2050 °F, making a vacuum-tight seal. It is used for such applications as glassed windows, leads for compression seals and relatively large-scale glass sealing applications where the size limitations of “dumet” (copper-coated 42 Alloy) make that composite wire unsuitable. Properties of 426 Alloy are shown in Table 3. *UNS K94760 10 Fig 5 Linear thermal expansion of 426 Alloy and soft glass vs temperature 11 Table 3 Properties of 426 Alloy Chemical Composition, % Nickel 42 nominal Chromium 5.6 nominal Carbon 0.07 maximum Manganese 0.25 maximum Phosphorus 0.025 maximum Sulfur 0.025 maximum Silicon 0.30 maximum Aluminum 0.20 maximum Iron Balance Thermal Expansion Coefficient 30-350 °C (86-662 °F) 8.5 to 9.2 × 10–6 cm/cm/°C 4.7-5.1 × 10–6 in./in./°F 30-425 °C (86-797 °F) 9.7 to 10.4 × 10 cm/cm/°C 5.4-5.8 × 10–6 in./in./°F Density 8.12 g/cc 0.294 Ib/in.3 Melting Pant 1425 °C 2597 °F 12.2 W/(m • °K) 82.8 Btu • in./h • ft2 • °F 95 microhm • cm 570 ohm • cmil/ft 295 °C 563 °F Tensile Strength 790 MPa 115,000 psi Yield Strength, 0.2% offset 720 MPa –6 Physical Properties Thermal Conductivity 20-100 °C (68-212 °F) Electrical Resistivity 20 °C (68 °F) Curie Temperature Mechanical Properties (Half-hard) 105,000 psi Elongation, % in 2 in.(5.08cm) 5 Hardness (Vickers equivalent) 210 Modulus of Elasticity 158,500 MPa Poisson's Ratio 23,000,000 psi 0.28 NOTE: By controlling the processing variables, the mill can effect changes in the above mechanical properties. It is suggested that you consult your supplier to discuss the range of possibilities available. 12 46 Alloy* This iron-nickel sealing alloy (ASTM F 30) has been used extensively as terminal bands for vitreous enameled resistors and for sealing metallized ceramics. It finds application for seals that are not hydrogen annealed prior to sealing to assure freedom from gas pockets. Properties of 46 Alloy are shown in Table 4 and Fig. 6 *UNS K94600 13 Fig 6 Linear thermal expansion of 46 Alloy and 94% alumina vs temperature 14 Table 4 Properties of 46 Alloy Chemical Composition, % Nickel 46 nominal Cobalt 0.50 Chromium 0.25 maximum Manganese 0.80 maximum Silicon 0.30 maximum Carbon 0.05 maximum Aluminum 0.10 maximum Phosphorus 0.025 maximum Sulfur 0.025 maximum Iron maximum Balance Thermal Expansion Coefficient 30-350 °C (86-662 °F) 7.1 to 7.8 × 10–6 cm/cm/°C 3.9 to 4.3 × 10–6 in./in./°F 30-500 °C (86-932 °F) 8.2 to 8.9 × 10–6 cm/cm/°C 4.6 to 4.9 × 10–6 in./in./°F Density 8.24 g/cc 0.298 Ib/in.3 Melting Point 1425 °C 2597 °F 11.3 W/(m • °K) 79.2 Btu • in./h • ft2 • °F Physical Properties Thermal Conductivity 20–100 °C (68–212 °F) Electrical Resistivity 20 °C (68 °F) Curie Temperature 51 microhm • cm 310 ohm • cmil/ft 450 °C 842 °F Mechanical Properties (Half-hard) Tensile Strength 790 MPa Yield Strength, 0.2% offset 720 MPa 115,000 psi 105,000 psi Elongation, % in 2 in.(5.08cm) 5 Hardness (Vickers equivalent) Modulus of Elasticity 210 158,500 MPa Poisson's Ratio 23,000,000 psi 0.28 NOTE: By controlling the processing variables, the mill can effect changes in the above mechanical properties. It is suggested that you consult your supplier to discuss the range of possibilities available. 15 52 Alloy* 52 Alloy (ASTM F 30) has thermal expansion characteristics that match vitreous potash-soda-lead glass. Its rate of thermal expansion is virtually constant to about 565 °C (1050 °F) (Fig. 7). A modified 52 Alloy with higher nickel (51-51.5%) exhibits the combination of controlled expansion and magnetic properties required for mercury-wetted reed switches. Properties of 52 Alloy are shown in Table 5. *UNS N14052 16 Fig 7 Linear thermal expansion of 52 Alloy and soft glass vs temperature 17 Table 5 Properties of 52 Alloy Chemical Composition, % Nickel Cobalt 50.5 nominal .50 maximum Chromium 0.10 maximum Manganese 0.60 maximum Silicon 0.30 maximum Carbon 0.05 maximum Aluminum 0.10 maximum Phosphorus 0.025 maximum 0.025 maximum Sulfur Iron Balance Thermal Expansion Coefficient 30-450 °C (86-842 °F) 9.6 to 10.1 × 10–6 cm/cm/ °C 5.3 to 5.6 × 10–6 in./in./°F 30-550 °C (86-1022 °F) 10.2 to 10.7 × 10 cm/cm/°C 5.7 to 5.9 × 10–6 in./in./°F 30-450 °C 10.0 to 10.35 × 10–6 cm/cm/°C –6 * Modified Alloy for Reed Switch Applications Physical Properties Density 8.30 g/cc 0.30 Ib/in.3 Melting Point 1425 °C 2597 °F 13.4 W/(m • °K) 93.6 Btu • in./h • ft2 • °F 43 microhm • cm 259 ohm • cmil/ft 510 °C 950 °F Tensile Strength 790 MPa 115,000 psi Yield Strength, 0.2% offset 720 MPa Thermal Conductivity 20–100 °C (68–212 °F) Electrical Resistivity 20 °C (68 °F) Curie Temperature Mechanical Properties (Half-hard) 105,000 psi Elongation, % in 2 in.(5.08cm) 5 Hardness (Vickers equivalent) Modulus of Elasticity 210 165,000 MPa Poisson's Ratio 24,000,000 psi 0.29 NOTE: By controlling the processing variables, the mill can effect changes in the above mechanical properties. It is suggested that you consult your supplier to discuss the range of possibilities available. 18 Reference Data on Non-Metallic Materials Nickel alloys are often used in electronic applications in conjunction with non-metallic materials in sealing, mounting and packaging. Table 6 summarizes the properties of some of the non-metallic ceramics, glasses and plastics used in these applications. Table 6 Properties of Non-Metallic Materials Material Thermal Expansion Coefficient, cm/cm/°C × 10–6 Thermal Conductivity, W/(m • °K) Tensile Strength, psi MPa (25-700°C) 7.2 7.5 7.6 (25°C) 27.7 35.2 36.9 (300°C) 15.5 17.2 18.4 20.000 25.000 28.000 (140) (170) (190) (25-700°C) 7.8 (25°C) 247 (300°C) 117 23.000 (160) (25-150°C) 59 (25°C) .587 10.000 (70) (25-250°C) 22 (25°C) .503 6.000 (40) (–30 to +30°C) 21 (25°C) .503 7.000 (50) Alumina Ceramic 94% Al2O3 96% Al2O3 99.5% Al2O3 Beryllia Ceramic 99.5% BeO Epoxy Rigid, Filled Silicone Phenolic Electrical Grade Sealing Glasses Type Thermal Expansion Coefficient, cm/cm/°C (in./in./°F) × 10–6 Temp Range, °C (°F) Vitreous potash-soda-lead (eg. Coming 0120) borosilicate (eg. Corning 7052) lead-borate-zinc (eg. Corning 7585) borosilicate (eg. Coming 9741) 0-300 (32-572) 25-400 (77-752) 0-300 (32-572) 25-441 (77-826) 0-270 (32-518) 25-set pt. (77-set pt.) 0-300 (32-572) 25 to set pt. (77-set pt.) 8.95 (4.97) 9.9 (5.5) 4.6 (2.56) 5.31 (2.95) 6.8 (3.83) 6.75 (3.94) 3.8 (2.1) 5.5 (3.1) 0-300 (32-572) 25-480 (77-896) 0-300 (32-572) 25-400 (77-752) 8.4 (4.67) 8.3 (4.61) 8.0 (4.44) 7.8(4.33) Devitrefying lead -zinc-borosilicate (eg. Corning 7583) lead-zinc-borosilicate (eg. Corning 7589) 19 Invar* The Invar alloys have the lowest thermal expansion of any metals or alloys in the temperature range from ambient to about 230 °C (446 °F). The properties of Invar are shown in Table 7 and Fig 8. The “super-Invar” modification (31.5 Ni, 4.5 Co) has nearly zero expansivity over that range. Some of the applications for Invar alloys include: Low expansion side of thermostatic bimetals Precision measuring devices and gauges Clamps and fixtures requiring extreme dimensional stability Radar resonant cavities Tanks and pipelines for liquefied gas Special joints and washers *UNS K93600 20 Fig 8 Linear thermal expansion of 42 Alloy, Invar and carbon steel 21 Table 7 Properties of Invar Chemical Composition, % Nickel Manganese 36 nominal 0.35 maximum Silicon 0.30 maximum Carbon 0.12 maximum Iron Balance Thermal Expansion Coefficient 25-100 °C (70-212 °F) 1.18 × 10–6 cm/cm/°C 0.655 × 10–6 cm./cm./°C 25-200 °C (70-392 °F) 1.72 × 10 cm/cm/°C 0.956 × 10–6 in./in./°F Density 8.05 g/cc 0.291 Ib/in.3 Melting Point 1425 °C 2597 °F 20-100 °C (68-212 °F) 10.5 W/(m • °K) 72 Btu • in./h • ft2 • °F Electrical Resistivity 20 °C(66 °F) 82 microhm • cm 495 ohm • cmil/ft Curie Temperature 280 °C 537 °F Tensile Strength 450 MPa 65,000 psi Yield Strength, 0.2% offset 275 MPa –6 (See Expansion Curve, previous page) Physical Properties Thermal Conductivity Mechanical Properties (Annealed) 40,000 psi Elongation, % in 2 in.(5.08cm) 35 Hardness (Vickers equivalent) Modulus of Elasticity 125 141,000 MPa Poisson's Ratio 20,500,000 psi 0.29 NOTES: 1) By controlling the processing variables, the mill can effect changes in the above mechanical properties. It is suggested that you consult your supplier to discuss the range of possibilities available. 2) Cold worked or machined Invar may require stress-relieving for high-precision applications: a) 1525 °F - 30 min; water quench; b) 600 °F - 1 h; air cool c) 205 °F - 48 h; air cool 22 Nickel Beryllium Alloy* This is basically a nickel-base beryllium titanium alloy extensively used in springs, contacts and connectors, diaphragms and bellows, feather valves, clamps, clips and bearing retainers. It derives high strength from cold work and age hardening and exhibits excellent corrosion and fatigue resistance as well as stress relaxation resistance, wear and abrasion resistance. It is readily formable before or after aging. *UNS N03360 23 Table 8 Properties of Nickel Beryllium Thermal Expansion Coefficient 13.9 × 10–6 cm/cm/°C 8.0 × 10–6 in/in/°F Density 8.55 g/cc 0.309 Ib/in3 Thermal Conductivity 48 W(m• °K) 336 Btu⋅in/h⋅ft2⋅°F 20-550 °C (68-1022 °F) Physical Properties Electrical Conductivity Soln. H.T. & Cold Rolled 4% IACS Soln. H.T. & Age Hardened 7% IACS Melting Point 1379 °C 2515 °F Modulus of Elasticity 200,000 MPa 29,500,000 psi Mechanical Properties (Typical) Temper Annealed ¼ Hard ½ Hard Hard Annealed + Aged ¼ Hard + Aged ½ Hard + Aged Full Hard + Aged Tensile Strength MPa ksi 655-895 758-1033 895-1207 1069-1310 1480 (min) 1585 (min) 1689 (min) 1860 (min) 95-130 110-150 130-175 155-190 215 (min) 230 (min) 245 (min) 270 (min) Yield Strength (0.2% offset) MPa ksi 276-482 448-860 792-1170 1032-1310 1033 (min) 1207 (min) 1380 (min) 1585 (min) 24 40-70 65-125 115-170 150-190 150 (min) 175 (min) 200 (min) 230 (min) Elongation in 2 in. (50.8 mm), % Hardness, HV 30 15 4 1 12 10 9 8 106-200 153-293 160-383 180-491 343-528 383-598 395-695 446-695 Nickel 200, 201, 205, 233, 270/290* The intrinsic saturation induction value for nickel 200 is about 6000 G, for high purity nickel about 6200 G. The initial permeability of nickel 200 is about 200 and the maximum permeability is about 1000 at H = 20 Oe; for high purity nickel the values are about 200 and 2000 to 3000, respectively, at H = 1 Oe. The coercivity of nickel has been measured at 0.7 to 2.7 Oe, greatly affected by fabrication and heattreatment. Nickel has one of the largest magnetostrictive effects available in commercial materials and is extensively used in devices when this is required. The commercially pure nickels can be obtained in several grades, with slightly different compositional modifications for special needs. All grades are characteristically strong, ductile and corrosion-resistant over a wide temperature range. Properties of nickel are shown in Table 9 and Figs 9 and 10. Typical applications of wrought nickel include semi-conductor packaging cans, high-temperature electrical leads, magnetostrictive devices, battery plaques and electron tube cathodes and anodes. Nickel is readily deep drawn, spun, coined, etched, welded and brazed. Nickel is one of the three elements (iron and cobalt are the others) that are strongly magnetic at ambient temperatures. Studies indicate that the magnetic properties of really clean pure nickel films are the same as for bulk nickel. The Curie point for nickel (the temperature at which the change from ferromagnetism to paramagnetism occurs) is affect by prior thermal and mechanical treatment and the nature and amount of impurities present. Most alloying elements (except cobalt and iron) lower the Curie point. *UNS N02200, N02201, N02205, N02233, N02270/N02290 25 26 99.00 min 99.97 min 233 270/ 290 201 99.00 min 99.00 min 200 205 Nickel (plus Co) 99.00 min Nickel Chemical Composition, % Cu (max) 0.001 0.10 0.15 0.25 0.25 Fe (max) 0.005 0.10 0.20 0.40 0.40 0.001 0.30 0.35 0.35 0.35 Mn (max) 0.02 0.15 0.15 0.02 0.15 C (max) 0.001 0.10 0.15 0.35 0.35 Si (max) 0.001 0.008 0.008 0.01 0.01 S (max) Table 9 Properties of Commercially Pure Nickel 0.001 Crmax 0.001 Mgmax 0.001 Crmax 0.001 Timax 0.005 Timax 0.01/0.1 Mg 0.01/0.08 Mg 0.01/0.05 Ti Other high purity, exceptionally free from metallics, best thermal and electrical conductivity. Useful for etching, stamping and deep drawing requirements. tough, ductile, corrosion resistant, general purpose nickel, formerly "A" Nickel. Standard for many electrical and electronic applications. low carbon grade particularly suitable to spinning and coining; low rate of work hardening. Etching and deep drawing grade. specially selected to narrow chemical analysis range; formerly Electronic grade "A" Nickel. specially produced at closely controlled low residual element levels, used particularly for active cathodes. Specified for deep drawn cans where Nickel 200 chemistry is not suitable. Comments Table 9 Properties of Commercially Pure Nickel (continued) Thermal Expansion Coefficient 30-300 °C (86-572 °F) 30-450 °C (86-842 °F) 14.4 × 10–6 cm/cm/°C 14.9 × 10–6 cm/cm/°C 8.3 × 10–6 in./in./°F 8.3 × 10–6 in./in./°F 8.89 g/cc 0.321 lb/in.3 67 W/(m • °K) 79 W/(m • °K) 468 Btu • in./h • ft2 • °F 548 Btu • in./h • ft2 • °F 9.5 microhm • cm 7.5 microhm • cm 360 °C 1435-1450 °C 57 ohm • cmil/ft 45 ohm • cmil/ft 680 °F 2615-2640 °F 620/895 MPa 345/515 MPa 90,000-130,000 psi 50,000-75,000 psi 485/795 MPa 105/205 MPa 70,000-115,000 psi 15,000-30,000 psi Physical Properties Density Thermal Conductivity 20-100 °C (68-212 °F) Nickel 270: Electrical Resistivity 20 °C (68 °F) Nickel 270: Curie Temperature Melting Range Mechanical Properties Tensile Strength cold worked annealed Yield Strength, 0.2% offset cold worked annealed Elongation, % in 2 in.(5.08cm) cold worked annealed Hardness (Vickers equivalent) cold worked annealed Modulus of Elasticity Tension Torsion Poisson’s Ratio (longitudinal) ASTM method (longitudinal) dynamic calc. 2-15 40-55 210 min 114 max 204 MPa 80 MPa 29,600,000 psi 11,600,00 psi 0.287 0.264 NOTE - These properties are typical of Nickel 200 (N02200). Properties of the other nickel grades differ slightly depending on their composition. The significant differences in thermal and electrical conductivity values of nickel 270 (N02270) are noted. NOTE - By controlling the processing variables, the mill can effect changes in the above mechanical properties. It is suggested that you consult your supplier to discuss the range of possibilities available. SPECIFICATIONS Nickel 200 – ASTM B 160, B 161, B 162 Nickel 201 – ASTM B 160, B 161, B 162 SAE-AMS 5553 Nickel 205 – ASTM F 9, B 162 Nickel 233 – ASTM F 1, F 2, F 3, F 4 27 Fig 9 Thermal conductivity of nickel alloys Fig 10 Linear thermal expansion of Nickel 200 28 Copper Alloy C72500 Resistance to Stress Relaxation C72500 is a copper-nickel-tin alloy developed for electronic applications where a combination of excellent solderability, high strength and resistance to stress relaxation is required (Table 10 and Fig. 11). Applications of C72500 include: connector and relay springs, clips, lugs, spade terminals, wire wrap and posts and printed circuit board card edge connector contact posts. C72500 is superior to phosphor bronze alloy C51000 in this important spring property in the highly worked condition. This advantage should also be true in other common commercial tempers. Directionality Economical use can be made of C72500 because the transverse and longitudinal properties are quite similar, allowing design freedoms. Directionality is similar to the nickel-silver alloys. Other Properties Corrosion Resistance Copper alloy C72500 combines excellent corrosion resistance with superior oxidation resistance at ambient conditions. It is possible to eliminate a protective plating for many uses because of this combination of properties. Alloy C72500 wire has successfully passed the test for electrolytic stresscorrosion cracking susceptibility to nitrate salts in high-humidity conditions. The alloy shows excellent resistance to stress corrosion cracking in most ammoniacal environments. Fabricability C72500 may be formed by any of the conventional fabrication techniques. It often does not require gold plating for solderability; thus it is possible to realize cost savings by selective plating or cladding only in the contact areas. C72500 is available in the following mill forms: sheet, strip, plate, wire, and tubing. Solderability The corrosion and oxidation resistance of C72500 imparts excellent solderability. After exposure at 150°F and 100% relative humidity for two years, C72500 was still solderable. Fatigue Strength 8 Reverse bending fatigue life at 10 cycles is comparable with other copperbase spring materials at equivalent tempers. Higher levels of cold working increases the fatigue strength of C72500 over similarly cold-worked phosphor bronze. 29 Table 10 Properties of C72500 Chemical Composition, % Nickel 9 nominal Tin 2 nominal Manganese 0.30 maximum Iron 0.60 maximum Zinc 0.50 maximum Lead 0.05 maximum Copper Balance Physical Properties Density 0.321 lb/in.3 8.89g/cc Melting Point 2064 °F 1129 °C 335 Btu • in./h • ft2 • °F 47.8 W/(m • °K) Thermal Conductivity at 68 °F (20 °C) Electrical Conductivity 68 °F (20 °C) 11% IACS Electrical Resistivity 68 °F (20 °C) 94 ohm • cmil/ft 15.6 microhm • cm 9.2 × 10–6 in./in./°F 16.6 × 10–6 cm/cm/°C Thermal Expansion 77 °-572 °F (25 °-300 °C) Mechanical Properties Temper (% Reduction) Soft (0) ¼ Hard (11) ½ Hard (21) Hard (37) Ex-Hard (50) Spring (60) Super Spring (~ 95) Tensile Strength, ksi MPa 55 60 70 82 87 95 115 380 415 480 565 600 655 790 Yield Strength @ .2% (offset) @ .01% 23 53 66 78 84 89 110 17 32 40 49 51 55 70 30 Elongation in 2 in. (50.8 mm),% 37 20 6 2 1.5 1.5 1.5 Hardness Hardness HRB Vickers 45 71 78 85 88 90 99 – 127 144 165 176 185 234 Fig 11 Mechanical properties of copper-nickel-tin alloy C72500 (Composite average data vs rolling direction for combined gages) 31 Fig 11 Mechanical properties of copper-nickel-tin alloy C72500 (Composite average data vs rolling direction for combined gages) (Continued) 32 Copper Alloy C76200 Directionality C76200 is a nickel silver alloy (59Cu12Ni-29Zn) that has excellent cold working characteristics and good ductility in hard tempers (Table 11 and Fig. 12). Applications of C76200 include currentcarrying springs for relays, condensers, rheostats and other components and assemblies where soldering, brazing and plating are necessary. There is little difference in the transverse and longitudinal mechanical properties of C762000 and it is unnecessary to make allowances for directionality in designing with this alloy. Fabricability C76200 can be formed by any of the conventional fabricating procedures. It has excellent cold working characteristics, retaining useful formability after cold rolling to high strength levels. Thus, parts requiring severe bending, such as springs, which would fracture in more brittle metals, can be made in C76200. Other Properties Corrosion Resistance C76200 has good resistance to tarnishing and corrosion in industrial, marine and rural atmospheres. The nickel content of this alloy makes it more resistant to stress-corrosion cracking than copper-zinc yellow brass. Resilience and Stiffness Solderability and Plateability The relatively high modulus of elasticity of C76200 (18,000 ksi) makes it a spring material with the ability to maintain good contact pressures and at the same time can be displaced more than steel without taking a permanent set. This combination of properties provides a damping characteristic important in stacked springs used in communications equipment where minimum vibration is desired. C76200 has good solderability and can be joined readily with lead-tin solders using conventional activate resin fluxes. The minimal non-refractory oxide film formed on C76200 is easily removed for plating or brazing as well. Fatigue Strength Reverse bending fatigue life of C76200 8 alloy at 10 cycles is similar to that of other copper-nickel-zinc alloys at equivalent tempers (23000 to 33000 psi). With its superior corrosion resistance, the corrosion-fatigue life of C76200 is superior to that of the copper-zinc brasses in many environments. Resistance to Stress Relaxation The behavior of C76200 is similar to that of C77000. Recent 1000-hour tests at room temperature have shown relaxation ranging from 0.5% under an initial surface stress of 10.9 ksi (75 MPa) to 9.5% under an initial surface stress of 71 ksi (489 MPa). 33 Table 11 Properties of C76200 Chemical Composition, % Copper 59 Nickel 12 nominal nominal Lead 0.10 maximum Iron 0.25 maximum Manganese 0.50 maximum Total Other Elements 0.05 maximum Zinc Balance Physical Properties Density 0.310 Ib/in.3 8.58 g/cm3 Melting Point 1900 °F 1040 °C 864 Btu • in./h • ft2 • °F 41.9 W/(m • °K) 9% IACS 0.05 megmho • cm 115 ohm • cmil/ft 19 microhm • cm 8.5 × 10–6 /°F 16 × 10–6 /°C Thermal Conductivity 68 °F (20 °C) Electrical Conductivity 68 °F (20 °C) Electrical Resistivity (annealed) 68 °F (20 °C) Thermal Expansion 68°-572 °F (20°-300 °C) Modulus of Elasticity (tension) 18,000,000 psi 124,000 MPa Modulus of Rigidity 6,800,000 psi 46,800 MPa Mechanical Properties (Typical) Temper (% Reduction) Annealed (0) ¼ Hard (11) ½ Hard (21) Hard (37) Ex-Hard (50) Tensile Strength ksi MPa 58 400 73 505 83 570 98 675 108 745 Yield Strength (0.5% Extension) ksi MPa 33 225 52 360 70 480 90 620 98 675 34 Elongation in 2 in. (50.8 mm), % 44 35 18 4 2 Hardness HRB 44 73 85 92 96 Vickers 86 132 164 188 220 Fig 12 Mechanical properties of nickel-silver alloy C76200 35 Fig 12 Mechanical properties of nickel-silver alloy C76200 (Continued) 36 Copper Alloy C77000 Directionality C77000 is a nickel silver alloy (55Cu18Ni-27Zn) that work hardens to a yield strength that is superior to that of most other copper-base alloys (Table 12 and Fig. 13). Applications of C77000 include relay springs, multi-point circuit board connectors and sockets, and low profile soldered and wire-wrap sockets for integrated circuits. The transverse and longitudinal properties of C77000 are quite similar and, therefore, it is not necessary to make allowances for directionality in designing parts to be produced from this alloy. Fabricability C77000 may be fabricated by all of the conventional forming techniques. It has excellent cold working characteristics. C77000 is available in the following mill forms: sheet, strip, tube, rod and wire. Other Properties Corrosion Resistance C77000 has good resistance to tarnishing and corrosion in industrial, marine and rural atmospheres and in fresh and saline waters. The alloy can be used without a protective coating in applications involving sliding of one surface over another. The nickel content of this alloy increases its resistance to stress corrosion cracking in ammoniacal environments over that of simple copperzinc alloys of equivalent copper content. Solderability C77000 has good solderability and can be joined readily with soft solders using normal activated resin fluxes. Fatigue Strength 8 Reverse bending fatigue life at 10 cycles is higher than that of the phosphor bronzes at equivalent tempers. Recent tests of C77000 hard temper sheet showed a fatigue strength of 35 ksi 241 MPa (24.6 kgf/sq mm) at 8 10 cycles. Resistance to Stress Relaxation C77000 occupies an intermediate position between phosphor bronze and beryllium copper in resistance to stress relaxation at room temperature. 37 Table 12 Properties of C77000 Chemical Composition, % Copper 55 nominal Nickel 18 nominal Lead 0.10 maximum* Iron 0.25 maximum Manganese 0.50 maximum Total Other Elements 0.50 maximum Zinc Balance * For rod and wire, maximum is 0.05%. Physical Properties Density 0.314 Ib/in.3 8.70 g/cm3 Melting Point 1930 °F 1055 °C 612 Btu • in./h • ft2 • °F 29.3 W/(m • °K) 5.5% IACS 0.0319 megmho • cm 189 ohm • cmil/ft 31.4 microhm • cm 9.3 × 10–6 /°F 16.7 × 10–6 /°C Thermal Conductivity 68 °F (20 °C) Electrical Conductivity 68 °F (20 °C) Electrical Resistivity (annealed) 68 °F (20 °C) Thermal Expansion 68°-572 °F (20°-300 °C) Modulus of Elasticity (Tension) 18,000,000 psi 124,000 MPa Modulus of Rigidity 6,800,000 psi 46,800 MPa Mechanical Properties (Typical) Temper (% Reduction) Annealed (0) Hard (37) Ex-Hard (50) Spring (60) Tensile Strength ksi MPa 60 413 100 689 108 745 115 793 Yield Strength (0.5% Extension) ksi MPa 27 185 85 585 90 620 – – 38 Elongation in 2 in. (50.8 mm), % 40 3 2.5 2.5 Hardness HRB 55 91 96 99 Vickers 100 190 216 234 Fig 13 Mechanical properties of nickel-silver alloy C77000 39 Spinodal Copper Alloy C72900 C72900 is a new copper-nickel-tin alloy with exceptionally high elastic strength levels, resistance to stress relaxation at elevated temperatures, excellent dimensional stability after forming and heat-treating and excellent corrosion resistance. This combination provides designers with new possibilities for high-performance miniaturized sockets, connectors, springs and other precision-stamped parts in electronics applications. Properties are shown in Table 13 and Figs. 14, 15, 16, and 17. Excellent plateability, solderability, corrosion resistance and nearly constant electrical conductivity up to 250°C are additional attributes. Note.—Much of the data on C72900 is from “Demands on Connectors Lead to New Materials Development,” W.T. Ward, Electronics , June 1984. 40 Table 13 Properties of C72900 Chemical Composition, % Copper 77 nominal Nickel 15 nominal Tin 8 nominal Manganese 0.05-0.30 Iron 0.50 maximum Zinc 0.50 maximum Columbium 0.10 maximum Magnesium 0.15 maximum Lead* 0.02 maximum Density 0.323 lb/in.3 8.40 g/cm3 Melting Point 1742 °F 950 °C 612 Btu • in./h • ft2 • °F 29.7 W/(m • °K) * 0.005 if hot rolled. Physical Properties Thermal Conductivity 68 °F (20 °C) Electrical Conductivity 68 °F (20 °C) 7.8% IACS 0.043 megmho • cm 392 °F (200 °C) 7.3% IACS 0.041 megmho • cm 9.1 × 10–6 /°F 17 × 10–6 /°C Modulus of Elasticity (Tension) 18,500,000 psi 127,000 MPa Modulus of Rigidity 7,500,000 psi 51,700 MPa Thermal Expansion 68°-572 °F (20°-300 °C) Tensile Properties at Various Tempers ASTM B601 Ultimate Tensile Strength Temper ksi MPa As rolled (after soln. treat & C.W.) TB00 TD01 TD02 TD04 TD08 TD12 64-85 74-100 85-110 100-125 122-140 135-150 Yield Strength (.05% offset) ksi MPa %E 441-585 509-689 441-758 689-861 840-965 930-1034 24-34 50-66 65-84 85-108 100-125 110-130 165-234 345-455 448-579 441-744 689-861 758-896 32 18 8 <2 <2 <2 105-135 120-146 130-154 145-167 160-184 165-197 723-930 827-1006 896-1061 999-1151 1102-1268 1137-1357 60-102 90-117 105-128 130-147 145-166 152-175 413-703 620-806 723-882 896-1013 999-1145 1047-1206 10 8 5 3 2 <2 110-125 120-133 130-142 140-155 150-178 758-861 827-916 869-978 965-1068 1034-1226 75-95 90-110 105-125 120-145 140-170 517-655 620-758 723-861 827-999 965-1171 26-36 20-30 14-24 8-16 2-10 Hardness HR30N Aged (after spinodal H.T.) TX00 TS01 TS02 TS04 TS08 TS12 Mill Hardened TM00 TM02 TM04 TM06 TM08 Note: Data from Connectors and Interconnections Handbook - Vol. 4., Electronic Connectors Study Group, 1983 41 36-44 43-48 47-52 50-55 52-58 Fig 14 Yield strength vs ductility of C72900 alloy 42 Fig 15 Bend formability of C72900 alloy 43 Fig 16 Thermal relaxation of C72900 alloy 44 Fig 17 Electrical conductivity vs temperature of C72900 alloy 45 Stainless Steel Alloys AISI 301* and 304* AISI 304 and 304L AISI 301 and 304 are two widely-used 18Cr-8Ni stainless steels, work hardenable to high strength levels and with excellent corrosion resistance, weldability and formability. The outstanding spring properties developed in AISI 301 at both ambient and elevated temperatures lead to its application in non-current carrying springs of all sizes. The corrosion resistance and fabricability of AISI 304 lead to many uses as structural members of components and protective enclosures for system assemblies where strength, toughness, durability and protection from aggressive and corrosive environments are necessary. Composite stainless strip using precious metal cladding, inlay or plating makes it possible to obtain the structural and spring properties of stainless steel with the contact properties of a highly conductive metal stripe, spot or layer at an economical cost. Properties of AISI 301 and 304 are shown in Table 14. Type 304 (and its low-carbon variant 304L), the most widely used stainless grade, will withstand ordinary rusting, is immune to most food processing environments, organic chemicals, dyestuffs and a wide variety of inorganic chemicals. It resists many oxidizing acids (e.g., nitric acid, cold concentrated sulfuric acid, peracetic acid). It can be used in electronic packaging applications or as a structural or enclosure material for electronic or electrical components and systems where high reliability and protection from aggressive or corrosive environments are necessary. Type 304L is used where the regular carbon grade would be sensitized to intergranular corrosion, as by welding or hotforming during fabrication. Titanium- or columbium-stabilized variants (e.g., Types 321 or 347) are used for elevated temperature service. AISI 301 AISI 301 stainless steel, because of its higher carbon and lower alloy content, can be work hardened to higher strength levels than other austenitic grades. It is widely used in electrical and electronic spring applications where excellent spring characteristics, endurance limits and high stress relaxation properties combined with corrosion resistance are needed. The effect of cold work on AISI 301 is shown in Fig. 18. *UNS S30100 and S30400 46 Table 14 Properties of Stainless Steel Chemical Composition, % AISI 301 (S30100) AISI 304 (S30400) AISI 304L (S30403) Carbon Manganese Phosphorus Sulfur Silicon Chromium Nickel 0.15 2.00 0.045 0.030 1.00 16.00-18.00 6.00-8.00 0.08 2.00 0.045 0.030 1.00 18.00-20.00 8.00-10.50 0.03 2.00 0.045 0.030 1.00 18.00-20.00 8.00-12.00 Molybdenum Iron – Bal. – Bal. – Bal. Physical Properties of AISI 301 and 304 Melting Point 2550-2650 °F (1398-1454 °C) Density lb/in3(kg/m3) 0.29 (8060) Specific Heat btu/Ib/°F 0.12 (503) (J/kg/K)32-212 °F(0-100 °C) Thermal Conductivity btu/h/ft2/ ft/°F(J/kg/°K)212 °F(100 °C) 932 °F(500 °C) 9.4 (0.113) 12.4 (0.149) Mean Coeff. of Thermal Expansion x 10–6 /°F( × 10–6 /°C) 32-212 °F(0-100 °C) 9.6 (17.3) 32-600 °F(0-315 °C) 9.9 (17.9) 32-1000 °F(0-538 °C) 10.2 (18.4) 32-1200 °F(0-648 °C) 10.4 (18.8) Modulus of Elasticity Tension, psi (MPa) Torsion, psi (MPa) 29,000,000 (193,000) 12,500,000 (86,200) 47 max max max max max Fig 18 Effect of cold work on mechanical properties of Type 301 stainless steel 48 Nickel Electroplating Evaluation and Testing, Preparation and Elimination of Rejects Electrodeposited nickel is widely used in electronic components and parts to improve corrosion resistance as a barrier underplate between a basis metal and a gold or silver contact or bonding area, to prevent migration of aluminum dendrites or copper atoms into the precious metal. Corrosion and Porosity Tests Examination of the coated part after immersion in hot water for 2 to 5 hours for rust is one technique used in studying the corrosion resistance of plated steel. The number of rust spots in a given area is then used as the qualification for accepting or rejecting the piece. Modifications of this test include immersion for up to 5 hours in distilled water, in distilled water saturated with carbon dioxide, or in distilled water containing 0.5 per cent by weight sodium chloride, at test temperatures of 82 to 85°C (180 to 185°F). Several salt spray tests have been used to simulate marine environments. These tests are commonly used to evaluate nickel and nickel-chromium coatings on ferrous and non-ferrous substrates. The salt spray tests are also used as accelerated quality control tests and are described in the following ASTM standards: The producer and end-user of a plated article are always concerned with the quality of the end-product. Methods that measure the thickness, the adhesion, and the corrosion resistance of the coating are available as means of quality control. Properties such as porosity, ductility, tensile strength, internal stress, hardness, and wear resistance are important in industrial nickel plating applications and can be measured to control the quality of electroplating articles. Evaluation and Testing 1) Salt Spray (ASTM B 117). Thickness 2) Acetic Acid-Salt Spray (ASTM B 287). Accurate methods for determining the thicknesses of electrodeposited coatings can be found in ASTM and other national and international standards. Equipment is available for tests involving magnetic (ASTM B 530), X-ray fluorescence, magnetic inductance (ISO 2178), beta backscatter (ASTM B 567), and coulometric (ASTM B 504) measurements of thickness. Micrometer readings are often used to determine the thickness of a coating at a particular point when the deposit thickness exceeds 125 µm (0.005in). ASTM B 487 describes a method based on metallographic examination of cross sections of the plated object. 3) Copper-Accelerated Acetic AcidSalt Spray (CASS Test: ASTM B 368). The ferroxyl test is another porosity test which is employed for coatings on ferrous metal substrates and involves the formation of Prussian blue color within exposed pits. The solution utilizes sodium chloride and potassium ferricyanide as reagents to develop the color. The only truly satisfactory method of establishing the relative performance of various coating systems is by service testing. Care should, therefore, be exercised in interpreting the results of 49 Ductility accelerated corrosion tests. Once an acceptable service life has been determined for a specific thickness and type of coating, the performance of other candidate coatings may be compared in accelerated corrosion tests to the performance obtained with the coating for which an acceptable service life has been established. Most of the tests that have been used for evaluating the ductility of plated coatings are rather qualitative in nature. Two bend tests are described in ASTM B 489 and B 490. Both of these procedures require a minimum amount of equipment. Another method for measuring the ductility of thick deposits is to determine the elongation of a specimen in a tensile testing machine. This method is limited to relatively thick foils of controlled geometry and thickness. A method specifically designed for plated thin foils has been used and is known as the hydraulic bulge test. Hardness Hardness measurements involve making an indentation on the surface (or cross section for thin coatings) of the deposit. The indenter has a specified geometry and is applied with a specified load. In the case of industrial nickel coatings, the most common hardness determination is the Vickers method of forcing a diamond point into the surface under a predetermined load (normally 100). This provides a measure of that surface to permanent deformation under load. The figure obtained is not necessarily related to the frictional properties of the material nor to its resistance to wear or abrasion. Adhesion The adhesion of a coating to the basis material is important. In general, the adhesion between a nickel coating and the basis material exceeds the tensile strength of the weaker material. As a result, when a force is applied to a test specimen which tends to pull the coating away from the basis metal, separation occurs within one of the two metals rather than at the boundary between the basis metal and the nickel coating. A number of qualitative tests have been used which utilize various forces applied in a multitude of directions with regard to the composite basis metal and coating, such as hammering, filing, grinding, and deforming. Two tests are recommended in ISO 1456 and 1457. The first is a simple file test where a sample is held in a vise and the file is used at an angle of 45° in an attempt to raise the deposit–poorly adherent deposits are easily raised. The second test involves heating the sample or component in an oven (to 300°C (572°F) for steel, 150°C (302°F) for zinc alloys and 250°C (482°F) for copper alloys), followed by quenching by water at room temperature. The rapid contraction of the metal detaches any poorly adherent deposit. Tensile Strength The measurement of the tensile strength of an electrodeposited coating is performed after the coating is separated from the basis metal; and the coating is then pulled in a tensile machine. In general, plating plant operators seldom perform this test. Internal Stress The magnitude of internal stress obtained in deposits is determined by plating onto one side of a thin strip of basis metal and measuring the force causing the strip to bend. One method used in commercial practice involves plating the exterior surface of helically wound strip and measuring the resultant change of curvature. Another method is based on the flexure of a thin metal disc. 50 receptivity to electroless nickel coating as follows: Preparation of Basis Metals for Plating 1) Directly Coated – iron, cobalt, nickel, platinum metals, aluminum, beryllium and titanium alloys (aluminum, beryllium and titanium require special pretreatment and post-plating heat treatment to insure adequate adhesion.) 2) Indirectly Coated by Galvanic Initiation – preliminary electrolysis or contact to a catalytic metal is required for copper, silver, gold, carbon, vanadium, molybdenum, tungsten, chromium, selenium, and uranium. 3) Indirectly Coated by First Nickel plating for engineering and industrial uses requires a sound bond between the substrate and the coating. The coating should adhere tightly to the basis material. A sound metallurgical bond may be achieved on most materials. The selection of grinding, polishing, pickling and conditioning treatments for a variety of basis metals varies from one material to another, and depends on the initial surface condition of the metal. The activating treatments which follow, polishing and cleaning operations are listed in Table 15 for the basis metals most commonly plated. The ASTM standards referred to provide additional information. Table 16 gives selected procedures for the preparation of less commonly plated basis metals which are coated with nickel. Units commonly used in the plating industry are listed in Table 17. Alloys containing lead, on the surface or as part of the composition of the metal being plated, can lead to poor adhesion. The presence of lead can be overcome by a cleaning cycle that includes, for example, a combination of fluoboric plus other mineral acids in the acid part of the cleaning cycle. Non-conductive plastics and other materials can be plated by metallizing the material, using etching and catalyzing techniques. The mechanism of adhesion between metal and plastic is not fully known. A mechanical “locking” or “keying” action may take place at the plastic to metal interface and thereby provides for a moderately adherent deposit. Further information on plating of plastics may be obtained by contacting plating supply houses. A clean surface is as essential in electroless nickel plating as it is in normal electroplating. Certain metals, however, cannot be coated directly with electroless nickel because they do not catalyze the reduction of nickel. Metals can be categorized with respect to Striking with Copper or Other Metal – bismuth, cadmium, tin, lead, and zinc. In the case of electroless nickel plating on certain metals, heat treatment improves the adhesion between the coating and the substrate. For aluminum, titanium, nickel, and steel alloys, the following heat treatments are recommended: Aluminum & Alloys Steel Nickel & Alloys Titanium 140°C 175°C 210°C 400°C (284°F) (347°F) (410°F) (752°F) 1h 3h 6h 1h Elimination of Rejects On average, platers are likely to lose three per cent of output due to rejects. Rejects arise mainly from the following defects: Blistering or detached plating Pitting Roughness High stress and low ductility Discoloration or poor mechanical properties at low-current-density areas Burning (cracking) at high-currentdensity areas Accidental damage Poor preparation of the basis metal 51 Table 15 ASTM recommended practices for preparing metals for plating Conditioning Step 1 Solution Conditioning Step 2 (if needed) Basis Metal ASTM Operation Solution Aluminum alloys B 253 Alkaline zincate Immerse long enough to deposit .02 to .05 mg Zn/ cm2 Copper alloys B 281 Sulfuric or hydrochloric acid soln. Acid dip Iron castings B 320 Sulfuric or hydrochloric acid soln. Room temp Brief dip Cold water rinse Lead alloys B 319 Fluoborate dip 10% HBF4 Dip 10 to 15 seconds Rochelle type copper strike. pH 10.2 to 10.5 Final Rinse Before Plating Operation 2 Deposit Cu at 258 A/m (24 A/ft2) for 2 min then 129 A/m2(12 A/ft2) for 4 min Double rinse or spray Single rinse or spray 2 Anodic clean Anodic at 646 to 1076 A/m2 (60 to 100 A/ft2) to remove smut Rinse, acid dip, then cold water rinse Cold water rinse and spray 2 Nickel B 343 Acid nickel chloride 323 A/m (30 A/ft ) soln. 240 g/L anodic 2 min (32 oz/gal) plus cathodic 6 min HCI 94 mL/L (12 fl oz/gal) Stainless steels B 254 65% H2SO4 Cathodic 2 min Acid nickel chloride 240 g/L (32 oz/gal) plus HCI 94 mL/L (12 fl oz/gal) Cathodic 2 min at 1614 A/m2 (150 A/ft2) None Steels, low carbon B 183 Alkaline anodic clean Anodic at 6 volts for 1 to 2 min. Cold water rinse 4 to 10 vol per cent H2SO4 Dip at room temp for 5 to 15 secs Cold water rinse Steels, high carbon B 242 Smut removal Sodium cyanide soln. Dip or short anodic treatment. Rinse H2SO4 250 to 1000 g/L (34 to 134 oz/gal) plus 125 g/L (17 oz/ gal) Na2SO4 Keep below 25 °C (77 °F) Anodic at 1076 to 4304 A/m2 (100 to 400 A/ft2) for not more than 60 sec Fast rinse Zinc alloys B 252 Copper strike soln. Deposit 1.3 µm Rochelle type (50 millionths in.) Cu Cyanide copper plating bath Copper plate 5 µm (0.2 mil) thick Cold water 42-50% Nickel-iron alloys 25% H2SO4 21-26 °C None Anodic at 20 A/dm2 (200 A/ft2) for 3 min. after onset of passivity Rinse 52 53 3. Alkaline clean 4. W 3. Alkaline clean 4. W 5. HF dip 219 mL/L (28 fl oz/gal) Time: 10 min W = water rinse. v/o = vol. % W/o = wt. % 12. Heal for 1 h at 500 °C (930 °F) 15. Nickel plate 14. W 13. Cyanide copper plate 7.6 µm (0.3 mil) copper deposit 12. W 11. Dow zinc Immersion treatment 11. Dry 10. W 10. W 9. Activating dip Phosphoric acid 20 v/o NH4HF2 100 g/L (13 oz/gal) for electrodeposited Ni replace steps 9-11 by following: 11. Electroless nickel (Dow process) 10. W 9. Hydrofluoric dip 54 mL/L (7 fl oz/gal) 10 minutes 8. W 7. Dow #5 etch 6. W 2. Outgas at 980 °C (1800 °F) 2h in Hydrogen 2. W 12. Nickel plate 11. W 10. Nickel strike 240 g/L (32 oz/gal) NiCl2 • 6H2O 94 mL/L (12 fl oz/gal) HCI 2 C.D. 538 A/m 2 (50 A/ft ) Cathodic 9. Dip in 50 v/o HCI 8. W 7. Chromium plate (low contraction) CrO3 404 g/L (54 oz/gal) Sulfate 1/100 2 C.D. 8070 A/m 2 (750 A/ft ) 82 °C (180 °F) 6. W 5. Alternate anodic etch CrO3 100 g/L (13.4 oz/gal) Na2Cr2O7 11 g/L (1.3 oz/gal) Time: 2 min 21-24 °C (70-75 °F) 2 C.D. 3766 A/m 2 (350 A/ft ) 5. Anodic etch H2SO4(96%) 50v/o H2PO4(85%) 50v/o Tine: 2-3 min 2 C .D. 215-1076 A/m 2 (20-100 A/ft ) 1. Prepare fresh surface by grinding 1. Degrease and descale Molybdenum 16. Heat at 760 °C (1400 °F) for 2 min 15. Dry 14. W 11. Nickel plate 12. W 11. Nickel strike Acid NiCl2 10. Etch HCl (40%) 50 v/o 9. W 8. Chromium plate CrO3 403 g/L (54 oz/gal) Sulfate 1/100 2 C. D. 10760 A/m (1000 AM) Temp. 85 °C (185 °F) 7. W 6. Activate HF (48%) 12.5 v/o Acetic (99%) 87.5 v/o Soak 10-15 min Connect A.C. 60 cycle 10 mm 2 at 161-323 A/m 2 (15-30 A/ft ) 5. Dry 4. W 3. Bright dip HF (48%) 18.5 v/o HNO3 (70%) 1 v/o Temp. 21-24 °C ° (70-75 F) ½ to 2 min 2. W. 1. Degrease Titanium Uranium 9. W 7. Nickel strike Acid NiCl2 2 60 sec at 430 A/m 2 (40 A/ft ) 9. Nickel plate 10. Nickel plate in Wafts bath 8. W 6. Spray rinse 5. W 7. Neutralize in satd soln of sod. bicarbonate 6. Rinse and spray 5. W 4. Dip in clean conc HNO3 60 sec at 70 °C (158 °F) 3. Soak in conc HNO3 8 min at 95 °C (203 °F) 2. W 1. Cathodic alkaline clean 4. W 3. Chromium plate Standard soln 100 1 ratio Time: 20-30 sec Temp 4957 °C (120-135 °F) 2 C.D. 2152 A/m 2 (200 A/ft ) 2. W 1. Anodic Electropolish trisodium phosphate 15 w/o Time: 10-60 sec Temp 49 °C (120 °F) Tungsten Vanadium Alkaline clean soak at 82-93 °C (180-200 °F) 7. Nickel plate Watts–pH 4.0 60 °C (140 °F) 2 C.D. 54-1076 A/m 2 (5-100 A/ft ) 6. W 5. Catholic treatment In 2 w/o H2SO4 Time: 5-15 sec ° Temp. 24-29 C ° (70-85 F) 2 C.D. 108-1076A/m 2 (10-100 A/ft ) 4. W 3. Etch in 10 w/o HF 2. W 1 Table 16 Preparation of Basic Metals Less Commonly Plated Magnesium 9. Nickel plate Watts bath 8. W 7. Nickel strike Nickel sulfate 142 g/L (19 oz/gal) Mg sulfate 75 g/L (10 oz/gal) Am. chloride 15g/L (2 oz/gal) Boric acid 15 g/L (2 oz/gal) Wetting agent pH 5.5 30 min 32 °C (90 °F) 2 C.D. 161 A/m 2 (15 A/ft ) 6. W 5. Add dip conc HNO3 2 minutes 27-32 °C (80-90 °F) 4. W 3. Anodic pickle Phosphoric 10 v/o Hydrochloric 2 v/o 2 min 27 °C (80 °F) 2 538-1076 A/m 2 (50-100 A/ft ) 2. W 1. Degrease Beryllium Zirconium Descale Nickel plate Watts bathsod. acetate 15 g/L (2 oz/gal) pH 4-0 No wetting agent 9 12. Heat at 677 °C (1250 °F) for 30 min in vacuum 11. Dry 10. W W Etch (U.S 2.711.389) NH4F 36 g/I (4.8 oz/gal) HF 148%) 31 g/L (41 oz/gal) Time. 1-3 min Temp 38 °C (100 °F) W Chemical polish (U.S. 2.711.364) NH4HF2 100 g/L (13.3 oz/gal) HNO3(70%) 40v/o H2SiF6(48%) 20v/o Time 45-180 sec Temp 38 °C (100 °F) W Alkaline clean 8 7 6 5 4 3 2. Outgas at 204 °C (400 °F) 2-4 h 1 Table 17 SI Units for the Plating Industry To convert from A to B B to A Multiply by Quantity A Conventional unit B SI unit Coating thickness mil (= .001 in.) (in.) µm mm Coating weight mg/in.2 2 mg/in. 2 oz/in. oz/ft2 g/m2 2 mg/cm 2 kg/m kg/m2 1.55 0.155 43.9 0.305 Current density A/ft A/in.2 2 A/in. A/m2 A/m2 2 A/cm 10.76 1550 0.155 .0929 6.45 × 10–4 6.45 2 As/m - µm 1530 6.55 × 10 Plating rate 2 Ah/ft - mil 2 3 Volume gallon Mass concentration oz/gal m L mL g/L 3 kg/m Volume concentration fl oz/gal mL/L 3 cm /L fl oz Pressure 1000 psi 25.4 25.4 .00379 3.79 29.6 2 MPa (MN/m ) ASTM Committee B 08, Subcommittee 1. 54 .0394 .0394 0.645 6.45 .0228 3.28 –4 264 0.264 .0338 7.49 0.134 7.81 0.128 6.89 0.145 Too low a concentration of wetting agent Blistering or Detached Plating Process blisters which occur during, or immediately after, plating on zincbased diecastings are generally due to subsurface porosity and surface imperfections such as cold shuts and local sites of corrosive attack that sometimes occur on stored, unplated diecastings. The components should be carefully inspected by the plater before acceptance for plating. Unplated diecastings should be wrapped if they are to be stored for long periods. Lack of adhesion may be due to: Other causes of pitting are: The presence of organic contaminants Presence of copper ions and other inorganic contaminants Incomplete cleaning of the basis metal Incomplete solution of additions of the leveling agent coumarin which, at plating temperatures, forms oily globules which settle on the work to form characteristically wide, shallow pits Incomplete removal of grease, oil or oxides Formation of metal soaps from polishing compounds Roughness This is caused by the incorporation in the deposit of insoluble particles present in the solution. These particles arise from: Films of silica from cleaning solutions or chromate trapped in damaged coatings on racks and then returned to the cleaning solution Incomplete cleaning Incorrect application of such intermediate deposits as cyanide copper, acid copper and acid chloride solutions Detached flakes of deposit from the racks Dust carried into the vat by air currents and the air-agitation pipes Pitting Metallic residues from the anode Most pitting is caused by adhesion of air or hydrogen bubbles to the work. Air bubbles occasionally appear in a solution which has been heated after standing cold for some time, during which it dissolves air. The cure is to heat the solution above its normal operating temperature for a short period to expel the air. If air leaks into the filtration system and forms bubbles within a critical range of size, these will cling to the cathode and cause pitting. Pitting from adherent hydrogen bubbles can result from: Insoluble salts in the solution caused by incorrect composition or contamination Airborne dust can be controlled by installing the surface-preparation and polishing workshops well away from the plating area, providing an adequate supply of clean air, removing dirt from all areas near and above the vats and protecting the vats against condensation droplets which tend to carry dissolved dirt into the solution. Anode residues must be retained within the anode bags. Escape of residues into the solution can be caused by: A solution which is chemically out of balance Too low a pH Inadequate agitation Faulty bags or bags of inferior quality Incorrect racking of complicated components Disturbance of the bags 55 Accidentally raising the solution level above the normal working level (this may cause the solution to wash over the top of anode baskets) High- or Low-CurrentDensity Effects Discoloration or inadequate mechanical properties can be caused in low-current-density areas as a consequence of metallic contamination of the solution. The effects can be examined systematically by plating over a reproducible range of current densities on a Hull-cell cathode under standard conditions. Burning may occur at highcurrent-density areas as a result of phosphate entering the solution via contaminated activated carbon. When phosphate has been introduced accidentally the maximum current density 2 2 should be reduced to 4.0 A/dm (40 A/ft ) to minimize burning. Burning can also be caused if the full rectifier output is applied to the lowest components on a rack being lowered into the solution. This can be avoided by applying a reduced current during immersion. Pieces of nickel which drop to the bottom of the vat and become bipolar, where they dissolve in the solution and, since they are outside the anode bags, their residues are released into the solution Anodes should always be withdrawn slowly from the plating solution to avoid disturbing any residues and, for the same reason, never stood on the floor. Formation of insoluble salts in solutions due to incorrect composition can be prevented by regular analysis. Hard water used for topping-up can form insoluble calcium sulfate which tends to deposit on the anodes, anode bags and around the holes in the air-agitation pipes. In hard-water areas the installation of deionizing or water-softening plant should be considered. Continuous filtration at a rate which turns over the plating solution at least once per hour should be used during plating operations. Accidental Damage Reduction of accidental damage through mishandling is mostly a question of educating operators and of providing a clear and uncluttered working area. Often work is handled less carefully when piecework schemes are operated. An additional bonus for low rejects is sometimes offered to reward careful working. When rejects are to be recovered for re-plating, it is important that they should also be handled with care to minimize polishing requirements. High Stress and Low Ductility Unacceptable values of deposit stress and inadequate ductility result from having addition agents out of balance, or from organic or inorganic impurities. Impaired Brightness This can be caused by: Defects Arising from Incorrect Mechanical Preparation Lack of balance between the addition agents making up the brightener system, which should be referred to the supplier Plated components are often rejected for inadequate polishing. For example, the overall standard of polishing may be too low or the polished surface may cover hidden defects such as pores and holes which have been “flowed over” by Metallic or organic contamination Incorrect pH level, current density or operating temperature Too thin a deposit 56 the polisher and which reappear during cleaning and/or etching processes prior to nickel plating. These rejects can often be prevented by proper inspection. Whenever possible, the plating solution should be passed through a separate plating compartment where certain metallic impurities such as zinc, lead and copper can be plated out continuously by lowcurrent-density electrolysis. A few of the sources of organic impurities are: Specification Not Met The most frequent cause of failure to meet specification, particularly when using racks, is the application of too low a plating current and/or too short a plating time, giving too thin a deposit. Another cause, often combined with low average thickness, is non-uniform distribution of current, leading to insufficient deposit in low-current-density areas. Poor electrical contact can also cause thin deposits and attention should therefore be paid to the cleanliness of the anode and cathode bars, the anode hooks and contacts of racks. Quality can only be maintained by tests which include regular checks of thickness. Breakdown of leveling or brightening agents Accidental introduction of lubricating oils or greases from overhead conveyors Oil-contaminated compressed air supply Extracts from rubber tanks and hoses Rack coatings Filter cloths and anode bags Buffing media Accidental contamination by oil or grease is particularly serious when wetting agents are used in the solution, since visual detection and subsequent physical removal from the surface are impossible. In the case of organic contamination, the usual method of purification is as follows: the solution is pumped to an auxiliary tank where it is digested with 6 g/L (1 oz/gal) of activated carbon for several hours. Two such treatments at half strength are more effective than one treatment at full strength. After treatment, the solution is filtered before use. To overcome the inconvenience of batch purification, modern bright nickel solutions may be continuously purified by passing the solution through a filter packed with activated carbon up to 1 g/L (1 lb/100 gal). The organic brighteners are so chosen that their decomposition products may be removed by the carbon without the simultaneous removal of undecomposed brightener agents. In low-current-density purification of solutions containing organic addition agents, the breakdown and consumption of brighteners per ampere hour can Purification of Solutions Very small amounts of metallic and organic impurities in the solution can impair the appearance or mechanical properties of the deposit. For good quality plating, solutions must be maintained in a state of high purity. A few of the many sources of metallic impurities are: Drag-over from preceding treatments Components which have fallen off racks and are allowed to remain in the vat Corrosion products from surrounding equipment and steel roof girders Tools dropped into the vat Impure nickel salts and anodes Metallic contamination is usually from zinc, iron and copper and even in low concentrations these have undesirable effects. Table 18 lists the common metallic impurities and suggests methods for their removal from various types of nickel plating solution. 57 Table 18 Effects of Impurities in Nickel Plating Solutions and Methods of Purification Impurity Chromium Range investigated, PPM Chromiumiii 0-250 0-50 Solution Watts pH 2.2 No effect up to 50 ppm; thereafter deposits are smoother and finer grained Watts pH 5.2 All deposits rough 0-250 Co-Ni pH 3.75 0-125 Organic pH 3.2 Chromate* 0-70 Appearance No effect up to 75 ppm; thereafter organic deposits become milky and Co-Ni deposits become more highly stressed Watts pH 2.2 Whitens deposit 0-15 Watts pH 5.2 Deposits rough, due to precipit-, ated Cr iii Whitening of deposit 0-40 Co-Ni pH 3.75 Unaffected 0-35 Organic pH 3.2 Unaffected Adhesion                                                                 Unaffected provided correct plating conditions were maintained Unaffected if pH and iii Cr content are carefully controlled Ductility corrosion resistance in salt-spray test Hardness                                     Throwing power Decrease after 12.5-25 ppm Decrease at all concentrations Decrease after 5 ppm Increase with increasing concentralion Decrease after 50 ppm Slight increase: (max at 12.5 ppm) Decrease after 25 ppm Decrease (min at 12 ppm) 9-16% decrease Decrease at all concentrations Substantial increase in thick deposits at high concentrations; otherwise no great change Decrease 55-85% decrease Increase (43% at 15 ppm) As for pH 2.2 solution Slight increase 33-60% decrease 25-50% decrease 58  Mainly   decrease  but   variable   Slight increase General decrease in corrosion resistance Slight increase Slight decrease Slight increase Slight decrease   at all thick nesses  and con centrations Slight decrease Slight increase Removal technique Removal by electrolytic means is unsatisfactory. Reduction of Crvi to Criii, using nickel metal at low pH (< 3.0) and agitating. Criii is removed by raising the temperature to 75 °C (165 °F) for several hours and precipitating at high pH (5.2-5.5), using nickel carbonate Table 18 Continued Impurity Copper Range investigated, ppm 0-100 Solution Watts pH 2.2 Watts pH 5.2 Co-Ni pH 3.75 Organic pH 3.2 Iron 0-200 Appearance              Watts pH 5.2 Organic pH 3.5 At 10 ppm milky; at higher concentration deposits dull and rough Whitens deposit at concentrations of 10200 ppm, Some brightness 50-200 ppm Watts pH 2.2 Co-Ni pH 3.75 50 ppm causes blackening in lowcurrentdensity areas         Unaffected up to 200 ppm Adhesion Unaffected up to 100 ppm          Un affected  up to 200  ppm   Ductility Decreases as copper content increases above 10-25 ppm Decreases at 2550 ppm Unaffected up to 200 ppm Decreases at 2550 ppm Hardness Max (+86%) at about 75 ppm; less significant increases for other solutions    Increase  to max at  10-25   ppm; de crease  to min at  50 ppm   then in crease  at higher  concen  trations   Corrosion resistance in salt-spray test Small amounts cause large reduction in corrosionresistance (50% reduction at 40 ppm for all solutions) Slight changes only in thin deposits Unaffected 10-20% increase at 25 ppm. Slight changes only, at all thicknesses Table 18 Continued on Next Page 59 Throwing power Insignificant changes at all concentrations and in all solutions               Insig nificant  changes             Removal technique Lowcurrentdensity treatment. At 0.2 A/dm2 2 (2 A/ft ) Ni: Cu ratio of deposit is twice that obtained at 0.1 A/dm2 (1 A/ft2); at 0.3 A/dm2 (3 A/ft2) it is 15 times as great. High-pH treatment (pH 6.0); reduces Cu to 15 ppm but with loss of nickel Oxidation with H2O2 (1% by volume of 3% H2O2) and high pH (5.55.7) with NiCO3 No loss of nickel Also by lowor highcurrentdensitytreatment Impurity Zinc Range Investigated, PPM 0-300 Appearance Solution Watts pH 2.2 Darkening in lowcurrentdensity areas above 10 ppm, Brightening in highcurrentdensity areas at 300 ppm Watts pH 5.2 Darkening above 10 ppm Co-Ni pH 3.75 Gradual change to dull deposit at 300 ppm Organic pH 3.2 Lead 0-15** Wafts pH 2.2 Watts pH 5.2 Co-Ni pH 3.75 Organic pH 3.2 Improved brightness at 150-300 ppm but darkness in lowcurrentdensity areas                           Pronounced levelling and brightening effects even at low concenttration. Blackening in lowcurrentdensity areas at 20 ppm; otherwise some levelling Adhesion                                                         Ductility            Gradual  decrease            Unaffected up to 300 ppm               Un affected            Little change until 300 ppm, at which concentration deposit becomes unusable Corrosion resistance in salt-spray test Hardness                        General increase; greater at pH 2.2 than at pH 5.2 Increase: (max at 25 ppm) Unaffected Max 5 ppm Min 15 ppm Decrease General increase (50% at 20 ppm) Unaffected Decrease Increase (12% at 10 ppm). Decrease                                                                         Throwing power General decrease General improvement; greatest change in corrosionresistance (10-60% increase) up to 50 PPM General slight increase in corrosionresistance, especially in thicker deposits Slight decrease (8% at 20 ppm) From 25 ppm improve ment Removal technique By lowcurrentdensity treatment at 0.2-0.4 2 A/dm (2-4 A/ft2), down to 1 ppm Cannot be removed by high pH treatment without much loss of nickel               General  improve ment                             General slight decrease Variable at different concentrations. Slight increase By lowcurrent density treatment, 0.1 A/dm2 (1A/ft2) to minimum of 2.5 ppm By high-pH treatment (pH 5.56.0). Some nickel also precipitated at the higher pH *In all tests with chromate impurity some Criii was also present. The concentration of Criii was kept below 40 ppm. **Higher concentrations of Pb are possible, especially in solutions containing organic additions and having a high chloride content. 60 occur at a rate about 3 times that occurring at the work. Thus if 1 per cent of the total plating current is used in lowcurrent-density electrolysis, an extra 3 per cent of brighteners may be used. It pays to avoid excessive destruction of brighteners by controlling the purification process so as to keep the level of metallic impurities just below the level at which they adversely affect the appearance or properties of the deposit. Severe Organic Contamination In some cases of contamination by organic substances, filtration through activated carbon will not bring the solution back to working condition. In these circumstances all organic substances in the solution must be destroyed. Production must be stopped and a small amount of potassium permanganate solution added (0.25–0.75 ml/L of a one gram per litre solution of KMnO 4 ). For heavy contamination a stronger solution of KMnO 4 may be necessary. The amount and strength required can be determined by trials with a small quantity of plating solution by adding permanganate until the color changes. When decomposition of the permanganate is complete, the precipitated manganese dioxide must be filtered off before plating is restarted. If possible the treatment is best carried out in a separate tank to avoid deposition of manganese dioxide on the tank walls, on the anode bags, and so on. This treatment should only be carried out on a proprietary solution after consultation with the plating supplier. 61 Standards and Specifications The most important standards and specifications in this area are those promulgated by the American Society for Testing and Materials (ASTM), Federal Government and Semiconductor Equipment and Materials Institute (SEMI). Copies of these documents are included in the following order: ASTM F 15 Iron-Nickel-Cobalt Sealing Alloy ASTM F 30 Iron-Nickel Sealing Alloys ASTM F 31 42% Nickel - 6% Chromium - Iron Sealing Alloy MIL-I-23011 Iron-Nickel Alloys for Sealing to Glasses and Ceramics MIL-M-38510 Microcircuits, General Specification for (Sections dealing with lead frames and plating or finishes) QQ-N-290 Nickel Plating (Electrodeposited) SEMI G2 Metallic Leadframes for Cer-DIP Packages SEMI G4 Integrated Circuit Leadframe Materials Used in the Production of Stamped Leadframes SEMI G22 Ceramic Pin Grid Array Packages 62 Designation: F 15–78 (Reapproved 1983) Reprinted, with permission, from the Annual Book of ASTM Standards, copyright American Society for Testing and Materials, 1916 Race Street, Philadelphia, PA 19103. Standard Specification for IRON-NICKEL-COBALT SEALING ALLOY1 This standard is issued under the fixed designation F 15; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (ε) indicates an editorial change since the last revision or reapproval. 1. Scope 3.1.5 Certification if required. 1.1 This specification covers an iron-nickelcobalt alloy, containing nominally 29% nickel, 17% cobalt, and 53% iron, in the forms of wire, rod, bar, strip, sheet, and tubing, intended primarily for sealing to glass in electronic applications. 1.2 The values stated in inch-pound units are to be regarded as the standard. 4. General Requirements 4.1 The material shall be commercially smooth, uniform in cross section, in composition, and in temper; it shall be free of scale, corrosion, cracks, seams, scratches, slivers, and other defects as best commercial practice will permit. 5. Chemical Requirements 5.1 The material shall conform to the requirements as to chemical composition prescribed in Table 1. 2. Applicable Documents 2.1 ASTM Standards: B 95 Test Method for Linear Expansion 2 of Metals E 3 Methods of Preparation of Metallo3 graphic Specimens E 8 Methods of Tension Testing of 4 Metallic Materials E 18 Test Methods for Rockwell Hardness and Rockwell Superficial Hardness of 4 Metallic Materials E 112 Methods for Determining Average 3 Grain Size F 14 Practice for Making and Testing 5 Reference Glass-Metal Bead-Seal F 140 Practice for Making Reference Glass-Metal Butt Seals and Testing for Expansion Characterisitics by 5 Polarimetric Methods F 144 Practice for Making Reference Glass-Metal Sandwich Seal and Testing for Expansion Characteristics 5 by Polarimetric Methods 6. Surface Lubricants 6.1 All lubricants used during cold-working operations, such as drawing, rolling, or spinning, shall be capable of being removed readily by any of the common organic degreasing solvents such as, for example, trichloroethylene. 7. Temper 7.1 The desired temper of the material shall be specified in the purchase order. 7.2 Tube —Unless otherwise agreed upon by the supplier or manufacturer and the purchaser, these forms shall be given a final bright anneal by the manufacturer and supplied in the annealed temper. 7.3 Strip and Sheet —These forms shall be supplied in one of the tempers given in Table 2 or in deep-drawing temper, as specified. 3. Ordering Information 3.1 Orders for material under this specification shall include the following information: 3.1.1 Size, 3.1.2 Temper (Section 7), 3.1.3 Surface finish (Section 11), 3.1.4 Marking and packaging (Section 17), and 1 This specification is under the jurisdiction of ASTM Committee F-1 on Electronics and is the direct responsibility of Subcommittee F01.03 on Metallic Materials. Current edition approved Jan. 27,1978. Published March 1978. Originally published as F15 — 61 T. Last previous edition F15 — 77. 2 Discontinued, see 1985 Annual Book of ASTM Standards , Vol 14.02 3 Annual Book of ASTM Standards, Vol 03.03. 4 Annual Book of ASTM Standards, Vol 03.01. 5 Annual Book of ASTM Standards. Vol 10.04. 63 F 15 11.1.3 11.1.4 11.1.5 11.1.6 7.4 Wire and Rod—These forms shall be supplied in one of the tempers given in Table 3 as specified. Unless otherwise specified, the material shall be bright annealed and supplied in temper A (annealed). Centerless grinding (rod), Belt polishing, Cold rolling, and Wire drawing. 12. Thermal Expansion Characteristics 8. Grain Size 12.1 The average linear coefficients of thermal expansion shall be within the limits specified in Table 4 8.1 Strip and sheet for deep drawing shall have an average grain size not larger than ASTM No. 5 (Note 1), and no more than 10% of the grains shall be larger than No. 5 when measured in accordance with Methods E 112. 13. Test for Thermal Expansion 13.1 Heat the specimen in a hydrogen atmosphere for 1 h at 900°C, followed by 15 min at 1100°C. Between the 900 and 1100°C heat-treatment periods, the specimen may be cooled to room temperature if desired. Cool the specimen from 1100 to 200°C in the hydrogen atmosphere at a rate not to exceed 5°C/min. 13.2 Reheat the specimen to 500°C in the dilatometer and determine the coefficient of thermal expansion from the cooling curve. 13.3 Determine the thermal expansion characteristics in accordance with Test Method B95. NOTE 1—This corresponds to a grain size of 0.065 mm, 2 or 16 grains/in. of image at 100 ×. 9. Hardness 9.1 Deep-Drawing Temper—For deep drawing, the hardness shall not exceed 82 HRB for material 0.100 in. (2.54 mm) and less in thickness and 85 HRB for material over 0.100 in. in thickness when determined in accordance with Methods E 18. 9.2 Rolled and Annealed Tempers— Hardness tests when properly applied can be indicative of tensile strength. Hardness scales and ranges for these tempers, if desirable, shall be negotiated between supplier and purchaser. NOTE 2—Although not required, the thermal expansion match between the alloy and a glass may be evaluated by preparing and testing an assembly in accordance with Practices F14, F140 or F144, whichever glass-metal seal test is appropriate. 10. Tensile Strength 14. Transformation 10.1 Sheet and Strip; 10.1.1 Tensile strength shall be the basis for acceptance or rejection for the tempers given in Table 2 and shall conform with the requirements prescribed. 10.1.2 Tension test specimens shall be taken so the longitudinal axis is parallel to the direction of rolling and the test shall be performed in accordance with Methods E 8. 10.2 Wire and Rod; 10.2.1 Tensile strength shall be the basis for acceptance or rejection for the tempers given in Table 3 and shall conform with the requirements prescribed. 10.2.2 The test shall be performed in accordance with Method E 8. 14.1 The temperature of the gamma-toalpha transformation shall be below –78.5°C when the material is tested in accordance with Section 15. However, for material whose smallest dimension is over 7/8 in. (22.2 mm), some localized transformation, acceptable to the purchaser, may be tolerated. 15. Test for Transformation 15.1 Cut the specimen from any part of the material, but preferably including the entire cross section, degrease it, then heat treat it as described in 13.1. When cool, polish the cross section of the specimen and etch (Note 3) it in accordance with Method E3. Then subject the specimen to the temperature produced by an excess of dry ice in acetone 0 (–78.5 C) for at least 4 h. After the lowtemperature treatment, examine the specimen at a magnification of 150× for the presence of the acicular crystals characteristic of the alpha phase. Because these crystals may oc- 11. Surface Finish 11.1 The standard surface finishes available shall be those resulting from the following operations: 11.1.1 Hot rolling, 11.1.2 Forging, 64 F 15 cur only in small localized areas, examine carefully the entire polished cross section. 15.2 Specimens that show no transformation and that show partial transformation are illustrated in Figs. 1 and 2, respectively. dimensions prescribed in Table 8. 16.3 Cold-Drawn Tubing—Cold-drawn tubing, available either as seamless or welded, shall conform to the permissible variations prescribed in Table 9. NOTE 3—A suggested etchant is a solution of three parts by volume of concentrated hydrochloric acid and one part of concentrated nitric acid saturated with cupric chloride (CuCl 2 ·2H 2 0). This etchant is more effective when allowed to stand for 20 min after mixing. After several hours it loses its strength and should be discarded at the end of the day. Etching is best accomplished by swabbing the specimen with cotton soaked with the etchant. Etching is usually complete when the surface of the metal appears to have turned dull. 17. Packaging and Marking 17.1 Packaging shall be subject to agreement between the purchaser and the seller. 17.2 The material as furnished under this specification shall be identified by the name or symbol of the manufacturer and by melt number. The lot size for determining compliance with the requirements of this specification shall be one heat. 18. Investigation of Claims 16. Dimensions and Permissible Variations 16.1 Cold Rolled Strip-Cold–rolled strip shall conform to the permissible variations in dimensions prescribed in Tables 5, 6, and 7. 16.2 Round Wire and Rod–Wire and rod shall conform to the permissible variations in Table 1 Table 3 Chemical Requirements Composition, % 53A 29A 17A 0.50 0.20 0.04 0.10B 0.10B 0.10B 0.10B 0.20 0.20 0.20 Element Iron, nominal Nickel, nominal Cobalt, nominal Manganese, max Silicon, max Carbon, max Aluminum, max Magnesium, max Zirconium, max Titanium, max Copper, max Chromium, max Molybdenum, max A 18.1 Where any material fails to meet the requirements of this specification, the material so designated shall be handled in accordance with a mutual agreement between the purchaser and the seller. Temper Designation A B C D E of Thermal Expansion, A µm/m•°C 30 to 400 30 to 450 4.60 to 5.20 5.10 to 5.50 A The following typical thermal expansion data for the alloy covered by these specifications are given for information only: coefficient of thermal expansion given in Table 4. The total of aluminum, magnesium, zirconium, and titanium shall not exceed 0.20%. Table 2 Tensile Strength Requirements for Sheet and Strip A B C D E Temper Name Tensile Strength, ksi (MPa) annealed ¼ hard half hard ¾ hard hard 85 (585) max 85 to 105 (585 to 725) 95 to 115 (655 to 795) 105 to 125 (725 to 860) 125 (860) min Temperature Range, °C The iron, nickel and cobalt requirements listed are nominal. They shall Temper Designation Tensile Strength, ksi (MPa) Table 4 Coefficients of Thermal E i Average Linear Coefficient be adjusted by the manufacturer so that the alloy meets the requirements for B Tensile Strength Requirements for Wire and Rod 82 max (570 max) 75 to 90 (520 to 630) 85 to 100 (590 to 700) 95 to 110 (660 to 770) 100 min (700 min) 65 Temperature Range, °C Average Linear Coefficient of Thermal Expansion, µm/m•°C 30 to 200 30 to 300 30 to 400 30 to 450 30 to 500 30 to 600 30 to 700 30 to 800 30 to 900 5.5 5.1 4.9 5.3 6.2 7.9 9.3 10.4 11.5 F 15 Table 5 Permissible Variations in Thickness of Cold-Rolled Strip NOTE—Measurement shall be made at least 3/8 in. (9.5 mm) from the edge of strip over 1 in. (25.4 mm) wide. Specified Thickness, in. (mm) Permissible Variations in Thickness for Width Given, ± in. (mm) Over 3 to 6 Over 6 to 12 Over 12 to 16 Under 3 (76) (76 to 152) (152 to 305) (305 to 406) 0.002 (0.051) 0.002 (0.051) 0.002 (0.051) 0.002 (0.051) 0.0015 (0.038) 0.0015 (0.038) 0.001 (0.025) 0.001 (0.025) 0.001 (0.025) 0.001 (0.025) 0.001 (0.025) 0.00075 (0.019) 0.0005 (0.013) 0.160 to 0.100 (4.06 to 2.54), incl 0.099 to 0.069 (2.51 to 1.75), incl 0.068 to 0.050 (1.73 to 1.27), incl 0.049 to 0.035 (1.24 to 0.89), incl 0.034 to 0.029 (0.86 to 0.74), incl 0.028 to 0.026 (0.71 to 0.66), incl 0.025 to 0.020 (0.64 to 0.51), incl 0.019 to 0.017 (0.48 to 0.43), incl 0.016 to 0.012 (0.41 to 0.31), incl 0.011 to 0.0101 (0.28 to 0.26), incl 0.010 to 0.0091 (0.25 to 0.23), incl 0.009 to 0.006 (0.23 to 0.15), incl Under 0.006 (0.15) 0.003 (0.076) 0.003 (0.076) 0.003 (0.076) 0.0025 (0.064) 0.002 (0.051) 0.0015 (0.038) 0.0015 (0.038) 0.001 (0.025) 0.001 (0.025) 0.001 (0.025) 0.001 (0.025) 0.00075 (0.019) 0.0005 (0.013) 0.004 (0.102) 0.003 (0.076) 0.003 (0.076) 0.003 (0.076) 0.0025 (0.064) 0.002 (0.051) 0.002 (0.051) 0.0015 (0.038) 0.0015 (0.038) 0.001 (0.025) 0.001 (0.025) ... ... 0.004 (0.102) 0.004 (0.102) 0.003 (0.076) 0.003 (0.076) 0.0025 (0.064) 0.002 (0.051) 0.002 (0.051) 0.002 (0.051) 0.0015 (0.038) 0.0015 (0.038) 0.001 (0.025) ... ... Table 6 Permissible Variations in Thickness Across Width of Strip Maximum Variation in Thickness Across Width of Strip, Within Those Provided for in Table 4 for Edge Measurements for Widths and Thicknesses Given, in. (mm) Over 5 to 12 Over 12 to 24 5 (127) and Under (127 to 300) (300 to 600), incl in. mm in. mm in. mm Specified Thickness in. mm 0.005 to 0.010, incl Over 0.010 to 0.025, incl Over 0.025 to 0.065, incl Over 0.065 to , 3/16, excl 0.17 to 0.03, incl 0.03 to 0.06, incl 0.06 to 0.16, incl 0.16 to 0.48, excl 0.00075 0.001 0.0015 0.002 0.0191 0.025 0.038 0.051 0.001 0.0015 0.002 0.0025 0.025 0.038 0.051 0.064 0.0015 0.002 0.0025 0.003 0.038 0.051 0.064 0.076 Table 7 Permissible Variations in Width of Cold-Rolled Strip Supplied in Coils Permissible Variations in Width for Widths Given, ± in. (mm) Specified Thickness, in. (mm) 0.187 to 0.161 (4.75 to 4.09) 0.160 to 0.100 (4.06 to 2.54) 0.099 to 0.069 (2.51 to 1.75) 0.068 (1.73) and under Under ½ to 3/16 (12.7 to 4.8) ½ to 6 (12.7 to 152) Over 6 to 9 (152 to 229) Over 9 to 12 (229 to 305) Over 12 to Over 20 to 20 (305 to 2315/16 (508 to 608) 508) ... 0.010 (0.25) 0.008 (0.20) 0.005 (0.13) 0.016 (0.41) 0.010 (0.25) 0.008 (0.20) 0.005 (0.13) 0.020 (0.51) 0.016 (0.41) 0.010 (0.25) 0.005 (0.13) 0.020 (0.51) 0.016 (0.41) 0.010 (0.25) 0.010 (0.25) 0.031 (0.79) 0.020 (0.51) 0.016 (0.41) 0.016 (0.41) 66 0.031 (0.79) 0.020 (0.51) 0.020 (0.51) 0.020 (0.51) F 15 Table 8 Permissible Variations in Diameter of Wire and Rod Permissible Variations in Diameter, ± in. (mm) Specified Diameter, in. (mm) Wire (Coiled, Spooled or Straight Lengths) 0.002 0.0044 0.008 0.015 0.020 0.031 0.041 0.061 0.081 0.126 0.157 to 0.0043 to 0.0079 to 0.0149 to 0.0199 to 0.0309 to 0.0409 to 0.0609 to 0.0809 to 0.1259 to 0.1569 to 0.250 (0.05 to 0.110) (0.111 to 0.202) (0.20 to 0.379) (0.38 to 0.507) (0.51 to 0.786) (0.79 to 1.04) (1.04 to 1.548) (1.55 to 2.056) (2.06 to 3.199) (3.20 to 3.99) (4.00 to 6.35) 0.0002 0.00025 0.0003 0.0004 0.0005 0.0006 0.0007 0.0008 0.001 0.0015 0.002 (0.005) (0.006) (0.008) (0.010) (0.013) (0.015) (0.018) (0.020) (0.025) (0.038) (0.051) Rod, Centerless Ground Finish (Straight Lengths) 0.030 to 0.0549 0.055 to 0.1249 0.125 to 0.499 0.500 to 0.999 1.000 to 1.625 1.626 to 1.749 1.750 to 1.999 2.000 to 4.000 (0.76 to 1.396) (1.40 to 3.174) (3.18 to 12.70) (12.7 to 25.37) (25.4 to 41.28) (41.30 to 44.40) (44.45 to 50.77) (50.80 to 101.60) 0.0005 0.001 0.0015 0.002 0.0025 0.003 0.004 0.005 (0.013) (0.035) (0.038) (0.051) (0.064) (0.08) (0.10) (0.13) Table 9 Permissible Variations in Dimensions of Standard Tubing Permissible VariationsA Specified Outside Diameter, in. (mm) Under 0.093 (2.36) 0.093 to 0.187 (2.36 to 4.76), excl 0.187 to 0.500 (4.76 to 12.70), excl 0.500 to 1.500 (12.70 to 38.10), excl A Outside Diameter, in. (mm) Inside Diameter, in. (mm) + 0.002 (0.05) – 0.000 + 0.003 (0.08) – 0.000 + 0.004 (0.10) – 0.000 + 0.005 (0.13) – 0.000 + 0.000 – 0.002 (0.05) + 0.000 – 0.003 (0.08) + 0.000 – 0.004 (0.10) + 0.000 – 0.005 (0.13) Any two of the three dimensional tolerances listed may be specified. 67 Wall Thickness, ± % 10 10 10 10 F 15 150× Figure 1. Normal Annealed Specimen Showing No Transformation 68 F 15 150 × Figure 2. Partially Transformed Specimen The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, Pa. 19103. 69 Designation: F 30—85 Reprinted, with permission, from the Annual Book of ASTM Standards, copyright American Society for Testing and Materials, 1916 Race Street, Philadelphia, PA 19103. Standard Specification for IRON-NICKEL SEALING ALLOYS 1 This standard is issued under the fixed designation F 30; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (ε) indicates an editorial change since the last revision or reapproval. 1. Scope 4. General Requirements 1.1 This specification covers iron-nickel alloys that are intended primarily for sealing to glass in electronic applications. 4.1 The material shall be commercially smooth, uniform in cross section, in composition, and in temper; it shall be free from scale, corrosion, cracks, seams, scratches, slivers, and other defects as best commercial practice will permit. NOTE 1—Some of these alloys may be used for sealing to ceramics, but this specification in its present form is not intended to cover material for metal-to-ceramic seals. 5. Chemical Composition 5.1 The material shall conform to the requirements as to chemical composition prescribed in Table 1. 1.2 The values stated in inch-pound units are to be regarded as the standard. 2. Applicable Documents 2.1 ASTM Standards: E 18 Test Methods for Rockwell Hardness and Rockwell Superficial Hardness of 2 Metallic Materials E 29 Practice for Indicating Which Places of Figures Are to Be Considered Signifi3 cant in Specified Limiting Values E 112 Method for Determining Average 3 Grain Size F 14 Practice for Making and Testing 4 Reference Glass-Metal Bead-Seal F 140 Practice for Making Reference Glass-Metal Butt Seals and Testing for Expansion Characteristics by Polari4 metric Methods F 144 Practice for Making Reference Glass-Metal Sandwich Seal and Testing for Expansion Characteristics by 4 Polarimetric Methods 6. Surface Lubricants 6.1 All lubricants used in processing shall be thoroughly removed. Protective coatings present on the material as shipped shall be readily removable by any of the common organic degreasing solvents, for example, trichloroethylene. 7. Temper 7.1 The desired temper of the material shall be specified on the purchase order. Unless otherwise specified, wire, rod, and tubing shall be given a final bright anneal by the manufacturer. Strip and sheet shall be annealed properly to develop deep drawing properties. For deep drawing the hardness shall not exceed Rockwell B 82 for material 0.100 in. (2.54 mm) and less in thickness, and B 85 for material over 0.100 in. thick when determined in accordance with Test Methods E 18. 3. Ordering Information 3.1 Orders for material under this specification shall include the following information: 3.1.1 Size, 3.1.2 Temper (Section 6), 3.1.3 Surface finish (Section 8), 3.1.4 Marking and packaging (Section 15), and 3.1.5 Certification, if required. 1 This specification is under the jurisdiction of ASTM Committee F-1 on Electronics and is the direct responsibility of Subcommittee F01.03 on Metallic Materials. Current edition approved Aug. 30, 1985. Published October 1985. Originally published as F30 – 77. Last previous edition F30 – 77. 2 Annual Book of ASTM Standards, Vol 03.01. 3 Annual Book of ASTM Standards, Vol 03.03. 4 Annual Book of ASTM Standards, Vol 10.04. 70 F 30 8. Grain Size 13. Test for Porosity 8.1 Strip and sheet for deep drawing applications shall have an average grain size not larger than ASTM No. 5 (Note 3) and no more than 10% of the grains shall be larger than No. 5 when measured to accordance with Method E 112. For materials less than 0.005 in. (0.13 mm) in thickness the grain size shall be such that there are no less than 4 grains across the thickness. 13.1 Machine the specimen in accordance with Fig. 1. Degrease and slightly pickle the specimen in a 1 + 1 hydrochloric acid solution containing an inhibitor at a temperature of 65°C; then wash and dry it at 105 to 110°C. Heat treat the specimen at 1100°C for 30 min. in wet hydrogen and allow it to cool in this atmosphere. 13.2 Connect the tubulation of the test fixture, Fig. 2, to a helium leak detector. The sensitivity of the leak detector shall be such that -9 3 a leak of 1 × 10 cm /s measured at 20°C and 1 atm pressure, will give a deflection of at least 5% of full scale. Exhaust the test fixture, and test the specimen for leakage by probing all of the exposed surface with a helium jet. If leakage is found, squirt alcohol all around the specimen-to-neoprene seal to make certain that the leak is through the specimen and not at the gasket seal. Make this test within 24 h after the specimen is removed from the heat-treating furnace. NOTE 2—This corresponds to a grain size of 0.065 mm 2 or 16 grains/in. of image at 100 x. 9. Surface Finish 9.1 The standard surface finishes available shall be those resulting from the following operations: 9.1.1 Hot-rolling, 9.1.2 Forging, 9.1.3 Centerless grinding (rod), 9.1.4 Belt polishing, 9.1.5 Cold rolling, and drawing, and 9.1.6 Wire drawing. 14. Dimensions and Permissible Variations 10. Thermal Expansion Characteristics 14.1 Cold-Rolled Strip—Cold-rolled strip shall conform to the permissible variations in dimensions prescribed in Tables 3, 4, and 5. 14.2 Round Wire and Rod—Wire and rod shall conform to the permissible variations in dimension prescribed in Table 6. 14.3 Cold-Drawn Tubing—Cold-drawn tubing, available either as seamless or welded, shall conform to the permissible variations prescribed in Table 7. 10.1 The average linear coefficients of thermal expansion shall be within the limits specified in Table 2. 11. Test for Thermal Expansion 11.1 Determine the thermal expansion characteristics with a precision dilatometer after heat treating the specimen as follows: 11.1.1 Heat the specimen in a hydrogen atmosphere for 1 h at 900°C and then cool it from 900 to 200°C at a rate not exceeding 5°C/min. 11.1.2 Reheat the specimen to 25°C above the highest temperature specified for the thermal expansion and determine the expansion from the cooling curve. See Method E 228. 11.2 The thermal expansion match between the alloy and a glass may be evaluated by testing the assembly in accordance with Practices F 14, F 140, or F 144. 15. Rounding Results 15.1 Observed or calculated values obtained from analysis, measurements, or tests shall be rounded in accordance with Recommended Practice E 29, to the nearest unit in the last right place of figures used in expressing the specified limit. 16. Packaging and Package Marking 16.1 Packaging shall be subject to agreement between the purchaser and the seller. 16.2 The material as furnished under this specification shall be identified by the name or symbol of the manufacturer and by melt number. The lot size for determining compliance with the requirements of this 12. Porosity in Bar or Rod 12.1 Specimens from bar or rod ½ in. (12.7 mm) in diameter or over, when tested in accordance with Section 12, shall show no leakage in the helium leak detector. 71 F 30 requirements of this specification, the material so designated shall be handled in accordance with the agreement mutually agreed upon by the purchaser and the seller. specification shall be one heat. 17. Investigation of Claims 17.1 Where any material fails to meet the Table 1 Chemical Requirements Composition, % 42 Alloy Nickel,Anominal Manganese, max Silicon, max Carbon, max Chromium, max Cobalt, max Phosphorous, max Sulfur, max Aluminum, max Iron 46 Alloy 48 Alloy 52 Alloy 41 0.80 0.30 0.05 0.25 46 0.80 0.30 0.05 0.25 48 0.80 0.30 0.05 0.25 50.5 0.60 0.30 0.05 0.25 B B B B 0.025 0.025 0.10 remainder 0.025 0.025 0.10 remainder 0.025 0.025 0.10 remainder 0.025 0.025 0.10 remainder A The nickel contents listed are nominal. The nickel contents of the alloys shall be adjusted by the manufacturer so that the alloys meet the requirements for thermal expansion. The 52 Alloy is specifically intended to match lead (Pb) sealing glasses. B Cobalt is present as an incidental element and shall be reported separately. Table 2 Thermal Expansion RequirementsA Temperature Range, °C Average Linear Coefficient of Thermal Expansion, µm/m•°C 42 30 to 300 30 to 450 4.0 to 4.7 6.7 to 7.4 46 30 to 350 30 to 500 7.1 to 7.8 8.2 to 8.9 48 30 to 400 30 to 550 8.2 to 9.2 9.6 to 10.3 52 30 to 450 30 to 550 9.7 to 10.2 10.0 to 10.5 Alloy No. A Typical expansion data up to 1000°C are given in the Appendix. 72 F 30 Table 3 Permissible Variations in Thickness of Cold-Rolled Strip NOTE—Measurements shall be made at least 3/8 in. (9.5 mm) from the edge of strip that is over 1 in. (25.4 mm) wide. Permissible Variations in Thickness for Width Given, plus or minus, in. (mm) Specified Thickness, in. (mm) Over 3 to 6 (76 to 152) Under 3 (76) 0.160 to 0.100 (4.06 to 2.54), incl 0.099 to 0.069 (2.51 to 1.75), incl 0.068 to 0.050 (1.73 to 1.27), incl 0.049 to 0.035 (1.24 to 0.89), incl 0.034 to 0.029 (0.86 to 0.74), incl 0.028 to 0.026 (0.71 to 0.66), incl 0.025 to 0.020 (0.64 to 0.51), incl 0.019 to 0.017 (0.48 to 0.43), incl 0.016 to 0.012 (0.41 to 0.31), incl 0.011 to 0.0101 (0.28 to 0.26), incl 0.010 to 0.0091 (0.25 to 0.23), incl 0.009 to 0.006 (0.23 to 0.15), incl Under 0.006 (0.15) 0.002 0.002 0.002 0.002 0.0015 0.0015 0.001 0.001 0.001 0.001 0.001 0.00075 0.0005 (0.051) (0.051) (0.051) (0.051) (0.038) (0.038) (0.025) (0.025) (0.025) (0.025) (0.025) (0.019) (0.013) 0.003 0.003 0.003 0.0025 0.002 0.0015 0.0015 0.001 0.001 0.001 0.001 0.00075 0.0005 Over 6 to 12 (152 to 305) (0.076) (0.076) (0.076) (0.064) (0.051) (0.038) (0.038) (0.025) (0.025) (0.025) (0.025) (0.019) (0.013) 0.004 0.003 0:003 0.003 0.0025 0.002 0.002 0.0015 0.0015 0.001 0.001 … … (0.102) (0.076) (0.076) (0.076) (0.064) (0.051) (0.051) (0.038) (0.038) (0.025) (0.025) Over 12 to 16 (305 to 406) 0.004 0.004 0.003 0.003 0.0025 0.002 0.002 0.002 0.0015 0.0015 0.001 … … (0.102) (0.102) (0.076) (0.076) (0.064) (0.051) (0.051) (0.051) (0.038) (0.038) (0.025) Table 4 Permissible Variations in Thickness Across Width of Strip Maximum Variation in Thickness Across Width of Strip (Within Limits Specified in Table 3 for Edge Measurements) for Widths and Thicknesses Given, in. (mm) Specified Thickness, in. (mm) 0.005 to 0.010 (0.13 to 0.25), incl Over 0.010 to 0.025 (0.25 to 0.64), incl Over 0.025 to 0.065 (0.64 to 1.65), incl Over 0.065 to 3/16 (1.65 to 4.8), excl 0.00075 0.001 0.0015 0.002 (0.019) (0.025) (0.038) (0.051) 0.001 0.0015 0.002 0.0025 (0.025) (0.038) (0.051) (0.064) 0.0015 0.002 0.0025 0.003 (0.038) (0.051) (0.064) (0.076) Table 5 Permissible Variations in Width of Cold-Rolled Strip Supplied in Coils Specified Thickness in. (mm) 0.187 to 0.161 (4.75 to 4.09) 0.160 to 0.100 (4.06 to 2.54) 0.099 to 0.069 (2.51 to 1.75) 0.068 (1.73) and under Permissible Variations in Width or Widths Given, plus or minus, in. (mm) Under ½ to 3/16 (12.7 to 4.8) ½ to 6 12.7 to 152) Over 6 to 9 (152 to 229) Over 9 to 12 (229 to 305) Over 12 to 20 (305 to 508) … 0.010 (0.25) 0.008 (0.20) 0.005 (0.13) 0.016 (0.41) 0.010 (0.25) 0.008 (0.20) 0.005 (0.13) 0.020 (0.51) 0.016 (0.41) 0.010 (0.25) 0.005 (0.13) 0.020 (0.51) 0.016 (0.41) 0.010 (0.25) 0.010 (0.25) 0.031 (0.79) 0.020 (0.51) 0.016 (0.41) 0.016 (0.41) 73 F 30 Table 6 Permissible Variations in Diameter of Wire and Rod Permissible Variations in Diameter, plus or minus, in. (mm) Wire (Coiled, Spooled, or Straight Lengths) Specified Diameter, in. (mm) 0.002 0.0044 0.008 0.015 0.020 0.031 0.041 0.061 0.081 0.126 0.157 to 0.0043 to 0.0079 to 0.0149 to 0.0199 to 0.0309 to 0.0409 to 0.0609 to 0.0809 to 0.1259 to 0.1569 to 0.250 (0.051 to 0.109) (0.112 to 0.201) (0.203 to 0.378) (0.381 to 0.505) (0.508 to 0.785) (0.787 to 1.039) (1.041 to 1.547) (1.549 to 2.055) (2.057 to 3.198) (3.200 to 3.985) (3.99 to 6.35 ) 0.002 0.00025 0.0003 0.0004 0.0005 0.0006 0.0007 0.0008 0.001 0.0015 0.002 (0.051) (0.006) (0.007) (0.010) (0.013) (0.015) (0.018) (0.020) (0.025) (0.038) (0.051) Rod, Centerless Ground Finish (Straight Lengths) 0.030 0.055 0.125 0.500 1.000 1.626 1.750 2.000 to 0.0549 to 0.1249 to 0.499 to 0.999 to 1.625 to 1.749 to 1.999 to 4.000 Table 7 (0.762 to 1.394) (1.397 to 3.172) (3.175 to 12.67) (12.70 to 25.38) (25.40 to 41.27) (41.30 to 44.43) (44.45 to 50.78) (50.80 to 101.60) Under 3/32 (2.4) 3/16 to (0.013) (0.025) (0.038) (0.051) (0.064) (0.076) (0.102) (0.13) Permissible Variations in Dimensions of Standard TubingA Specified Outside Diameter, in. (mm) 3/32 to 3/16 0.0005 0.001 0.0015 0.002 0.0025 0.003 0.004 0.005 (2.4 to 4.8), excl ½ (4.8 to 12.7), excl ½ to 1½ (12.7 to 38.1), excl Outside Diameter, in. (mm) + 0.002 (0.051) – 0.000 + 0.003 (0.076 – 0.000 + 0.004 (0.102) – 0.000 + 0.005 (0.127) – 0.000 A Any two of the three dimensional tolerances listed may be specified. 74 Inside Diameter, in. (mm) + 0.000 – 0.002 (0.051) + 0.000 – 0.003 (0.076) + 0.000 – 0.004 (0.102) + 0.000 – 0.005 (0.127) Wall Thickness, plus or minus, % 10 10 10 10 F 30 Section A—A Diameter, in. 0.5 to 1 1 to 2 Thickness, in. 0.090 ± 0.005 0.125 ± 0.005 Metric Equivalents in. mm in. mm 1/32 0.8 1.2 0.13 2.29 0.125 0.5 1.0 2.0 3.18 12.7 25.4 50.8 3/64 0.005 0.090 Figure 1. Machined Specimen for Porosity Test Metric Equivalents in. 1/8 ¼ 7/16 1 mm 3.2 6.4 11.1 25.4 in. 111/16 2½ 3 mm 42.8 63.5 76.2 Figure 2. Test Fixture for Porosity Test 75 F 30 APPENDIX X1. THERMAL EXPANSION DATA X1.1 Typical thermal expansion data for the alloys covered by this specifications are given in Table X1.1 for information only. Table X1.1 Temperature Range, °C 30 to 300 30 to 400 30 to 500 30 to 600 30 to 700 30 to 800 30 to 900 30 to 1000 Typical Results of Thermal Expansion Tests Average Linear Coefficient of Thermal Expansion, µm/m•°C 42 Alloy 46 Alloy 48 Alloy 52 Alloy 4.4 6.0 7.9 9.6 10.5 11.4 12.3 13.2 7.5 7.5 8.5 9.8 10.7 11.6 12.5 13.4 8.8 8.7 9.4 10.4 11.3 12.1 13.0 13.9 10.1 9.9 9.9 10.8 11.7 12.5 13.3 14.2 The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103. 76 Designation: F 31–68 (Reapproved 1983)ε 1 Reprinted, with permission, from the Annual Book of ASTM Standards, copyright American Society for Testing and Materials, 1916 Race Street, Philadelphia, PA 19103. Standard Specification for 1 42% NICKEL-6% CHROMIUM-IRON SEALING ALLOY This standard is issued under the fixed designation F 31; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (ε) indicates an editorial change since the last revision or reapproval. 3.1.4 Marking and packaging (Section 16), and 3.1.5 Certification if required. 1. Scope 1.1 This specification covers an iron-nickelchromium alloy used primarily for glasssealing applications in electronic devices. 4. General Requirements 4.1 The material shall be commercially smooth, uniform in cross section, in composition, and in temper; it shall be free from scale, corrosion, cracks, seams, scratches, slivers, and other defects as best commercial practice will permit. 2. Applicable Documents 2.1 ASTM Standards: E 18 Test Methods for Rockwell Hardness and Rockwell Superficial Hardness of 2 Metallic MateriaIs E 29 Recommended Practice for Indicating Which Places of Figures Are to Be Considered Significant in Specified Limiting 3 Values E 38 Methods for Chemical Analysis of Nickel-Chromium and Nickel-Chromium4 Iron Alloys E 112 Methods for Determining Average 5 Grain Size E 228 Test Method for Linear Thermal Expansion of Rigid Solids with a Vitreous 3 Silica Dilatometer F 14 Practice for Making and Testing 6 Reference Glass-Metal Bead-Seal F 140 Practice for Making Reference GlassMetal Butt Seals and Testing for Expansion 6 Characteristics by Polarimetric Methods F 144 Practice for Making Reference GlassMetal Sandwich Seal and Testing for Expansion Characteristics by Polarimetric 6 Methods 5. Chemical Requirements 5.1 The material shall conform to the requirements of Table 1 as to chemical composition. NOTE 1—The major constituents of this alloy may be adjusted by the manufacturer so that the alloy meets the requirement for thermal expansion. 6. Chemical Analysis 6.1 Chemical analysis shall be made, when desired, in accordance with Methods E 38. 7. Surface Lubricants 7.1 All lubricants used during cold-working operations such as drawing, rolling or spinning, shall be capable of being removed readily by any of the common organic degreasing solvents as, for example, trichloroethylene. 8. Temper 8.1 The desired temper of the material shall 3. Ordering Information 3.1 Orders for material under this specification shall include the following information: 3.1.1 Size, 3.1.2 Temper (Section 7), 3.1.3 Surface finish (Section 9), 1 1 This specification is under the jurisdiction of ASTM Committee F-1 on Electronics and is the direct responsibility of Subcommittee F01.03 on Metallic Materials. Current edition effective Aug. 15, 1968. Originally issued 1963. Replaces F 31 – 63 T. 2 Annual Book of ASTM Standards, Vol 03.01. 3 Annual Book of ASTM Standards, Vol 14.02. 4 Annual Book of ASTM Standards, Vol 03.05. 5 Annual Book of ASTM Standards, Vol 03.03. 6 Annual Book of ASTM Standards, Vol 10.04. NOTE – Section 2 was added editorially and subsequent sections renumbered in April 1984. 77 F 31 be specified on the purchase order. Unless otherwise specified, wire, rod, and tubing shall be given a final bright anneal by the manufacturer. Strip and sheet shall be annealed properly to develop drawing properties. For deep drawing, the hardness shall not exceed Rockwell B90 when determined in accordance with Methods E 18. 12.3 The thermal expansion match between the alloy and a glass may be evaluated by preparing and testing an assembly in accordance with Practice F 14, Practice F 140, or Practice F 144. 13. Porosity in Bar or Rod (½-in. Diameter and Over) 13.1 The specimen of bar or rod ½ in. (12.7 mm) in diameter or over, when tested in accordance with Section 14 shall show no leakage in the helium leak detector. 9. Grain Size 9.1 Strip and sheet for deep drawing applications shall have an average grain size not larger than ASTM No. 5 (Note 2), and no more than 10% of the grains shall be larger than No. 5 when measured in accordance with Methods E 112. For materials less than 0.005 in. (0.13 mm) in thickness, the grain size shall be such that there are no less than 4 grains across the thickness. 14. Test for Porosity 14.1 Machine the specimen in accordance with the dimensions of Fig. 1. Degrease the specimen and lightly pickle it in 1 + 1 hydrochloric acid containing an inhibitor at a temperature of 65°C; then wash and dry it at 105 to 110°C. Heat treat the specimen at 1100°C for 30 min in a wet-hydrogen atmosphere and allow it to cool in this atmosphere. 14.2 Connect the tubulation of the test fixture shown in Fig. 2 to a helium leak detector. The sensitivity of the leak detector –9 3 shall be such that a leak of 1 × 10 cm /s measured at 20°C and 1 atm pressure, will give a deflection of at least 5% of full scale. Exhaust the test fixture, and test the specimen for leakage by probing all of the exposed surface with a helium jet. If leakage is found, squirt alcohol all around the specimen-toneoprene seal to make certain that the leak is through the specimen and not at the gasket seal. Make this test within 24 h after the specimen is removed from the heat-treating furnace. NOTE 2—This corresponds to a grain size of 0.065 mm 2 or 16 grainslin. of image at 100 ×. 10. Surface Finish 10.1 The standard surface finishes available shall be those resulting from the following operations: 10.1.1 Hot rolling, 10.1.2 Forging, 10.1.3 Centerless grinding (rod), 10.1.4 Belt polishing, 10.1.5 Cold rolling, and drawing, and 10.1.6 Wire drawing. 10.2 Care shall be taken to prevent the depletion of surface chromium during processing. 11. Thermal Expansion Characteristics 11.1 The average linear coefficient of thermal expansion expressed as cm per cm per ° Celsius shall be within limits given in Table 2. 15. Dimensional Tolerances 15.1 Cold-Rolled Strip-Cold–rolled strip shall conform to the permissible variations in dimensions prescribed in Tables 3, 4, and 5. 15.2 Round Wire and Rod–Wire and rod shall conform to the permissible variations in dimension prescribed in Table 6. 15.3 Cold-Drawn Tubing–Cold-drawn tubing, available either as seamless or welded, shall conform to the permissible variations prescribed in Table 7. 12. Test for Thermal Expansion 12.1 Heat the specimen for 15 min at 1100°C in a hydrogen or cracked-ammonia atmosphere with a dew point of –40°C and cool to room temperature at a rate not exceeding 5°C/min. 12.2 Reheat the specimen to 450°C in a dilatometer. Hold at 450°C for 25 min; then determine the thermal expansion curve on cooling with a precision dilatometer as specified in Test Method E 228. 16. Test Results 16.1 78 Observed or calculated values F 31 obtained from analysis, measurements, or tests shall be rounded off in accordance with the rounding-off method of Recommended Practice E 29, to the nearest unit in the last right-hand place of figures used in expressing the specified limit. the purchaser and the seller. Table 1 17. Packaging and Marking 17.1 Packaging shall be subject to agreement between the purchaser and seller. 17.2 The material as furnished under this specification shall be identified by the name or symbol of the manufacturer and by melt number. The lot size for determining compliance with the requirements of this specification shall be one heat. Element Composition,% Nickel, nominal Chromium, nominal Carbon, max Manganese, max Phosphorus, max Sulfur, max Silicon, max Aluminum, max Iron 42.0 5.6 0.07 0.25 0.025 0.025 0.30 0.20 remainder Table 2 Coefficient of Thermal Expansion Coefficient, µm/m °CA 9.7 to 10.4 8.5 to 9.2 Temperature Range. °C 30 to 425 30 to 350 18. Investigation of Claims 18.1 Where any material fails to meet the requirements of this specification, the material so designated shall be handled in accordance with the agreement mutually agreed upon by Table 3 Chemical Requirements A Typical expansion data up to 700°C are given in the Appendix. Permissible Variations in Thickness of Cold-Rolled Strip Note—Measurement shall be made at least 3/8 in. (9.5 mm) from the edge of strip over 1-in. (25.4mm) wide. Specified Thickness Permissible Variations in Thickness for Width Given, ± in. mm Under 3 in. in. Under 76 mm mm Over 3 76 to Over 6 150 to Over 12 300 to to 6 in. 150 mm to 12 in. 300 mm to 16 in. 400 mm in. mm in. mm in. mm 0.160 to 0.100, incl 0.099 to 0.069, incl 0.068 to 0.050, incl 0.049 to 0.035, incl 0.034 to 0.029, incl 0.028 to 0.026, incl 0.025 to 0.020, incl 0.019 to 0.017, incl 0.016 to 0.012, incl 0.011 to 0.0101, incl 0.010 to 0.0091, incl 0.009 to 0.006, incl Under 0.006 4.06 to 2.54 2.51 to 1.75 1.73 to 1.27 1.24 to 0.89 0.86 to 0.74 0.71 to 0.66 0.64 to 0.51 0.48 to 0.43 0.41 to 0.30 0.28 to 0.256 0.254 to 0.231 0.228 to 0.152 0.152 0.002 0.002 0.002 0.002 0.0015 0.0015 0.001 0.001 0.001 0.001 0.001 0.00075 0.0005 0.05 0.05 0.05 0.05 0.038 0.038 0.025 0.025 0.025 0.025 0.025 0.019 0.013 0.003 0.003 0.003 0.0025 0.002 0.0015 0.0015 0.001 0.001 0.001 0.001 0.00075 0.0005 79 0.076 0.076 0.076 0.064 0.05 0.038 0.038 0.025 0.025 0.025 0.025 0.019 0.013 0.004 0.003 0.003 0.003 0.0025 0.002 0.002 0.0015 0.0015 0.001 0.001 … … 0.10 0.076 0.076 0.076 0.064 0.05 0.05 0.038 0.038 0.025 0.025 0.004 0.004 0.003 0.003 0.0025 0.002 0.002 0.002 0.0015 0.0015 0.001 … … 0.10 0.10 0.076 0.076 0.064 0.05 0.05 0.05 0.038 0.038 0.025 80 in. 0.187 to 0.161 0.160 to 0.100 0.099 to 0.069 0.068 and under mm 4.75 to 4.09 4.06 to 2.54 2.51 to 1.75 1.73 Specified Thickness Under ½ to 3/16 in. in. ... 0.010 0.008 0.005 0.019 0.025 0.038 0.051 127 mm and Under mm 0.001 0.0015 0.002 0.0025 Over 5 to 12 in. in. 0.0015 0.002 0.0025 0.003 Over 12 to 24 in., incl in. 0.25 0.20 0.13 Under 12.7 to 4.75 mm in. 0.016 0.010 0.008 0.005 ½ to 6 in 12.7 to 150 mm mm 0.41 0.25 0.20 0.13 Over 6 to 9 in. in. 0.020 0.016 0.010 0.005 150 to 225 mm mm 0.51 0.41 0.25 0.13 Over 9 to 12 in. in. 0.020 0.016 0.010 0.010 225 to 300 mm mm 0.51 0.41 0.25 0.25 Over 12 to 20 in. in. 0.031 0.020 0.016 0.016 Permissible Variations in Width for Widths Given, ± . 0.025 0.038 0.051 0.064 Over 127 to 300 mm mm 0.038 0.051 0.064 0.076 Over 300 to 600 mm mm 300 to 500 mm mm 0.79 0.51 0.41 0.41 Permissible Variations in Width of Cold-Rolled Strip Supplied in Coils 0.00075 0.001 0.0015 0.002 0.13 to 0.25 0.25 to 0.64 0.64 to 1.65 1.65 to 4.74 0.005 to 0.010, incl Over 0.010 to 0.025, incl Over 0.025 to 0.065, incl Over 0.065 to 3/16, excl Table 5 5 in. and Under in. mm Maximum Variation in Thickness Across Width of Strip, Within Those Provided for in Table 1 for Edge Measurements for Widths and Thicknesses Given. in. Specified Thickness Table 4 Permissible Variation In Thickness Across Width of Strip Over 20 to 2315/16 in. in. 0.031 0.020 0.020 0.020 500 to 600 mm mm 0.79 0.51 0.51 0.51 F31 F 31 Table 6 Permissible Variations in Diameter of Wire and Rod Specified Diameter in. Permissible Variations in Diameter, ± mm in. mm Wire (Coiled, Spooled or Straight Lengths) 0.002 to 0.0043 0.0044 to 0.0079 0.008 to 0.0149 0.015 to 0.0199 0.020 to 0.0309 0.031 to 0.0409 0.041 to 0.0609 0.061 to 0.0809 0.081 to 0.1259 0.126 to 0.1569 0.157 to 0.250 0.0002 0.00025 0.0003 0.0004 0.0005 0.0006 0.0007 0.0008 0.001 0.0015 0.002 0.051 to 0.109 0.112 to 0.200 0.203 to 0.378 0.381 to 0.505 0.508 to 0.785 0.787 to 1.039 1.041 to 1.547 1.549 to 2.055 2.057 to 3.198 3.200 to 3.985 3.988 to 6.35 0.005 0.0064 0.0076 0.0102 0.0127 0.0152 0.0178 0.0203 0.0254 0.038 0.051 Rod, Centerless Ground Finish (Straight Lengths) 0.030 to 0.0549 0.055 to 0.1249 0.125 to 0.499 0.500 to 0.999 1.000 to 1.625 1.626 to 1.749 1.750 to 1.999 2.000 to 4.000 0.766 to 1.397 to 3.175 to 12.70 to 25.4 to 41.3 to 44.45 to 50.8 to 1.394 3.172 12.67 25.37 41.27 44.42 50.17 101.6 0.0005 0.001 0.0015 0.002 0.0025 0.003 0.004 0.005 0.0127 0.0254 0.038 0.051 0.064 0.076 0.010 0.013 Table 7 Permissible Variations in Dimensions of Standard Tubing Permissible VariationsA Specified Outside Diameter, Outside Diameter in. A mm Under 0.093 2.36 0.093 to 0.187, excl 2.36 to 4.75 0.187 to 0.550, excl 4.75 to 12.7 0.500 to 1.500, excl 12.7 to 38.1 Inside Diameter in. mm in. mm + 0.002 – 0.000 + 0.003 – 0.000 + 0.004 – 0.000 + 0.005 – 0.000 + 0.051 – 0.000 + 0.076 – 0.000 + 0.102 – 0.000 + 0.13 – 0.00 + 0.000 – 0.002 + 0.000 – 0.003 + 0.000 – 0.004 + 0.000 – 0.005 + 0.000 – 0.051 + 0.000 – 0.076 + 0.000 – 0.102 + 0.000 – 0.13 Any two of the three dimensional tolerances listed may be specified. 81 Wall Thickness, plus or minus, % 10 10 10 10 F 31 Section A—A Diameter, in. ½ to 1 1 to 2 Thickness, in. 0.090 ± 0.005 0.125 ± 0.005 Figure 1. Machined Specimen for Porosity Test Figure 2. Test Fixture for Porosity Test 82 F 31 APPENDIX (Nonmandatory Information) XI. THERMAL EXPANSION DATA XI.1 The following typical thermal expansion data for 42% nickel-6% chromium-iron sealing alloy are given for information only. Temperature Range. °C 30 to 300 30 to 400 30 to 500 30 to 600 30 to 700 Average Linear Coefficient of Thermal Expansion. µm/m. °C 8.2 10.1 11.2 12.1 13.0 The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards. 1916 Race St., Philadelphia, Pa. 19103. 83 MIL-I-23011C 29 March 1974 Military Specification Superseding MIL-I-23011 B (ASG) 30 April 1965 IRON-NICKEL ALLOYS FOR SEALING TO GLASSES AND CERAMICS This specification is approved for use by all Departments and Agencies of the Department of Defense. 1. Scope Cold drawn or rolled Belt polished * 1.2.4 Condition and temper. Condition and temper shall be as follows (see Tables IV and V): Annealed ¼ hard (one quarter hard temper) ½ hard (one half hard temper) Hard (full hard temper) 1.1 Scope. This specification covers a series of iron-nickel, iron-nickel-cobalt, and ironnickel-chromium alloys used for sealing to glasses and ceramics in electronic applications (see 6.1) * 1.2 Classification. The alloys shall be of the following classes, forms, finishes, and conditions, as specified (see 6.2): * 1.2.1 Classes. Classes shall be as follows: Class 1 - Iron-nickel-cobalt alloy (29% Ni, 17% Co, remainder Fe) Class 2 - Iron-nickel alloy (50.5% Ni, remainder Fe) Class 3 - Iron-nickel alloy (48% Ni, remainder Fe) Class 4 - Iron-nickel alloy (46% Ni, remainder Fe) Class 5 - Iron-nickel alloy (41% Ni, remainder Fe) Class 6 - Iron-nickel-chromium alloy (41 % Ni, 5.5% Cr, remainder Fe) Class 7 - Iron-nickel alloy (36% Ni, remainder Fe) * 1.2.2 Forms. Alloys shall be in the form specified in Table I. Table I. Forms Bar 1 X 2. Applicable Documents 2.1 The following documents, of the issue in effect on date of invitation for bids or request for proposal, form a part of this specification to the extent specified herein: Specifications: Military MIL-C-16173 Corrosion Preventive Compound, Solvent Cutback, ColdApplication Standards: Federal Fed. Std. No. 48 Tolerances for Steel and Iron Wrought Products Fed. Test Method Metal; Test Methods Std. No. 151 Military MIL-STD-105 Sampling Procedures and Tables for Inspection by Attributes MIL-STD-163 Steel Mill Products; Preparation for Shipment and Storage Availability of forms 2 X 3 X Class 4 5 X X 6 --- 7 X X Rods X X X X X --- Ribbon X X --- X X X -- Strip X X X X X --- X Tubing X --- --- --- --- --- -- Wire X X X X X X X (Copies of specifications, standards, drawings, and publications required by suppliers in connection with specific procurement functions should be obtained from the procuring activity or as directed by the contracting officer.) * 2.2 Other publications. The following documents form a part of this specification to the extent specified herein. Unless otherwise indicated, the issue in effect on date of invitation for bids or request for proposal shall apply: * 1.2.3 Finishes. Finishes shall be as follows: Hot rolled or forged Centerless ground 84 MIL-I-23011 C es 2 to 6, inclusive, which are less than 0.005 inch in thickness, the grain size shall be such that there are no less than 9 grains across the thickness in the short transverse direction. 3.6 Phase transformation. No phase transformation shall occur in the finished forms of the Class 1 alloy from 1100°C to –80°C (see 4.5.6), except that material having a thickness or diameter exceeding 0.75 inch, some localized transformation may be tolerated if it does not exceed 1 percent of the cross section. 3.7 Porosity. When specified in the contract or order (see 6.2), material shall show no leakage, when tested with a helium leak detector (see 4.5.7). 3.8 Permissible variations in dimensions. The permissible variations in dimensions shall be as shown in applicable paragraph and table for the various forms of material (see 4.4.1). 3.8.1 Bars, rods, and wire diameter, thickness, or width. Bars, rods, and wire, measured on their diameters or between parallel faces, shall not vary at any point from the specified dimensions by more than the amounts shown in Tables VI, VII, VIII, and IX. 3.8.1.1 Straightness. The permissible variation in straightness of rods and bars as determined by the departure from true straightness (thrown in one revolution for rods or depth of chord for bars) shall be as specified in Table X. 3.8.2 Ribbon width. The permissible variation in width of ribbon shall be as specified in Table XI. 3.8.2.1 Ribbon thickness. The permissible variation in thickness of ribbon shall be the same as those applicable to wire in Table VI. Strip dimensions. The strip 3.8.3 dimensions and allowable variation shall conform to Tables XII, XIII, and XIV. 3.8.3.1 Thickness. Permissible variation in thickness of cold rolled strip shall be as specified in Table XII. 3.8.3.2 Strip crown tolerance. Permissible variation in crown tolerance, which is a permissible additive variation at the middle of the strip to the permissible variation at the edge as specified in 3.8.3.1 and Table XI, shall be as specified in Table XIII. 3.8.3.3 Strip width. Permissible variation in width of cold rolled slit edge strip shall be as specified in Table XIV. The dimensions for American Society for Testing and Materials Publications ASTM E8 - Methods of Tension Testing of Metallic Material ASTM E18 - Methods of Test for Rockwell Hardness and Rockwell Superficial Hardness of Metallic Materials ASTM E112 - Methods for Estimating the Average Grain Size of Metals ASTM E228 - Method of Test for Linear Thermal Expansion of Rigid Solids with a Vitreous Silica Dilatometer (Application for copies of ASTM publications should be addressed to American Society for Testing and Materials, 1916 Race Street, Philadelphia, PA 19103.) 3. Requirements 3.1 Condition and temper. Unless otherwise specified in the contract or purchase order, rod, ribbon, tubing, and wire shall be bright annealed. Strip shall be annealed properly to have deep drawing or spinning properties. (see 6.2). 3.1.1 Drawing and forming. Compounds and lubricants used in drawing and forming operations and during cold working shall be capable of being completely removed by vapor degreasing. * 3.2 Chemical composition. The chemical composition of the iron-nickel alloys shall be as specified in Table II (see 4.5.1). * 3.3 Linear coefficient of thermal expansion. The linear coefficient of thermal expansion shall conform to the value for the applicable class as listed in Table III (see 4.5.2). * 3.4 Tensile strength or hardness. The tensile strength for the applicable class of materials in the finished form and in the specified condition and temper shall conform to Table IV (see 4.5.3). If the size of product prevents the cutting of tensile specimens as defined by ASTM E8, conformance to hardness requirements of Table V may be substituted. 3.5 Grain size. The average grain size of annealed strip materials to be used for deep drawing or spinning purposes shall be no larger than No. 5 and no more than 10 percent of the individual grains may be larger than No. 5 (see 4.5.5). However, for material of Class- 85 MIL-I-23011 C either as seamless or welded, shall be as specified in Table XV. 3.9 Identification. Material shall be furnished in lots which shall be identified by this specification number, class number, finish, manufacturer’s alloy designation, name or symbol of supplier, melt number and size. strip, other than slit edge, shall be as negotiated between the vendor and procuring activity, and permissible variations in width shall be as specified in Fed. Std. No. 48 for low alloy steel strip. * 3.8.4 Tubing dimensions. Permissible variation in dimensions of cold drawn tubing, Table II. Chemical composition Class Elements (percent) 1/ Nickel (Ni) Cobalt (Co) Chromium (Cr) Manganese (Mn) Silicon (Si) Carbon (C) Aluminum (AI) Magnesium (Mg) Zirconium (Zr) Titanium (Ti) Phosphorus (P) Sulfur (S) Iron (Fe) 1 2 3 4 5 6 7 2/ 29 2/ 17 --0.50 0.20 0.06 3/ 0.10 3/ 0.10 3/ 0.10 3/ 0.10 ----Remainder 2/ 50.5 0.50 0.10 0.60 0.30 0.05 0.10 ------0.025 0.025 Remainder 2/ 48 0.50 0.10 0.80 0.30 0.05 0.10 ------0.025 0.025 Remainder 2/ 46 0.50 0.10 0.80 0.30 0.05 0.10 ------0.025 0.025 Remainder 2/ 41 0.50 0.10 0.80 0.30 0.05 0.10 ------0.025 0.025 Remainder 2/ 42.0 --2/ 5.6 0.25 0.30 0.07 0.20 ------0.025 0.025 Remainder 2/ 35.5-36.5 --0.25 0.50 0.25 0.05 3/ 0.10 3/ 0.10 3/ 0.10 3/ 0.10 0.020 0.020 Remainder 1/ All percentages are maximum, unless otherwise indicated. 2/ Nominal contents. The nominal contents of the alloys shall be adjusted by the supplier so that the alloys meet the requirements for thermal expansion (see 3.4) 3/ Total permissible contents of aluminum, magnesium, zirconium, and titanium shall not exceed 0.20 percent. Table III. Linear coefficients of thermal expansion Linear coefficient of thermal expansion –6 cm. per cm. per °C × 10 Temperature Range — °C 30-100 30-200 30-300 30-350 30-400 30-425 30-450 30-500 30-550 Class 1 2 3 4 5 6 7 --------4.6-5.2 --5.1-5.5 ----- ------------9.6-10.1 --10.2-10.7 --------8.2-9.2 ------9.6-10.3 ------7.1-7.8 ------8.2-8.9 --- ----4.0-4.7 ------6.7-7.4 ----- ------8.5- 9.2 --9.7-10.4 ------- 0.8-1.6 1.3-2.1 --6.2-7.0 ----8.5-9.2 ----- Table IV. Tensile Strength (1,000 psi) Condition All classes Annealed 1/4 Hard 1/2 Hard Hard 85 max. 90 to 115 105 to 125 120 min. 86 MIL-I-23011 C Table V. Condition Hardness, Rockwell B Class 2,3,4,5,7 1 Annealed 1/4 Hard 1/2 Hard 35 max. 90 to 93 94 to 96 70 max. 78 to 83 84 to 88 1/ 70 max. 78 to 83 84 to 88 1/ 2/ 1/ Hardness for deep drawing strip material less than 0.100 inch shall be Rockwell B82 maximum and Rockwell B85 maximum for material over 0.100 inch. 2/ The maximum hardness for deep drawing strip material shall be Rockwell B90. Table VI. Permissible variation in diameter of cold drawn wire and rods Specified diameter, inch Permissible variation plus or minus, inch Under 0.008 Over 0.008 to 0.015, incl. Over 0.015 to 0.020, incl. Over 0.020 to 0.030, incl. Over 0.030 to 0.040, incl. Over 0.040 to 0.060, incl. Over 0.060 to 0.080, incl. Over 0.080 to 0.125, incl. Over 0.125 to 0.156, incl. Over 0.156 to 0.188, incl. Over 0.188 to 0.250, incl. Over 0.250 to 0.500, incl. Over 0.500 to 1.000, incl. 0.00025 0.0003 0.0004 0.0005 0.0006 0.0007 0.0008 0.001 0.0015 0.002 0.005 0.010 0.020 Table VII. Permissible variation in distance between parallel surfaces of cold drawn bars Permissible variation under specified dimension, inch Specified dimension, inch 1/ 0.0002 0.00025 0.0003 0.0004 0.0005 0.0006 0.0007 0.001 0.002 0.002 0.0043 and under 0.0044 to 0.0079, incl. 0.008 to 0.0149, incl. 0.0150 to 0.0199, incl. 0.020 to 0.031, incl. 0.032 to 0.045, incl. 0.046 to 0.079, incl. 0.080 to 0.1875, incl. 0.1876 to 0.406, incl. Over 0.406 1/ 6 Dimensions apply to the distance between flats for hexagons and squares and separately to width and thickness of rectangles. 87 MIL-I-23011 C Table VIII. Permissible variation in diameter of hot rolled rods Specified diameter, inch Permissible variation from specified diameter plus or minus, inch 0.250 to 0.750, incl. Over 0.750 to 1.250, incl. Over 1.250 to 3.500, incl. 0.010 0.015 0.025 Table IX. Permissible variation in diameter of centerless ground rods Specified diameter, inch Permissible variation, inch 0.835 and under 0.836 to 1.125, incl. 1.126 to 1.750, incl. 1.751 to 2.000, incl. 2.001 to 3.000, incl. Table X. Plus Minus 0.000 0.002 0.0025 0.004 0.005 0.002 0.002 0.0025 0.004 0.005 Permissible variation in straightness of rods and bars Specified diameter or distance between parallel surfaces, inch 1/ Permissible variation in given lengths, inch Rods — cold drawn: 0.500 and under Over 0.500 to 1.000, incl. Throw in one revolution: 0.003 in 18 inches of length 0.005 in 42 inches of length Rods — hot rolled: All sizes Throw in one revolution 0.150 in 36 inches of length Bars — cold drawn: All sizes 2/ Depth of chord: 0.150 in 36 inches of length 1/ Dimensions apply to the diameter of rods, distance between parallel flats for hexagons and squares, and separately to width and thickness of rectangles. 2/ Bars are available with square, rectangular, and hexangular cross-sectional areas. Table XI. Permissible variation in width of ribbon or flattened round wire Specified width, inch Permissible variation in width, plus or minus, inch 0.0156 and under 0.0157 to 0.0468, incl. 0.0469 to 0.0781, incl. 0.0782 to 0.1875, incl. Over 0.1875 0.0015 0.002 0.0025 0.003 0.005 88 MIL-1-23011 C Table XII. Permissible variation in thickness of cold rolled strip 1/ Permissible variation in thickness, plus or minus, for given width, inch Over Over Over Less than 3 to 6 6 to 12 12 to 16 3 inches inches inches inches Specified thickness, inch Under 0.006 0.006 to 0.009, incl. 0.0091 to 0.010, incl. 0.0101 to 0.011, incl. 0.012 to 0.016, incl. 0.017 to 0.019, incl. 0.020 to 0.025, incl. 0.026 to 0.028, incl. 0.029 to 0.034, incl. 0.035 to 0.049, incl. 0.050 to 0.068, incl. 0.069 to 0.099, incl. 0.100 to 0.160, incl. 1/ 0.0005 0.00075 0.001 0.001 0.001 0.001 0.001 0.0015 0.0015 0.002 0.002 0.002 0.002 0.0005 0.00075 0.001 0.001 0.001 0.001 0.0015 0.0015 0.002 0.0025 0.003 0.003 0.003 ----0.001 0.001 0.0015 0.0015 0.002 0.002 0.0025 0.003 0.003 0.003 0.004 ----0.001 0.0015 0.0015 0.002 0.002 0.002 0.0025 0.003 0.003 0.004 0.004 Measurements shall be made at least 3/8 inch from the edge of strips over 1-inch wide. Table XIII. Permissible crown in cold rolled strip Permissible additional thickness at middle of strip over that provided for in Table XI for edge measurements, for given widths, inch Over Over To 5 to 12 12 to 24 5 inches inches inches incl. incl. incl. Specified thickness, inch 0.010 and under Over 0.010 to 0.025, incl. Over 0.025 to 0.065, incl. Over 0.065 to 0.188, incl. Table XIV. 0.00075 0.001 0.0015 0.002 0.001 0.0015 0.002 0.0025 0.0015 0.002 0.0025 0.003 Permissible variation in width of cold rolled strip Specified thickness, inch Specified width, inches Permissible variation in width, plus or minus, inch Under 0.125 0.125 to 0.188, incl. Over 0.750 to 5, incl. Over 5 to 16, incl. 0.005 0.010 Table XV. Specified outside diameter, inch Less than and excluding 3/32 3/32 to 3/16, excl. 3/16 to 1/2, excl. 1/2 to 1-1/2, excl. Permissible variation in dimensions of seamless or welded cold-drawn tubing Outside diameter, inch Plus Minus 0.002 0.003 0.004 0.005 0.000 0.000 0.000 0.000 89 Permissible variation Inside diameter, inch Plus Minus 0.000 0.000 0.000 0.000 0.002 0.003 0.004 0.005 Wall thickness, percent Plus or Minus 10 10 10 10 MIL-I-23011 C 3.10 Workmanship. All forms shall have uniform surface finishes. The surfaces shall be commercially smooth, free from scale, corrosion, cracks, scratches, seams, laps or folds, slivers and other injurious defects which would impair their serviceability for the use intended. or prepared from each group of ingots of the same alloy poured simultaneously from the same source of molten metal by the supplier for test of 4.5.2. The sample shall then be worked down to small rounds for testing. Specimens for thermal expansion tests may be taken from the same sample as the specimens for chemical analysis when dimensions permit. 4.3.2.2 Finished product sampling. Finished products need not be sampled unless in the form of bars and rods over ¼ inch in diameter. When sampling has not been made in accordance with 4.3.2.1, a sample over 6 inches in length shall be selected at random from each lot to provide a specimen for the test of 4.5.2. 4.3.3 Tensile test. A total of three specimens shall be taken from three individual lengths, selected at random from each lot. If the lot consists of less than three lengths, a specimen shall be taken from each length (see 4.5.3). 4.3.4 Hardness test. A total of three specimens shall be taken from three individual lengths selected at random from each lot. If the lot consists of less than three lengths, a specimen shall be taken from each length (see 4.5.4). 4.3.5 Grain size. Sampling shall be performed only on sheet and strip materials to be used for deep drawing purposes. A total of three specimens shall be taken from three individual lengths selected at random from each lot. If the lot consists of less than three lengths, a specimen shall be taken from each length (see 4.5.3). 4.3.6 Phase transformation test. Unless otherwise specified, one specimen ½ inch in length shall be taken from one individual length selected at random from each lot. The specimen shall be taken only from materials whose minimum cross-sectional dimension is less than 7/8 inch. The specimen shall include the entire cross-sectional area of the material if possible (see 4.5.6). 4.3.7 Porosity. When specified, one specimen shall be taken from one individual length selected at random from each lot. The specimen shall be taken only from material which can provide the dimensional requirements specified for a porosity test 4. Quality Assurance Provisions * 4.1 Responsibility for inspection. Unless otherwise specified in the contract or purchase order, the supplier is responsible for the performance of all inspection requirements as specified herein. Except as otherwise specified, in the contract or order, the supplier may use his own or any other facilities suitable for the performance of the inspection requirements specified herein, unless disapproved by the Government. The Government reserves the right to perform any of the inspections set forth in the specification where such inspections are deemed necessary to assure supplies and services conform to prescribed requirements. 4.2 Lot. Unless otherwise specified in the contract or purchase order (see 6.2), a lot shall consist of material of the same class, of one form, of the same cross-sectional area, condition, temper, and finish produced under the same conditions and submitted for delivery at one time. 4.3 Sampling. 4.3.1 Chemical test. 4.3.1.1 Ingot sampling. At least one sample shall be taken from each group of ingots of the same alloy poured simultaneously from the same source of molten metal by the supplier for the test of 4.5.1. Complete ingot analysis record shall be available to the procuring activity. 4.3.1.2 Finished product sampling. When sampling has not been made in accordance with 4.3.1.1, four individual lengths shall be selected at random from each lot of material to provide a composite sample for the test of 4.5.1. If the lot consists of less than 4 lengths, a sample piece shall be taken from each length. 4.3.2 Linear thermal expansion test. * 4.3.2.1 Ingot sampling. At least one sample from 6 to 10 inches in length and over ¼ inch in diameter shall be taken from each group 90 MIL-I-23011 C expansion of the alloy class in Table III in the dilatometer. * 4.5.2.1 Heat treatment of specimens. Prior to test, specimens for the thermal linear coefficient of expansion test (see 4.5.2) and phase transformation test (see 4.5.6) shall be heat treated in a furnace atmosphere of hydrogen as follows: Heat Class 1 alloy specimens for 1 hour at 900°C, raise temperature to 1100°C and soak specimens for 15 minutes. Between the 900°C and the 1100°C heat-treatment periods, the specimens may be cooled to room temperature. Heat soak Classes 2 through 5 and Class 7 specimens for 1 hour at 900°C, and Class 6 specimens for 15 minutes at 1100°C. At the end of the soak period, furnace cool to 175°C or less, preferably room temperature, at a cooling rate not to exceed 5°C per minute before removal from the oven. * 4.5.3 Tensile test. The samples selected in accordance with 4.3.3 shall be tested in accordance with ASTM E8 to assure compliance with the condition or temper specified in 3.4 and Table IV. * 4.5.4 Hardness test. The samples selected in accordance with 4.3.4 shall be tested in accordance with ASTM E18 to assure compliance with the condition or temper specified in Table V. * 4.5.5 Grain size. The specimens selected in accordance with 4.3.5 shall be polished, etched, and examined at 100 magnifications on a metallograph to assure compliance with the requirements of 3.5. Determinations of grain size shall be performed in accordance with ASTM E112. The specified grain size No. 5 represents grains having diameters between 0.060 to 0.064 mm or 16 grains per a square inch of image at 100 magnifications. 4.5.6 Phase transformation test. The specimen selected in accordance with 4.3.6 shall be examined for phase transformation or the presence of the alpha phase as follows: heat treat as specified in 4.5.2.1. When cool, polish and etch in an etchant consisting of three parts of concentrated hydrochloric acid and one part of concentrated nitric acid saturated with cupric chloride, prepared from 20 to 60 minutes prior to etching. Soak the etched specimen at –80°C, produced by an excess of dry ice in alcohol, for a minimum specimen in Figure 1 (see 4.5.7). 4.3.8 Visual and dimensional. A random sample shall be selected from each lot in accordance with MIL-STD-105, Inspection Level II, Acceptable Quality Level 2.5 percent defective for bars, rods, tubing and flat strip and an Acceptable Quality Level of 2.5 percent defects per 100 feet of coiled strip, ribbon, and wire. The sample footage of alloy material shall consist of approximately equal length of strips taken from the outer end of each coil or spool of wire, ribbon, and sheared strip in the lot. The total sample shall consist of a minimum of 50 feet from each lot. 4.4 Examinations 4.4.1 Visual and dimensional examination. Finished material selected in accordance with 4.3.8 shall be visually inspected to determine compliance with 3.10 and dimensionally examined to determine conformance to dimensional requirements of 3.8. 4.4.2 Preparation for delivery. The entire lot shall be visually examined to assure compliance with the identification requirements of 3.9 and the preservation, packaging, packing, and marking requirements of Section 5. 4.5 Tests. 4.5.1 Chemical Analysis Specimens shall be prepared from the samples selected in accordance with 4.3.1.1 or 4.3.1.2 and tested in accordance with Method 111 or Method 112 of Fed. Test Method Std. No. 151 to determine conformance to the chemical requirements of Table II. If the ingot sample fails to conform to Table II, the ingot shall be rejected. If the finished product sample fails to conform to Table II, the lot shall be rejected. 4.5.2 Linear thermal expansion. The sample selected as specified in 4.3.2.1 or the bar and rod finished product sample selected as specified in 4.3.2.2 shall be used to determine conformance of the material to 3.3. Dilatometric determination of the linear coefficient of thermal expansion shall be performed in accordance with the procedure described in ASTM E228. Prior to the dilatometric analysis, the specimen shall be heat treated as specified in 4.5.2.1. The linear thermal coefficient of expansion shall be determined from the cooling curve after heating the specimen 25° to 50°C above the highest temperature specified for the thermal 91 MIL-I-23011 C prepared specimen shall be decarburized in a furnace at 1100°C for 30 minutes and subsequently furnace cooled to 200°C or room temperature at a cooling rate not to exceed 5°C per minute. The furnace atmosphere during decarburization and cooling shall have a controlled hydrogen atmosphere at a dew point from 20°C to 30°C. The porosity test shall be performed upon the decarburized specimen, mounted as illustrated in Figure 2, upon the specimen containing fixture. After the decarburizing treatment, specimens should only be handled with tweezers, clean plastic gloves or finger cots. The tubulation of the specimen containing fixture shall be connected to the inlet of a fixed focus mass spectrometer. The fixture shall then be evacuated and the entire surface of the test specimen probed with a helium jet in accordance with Method 441 of Fed. Test Method Std. No. 151. When leakage is detected, the procedure shall be repeated by first of 4 hours. Examine microscopically at 150 magnifications over the entire surface. The presence of an acicular structure at any point on the etched surface shall be cause for rejection as specified in 3.6. * 4.5.7 Porosity test. When required, the specimen selected as specified in 4.3.7 and machined in accordance with Figure 1, shall be subjected to the porosity test using a helium leak detector sufficiently sensititve to -9 detect a leak of 1 × 10 cc per second at 20°C and one atmosphere pressure at a deflection of at least 5 percent of full scale. Prior to performing the actual test, the specimen shall be chemically prepared and metallurgically conditioned. Chemical preparation: The machined specimen shall be degreased in a solvent, such as acetone, pickled in an aqueous solution of 1 to 1 inhibited hydrochloric acid, rinsed and dried at a temperature from 105° to 110°C. Metallurgical conditioning: The chemically Specimen dimensions, inch A B C D E 1/2 to 1 1 to 2 0.090 ± 0.005 0.125 ± 0.005 0.250 0.250 .031 to .047 .031 R Max. Figure 1. Porosity Test Specimen 92 MIL-1-23011C Figure 2. Specimen Containing Fixture for Porosity Test 5. Preparation for Delivery A or C, as specified (see 6.2), in accordance with MIL-STD-163. 5.3 Packing. Packing of the bars, rods, ribbon, strips, tubing and wire shall be level A or C, as specified (see 6.2), in accordance with MIL-STD-163. 5.4 Marking. In addition to any special marking specified in contract or order, marking shall be in accordance with MIL-STD-163. 5.1 Preservation. When specified in the contract or order (see 6.2), the bars, rods, ribbon, strips, tubing, and wire shall be coated with preservative conforming to MIL-C-16173, grade 2. 5.2 Packaging. Packaging of the bars, rods, ribbon, strips, tubing, and wire shall be level 6. Notes 6.1 Intended use. Material procured by this specification is intended for applications in electronic components where hermetic seals are required between glass and metal or ceramic and metal. 6.1.1 Class 1 alloy is the sealing alloy most squirting or painting alcohol all around the specimen-to-neoprene seal and then probing with the helium jet to prove that the leakage is through the specimen and not at the seal. 4.6 Rejection criteria. Failure of any specimen to conform to this specification shall be cause for rejection of the lot represented. 93 MIL-I-23011 C commonly used with hard, low expansivity, borosilicate glasses where the applications require glasses of low thermal expansion, high thermal shock resistance, high strength, and high electrical resistance. In current commercial practice, the borosilicates have setting point temperatures ranging from 450°C to 472°C and thermal coefficients of expansion at these temperatures ranging from –6 5.0 to 5.8 × 10 cm/cm/°C. 6.1.2 Classes 2, 3, and 6 alloys are the sealing alloys used with soft glasses belonging to the potash-soda-lead and sodalime series. The setting point temperatures of these glasses range from 410° to 590°C, and the thermal coefficients of expansion at these –6 temperatures range from 9.7 to 10.2 × 10 cm/cm/°C. 6.1.3 Class 4 alloy is most frequently used for sealing applications with glazed ceramics. 6.1.4 Class 5 alloy is the sealing alloy used with the softer borosilicate glasses and leaded glasses. The leaded glasses are used where the applications demand glasses with very high surface resistivity or controlled radiaation shielding. * 6.1.5 Class 7 alloy is a low expansion material used as the sealing alloy in special applications, such as with optical glasses, where dimensional changes must be minimized when exposed to low temperatures such as –40°C to 0°C. * 6.2 Ordering data. Procurement documents should specify: strip if applicable (see 3.8). (i) Quantity of material required (see 4.2). (j) Additional specimens for phase transformation test (see 4.3.6). (k) Preservation, if required (see 5.1). (I) Level of packaging and packing required (see 5.2 and 5.3). (m) Special marking, if required (see 5.4). 6.3 Bar stock. Bar stock with square, rectangular, or hexagonal cross-sectional areas are generally not stock items, but are available upon request. * 6.4 Phase transformation. Specimens of Class 1 alloy being microexamined for phase transformation (see 4.5.6) may be compared with the illustrations shown in ASTM F 15, specification for Iron-Nickel-Cobalt Sealing Alloy, for presence or absence of an acicular structure. Figure 1 shows specimen with no transformation, whereas Figure 2 shows specimen with partial transformation. * 6.5 Typical thermal expansion data for the alloys are given in Table XVI to assist in the selection of material and for information only. * 6.6 For ease and simplicity of referencing this document with those documents issued by the American Society for Testing and Materials, the following cross reference is included for information only: MIL-I-23011 ASTM Designation Class 1 F15, Iron-nickel-cobalt sealing alloy F30, Alloy No. 52 Iron-nickel sealing alloy F30, Alloy No. 48 Iron-nickel sealing alloy F30, Alloy No. 46 Iron-nickel sealing alloy F30, Alloy No. 42 Iron-nickel sealing alloy F31, 42 percent nickel - 6 percent chromium iron sealing alloy Class 2 (a) Title, number, and date of this specification. (b) Class, form, and finish of material required (see 1.2, 1.2.1, 1.2.2, and 1.2.3). (c) Condition, and if applicable, temper (see 1.2, 1.2.4, and 3.1). (d) Porosity test, if required (see 3.7 and 4.3.7). (e) Diameter of rod and wire, if applicable (see 3.8). (f) Dimensions of bar stock, if applicable, as well as shape (square, rectangular, or hexangular (see 3.8). (g) Dimensions of tubing, if applicable (see 3.8). (h) Thickness dimension of ribbon and Class 3 Class 4 Class 5 Class 6 6.7 Changes from previous issues. The outer margins of this specification have been marked “*” to indicate where changes (deletions, additions, etc.) from the previous issue have been made. This has been done as a convenience only and the Government assumes 94 MIL-I-23011 C no liability whatsoever for any inaccuracies in these notions. Bidders and contractors are cautioned to evaluate the requirements of this document based on the entire contents as written irrespective of the marginal notations and relationship to the last previous issue. User Activities: Army - AT, AV, MI Navy - OS Air Force - 17 Review/user information is current as of the date of this document. For future coordination of changes to this document, draft circulation should be based on the information in the current Federal Supply Classification Listing of DoD Standardization Documents. Preparing Activity: Navy - AS Project No. 9505-0071 Custodians: Army - MR Navy - AS Air Force - 11 Review Activities: Army - ME Air Force - 84 Table XVI. Typical thermal expansion data Linear coefficient of thermal expansion — cm. per cm. per °C x 10–6 Temperature range °C Class 1 2 3 4 5 6 7 30 to 100 — 10.5 9.4 8.2 4.8 — 1.18 30 to 150 — 10.5 9.4 8.1 4.6 — — 30 to 200 5.5 10.4 9.4 7.9 4.5 — 1.72 30 to 250 — 10.4 9.3 7.8 4.5 — — 30 to 300 5.1 10.2 8.8 7.5 4.5 8.2 4.92 30 to 325 — — — — 4.7 — — 30 to 350 — 10.2 9.0 7.4 5.0 8.7 6.60 30 to 375 — — — 7.5 5.5 — — 30 to 400 4.9 10.1 8.7 7.5 6.0 10.0 7.82 30 to 425 — — 8.9 7.6 — — — 30 to 450 5.3 10.1 9.0 7.9 7.1 10.6 8.82 30 to 475 — 10.1 9.3 — — — — 30 to 500 30 to 525 30 to 550 6.2 — — 10.0 10.4 10.5 9.4 — 10.2 8.6 — 9.3 8.0 — 8.8 11.2 — 11.7 9.72 — — 30 to 600 7.9 10.8 10.4 9.8 9.5 12.2 11.35 30 to 700 9.3 11.7 11.3 10.7 10.5 13.0 12.70 30 to 800 10.4 12.5 12.1 11.6 11.4 13.7 13.45 30 to 900 11.5 13.3 13.0 12.5 12.3 14.6 13.85 30 to 1,000 — 14.2 13.9 13.4 13.2 15.4 — 95 MIL-M-38510F Military Specification MICROCIRCUITS, GENERAL SPECIFICATION FOR This specification is approved for use by all Departments and Agencies of the Department of Defense. This specification is intended to support Government microcircuit application and logistic programs. Detailed characteristics of microcircuits needed for a program are to be defined by detail drawings or specifications. 1. Scope Military MIL-STD-129 - Marking for Shipment and Storage. MIL-STD-280 - Definitions of Item Levels, Item Exchangeability, Models and Related Terms. MIL-STD-883 - Test Methods and Procedures for Microelectronics. 1.1 Statement of scope. This specification establishes the general requirements for monolithic, multichip, and hybrid microcircuits and the quality and reliability assurance requirements which must be met in the acquisition of microcircuits. Detail requirements, specific characteristics of microcircuits, and other provisions which are sensitive to the particular use intended shall be specified in the applicable device specification. Multiple levels of product assurance requirements and control for monolithic and multichip microcircuits and two levels for hybrid microcircuits are provided for in this specification. Military MIL-STD-976 - Certification Requirements for Microcircuits. MIL-STD-1331 - Parameters to be Controlled for the Specification of Microcircuits. MIL-STD-45662 - Calibration Systems Requirements. 2. Applicable Documents 2.1.2 Other Government documents, drawings, and publications. The following other Government documents, drawings, and publications form a part of this specification to the extent specified herein. 2.1 Government documents. 2.1.1 Specifications and standards. Unless otherwise specified, the following specifications and standards of the issue listed in that issue of the Department of Defense Index of Specifications and Standards (DoDISS) specified in the solicitation form a part of this specification to to the extent specified herein. Specification: Military MIL-M-55565 - Microcircuits, Packaging of. Cataloging Handbook H4-1 - Federal Supply Code for Manufacturers. DLAM 8200.2 - Procurement Quality Assurance Support Manual for Defense Contract Administration Service. NAVSHIPS 0967-190-4010 - Manufacturer's Designating Symbols. Standards: Federal FED-STD-209 - Clean Room and Work Station Requirements, Controlled Environments. FED-STD-595 - Color (Requirements for Individual Color Chips). Single copies of military specifications, standards and handbooks may be requested by mail or telephone from the Naval Publications and Forms Center, 5801 Tabor Avenue, Philadelphia, PA 19120. Not more than five items may be ordered on a single request; the invitation for bid or contract number should be cited where applicable. Beneficial comments (recommendations, additions, deletions) and any pertinent data which may be of use in improving this document should be addressed to: Rome Air Development Center (RBE-2). Griffiss AFB, NY 13441. 96 MIL-M-38510F Only latest revisions (complete with latest amendments) are available; slash sheets must be individually requested. Request all items by document number. For information on subscription service, direct inquiries to the above address with additional marking ATTN: Code 56, or telephone (215) 697-2179, Inquiry desk. Information on ordering copies of Federal specifications and standards may be obtained from General Services Administration offices in Atlanta; Auburn, Washington; Boston; Chicago; Denver; Fort Worth; Kansas City, MO; Los Angeles; New Orleans; New York; San Francisco; and Washington, DC. 2.2 Other Publications. The following documents form a part of this specification to the extent specified herein. The issues of the documents which are indicated as DoD adopted shall be the issue listed in the current DoDISS and the supplement thereto, if applicable. 3.5.1 Package. All devices supplied under this specification shall be hermetically sealed in glass, metal, or ceramic (or combinations of these) packages. No organic or polymeric materials (lacquers, varnishes, coatings, adhesives, greases, etc.) shall be used inside the microcircuit package unless otherwise specified. Desiccants may be used in the microcircuit package (except for class S devices where they are prohibited) only if each lot is subjected to and passes group B, subgroup 6 tests of method 5005 of MILSTD-883. The internal moisture content for class S devices after completion of all screening shall not exceed 5,000 ppm at 100°C. Polymer impregnations (backfill, docking, coating, or other uses of organic or polymeric materials to effect, improve, or repair the seal) of the microcircuit packages shall not be permitted. In addition, packages for class S microcircuits shall have metal body with hard glass seals, hard glass body, or ceramic body and the lids shall be welded, brazed, preform soldered, or glass frit sealed with a frit sealing temperature in excess of 385°C. In addition, glass frit sealed packages shall pass the Lid Torque Test (method 2024 of MILSTD-883) and Internal Water-vapor Content (method 1018 of MIL-STD-883) specified in the class S, group B tests. Packages with the lead frame attached to the body using a glass frit shall have glass on the mating surfaces only and the inside surfaces of the cavity shall not be coated with the seal glass. Single layer alumina metallized (SLAM) chip carrier packages are prohibited. American Society For Testing and Materials (ASTM) ASTM B487-79 - Measurement of Metal and Oxide Coating Thicknesses by Microscopical Examination of a Cross Section ASTM B567-79A - Measurement of Coating Thickness by the Beta Backscatter Method (Application for copies should be addressed to the American Society for Testing and Materials, 1916 Race Street, Philadelphia, PA 19103.) Electronic Industries Association (EIA) NOTE: Packages containing beryllia shall not be ground, sand-blasted, machined, or have other operations performed on them which will produce beryllia or beryllium dust. Furthermore, beryllium oxide packages shall not be placed in acids that will produce fumes containing beryllium. EIA-STD-RS-471 - Symbol and Label for Electrostatic Sensitive Devices (Application for copies should be addressed to the Electronic Industries Association, 2001 Eye Street, N.W., Washington, DC 20006.) MIL-M-38510F (Industry association specifications and standards are generally available for reference from libraries. They are also distributed among technical groups and using Federal Agencies.) 3.5.2 Metals. External metal surfaces shall be corrosion-resistant or shall be plated or treated to resist corrosion. External leads shall meet the requirements specified in 3.5.6. 3.5.3 Other materials. External parts, elements or coatings including markings shall be inherently nonnutrient to fungus and shall not blister, crack, outgas, soften, flow or 2.3 Order of precedence. In the event of a conflict between the text of this specification and the references cited herein, the text of this specification shall take precedence. 97 MIL-M-38510F strates(s) and package terminals or lands as applicable to the specific type of microcircuit supplied. If these interconnections show clearly on the die intraconnection pattern photograph, an additional photograph or drawing is not required. 3.5.4.4 Schematic diagrams. For microcircuits supplied under this specification, the actual schematic diagram(s), logic diagram(s), or combination thereof shall be provided, sufficient to represent all electrical elements functionally designed into the microcircuit together with their values (when applicable). For simple devices, this shall be a complete detailed schematic circuit showing all functional elements and values. For complex devices or those with redundant detail, the overall microcircuit may be represented by a logic diagram in combination with schematic details. As a minimum, details which must be included are: (a) a schematic presentation of input/output stages and protection network details identified by appropriate pin numbers, and (b) sufficient details to depict addressing or other device elements where the test parameters, conditions, or limits are sensitive to the specific device schematics. Where parasitic elements are important to the proper functioning of any microcircuit, they shall be included in the schematic diagram. 3.5.5 Internal conductors. Internal thin film conductors on silicon die or substrate (metallization stripes, contact areas, bonding interfaces, etc.) shall be designed so that no properly fabricated conductor shall experience in normal operation (at worst case specified operating conditions), a current density in excess of the maximum allowable value shown below for the applicable conductor material: exhibit defects that adversely affect storage, operation, or environmental capabilities of microcircuits delivered to this specification under the specified test conditions. 3.5.4 Design documentation. Design, topography, and schematic circuit information for all microcircuits supplied under this specification shall be submitted to the qualifying activity and shall be available inplant for review by the acquiring activity and the qualifying activity upon request. This design documentation shall be sufficient to depict completely the physical and electrical construction of the microcircuits supplied under this specification, and shall be traceable to the specific part, drawing or type numbers to which it applies, and to the production lot(s) and inspection lot codes under which microcircuits are manufactured and tested so that revisions can be identified. 3.5.4.1 Die topography. For semiconductor die (monolithic die or dice for inclusion in multichip or hybrid microcircuits), there shall be an enlarged color photograph(s) or transparency of diazotypes of the mask set showing the topography of elements of the die without the intraconnection pattern to a minimum magnification of 80 ×. If this results in a photograph larger than 8" × 10", the magnification may be reduced to accommodate an 8" × 10" view. 3.5.4.2 Die intraconnection pattern. There shall be an enlarged photograph(s) or transparency of diazotypes of the mask set to the same scale as the die topography (see 3.5.4.1) showing the specific intraconnection pattern used to connect the elements on the die so that elements used and those not used can be easily determined. For film hybrid or multichip microcircuits, this requirement shall apply to the substrate and all conductor pattern and active or passive circuit elements deposited thereon, as well as to semiconductor die, as applicable. 3.5.4.3 Die to terminal interconnection. There shall be an enlarged photograph(s), transparency, or drawing(s) to scale and of sufficient magnification to clearly depict the interconnection pattern for all connections made by wire or ribbon bonding, beam leads or other methods between the semiconductor die, other elements of the microcircuit, sub- Conductor material Aluminum (99.99% pure or doped) without glassivation or without glassivation layer integrity test Aluminum (99.99% pure or doped) glassivated (see 3.5.5.4) Gold All other (unless otherwise specified) 98 Maximum allowable current density 2 × 105 A/cm2 5 × 105 A/cm2 6 × 105 A/cm2 2 × 105 A/cm2 MIL-M-38510F bonding interfaces, etc.) shall be designated so that no properly fabricated conductor shall 2 dissipate more than 4 watts/cm when carrying maximum design current. 3.5.5.1 Metallization thickness. For class S microcircuits, the minimum metallization thickness shall be 8,000 Å (800 nm) for single level metal and for the top level of multilevel metal, and 5,000 Å (500 nm) for the lower level(s) of multilevel metal. In all cases, the current density requirements of 3.5.5 shall also be satisfied. 3.5.5.2 Internal wire size and material. For class S microcircuits, the internal wire diameter shall be 0.001 inch minimum (0.03 mm) and, except for hybrid microcircuits, the internal lead wire shall be of the same metal as the die metallization. 3.5.5.3 Internal lead wires. Internal lead wires or other conductors which are not in thermal contact with a substrate along their entire length (such as wire or ribbon conductors) shall be designed to experience, at maximum rated current, a continuous current for direct current, or an RMS current (peak current divided by √2), for alternating or pulsed current, not to exceed the values established by the following relationship. The current density shall be calculated at the point(s) of maximum current density (i.e., greatest current [see 3.5.5a] per unit cross section) for the specific device type and schematic or configuration. a. Use a current value equal to the maximum continuous current (at full fanout for digitals or at maximum load for linears) or equal to the simple timeaveraged current obtained at maximum rated frequency and duty cycle with maximum load, whichever results in the greater current value at the point(s) of maximum current density. This current value shall be determined at the maximum recommended supply voltage(s) and with the current assumed to be uniform over the entire conductor crosssectional area. b. Use the minimum allowed metal thickness per manufacturing specifications and controls including appropriate allowance for thinning experienced in the metallization step. The thinning factor over a metallization step is not required unless the point of maximum current density is located at the step. I = Kd3/2 c. Use the minimum actual design conductor widths (not mask widths) including appropriate allowance for narrowing or undercutting experienced in metal etching. where: I = Maximum allowed current in amperes. d = Diameter in inches for round wire (or equivalent round wire diameter which would provide the same crosssectional area for other than round wire internal conductor). K = A constant taken from the table below for the applicable wire or conductor length and composition used in the device. d. Areas of barrier metals and nonconducting material shall not be included in the calculation of conductor cross section. Thick film conductors on hybrid microcircuits or multichip substrates (metallization strips, Composition Aluminum Gold Copper Silver All other “K” values for bond-to-bond total conductor length Length ≤ 0.040" (0.10 cm) 22,000 30,000 30,000 15,000 9,000 99 Length > 0.040" (0.10 cm) 15,200 20,500 20,500 10,500 6,300 MIL-M-38510F 3.5.5.4 Verification of glassivation layer integrity. Where the current density of aluminum metallization for a device type to be qualified exceeds the allowable current density for unglassivated aluminum, the device type shall be subjected to and pass the requirements of MIL-STD-883 test method 2021 prior to part I or part II qualification (whichever comes first) and a photograph of the etched die shall be submitted with the qualification test report. One resubmission is permitted at twice the sample size. Unless otherwise specified by the qualifying activity, the device type shall be tested after sealing (or after exposure to the time/temperature sealing profile) in each package type for which the device type is to be qualified. Changes in design, materials, or process which affect current density or glassivation shall also be evaluated using MIL-STD-883, test method 2021. This evaluation applies only when the current density requirements for unglassivated aluminum are exceeded. 3.5.6 Lead or terminal material and finish. 3.5.6.1 Lead or terminal material. Lead or terminal material shall conform to one of the following chemical compositions: a. Type A Iron ............................. 53 percent, nominal Nickel ................................. 29 ± 1 percent Cobalt .................................. 17± 1 percent Manganese ........... 0.65 percent, maximum Carbon.................. 0.06 percent, maximum Silicon................... 0.20 percent, maximum Aluminum.............. 0.10 percent, maximum Magnesium ........... 0.10 percent, maximum Zirconium.............. 0.10 percent, maximum Titanium................ 0.10 percent, maximum (Combined total of aluminum, magnesium, zirconium and titanium to be a maximum of 0.20 percent). b. Type B Nickel ................................ 40 - 43 percent Manganese ........... 0.80 percent, maximum Silicon................... 0.30 percent, maximum Carbon.................. 0.10 percent, maximum Chromium ............. 0.25 percent, maximum Cobalt ................... 0.50 percent, maximum Phosphorus ........ 0.025 percent, maximum Sulfur.................. 0.025 percent, maximum Aluminum ..............0.10 percent, maximum Iron .......................................... Remainder c. Type C Co-fired metallization such as nominally pure tungsten. The composition and application processing of these materials shall be subject to qualifying activity approval and submitted with the application to test and as otherwise requested by the qualifying activity. 3.5.6.2 Microcircuit finishes. Finishes of all external leads or terminals and all external metallic package elements shall conform to either 3.5.6.2.1 or 3.5.6.2.2, as applicable. The lead finish designator (see 3.6.2.7) shall apply to the finish of the leads or terminals. The leads or terminals shall meet the applicable solderability and corrosion resistance requirements. The other metallic package elements (including metallized ceramic elements) shall meet the applicable corrosion resistance requirements. Finishes on interior elements (e.g., bonding pads, posts, tabs) shall be such that they meet lead bonding requirements and any applicable design and construction requirements. The use of strike plates is permissible to a maximum thickness of 10 microinches (0.25 µm). All plating of finishes and undercoats shall be deposited on clean, nonoxidized metal surfaces. Suitable deoxidation or cleaning operations shall be performed before or between plating processes. As defined above, all parts shall meet MIL-STD-883; method 2004, test condition B2, Bending Stress (except leadless chip carriers); method 1009, Salt Atmosphere; method 2003 or method 2022, Solderability (plus the time/temperature exposure of burn-in); method 2025, Adhesion of Lead Finishes; ASTM B487, Measurement of Metal and Oxide Coating Thicknesses by Microscopical Examination of a Cross Section, or ASTM B567, Measurement of Coating Thickness by the Beta Backscatter Method, or equivalent, and this capability shall be demonstrated when and as specified. The aforementioned ASTM methods are provided as reference methods to be used when the failure to pass other finish requirements suggests deficiencies in plating thickness. 100 MIL-M-38510F 3.5.6.2.1 Lead finish. The finish system on all external leads or terminals shall conform to one of the following: a. Hot solder dip. The hot solder dip shall be homogeneous with a minimum thickness of 60 microinches (1.52 µm) for round leads and, for other shapes, a minimum thickness at the crest of the major flats of 200 microinches (5.08 gm) solder (SN60 or SN63). In all cases, the solder dip shall extend up to and beyond the effective seating plane or to the glass seal for flushmounted devices. The hot solder dip is applicable: (1) over a finish in accordance with 3.5.6.2.1b or 3.5.6.2.1c (2) over electroplated nickel or electroless nickel phosphorus, per 3.5.6.2.3, or (3) over the basis metal. When applied over the basis metal, hot solder dip shall cover the entire lead to the glass seal or point of emergence of the lead or metallized contact through the package wall. b. Tin plate. As-plated tin shall be a minimum of 300 microinches thick and shall be dense, homogeneous and continuous. Asplated tin shall contain no more than 0.05 percent by weight co-deposited organic material measured as elemental carbon. Tin plate shall be fused after plating before or after burn-in by heating above its liquidus temperature. Fused tin plate shall be visually inspected after fusing and shall exhibit a dense, homogeneous and continuous coating. Fused tin plate shall be a minimum of 200 microinches thick when measured at the crest of major flats. This measurement shall be taken halfway between the seating plane and the tip of the lead. (This requirement is to avoid having the inspector select a nontypical portion of the lead on which to perform the measurement.) Fused tin plate is applicable: (1) over electroplated nickel or electroless nickel-phosphorous (only for rigid leads or package elements other than leads), per 3.5.6.2.3; or (2) over the basis metal. As-plated tin need not be fused if the leads are subsequently hot solder dipped in complete accordance with 3.5.6.2.1 a. Tinlead plating may be used as an alternative to tin plate and shall have in the plated deposit two percent to 50 percent by weight lead (balance nominally tin) homogeneously co-deposited. As-plated tin-lead shall be a minimum of 300 microinches thick. Asplated tin-lead shall contain no more than 0.05 percent by weight co-deposited organic material measured as elemental carbon. Tin-lead plate is applicable: (1) over as plated tin; (2) over electroplated nickel or electroless nickel phosphorous per 3.5.6.2.3; (3) over the basis metal. Tinlead plating may be fused after plating before or after burn-in by heating above its liquidus temperature. Fused tin-lead shall be visually inspected after fusing, and shall exhibit a dense, homogeneous and continuous coating. Fused tin-lead shall be a minimum of 200 microinches thick measured at the crest of the major flats. This measurement shall be taken halfway between the seating plane and the tip of the lead (this requirement is to avoid having the inspector select a nontypical portion of the lead on which to perform the measurement). The maximum carbon content for both tin and tin-lead plate (and minimum lead content in the tin-lead plate) on the as-plated finish shall be determined by the manufacturer on at least a weekly basis. The visual inspection after fusing shall be conducted on a sampling basis by the manufacturer as an in-process control. Visual inspection of the fusing shall be performed at a frequency sufficient to assure uniform compliance with these requirements on the finished product. The determination of carbon and lead content may be made by any accepted analytical technique (e.g., for carbon: pyrolysis, infrared detection [using an IR212, IR244 infrared detector or equivalent]; for lead: Xray fluorescence, emission spectroscopy) so long as the assay reflects the actual content in the deposited finish. c. Gold plate. Gold plating shall be a minimum of 99.7 percent gold, and only cobalt shall be used as the hardener. Gold plating shall be a minimum of 50 microinches (1.27 µm) and a maximum of 225 microin- 101 MIL-M-38510F ches (5.72 gm) thick. Gold plating shall be permitted over nickel plate or undercoating as per 3.5.6.2.3. 3.5.6.2.2 Package element (other than lead) finish. External metallic package elements other than leads or terminals (e.g., lids, covers, bases, seal rings, etc.) shall meet the applicable corrosion resistance and environmental requirements without additional finishing of the base material or else they shall be finished so that they meet those requirements using finishes conforming to one or more of the following as applicable: a. Solder per 3.5.6.2.1a. b. Tin plate per 3.5.6.2.1b. c. Gold plate per 3.5.6.2.1c except that for elements other than leads the gold plate shall be applied over electroless or electroplated nickel undercoating per 3.5.6.2.3. d. Nickel plate per 3.5.6.2.3. 3.5.6.2.3. Nickel plate or undercoating. Electroplated nickel undercoating or finishes from a sulfamate nickel bath is preferred and shall be 50 to 350 microinches (1.27 to 8.89 µm) thick measured on major flats or diameters. Electroless nickel undercoating or finishes, when allowed, shall be 50 to 100 microinches (1.27 to 2.54 µm) thick for leads and 50 to 250 microinches (1.27 to 6.35 µm) thick for package elements other than leads measured on major flats or diameters. The addition of organic addition agents is prohibited for either sulfamate or phosphorous nickel baths. Electroplate or electroless nickel plate (or combinations thereof) as well as nickel cladding may be used as the finish for package elements other than leads or terminals provided the corrosion resistance and environmental requirements are met. In all cases, electroplated nickel undercoating from a nickel sulfamate bath is preferred for lead and terminal finishes. Electroless nickel phosphorous shall not be used as the undercoating on flexible or semi-flexible leads (see 3.3.1 and 3.3.2 of method 2004 of MILSTD-883) and shall be permitted only on rigid leads or package elements other than leads. 102 QQ-N-290A November 12, 1971 Federal Specification Superseding Fed. Spec. QQ-N-290 April 5, 1954 NICKEL PLATING (ELECTRODEPOSITED) This specification was approved by the Commissioner, Federal Supply Service, General Services Administration, for the use of all Federal agencies. 1. Scope and Classification 1.1 Scope. This specification covers the requirements for electrodeposited nickel plating on steel, copper and copper alloys, and zinc and zinc alloys. 1.2 Classification. 1.2.1 Classes. Electrodeposited nickel plating covered by this specification shall be of the following classes, as specified (see 6.2): Class 1 - Corrosion protective plating Class 2 - Engineering plating 1.2.2 Grades. Class 1 plating shall be of the following grades, as specified (see 6.2): Grade A - 0.0016 inch thick Grade B - 0.0012 inch thick Grade C - 0.0010 inch thick Grade D - 0.0008 inch thick Grade E - 0.0006 inch thick Grade F - 0.0004 inch thick Grade G - 0.0002 inch thick 2. Applicable Documents 2.1 The following documents, of the issue in effect on date of invitation for bids or request for proposal, form a part of the specification to the extent specified herein. Federal Specification: QQ-S-624 - Steel Bar, Alloy, Hot Rolled and Cold Finished (General Purpose). Federal Standard: Fed. Test Method Std. No. 151 - Metals; Test Methods. (Activities outside the Federal Government may obtain copies of Federal Specifications, Standards, and Handbooks as outlined under General Information in the Index of Federal Specifications and Standards and at the prices indicated in the Index. The Index, which includes cumulative monthly supplements as issued, is for sale on a subscription basis by the Superintendent of Documents, U.S. Government Printing Office, Washington, DC 20402. (Single copies of this specification and other Federal Specifications required by activities outside the Federal Government for bidding purposes are available without charge from Business Service Centers at the General Services Administration Regional Offices in Boston, New York, Washington, DC, Atlanta, Chicago, Kansas City, MO, Fort Worth, Denver, San Francisco, Los Angeles, and Seattle, WA. (Federal Government activities may obtain copies of Federal Specifications, Standards, and Handbooks and the Index of Federal Specifications and Standards from established distribution points in their agencies.) Military Specification: MIL-S-5002 - Surface Treatments and Inorganic Coatings for Metal Surfaces of Weapons Systems. Military Standard: MIL-STD-105 - Sampling Procedures and Tables for Inspection by Attributes. (Copies of Military Specifications and Standards required by contractors in connection with specific procurement functions should be obtained from the procuring activity or as directed by the contracting officer.) 2.2 Other publications. The following documents form a part of this specification to the extent specified herein. Unless a specific issue is identified, the issue in effect on date of invitation for bids or request for proposal shall apply. American Society for Testing and Materials (ASTM) Standards: B487 - Measuring Metal and Oxide Coating Thickness by Microscopic Examination of a Cross Section. B504 - Measuring the Thickness of Metallic Coatings by the Coulometric Method. B529 - Measurement of Coating Thickness by the Eddy Current Test Method; Nonconductive Coatings on Nonmagnetic Basis Metals. 103 QQ-N-290A B530 - Measurement of Coating Thickness by the Magnetic Method: Electrodeposited Nickel Coatings on Magnetic and Nonmagnetic Substrates. (Application for copies should be addressed to the American Society for Testing and Materials, 1916 Race Street, Philadelphia, Pennsylvania, 19103.) 3. Requirements 3.1 Materials. The materials used shall be such as to produce platings which meet the requirements of this specification. 3.2 General requirements. 3.2.1 High tensile strength steel parts. Unless otherwise specified, steel parts having an ultimate tensile strength greater than 240,000 pounds per square inch (psi) shall not be plated without specific approval of the procuring activity (see 6.2). 3.2.2 Stress relief treatment. Unless otherwise specified, all steel parts which are machined, ground, cold formed or cold straightened shall be given a heat treatment at a minimum of 375 ± 25°F (191 ± 14°C) for three hours or more prior to cleaning and plating for the relief of damaging residual tensile stresses (see 6.2 and 6.4). 3.2.3 Cleaning. Unless otherwise specified, all steel parts shall be cleaned in accordance with MIL-S-5002 (see 6.2). Other basis metals shall be cleaned by methods which shall not damage the substrate and shall not interfere with adhesion of the deposit (see 6.5). 3.2.4 Plating application. Unless otherwise specified, the plating shall be applied after all basis metal heat treatments and mechanical operations such as machining, brazing, welding, forming and perforating of the article have been completed (see 6.2). 3.2.5 Underplating. When specified in the contract, purchase order or applicable drawing (see 6.2), Class 1 plating shall be applied over a plating of copper on steels, copper and copper based alloys. Class 1 plating shall be applied over an underplating of copper or yellow brass on zinc and zinc based alloys. In no case, shall the copper underplate (see 3.3.1.1.2 and Table I) be substituted for any part of the specified nickel thickness. 3.2.6 Class 1 processing. Parts for Class 1 deposition shall be plated to specific dimen- sions as specified (see 3.3.1.1). When specified, parts shall be processed in accordance with procedural instructions for form of nickel deposit. (see 6.2 and 6.7). 3.2.7 Class 2 processing. Parts for Class 2 deposition shall be plated to specific dimensions as specified (see 3.3.1.2). When specified, parts shall be processed in accordance with procedural instructions of the procuring activity (see 6.2). 3.2.8 Coverage. Unless otherwise specified, the plating shall cover all surfaces including roots of threads, corners and recesses (see 6.2). 3.2.9 Boundaries. Boundaries of Class 2 plating which cover only a portion of the surface shall be free from beads, nodules, jagged edges and other irregularities. 3.2.10 Surface finish. Unless otherwise specified, either a fully bright or dull (semibright finish shall be acceptable [see 6.2 and 6.7]). 3.2.11 Embrittlement relief. All steel parts having a hardness of Rockwell C40 and higher shall be baked at a minimum of 375 ± 25°F (191 ± 14°C) for three hours or more, within four hours after plating, to provide hydrogen embrittlement relief (see 6.6). The baked parts, when tested in accordance with 4.5.3, shall not crack or fail by fracture (see 4.4.3.3). Plated springs and other parts subject to flexure shall not be flexed prior to the hydrogen embrittlement relief treatment. 3.3 Detail requirements. 3.3.1 Thickness of plating. 3.3.1.1 Class 1. Unless otherwise specified, the minimum thickness of Class 1 nickel plating shall be as specified in Table 1 on all visible surfaces which can be touched by a ball 0.75 inch (19 mm) in diameter. All other surfaces which cannot be touched by the 0.75 inch (19 mm) diameter ball shall not be less than the minimum thickness specified in Table 1. 3.3.1.1.1 Unless otherwise specified, the minimum nickel plating for ferrous materials or for zinc and zinc base alloys shall be Grade C. Unless otherwise specified, the minimum nickel plating for copper and copper alloys shall be Grade D. If the maximum thickness for Grade A is not specified in the contract, order or applicable drawing, the thickness 104 QQ-N-290A shall not exceed 0.0020 inch (51 micrometers) on all visible surfaces which can be touched by the 0.75 (19 mm) diameter ball. 3.3.1.1.2 Underplate. When an underplate is employed (see 3.2.5), the thickness of the copper or other copper base alloy shall be as specified (see Table 1). The thickness of the underplate shall not be used in the determination of the specified nickel plating thickness. 3.3.1.2 Class 2. The thickness for Class 2 nickel plating shall be as specified in the contract, purchase order or on the applicable drawing (see 6.2). If a thickness is not specified, it shall be 0.003 inch (0.076 mm) for the finished part. In no case, shall the minimum nickel plating thickness be less than 0.002 inch (0.051 mm). The thickness requirement for Class 2 plating shall apply after all metal finishing operations have been completed. 3.3.2 Adhesion. The adhesion of the nickel plating and any undercoat or nickel layers shall be such that when examined at a magnification of approximately 4 diameters, Table I. neither the nickel plating, any layers of nickel plating nor any electrodeposited undercoat shall show separation from the basis metal or from each other at their common interface(s) when subjected to the test described in 4.5.2. The interface between a plating and the basis metal is the surface of the basis metal before plating. The formation of cracks in the basis metal or plate which do not result in flaking, peeling or blistering of the plate shall be considered as conformance to this requirement. 3.4 Workmanship. 3.4.1 Basis metal. The basis metal shall be free from visible defects that will be detrimental to the appearance or protective value of the plating. The basis metal shall be subject to such cleaning and plating procedures as necessary to yield deposits herein specified. 3.4.2 Plating. The nickel plating shall be smooth, fine grained, adherent, uniform in appearance, free from blisters, pits, nodules, excessive edge buildup and other defects. Minimum thickness of class 1 nickel plating Basis Metal Steels 1/, Zinc and Zinc Alloys 2/ Coating Grade A B C D E F – Plating Thickness Copper and Copper Alloys 3/ Coating Grade Surface touched by 0.75 inch dia. ball (see 3.3.1.1) All other surfaces 5/ Inch-Min. Inch-Min. – B C D E F G Equiv. Micrometers 4/ (approx.) 0.0016 0.0012 0.0010 0.0008 0.0006 0.0004 0.0002 40 30 25 20 15 10 5 0.0012 0.0010 0.0008 0.0006 0.0004 0.0002 0.0001 Equiv. Micrometers 4/ (approx.) 30 25 20 15 10 5 3 1/ Copper underplate shall be 0.0002 inch minimum. May range to 0.0010 inch depending on thickness of nickel plating. Use of extremely thin strikes may cause operational difficulties. 2/ Zinc and zinc alloys shall have a copper underplate of 0.0002 inch minimum thickness. 3/ Copper alloys containing zinc equal to or greater than 40 percent shall have a copper underplate of 0.0003 inch minimum thickness. 4/ 0.001 inch = 1 mil = 25.4 micrometers (microns). 5/ Threads, holes, deep recesses, bases of angles and similar areas. 105 QQ-N-290A The plating shall show no indication or contamination or improper operation of equipment used to produce the nickel deposit, such as excessively powdered or darkened platings, buildup and other defects. The size and number of contact marks shall be at a minimum consistent with good practice. The location of contact marks shall be in areas of minimum exposure to service environmental conditions where important to the function of the part. Superficial staining which has been demonstrated as resulting from rinsing, or slight discoloration resulting from baking operations to relieve embrittlement, as specified above (see 3.2.11), shall not be cause for rejection. All details of workmanship shall conform to the best practice for high-quality plating. 4. Quality Assurance Provisions 4.1 Responsibility for inspection. Unless otherwise specified in the contract or purchase order, the supplier is responsible for the performance of all inspection requirements as specified herein. Except as otherwise specified in the contract or order, the supplier may use his own or any other facilities suitable for the performance of the inspection requirements specified herein, unless disapproved by the Government. The Government reserves the right to perform any of the inspections set forth in the specification where such inspections are deemed necessary to assure that supplies and service conform to prescribed requirements. 4.2 Classification of inspection. The inspection requirements specified herein are classified as follows: 1 - Production control inspection (see 4.3) 2 - Quality conformance inspection (see 4.4) 4.3 Production control inspection. 4.3.1 Control records. When specified in the contract or order (see 6.2), the supplier shall maintain a record of each processing bath, showing all additional chemicals or treatment solutions to the unit, the results of all analyses performed and the quantity of parts plated during operation. Upon request of the procuring activity, such records shall be made available. These records shall be maintained for not less than one year after completion of the contract or purchase order. 4.3.2 Production control. The equipment, procedures and operations employed by a supplier shall be capable of producing highquality electrodeposited platings of nickel on ferrous alloys, copper and copper alloys, zinc and zinc alloys as specified in this document. When specified by the procuring activity (see 6.2), the supplier, prior to production, shall demonstrate the capability of the process used to show freedom from hydrogen embrittlement damage as indicated by satisfactory behavior of specimens prepared (see 6.2.2) and tested in acordance with 4.3.2.1 to comply to the requirements of MIL-S-5002 for preproduction process qualification. Preproduction control. For 4.3.2.1 preproduction control four round notched steel specimens shall be prepared in accordance with 4.4.4.2 from four individual heats for a total of 16 specimens, using the specified steel alloy for which preproduction examination of the process is to be demonstrated. Specimens shall be heat treated to the maximum tensile strength representing production usage. The specimens shall be given the same pretreatments, proposed for production. The specimens shall be subject to test detailed in 4.5.3. The process shall be considered satisfactory if all specimens show no indication of cracks or failure. The test results and production control information shall be submitted to the procuring activity for approval. Until approval has been received, parts shall not be plated. 4.3.3 Frequency of tests. To assure continuous control of the process as required by MIL-S-5002 and to prevent detrimental hydrogen embrittlement during production, the satisfactory behavior of specimens, prepared and tested in accordance with Table II, shall be made once each month or more frequently if required by the procuring activity. The results of tests made to determine conformance of electrodeposited platings to all requirements of this specification for definite contracts or purchase order are acceptable as evidence of the properties being obtained with the equipment and procedures employed. 4.3.4 Production control specimens. Test specimens for production control shall be prepared in accordance with 4.4.4 and 4.4.4.1 as 106 QQ-N-290A Table II. Production control tests and specimens Test For coating classes Requirement paragraphs Thickness 1 and 2 3.3.1, 3.3.1.1 and 3.3.1.2 4.4.4 and 4.4.4.1 4.5.1 Adhesion 1 and 2 3.3.2 4.4.4 and 4.4.4.1 4.5.2 Hydrogen embrittlement 1 and 2 3.2.11 4.3.4, 4.4.4, and 4.4.4.2 4.5.3 1/ Test reference paragraphs Standard alloy steels shall be used for production control specimens. The selection shall be at the option of the supplier; however, alloy steels such as AISI or SAE numbers 4130, 4135, 4140, 4145, 4340, 8645 and 8740 conforming to QQ-S-624 shall be used. applicable for the thickness and adhesion tests detailed in Table II. Specimens for the production control embrittlement relief test shall be four round notched steel specimens of alloy steel 4340 conforming to QQ-S-624, heat treated to the maximum tensile strength, from one or more heats, and prepared in accordance with 4.4.4.2. 4.4 Quality conformance inspection. 4.4.1 Lot. A lot shall consist of plated articles of the same metal composition, class and grade plated and treated under the same conditions and approximately the same size and shape submitted for inspection at one time. 4.4.2 Sampling for visual examination and non-destructive tests. Sampling for visual Table III. examination and non-destructive tests shall be conducted as directed by the procuring activity (see 6.2) in accordance with MILSTD-105 or using Table III. A sample of coated parts or articles shall be drawn by taking at random from each lot the number of articles in accordance with MIL-STD-105, Level 11, Acceptable Quality Level (AQL) 1.5 percent defective, or as indicated in Table Ill. The lot shall be accepted or rejected according to the procedures in 4.4.2.1 for visual examination and 4.4.2.2 for plating thickness (non-destructive tests). 4.4.2.1 Visual examination. Samples selected in accordance with 4.4.2 shall be examined for compliance with the requirements of 3.4.2 Sampling for visual examination and non-destructive tests Numbers of items in lot inspections 15 or less 16 to 40 41 to 110 111 to 300 301 to 500 501 and over 1/ Specimen preparation paragraphs 1/ Number of items in samples (randomly selected) 7 10 15 25 35 50 1/ Acceptance number (maximum number of sample item nonconforming to any test) 0 0 0 1 1 2 If the number of items in the inspection lot is less than 7, the number of items in the sample shall equal the number of items in the inspection lot. 107 QQ-N-290A after plating. If the number of nonconforming articles exceeds the acceptance number for the sample, the lot represented by the sample shall be rejected. 4.4.2.2 Thickness of plating (non-destructive tests). Samples selected in accordance with 4.4.2 shall be inspected and the plating thickness measured by the applicable tests detailed in 4.5.1, at several locations on each article as defined in 3.3.1, 3.3.1.1 or 3.3.1.2, as applicable, for compliance with the requirements. The part or article shall be considered nonconforming if one or more measurements fail to meet the specified minimum thickness. If the number of defective items in any sample exceeds the acceptance number for the specified sample, the lot represented by the sample shall be rejected. Separate specimens (see 4.4.4.1) shall not be used for thickness measurements unless a need has been demonstrated. 4.4.3 Sampling for destructive tests. A random sample of four plated parts or articles shall be taken from each lot for each destructive test or separately plated specimens shall be prepared in accordance with 4.4.4, 4.4.4.1 and 4.4.4.2 to represent each lot. If the number of articles in the lot is four or less, the number of articles in the sample shall be specified by the procuring activity (see 6.2). 4.4.3.1 Thickness of plating (destructive tests). If sampling and testing for thickness of plating by non-destructive testing is not the option of the supplier, samples selected in accordance with 4.4.3 shall be measured for plating thickness by the applicable tests detailed in 4.5.1 at several locations as defined in 3.3.1, 3.3.1.1 or 3.3.1.2, for compliance with the requirements. If the plating thickness at any place on any article or specimen is less than the specified minimum thickness, the lot shall be rejected. Separate specimens (see 4.4.4.1) shall not be used for thickness measurements unless a need has been demonstrated. 4.4.3.2 Adhesion (destructive tests). The articles or specimens used for the destructive thickness test (see 4.4.3.1), if of suitable size and form, may be used as the test pieces for the adhesion test to determine compliance with the requirements of 3.3.2. Failure of one or more of the test pieces shall constitute failure of the lot. 4.4.3.3 Hydrogen embrittlement relief (destructive tests). Unless otherwise specified in the contract or order, conformance to the requirements of 3.2.11 for hydrogen embrittlement relief of treated steel parts shall be determined for those parts having a tensile strength of or heat treated to a tensile strength of 240,000 psi or above and which will be subject to a sustained tensile load in use (see 6.2). A random sample of four plated articles shall be taken from each lot or four specimens, prepared in accordance with 4.4.4 and 4.4.4.2, shall be used to represent the lot. When tested as specified in 4.5.3, cracks or failure by fracture shall be cause for rejection. Failure of one or more of the test pieces shall reject the lot. 4.4.4 Quality conformance specimen preparation. When the plated articles are of such form, shape, size and value as to prohibit use thereof, or are not readily adaptable to a test specified herein, or when destructive tests of small lot sizes are required, the test shall be made by the use of separate specimens plated concurrently with the articles represented. The separate specimens shall be of a basis metal equivalent to that of the articles represented. “Equivalent” basis metal includes chemical composition, grade, condition and finish of surface prior to plating. For example, a cold-rolled steel surface should not be used to represent a hot-rolled steel surface. Due to the impracticality of forging or casting separate test specimens, hot-rolled steel specimens may be used to represent forged and cast-steel articles. The separate specimens may be also cut from scrap castings when ferrous alloy castings are being plated. These separate specimens shall be introduced into a lot at regular intervals prior to the cleaning operations, preliminary to plating, and shall not be separated therefrom until after completion of plating. Conditions affecting the plating of specimens including the spacing, plating media, residual air pressure, temperature, etc. in respect to other objects being plated shall correspond as nearly as possible to those affecting the significant surfaces of the articles represented. Separate specimens shall not be used for thickness measurements, however, unless the 108 QQ-N-290A necessity for their use has been demonstrated. 4.4.4.1 Specimens for thickness and adhesion tests. If separate specimens for thickness and adhesion tests are required, they shall be strips approximately 1 inch wide, 4 inches long and 0.04 inch thick. 4.4.4.2 Specimens for embrittlement relief. Separate specimens for embrittlement relief test shall be round notched specimens with the axis of the specimen (load direction) perpendicular to the short transverse grain flow direction. The configuration shall be in accordance with Figure 8 of ASTM E8 for rounded specimens. Specimens shall have a 60 degree V-notch located approximately at the center of the gage length. The cross section area at the root of the vee shall be approximately equal to half the area of the full cross section area of the specimen's reduced section. The vee shall have a 0.010 ± 0.0005 inch radius of curvature at the base of the notch (see 6.2.2). 4.5 Tests. 4.5.1 Thickness. For non-destructive measuring of plating thickness, procedures in accordance with Federal Test Method Standard No. 151, Method 520 (electronic test), ASTM B529 (eddy current), or ASTM B530 (magnetic test) may be used. For destructive measuring of plating thickness, procedures in accordance with ASTM B487 (microscopic) or ASTM B504 (coulometric) may be used. At the option of the supplier other instruments, such as those employing the principle of beta-radiation back scatter or X-ray spectrometry may be used. 4.5.2 Adhesion. Adhesion may be determined by scraping the surface or shearing with a sharp edge, knife, or razor through the plating down to the basis metal and examining at four diameters magnification for evidence of non-adhesion. Alternately the article or specimen may be clamped in a vise and the projecting portion bent back and forth until rupture occurs. If the edge of the ruptured plating can be peeled back or if separation between the plating and the basis metal can be seen at the point of rupture when examined at four diameters magnification, adhesion is not satisfactory. 4.5.3 Embrittlement relief. Compliance with 3.2.11 shall be determined with samples of plated parts taken as specified in 4.4.3.3. Parts such as spring pins, lock rings, etc. which are installed in holes or rods shall be similarly assembled using the applicable parts specifications or drawing tolerances which impose the maximum sustained tensile load on the plated part. The selected samples shall be subjected to a sustained tensile load equal to 115 percent of the maximum design yield load for which the part was designed. Parts which require special fixtures, extreme loads to comply with the above requirements, or where the maximum design yield load is not known may be represented by separate specimens prepared in accordance with 4.4.4.3. The notched specimens shall be subject to a sustained tensile load equal to 75 percent of the ultimate notch tensile strength of the material. The articles, parts or specimens shall be held under load for at least 200 hours and then examined for cracks or fracture. 5. Preparation for Delivery 5.1 Packaging and packing. Preservation, packaging and packing methods for electrodeposited nickel plated parts or articles employed by a supplier shall be such as to preclude damaging during shipment and handling. 6. Notes 6.1 Intended use. 6.1.1 Class 1 plating. Class 1 plating is used to protect iron, copper, or zinc alloys against corrosive attack in rural, industrial or marine atmospheres depending upon the thickness of the nickel deposit or is used as an undercoat for chromium or one of the precious metals. Class 1 plating is used also for decorative purposes. 6.1.2 Class 2 plating. Class 2 plating is used for wear resistance, abrasion resistance and such incidental corrosion protection of parts as the specified thickness of the nickel plating may afford. Heavy deposits of the Class 2 plating, especially when the Watts bath process is employed, may be used for buildup of worn or undersized parts, or for salvage purposes, and to provide protection against corrosive chemical environments. 109 QQ-N-290A 6.2 Ordering data. Purchasers should select the preferred options permitted herein and include the following information in procurement documents: (a) Title, number, and date of this specification. (b) Class of plating (see 1.2.1). (c) Grade of Class 1 plating if applicable (see 1.2.2). (d) When plating is to be applied, if other than specified (see 3.2.1, 3.2.4, 3.2.6 and 3.2.7). (e) Stress relief treatment, if other than specified (see 3.2.2). (f) Cleaning of steel, if other than specified (see 3.2.3). (g) Underplating required (see 3.2.5). (h) Coverage, if other than specified (see 3.2.8). (i) Surface finish, if particular finish required (see 3.2.10). (j) Thickness of coating, if other than specified (see 3.3.1, 3.3.1.1, 3.3.1.1.1 and 3.3.1.2). (k) Control record requirement (see 4.3.1). (I) Preproduction control examination (see 4.3.2). (m) Sampling plan (see 4.4.2). (n) Number of samples for destructive testing (see 4.4.3). (o) Whether hydrogen embrittlement relief test is required. (see 4.4.3.3). 6.2.1 The manufacturer of the basis metal parts should provide the plating facility with the following data: (a) Hardness of steel parts (see 3.2.1). (b) Heat treatment for stress relief, whether has been performed or is required (see 3.2.2). (c) Tensile loads required for embrittlement relief test, if applicable (see 4.5.3). 6.2.2 The manufacturer of the basis metal parts should provide the plating facility with notched tensile specimens (see 4.4.4.2) to be plated for conformance with 3.2.11 required for production control (see 4.3.2.1 and 4.3.4) and lot acceptance (see 4.4.3 and 4.4.3.3). 6.3 Black nickel plating. Electrodeposited black nickel plating, in accordance with MILP-18317, has little protective value and is used primarily to obtain a dark, nonreflective, decorative finish on steel and copper alloy instrument parts. 6.4 Stress relief. There is a hazard that hardened and tempered cold-worked or coldstraightened steel parts may crack during cleaning and plating. Such parts should have a suitable heat treatment for stress relief prior to cleaning and plating (see 3.2.2). 6.5 Cleaning. Copper and copper-based alloys may be cleaned as detailed in ASTM B281, Recommended Practice for Preparation of Copper and Copper-Base Alloys for Electroplating. Zinc and zinc-based alloys may be cleaned as detailed in ASTM B252, Recommended Practice for Preparation of Zinc-Base Die Castings for Electroplating (see 3.2.3). 6.6 Baking time. For high-strength materials (Rockwell C40 and above), it may be beneficial to extend the baking time to 23 hours to insure complete hydrogen embrittlement relief (see 3.2.11). 6.7 Class 1 processing. Class 1 plating may be processed for the following forms of nickel deposition: SB - Single layer coating in a fully bright finish. SD - Single layer coating in a dull or semibright finish, containing less than 0.005 percent sulfur and having an elongation greater than 8 percent. A full brightness finish may be obtained by polishing the coating. M - Multilayer coating, either double-layer or triple-layer. The bottom layer should contain less than 0.005 percent sulfur and have an elongation greater than 8 percent. The top layer should contain more than 0.04 percent sulfur. In a double-layer coating, the thickness of the bottom layer should be not less than 60 percent of the total nickel thickness, except on ferrous parts where the bottom thickness should be not less than 75 percent of the total nickel thickness. In a triple-layer coating, the thickness of the bottom layer should be not less than 50 percent of the total nickel thickness. The intermediate layer of the triple-layer coating should contain more sulfur than the top layer and the thickness should be not greater than 10 percent of the total nickel thickness. The 110 QQ-N-290A thickness of the top layer of either double- or triple-layer coating should be not less than 10 percent of the total nickel thickness. 6.7.1 Correlation. The correlation between the grades of nickel plating used in this specification and the forms of nickel deposition are indicated in Table IV. 6.7.2 Thickness measurements. Thickness measurements for the single layer Class 1 plating should be made whenever applicable by the non-destructive test methods, especially the magnetic method. Thickness measurements for the double or triple layer Class 1 plating should be made on cross sections taken perpendicular to the significant surfaces by the microscopic method. This permits measurements of the thickness of the individual nickel layers when suitable etchants are used. Suitable etchants are as follows: (a) Etchant No. 1. Nitric acid (sp. gr. 1.42) 1 volume Glacial acetic acid 1 volume (b) Etchant No. 2. Sodium cyanide 100 gms per liter of water Sodium or 100 gms per ammonium persulfate liter of water NOTE: Equal parts of the two water solutions (the cyanide and the persulfate) are mixed. Caution must be taken as toxic fumes are evolved when these solutions of the chemicals are mixed. Use of this etchant must be confined to a well-ventilated hood. When either of the two etchants are used, the microstructure of the dull or semi-bright nickel layer will be shown to be columnar, whereas that of the bright nickel layer will be banded or unresolved. 6.7.3 Sulfur contents. The sulfur contents stated in 6.7 indicate the kind of nickel plating solution that is to be used by the supplier. No simple method exists for the determination of the sulfur content of a nickel deposit on a coated article; however, X-ray fluorescence techniques can be used. 6.7.4 Corrosion protection. In a double-layer nickel deposition, as the undercoat with other electrodeposited top coats, the nickel immediately under the top coat is a bright nickel containing sulfur while the bottom layer under that is a semi-bright nickel essentially free of sulfur. In any galvanic electrolytic cell set up with the top coat, the bright nickel reacts anodically to the purer semi-bright nickel. If microscopic corrosion sets in through pores in the top coat material and penetrates the bright nickel layer, galvanic action between the two kinds of nickel tends to cause the microscopic pit to spread laterally in the outer nickel layer. The net effect is to retard penetration toward the base metal, hence to lengthen the useful life of the coating. This galvanic corrosion system may be further complicated by the use of three layers of nickel of different sulfur contents with further improvement against corrosion at a slightly Table IV. Correlation of class 1 nickel plating grades and deposition 1/ Grades A B C D E F G Forms of Deposition for Steels, Zinc and Zinc Alloys SD and M SD and M M SB, SD and M SB, SD and M SB, SD and M — 2/ 2/ 2/ For Copper and Copper Alloys — SB and M SB, SD and M SD and M SB, SD and M SB, SD and M SB, SD and M 2/ 2/ 2/ 1/ Where a dull or satin-like finish is required, unbuffed Form SD processed nickel may be substituted for Form SB processed nickel or for the bright layer of Form M processed nickel. 2/ Nickel deposited under Forms SD or M conditions may be substituted for nickel deposited in Form SB condition where the nickel deposit and top coat are subject to mild or moderate service conditions. 111 QQ-N-290A greater cost. 6.8 Cross-reference. The correlation between the grades of Class 1 nickel plating Table V. used in this specification and the previous designation (types) of Class 1 in QQ-N-290 are indicated in Table V. Correlation of class 1 nickel plating Basis Metal QQ-N-290 QQ-N-290A Types Grades Suggested forms of plating deposition (see 6.7) Steel I II III IV (DS) (FS) (KS) (QS) C E F G M SB SB SB Copper and Copper-based alloys V VI VII (FC) (KC) (QC) E F G SB SB SB Zinc and Zinc-based alloys VIII (FZ) IX (KZ) X (QZ) E F F SB SB SB 1/ 2/ 1/ When copper undercoat is omitted, the minimum nickel should be equivalent to Grade B, deposition forms SD or M (see 6.7). 2/ When copper undercoat is omitted, the minimum nickel should be equivalent to Grade D, plating form SB (see 6.7). 112 G2 Reprinted by the Nickel Development Institute with permission, from the Semiconductor Equipment and Materials Institute, Inc., Book of SEMI Standards, Copyright the Semiconductor Equipment and Materials Institute, Inc., 805 E. Middlefield Road, Mountain View, CA 94043. G2-86 SEMI SPECIFICATION METALLIC LEADFRAMES FOR CER-DIP PACKAGES 1. Preface This specification covers stamped or etched metallic leadframes used in construction of Cer-DIP packages. 2. Applicable Documents 2.1 This document specifically refers to: 1 MIL-I-23011 Iron/Nickel Alloys for Sealing to Glasses and Ceramics MIL-M-38510 General Specifications for Microcircuits MIL-STD-883 Test Methods and Procedures for Microelectronics 2.2 Related information may also be found in: MIL-STD-105 Sampling Procedures and Tables for Inspection by Attributes. 3. Selected Definitions bonding area - coined area on bond fingers within a distance of .030" (.762 mm) from lead tips. bottom formed width - see Figure 3. bow - curvature of the leadframe strip in the vertical plane; see Figure 1. burr - fragment of excess parent material attached to the leadframe edges. camber - curvature of the leadframe strip edge in the horizontal plane; see Figure 2. coined area - the area of the bond fingers planished to produce a flattened area for functional use; see Figure 3. coplanarity - the total indicator reading difference of the lead tips in the Z direction. datum plane - M is datum plane; see Figure 3. discoloration - a darkening or stain of the aluminum (metallization). foreign material - any adhering residue which is not of the leadframe composition. pit - a shallow surface depression or crater with a visible edge. planarity - total indicator reading of the lead tips in the Z direction relative to datum M. projection - a raised portion of the surface indigenous with the parent material, other than a burr. slug marks - random dents in the leadframe. stamped leadframe terminology - see Fig. 3. tilt - the deviation of the plane of the coined area from a condition parallel to the plane on datum M. top formed width - see Figure 3. twist - the angular rotation of one end of the leadframe or strip with reference to the other end; see Figure 4. void - an absence of aluminization from a designated area of the leadframe. 4. Ordering Information Purchase order for Cer-DIP metallic leadframes furnished to this specification shall include the following items: 1. Drawing number and revision level 2. Material 3. Number of leads 4. Description, see Table 1 5. Metallization thickness, type, and surface location 6. Form of leadframes (i.e., singles, scored strips or unscored strips) 7. Number of frames per strip; as applicable 8. Material certification 9. Packaging and marking 5. Dimensions and Permissible Variations The leadframe dimension shall conform to the specifications given in Table 1. 1 113 Military Standards, Naval Publications and Form Center, 5801 Tabor Ave., Philadelphia, PA 19120 G2 6. Materials 6.1 Leadframe 6.1.1 Chemical composition shall conform to the requirements of MIL-M-38510, Type A or B. 6.1.2 Material tensile strength shall be supplied per MIL-I-23011 6.2 Metallization - Aluminum 6.2.1 Thickness - 100 microinches minimum, 600 microinches maximum. 6.2.2 Coverage -.030" (.762 mm) minimum; measured from lead tip. Maximum to be determined by ceramic size. 6.2.3 Composition 6.2.3.1 Clad material - 99.4% minimum aluminum 6.2.3.2 Vapor deposition - 99.9 % minimum aluminum NOTE–The two types of aluminum may exhibit different visual appearances and non-functional characteristics after processing. 7. Defect Limits 7.1 Burrs 7.1.1 Horizontal 7.1.1.1 Bonding Area - .001" (.025 mm) max. 7.1.1.2 Other areas -.002" (.051 mm) max. 7.1.2 Vertical 7.1.2.1 Bonding Area -.001" (.025 mm) max. 7.2 Planarity/Coplanarity - See Table 1. 7.3 Foreign Materials - Leadframes shall be clean and free from foreign material such as photoresist, lubricants, solvent residue, water marks, and rust spots. Protective coatings acceptable to both vendor and user are not considered foreign material. 7.4 Pits and Slug Marks 7.4.1 Bonding Area -.001" (.025 mm) max. surface dimension × .0005" (.013 mm) max. depth. 7.4.2 Other Areas -.010" (.254 mm) max. surface dimension × .0005" (.013 mm) max. depth. 7.5 Projections 7.5.1 Bonding Area - None allowed. 7.5.2 Other Areas - .010" (.254 mm) max. surface dimension × .002" (.051 mm) max. height. 7.6 Scratches - There shall be no scratches in the aluminum metallization that penetrate to the underlying base material. 7.7 Voids - All metallized areas of the leadframe within the bonding area shall have no voids larger than .001" (.025 mm) in any dimension. 7.8 Twist - .004 inch per inch (.102 mm per mm) max. 7.9 Coining 7.9.1 Coined Depth - Minimum .0005" (.013mm); maximum .002" (.051 mm). Minimum coined depth may be controlled by minimum flat area. 7.9.2 Coined Flat Area - Minimum of 80% of normal lead width; measured .005" (.127 mm) back from lead tip. 7.9.3 Coined Length - Minimum .025" (. 635 mm) from lead tip. 7.10 Lead Position 7.10.1 Lead Position - A .007" (.178 mm) diameter circle must be 100% within nominal lead position when centered at lead nominal centerline and .007" (.178 mm) back from lead tip. 7.10.2 Minimum Spacing -.006" (.152 mm) minimum. 7.11 Bowing 7.11.1 Convex - .0025 inch per inch (.0025 mm per mm) maximum. 7.11.2 Concave -.0025 inch per inch (.0025 mm per mm) maximum. 7.12 Camber -.005 inch per inch (.005 mm per mm) maximum. NOTE–Items 7.11 and 7.12 refer to scored strips only. 8. Sampling Sampling will be determined between supplier and purchaser. 9. Test Methods 9.1 Sequence of Events and Tests The sequence of testing should be: 1. Degrease 2. Metallurgical Bond Adhesion (9.3.1) 3. Frame Attach 4. Die Attach 5. Bond 6. Pre-Seal Bond Pull (9.3.2) 7. Seal 8. Mechanical Testing (9.2) 9. Lead Trim 10. Post-Seal Bond Pull (9.3.2) NOTE—It is acknowledged that the leadframe manufacturer may not perform all these tests due to equipment and component limitations. Regardless, leadframes must fulfill these requirements, subject to the influence of the testing facility and associated components. 114 G2 9.2 Mechanical and Thermal 9.2.1 Temperature cycling - per MILSTD-883, Method 1010.4, Condition C. 9.2.2 Thermal shock - per MIL-STD-883, Method 1011.2, Condition C. 9.2.3 Centrifuge - per MIL-STD-883, Method 2001.2, Condition E. 9.2.4 Lead Integrity 9.2.4.1 A 500°C ± 20° –55% R.H. heat soak for 15 minutes ± 1 minute. Cooled at no more than 50°C per minute. Afterwards the frame is clamped between plates of a suitable size for the lead spacing (see 9.2.4.2); then (3) 90° cycles are performed. Frames are examined at 20× magnification and if cracks are observed at the Apex A (Figure 3) then the frame is rejected. 9.2.4.2 Plate shall be of equivalent planform to the ceramic being employed for the particular frame. An edge radius equivalent to 2T, where T is the leadframe thickness, shall be on the contacting surface of the plate. 9.3 Functional Test Methods 9.3.1 Metallurgical Bond Adhesion Aluminization - The metallurgical bond between the aluminization and the base metal shall permit the leadframe to be heated in air to 525°C ± 10°C for five (5) minutes minimum without evidence of aluminum peeling, blistering or discoloring when viewed at 20× magnification. (Discoloration must not jeopardize the user's standard part reliability.) Subsequently, the aluminized layer must pass the following two adhesion tests: 9.3.1.1 A cellophane type adhesive tape is firmly applied to the aluminization and removed toward the center of the cavity in a continuous rapid motion. This test is to be performed over the same area three times. No evidence of aluminum separation from the base metal shall be visible at 20× magnification. 9.3.1.2 The aluminization shall be capable of passing a functional wirebond test without separating. 9.3.2 Lead Bond Quality - Minimum pre-seal and post-seal bond strength test per MILSTD-883, Method 2011.2, Test Condition D. Applicable failure categories: A - 4 and A - 6. 10. Packaging and Marking 10.1 Packaging - Leadframes must be packaged in containers designed and constructed to prevent damage and/or contamination. Specific protection must be provided against foreseeable mechanical and environmental hazards. 10.2 Marking - The outer containers shall be clearly marked identifying the user, stock number, user purchase order number, drawing number, and vendor lot number. Table 1 Typical Ceramic Cer-DIP Metallic Leadframes Dimensions and Tolerance Requirements Description 8SSI Cavity Length — 8MSI — 8LSI — 14SSI 14MSI 16SSI 16MSI 16LSI .160 ± .007 4.06 ± .178 .260 ± .007 6.60 ± .178 .160 ± .007 4.06 ± .178 .260 ± .007 6.60 ± .178 .260 ± .007 6.60 ± .178 Cavity Width .120 ± .007 3.05 ± .178 .140 ± .007 3.56 ± .178 .160 ± .007 4.06 ± .178 .120 ± .007 3.05 ± 1.78 .140 ± .007 3.56 ± 1.78 .120 ± .007 3.05 ± .178 .140 ± .007 3.56 ± .178 .170 ± .007 4.32 ± .178 Lead-Formed Width, Top .311 ± .003 .790 ± .076 .311 ± .003 .790 ± .076 .311 ± .003 .790 ± .076 .311 ± .003 .790 ± .076 .311 ± .003 .790 ± .076 .311 ± .003 .790 ± .076 .311 ± .003 .790 ± .076 .311 ± .003 .790 ± .076 115 Bond Finger Layout End vs. Side 0 4 0 4 0 4 4 3 4 3 4 4 4 4 4 4 Nominal Progression .945 24.00 .945 24.00 .945 24.00 .945 24.00 .945 24.00 .945 24.00 .945 24.00 .945 24.00 Units in mm in mm in mm in mm in mm in mm in mm in mm G2 Table 1 (continued) Description 16SLSI 16VLSI 18MSI 18LSI 18VLSI 20MSI 20LSI 20VLSI 22MSI 22LSI 22VLSI 24MSI 24LSI 24VLSI 24SD3S 24SD3M 24SD4M 28MSI 28LSI 28VLSI 40MSI 40LSI Cavity Length .360 ± .007 9.14 ± .178 .330 ± .007 8.38 ± .178 .260 ± .008 6.60 ± .203 .260 ± .008 6.60 ± .203 .330 ± .008 8.38 ± .203 .210 ± .008 5.33 ± .203 .260 ± .008 6.60 ± .203 .330 ± .008 8.38 ± .203 .270 ± .010 6.86 ± .254 .310 ± .010 7.87 ± .254 .350 ± .010 8.89 ± .254 .260 ± .010 8.38 ± .254 .330 ± .010 8.38 ± .254 .420 ± .010 10.67 ± .254 .260 ± .010 6.60 ± .254 .430 ± .010 10.92 ± .254 .210 ± .010 5.33 ± .254 .260 ± .011 6.60 ± .279 .325 ± .011 8.26 ± .279 .420 ± .011 10.67 ± .279 .270 ± .012 6.86 ± .305 .375 ± .012 9.53 ± .305 Cavity Width .170 ± .007 4.32 ± .178 .180 ± .007 4.57 ± .178 .140 ± .008 3.56 ± .203 .170 ± .008 4.32 ± .203 .180 ± .008 4.57 ± .203 .140 ± .008 3.56 ± .203 .170 ± .008 4.32 ± .203 .175 ± .008 4.45 ± .203 2.10 ± .010 5.33 ± .254 .240 ± .010 6.10 ± .254 .260 ± .010 6.60 ± .254 .260 ± .010 6.60 ± .254 .285 ± .010 7.24 ± .254 .290 ± .010 7.37 ± .254 .170 ± .010 4.32 ± .254 .180 ± .010 4.57 ± .254 .210 ± .010 5.33 ± .254 .260 ± .011 6.60 ± .279 .275 ± .011 6.99 ± .279 .280 ± .011 7.11 ± .279 .260 ± .012 6.60 ± .305 .295 ± .012 7.49 ± .305 Lead-Formed Width, Top Bond Finger Layout End vs. Side .311 ± .003 .790 ± .076 .311 ± .003 .790 ± .076 .311 ± .003 .790 ± .076 .311 ± .003 .790 ± .076 .311 ± .003 .790 ± .076 .311 ± .003 .790 ± .076 .311 ± .003 .790 ± .076 .311 ± .003 .790 ± .076 .411 ± .003 10.44 ± .076 .411 ± .003 10.44 ± .076 .411 ± .003 10.44 ± .076 .611 ± .003 15.01 ± .076 .611 ± .003 15.01 ± .076 .611 ± .003 15.01 ± .076 .311 ± .003 7.90 ± .076 .311 ± .003 7.90 ± .076 .411 ± .003 10.44 ± .076 .611 ± .003 15.01 ± .076 .611 ± .003 15.01 ± .076 .611 ± .003 15.01 ± .076 .611 ± .003 15.01 ± .076 .611 ± .003 15.01 ± .076 4 4 6 2 4 5 6 3 6 3 4 6 6 4 6 4 6 5 6 5 8 3 6 6 6 6 6 6 6 6 8 4 6 6 8 6 8 6 8 6 10 10 12 8 Nominal Progression Units .945 24.00 .945 24.00 1.061 26.95 1.061 26.95 1.061 26.95 1.175 29.85 1.175 29.85 1.175 29.85 1.250 31.75 1.250 31.75 1.250 31.75 1.510 38.35 1.150 38.35 1.510 38.35 1.510 38.35 1.510 38.35 1.510 38.35 1.724 43.79 1.724 43.79 1.724 43.79 2.300 58.42 2.300 58.42 in mm in mm in mm in mm in mm in mm in mm in mm in mm in mm in mm in mm in mm in mm in mm in mm in mm in mm in mm in mm in mm in mm NOTE: While a .311 top form is still currently being used, numerous users have changed to a .314 top form to prevent interference between the Cer-DIP base and leadframe. 116 G2 Figure 1. Bow Figure 2. Camber Figure 3. Stamped Leadframe Terminology 117 G2 Using surface plate, establish a reference plane the whole length of the frame strip. Place frame strip, either method 1 or 2, whichever method gives a 3 point contact with reference plane A, using thickness gauges to determine height between reference plane and 4th point noted as t. This measurement will determine frame twist over entire length. Figure 4. Twist Strip Figure 5. Standoff Lead Length NOTICE: SEMI makes no warranties or representations as to the suitability of the standards set forth herein for any particular application. The determination of the suitability of the standard is solely the responsibility of the user. Users are cautioned to refer to manufacturer's instructions, product labels, product data sheets, and other relevant literature respecting any materials mentioned herein. These standards are subject to change without notice. 118 G4 Reprinted by the Nickel Development Institute with permission, from the Semiconductor Equipment and Materials Institute, Inc., Book of SEMI Standards. Copyright the Semiconductor Equipment and Materials Institute, Inc., 805 E. Middlefield Road, Mountain View, CA 94043. G4-86 SEMI SPECIFICATION INTEGRATED CIRCUIT LEADFRAME MATERIALS USED IN THE PRODUCTION OF STAMPED LEADFRAMES (PROPOSED) 1. Scope This specification covers the special requirements for metal strip to be used to fabricate integrated-circuit leadframes by stamping. 2. Applicable Documents ASTM B601 ASTM E8 ASTM B193 1 Recommended Practice for Temper Designations for Copper and Copper Alloys Wrought and Cast. Methods of Tension Testing of Metallic Materials Test Method for Resistivity of Electrical Conductor Materials this specification. Samples can be obtained from the ID or the OD of each coil. If the material does not conform to this specification, remove 2 wraps from the ID and OD of each coil and test for conformance again. 5.2 Thickness and Width - The tolerances for thickness and width shall be as shown on Table 1. More restrictive tolerances than those shown below or tolerances for other thickness and widths shall be as agreed upon by purchaser and supplier. Table 1 Thickness and Width Tolerances 3. Ordering Information Orders for material under this specification shall include the following information: 1. Quantity of each size 2. Alloy name and number 3. Temper or mechanical properties 4. Dimensions: thickness and width (See 5) 5. How furnished: coils and coil size (See 8) 6. Certification or test report requirements (See 9), and 7. Packaging and marking requirements (See 10) 4. General Requirements 4.1 The materials covered by this specification shall conform to the requirements detailed herein, unless otherwise agreed upon by supplier and purchaser. 5. Dimensions and Tolerances 5.1 The following tests shall be used to determine conformance or non-conformance to Thickness .006" (.152 mm) .008" (.203 mm) .010" (.254 mm) .015" (.381 mm) .020" (.508 mm) Tolerance ± .0003" (.008 mm) ± .0003" (.008 mm) ± .0003" (.008 mm) ± .0004" (.010 mm) ± .0005" (.013 mm) Width ≤ 2.000" (50.80 mm) 2.001-2.500" (50.83-63.50 mm) Tolerance ± .002" (.054 mm) ± .002" (.051 mm) 5.3 Camber (Edgewise Curvature) - A six or eight foot long strip sample shall be placed on a flat surface against the edge of a six foot (or longer) straight edge. The largest amount of separation of the strip sample from the straight edge shall be measured. Extreme care must be exercised with this test to ensure that the sample illustrates a uniform camber (no reverse curvature should be present in the sample), and also that it is not bent or kinked, as this could result in a grossly inaccurate measurement. The maximum camber allow1 119 ASTM Specifications, 1916 Race Street, Philadelphia, PA 19103 G4 able in any 72" or 96" length is shown in Table 2. Table 2 Camber Limits Specified Width inches .600-.949 (15.24-24.11 mm) ≥ .950 (24.13 mm) Camber in any 72" length, inches .250 (6.35 mm) .125 (3.18 mm) Camber in any 96" length, inches .438 (11.13 mm) .219 (5.56 mm) 7. Corrosion 5.4 Coil Set - A three foot long sample shall be held with one end against a flat vertical surface. The distance between the flat vertical surface and the free hanging end of the strip (that is positioned for maximum distance from the flat vertical surface) shall be measured. The measured coil set shall not exceed 1.5" (38.10 mm). Coil set is dependent on alloy, temper, and coil diameter and, where the combination of these requirements results in coil set (1.5" [38.10 mm] or less), it shall be uniformly in the direction of coiling. 5.5 Twist - The twist shall not exceed 20° over the three foot sample. (See Figure 1 for an example of a fixture commonly used to measure twist.) 5.6 Edge Burrs - Undesirable and, if present, their height shall not exceed 10% of the metal thickness. 5.7 Crossbow (dish) - Crossbow shall be measured using a toolmaker's microscope or equivalent, with any burrs present being removed prior to measurement. The maximum crossbow allowable shall be shown in Table 3 unless otherwise agreed upon between supplier and purchaser. Table 3 Maximum Crossbow Specified Width, inches Up to 1.000" (25.4 mm) incl. Over 1.000" (25.4 mm) up to 2.000" (50.8 mm), incl. mm) in depth shall be acceptable unless otherwise agreed upon between supplier and purchaser. 6.3 Material shall meet an 8 micro inch (RMS) maximum surface roughness as measured across the direction of rolling. Maximum Crossbow .003 (.076 mm) .006 (.152 mm) 6. Surface Finish 6.1 The material shall be commercially free of surface imperfections such as pits, nicks, dents, gouges, scratches, laminations, or inclusions. 6.2 Surface defects less than .0003" (.0076 7.1 Visual inspection shall be used to determine if objectionable surface oxides are present which would render the product unusable for the intended application. Objectionable conditions, if present, should be reported to the supplier within 60 days after the receipt of the material. 7.2 There shall be no visible rust on the surface of the Alloy 42 material. 8. Coils 8.1 Unless otherwise specified, coils shall be supplied with an inside diameter that provides for good packing practice without resulting in excessive coil set. 8.2 All coils supplied shall be continuous, uniform lengths, and free of welds. Autogenous welds made at heavy gauge, prior to finish reductions that ultimately provide homogeneous structures, are allowed. 9. Certification or Test Reports 9.1 Requests for certifications or test reports shall be made at the time of order entry or contract agreement. They shall be furnished by the manufacturer within one week of date of shipment. 9.2 When certifications are required, the following information shall be supplied as a minimum: 1. Vendor name 2. Purchase order number 3. Vendor order number 4. Alloy name and number 5. Chemical analysis 6. Temper designation, reference only (for copper base alloys only) (ASTM 13601) 7. Tensile strength (ASTM E8) 8. Elongation percent in 2" (ASTM E8) 9. Electrical conductivity % IACS (for copper base alloys only) (ASTM 13193) 9.3 In the event of a disagreement between supplier and purchaser, an independent test shall be conducted on strip to verify the data 120 G4 supplier and purchase. provided in the certification. 10. Packaging and Marking 10.1 the material shall be separated by size, compositions, and temper, and prepared for shipment in such a manner as to ensure acceptance by a common carrier for transportation at the lowest applicable rate. 10.2 The material shall be suitably packaged to protect from condensation, contamination, etc., and to afford protection from the normal hazards of transportation. 10.3 Each shipping unit shall be legibly marked with the purchase order number, alloy name or number, temper, size, gross and net weight, and name of the supplier. The specification number shall be shown when specified on the purchase order. 10.4 Any special packaging or shipping requirements shall be agreed upon between purchaser at the time of 11. Basis for Rejection 11.1 For the purposes of determining conformance with the requirements prescribed in the specifications, any measured value outside the specified limiting values shall be cause for rejection. 11.2 If objectionable material is found and rejected, samples of the questionable material, with the defects identified and marked, should be sent to the supplier along with information as to order number, quantity originally received, date received, and quantity rejected. Rejected material should be held with adequate protection and identification by the purchaser for a reasonable amount of time, pending investigation by the supplier. Figure 1. Twist Measurement Fixture (Continued on next page) 121 G4 Figure 1. (cont.) NOTICE: SEMI makes no warranties or representations as to the suitability of the standards set forth herein for any particular application. The determination of the suitability of the standard is solely the responsibility of the user. Users are cautioned to refer to manufacturer's instructions, product labels, product data sheets, and other relevant literature respecting any materials mentioned herein. These standards are subject to change without notice. 122 G22 Reprinted by the Nickel Development Institute with permission, from the Semiconductor Equipment and Materials Institute, Inc., Book of SEMI Standards. Copyright the Semiconductor Equipment and Materials Institute, Inc., 805 E. Middlefield Road, Mountain View, CA 94043 G22-86 SEMI SPECIFICATION CERAMIC PIN GRID ARRAY PACKAGES (PROPOSED) 1. Preface This specification defines the acceptance criteria for cofired ceramic pin grid array packages. 2. Applicable Documents MIL-STD-105 1 Sampling Procedures and Tables for Inspection by Attributes MIL-STD-883 Test Methods and Procedures for Microelectronics MIL-STD-7883 Brazing MIL-G-45204 Gold Plating, Electrodeposited MIL-M-38510 General Specifications for Microcircuits 1 Nickel Plating QQ-N-290A 2 Dimensioning and Tolerancing ANSI Y14.5 MIL-I-23011 Iron Nickel Alloys for Sealing to Glasses and Ceramics 3 JEDEC Publication No. 95 Registered and Standard Outlines for Semiconductor Devices 3. Selected Definitions blister (bubble) ceramic - Any separation within the ceramic which does not expose underlying ceramic material. blister (bubble) metal - Any localized separation within the metallized or between the metallization and ceramic which does not expose underlying metal or ceramic material. braze - An alloy with a melting point equal to or greater than 450°C. burr - An adherent fragment of excess parent material at the component edge. chip - A region of ceramic missing from the surface or edge of a package which does not go completely through the package. Chip size is given by its length, width and depth from a projection of design plan form (Figure 1). cofired - A process or technology to manufacture product in which the ceramic and refractory metallization are fired simultaneously. Figure 1. Chip Illustration crack - A cleavage or fracture that extends to the surface of a package. It may or may not pass through the entire thickness of the package. contact pad - That metallized pattern that provides mechanical or electrical connection to the external circuitry. delamination - The separation of the individual layers of the ceramic. die attach area - A dimensional outline designated for die attach. discoloration - Any change in the color of the package plating as detected by the unaided eye after the application of heat per G22 9.1.1. flatness - The allowable deviation of a surface from a reference plane. The tolerance zone is defined by two parallel planes within which the surface must lie. footprint - Pin pattern. foreign material - An adherent particle other than parent material. isolation gap – Metal-free space between conductive areas. layer - A dielectric sheet with or without metallization that performs a discrete function as part of the package. peeling (flaking) - Any separation of metallization from the base material exposing the base material. 1 2 3 123 Military Standards, Naval Publications and Form Center, 5801 Tabor Ave., Philadelphia, PA 19120 ANSI, 1430 Broadway, New York, NY 10018 JEDEC, 2001 Fye St. N.W., Washington, DC 20006 G22 pit - Any unspecified depression in the package. projection - An adherent fragment of parent material on the package surface. pullback - The linear distance between the edge of the ceramic and the first measurable metallization (see Figure 2). rundown - The vertical extension of metallization from the ceramic (see Figure 2). seal area - A dimensional outline area designated for either metallization or bare ceramic to provide a surface area for sealing. seating plane - Is defined by the standoff features or the package base plane if no standoff is used (See Figure 3). standoff - The designed separation between the base plane and the seating plane created by a physical feature. Standoff use configuration and placement are optional (See Figure 3). terminal - Case outline at point of entry or exit of an electrical contact. TIR - Total Indicator Reading. voids - An absence of metallization or plating from a designated area. 4. Ordering Information Purchase orders for Pin Grid Array Packages furnished to this specification shall include the following items: 1. Drawing number and revision level 2. Certification requirements 3. Quantity 4. Reference to this document 5. Any exceptions to print or specifications 5. Dimensions and Permissible Variations The dimensions of the pin grid array package shall conform to the SEMI Standards or to the customer drawing and be within the outline of the appropriate JEDEC standard. Refer to MIL-M-38510, Appendix C as appropriate. 6. Material Parameters The definitions, defects and functional testing described in this specification relate directly to a nominal package made with the following materials. They may also be applicable to similar pin grid array packages made with other materials. 6.1 Ceramic Properties 6.1.1 Materials - Alumina content 90% Figure 2. Metallization Misalignment Note – Standoff use, configuration, and placement are optional. Figure 3. Seating Plane minimum. Beryllia content to be determined. 6.1.2 Color - Dark or white. 6.2 Metal Properties 6.2.1 Metallized circuits and areas shall be refractory metal tungsten, molybdenum, or an approved equivalent, .0003" (.00762 mm) minimum thickness. 6.2.2 Finish shall be per MIL-M-38510; Nickel plating (if designated) shall be per QQN-290A, 50µ" -350µ" (.0013 mm - .00889 mm). Gold plating shall conform to MILG-45204, Type III and 50µ" -225µ" (.0013 mm - .00508 mm). 6.2.3 Braze shall be per MIL-STD-7883. 6.2.4 Pin Material - Iron nickel cobalt alloy per MIL-M-38510, Type A (Kovar). Iron nickel alloy per MIL-M-38510, Type B (Alloy 42). Phosphor bronze per ASTM B159. 7. Defect Limits A magnification of 10× shall be used to inspect the packages unless otherwise specified. 7.1 Ceramic 7.1.1 Cracks - Per MIL-STD-883, Method 2009. 7.1.2 Chips - (See Figure 1). 7.1.2.1 Edge - .100" length × .030" (.762 mm) width × .020" (.508 mm) (see Figure 1,A) 124 G22 7.1.2.2 Corner - .030" (.762 mm) length × .030" (.762 mm) width × .030" (.762 mm) (see Figure 1,B). 7.1.2.3 Chips cannot encroach upon contact pad or expose any buried metallization. 7.1.2.4 Seal Area - .060" (1.52 mm) length × .020" (.508 mm) width × .020" (.508 mm) depth maximum. Chips cannot reduce the seal width by more than 1/3 of the design width. 7.2 Package Flatness - .004 inch/inch maximum. 7.2.1 Seal Area Flatness Seal Area Size .000" - .500" (0 - 12.7 mm) .501" - .750" (12.72 - 19.05 mm) .751" & greater (19.07 mm) Seal Area Flatness (TIR) .002" (.051 mm) Maximum .003" (.076 mm) Maximum .004" (.101 mm) Maximum 7.2.2 Die Attach Area Flatness Die Attach Area Size .000" - .500" (0 - 12.7 mm) .501 " - .750"(12.72 - 19.05 mm) Die Attach Area Flatness (TIR) .002" (.051 mm) Maximum .0035" (.088 mm) Maximum 7.3 Metallization Voids (voids greater than .003" should be considered). 7.3.1 Seal Area - Maximum number of 3 voids per seal ring allowed. The maximum void dimension is .010" and voids must be separated by a minimum of .030" (.762 mm). 7.3.2 Wire Bond Finger - Be free of voids or bare spots in the bonding area as defined by customer drawing. 7.3.3 Die Attach Area - Three voids allowed, maximum .010" (.254 mm) diameter voids separated by a distance greater than .010" (.254 mm). Voids within .015" (.381 mm) of die attach cavity wall shall not be considered as the basis for rejection. 7.3.4 Braze Metallization - A .010" (.254 mm) maximum diameter void is acceptable, one void per pad. 7.4 Metallization Misalignment (see Figure 2). 7.4.1 Metallization Rundown - Internal cavity not to exceed .010" maximum. 7.4.2 Wire Bond Finger Pullback - .010" (.254 mm) maximum. 7.4.3 Wire Bond Finger Rundown - Metallization rundown not to exceed 0.10" maximum. 7.4.4 Pattern Isolation - Minimum shall not be reduced by more than 50% of the design. 7.5 Pin Attachment 8. Sampling NOTE: This topic currently under revision in another committee. Sampling size must meet the requirements of MIL-STD-105 or MIL-M-38510, o r as agreed to between vendor and customer. Single, double or multiple samples may be used per vendor and customer agreement. 9. Test Methods 9.1 Mechanical, electrical and thermal test methods per MIL-STD-883 unless otherwise noted. 9.1.1 Gold plating and bake test of gold plated package shall be tested by placing parts on a calibrated heater per MIL-STD-883, Method 1008 (excluding temperature). 9.1.1.1 Condition A - 450°C ± 10°C for two minutes in air or 9.1.1.2 Condition B - 470°C ± 10°C for one minute in nitrogen. 9.1.1.3 After cooling at room temperature the packages will be examined for the following criteria: 1. Blisters - None allowed at 10× magnification. 2. Any non-uniform color change of the gold at die attach pad edges up to .015" (.381 mm) from the cavity walls is acceptable. 3. Any non-uniform color change of the bonding fingers, seal ring surface, or external pins is not acceptable. 4. There shall be no flaking or peeling of the package plating when viewed at 10× magnification. 5. Superficial stains left during drying or prior operations is not cause for rejection. 6. Plating adhesion tape test. 9.1.2 Lead Pull - Under the test condition of five (5) pounds ± one-quarter (¼) pound pull at an angle of 20° or less from the pins vertical line, measured perpendicular to the package, there shall be no visible separation of the braze joint under 10× magnification. This excludes plating. 9.1.3 Lead Fatigue - Test per MIL-STD-883, Method 2004 Test Condition B2, Paragraph 3.2. 9.2 Functional Test Methods 9.2.1 Die Attach Quality - Destructive die shear test post environmental testing per MIL- 125 G22 STD-883, Method 2019, Paragraph 3.2C. 9.2.2 Wire Bond Quality - Minimum pre-seal and post-seal bond strength test per MIL-STD-883, Method 2011, Test Condition D. Reject for bonds which cause plating to lift from the base metal of the bonding fingers or fail to meet minimum strength requirement. 9.2.3 Solderability - Test per MIL-STD-883, Method 2003 (omit aging). 9.2.4 Insulation Resistance - Test per MILSTD-883, Method 1003, Condition D. 9.2.5 Hermetic and Environmental Testing per MIL-STD-883. 9.2.5.1 The hermetic integrity of the package must be maintained after all environmental testing. Hermetic checks shall comply with MIL-STD-883, Method 1014, Test Conditions A, B, C, or D. 9.2.5.2 Environmental testing shall include, but not be limited to, the following: 1. Temperature Cycle, MIL-STD-883, Method 1010, Condition C w/o heat sink; Condition B w/ heat sink. 2. Thermal Shock, MIL-STD-883, Method 1011, Condition C w/o heat sink; Condition B w/ heat sink. 3. Centrifuge, MIL-STD-883, Method 2001, Condition E, Y1 axis only - cavity up; Y2 axis only cavity down- (optional). 4. Mechanical Shock, MIL-STD-883, Method 2002, Condition B. 5. Vibration, MIL-STD-883, Method 2007, Condition A. NOTE 1 – Package applications requiring a heat sink attach will require the environmental test requirements (temp. cycle, shock, etc.) to be evaluated on an individual basis. The material, form factor, and method of attach used for heat sinks may result in severe stresses being induced on the package assembly during environmental testing. Actual accelerated test requirements should be based on the expected product application environment and may be less rigorous than those tests for packages without heat sinks. 10. Sequence of Events and Incoming Testing During incoming inspection the sequence of testing shall be: A. Visual B. Dimensional C. Functional (typical functional tests which may be applied) Die Attach Wire Bond Pre-seal Wire Pull Seal Heat Sink Attach (if applicable) Environmental Test Fine Leak MIL-STD-883, Method 1014, Condition B. Gross Leak -MIL-STD-883, Method 1014, Condition C. Post-Seal Bond Pull Radiography Die Shear, MIL-STD-883, Method 2019 Solderability, MIL-STD-883, Method 2003 NOTE 2 – An initial vendor qualification may be performed on the thermal and electrical characteristics of the package. The characteristics tested will be: Insulation Resistance — MIL-STD-883, Method 1003, Test Condition D. Thermal Dissipation — MIL-STD-883, Method 1012. 11. Packaging and Marking 11.1 Packaging - Container selected shall be strong enough and suitably designed to provide maximum protection against crushing, spillage and other forms of damage to the container or its contents to contamination from exposure to excessive moisture or oxidation by gases. Packaging materials shall be so selected to prevent any contamination of the ceramic components parts with fibers or organic particles. 11.2 Marking - The outer containers shall be clearly marked identifying the customer part no., customer purchase order number, drawing number (optional), quantity, date and vendor lot number (optional). NOTICE: SEMI makes no warranties or representations as to the suitability of the standards set forth herein for any particular application. The determination of the suitability of the standard is solely the responsibility of the user. Users are cautioned to refer to manufacturer's instructions, product labels, product data sheets, and other relevant literature respecting any materials mentioned herein. These standards are subject to change without notice. 126