Methods for Deposit Stress Determination Frank H. Leaman Specialty Testing & Development, Inc. York, PA Bent Strip (simple beam theory) Spiral Contractometer Simple Beam Theory Where: Then: N = Thickness of the plated coating (inches) T = Thickness of the test strip (inches) D = Deflection of the strip due to bending (inches) L = Length of the test section (inches) E = Modulus of elasticity of the test strip (lb/in2) I = Moment of inertia of the cross section of test strip about its neutral axis S = Stress in plated layer (lb/in2) S = 4E (N+T) D 3NTL Bent Strip Method (Initial Approach) During the application of a coating, one end of the test piece is held in a fixed position and the other end is free to move. It is difficult to measure the value for D. Bent Strip Method (Different Approach) A test piece split into two legs spreads outward due to the deposit stress The deflection is easily read by placing the test piece over a scale Calculate the deposit stress value by using a simple formula Simple Beam Tensile and Compressive Stress Tensile Compressive Compressive and Tensile Stress Stress Evaluation Using the Bent Strip Method Test Strip in a Plating Cell In-Site 1 Plating Cell Ideal for small solution volumes and lab studies, particularly when working with precious metals Bent Strip Test Piece Measuring Stand Stress Evaluation Using the Bent Strip Method Bent Strip Plating Test Cell Test Strip Plating Cell with Accessories Typical Deposit Stress Evaluation Plating Set-Up Nickel Deposit Stress Calculations For Test Strips Using The Modified Stoney Formulua Stoney Formula Modified for M: = E T² M δ 3 L² t E = Modulus of elasticity of the substrate = 120,690 MPa. T = Thickness of the substrate in millimeters = 0.05077 mm. δ = 1/2 the distance between the test strip leg tips in mm. Example: 0.540 inch spread ÷ 2 x 25.385 mm/inch = 6.85 mm. = Stress in megapascals, MPa. Note: MPa x 145 = PSI. L = Length of substrate on which the deposit is applied in mm. For Deposit Stress Analyzer test strips, this value is 76.2 mm. t = Deposit average thickness in millimeters. M = Correction for modulus of elasticity difference between the deposit and substrate: M = EDeposit ÷ ESubstrate = 206,900 MPa÷ 120,690 MPa = 1.714 = E (.05077 mm) ² M ( δ mm) = 3652 mm³ = 82.6 MPa 3(76.2 mm)²(.002538 mm) 44.21 mm³ Deposit Stress in PSI = MPa x 145 = 11,977PSI Spiral Contractometer Older Design • The test piece is a helix. One end of the helix is held, other end is free to move. As the free end moves, a dial registers the movement in degrees. The stress of the coating can be calculated. Helix on Older Spiral Contractometer With Center Rod Exposed Helix Plated on Older Type Contractometer for Target Nickel Deposit Thickness of 500µ” in a Semi-bright Bath Deposit Location Thickness, µ” Outside Surface Inside Surface 410 85 New Helix Properties New design helices are constructed from 0.010 inch thick stainless steel and have a precise surface area of 13.57 in2. Helices mount on the contractometer in a way that the entire helix plates from end to end and deposition of metal on the inside of the helix is minimal even if it is void of a masking material. The average test deposit thickness is 500 microinches. Nickel Plating Conditions for Spiral Contractometer Tests Helix Material Stainless Steel Helix Surface Area, in2 13.57 Square Feet 0.0942 Amps per square foot 30 Amps 2.90 Stock Thickness, inches 0.010 Avg. Deposit Thickness µ” 500 Plating Time 20M 40S Solution Temperature 140° ± 1° F Spiral Contractometer New Design The test piece is a helix. One end of the helix is free to move and the other end is not. As the free end moves, a measurement dial in degrees rotates. From the final degree value, the internal deposit stress can be calculated. The new design provides masking of the interior surface by geometry and enables helices to be plated tip to tip so the plated surface area is a constant value. The new geometry solves problems related to an exposed interior that allows deposition of the applied deposit to occur on the inside surface. Interior deposits reverse the type of stress and reduce calculated results as much as 30%, so interior masking is critical. Other advantages: Stainless steel inserts and 25% glass filled nylon construction prevent thread damage and helix slippage. Less labor, and more accurate results. Spiral Contractometer Equipment to Determine Internal Nickel Deposit Stress Spiral Contractometer with calibration weights, support stand and helix test pieces. Titanium Mesh Anode Basket 3.5” outside and 2.25” inside diameter, 8” high with support contact tabs and cover for Wood’s nickel strike if a strike is required for adhesion of the applied deposit. Titanium Mesh Anode Basket 5” outside and 4” inside diameter with support contact tabs. Nickel anode buttons to fill the anode baskets. Pyrex beaker 4,000 ml to contain the nickel plating bath. Support stand – designed to perfectly center the helix over the beaker. Magnetic stirrer hot plate, 115 volt output. Digital temperature Controller pre-wired with probe to control ± 10 F. Power Supply constant current, constant voltage, 0-5 amps, 0-30 volts. Magnetic stirrer hot plate, 115 volts. Contractometer Stand, Anode Basket & Beaker Contractometer Plating Set-Up Data Recording for Spiral Contractometer Tests Deposit weight in grams: Kc degrees: Kt degrees: Degrees deflection caused by the deposit: Helix weight in grams: Deposit weight in grams by subraction: Deposit thickness in microinches: Average Deposit Thickness Calculation in Inches T= W = Inch D (87.55 cm2) (2.54 cm/inch) W = Grams of nickel D = Density of nickel = 8.90 g/cm3, and T = Deposit thickness in inches For the new helices plated on the new design contractometers, the constant helix plated surface area is 13.57 in2 and the following shortened formula applies: T= W = Inches 1979.2 Calculating Spiral Contractometer Nickel Deposit Stress On Helices Stress = 13.02 (D) x 1 + 30,000 ,050 (d) = PSI w (d) 28,600,000 (t) D = Degrees caused by the deposit, M = Modulus of Elasticity of the deposit ÷ that of the substrate =30,000,050 ÷ 28,600,000 = 1.049 for nickel deposits over helices that are 0.010 inch thick, w = degrees Kt from helix calibration if the stress is tensile or degrees Kc if the stress is compressive, d = Deposit thickness in inches = 0.000536 in, and t = Helix thickness in inches = 0.010 in. Calculation : S = 13.02 (26) x 1 + 30,000,050 (d) = 20,209 PSI 33 (0.000536) 28,600,000 (0.010 in) Modulus of Elasticity Values Stock Material ES* Stock Thickness, in Metal ED** Cadmium 31,720 Chromium 248,280 Cobalt 206,897 Copper 117,240 Gold 74,480 Nickel 206,900 Platinum 146,900 Rhodium 289,650 Tin 59,310 Silver 75,860 Zinc 82,760 Cu-Fe Alloy 120,690 0.0020 0.263 2.06 1.72 0.971 0.617 1.71 1.22 2.40 0.49 0.629 0.686 Ni –Fe Alloy 144,830 0.0015 Values for M*** 0.219 1.71 1.43 0.810 0.514 1.42 1.02 2.00 0.41 0.524 0.571 Ni-Fe Alloy 179,310 0.0010 0.177 1.39 1.15 0.654 0.415 1.14 0.819 1.62 0.33 0.423 0.462 Pure Ni 206,900 0.0010 0.153 1.20 1.00 0.567 0.360 1.00 0.710 1.400 0.29 0.367 0.400 ES*, modulus of elasticity of substrate material in the Stoney Formula. ED**, Modulus of elasticity of deposit for use in modified Deposit Stress Analyzer and Stoney formulas. M***, modulus of elasticity of deposit ÷ modulus of elasticity of substrate for deposit stress determinations using the modified Deposit Stress Analyzer and Stoney Formulas. A Frequent Mistake in Test Procedure Spiral 1 Deposit Thickness To Stock Ratio Stock Thickness, Inches Deposit Thickness, µ Inches Minutes Plated Current Density, ASF Deposit Stress, PSI 1:20 0.010 500 20 30 14,060 Test Strips 2 1:20 0.002 500 4 30 14,127 3 1:5 0.002 100 20 30 6,865 Note: Extra thick deposits of the harder metals increases the degree of stiffness which results in lower proportional test strip spread. Formulas for Bent Strip with One End Stationary Bent Strip Stress Curve For the comparison of equations that follow that apply to calculating the internal deposit stress of applied metallic coatings over various substrate materials, the value of U = 8.5 units = 0.780 inch will consistently be used as a basis. It will be noted that the calculated internal deposit stress values vary from equation to equation, particularly where the equation fails to address Modulus of Elasticity differences between the substrate and the applied metallic deposit. FOR A GIVEN TEST STRIP U = 8.5 units = 0.780 inch. δ = U in inches x 25.385 mm/inch ÷ 2 = 9.90 mm. Z = δ ÷ 4 = 9.90 mm ÷ 4 = 2.475 mm. R = L² + 4 Z² = 5831 = 294.5 mm 8Z 19.8 Stoney Formula Without and With Modulus of Elasticity Correction for Modulus of Elasticity Differences Example: Nickel deposit on copper test strip, U = 8.5 units = 0.780 inch and δ = U in inches x 25.385 mm/ in ÷ 2 = 9.900 mm. WITHOUT CORRECTION σ = 4ET²Z = ET² δ = 91.137 MPa = 13,214.9 PSI 3L²t 3L²t L = test strip plating length = 76.2mm, T = Stock thickness = 0.05077mm and t = Deposit thickness = 0.000075µʺ = 0.001904mm WITH CORRECTION M = EDeposit ÷ESubstrate = 206900 ÷120690 = 1.714 σ = ET²δM = 120690(0.05077)²(9.900 mm)(1.714) = 159.16 MPa 3 L² t 3(76.2mm)²(0.001904 mm) σ = MPa (145 PSI/MPa) σ = 23,077 PSI Other Bent Strip Formulas to Determine Internal Deposit Stress in Applied Metallic Coatings Barklie and Davies Formula σ= ET² 6Rt (1 – t/T) Heussner, Balden and Morse Formula σ = 4ET²Z 3t (T + t) L Brenner and Senderoff Formula σ = ET(T+ ᵦt) 6Rt ᵦ= EDeposit ÷ ESubstrate BRENNER AND SENDEROF FORMULA CORRECTED FOR MODULUS 0F ELASTICITY DIFFERENCES σ = E T(T+ ᵦ t) ᵦ = EDeposit ÷ ESubstrate = 1.714 6Rt σ = 95.538 MPa x 145PSI/MPa = 13,853 PSI This formula becomes erroneous as differences in modulus of elasticity values increase. To be correct, this Brenner and Senderoff formula requires modification as follows: Corrected Formula: σ = E T² ᵦ ( 1+ ᵦt ) 6Rt ᵦ = 1.714 t = 0.001904 mm σ = (120690 MPa)(0.05077²mm)(ᵦ)( 1+ ᵦ x 0.001904) 6(294.5 mm) (0.001904mm) σ = 159.0 MPa (145 PSI/MPa) = 23,055 PSI. Note: Corrected Stoney formula result = 23,077 PSI