Single Press / Single Sinter Solutions to High Density Francis Hanejko Hoeganaes Corporation Cinnaminson, NJ 08077 USA Abstract: Powder metallurgy main asset is its ability to produce structural components that meet functional requirements in a cost efficient manner. Many PM parts are produced at densities lower than 7.1 g/cm³ because achieving higher densities often require additional processing steps, which result in increased part cost. Although warm powder warm die processing is not new, new methods that employ die heating only have been introduced that enable high green density via single press / single sinter. This simplified processing will potentially lead to greater market acceptance of high density PM parts. However, drawbacks of die heat only are part size restrictions and higher compaction loads. Both processes are useful in the production of high density PM components. This paper will detail the advantages and disadvantages of both processes. Practical part production will be discussed with mechanical properties achievable via high density processing. Introduction: The PM community must continue to advance its parts making potential, mechanical performance of it components, and dimensional precision so as to continue to improve and solidify its competitive position within the various parts making disciplines. Longestablished lower density / lower performance parts potentially will be lost to competitive processes or to emerging countries with lower labor costs. Higher densities in conjunction with more exacting tolerances and higher mechanical properties are key strategies toward improving PM’s competitiveness. Methods to increase density via single press single sinter have followed two paths; one utilizes heated powder and heated dies, so called warm compaction. This process uses tooling and powder temperatures of ~130 °C to ~150 °C. [1] Incorporating both powder and die heating results in reduced compaction pressures to achieve higher densities. Parts produced via this technique including turbine hubs for automotive automatic transmissions, gearing for industrial power tools, engine timing sprockets, etc. [2] Size restrictions on parts were limited to press capacity coupled with an adequate supply of heated powder through the powder heating and delivery system. The disadvantage of this processing was the tight temperature control (+ / - 5 °C) of powder temperature required to achieve steady state production. If this condition was not satisfied then excessive green scrap could result, thus increasing overall part cost. A second strategy for increasing green density utilized die heating without any powder preheating. This process referred to as warm die compaction has advantages of reduced capital cost, no restriction on through put of a powder delivery system, plus simplified press set up and part production. Die temperatures of 50 °C to 100 °C are most common. [3] Successful applications of this processing system include: speed sensors, gears for industrial power tools, recreational vehicle applications, etc. Development of proprietary lubricants and premixing technologies enabled reduced amounts of powder lubricant thus facilitating higher green densities with reduced lubricant burn-off. A key restriction of this process is a size limitation of parts that can be made: components weighing in excess of 0.75 kilogram with wall thickness greater than 20 mm have proven difficult. Components of this size do not achieve uniform powder temperature within the die during compaction, resulting in increased compaction pressure to achieve the specified part density. Effects of Die Compaction Temperature on Final Part Density Figure 1 presents the effects of die temperature on the green density attained at various compaction pressures. The material evaluated in Figure 1 was a 0.3% molybdenum prealloyed steel powder with 0.4% added graphite and 0.4% proprietary warm die compaction lubricant, this binder treated material had a pore free density of ~7.58 g/cm³. Green density increased with increasing die temperature, the amount of increase in density was approximately 0.08 / 0.10 g/cm³ for each 60 °C increase in die temperature. Although the data shown in Figure 1 was generated using a laboratory hydraulic compaction press, comparable results were achieved in production compaction equipment at pressing rates up to 12 parts per minute. One concern with larger parts is the need to de-aerate the powder mass during compaction. Assuming an apparent density of powder of ~3.2 g/cm³ and a final part density of 7.2 g/cm³, the part will have approximately 125% of its final compacted volume of air that needs to escape during compaction. Unless consideration is given to this effect green cracking may occur. Introducing a cycle delay during compaction and / or incorporating top punch hold down after compaction facilitates removal of the entrapped air. Figure 1: Effects of die preheat temperature on part density Coincident with the increase in green density, increasing die temperature also increase the green strength of the part as shown in Figure 2. This increase in green strength results from the greater deformation of the powder particles and viscoplastic flow of the lubricant. An additional benefit to reduced lubricant content is also the reduced green expansion after compaction. The resulting higher green strength and lower green expansion proposes a potential for reduced green part damage and corresponding reduced rejection rates. Figure 2: Effect of compaction pressure on green strength The trend in Figure 1 verified that increasing die temperature (hence part temperature) increased green density at any given compaction pressure. A logical extension of this data is to evaluate the effects of still higher compaction temperatures on green density. The development of advanced lubricants enabled compaction die temperatures up to 175 °C (at this die it recommended that powder preheating be utilized). Shown in Figure 3 is the effect of various die temperatures (and powder preheat as noted) on the green density of an MPIF FLN2-4400 material with 0.35% graphite. Compaction conditions are detailed in Table 1. Differences in final green densities at either 700 or 830 MPa are explained by the differences in pore free density for each of the materials, Table 1. The standard premix material has the lowest overall compressibility. Increasing both the powder temperature and die temperature improves the green density at any compaction pressure. Implications of the data shown in Figure 3 are as follows: Higher densities can be achieved at lower compaction tonnage with increasing die temperature and / or powder temperature. Increasing powder or die temperature will lower the required compaction pressure to achieve a specified density. Larger parts benefit from powder preheating because of reduced temperature gradients within the part. The cross over of the warm die material vs. the warm compaction 1 material at ~7.3 g/cm³ green density is a result of differing lubricant amounts within the two materials. The data shown in Figure 3 indicates that a green density of 7.45 g/cm³ may represent the practical upper limit for an engineered PM premix utilizing internal lubricant. Development of new lubricants that can operate at reduced levels and / or advances in die wall lubrication are required for further increases in green density. Figure 3: Effect of compaction conditions on green density of an MPIF FLN2-4405 Table 1 Compaction Conditions for Data Shown in Figure 3 Material Std Premix AncorMax 200™ ANCORDENSE™ ANCORDENSE 450™ Lubricant type Acrawax Proprietary warm die Proprietary warm powder Proprietary warm powder Lubricant Amount, % 0.75 0.40 Die Temp. °C 25 93 Powder Temp. °C NA NA Pore Free Density, g/cm³ 7.41 7.58 0.60 140 130 7.48 0.40 175 160 7.58 Mechanical properties of a PM material (FLN2-4405) compacted and sintered to high density were compared to wrought AISI 8620 steel (0.8% Mn, 0.25% Si, 0.55% Ni, 0.5% Cr, 0.2% Mo, 0.2% C). Table 2 presents the mechanical property comparison. Both materials were austenitized at 925 °C (1700 °F) for 1 hour in a 75 % hydrogen / 25% nitrogen atmosphere, oil quenched in 70 °C oil, and subsequently tempered at 205 °C. As expected, the wrought steel has higher tensile elongation and impact energy compared with the PM steel. However, the wrought steel shows a marked directionally of properties from the longitudinal direction (direction of primary working) to the direction perpendicular to the primary working direction (transverse). For the wrought steel, the notched impact energy is reduced from 37 Joules to about 14 joules. Additionally, the 50% fatigue endurance limit (as measured by rotating bending fatigue) is reduced from 490 MPa to 370 MPa. The PM steel has comparable yield and tensile strengths to wrought steel. Comparing the fatigue response, the PM material has equivalent fatigue properties to the properties in the transverse direction of the wrought steel. PM has little if any directionality of mechanical properties. Rolling contact fatigue of PM components can be enhanced via surface densification to levels equal to wrought steel. Thus achieving a minimum density of 7.4 g/cm³ is key to obtaining this parity in both tensile strength and fatigue properties. [3,4] Table 2 Mechanical Properties of PM vs. AISI 8620 Steel Property Yield St. MPa (103 psi) Yield St. MPa (103 psi) Tensile Elongation, % Hardness, HRA Notched Impact Energy, Joules (ft.lbf) Un-notched Impact Energy, Joules (ft.lbf) 50% Fatigue Endurance Limit, MPa (103 psi) AISI 8620 Steel Longitudinal Transverse 1075 (156) 1070 (155) 1355 (197) 1330 (193) 8.0 6.1 71 70 PM at 7.4 g/cm³ 1240 (180) 1445 (210) 1.0 81 37 (27) 14 (10) NA 312 (230) 308(227) 18 (13) 490 (71) 370 (54) 405 (59) Effects of Binder Treatment on Dimensional Stability of Gears A study was conducted comparing an MPIF FC-0208 with a prealloyed 0.3% molybdenum steel with 0.8% added graphite. Two types of premixes were prepared for both materials, one was a standard premix with 0.75% acrawax and the second was a warm die compaction grade with 0.4% lubricant. Compressibility information of the four materials is present in Figure 4. As was shown earlier in Figure 1, increasing the die temperature from ambient conditions to 93 °C resulted in a ~0.08 to 0.10 g/cm³ increase in green density. Prototype gears were produced using the four materials shown in Figure 4. The gears were compacted on a Dorst 140 metric ton mechanical press at a rate of 10 parts per minute. The gears were sintered in a continuous belt sintering furnace at 1120 °C (2050 °F) in a 90% nitrogen / 10% hydrogen atmosphere with a time at temperature of ~20 minutes. After sintering approximately 50 gears from each material grouping were heattreated by quenching and tempering utilizing a commercial heat-treat cycle for FC0208. After quenching, the gears were then tempered at 205 ° C (400 °F). The gears were checked for dimensional variation using 3.162 mm (0.1245-inch) diameter pins. Measurements were taken at four locations around the gear starting with the front of the gear (as compacted) and then measuring three additional locations around the outside diameter. The results of the measurement over wires (MOW) are presented in Table 3. Figure 4: Compressibility information of MPIF FC-0208 and a prealloyed 0.30% molybdenum steel with 0.8% graphite. Table 3 Dimensional Variations of Heat Treated Gears Material FC-0208 (regular premix) 0.3% Mo with 0.8% gr (regular premix) FC-0208 (bonded premix 0.3% Mo with 0.8% gr (bonded premix) Av. MOW Inches (mm) 1.2096 (30.72) Max – Min Inches (mm) 0.0043 (0.11) St Dev MOW Inches (mm) 0.0013 (0.03) 1.2090 (30.71) 0.0015 (0.04) 0.0003 (0.01) 1.2099 (30.73) 0.0036 (0.09) 0.0008 (0.02) 1.2084 (30.69) 0.0014 (0.04) 0.0003 (0.01) This data demonstrates the reduced scatter realized with the prealloyed 0.3% molybdenum steel relative to a standard FC-0208 material. However, the data also shows that a bonded premix reduced the scatter in MOW for the FC-0208 material by ~30%. Thus, the binder treatment results in reduced part-to-part scatter even for the inherently variable copper-containing steel. No measurable difference in dimensional variation was observed for the binder treated 0.3% molybdenum steel. Conclusions: 1. The use of proprietary lubricants enabled warm die compaction with die temperatures up to 110°C. In addition to increased green density, the green strength also increases with increasing part / die temperature. 2. Warm die compaction is not suitable for all parts, parts possessing weights in excess of 0.75 kilograms or having wall thickness greater than 20 mm thwart uniform powder temperatures in the die increasing the compaction pressure or lowering the green density. 3. For larger parts, heating of both powder and die are recommended. Recent lubricant developments enable die temperatures up to 175 °C. This gives higher green density and more uniform part densities. 4. Using a “binder treated” powder showed ~ a 30% reduced variability in measurement over wires for heat treated FC-0208. Although not seen with the 0.30% molybdenum prealloyed steel, similar trends are expected for other materials. 5. Mechanical properties of high density PM materials have equivalent yield and tensile strengths to wrought steels. However, the PM steel has reduced impact and tensile ductility. The PM steel has equivalent fatigue to the wrought steel in the transverse direction. References: 1. H. G. Rutz, F. G. Hanejko, “High Density Processing of High Performance Ferrous Materials”, Advances in Powder Metallurgy and Particulate Materials – 1994, Vol. 5, Metal Powders Industries Federation, 1994, pp 117-133. 2. T. Miller, F. Hanejko, “Development of a Warm Compacted Automatic Transmission Torque Converter Hub”, Paper 970428, Society of Automotive Engineers. 3. G. Poszmik, S. Luk, “Binder Treated Products for Higher Density and Better Precision”, Advances in Powder Metallurgy and Particulate Materials – 2003, Metal Powder Industries Federation, 1993, p. 3-33 to 3-44. 4. MPIF, Std 35 2007 edition, Metal Powder Industries Federation, p. 63. 5. G. Hoffmann, C. Landgraf, J. Mandel, “Effect of Pore and Porosity on Rolling Contact Fatigue of Sinter Hardened P/M Steel”, Advances in Powder Metallurgy and Particulate Materials-2003, Part 7, pp. 7-229 – 7-313, Metal Powders Industry Federation, Princeton, NJ, 2003.