Chiang Mai J. Sci. 2006; 33(2) Chiang Mai J. Sci. 2006; 33(2) : 293 - 300 www.science.cmu.ac.th/journal-science/josci.

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Analysis of Compaction and Sintering of Stainless Steel Powders

Ornmanee Coovattanachai*, Prayoon Lasutta, Nattaya Tosangthum, Rungtip Krataitong, Monnapas Morakotjinda, Anan Daraphan, Bhanu Vetayanugul and Ruangdaj Tongsri
Powder Metallurgy Research and Development Unit (PM_RDU), National Metal and Materials Technology Center, Thailand Science Park, 114 Paholyothin Rd., Klong 1, Klong Luang, Pathum Thani 12120, Thailand. *Author for correspondence; e-mail: ornmanc@mtec.or.th Received: 20 September 2005 Accepted: 14 February 2006.

ABSTRACT Compaction and sintering are basic processing steps employed for producing powder metallurgy (P/M) parts. Information of materials property change during the processing steps is primarily essential for design and manufacturing engineers. In this study, stainless steel powders (316L, 304L, 409L and 434L) were selected for investigation on the effect of densities on mechanical property. It was found that measurable parameters such as green density, sintered density and mechanical property showed linear relationships with one another for the 304L stainless steel powder. Equations, derived by using Least Square Method (LSM), may be employed with high confident for the 304L stainless steel powder. LSM analyses for other materials (316L, 409L and 434L) failed to get good agreement between the experimental data and the LSM results. Equations, derived by using LSM, are not recommended for the 316L, 409L and 434L stainless steel powders. Keywords : density, Least Square Method, mechanical property, stainless steel powders.

1. INTRODUCTION

Powder metallurgy process offers greater flexibility in part design with superior properties and dimensional accuracy. The P/M process has been becoming more attractive among the various metal forming processes. It offers lower production cost when number of P/M parts, those are higher than economy-scale quantity, are produced. The attraction of P/M is mainly resulted from the ability to produce various parts such as porous, precise (close tolerance), and high performance components in an economical manner [1, 2]. Stainless steel P/M parts represent an important and growing segment of the P/M

industry. The stainless steel powders have been selected to replace P/M ferrous alloys due to their superior characters such as corrosion resistance, oxidation resistance, wear resistance and mechanical properties (ductility and impact strength) [3]. Stainless steel series 300 powders are used in several applications such as aerospace, agriculture, appliances, automotive, building and construction, chemical, electrical and electronic, hardware, industrial, jewelry, marine, medical, office equipment, recreation and leisure [4]. Stainless steel series 400 powders have been being widely used in P/M applications for

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a decade. This is because of their ferromagnetic properties, fairly good corrosion resistance, good strength and low cost. Applications of 400 series alloys can be found as automotive parts. The examples of them include automotive rearview mirror mounts, antilock brake system (ABS) and sensor rings [5, 6]. Several exhaust components, including coupling flanges and hot exhaust gas oxygen sensor (HEGOS) bosses, are excellent candidate applications for P/M parts makers to manufacture [7]. Recently, there has been considerable interest in the potential for 400 series P/M parts for automotive exhaust system components, including flanges [6, 8]. In conventional P/M process, there are many factors controlling P/M parts characters. Density is one of various important factors. Compaction of loose powder particles into green parts results in that green density is dependent on compacting load and powdered materials property. The green density controls sintered density, which in turn controls mechanical properties [9]. In this study, effect of density on mechanical properties was analysed using the Least Square Method (LSM).
2. MATERIALS AND METHODS

Each stainless steel powder grades (304L, 316L, 409L and 434L obtained from Coldstream of Belgium) was compacted into tensile test bars (TTBs) with various green densities. Numbers of green TTBs used for each experimental condition were 20 pieces. The green TTBs were then debinded with batch-type furnace at 600 C for 60 minutes under argon atmosphere. The debinded TTBs those made from series 300 stainless steel powders were sintered at 1300 C for 45 minutes, and the debinded TTBs those made from series 400 stainless steel powders were sintered at 1350C for 45 minutes. Both series were sintered under pure hydrogen atmosphere with a flow rate of 250 litres/hr. Densities of green and sintered samples were determined using the Archimedes method. A universal testing machine (Instron model 8801) was employed to measure mechanical properties of the sintered TTBs. Hardness of the sintered TTBs was carried out using a hardness tester (Rockwell scale B).

RESULTS AND DISCUSSION 3.1 Effect of Green Density on Sintered Density LSM analyses of experimental data of 316L, 304L, 409L and 434L materials resulted in equations for green density ( G )-sintered density ( S ) relationships (Table 1). The 304L and 409L stainless steel powders (Figure 1(b) and (c)) showed linear relationship between experimental values of G and S .The R2 values, computed from experimental data and calculated values according to the equations for 304L and 409L materials, were higher than 0.900 (Table 1). The 316L and 434L stainless steel powders (Figure 1(a) and (d)), showed the G - S relationships with R2 values less than 0.900. Experimental errors occurred with the 316L material. The R 2 value was 0.799. Deviation of experimental values from the LSM ones occurred when green densities were higher than 6.45 g/cm3. It was observed that when green densities were higher than 6.45 g/cm3 the sintered densities dropped. The causes of errors are not understood yet. In general, the green TTBs with higher green density have lower porosity, thus contain higher number of points of contact. When the green parts have higher number of points of contact, the sintering opportunity would be higher. Therefore densification of the TTBs with higher green density occurs faster within a certain time. For the 434L stainless steel, the experimental green-sintered density relationship was not in common. However, the LSM seemed not to be fitted with the experimental trend. This causes the R2 value lowered than 0.900. The equation general form of the G - S relationships for the stainless steel powders investigated was as follows; 2 (1) S = AG + BG + C where A, B and C are materials-dependent constants. The values of A and B are shown in Table 1. The constant C for 316L, 304L and 409L were too small (<0.001) so they were omitted.
3.

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Table 1. Equations for green and sintered density. Sintered Specimens 316L 304L 409L 434L R2 0.799 0.979 0.924 0.896 Equations
2 S = 0.158G + 2.134 G 2 S = 0.132 G + 1.966 G

2 S = 0.125G + 1.928 G 2 S = 0.228 G + 2.581G + 0.004

(a) 316L

(b) 304L

(c) 409L

(d) 434L

Figure 1. Plots of sintered density against green density of compacted stainless steels. 3.2 Effect of Sintered Density on Mechanical Properties 3.2.1 Ultimate Tensile Strength (UTS) The sintered density-UTS relationships of 316L and 304L stainless steels, Figure 2(a) and (b), respectively, showed good agreement between the experimental data and the LSM results. The R2 values for the 316L and 304L materials were 0.954 and 0.998, respectively. For the 409L material, some TTBs with different green densities yielded close sintered density values (Figure 1(c)). However, the sintered TTBs with close sintered density values showed different UTS values (Figure 2(C)). This causes the low R2 value for the sintered density-UTS relationship of the 409L material. The 434L material showed low level of agreement between the experimental trend and the LSM result (Figure 2(d)).

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Table 2. Equations for UTS and sintered density. Sintered Specimens 316L 304L 409L 434L R2 0.954 0.998 0.731 0.790
UTS UTS UTS UTS

Equations = 143.719 2 982.688 S 0.001 = 135.126 2 905.549 S 0.005 = 28.554 2 151.199 S 0.057 = 25.306 2 131.453 S 0.170
S S S S

(a) 316L

(b) 304L

(c) 409L

(d) 434L

Figure 2. Plots of tensile strength against sintered density of sintered stainless steels.

3.2.2 Yield Strength ( Y ) The sintered density ( S ) and yield strength ( Y ) relationships of some sintered specimens (316L, 409L and 434L shown in Figure 3(a), (c) and (d), respectively) showed low level of agreement between the experi-

mental trend and the LSM result. The R2 values for those materials were lower than 0.800. The only material showing high R2 value was P/M 304L stainless steel.

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Table 3. Equations for yield strength and sintered density. Sintered Specimens 316L 304L 409L 434L R2 0.744 0.976 0.509 0.738
Y Y Y Y

Equations = 64.730 2 440.733 S 0.006 = 49.807 2 323.947 S 0.003 = 22.898 2 133.458 S 0.077 = 11.481 2 48.204 S 0.129
S S S S

(a) 316L

b) 304L

(c) 409L

(d) 434L

Figure 3. Plots of yield strength against sintered density of sintered stainless steels. 3.2.3 Elongation For sintered metals, the ductility change with fractional density (), which is the density of the porous material (equivalent to sintered density ( S ) divided by the density of equivalently processed wrought material), was approximated as follows [10]:
= 3/ 2 (1 + c 2 )1 / 2

(2)

where c is an empirical constant that relates to the sensitivity to pores, and y is porosity.

The relative ductility ( ) is the ductility, indicated by elongation ( ) value, of the porous material divided by the ductility of equivalently processed wrought material. According to Equation (2), it was not uncommon that elongation of most sintered stainless steels (316L, 304L and 434L) increased with increasing sintered density (Fig. 4). Increased sintered density indicates increased volume fraction of metallic bonds (sintered necks) and decreased volume fraction of pores, during sintering process.

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Table 4. Equations for elongation and sintered density. Sintered Specimens 316L 304L 409L 434L R2 0.902 0.959 0.033 0.993 Equations
= 18.452 S2 129.613 S 0.001 = 11.669 S2 79.812 S 0.001 = 2.443 S2 + 19.659 S + 0.009 = 4.057 S2 27.504 S 0.001

(a) 316L

(b) 304L

(c) 409L

(d) 434L

Figure 4. Plots of elongation against sintered density of sintered stainless steels.

3.2.4 Hardness Relationships between sintered density and hardness as shown in Fig. 5 were analyzed by using the LSM. Results of fitting equations of hardness versus sintered density are shown

in Table 5. The R2 values indicates that the equations for 316L, 304L and 409L stainless steels are acceptable, particularly the equation for the 304L material.

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Table 5. Equations for hardness and sintered density. Sintered Specimens 316L 304L 409L 434L R2 0.9200 0.9870 0.9575 0.853
H H H H

Equations = 51.068 2 361.776 S 0.001 = 23.896 2 166.453 S 0.001 = 7.685 2 47.689 S 0.002 = 13.508 2 89.581 S 0.044
S S S S

(a) 316L

(b) 304L

(c) 409L

(d) 434L

Figure 5. Relationship between sintered density and hardness.

3.3 Degree of Confidence It can be concluded that all the equations for the 304L stainless steel, shown in Table 6, can be used with high confidence. For other materials (316L, 409L and 434L), equations for relationships between physical properties

(i.e. green and sintered densities) and mechanical properties (strength, hardness and elongation) are not recommended to apply without laboratory test results as references.

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Table 6. The R2 values for stainless steel powders. Relationship Green-sintered density Sintered density-UTS Sintered density-YS Sintered density-E Sintered density-H Note: = R2 value > 0.900
4. CONCLUSIONS

316L 0.799 0.954 0.744 0.902 0.920

Materials 304L 409L 0.979 0.924 0.998 0.731 0.976 0.509 0.959 0.033 0.987 0.958

434L 0.896 0.790 0.738 0.993 0.853

During P/M processes, the 304L stainless steel powder exhibited linear relationships between parameters such as green density, sintered density and mechanical properties. The R2 values computed from the experimental data and the LSM results were higher than 0.900. Equations, derived by using LSM, may be employed with high confident for the 304L stainless steel powder. LSM analyses for other materials (316L, 409L and 434L) failed to get REFERENCES [1] German, R. M., Powder Metallurgy of Iron and Steel, John Wiley & Sons, INC, 1998, 9-13. [2] Schatt, W. and Wieters, K-P., Powder Metallurgy, EPMA, 1997, 147-157. [3] Rosso, M., Porto, G. and Wood, J. V., Properties of High Density Sintered 316L Stainless Steels, Advances in Powder Metallurgy and Particulate Materials, 1996, (17-87)(17-97). [4] Reinshagen, J. H. and Neupaver, A. J., Fundamentals of P/M Stainless Steels, Advances in Powder Metallurgy, 1989, 283295. [5] Reinshagen J. H. and Mason R. P., The Basic of 400 Series P/M Stainless Steels, Advances in Powder Metallurgy and Particulate Materials, 1997, (9-3)-(9-17). [6] Flick G. D., Compaction of Alloy 409 Cb Stainless Steel Employing a Die Wall Lubricant System, Advances in Powder Metallurgy and Particulate Materials, 1998, (9-95)-(9-104).

good agreement between the experimental data and the LSM results. Equations, derived by using LSM, are not recommended for the 316L, 409L and 434L stainless steel powders. ACKNOWLEDGEMENTS The authors express their gratitude to National Metal and Materials Technology Center (MTEC), Pathum Thani, Thailand, for financial support.

[7] Kopech H. M. and Haberberger T. E., Evaluation of P/M Ferritic Stainless Steel Alloys for Automotive Exhaust Applications, Advances in Powder Metallurgy and Particulate Materials, 1997, (9-45)(9-59). [8] Rawlings A. J., Kopech H. M. and Rutz H. G., The Effect of Processing and Service Temperature on the Properties of Ferritic Stainless Steels, Advances in Powder Metallurgy and Particulate Materials, 1997, (9-19)-(9-36). [9] Vetayanugul, B., Coovattanachai, O., Lasutta, P., Mata, S., Sudasna Na Ayudhya, C., Krataitong, R. and Tongsri, R., Effect of Green Density on Mechanical Properties of P/M Stainless Steel 316L Parts, 29th Congress on Science and Technology of Thailand, 2003, 208. [10] German, R. M., Powder Metallurgy & Particulate Materials Processing, Metal Powder Industries Federation, 2005, 386387.