Materials and Design 33 (2012) 153–157

Contents lists available at ScienceDirect

Materials and Design

journal homepage: www.elsevier.com/locate/matdes

Technical Report

Effects of forming parameters and sintering schedules to the

mechanical properties and microstructures of final components
M.M. Rahman a,⇑, S.S.M. Nor a, H.Y. Rahman a, I. Sopyan b
a
Dept. of Mechanical Engineering, Universiti Tenaga Nasional, Putrajaya Campus, Jalan IKRAM-UNITEN, 43000 Kajang, Selangor, Malaysia
b
Department of Manufacturing and Materials Engineering, Kulliyyah of Engineering, International Islamic University, Malaysia

a r t i c l e i n f o a b s t r a c t

Article history: This paper presents the effects of forming parameters and sintering schedules to the mechanical proper-
Received 24 May 2011 ties and microstructures of products formed through warm compaction route. A lab scale warm compac-
Accepted 7 July 2011 tion rig is designed and fabricated which enabled the generation of green compacts at different forming
Available online 18 July 2011
parameters. The feedstock was prepared by mechanically mixing the main powder constituent, i.e., iron
ASC 100.29 powder with zinc stearate to reduce the die–wall as well as inter-particle frictions hence
inhomogeneous density distribution could be avoided. The powder mass is formed at different temper-
ature, i.e., 120 °C and 180 °C applying 130 kN axial loading simultaneously from top and bottom punches.
The defect free green compacts were sintered in inert gas fired sintering furnace for different sintering
schedules. The final products were characterized through density measurement, hardness test, and three
point bending test whereas the microstructures were analyzed by Scanning Electron Microscopy (SEM).
The results revealed that the properties of sintered parts formed at 180 °C are better than those formed at
120 °C. The suitable forming parameters and sintering schedules were identified from this study.
Ó 2011 Elsevier Ltd. All rights reserved.

1. Introduction
A major advance in powder compaction technology is the form-
ing of powder mass at above ambient temperature, which can uti-
lize traditional powder forming equipment. The powder mass
together with the die assembly is required to be heated up to a
temperature below the re-crystallization temperature of the main
powder constituent [1–5]. The process can produce components
having good surface finish and dimensional tolerance hence mini-
mal further processing is required, therefore less time is taken to
produce an engineering component [6].
Density gradients are often evident in green compacts mainly
due to the complex powder deformation mechanisms occur during
the compaction phase. These gradients are the main causes of part
distortion during the subsequent process of sintering and may
even lead to part fracture during its ejection from the die cavity.
In order to achieve the required strength in the products, the green
compacts formed through warm compaction route are required a
firing treatment known as sintering, which refers to the heat treat-
ment of a powder metallurgy green compact for the purpose of
increasing its strength by bonding together of the particles. Sinter-
ing is normally conducted at a temperature where atomic motion
leads to growth of weld bonds among contacting particles [7]. With
higher temperature or longer holds at the peak temperature, which
⇑ Corresponding author. Tel.: +60 3 89297269; fax: +60 3 89212116.
E-mail address: mujibur@uniten.edu.my (M.M. Rahman).
is about 60% of the melting temperature of the main powder con-
stituent, more cumulative atomic motion occurs, leading to im-
proved inter-particle bonding. However, high temperature, longer
holding time, and small particle size are not always economically
viable for conducting sintering operation. Therefore, control over
heating rate, time, temperature and atmosphere is required for
producible results. In general, the parts tend to densify and im-
prove the mechanical properties as sintering proceeds. Increase
the density implies an overall shrinkage which leads to complica-
tions. The dimensional change is influenced by the green density;
the lower this is the greater the tendency to shrink [8].
Manufacturing of engineering components through warm form-
ing route involves several key parameters during feedstock prepa-
ration, powder forming, and sintering. Powder forming at above
ambient temperature is initiated recently and extensive research
papers were published [9–17], however less information on the ef-
fects of warm forming and sintering schedule to the mechanical
properties and microstructures are found. Therefore, this paper
presents the outcome of an extensive research on the effects of
forming and sintering parameters to the final performance of the
products formed through warm compaction route.
2. Experimental procedure
A lab scale warm compaction rig was designed and fabricated
(Fig. 1) which enabled the generation of green compacts at differ-
ent forming parameters. Iron ASC 100.29 powder was used during

0261-3069/$ - see front matter Ó 2011 Elsevier Ltd. All rights reserved.
doi:10.1016/j.matdes.2011.07.019
154 M.M. Rahman et al. / Materials and Design 33 (2012) 153–157

0.88
120ºC

0.878 180ºC

0.876

Relative Density ( ρr)

0.874

0.872

0.87

0.868

0.866

0.864
0.4 0.8
Lubricant Content (wt%)

Fig. 3. Relative densities of sintered parts.

Fig. 1. Warm compaction rig.

the samples were sintered at 900 °C and 1000 °C. The relative den-
the experiment because this type of powder is normally used in sities of the sintered products were measured through dimensional
most of the powder compaction industries [18–20]. The as received measurement and the hardness of the compacts was tested
powder has the particle size range of 20–180 lm. The experiment through Rockwell hardness tester. The strengths of the products
is divided into three sections which are compaction of solid cylin- were measured through three-point bending test (ASTM E290-
drical shape green compacts (Fig. 2), sintering of green compacts in 09) and the microstructures were evaluated through Scanning
argon gas fired sintering furnace, and characterization of final Electron Microscopy (SEM).
products through mechanical testing and microstructure
evaluation.
3. Results and discussions
In order to examine the efficacy of lubricant content, the feed-
stock was prepared by mechanically mixing iron ASC 100.29 pow-
Figs. 3–6 depict the relative density, hardness, bending
der with different weight percent of zinc stearate for 30 min, which
strength, and dimensional changes of the sintered parts formed
is seemed to be adequate [7]. Green sample generation consists of
at different compaction temperature and lubricant content. It is
four consecutive steps which are, die filling with premixed powder
clearly observed that higher relative density can be obtained by
mass, heating of powder mass together with the die assembly,
forming the powder mass at lower temperature both by adding
simultaneous compaction, and ejection of green compacts from
either 0.4 wt% or 0.8 wt% of zinc stearate (Fig. 3). However, addi-
the die cavity by means of bottom punch. The defect-free green
compacts were then sintered in controlled environment, i.e., at a
heating/cooling rate of 10 °C/min, a holding time of 30 min. All 107

120ºC

180ºC
106
Rockwell Hardness (HRF)

105

104

103
0.4 0.8
Lubricant Content (wt%)

Fig. 2. Cylindrical shape green compacts. Fig. 4. Hardness of sintered parts.

 M.M. Rahman et al. / Materials and Design 33 (2012) 153–157 155

700 0.88
120ºC 30ºC
150ºC
600 180ºC
180ºC
0.86 180ºC 0.4wt%

500

Relative Density ( ρr )
Strength (MPa)

0.84
400

300
0.82

200

0.80
100

0 0.78
0.4 0.8 900 1000
Lubricant Content (wt%) Sintering Temperature (ºC)

Fig. 5. Strength of sintered parts. Fig. 7. Relative densities of sintered parts at different sintering temperature.

1.40 110
30ºC
120ºC 150ºC
180ºC
1.20 180ºC 180ºC 0.4wt%
108
Rockwell Hardness (HRF)
Dimensional Changes (%)

1.00

106
0.80

0.60 104

0.40
102

0.20

100
900 1000
0.00
0.4 0.8 Sintering Temperature (ºC)
Lubricant Content (wt%)
Fig. 8. Hardness of sintered parts at different sintering temperature.
Fig. 6. Dimensional change of sintered parts.

believed that at 180 °C compaction temperature, significant cold

tion of 0.8 wt% of zinc stearate could result higher final density
even though the powder mass is formed at the same temperature.
As the melting temperature of zinc stearate is 130 °C, the effective
working temperature of lubricant is around 120 °C instead of
180 °C. Therefore, 120 °C forming temperature has given higher
relative density during compaction process and as the samples
are sintered at the same schedules, higher relative density of final
product is achieved at a higher density sample. Furthermore, due
to the addition of higher weight percent of lubricant, i.e., 0.8 wt%,
some zinc stearate is trapped inside the powder mass, which re-
duces the inter particle friction and eases the motion of powder
particles, as a consequence, the volume becomes smaller hence
density becomes higher [21] compared to the addition 0.4 wt%
lubricant.
It can be observed in Fig. 4 that lower lubricant content inside
the powder mass could result harder products in the case of com-
paction at lower temperature. In terms of strength, it is observed
that superior bending strength could be achieved by adding only
0.4 wt% of lubricant and forming the powder mass at 180 °C. It is
working phenomenon [22] has occurred resulted in strength incre-
ment. Dimensional changes of the final products are also almost
same for both lubricant content and forming temperature. It is
shown that amount of lubricant used is acceptable and also larger
amount of lubricant is believed to have been forced out from the
component accumulated at the side wall during the compaction
process.
Relative density, hardness, and strength of final parts sintered at
different temperature are shown in Figs. 7–9 whereas the micro-
graphs of sintered parts formed from iron powder without lubri-
cant, 0.4 wt% admixed lubricant formed at 180 °C, and 0.8 wt%
admixed lubricant formed at 120 °C are shown in Figs. 10–12. It
is clearly observed that final densities and strengths are higher
for the products formed at 180 °C by adding 0.4 wt% of lubricant,
however hardness is slightly lower. Adding optimum amount of
zinc stearate which is 0.4 wt% has promoted the increase in density
during compaction stage. Furthermore, as larger amount of zinc
stearate has been forced out from the green samples during com-
paction, it generated larger total contact area among the iron par-
156 M.M. Rahman et al. / Materials and Design 33 (2012) 153–157

700
30ºC
600 150ºC
180ºC
180ºC 0.4wt%
500
Strength (MPa)

400

300

200

100

0 Fig. 11. Micrograph of sintered product; 0.4 wt% lubricant, formed at 180 °C.
900 1000
Sintering Temperature (ºC)

Fig. 9. Strength of sintered parts at different sintering temperature.

Fig. 12. Micrograph of sintered product; 0.8 wt% lubricant, formed at 120 °C.

increase the strength of samples with less lubricant content. There-

fore, in order to get higher final density and strength, iron powder
Fig. 10. Micrograph of sintered product; without lubricant, formed at 180 °C. is required to be mixed with an optimum amount of lubricant, say
0.4%, formed at around 180 °C, and sintered at around 1000 °C.

ticles. Hence, as the density increased during sintering, strength is 4. Conclusions

also improved excellently albeit of having lubricant inside the
powder mass at early compaction stage. Higher density and
strength are also obtained by sintering the green compacts at high-
er temperature, i.e., 1000 °C. Structure re-crystallization occurred
steadily and fusion rate among particles increased during sintering
at higher temperature thus improved bonding among iron particles
during the sintering process.
The green compacts formed at 180 °C by adding 0.4 wt% of lu-
bricant and subsequently sintered at 1000 °C for 30 min also show
more uniform grain distribution (Fig. 11). Non-uniform grain dis-
tribution and localized voids are observed for the compacts formed
without lubricant as well as higher content of admixed lubricant
(Figs. 10 and 12).
Iron powder mixed with 0.8 wt% zinc stearate and formed at
180 °C is proven to result green compacts with higher relative den-
sity and strength [23], however the excessive lubricant might be
trapped inside the product when sintered, results the poor densifi-
cation hence the final density and strength become lower [24].
During sintering at higher temperature, more pores are resulted
because zinc stearate becomes spheroid that weakens the iron par-
ticles fusion. Less pores trapped inside the sample also believed to
The results revealed that higher density and harder green com-
pacts could be produced by adding 0.8 wt% zinc stearate and form-
ing the powder mass at 120 °C. However, the sintered results
showed that the suitable lubricant content is around 0.4 wt%, and
the forming temperature is around 180 °C. The green compacts
are suitable to be sintered in inert gas fired sintering furnace at a
heating/cooling rate of 10 °C/min, sintering time and temperature
of 30 min and 1000 °C, respectively. The end products are defect-
free yet high strength, near-net shape components.
Acknowledgement
This research is financially supported by Universiti Tenaga
Nasional through the research Project J510050356.
References
[1] Rahman MM, Nor SSM. An experimental investigation of metal powder
compaction at elevated temperature. Mech Mater 2009;41:553–60.
[2] Yamaguchi K, Takamura N, Imatani S. Compaction and sintering characteristics
of composite metal powders. J Mater Process Technol 1997;63:364–9.
 M.M. Rahman et al. / Materials and Design 33 (2012) 153–157
[3] Takeuchi K. The p/m materials from the viewpoint of environment. In:
Proceedings of 2000 PM world congress 1; 2000. p. 204–8.
[4] Ariffin AK, Rahman MM. The study of warm metal powder compaction. J Ins
Mater Malay 2003;1:161–74.
[5] Engston U, Johanson E. Experience with warm compaction of Densmix™
powder in the production of complex parts. Sweden: Höganäs AB; 2003.
[6] Nor SSM, Rahman MM, Tarlochan F, Shahida B, Ariffin AK. The effect of
lubrication in reducing net friction in warm powder compaction process. J
Mater Process Technol 2008;Vol. 207:118–24.
[7] Rahman MM, Nor SSM. An experimental investigation of metal powder
compaction at elevated temperature. Mech Mater 2009;41:553–60.
[8] Kalpakjian S. Manufacturing processes for engineering materials. California:
Addison Wesley Longman, Inc.; 1997.
[9] Simchi A. Effects of lubrication procedure on the consolidation sintering and
microstructural features of powder compacts. Mater Des 2003;24:585–94.
[10] Rahman MM, Tarlochan F, Ramesh S, Ariffin AK, Nor SSM. Numerical
simulation and experimentation of warm metal powder compaction process.
Key Eng Mater 2010;462–463:704–9.
[11] Kanno Y, Martins JAC, Costa AP. Three-dimensional quasi-static frictional
contact by using second-order cone linear complementarity problem. Int J
Numer Methods Eng 2006;65:62–83.
[12] Wang JZ, Qu XH, Yin HQ, Yi MJ, Yuan XJ. High velocity compaction of ferrous
powder. Powder Technol 2009;192:131–6.
[13] Rahman MM, Nor SSM. An experimental investigation of T-shape component
forming through warm powder compaction route. In: Malaysian symposium
on advances in powder metallurgy and particulate materials 2007 (APM2.07),
Universiti Teknologi MARA (UiTM) Shah Alam; 21–22 August.
[14] Rahman MM, Nor SSM. An experimental investigation of the metal powder
compaction at various lubricant contents and forming loads. In: The 2nd
international conference on engineering and ICT (ICEI2010) Holiday Inn
Melaka; 18th–20th February 2010.
157
[15] Babakhani A, Haerian A, Ghambari M. On the combined effect of lubrication
and compaction temperature on properties of iron-based p/m parts. Mater Sci
Eng A 2006;437:360–5.
[16] Michrafy A, Kadiri MS, Dodds JA. Wall friction and its effects on the density
distribution in the compaction of pharmaceutical excipients A8. Part Technol
2003;81:946–52.
[17] Kondoh M. High density powder compaction using die wall lubrication. Adv
Powder Metall Part Mater 2002;3:47–54.
[18] Turenne S, Godere C, Thomas Y, Mongeon PE. Evaluation of friction condition
in powder compaction in admixed and die wall lubrication. Int J Powder Metall
1999;42:263–8.
[19] Pavier E, Doremus P. Triaxial characterisation of iron powder behaviour.
Powder Metall 1999;42:345–52.
[20] Coube O, Cocks ACF, Wu CY. Experimental and numerical study of die filling,
powder transfer and die compaction. Powder Metall 2005;48:68–76.
[21] Rahman MM, Nor SSM, Rahman HY, Investigation on the effect of lubrication
to the mechanical properties of green compacts formed through warm
compaction route. In: World engineering congress 2010, Kuching, Sarawak,
Malaysia, 2–5th August 2010.
[22] Shackelford JF. Introduction to materials science for engineers. 5th ed. New
Jercy: Prentice-Hall, Inc.; 2000.
[23] Rahman MM, Tarlochan F, Ramesh S, Ariffin AK, Nor SSM, Jamli MR. Production
of near-net-shape metal powder compact through warm compaction route- an
experimental investigation. In: International conference on recent advances in
mechanical & materials engineering, Kuala Lumpur, Malaysia, 30–31 May
2005.
[24] Youseffi M, Wright CS, Jeyacheya FM. Effect of carbon content sintering
temperature density and cooling rate upon properties of prealloyed Fe–1.5Mo
powder. Powder Metall 2000;43:270–4.