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Materials and Design 33 (2012) 153–157

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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 is about 60% of the melting temperature of the main powder con-
stituent, more cumulative atomic motion occurs, leading to im-
A major advance in powder compaction technology is the form- proved inter-particle bonding. However, high temperature, longer
ing of powder mass at above ambient temperature, which can uti- holding time, and small particle size are not always economically
lize traditional powder forming equipment. The powder mass viable for conducting sintering operation. Therefore, control over
together with the die assembly is required to be heated up to a heating rate, time, temperature and atmosphere is required for
temperature below the re-crystallization temperature of the main producible results. In general, the parts tend to densify and im-
powder constituent [1–5]. The process can produce components prove the mechanical properties as sintering proceeds. Increase
having good surface finish and dimensional tolerance hence mini- the density implies an overall shrinkage which leads to complica-
mal further processing is required, therefore less time is taken to tions. The dimensional change is influenced by the green density;
produce an engineering component [6]. the lower this is the greater the tendency to shrink [8].
Density gradients are often evident in green compacts mainly Manufacturing of engineering components through warm form-
due to the complex powder deformation mechanisms occur during ing route involves several key parameters during feedstock prepa-
the compaction phase. These gradients are the main causes of part ration, powder forming, and sintering. Powder forming at above
distortion during the subsequent process of sintering and may ambient temperature is initiated recently and extensive research
even lead to part fracture during its ejection from the die cavity. papers were published [9–17], however less information on the ef-
In order to achieve the required strength in the products, the green fects of warm forming and sintering schedule to the mechanical
compacts formed through warm compaction route are required a properties and microstructures are found. Therefore, this paper
firing treatment known as sintering, which refers to the heat treat- presents the outcome of an extensive research on the effects of
ment of a powder metallurgy green compact for the purpose of forming and sintering parameters to the final performance of the
increasing its strength by bonding together of the particles. Sinter- products formed through warm compaction route.
ing is normally conducted at a temperature where atomic motion
leads to growth of weld bonds among contacting particles [7]. With
2. Experimental procedure
higher temperature or longer holds at the peak temperature, which
A lab scale warm compaction rig was designed and fabricated
⇑ Corresponding author. Tel.: +60 3 89297269; fax: +60 3 89212116. (Fig. 1) which enabled the generation of green compacts at differ-
E-mail address: mujibur@uniten.edu.my (M.M. Rahman). 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 working phenomenon [22] has occurred resulted in strength incre-
even though the powder mass is formed at the same temperature. ment. Dimensional changes of the final products are also almost
As the melting temperature of zinc stearate is 130 °C, the effective same for both lubricant content and forming temperature. It is
working temperature of lubricant is around 120 °C instead of shown that amount of lubricant used is acceptable and also larger
180 °C. Therefore, 120 °C forming temperature has given higher amount of lubricant is believed to have been forced out from the
relative density during compaction process and as the samples component accumulated at the side wall during the compaction
are sintered at the same schedules, higher relative density of final process.
product is achieved at a higher density sample. Furthermore, due Relative density, hardness, and strength of final parts sintered at
to the addition of higher weight percent of lubricant, i.e., 0.8 wt%, different temperature are shown in Figs. 7–9 whereas the micro-
some zinc stearate is trapped inside the powder mass, which re- graphs of sintered parts formed from iron powder without lubri-
duces the inter particle friction and eases the motion of powder cant, 0.4 wt% admixed lubricant formed at 180 °C, and 0.8 wt%
particles, as a consequence, the volume becomes smaller hence admixed lubricant formed at 120 °C are shown in Figs. 10–12. It
density becomes higher [21] compared to the addition 0.4 wt% is clearly observed that final densities and strengths are higher
lubricant. for the products formed at 180 °C by adding 0.4 wt% of lubricant,
It can be observed in Fig. 4 that lower lubricant content inside however hardness is slightly lower. Adding optimum amount of
the powder mass could result harder products in the case of com- zinc stearate which is 0.4 wt% has promoted the increase in density
paction at lower temperature. In terms of strength, it is observed during compaction stage. Furthermore, as larger amount of zinc
that superior bending strength could be achieved by adding only stearate has been forced out from the green samples during com-
0.4 wt% of lubricant and forming the powder mass at 180 °C. It is 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 The results revealed that higher density and harder green com-
strength are also obtained by sintering the green compacts at high- pacts could be produced by adding 0.8 wt% zinc stearate and form-
er temperature, i.e., 1000 °C. Structure re-crystallization occurred ing the powder mass at 120 °C. However, the sintered results
steadily and fusion rate among particles increased during sintering showed that the suitable lubricant content is around 0.4 wt%, and
at higher temperature thus improved bonding among iron particles the forming temperature is around 180 °C. The green compacts
during the sintering process. are suitable to be sintered in inert gas fired sintering furnace at a
The green compacts formed at 180 °C by adding 0.4 wt% of lu- heating/cooling rate of 10 °C/min, sintering time and temperature
bricant and subsequently sintered at 1000 °C for 30 min also show of 30 min and 1000 °C, respectively. The end products are defect-
more uniform grain distribution (Fig. 11). Non-uniform grain dis- free yet high strength, near-net shape components.
tribution and localized voids are observed for the compacts formed
without lubricant as well as higher content of admixed lubricant Acknowledgement
(Figs. 10 and 12).
Iron powder mixed with 0.8 wt% zinc stearate and formed at This research is financially supported by Universiti Tenaga
180 °C is proven to result green compacts with higher relative den- Nasional through the research Project J510050356.
sity and strength [23], however the excessive lubricant might be
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