Single step of binder thermal debinding and sintering of injection moulded

316L stainless steel

Indra Putra Almanar1,a, Zuhailawati Hussain 2,b and Mohd Afian Omar3,c
1
School of Mechanical Engineering,
2
School of Materials and Mineral Resources Engineering,
Engineering Campus,
Universiti Sains Malaysia, 14300 Nibong Tebal, Penang, Malaysia
3
Advanced Materials Research Centre, Sirim Berhad, Lot 34, Jalan Hi-Tech 2/3, Kulim Hi-Tech Park, 09000
Kedah, Malaysia
a
meinput@yahoo.co.uk, bzuhaila@eng.usm.my, cafian@sirim.my

Keywords: Metal injection moulding, stainless steel, sintering

Abstract. Metal injection moulding was performed with gas atomized 316L stainless steel powders.
Feedstocks were prepared using a paraffin wax/polyethylene/stearic acid binder system and
subsequently molded into tensile bar specimens. Solvent extraction done at 80○C has shortened the
debinding process to 30 minute. Single step of thermal binder debinding and sintering was done in a
vacuum furnace. Sintering at 1380○C has reduced the porosity and associated with grain growth that
result in an increase in ultimate tensile strength to 444 MPa while the elongation increased to 29%
before fracture.

Introduction
Injection moulding using stainless steels powder has significant utilisation in the manufacturing
of relatively small, complex shaped parts requiring high strength and good corrosion resistance. The
debinding in PIM is a critical processing step and has been identified as that part of the technique,
which had primarily to be improved. Long debinding times or alternatively high risk of sample
distortion have been a major obstacle for the economic success of PIM. Thermal, solvent, and
vacuum debinding processes have been widely adopted by the powder injection molding (PIM)
industry [1,2].
A more recent developed vacuum debinding process combines debinding and sintering cycles
into a single step and minimizes damage caused by the handling of fragile debound parts [3,4]. In
this process, a high vacuum is employed at low temperatures to enhance the thermal debinding rate
of low temperature binder components such as paraffin wax. At high temperatures, low vacuum is
used to remove the remaining major binders. After debinding, the parts are sintered in the same
furnace. This combination of debinding and sintering cycles is made possible by using a special
pumping system which avoids the build up of condensed binder vapours in the pipings. The present
work deals with metal injection moulding of 316L stainless steel using two steps of debinding
process which are solvent debinding followed by thermal debinding. The relationship between the
sintering temperature and mechanical properties of the sintered products are discussed.

Methodology
In this study, gas atomized 316L stainless steel powder supplied by Anval, Sweden with 15 µm
median particle size was used. 55 wt. % of paraffin wax, 35 wt. % of polyethylene and 10 wt. % of
stearic acid were used as binder system. Tensile bar specimen was produced using MCP HEK-
GMBH Injection Moulding at 180oC and 30 MPa (300 bar). Solvent extraction debinding was
performed to remove paraffin wax component of the binder. The solvent used was heptane which is
heated to 40○C, 60○C or 80 ○C. The specimens were immersed in the heated solvent for 10, 30, 60,
120, 150, 240 and 360 minutes. Then, the specimens were removed from heptane and placed in a
drying oven at 45○C± 5○C for 2 hours to removed any remaining heptane from specimens.
Thermal pyrolysis debinding was done in a vacuum furnace for 440○C for 1 to remove the
remaining binder, polyethylene and stearic acid. Sintering cycle was proceeded in the same furnace
after the thermal pyrolysis process by increasing the temperature 1300○C, 1320○C, 1340○C, 1360○C
and 1380○C. After sintering, weight loss and dimensions were measured to calculate the sintered
shrinkage and the densities were then examined by using water immersion. Tensile testing was
performed on the specimens after sintering. Nital solution was used to reveal the microstructure
under optical microscope.

Results & Discussion

Fig. 1 shows the percentage of paraffin wax removed at various times for three different
temperatures during solvent extraction process. It is proposed that the solvent reaction should be
done at 80oC for 30 minute to shorten the solvent extraction process. During immersion in heptane
in the water bath, the paraffin wax begin to dissolve in the heptane and fine pore channels begin to
form. As the time increased, the weight loss of the specimen due to the dissolution of paraffin wax
is increased and the pore channels enlarged. Fig. 2 presents a scanning electron micrograph of the
moulded specimens after immersed in the heptane for 30 minute at 80○C which give evidence that
the open pore channels were formed by the removal of paraffin wax. The formation of open pore
channels allows the rapid removal of the remaining binder without cracking, blistering or swelling
during subsequent thermal pyrolysis. The whole debinding cycle is about 7 hours in duration. This
is short enough compared with the 10 hours taken by conventional thermal degradation process.
Paraffin wax removed (%)

120.0
100.0
80.0
40 oC
60.0
60 oC
40.0
80 oC
20.0
0.0
0 100 200 300 400
Time ( Minutes )

Fig. 1 The effect of debinding time and temperature on the percentage of paraffin wax removed.

Fig. 2 SEM show the development of interconnected pores

 Fig. 3 shows the density of the sintered sample and shrinkage. Higher shrinkage contributed to
higher density. A relative density of sintered specimens was obtained as 87.8% at 1300○C and as
99.8%, very close to theoretical density, at 1380○C.

16 8
14 7.8

Density (g/cm3)
12
Shrinkage (%)
7.6
10
7.4
8
Shrinkage 7.2
6
4 Density 7
2 6.8
0 6.6
1300 1320 1340 1360 1380
Temperature (C)

Fig. 3 Shrinkage and density of the sample after sintering at different temperature
Fig. 4 presents the optical micrographs of the specimens for different sintering temperature. The
porosity of the sintered specimens is decreased as the sintering temperatures are increased. Pore of
sintered specimens become more rounded and appeared to be isolated in then distribution as the
sintering temperature was increased. The pore present in the specimen generally very fine, closed
and uniformly distributed (at 1360○C and 1380○C). The pores after sintering process occupy both
location that is the grain boundaries and in the grain interiors. Substantial grain growth has been
observed at higher temperature.

(a) (b) (c)

20 µm 20 µm 20 µm

(d) (e)

20 µm 20 µm

Fig. 4 Optical micrographs of etched 316L stainless steel for different sintering temperature (a)
1300○C, (b) 1320○C, (c) 1340○C, (d) 1360○C and (e) 1380○C

The variation of the ultimate tensile strength and percentage of elongation for the specimens with
the sintering temperature are shown in Fig. 5. Low porosity gives good mechanical properties of
the specimens. The ultimate tensile strength increased from 327 to 444 MPa when the sintering
temperature was increased from 1300○C to 1380○C while the elongation increased from 19% to 29 %
before fracture.

Conclusions
In this study, solvent extraction debinding process coupled with the thermal removal of the
remaining binder phase during sintering has been applied on injection molding part of 316L
stainless steel. The rate of extraction of paraffin wax from the green body increased with increasing
solvent extraction temperature. As the time increased, the weight loss increased and the pores
channels enlarged. The pores present in the sintered part generally very fine, closed and uniformly
distributed (at 1360○C and 1380○C). Low porosity in the sample sintered at higher temperature
exhibited good ultimate tensile strength and elongation.

Acknowledgement
Financial support provided by Universiti Sains Malaysia under the schemes of TPLN and Research
University Grant are acknowledged. Acknowledgement is also extended to Ms. Yew Sin Lin for her
assistance in experimental work.

References
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Binder For Powder Injection Moulding, PIM Symposium Proceedings, San Francisco (1992).
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[4] M.A. Omar, R. Ibrahim, M.I. Sidik, M. Mustapha and M. Mohamad, J. Mater. Process.
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