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Thermal Debinding Process of SS 17-4 PH in Metal Injection Molding Process

with Variation of Heating Rates, Temperatures, and Holding Times

Article  in  Diffusion and Defect Data Pt.B: Solid State Phenomena · October 2017
DOI: 10.4028/www.scientific.net/SSP.266.238

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Solid State Phenomena Submitted: 2017-06-25
ISSN: 1662-9779, Vol. 266, pp 238-244 Accepted: 2017-06-26
doi:10.4028/www.scientific.net/SSP.266.238 Online: 2017-10-02
© 2017 Trans Tech Publications, Switzerland

Thermal Debinding Process of SS 17-4 PH in Metal Injection Molding

Process with Variation of Heating Rates,
Temperatures, and Holding Times
Sugeng Supriadi1,a, Bambang Suharno2,b, Rizki Hidayatullah2,c,
Gerra Maulana2,d, Eung-Ryul Baek3,e
1
Mechanical Engineering, Faculty of Engineering, University of Indonesia, Depok, Indonesia
2
Metallurgy and Materials Engineering, Faculty of Engineering, University of Indonesia, Depok,
Indonesia
3
School of Materials Science and Engineering, Yeungnam University, South Korea
a
[email protected], [email protected], [email protected],
d
[email protected], [email protected]

Keywords: Metal Injection Molding, SS 17-4 PH, Thermal Debinding, Holding Time, Temperature,
Heating Rate

Abstract. Generally, metal injection molding (MIM) method utilizes SS 17-4 PH as material for
application of orthodontic bracket. One of the process of MIM is thermal debinding, which binder is
eliminated by thermal energy. In this study, thermal debinding process is conducted with variation
of temperature, i.e. 480, 510, and 540oC, holding time, i.e. 0.5, 1 and 2 hours, heating rate, i.e. 0.5,
1, 1.5, and 2oC/min.The effect of temperature shows that the increased temperature will result in the
mass reduction percentage due to formation of oxide on the sample, which will be proven through
TGA testing. The highest mass reduction was 6.4137 wt% which was obtained at 480 oC. For the
variation of holding time, the longer the holding time will result in increased mass reduction and the
highest mas reduction was 6.255 wt% which was obtained during 2 hours of holding time. For the
heating rate, the slower the heating rate will result in increased mass reduction and decreased the
presence of crack formation. The best variable was obtained at heating rate of 0.5oC/min, which
resulted mass reduction of 6.2488 wt% and less crack formation.

Introduction
Malocclusion is one of the most common problems in the orthodontics field. The use of
orthodontic brackets aims to control and improve the position of the jaw so that the influence of
malocclusion can slowly be reduced. In Indonesia, orthodontic brackets production is still done by
imports. From here comes the discussion to produce an orthodontic bracket nationally. Our latest
research used Stainless Steel 17-4PH as the material and investment casting as the manufacturing
processes. However, it is obtained that investment casting result have rough surfaces that require
further processing end [1]. Therefore, it is necessary to study other manufacturing processes for
brackets production, namely metal injection molding.
One of the main problem of metal injection molding process is at the debinding step due to crack
formation on the surface caused by high thermal gradient [2][3]. We conducted an experiment to
enhance binder removal rate through the process of thermal debinding treatment without any crack
initiation point found on the surface of the brown part and also examine the effect of temperature
and holding time to brown part which have to be the significant factors of thermal debinding
process [4]. The experiment is done by comparing the effect of different value of heating rates,
temperature, and holding time on binder removal. In this study, we do not use the orthodontic
brackets as the sample experiment but a cubic sample of 5x5x5 mm. This approach is use to study
the phenomenon easier with a flat surface.

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 Solid State Phenomena Vol. 266 239

Experimental Works
Material. Stainless steel 17-4 PH is use in this experiment due to its high corrosion resistant with
high composition of chromium [5]. It is classified as Martensitic steel.
Table 1. Chemical composition of SS 17-4 PH
C (%) Si (%) Mn (%) P (%) S (%) Cu (%) O (%)

0,04 0,39 0,16 0,02 0,00 3,96 0,35

Cr (%) Mo (%) Ni (%) Cu (%) Nb (%) Co (%) Fe (%)
16,44 0,02 4,04 3,96 0,29 0,03 74,26

Feedstock was observed with SEM, it could be seen that there are grayish areas around the
powder, this shows the existence of binder around the grains of stainless steel [6]. TGA Testing was
also conducted and it is known that the binder degraded at temperatures of 167oC - 375oC and
407oC - 477oC. It is known that at a temperature of 167oC - 375oC is the primary binder degradation
temperature and 407 - 477oC the secondary binder degradation temperature.

101,0
100,0
99,0
% Weight Loss

98,0
97,0
96,0
95,0
94,0
93,0
92,0
0,0 200,0 400,0 600,0 800,0 1 000,0
Temperature (oC)

Fig. 1. a. TGA, b. SEM of feedstock SS 17-4 PH

Injection Molding & Thermal Debinding. Feedstock was injected into cubic mold of 5 mm x
5 mm x 5 mm. The samples were molded at the following conditions: nozzle and barrel temperature
at 180 – 200oC, mold temperature 50 – 60oC, pressure 2700 psi, and injection time 5 s.
Thermal debinding process of the green part is then carried out in a vacuum atmosphere with a
pressure of approximately -0.6 to -0.4 MPa. The binder removal rate in vacuum is higher than in the
normal atmosphere [7]. The schedule of thermal debinding proces:
Table 2. Schedule of Thermal Debinding
Variable Temperature Holding Time Heating Rate
o
Temperature 480 C, 510 1 Hour 1oC/min
o
C, 540 oC
Holding Time 510oC 0.5, 1, & 2 Hours 1oC/min
Heating Rate 510oC 1 Hour 0.5oC/min, 1 oC/min,
1.5 oC/min, 2 oC/min
Then the brown part product of thermal debinding is characterized by TGA and SEM/EDS to
determine whether there are binder remaining on the sampel or not [8]. In addition, the brown part
was observed using optical macroscope to see the formation of cracks that occur due to differences
in the heating rate values.
240 Material and Manufacturing Technology VIII

Results and Discussion

Percentage of Weight loss is increased with longer holding time, as in fig.2. This is due to the
longer period of time in isothermal make the remaining binder can be eliminated more evenly,
thereby reducing the remnants of the binder in the sample [9]. Test results showed an increase in
density on the sample with longer holding time, indicating that more binder is reduced from the
brown part.
a 6,27 b 5,8
6.255 5.7509
6,26 5,75

Density (g/cm3)
% Weight Loss

6,25 5.7057
6.2347 5,7
6,24 6.2258 5.6383
5,65
6,23
6,22 5,6

6,21 5,55
0 0,5 1 1,5 2 2,5 0 0,5 1 1,5 2 2,5
Holding Time (H) Holding Time (H)

Fig. 2. Effect holding time to a. weight loss, b. density

For different temperature variable, the percentage of the weight loss of the samples decreased
with increasing thermal debinding holding temperature. The binder removal rate should increase
with the increasing of thermal debinding temperatur. However, the density of the test results is
increasing with higher processing temperature, it is in accordance with the literature [4]. These are
indicated there is oxidation phenomena appears in the higher temperature instead of incomplete
binder removal [10].
a 6,60 b 5,9
6,50 6.4137 5,85
6,40 5.7885
% Weight Loss

Density (g/cm3)

5,8
6,30 6.2347 5.7057
5,75 5.6969
6,20
5,7
6,10
5.962 5,65
6,00
5,90 5,6
5,80 5,55
5,70 5,5
460 480 500 520 540 560 460 480 500 520 540 560
Temperature (oC) Temperature (oC)

Fig. 3. Effect of temperature to a. weight loss, b. density

SEM characterization conducted by comparing the samples at temperature of 480oC and 540oC,
Fig 4. At 540oC, test result showed high content of oxygen, chromium, and silicon in the sample,
Fig 5. This results show that there is oxidation reaction occurred during the 540oC treatment
temperature with the possibility of Cr2O3 and SiO2 formation [11]. It is indicated that the binder in
the 540oC sample were removed from the part much more than the 480oC samples. But the
formation of the oxides cause the increase of the sample mass and make the calculation of weight
loss percentage tend to decrease.
 Solid State Phenomena Vol. 266 241

a b

Fig. 4. a. SEM of 480oC sample, b. SEM of 540oC sample

a b

Fig. 5. a. EDS of 480oC sample, b. EDS of 540oC sample

In the heating rate variations, fig.6 showed the percentage of weight loss increased with a slower
rate of heating. With the decrease of the heating, the heat distribution in the sample are spread more
evenly and homogeneous [12].

a 6,28 b 6 5.9032
6.2499 5.7057
6,26
6.2347 5,8 5.6604
Density (g/cm3)
% Weight Loss

6,24
6,22 6.1893 5,6
6,20
6,18 6.1657 5,4
6,16 5.1328
5,2
6,14
6,12 5
0 0,5 1 1,5 2 2,5 0 0,5 1 1,5 2 2,5
Heating Rate (oC/min) Heating Rate (oC/min)

Fig. 6. Effect heating rate to a. weight loss, b. density

Crack is the major issue that can occurs when the heating rate of thermal debinding process is
too fast. From optical macroscope observation fig. 6, shows that the faster the heating rate, will
result in increased the probability of crack and defect formation in the final product. The faster the
heating rate will cause difference between surface and inside temperature of the sample, thermal
stress will arise that lead to the formation of cracks [13].
242 Material and Manufacturing Technology VIII

a b

c d

Fig. 7. Surface crack after thermal debinding a. 0.5oC/min, b. 1 oC/min, c. 1.5oC/min,

d. 2oC/min
Brown part from thermal debinding process with heating rate of 1oC/min to 510oC, and holding
time up to 2 hours was observed with SEM and TGA to prove the binder has been completely
eliminated from sample. In fig. 8 it can be seen that the grayish area in the sample had been gone
and showed a grain of stainless steel without the sheath surrounding binder. The porous also
appears around the grains, when sintering was conducted the pores will dissapear and shrinkage will
appear.

Fig. 8. SEM of a. Feedstock, b. Brown Part

TGA results showed no decrease in sample weight. These indicate binders have been removed
almost entirely from the samples. Graphic in fig.9 shows a mass increase at temperature around
540oC due to the flow of nitrogen gas from the TGA test diffused to porous formed during the
thermal debinding process. The nitrogen reacts with the other elements and produces nitrides. As
the result of the reaction, it causes an increase in the mass of the sample.
 Solid State Phenomena Vol. 266 243

101,4
101,2

% Sample Weight
101
100,8
100,6
100,4
100,2
100
99,8
0 200 400 600 800 1000
Temperature ( C)
o

Fig. 9. TGA graph of brown part

Conclusions
1. The most optimum temperature for the thermal debinding process in our research is 510oC
with binder removal percentage of 6.2% and fewer oxides content.
2. The increase of holding time enhances the binder removal percentage of the process.
3. Slower heating rate results in increasing amount of binder removal from the brown part with
less crack formed on the surface compare to other faster heating rate.
4. The use of vacuum pressure throughout the thermal debinding process is neccessary to
prevent any oxidation occurs during the process and avoid any binder stick back on the
brown part.

Aknowledgement
The authors acknowledge financial support from DIKTI for contribution in the development of this
work.

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