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International Journal of Advanced Materials and Metallurgical Engineering


2015, Volume 1, Issue 1, pp. 1-11, Article ID Tech-331
______________________________________________________________________________________________________

Research Article

Open Access

Optimization of Injection Moulding Process Parameters in MIM for


Impact Toughness of Sintered Parts
P. Pachauri and Md. Hamiuddin
Department of Mechanical Engineering, Z.H. College of Engineering & Technology, AMU, Aligarh, UP, India
Correspondence should be addressed to P. Pachauri, pp_niet@rediffmail.com; qumaispur422003@yahoo.co.in
Publication Date: 1 April 2015
Article Link: http://technical.cloud-journals.com/index.php/IJAMME/article/view/Tech-331

Copyright 2015 P. Pachauri and Md. Hamiuddin. This is an open access article distributed under the Creative
Commons Attribution License, which permits unrestricted use, distribution, and reproduction in any medium,
provided the original work is properly cited.

Abstract The identification of significant process parameters during injection moulding of feedstock in
Metal Injection Moulding (MIM) is essential because fine control is required for these parameters. A
small change in these parameters can cause large variation in the impact toughness of the parts
produced by MIM. The controlled parameters used for optimization in this work include injection
pressure, injection temperature, mould temperature, holding pressure, injection speed, powder
loading, holding time, and cooling time. These parameters have been optimized using analysis of
variance (ANOVA) for signal to noise ratios obtained in experiment performed by following Taguchi L 27
orthogonal array. The ANOVA also provides the contribution of significant process parameters to
impact toughness. Results show that the injection pressure, mould temperature and powder loading
are highly significant factors to the impact toughness, while the injection temperature, holding
pressure, injection speed, holding time, cooling time, the interaction of injection pressure and injection
temperature and interaction of injection pressure and mould temperature do not show significant effect
at 95% confidence level.
Keywords Analysis of Variance (ANOVA); Powder Injection Moulding (PIM); Taguchi Method; Impact
Toughness; Orthogonal Array
1. Introduction
Metal injection moulding (MIM) is an emerging technology to process metal powders into parts of
desired shapes. The MIM process combines the traditional shape-making capability of plastic injection
moulding and materials flexibility of powder metallurgy [1]. The process consists of four main steps:
mixing, injection moulding, debinding and sintering. In the mixing step, the powder is mixed with a
binder to form a homogeneous feedstock. The binder is key component, which provides the necessary
flowability and formability for moulding [2]. During injection moulding a green part with the desired
shape is formed by the feedstock flow into a mold under pressure. After moulding, the binder holds the
particles in place. The binder is then removed in the debinding step and the debound part is sintered to
achieve the required mechanical properties. The quality of the green parts affects the quality of the

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sintered parts. Once the parts have been molded to the required shape, there is little that can be done
to remedy defects caused during injection Moulding. The geometrical accuracy and mechanical
properties of the final parts after sintering depend strongly on the process parameters in the different
stages [3; 4]. Although the MIM process offers many advantages, it requires the proper moulding
condition. The classical Design of Experiment (DOE) technique has been used by many authors [5-7]
for optimization of single process parameters at a time. In order to obtain high efficiency in the
planning and analysis of experimental data, the Taguchi method is recognized as a systematic
approach for design and analysis of experiments to improve product quality [8; 9]. The Taguchi
method has been applied by many authors to investigate and optimize the process parameters [1013]. The majority of previous investigations in MIM have focused on the sintering parameters and the
amount of metal powder in the mixture. The effects of the injection moulding parameters on impact
toughness of the parts produced by MIM have not yet been thoroughly investigated. The objective of
this paper is to optimize the moulding parameters that simultaneously satisfy the requirements for
quality control of green part before it undergoes debinding and sintering processes to attain the
desired impact toughness. In this paper, the experiment is conducted by following Taguchi L 27
orthogonal array and data is analyzed by using analysis of variance (ANOVA) to find the significant
factors and their contribution in impact toughness of final part.
2. Materials and Methods
To make the working material, the SS316L stainless steel powder was mixed with the binder
comprised of polyethylene glycol (PEG), polymethyl methacrylate (PMMA), and stearic acid (SA) to
form the feedstock for moulding. The main advantage of using PMMA/PEG binder is that it can be
removed from the mouldings in a comparatively short time.
The SS316L metal powder used in this research was supplied by Osprey. The chemical composition
of the steel is presented in Table 1. The size distribution of metal powder is given in Table 2. The
percentage concentration of constituents by weight and densities are given in Table 3. The details of
the binder ingredients are given in Table 4.
Table 1: Composition of SS316 L Powder (Report Given by Osprey along with the Powder)

C
0.018

Si
0.55

Mn
1.5

P
0.031

Element %
S
Cr
0.017
16.9

Ni
11.6

Mo
2.2

Fe
balance

Table 2: Size Distribution of SS316 L Powder (Report given by Osprey)


Powder Tests Report by Sandvik Osprey Ltd.
d50
d90
-53 m
13.0 m
36.6 m
99.2 %

d10
3.9 m

Tap Density
5.0 gm/cc

Table 3: Theoretical Density of Constituents of SS316 L Powder


Element
C
Si
Mn
P
S
Cr
Ni
Mo

Percentage Concentration
0.018
0.55
1.5
0.031
0.017
16.9
11.6
2.2

Theoretical Density
2.267
2.33
7.47
1.823
1.96
7.14
8.9
10.28

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Fe
SS 316 L

67.184
100

7.874
7.88146

Table 4: The Binder Ingredients

Designation

Manufacturer

Polymethyl Methacrylate (PMMA)


Polyethylene Glycol(PEG)
Stearic acid(SA)

Vetec
Rankem
Fischer Scientific

Melting Temperature
C
157.77
35-40
70.1

Boiling
Point C
200
250
383

Density,
gm/cc
1.19
1.22
0.94

2.1. Feedstock Formulation


The metal powder and binder were mixed thoroughly for 90 minutes with the help of a Brookfield
Rheometer in the desired proportion under precise weight and temperature control condition. The
calculated amount of metal powder, PMMA, PEG and stearic acid were weighed and mixed together.
The mixing was carried out at 160C and 40 rpm to achieve a homogeneous distribution of the powder
particles and binder in feedstock. After thorough mixing, the mixture was first dried in air at ambient
temperature for 2 hours and then in an oven at a temperature of 50C for 1 hour. After compounding
the feedstock was allowed to cool to at ambient temperature and then granulated in a rotary feedstock
granulator.
2.2. Production of Test Specimen
A four-cavity mould was specifically designed and made by National Small Industries Corporation
(NSIC), Aligarh according to the specifications of the Demag injection moulding machine. The cavities
were created in accordance with MPIF Standard 50 and ASTM Standard E8-98. The impact specimen
geometry needed for this study was a 5mm x 10mm x 55mm (0.197 x 0.394 x 2.165) unnotched bar.
Using the known shrinkage factor for the given feedstock, the impact bars were molded to produce
oversize green parts as shown in Figure 1. The subsequent processing produced parts with the final
dimensions as specified in MPIF Standard 59 [14]. Either no machining or very fine machining was
needed to prepare the Charpy impact bars for testing. The green parts and sintered parts are shown in
Figure 2 and Figure 3 respectively.

Figure 1: Impact Test Bar (Specimen Size for Green Part)

Figure 2: The Samples Produced by Injection Moulding


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Figure 3: The Samples Produced after Sintering

2.3. Injection Moulding Procedure


Injection moulding process includes heating of the feedstock material to melting temperature, forcing
the molten material into the mould cavities, holding at high pressure, then cooling and ejection of the
molded parts out of the mould cavity. In the experimental work, a Demag injection moulding machine
with microprocessor control was used. It was loaded with LCD display, function keys, pump control,
heater control, manual function keys etc. Arrangements were provided for mould sensing and mould
cooling, and pneumatic ejectors in the control panel. On the machine, the injection pressure, injection
temperature, mould temperature, holding pressure, injection speed, holding time and cooling time
were set at the desired values. Since, the powder loading is an external factor; it is not to be taken
care by the machine control. Three types of feed stocks were developed before the start of the
experiment with fine weight control and homogeneous mixing. The twenty seven runs were divided in
three sets of nine runs each with the level of powder loading as constant. Each set of values was
repeated five times to make samples at each processing conditions after the machine has come to
smooth functioning. All the test parts were produced using only virgin feedstock. To achieve the
maximum uniformity of the green parts the same moulding sampling plan was followed for five runs.
Following the production of parts in each run the parts were visually inspected. In some cases there
was processing error, such parts were discarded and replaced with new parts.
2.4. Debinding Procedure
The green parts produced were debinded according to the process parameter control decided for
debinding. The solvent and thermal debinding techniques were used in this work to remove the
binders effectively. In the first step, solvent extraction was used to extract out the PEG from the green
parts. The green specimens were immersed in distilled water maintained at solvent debinding
temperature 60C for 6 hours with continuous stirring. The leached specimens were then dried in an
oven at 50C for 4 hours to completely remove the remains of water and then cooled. The second
step, referred to as thermal debinding was used to remove the PMMA and stearic acid after solvent
debinding. The leached specimens were put into an alumina tray in which the surrounding space was
filled with alumina powder to avoid any distortion of the specimens. The thermal debinding
temperature of 350C was achieved in a vacuum furnace in three steps. First, heating upto 200C at
the rate of 2.5C/min. Second, heating upto thermal debinding temperature of 350C at the rate 1
C/min. The temperature was held constant for 2 hours for the purpose to remove the polymers of the
binder. The brown part was allowed for slow cooling to ambient temperature (27C) at the rate of 1
C/min to release the residual stress from the part.
2.5. Sintering Procedure
For sintering the brown parts were first presintered then sintered. The peak temperature for
presintering after debinding was kept 900C. The heating rate was 3C/min and the holding time at
peak temperature was 60 minutes. The cooling rate was 5C/min. The presintered specimens were
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sintered afterwards in a batch furnace. The sintering was carried out in vacuum conditions at 1360C.
The heating cycle was completed in three steps. The specimen were heated upto 1360C at the rate of
10C/min, then held at isothermal sintering temperature for 90 minutes, and finally allowed to cool to
ambient temperature (27C) at the rate of 15C/min.
2.6. Design of Experiments and Testing Procedure
The objective of this work was to find the significant factors and their contribution during the injection
moulding of feedstock for best impact toughness. ANOVA was utilized to identify the significant level of
each variable. The Taguchi approach was used for this purpose. The method is based on balanced
orthogonal arrays [15]. For this experiment Taguchi L 27 orthogonal array consisting of 27 experiment
trials with 8 experimental parameters is used to obtain the signal to noise ratio (S/N ratio) of part
property. Based on the investigations [2; 12] and the expertise of the injection-moulding process eight
main parameters and two interactions were considered to study. Three factor levels were used to
conduct the experiment instead of two factor level. The controllable processing variables and their
variable values are shown in Table 5. Furthermore, interactions of injection pressure with injection
temperature and injection pressure with mold temperature were also investigated. Confirmation test is
done in order to verify within the range of optimum performance calculation. The raw data was
obtained using Taguchi Methodology. Taguchi technique utilises the signal to noise ratio (S/N)
approach to measure the deviation of the quality characteristic from the desired value instead of
average value [8]. Here the term Signal represents the desirable value (mean) and the Noise
represents the undesirable value. Thus S/N represents the amount of variation present in the
performance characteristic. Therefore, the experimental results were converted into S/N values for
optimization of parameters. The S/N ratio for higher the better was used. The ANOVA provided the
confidence level and the variance of the data. The confidence level is measured from the variance of
each parameter.
Table 5: Variable Process Controllable Parameters in Injection Moulding

Controllable Factor
Injection Pressure (MPa)

Injection Temperature ( C)

Mould Temperature ( C)
Holding Pressure (MPa)
Injection Speed (ccm/s)
Powder Loading (% vol.)
Holding Time (s)
Cooling Time (s)

Symbol
Pi
Ti
Tm
Ph
vi

th
tc

Level
Level 1
Level 2
50
60
140
150
45
50
65
70
5
10
60
61.5
5
10
5
8

Level 3
70
160
55
75
15
63
15
11

3. Results, Discussion and Conclusion


The effect of variable controllable parameters on the mean values of impact toughness is measured by
impact energy absorbed by the specimen during unnotched Charpy test. The calculated values for S/N
ratio and mean at all process parameter levels are shown in Table 6 and Table 7. The analysis of
variance made by using S/N ratio to find the significant factors is expressed in Table 8. The level
average response required for the analysis of the trend of performance characteristic with respect to
the variation of the factor under study is shown in Figure 4 and 5 respectively. From Figure 5 it can be
observed that the impact toughness has maximum value when injection pressure is 55MPa along with

mould temperature of 55 C and powder loading of 61.5% by volume. The dependence of impact
toughness on significant process parameters can also be observed from Figure 6, 7 and 8. It can be
observed from Figure 6 that high impact energy is absorbed by the specimen when the combination of
injection pressure and mould temperature is in dark green zone. From Figure 7 it can be observed that
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highest impact energy is absorbed when the injection pressure is in the range 53-58 MPa and powder
loading is in the range of 61-62% by volume. For the same powder loading the mould temperature

should be kept above 53 C to achieve high impact toughness as visible from Figure 8.
Table 6: Response Table for Signal to Noise Ratios (Larger is Better)
Level
1
2
3
Delta
Rank

Pi
39.93
40.48
40.59
0.66
1

Ti
40.42
40.19
40.41
0.23
6

Tm
40.11
40.31
40.59
0.48
2

Ph
40.14
40.43
40.45
0.31
5

vi
40.51
40.35
40.15
0.36
3

40.21
40.56
40.24
0.35
4

th
40.38
40.28
40.34
0.10
8

tc
40.38
40.35
40.27
0.11
7

Table 7: Response Table for Mean Value of Impact Energy Absorbed (J)
Level
1
2
3
Delta
Rank

Pi
99.60
106.20
107.56
7.96
1

Ti
105.24
102.80
105.31
2.51
6

Tm
101.71
104.04
107.60
5.89
2

Ph
102.07
105.51
105.78
3.71
5

vi
106.60
104.60
102.16
4.44
3

103.02
107.11
103.22
4.09
4

th
105.04
103.82
104.49
1.22
8

tc
105.04
104.64
103.67
1.38
7

Table 8: ANOVA Table using S/N Ratios for Impact Energy Absorbed
Factors/
Source
Pi
Ti
Tm
Ph
vi

th
tc
Pi x Ti
Pi x Tm
Residual
Error
Total

DOF,
v
2
(2)
2
(2)
(2)
2
(2)
(2)
(4)
(4)

Sums of
Squares
2.2432
0.3002
1.0337
0.5424
0.5859
0.6717
0.0473
0.0615
0.6904
0.7582

Variance,
Vn
1.1216
0.1501
0.5169
0.2712
0.2930
0.3359
0.0237
0.0308
0.1726
0.1896

20

3.0176

0.1509

26

6.9662

Variance
Ratio, Fn
7.43
3.42

2.23

Significance Pure Sum


Level,
Square
0.05
1.9414
Pooled
0.05
0.7319
Pooled
Pooled
0.05
0.3699
Pooled
Pooled
Pooled
Pooled

Contribution,
P in %
27.87
10.51

5.31

56.31
100
S = 0.1258 R-Sq = 99.5% R-Sq(adj) = 94.1%

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Figure 4: Main Effects Plot for Mean Values of Impact Energy Absorbed (J)

Figure 5: Interaction Plot of Injection Pressure, Mould Temperature and Powder Loading

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Effect of Injection Pressure and Mould Temperature on Absorbed Energy

Mould Temperature (C)

55.0

MEAN1
< 95
95 100
100 105
105 110
110 115
> 115

52.5

50.0

47.5

45.0
50

52

54

56

58

60

Injection Pressure (MPa)

Figure 6: Contour Curve for Injection Pressure and Mould Temperature

Effect of Injection Pressure and Powder Loading on Impact Energy Absorbed


63.0

MEAN1
< 95
95 100
100 105
105 110
110 115
> 115

Powder Loading (% vol.)

62.5

62.0

61.5

61.0

60.5

60.0
50

52

54

56

58

60

Injection Pressure (MPa)

Figure 7: Contour Curve for Injection Pressure and Powder Loading

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Effect of Mould Temperature and Powder Loading on Impact Energy Absorbed


63.0

MEAN1
< 95
95 100
100 105
105 110
110 115
> 115

Powder Loading (% vol.)

62.5

62.0

61.5

61.0

60.5

60.0
45.0

47.5

50.0

52.5

55.0

Mould Temperature (C)

Figure 8: Contour Curve for Mould Temperature and Powder Loading

From Table 8, it is observed that the factors: injection pressure, mould temperature, and powder
loading are the only significant factors, which influence the impact toughness of the parts. The injection
temperature, holding pressure, injection speed, holding time, cooling time, and the interactions are
insignificant factors at a confidence level of 95%, therefore the pooling is needed. After pooling the
contribution of injection pressure, mould temperature and powder loading is found to be 27.87%,
10.51% and 5.31% respectively at 95% confidence level. From Table 6, the highest value of S/N ratio
is noted for every factor to find the optimum level of process parameters for highest impact toughness.
The optimum level without considering the interaction factors can be noted as: (injection pressure) 3
(mould temperature)3 (powder loading)2. The optimum combination can be summed up as tabulated in
Table 9. From Table 6, it can further be noted from the rank of the parameters that variation in the
value of S/N ratio with the change in the value of parameter is maximum for injection pressure and
least for holding time.
Table 9: Optimum Factor Level for Highest Impact Energy Absorption

Controllable Parameters
Injection pressure (MPa)

Injection temperature ( C)

Mould temperature ( C)
Holding pressure (MPa)
Injection speed (ccm/s)
Powder loading (% vol.)
Holding time (s)
Cooling time (s)

Symbol
Pi
Ti
Tm
Ph
vi

th
tc

Value
60
170
55
75
5
61.5
5
5

3.1. Confirmation Test


Since, only Pi, Tm, and are the significant factors, the optimum value of impact toughness will
depend mainly on these factors and could be estimated by Eq. (1) at the optimum levels shown in
Table 9.

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IT =

+ [(Pi)3 -

+ [(Tm)3 -

+ [()2 -

(1)

Where, is the overall mean of impact energy absorbed = 104.45 J


(Pi)3 is the average value of impact energy absorbed at level 3 of factor Pi = 107.56 J
(Tm)3 is the average value of impact energy absorbed at level 3 of factor T m = 107.60 J
()2 is the average value of impact energy absorbed at level 2 of factor = 107.11 J
Hence, the expected impact energy absorbed at optimum condition is:
IT = 107.56 + 107.60 + 107.11 - (2x 104.45) = 113.36 J
The 95% confidence interval (CI) for the expected yield from the confirmation experiment can be
calculated using Eq. (2) as follows:
(2)
Where, neff = (N/(1+ total degree of freedom of all factors used for estimating )
r = sample size for the confirmation experiment, r 0.
level of significance . The confidence level is (1-),

is the variance ratio of

and

at

is the degree of freedom of mean (equal to 1)

and
is the degree of freedom for the pooled error. Variance for pooled error is V e. The confidence
interval indicates the maximum and minimum levels of the optimum performance. Tabulated F-ratio at
95% confidence level ( = 0.05): F0.05;(1,20) = 4.35 and neff = [27 x 5/7] = 19.28

CI = {4.35 x 0.1509[(1/19.28) + (1/5)]} = 0.4066


Therefore, the expected impact energy absorption at optimum condition = IT CI = 113.36 0.4066
i.e. 112.95 < IT < 113.766
To confirm the prediction, another five samples were made at the recommended settings as shown in
Table 9. The experimental observations if impact energy absorbed are given in Table 10.
Table 10: Results of Confirmation Experiments

Characteristic

Replication at Optimum Process Parameters


R1
R2
R3
R4
R5

Impact Energy
Absorbed (J)

110

112

111

114

112

Average
111.8

Minitab Predicted
Value
113.36

It can be observed that the average impact energy absorbed obtained from the confirmation
experiment is within the predicted 95% confidence interval. From Table 10, it can also be noted that
the experimental results are close to the predicted result by Minitab 17 software. The difference
between measured and predicted values is about 1.4%. It confirms the reliability of the control of
process parameters.
Acknowledgements
The authors would like to acknowledge the financial support and facilities provided by Noida Institute
of Engineering and Technology, Greater Noida for this research work.

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