Materials Chemistry and Physics 271 (2021) 124926

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Materials Chemistry and Physics

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

Rheological investigation and injection optimization of Fe–2Ni–2Cu

feedstock for metal injection molding process
Ali Askari a, *, Vahid Momeni b
a
Department of Mechanical Engineering, NazarAbad Center, Karaj Branch, Islamic Azad University, Karaj, Iran
b
Department of Mechanical Engineering, Faculty of Materials and Manufacturing Processes, Malek Ashtar University of Technology, Tehran, Iran

H I G H L I G H T S

• The Critical Solids Loading obtained for the developed feedstock by analysing various solids loading.
• Calculated flow activation energy, made an excellent fit to the Arrhenius equation.
• Calculated n-values and the small variations, indicated suitability of feedstock.
• Moldability index, which is a comprehensive rheological indicator was developed.
• It was observed that injection speed (unlike the holding pressure) plays a significant role in increasing the strength.

A R T I C L E I N F O A B S T R A C T

Keywords: In this study, rheological behavior and optimized injection parameters for Fe–2Ni–2Cu feedstock in the metal
Metal injection molding injection molding process were investigated using the capillary and Taguchi methods. For this purpose, the
Rheological behavior critical solids loading obtained for the feedstock by analyzing various solids loading (56–64 vol%). In the next
General moldability index
step, fundamental rheological characteristics of a homogenized feedstock, including flow behavior index (n),
Injection parameters
Mechanical properties
flow activation energy (E), and general moldability index (αstv ), were studied. Optimization of the most
important injection parameters, including injection speed, injection temperature, mold temperature, and holding
pressure, was conducted applying the Taguchi method. According to the results of experiments, injection speed
plays a significant role in increasing the density and flexural strength. Also, there are optimum points for in­
jection temperature and mold temperature, while holding pressure does not significantly influence the density
and flexural strength. Satisfying results have been shown in green density and flexural strength after the veri­
fication test. Rheological behavior analysis showed 60 vol% as critical solids loading, while the proper solids
loading considered to be 58 vol% in order to make an easier flow during the injection for the feedstock. The flow
behavior index of developed feedstock indicates the shear rate sensitivity was desirable since it shows less than
one value. Also, flow activation energy, which shows the feedstock sensitivity to the temperature changes, came
out to be 78.138 kJ/mol. Finally, The general moldability index was calculated to be 3.1302E-06 Pa− 1 K− 1 by
using these parameters.

1. Introduction
Novel processes and applications of metals, alloys, as well as their
composites should be noticed; also, the problems must be addressed to
improve different industries [1–7]. Metal injection molding (MIM) is an
automated mass production process used to produce complex parts
having accurate dimensions [8]. MIM consists of four main steps,
including compounding, injection, debinding, and sintering [9,10]. In
the first step, metal powders are mixing with a suitable binder system to
form the feedstock in order to make the powders injectable using an
injection molding machine [11]. In the next step, the feedstock is
molding into the required shape, and then the molded part undergoes a
debinding step where the binder gets extracted, and in the final step, the
remaining powder will sinter to get full or near full density [12].
The binder system is usually composed of a primary polymer to
support and maintain the part’s shape during the debinding and

* Corresponding author.
E-mail address: Ali.Askari@Kiau.ac.ir (A. Askari).

https://doi.org/10.1016/j.matchemphys.2021.124926
Received 7 December 2020; Received in revised form 10 April 2021; Accepted 4 July 2021
Available online 6 July 2021
0254-0584/© 2021 Elsevier B.V. All rights reserved.
A. Askari and V. Momeni Materials Chemistry and Physics 271 (2021) 124926

Table 3
Most effective factors and levels of the designed experiments.
Factors Symbols Levels

− 1 0 1

Injection speed (mm/s) A 20 40 60

Injection temperature (◦ C) B 150 160 170
Mold temperature (◦ C) C 40 50 60
Holding pressure (MPa) D 100 300 500

Table 4
Experimental design using the Taguchu method.
Test Factor 1 Factor 2 Factor 3 Factor 4
Number Injection Injection Mold Holding
Speed (mm/ Temperature Temperature Pressure
s) (◦ C) (◦ C) (MPa)

1 20 150 40 100
Fig. 1. Scanning electron micrograph of Fe–2Ni–2Cu gas atomized powder. 2 60 160 40 500
3 40 170 40 300
4 60 170 50 100
5 40 150 50 500
6 20 160 50 300
7 60 150 60 300
8 40 160 60 100
9 20 170 60 500

sintering process [13]. In order to reduce the viscosity of the feedstock

and to provide smooth injection during the mold filling, some additives
such as waxes and low molecular weight polymers are added to the
binder system. Therefore, the rheological behavior of the feedstock is an
important parameter that needs to be considered during the com­
pounding stage in order to get defect-free parts [14]. Many parameters
like powder loading, the type of binder system and its components,
powder dispersion, and size affect the feedstock’s rheological properties
[15]. Low shrinkage and good dimensional stability of the part during
the sintering can be a result of high powder loading. It can also lead to
high feedstock viscosity due to the friction between the powder parti­
Fig. 2. Particle Size Distribution of used Fe–2Ni–2Cu Powder particles. cles. On the other hand, low powder loading can create many defects
during the sintering stage.
M. Khakbiz et al. [16] investigated the rheological behavior and
Table 1 stability of TiC and stainless steel 316L feedstock. In this study, they
Characterization of the Fe–2Ni–2Cu powder. investigated the effect of TiC percentage, temperature, shear rate, and
Characteristics Fe–2Ni–2Cu powder loading on the feedstock viscosity using the capillary rheometer.
D10 2.11 Their research results showed that the feedstock instability increases
Particle Size (μm) D50 4.03 with decreasing the powder loading. Also, an increase in the tempera­
D90 7.41 ture and shear rate resulted in a decrease in viscosity and feedstock
Distribution slope parameter 2.56 4.69
Sw = ( ) instability [17]. Sotomayor et al. [18] studied the effects of the powder
D90
log 10
D10
particle dispersion and solids loading on the rheological properties of
Apparent density 2.63 stainless steel 316L with a double component binder system consisting
Density (g/cm3) Tap density 4.34 of 50 vol% polyethylene (PE) and 50 vol% paraffin wax. Their results
Pycnometer density 7.873
showed that with the increase in the shear rate, the viscosity of the
feedstock decreases. Also, as the particle size decreases, the rheological
behavior tends towards pseudo-plastic, and the flow behavior index (n)
Table 2 decreases. The particle size did not seem to affect the activation energy
Properties of used binder system components.
remarkably, unlike the solids loading, where the lowest activation en­
Component Density Aaverage Melting Decomposition ergy was observed in the highest solids loading of the feedstock. Other
(g/cm3) molecular temperature temperature
studies have also reported the role of binder system and powder loading
weight Mw (◦ C) (◦ C)
(g/mol)
on the viscosity, flow behavior index and flow activation energy
[19–22].
Paraffin wax 0.90 414 37–60 180–320
Apart from the feedstock’s appropriate rheological behavior to pro­
(PW)
Polypropylene 0.92 80504 115–135 350–470 vide a desirable and smooth flow for feedstock, applying the optimum
(PP) injection parameters are necessary to inject defect-free green parts. The
Polyethylene 0.90 154981 110–130 420–480 injection parameters are including injection pressure, injection speed,
(PE)
injection temperature, mold temperature, cooling time, holding pres­
Stearic acid 0.94 560 69–72 263–306
(SA)
sure, and time. Many studies have been conducted in this area [23–27],
which for example, one can refer to the study of Berginc et al. [28],

2
A. Askari and V. Momeni Materials Chemistry and Physics 271 (2021) 124926

Table 5
Flow behavior index (n), flow activation energy (E), and moldability index (αstv)
of feedstock at different temperatures.
Flow Activation Moldability index
behavior Energy (kJ/mol) (Pa− 1 K− 1)
index

Temperature 150 0.49

(◦ C) 160 0.57 78.138 3.1302E-06
170 0.61
Average value 0.56

Fig. 5. Calculation of the flow activation energy for the feedstock.

where they studied the effects of injection parameters on the mechanical

Fig. 3. Measurement of critical solids loading: a) mixing torque variations vs.
time, b) average torque values with different solids loading.
properties of stainless steel 316L MIM compact. They used the design of
experiments (DOE) method in order to optimize the injection parame­
ters. They reported that the best parameter combination for proper in­
jection of the stainless steel 316L feedstock is holding pressure of 500
bar, mold temperature of 40 ◦ C, the nozzle injection temperature of
200 ◦ C and injection speed of 40 mm/s.
In another study, for stainless steel 316L powder, Sulong et al. [29]
concluded that mold temperature and holding time has the highest effect
on the strength and surface finish, respectively, when using a binder
system consisting of 73 vol% PEG, 25 vol% PMMA, and 2 vol% SA.
It can be concluded that many parameters such as powder loading,
binder system type, binder system constituents, their percentages, and
powder properties are affecting the feedstock’s rheological properties
and, as a result, the injection parameters. In order to produce defect-free
and high-quality parts, the rheological properties of the feedstock need
to be analyzed, and the injection parameters need to be optimized.
Therefore, In this study, the rheological properties of a wax-based
Fe–2Ni–2Cu feedstock have been analyzed comprehensively for the
first time, and the injection parameters for this feedstock have been
optimized using the Taguchi method.

2. Theoretical and experimental procedures

2.1. Theoretical methods

2.1.1. General moldability index

Fig. 4. Association of the viscosity and shear rate of feedstock at different
temperatures.
The decreasing trend of a typical PIM feedstock viscosity with
increasing the shear rate represents time-dependent and non-Newtonian
feedstock behavior, identified as pseudo-plastic (shear-thinning).
Pseudo-plastic behavior in PIM feedstock can help the powder particles,
and binder system molecules match their direction towards the feed­
stock flow and prevent powder-binder segregation during the injection

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A. Askari and V. Momeni Materials Chemistry and Physics 271 (2021) 124926

Fig. 6. The process window of injection molding for injection speed and injection temperature.

Fig. 7. Injection defects in the green parts manufactured to obtain process window of injection molding. (For interpretation of the references to colour in this figure
legend, the reader is referred to the Web version of this article.)

stage [30,31].
Moldability index is a general indicator of a feedstock’s rheological
properties and is a function of viscosity, the sensitivity of viscosity to the
temperature, and shear rate sensitivity of feedstock viscosity. Mold­
ability index defined as [32]:
⃒ ⃒
⃒∂log η⃒
⃒ ⃒
1 ⃒ ∂log γ ⃒
αstv = ∂log η
(1)
η0 ∂(1/T)

In the Moldability index equation, Ƞ is viscosity, and Ƞ0 is the

Fig. 8. Injected parts in the temperature range of 150–170 ◦ C and injection
speed of 20–60 mm/s.
reference viscosity and temperature at a constant shear rate. Moreover, v
represents the feedstock viscosity, and t and s refer to the temperature
sensitivity and shear sensitivity of feedstock viscosity, which will
describe in the following. It is well-known that a lower value of Ƞ is more
desirable for the injection of feedstock [33]. A simplified form of the
Moldability index equation is shown in equation (2):
1 |n − 1|
αstv = (2)
η0 E/R

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A. Askari and V. Momeni Materials Chemistry and Physics 271 (2021) 124926

Table 6
Experimental design using the Taguchi.
Test Number Factor 1 Factor 2 Factor 3 Factor 4 Response 1 Response 2
Injection Speed (mm/s) Injection Temperature (◦ C) Mold Temperature (◦ C) Holding Pressure (MPa) Density (g/cm3) Flexural Strength (MPa)

1 60 170 50 100 4.81 63.71

2 60 150 60 300 4.47 56.62
3 40 160 60 100 4.31 54.11
4 20 150 40 100 3.35 37.64
5 40 150 50 500 4.059 49.13
6 60 160 40 500 4.89 65.4
7 40 170 40 300 4.08 49.75
8 20 160 50 300 4.1 50.06
9 20 170 60 500 3.83 45.18

Fig. 9. The effects of injection parameters on the density of the injected parts.

It should be noted that the feedstock having higher values of mold­ which is the linearized form of:
ability index have more appropriate and stable behavior during the ( )
E
mold filling. η = η0 exp (4)
RT
2.1.2. Flow activation energy
where Ƞ0 represents the viscosity at a reference temperature as if Ƞ is the
Due to the acute effects of temperature variations on the feedstock
viscosity of feedstock. R refers to the universal gas content, E is the
viscosity during the injection, feedstock’s temperature sensitivity is a
activation energy, and T is the absolute temperature. What determines
factor that is necessary to consider during the development of feedstock.
the PIM feedstock’s temperature sensitivity in the Arrhenius Equation
The Arrhenius equation as follows correlates the temperature to the
and depends on the binder system composition is Activation Energy. The
viscosity:
big difference between thermal expansion capacity between the metal
( )
Ea 1 powder and binder system is the most crucial reason for the temperature
ln η = ln η0 + (3)
R T sensitivity of the feedstock. Herein, researchers have shown that the
high sensitivity of viscosity to the temperature is undesirable due to the

5
A. Askari and V. Momeni
Fig. 10. The effects of injection parameters on the strength flexural of green parts. (For interpretation of the references to colour in this figure legend, the reader is
referred to the Web version of this article.)
abrupt viscosity changes of feedstock during the mold filling, leading to
the crack and distortion through the molded parts [34]. Recently re­
searches in the field of PIM feedstock’s rheological properties surveyed
that both the low viscosity and low activation energy are required for a
successful mold filling, especially in the complex geometry injection
molds [14].
2.1.3. Flow behavior index
The relationship between the stress and strain in a pseudo-plastic
fluid shown as follows [31]:
τ = Kγn
where K is a constant, and γ is shear rate. The n value is a gauge to
characterizing the type of fluid so that in the case of n = 1, the fluid is
Newtonian, n˃1 refers to the dilatant fluid (shear-thickening), and n<1
is illustrative of pseudo-plastic fluid (shear-thinning). Between the
different types of fluids, an appropriate PIM feedstock should have the
pseudo-plastic behavior to provide the uniform distribution of powder
particles through the binder system. Another noteworthy point about
the effect of shear on the viscosity is that the feedstock viscosity is
affected by the shear rate and shear stress. However, further analysis
showed that the viscosity dependence of shear rate is more desirable due
to the different injection molding machines. The viscosity (Ƞ) can be
written as follows too [22]:
Materials Chemistry and Physics 271 (2021) 124926
η = Kγn− 1
(6)
The (n-1) index is the shear-sensitivity exponent, which indicates the
viscosity dependency of feedstock to the shear rate and is calculable
from the slope of logȠ vs. logγ. In general, higher values of n are more
desirable in a PIM feedstock rheological behavior due to the lower shear
rate sensitivity followed by slower viscosity decreasing with shear rate
increasing. However, it was stated that too high shear rate sensitivity is
undesirable because it can cause flashing during the molding [35]. In
vitro studies have recently shown that PIM feedstock’s viscosity in the
(5)
shear rate range of 102 to 105 s− 1 has not passed from 1000 Pa s [16].
2.2. Experimental methods
2.2.1. Materials
In this study, Fe–2Ni–2Cu powder produced by using the gas atom­
ization technique supplied by Unifine Company was used. The scanning
electron microscopy (SEM) micrograph of this powder can be seen in
Fig. 1, which has shown that the powders are near to sphere with
sphericity equal to one. It can improve the density, microstructure, and
moldability of the part during the process. Furthermore, the agglomer­
ation phenomenon has not been observed. Also, the size distribution of
powder particles was observed using the laser diffraction particle size
analyzer (HORIBA, LA-960) with the average size particles of 4.03 μm
(Fig. 2).
6
A. Askari and V. Momeni
Fig. 11. The influence of high injection temperature on powder distribution in
the green part of the sample for run 7; region with a) high concentration of
powder, b) low amount of powder.
In Table 1, the characteristics of Fe–2Ni–2Cu powder have been
shown. The pycnometer density provides a theoretical density of the
powder and can indicate issues with internal voids within a powder. Tap
density (the apparent powder density obtained under standard tapping)
and the D-values (D10, D50, and D90) are the intercepts for 10, 50, and
90% of the cumulative mass.
Usually, the range of Sw for metal injection molding powder particles
lies between 2 and 7. A lower value of Sw shows a broader range of
particle size, which results in a more comfortable injection during the
process, while a higher value of Sw results in a part having a low density
[36]. The powder used in this study has the Sw of 4.69, which is an
optimal value for metal injection molding powder particles. Due to the
numerous advantages of wax-based binder systems in different steps of
MIM process, a wax-based binder system including polyethylene and
polypropylene as the backbone, paraffin wax as a controller of viscosity,
and stearic acid as a surfactant was used in this study [42]. The char­
acteristics of used binder system constituents in developing the
Table 7
The predicted and tested optimum values of inputs and outputs.
Factor 1 Factor 2 Factor 3
Injection Speed (mm/s) Injection Temperature (◦ C) Mold Temperature (◦ C)
Predicted 60 160 60
Tested 60 160 60
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Materials Chemistry and Physics 271 (2021) 124926
feedstock are shown in Table 2.
2.2.2. Feedstock preparation
The optimum amount of powder particles should be dispersed fully
through the binder system within a feedstock to provide a suitable
feedstock flowability. It can improve the dimensional stability of the
part while preventing local shrinkage. In order to compound the feed­
stock, a torque rheometer (Haake PolyLab QC Lab Mixer) was used to
measure the critical solids loading. The barrel temperature of 150 ◦ C,
blade rotational speed of 150 rpm for 30 min applied for the mixing
parameters. At the initial stage of mixing, the blade’s torque started to
increase with the powder’s addition to some extent, after which it
started to decrease and became stable, which is a sign of homogeneity of
the compound [37]. The critical solids loading was 60 vol%, while the
optimum amount of solids loading was considered as 58 vol% (2% lower
than critical solids loading) in order to produce easier flow. Then, to
produce the optimum feedstock, mixing by twin screw mixer (KMC-TZ)
at the temperature of 160 ◦ C was done three consecutive times.
2.2.3. Rheological behavior
Appropriate Mold filling depends on viscous flow into the die cavity,
creating assurance for producing the sound green body during the in­
jection process. It requires specific rheological characteristics and in­
dicates the importance of investigating feedstock’s flow behavior by
studying the rheological properties [14,38]. The most important prop­
erty is the viscosity, which relates the shear stress to the shear strain
rate. With this aim, a twin-bore capillary rheometer (Capillary Rheom­
eter, Rosand R&H, Malvern) having the L/D of 20 was applied to
measuring the viscosity of feedstock. To determining the effect of shear
rate and temperature as the most influential parameters on the viscosity,
melt flow index (n) and flow activation energy (E) were calculated by
varying the shear rate and temperature of feedstock. To evaluate the
fluid type, the viscosity was measured in a wide range from 100 to
10000 s− 1 until appearing the pseudo-plastic behavior [39]. After
measuring the viscosity in different shear rates, to perceive and deter­
mine feedstock’s viscosity sensitivity to the temperature, the rheological
behavior was determined in the three different temperatures of 150,
160, and 170 ◦ C around the injection temperature according to the
softening temperature of binder system components. Bagley correction
was considered during the viscosity measurement.
2.2.4. Injection molding
According to the injection experiments, the most critical parameters,
which have the greatest effects on the injection process and green bodies
produced in this step, were derived. The injection was done at the same
temperatures in which rheological experiments were done. Other
remained effective parameters, including injection speed, mold tem­
perature, and holding pressure, which have been varied until achieving
the sound green bodies in the wide ranges to achieve suitable levels in
each factor. Injection experiments were done by using a TR30EH in­
jection machine. Short shots, weld lines, and flashing were significant
defects in analyzing the process window of injection molding in this
study. Outputs were two diagrams of the process window for injection
speed with injection temperature and mold temperature with holding
pressure. In the next step, the design of experiments has been done to
optimize the injection parameters for Fe–2Ni–2Cu feedstock. This
method is a scientific approach to determine the cause and extent of the
factor on the outputs.
Factor 4 Response 1 Response 2
Holding Pressure (MPa) Density (g/cm3) Flexural Strength (MPa)
500 4.99 66.44
500 5.22 70.56
A. Askari and V. Momeni
Design-Expert software was used for designing the experiments. Each
factor was analyzed at three levels of highest (1), middle (0), and lowest
(− 1), which has been shown in Table 3.
With finding appropriate levels of factors, the Taguchi method was
applied to optimizing the parameters according to the inputs. After
injecting the feedstock using the influential factors and their levels, in­
jection parameters were evaluated using the green parts density and
flexural strength of the green three-point bending specimens. Planned
tests by the software are shown in Table 4. As it can be observed, overall,
there are nine experiments to be conducted.
3. Results and discussion
3.1. Determination of critical solids loading
The mean torque is shown for each solids loading between 56 and 64
vol% in Fig. 3. Obviously, the mean torque value linearly increased until
60 vol%, while linear behavior changed with a slope changing after this
critical value. This break shows that the binder system is not sufficient,
and the friction increased between excess amounts of powder particles
in the feedstock [43]. Generally, the optimal solids loading considers
being 2–5% lower than critical solids loading to provide stability for
feedstock’s rheological behavior.
3.2. General moldability index
As it was discussed, the general moldability index value depends on
the viscosity and its sensitivity to the temperature and shear rate; its
need to calculate these two factors in the developed feedstock. So, before
calculating the Moldability index (αstv ) for developed feedstock, it needs
to evaluate the flow behavior index (n) and flow activation energy (E).
Viscosity decreasing of the feedstock with increasing the shear rate in
Fig. 4, indicating the existing shear-thinning or pseudo-plastic behavior
of the feedstock. This characteristic makes powder particles and binder
system molecules direction same and towards the flow of feedstock [30].
There is a limitation for feedstock viscosity in the shear rates of 102 to
105 s− 1 to desirable mold filling at the operational molding temperature,
which should remain under 1000 Pa s [40]. A suitable linear fit of R2
(between 0.97 and 0.99) to the power-law or Ostwald de model (Eq. (5))
is evident in Fig. 4. Whatever lower value of n, higher shear rate
sensitivity, and faster viscosity decreasing with shear rate increasing.
Too low or too high (n-1) values are undesirable both. Besides, it has
been reported that lower values of Ƞ are more desirable for injection of
feedstock [41]. The slope of linear curves in Fig. 4 leads to calculating
the flow behavior index value shown in Table 5. The n-values in three
temperatures lower than one and the small variations of n-values in
different temperatures indicate pseudo-plastic behavior and suitability
of the MIM feedstock.
The second variable, which the general moldability index depends
on, is the flow activation energy as an indicator of feedstock’s temper­
ature sensitivity. The flow activation energy for the developed feedstock
is calculated from the slope of lnȠ (viscosity) vs. 1/RT (temperature)
graph and showed in Fig. 5. As it can be observed, it has an admirable fit
to the Arrhenius equation with the R2 value of ˃0.98 (Table 5). What­
ever more sensitivity of feedstock to the temperature, feedstock viscosity
will be unstable during mold filling due to the sudden viscosity changes.
This matter will be more critical when the feedstock will be immediately
cold to meet the inner wall of the mold.
Finally, the general moldability index (αstv ) was calculated according
to the results of the flow behavior index (n) and flow activation energy
(E), which are shown in Table 5. As it can be observed, the moldability
index of the developed feedstock in this study showing the value of
3.1302E-06 Pa− 1 K− 1, which is upper than the study of Askari et al. [14],
where they used the same wax-based binder system. This shows more
successive mold filling of present feedstock during the injection.
8
Materials Chemistry and Physics 271 (2021) 124926
3.3. Process window and injection defects
Injection molding defects in the MIM process can be apparent
directly after molding, or they may not manifest themselves until after
subsequent process steps. Molding is a multi-variable process where the
variables are heavily interactive; thus, there are multiple ways to solve a
problem. Also, the solution to one issue can cause defects of a different
form.
Fig. 6 shows one of the diagrams for the process window. As can be
seen, the experiments performed at a low injection speed of 10 mm/s
with injection temperatures 140 and 150 ◦ C have had severe defects,
such as a short shot. Before the complete filling of the mold, this defect
can reduce the capacity to flow, leading to incomplete solidification of
the melt feedstock. With the increase in injection temperature, the mold
was filled but with noticeable weld lines. At the low injection speed, the
cavity filling stage takes significant time and makes a suitable condition
for forming weld lines due to a non-uniformed cooling stage. Also, it can
be found out that the high injection temperature of 180 ◦ C causes blis­
tering and burn marks, and even in some samples, the evaporation of
binder constituents occurred. Some injection defects in the manufac­
tured green parts have been shown in Fig. 7.
On the contrary, a very low melt temperature of 140 ◦ C can lead to
incomplete mold filling because of the cool feedstock. As it can be
concluded that from Table 2, 140 ◦ C is near the melt temperature for PE
and PP. In this condition, with the increase of injection speed, the defects
in green parts appear as sink and flow marks. The high speed of injection
generates serious flash. Removing flash is costly, and this defect can
destroy one of the essential benefits of injection molding, which is cost-
efficient. Reducing the injection speed from 80 to 70 mm/s provides
lower defects, but voids were inevitable. Under the circumstance, there
were voids in all temperatures; only they were confronted with varying
sizes, which with increasing the melt temperature, the size of voids was
lessened. The process window of injection molding has shown that all
the green parts are of good quality in the range of injection temperature
150–170 ◦ C and injection speed 20–60 mm/s. The green parts are shown
in Fig. 8.
When a high holding pressure is applied, flash usually occurs, while
the low amount can leave low green density areas and incomplete filling
in the injected parts. Weld lines and flow marks are caused by low
feedstock temperatures and low mold temperatures (Fig. 7). Even
because of the high differences between the melt feedstock and low
mold temperature, crack forming is unavoidable. On the other hand,
exceeding a specific mold temperature can cause sink marks. The reason
for that is the increase of binder constituent’s volume when the feed­
stock enters the cavity. With this expansion, the lower amount of powder
could be injected into the mold, which leads to low density and sink
marks on the green parts.
3.4. Optimization of injection parameters
After measuring the sample’s density and flexural strength, the re­
sults (Table 6) were entered into the design-expert software after which,
the relation between input parameters and output properties was
investigated. Green flexural strengths obtained through a three-point
bending test by a universal testing machine (RB Model301 UNITECH)
are listed in Table 6. The highest green strength was observed to be 65.4
MPa for the sample of run 6. As can be seen from Table 6, run 6 has
shown the highest density too, with a value of 4.89 g/cm3 measured by
Archimedes density meter (Mettler Toledo XP205). The effect of injec­
tion parameters on the density and flexural strength has been shown in
Figs. 9 and 10.
All parts were produced with high quality by injection speeds in this
range regarding the process window. However, the variation of injection
speed can cause many different defects that some of them have a sig­
nificant impact on the mechanical properties of green parts, even though
the defects such as flow lines are not visible significantly. The effects of
A. Askari and V. Momeni
injection speed on density and flexural strength of green parts are shown
in Figs. 9 and 10. In this study, the complete filling of the cavity was
conductible in lower injection and mold temperatures, which improved
the injected part’s properties. Injection speed behaves similarly to both
outputs. Density and flexural strength increased by increasing injection
speed from 20 to 40 mm/s. In the present study, the highest density and
flexural strength were obtained using the injection speed of 60 mm/s. As
shown in Figs. 9 and 10, the increase rate is higher for 40–60 mm/s due
to decreasing possibilities in forming flow lines in the high injection
speeds.
The influence of injection temperature on density and flexural
strength was investigated (Figs. 9 and 10). This parameter can vary the
properties to a significant extent. Injection temperature is having a dual
impact (positive and negative) on an injected part’s properties. On the
one hand, the increase in injection temperature increases density and
flexural strength because using higher temperature provides more time
to exert higher holding pressure and time. On the other hand, it can
cause the expansion of polymeric constituents in the feedstock and
change powder particle’s distribution while decreasing part’s proper­
ties, particularly flexural strength. It can be observed that an increase in
the injection temperature from 150 to 160 ◦ C increases density and
flexural strength. Figs. 9 and 10 indicate that higher temperatures lead
to lower properties to some extent. It can be concluded that there is an
optimum amount of injection temperature for this study. As the results
have shown, increasing injection temperature has a greater impact on
the strength than density. It can be explained by this fact that the effect
of injection temperature on the expansion is high, but because of high
pressure during the injection, this parameter cannot be influential in the
changing powder loading of the injected feedstock significantly. How­
ever, this expansion exerts a change in powder distribution, leading to
more alteration in flexural strength than density. The powder particle’s
distribution for the sample of run 7 has been shown in Fig. 11.a and 11.b.
From Fig. 11.a and 11.b, it can be observed that the high injection
temperature can be an influential factor to change the amount of powder
in some regions of injected parts. At high injection temperatures, the
constituents of the binder system are subjected to an expansion, and it
can result in lower powder concentration in the regions which are filled
at the first stages of filling. However, holding pressure can compensate
for it to a certain extent, but the farthermost areas from the gate in the
injected parts can experience the lack of powder loading rather than the
near regions to the gate. In this study, the density and particle distri­
bution were improved from the two end sides of the parts to the center
because the gate for the injection process was placed in the middle of the
parts.
As can be seen, there is a slight improvement in the density and
strength of the part with the increase in the holding pressure from 100 to
300 MPa, then approximately constant in 300 MPa–500 MPa (Figs. 9
and 10). In fact, the crucial role of holding pressure is in determining the
process window to prevent substantial defects. In this range of holding
pressure investigated for this study, any remarkable variation in the
properties of the green part has not been seen.
Mold temperature behaves as an influential factor in producing high-
quality parts that cannot be injected in high pressure or temperatures.
Another important aspect of this parameter is that it is effective for
injecting sensitive materials to high temperatures. A low mold temper­
ature results in some defects because the injected feedstock was con­
fronted with high viscosity at the beginning of mold filling. In contrast,
with an increase in mold temperature, a slight expansion of the binder
system’s components can occur, leading to a lower amount of powder in
the cavity. In this study, the parts with high density and strength were
manufactured using a mold temperature of 50 ◦ C instead of 40 ◦ C. More
temperature increase can provide a proper situation to lessen density
and flexural strength due to low powder loading.
The optimum injection parameters with their outputs predicted by
the software are shown in Table 7. Additional experiments were done
three times using optimum injection temperature, injection speed, mold
9
Materials Chemistry and Physics 271 (2021) 124926
temperature, and holding pressure to confirm the results. The error
between the results of the confirmation experiment and predicted values
was found to be 4.7% for density and 6.2% for flexural strength.
Therefore, the optimized results can be considered reliable for the MIM
process.
4. Conclusion
In this study, the rheological properties and injection parameters,
and defects in the metal injection molding of Fe–2Ni–2Cu feedstock
were investigated. An optimized wax-based binder system was suc­
cessfully applied to develop the feedstock. The proper solids loading was
selected as 58 vol% which is slightly lower than critical solids loading in
order to provide smooth and stable feedstock flow during the mold
filling. Measuring the viscosity in different temperatures and shear rates
showed the pseudo-plastic behavior, which is desirable for PIM feed­
stock. Calculated n-values showed lower than one values, and also low
sensitivity of the feedstock viscosity to the shear rate showed a high
general moldability index, which indicates that feedstock is injectable
without any problem and the results can guarantee producing the defect-
free green bodies. After ensuring the desirability of the developed
feedstock, it’s time to investigating the injection parameters in order to
identify and selecting the suitable factors and their levels; why so these
two steps tied together, and one is useless without considering the other
one. It is observed that the injection parameters like injection speed,
injection temperature, mold temperature, and holding pressure can
affect the physical and mechanical properties of the green parts signif­
icantly. Making the process window for the injection process shows that
there is only a limit range for each parameter in order to prevent defects
in the metal injection molding of each feedstock. It can be concluded
that even in a suitable range, injection parameter’s influences differ
from each other. The RSM analysis results represent that the impact of
injection speed is more than other parameters, and high injection speed
can cause detrimental defects such as large voids or flash. However, the
holding pressure approximately shows little effect on the properties of
the output. On the contrary, the increase of injection temperature can
lead to an unbalanced distribution between powder particles and the
binder system, which is considered a pivotal factor in decreasing the
density and flexural strength. As can be seen from the results, the opti­
mum point for the injection temperature and mold temperature proves
the dual impacts of these parameters on the mechanical properties.
Declaration of competing interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
the work reported in this paper.
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