Materials Today: Proceedings xxx (xxxx) xxx

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Materials Today: Proceedings

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Sintering parameters consequence on microstructure and hardness

of copper alloy prepared by powder metallurgy
B. Deepanraj a, N. Senthilkumar b,⇑, T. Tamizharasan c
a
Department of Mechanical Engineering, Jyothi Engineering College, Thrissur, Kerala, India
b
Saveetha School of Engineering, Saveetha Institute of Medical and Technical Sciences, Chennai, India
c
SRM Technologies Pvt. Ltd, Chennai, Tamil Nadu, India

a r t i c l e i n f o a b s t r a c t

Article history: In this technical world, the properties and internal structure of materials renders a vital part in building
Available online xxxx up of the components for various specific purposes and improvise their efficiencies in a better way. The
combination of copper with other metals is always an interesting one. In this, brass of grade BS90 is an
Keywords: alloy of zinc added with copper and it is lustrous in nature. The amount of zinc that is mixed with copper
Copper Alloy can be varied to develop different categories of brass with different melting temperatures that develops
Brass distinct electrical and mechanical potency. In the process of better understanding of the powder metal-
BS90
lurgy technique and analyzing and improvising the properties of brass, this research is carried out.
Powder Metallurgy
Binder
Primarily, this process is carried out based on the powder metallurgy technique. The prime intention
Poly-vinyl alcohol of this investigation is to develop and process the specimens under predetermined conditions of powder
metallurgy and then their mechanical hardness and the microstructure are to be characterized. The sec-
ondary objective is to analyze these characteristic values and compare them relatively to the specified
conditions.
Ó 2021 Elsevier Ltd. All rights reserved.
Selection and peer-review under responsibility of the scientific committee of the International Confer-
ence on Nanoelectronics, Nanophotonics, Nanomaterials, Nanobioscience & Nanotechnology.

1. Introduction By adding with different metals, the properties of brass can be

Powder metallurgy (PM), one of the earliest technologies is
found increasing application allowing close control of tolerances,
low scrap losses, complex shape designs, and good reproducibility
[1]. The advent of improved atomization techniques for complex
alloys has allowed the metallurgical advantages of powder pro-
cessing over conventional casting and ingot-conversion techniques
due to rapid cooling rate observed in a small metal particle as com-
pared to that in an ingot [2]. In PM, uniformity and homogeneity of
the microstructure that lends to the powder product desirable
mechanical properties with a high degree of reproducibility [3].
Copper and copper alloy powders have been used in industrial
applications for many years due to high degree of ductility and
toughness at subzero temperatures [4]. Brass could be a metal
alloy with a mix of copper and zinc. By changing the quantity of
copper and zinc, the softer and harder types of brass can be
prepared.
⇑ Corresponding author.
E-mail address: nskmfg@gmail.com (N. Senthilkumar).
changed. It will become yellower, stronger, softer, harder, or high
corrosion-resistant, relying upon its chemical composition. With
increase in zinc content, the strength and malleability of these
alloys increases. Bronze is a copper-based alloy with a tin content
of around 12%. The alpha primary solid solution of tin in copper is
what gives bronze its color. 4–5 percent tin bronze alloys are
employed to create springs, blades, turbines and coins [5]. Bronzes
are typically very ductile alloys. Bronze is a better conductor of
electricity and heat than most steels. Brasses are utilized in appli-
cations like coining, blanking, piercing, drawing, fire extinguishers,
springs, jewelry, lamp fixtures, radiator cores, ammunition, flexible
hose, and the base for gold plate.
Ruzic et al. [6] adopted powder metallurgy process and hard-
ened copper and it alloys and formed various dispersoids deliber-
ated combined and single effect on strengthening mechanism at
elevated and room temperature and identified that by thermal
aging Cu-Ti compact can be strengthened due to the formation of
precipitation and modular structure of Cu4Ti(m). Wong-Angel
et al. [7] improved the mechanical strength of alloy with a compo-
sition of 0.3 wt% Mo, 0.6 wt% C, 0.7 wt% Mn and 1 wt% Ni and of Fe

https://doi.org/10.1016/j.matpr.2021.06.389
2214-7853/Ó 2021 Elsevier Ltd. All rights reserved.
Selection and peer-review under responsibility of the scientific committee of the International Conference on Nanoelectronics, Nanophotonics, Nanomaterials,
Nanobioscience & Nanotechnology.

Please cite this article as: B. Deepanraj, N. Senthilkumar and T. Tamizharasan, Sintering parameters consequence on microstructure and hardness of copper
alloy prepared by powder metallurgy, Materials Today: Proceedings, https://doi.org/10.1016/j.matpr.2021.06.389
B. Deepanraj, N. Senthilkumar and T. Tamizharasan
containing Cu by 8 wt% and found that doping with Cu improves
density and toughness and reduces porosity during the process
of sintering where a liquid phase forms and fills the spaces among
the binding particles. Wen et al. [8] evaluated the suitability of
alloy Cu-Sn-Pb with similar microstructure and composition pro-
duced by powder metallurgy for artifacts and found a phases, lead
phases and (a + d) phases, and in BZ-4 bronze alloy are formed in
the alloys. Furthermore, the amount of (a + d) phase in Cu-Sn alloys
increases as the tin content increases. Dovydenkova and Radomy-
sel’skii [9] reduced the porosity less than 3–5% achieved by
employing high-energy methods of densification, in particular
hot and cold forging of constructional copper alloy parts. For best
results, parts from a-brass powders should be produced by cold
forging and those a + b-brasses by hot forging with a zinc content
of 32–38%. Zhan et al. [10] used powder metallurgy and a hot
extrusion method to fabricate an innovative Cu–Cr–Zr alloy com-
posite strengthened with particles of Al2O3 to acquire combined
influence of reinforcements and aging related strength and identi-
fied that aging process is accelerated through Al2O3 addition. Ulti-
mate strength and hardness at higher temperatures were
enhanced effectively by increasing Al2O3 concentration. Church
et al. [11] investigated the grain size, elongation, density, yield
and tensile strength and thermal conductivity of Cu, Cu–Ag, Cu–
Al2O3, Cu–Ni, Cu-Cr, Cu-Invar and W–Cu and analyzed the out-
comes through alloy composition and porosity made through con-
ventional processing and powder metallurgy and found that
powder of metal oxide are used for developing structures of honey-
comb with similar properties in connection with conventional
powders. Price and Oakley [12] produced tin bronze by 90/10 by
powder compaction with 7.4 g/cm3 density to attain explicit prop-
erties as per requirements and acknowledged that incompletely
pre-alloyed powder removes any separation hazard and longer
time of sintering reduces these advantages. Selvakumar et al.
[13] studied the performance of pure aluminium alloy matrix rein-
forced with 4% copper and varying reinforcements of silicon car-
bide particles prepared by powder metallurgy, with increasing
percentage of SiC mechanical and wear properties improved, but
is restricted to 7.5% above which bonding strength decreases which
reduces the strength of composite.
In this work, BS90 brass alloy of copper, zinc and aluminium is
taken in powder form and formed in to specimens fabricated using
powder metallurgy route considering different sintering tempera-
ture, soaking time and binders and the best combination is identi-
fied for better microstructure and hardness.
2. Materials and methods
In this work, materials used are commercially available high
purity brass powder of grade BS90. Chemical analysis of BS90 pow-
der shows elemental composition of copper as 90%, zinc as 9.5%
and aluminium as 0.5%. BS90 powder is purchased from The Metal
Powder Company Limited, Sivakasi, TamilNadu, India. The specific
applications of BS90 are as adhesives, abrasives, chemicals, auto-
mobile parts, brake linings, diamond tools, space & aeronautics,
medicines, sintering parts, powder metallurgy parts, watch compo-
nents, etc. The scanning electron microscope (SEM) image of BS90
is given in Fig. 1.
The brass of grade BS90 is stable when it is dry and no decom-
position occurs, it can be mixed up with the binder and the wetting
agents under normal conditions. Three samples were fabricated.
For first and second samples, the binder added was Poly Vinyl Alco-
hol (PVA). The binder of 0.5% of the total weight of the specimen is
added. The addition of binder is just to bond the particles together
temporarily on compression and so it will be ready for sintering.
This binder will get evaporated around 207 °C during the sintering
2
Materials Today: Proceedings xxx (xxxx) xxx
Fig. 1. SEM of BS90 alloy.
process. For sample 3, water is added by 0.5% as a wetting agent
instead of adding PVA. It also helps the particle to be together on
compression and so the specimen will be ready for sintering.
Powder Metallurgy (PM) route was adopted to fabricate the
specimens with different wetting agents, the procedure followed
is: weighing, mixing, compacting, sintering and cooling [14]. The
process of powder compaction plays an important role in the final
properties of the specimen. A hydraulic pressing machine of 10 Ton
capacity was used to press the tool-steel die mechanically, in
which the powder alloy is present [15,16]. There will not any dif-
ferent in densities over the specimen, since the powder is com-
pacted under uniform pressure by the hydraulic press. Fig. 2
presents the PM route adopted for fabricating the samples.
The sintering procedure followed for preparation of PM samples are:
a. Sample 1: The compacted sample is processed in a normal
atmosphere furnace at a temperature of 850 °C and soaking
time as 45 min. The temperature rises at a rate of 5 °C/min-
ute. The sample is placed at the center of the heating zone
inside the furnace.
b. Sample 2: The compacted sample is processed under con-
trolled atmosphere with argon gas. The temperature kept
was 950 °C and the soaking time as 60 min. The temperature
constantly rises at a rate of 5 °C/minute.
c. Sample 3: The compacted sample is processed under con-
trolled atmosphere with argon gas. The temperature kept
was 975 °C and the soaking temperature as 60 min. The tem-
perature is raised at a constant rate 5 °C/minute.
All the three specimens were cooled after reaching their speci-
fied temperatures and with stipulated soaking time within the fur-
nace. Then the specimens are taken out of the furnace and the
physical appearances of the specimens are checked out. Table 1
provides the details of fabrication considered during sample prepa-
ration by PM technique. Insert atmosphere is used to avoid oxi-
dization of sample during sintering process [17]. Fig. 3 provides
the details of heating and soaking time of PM samples.
The method adopted for determining the hardness of the fabri-
cated samples is Vickers hardness test procedure as per ASTM E92
[18]. The Vickers test is often easier to use than other hardness
tests since the required calculations are independent of the size
of the indenter, and the indenter can be used for all materials irre-
spective of hardness. The Vickers hardness test is an indentation
hardness test in which a square-based diamond pyramid, having
an angle of 136° between the opposite faces at the vertex, is forced
B. Deepanraj, N. Senthilkumar and T. Tamizharasan Materials Today: Proceedings xxx (xxxx) xxx

Fig. 2. Procedure followed in PM route.

Table 1
Specimens and Conditions. micrographs and the effect of binder material, sintering tempera-
ture and soaking temperature are evaluated. Fig. 5 shows the sin-
Condition Sample 1 Sample 2 Sample 3
tered specimens subjected to examination.
Temperature (°C) 875 950 975 The samples prepared are subjected to optical microscopic
Soaking Time (min) 45 60 60
examination, for which the surface of the sample is cleaned to
Wetting Agent (0.5%) PVA PVA Water
Type of Atmosphere Normal Argon Argon
remove the unwanted foreign particles. Then the surfaces are pol-
ished and made smooth without any irregularities on the surface.
Without preparation of the samples, the tests cannot be carried
out and the results will not be accurate. Optical microscope image
is acquired to identify grain structure, boundaries, size and internal
defects that affects the mechanical behaviour [20,21]
Fig. 6 displays the optical microstructure of sample 1 captured
in 100X and 200X magnification etched with potassium dichro-
mate solution acidified and are compact treated at 875 °C. 100X
magnification image shows the microstructure shows large grains
of copper fused which are evenly sintered and the presence of
pores is lower, the distribution is even. Images captured at 200X
shows that the grains are resolved further and the grains are
observed in between the grains of copper solid solution. The grains
are held by the copper grains by fusion with neighboring matrix.
Fig. 7 displays the optical microstructure of sample 2 captured
in 100X and 200X etched with potassium dichromate solution
acidified and compact treated at 950 °C. 100X magnification image
shows large grains of copper fused with particles which are present
as large clusters. These clusters are trapped by the fused copper
Fig. 3. Sintering time vs temperature graph. grains. No presence of pores is observed in the field. The distribu-
tion of composite particles is uneven and formation of dendrite
in to the surface of a test piece and the length of the diagonals of structure is seen. But second image shows uniform grains of copper
the indentation left in the surface after removal of the test force phase with uniform distribution of the composite particles. At
is measured [19]. The unit of hardness given by the test is known 200X magnification, the grains are resolved further and the parti-
as the Vickers Pyramid Number (HV) or Diamond Pyramid Hard- cles are observed in between the grains of copper solid solution.
ness (DPH). Fig. 4 shows the schematic illustration of hardness The matrix also showed the presence of pores between grains. Last
measurement. The equation to find the Vickers hardness through image shows the grain boundary trapped particles around copper
the load applied and by the dent is as follows, sintered and fused grains. The particles are held by the copper
grains in the matrix.
P Fig. 8 displays the optical microstructure of sample 3 captured
HV ¼ 1:854 2
ð1Þ
d in 100X and 200X etched with potassium dichromate solution
acidified and compact treated at 975 °C. The microstructure shows
where P is the load in Newton and d is the average of two
uniform grains of copper effectively undergone fusion. All the
diagonals.
grains are uniform in sizes and no pores between the grains
observed. The compacting pressures has resulted in reducing the
3. Result and discussion pores in the matrix. It appears high temperature resulted in good
fusion and cooled from the temperature resulted in producing uni-
The PM fabricated specimens are examined to identify grain form grains without the presence of pores. At 100X magnification
structure, grain boundary and for any defects through optical both the images are identical even though the fields are different.
3
B. Deepanraj, N. Senthilkumar and T. Tamizharasan Materials Today: Proceedings xxx (xxxx) xxx

Fig. 4. Vickers hardness test method [18]

At 200X the grains are resolved further and some particles are
observed in between the grains of copper solid solution but they
are low in distribution. The matrix also showed freedom from
the presence of pores between grains. Last image shows the grain
boundary trapped particles around copper sintered and fused
grains. The particles are held by the copper grains in the matrix.
Vickers hardness test is used to measure the hardness of the
specimens. The three samples undergone for three trails each to
get the precise hardness values of the specimens processed under
different conditions. The dwell was kept as 10s at 0.5 kg of load.
Table 2 displays the hardness values obtained for all samples.
Observation made from the hardness values from Table 2 and
comparison from Fig. 9 show that with higher soaking time better
hardness is obtained. When compared with water, PVA binder pro-
duces higher hardness. Maximum hardness is attained with higher
soaking time and PVA as binder. The hardness value obtained can
be correlated with the microstructure of the PM samples that are
Fig. 5. Sintered specimens.

Fig. 6. Microstructures of sample 1.

4
B. Deepanraj, N. Senthilkumar and T. Tamizharasan Materials Today: Proceedings xxx (xxxx) xxx

Fig. 7. Microstructure of sample 2.

Fig. 8. Microstructure of sample 3.

5
B. Deepanraj, N. Senthilkumar and T. Tamizharasan
Table 2
Vickers hardness test values of the specimens.
Hardness Sample 1 Sample 2 Sample 3
Trial 1 96.9 107.7 99.5
Trial 2 97.4 107.1 102.5
Trial 3 95.8 104.3 101.3
Average (HV) 96.7 106.36 101.1
Fig. 9. Specimens’ hardness values.
characterized by uniform distribution of alloying particles and par-
ticles getting precipitated at grain boundaries and the copper pow-
ders are fused due to proper sintering.
4. Conclusion
Influence of sintering temperature, soaking time and type of
binder is studied in this work during the preparation of three dif-
ferent samples through powder metallurgy (PM) route. Brass of
grade BS90 is considered as the alloying powder and after prepara-
tion the samples are characterized through microstructure and
hardness. The outcomes of this study are:
1. The sintering temperature, soaking time, binding agent and
density played an important role this work, sintering tempera-
tures and the soaking time are maintained as 875 °C, 950 °C,
975 °C and 45, 60, 60 min respectively.
2. The binders that were added to the first two specimens is PVA
and water as a wetting agent for the third one and the sintering
was done in the normal and controlled atmosphere with argon
gas. It is notified that the addition of binder had no role to affect
the properties of the brass alloy.
3. The highest hardness values of the sample 1, 2 and 3 are 96.7
HV, 106.36 HV and 101.1 HV respectively and is observed that
the second specimen has the highest hardness and has dendrite
structure than the other two samples.
4. Sample 3 processed with water as a wetting agent has a very
good powder metallurgical grain structure and it possess the
moderate hardness among the three specimens.
5. On the flipside, sample 1 has good hardness and a descent grain
structure. So, it can be concluded that the brass of grade BS90
could possess a good hardness and a good grain structure when
processed at 875 °C and water as wetting agent with 60 min
soaking time in inert atmosphere.
Materials Today: Proceedings xxx (xxxx) xxx
Declaration of Competing Interest
The authors declare that they have no known competing finan-
cial interests or personal relationships that could have appeared
to influence the work reported in this paper.
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