Powder Metallurgy Routes for Composite Materials Production

Debasis Chaira, National Institute of Technology Rourkela, Odisha, India

r 2021 Elsevier Inc. All rights reserved.

Nomenclature MMC Metal matrix composite

AFF Accumulative fold forging ODS Oxide dispersion strengthened
BPR Ball to powder weight ratio PM Powder metallurgy
CIP Cold isostatic pressing PMC Polymer matrix composite
CMC Ceramic matrix composite SHS Self propagating high temperature synthesis
CNT Carbon nanotube SPD Severe plastic deformation
FGM Functionally graded material SPS Spark plasma sintering
HIP Hot isostatic pressing TD Theoretical density
HP Hot pressing UFG Ultra fine grained
LPS Liquid phase sintering

Introduction

Modern technologies require materials with unusual combinations of properties that cannot be met by the conventional metals,
alloys, ceramics and polymeric materials. This is especially true for materials that are used in critical applications like aerospace, high
temperature, underwater/corrosive environments and transportation applications. For such applications, there is a need of special
materials that exhibit better combinations of individual properties. A composite is that special material and considered to be a
multiphase material that exhibits a significant proportion of the properties of both constituent phases and have distinct interface
between the constituent phases. The composite materials constitute matrix and the reinforcement materials. The matrix phase is
generally soft which holds the reinforcement materials, whereas reinforcements are hard and brittle phase. The matrix phase transfers
the load from matrix to reinforcement, whereas reinforcement mainly bears the load of the composite. Depending on the nature of
the matrix and reinforcement phase, composite materials are categorized as metal matrix composite (MMC), ceramic matrix com-
posite (CMC) and polymer matrix composite (PMC). The reinforcement phase can be either particulate form or fiber form.
There are various fabrication methods available to manufacture the composite materials. Among them, powder metallurgy is
unique manufacturing method as it has the ability to fabricate high quality, complex parts to close tolerances in an economical
manner. Powder metallurgy is the study of the processing of metal powders, including the fabrication, characterization, and
conversion of metal powders into useful engineering components. It is a flexible manufacturing process capable of delivering a
wide range of new materials, microstructure and properties. Fig. 1 shows the conceptual flow chart for powder metallurgy from the
powder through the processing to the final product.
The applications of powder metallurgy are versatile since unique property or microstructure can be achieved using P/M approaches.
Some examples include porous materials, oxide dispersion strengthened alloys (ODS), cermet (ceramic-metal composites), cemented
carbide and biomaterials. The manufacturing of reactive and refractory metals and amorphous or glassy metals are quite difficult to
process by other techniques. Powder metallurgy is the only process by which these materials can be manufactured. This process wins the
cost competitions on the basis of its lower energy consumption, higher material utilization and reduced number of process steps, in
comparison with other production technologies. It is also possible to eliminate machining operations completely in PM processing but
that step is essential in other conventional manufacturing processes. It also has the abilities to form complex geometrical shapes directly
to hold close dimensional tolerance control in the sintered product. Fig. 2 shows the basic processes involved in powder metallurgy. The
key steps include powder production, blending/mixing powder, compaction and sintering of compact.

Powder Manufacturing Methods

The formation of powder involves the delivery of energy to the material to create new surface area. There are four methods by
which powders are prepared. The methods are-

(1) Mechanical fabrication technique

(2) Electrolytic fabrication technique
(3) Chemical reduction technique
(4) Atomization technique
(1) Mechanical fabrication technique – The four fundamental mechanical comminution methods: impaction, attritioning,
shearing and compression are involved during fabrication of powder by mechanical fabrication technique. The basic
comminution techniques used for powder production are-

Encyclopedia of Materials: Composites doi:10.1016/B978-0-12-803581-8.11703-5 1

2 Powder Metallurgy Routes for Composite Materials Production

Fig. 1 The conceptual flow chart for powder metallurgy from the powder through the processing to the final product.

Fig. 2 Basic processes involved in powder metallurgy.

(a) Machining – Machining of ingot during metal working processes generate powder. A large amount of scraps are generated and
powder can be produced by grinding these scraps. The powder produced is coarse and lack of control on powder char-
acteristics is major drawback of machining. Moreover, contamination of oxygen, oil and other metal is major disadvantage of
machining technique for producing powder.
(b) Milling and Mechanical alloying – Impacting and attritioning of powder/scraps using balls in a jar is another source of
producing powder. During milling process, alloying of two or more elements can be done and is termed as mechanical
alloying. Both milling/mechanical alloying is a complex phenomenon, as these involve with several parameters. The
parameters are as follows:
(i) Milling speed
(ii) Ball to powder weight ratio (BPR)
(iii) Vial filling
(iv) Temperature of milling
(v) Milling atmosphere
(vi) Wet/dry grinding
(vii) Use of surfactant
(viii) Contamination problem
The details of the effect of milling parameters during grinding effect are available (Suryanarayana, 2001; Chaira and Karak, 2015).
Ball mill, planetary mill, attritor mill, jar mill etc., are used as milling devices during milling and mechanical alloying. The
contamination is a major problem in milling technique. The synthesis of powder not only depends on the various milling parameters
 Powder Metallurgy Routes for Composite Materials Production 3

but also on the nature of material. The brittle materials are easily converted into powder by fracture, whereas ductile materials are
initially plastically deformed. In later stage, ductile materials are work hardened, become brittle and finally fractured into powder.
(2) Electrolytic fabrication technique – The raw metal is dissolved at the anode and deposited at the cathode in an electrolytic cell
under certain operating conditions. The main advantage of this technique is ability to produce high purity powder. Powder
formed by this technique is dendritic or sponge in shape, although particle size and shape can be controlled. The powders of
Pd, Cu, Ni Z, Mn and Ag can be produced by this technique.
(3) Chemical reduction technique – In this technique a metal oxide is reduced by reducing gases (CO, H2) at suitable temperature
and pressure and metal powder is produced. Oxides of Fe, W and Cu are reduced by reducing gases and powders are produced
by this technique. The particles size and shape varies depending on the reduction parameters like gas composition, temperature,
gas partial pressure and reaction kinetics. The powder produced by this technique generally exhibit poor flowability and packing
characteristics.
(4) Atomization technique – Powder is produced commercially and at very high rates as high as 400 kg/min. This technique
involves the formation of powder from molten metals or alloys using a spray of droplets. Powder is produced by three
atomization techniques-
(a) Gas atomization – high velocity gases (air, N2, Ar or He) exit from a nozzle break up a molten metal stream into finely
divided liquid droplets which finally solidify and form metal powder. The melt must be superheated over the melting
temperature. The designs vary with metal feed mechanism, sophistication of the melting, collection chamber and gas
atomization is categorized as horizontal and vertical gas atomization. The basis of gas atomization is to deliver energy from
a rapidly expanding gas to the metal stream to form droplets. The gas atomization process has a large number of operating
variables – gas type, gas pressure and velocity, melt temperature and viscosity as it enters the nozzle, metal/alloy type, metal
feed rate. These parameters are adjusted to tailor powder characteristics for various uses. Powder produced by atomization
is spherical in shape with wide size distribution and integrity of metal/alloy powder can be maintained if performed totally
under inert atmosphere. Atomization technique is used to produce powder of Al, Ni, Mg, Co, Pd, Cu, Fe, Au, Sn, Zn and Be
alloys. The detail of atomization process is available elsewhere (German, 1994; Upadhyay and Upadhyay, 2011).
(b) Water atomization – In water atomization, high pressure water jets are directed against molten metal/alloy stream, forcing
disintegration and rapid solidification. This process is similar to gas atomization, only difference is rapid quenching and
differing fluid behavior. Here, control of particle shape and size is difficult due to rapid cooling. Moreover, oxidation of
powder particle is a major drawback. Powder of stainless steel, Cu, brass, bronze, tool steel, Co and Ni alloys, precious
metals and low melting temperature metals (Pb, Sn and Zn alloys) are prepared by water atomization technique.
(c) Centrifugal atomization – Powder of reactive metals/alloys is produced by centrifugal atomization technique. In this process,
centrifugal force throws off the molten metal as a fine spray which solidifies into a powder. Reactive metals or alloys like Zr, Ti
and Ni superalloys are produced by centrifugal atomization using rotating electrode concept. The consumable electrode made
from desired material is melted at its end by either plasma arc or stationery W electrode and rotates at very high velocity
(up to 50,000 rpm). Centrifugal atomization is carried out either vacuum or inert atmosphere to prevent oxidation. The main
advantage of centrifugal atomization is powder cleanliness, spherical shape with high packing density and good flowability
and uniform particle size. The main disadvantages are low production rate, high equipment and processing cost.

Table 1 shows the comparison of three atomization techniques. The table compares the size, shape and morphology of the
powder produced by three atomization techniques.

Basic Processes in Powder Metallurgy

Mixing/Blending of Powder
A composite powder particle has two or more phases present with variation of size, shape and density. Composite particles are
assembled to generate unique flow, packing, homogeneity and sintering. Homogeneous mixture is required with controlled
segregation to obtain optimum properties of final consolidated composite product. Hence, most metal/alloy composite mixtures
are prepared by blending or mixing in rotating containers. The schematic diagrams of such mixing devices are shown in Fig. 3. The
volume of powder in mixer determines the mixing efficiency. A powder volume of 20%–40% of the mixer capacity is usually
optimal. The rotational speed of mixer also plays an important role in mixing and optimal mixing of powder occurs at 75% of
critical speed.

Table 1 Comparison of atomization techniques

Process Size range, mm Particle shape Size distribution Cost

Gas atomization 15–300 Rounded, spherical Moderate Moderate

Water atomization 5–800 Irregular, nodular Wide Low
Centrifugal atomization 200–600 Spherical Bimodal High
4 Powder Metallurgy Routes for Composite Materials Production

Fig. 3 Some common equipment used for mixing or blending powders: (a) rotating cylinders (b) rotating cube (c) double cone (d) twin shell and
(e) Turbula shaker mixer T2FTM. Reprinted with permission from German, R.M., 2005. Powder Metallurgy and Particulate Materials Processing.
Princeton, NJ: Metal Powder Industries Federation, p. 173, Fig. 5.13. (d) German, R.M., 1994. Powder Metallurgy Science, second ed. Princeton,
NJ: Metal Powder Industrial Federation.

Mixing with binders and lubricants

Mixing is the first step in the preparation of a powder-binder feedstock for shaping. Mixing is very crucial, since mixing deficiencies
can not be corrected by subsequent processing. The inhomogeneties in a mixture occur in two main forms, separation of
the binder from the powder and segregation according to particle size within the binder. The main aims in mixing are to coat
the particles with binder, to break up agglomerates, and to attain uniform distribution of binder and particle size throughout the
feedstock.
Friction between die wall and powder during compaction is a major problem. As the compaction pressure is increased, ejection of
powder mass from the die becomes more difficult and lubricants are used to minimize die wear and ease ejection. Lubricants are usually
mixed with metal/alloy powder as a final step before pressing. Usually stearate powders of Ca, Zn, Li, Mg and Al of 0.5–1.5 wt. %
are added with metal/alloy powder. During pressing, lubricants form a fluid that lowers friction by creating a thick film of high viscosity
polymer. Low viscosity fluids are not effective since they will be forced away from the friction points by the high pressure used in powder
compaction. It has been observed that flowability improves (flow time measured from hall flowmeter, 50 g sample) reduces with
increasing lubricant content and ejection pressure decreases with increasing lubricant amount. It has also been found that the green
density after compaction reaches maximum at 1 wt. % of lubricant content and further addition of lubricant reduces green density
(German, 1994).

Powder Compaction
After mixing the powder with lubricants and additives, the next step to be followed is compaction of powder. Loose powder
particles can not be packed together more than tap density. To achieve higher density, external application of pressure is required.
The rate of initial densification is high with application of pressure. As compaction proceeds, rate of densification decreases due to
work hardening. As pressure is applied, initially rearrangement of particle takes place with filling of large pores giving a higher
packing coordination. A sketch of the density versus compaction pressure during metal powder compaction, showing key stages
and schematic of powder compaction are shown in Fig. 4(a) and (b) respectively.
During compaction, contact area and number of contacts increases with increasing pressure and also with progress of com-
paction. The point contacts undergo elastic deformation and at all contact points elastic energy is stored in the compact. High
pressure increases density by contact enlargement through plastic deformation. As pressure increases, homogeneous plastic flow
spreads from the contacts and entire particle becomes work hardened. Although strain hardening occurs in case of ductile
materials, but in case of brittle materials densification occurs by fragmentation. The hardness and work hardening behavior both
influence compaction. The particle size and shape also affect compaction behavior. Small particle size and irregular particle
hinders compaction because of higher interparticle friction and higher particle work hardening rate.

Powder compaction techniques

Conventional compaction
Conventional compaction is carried out using cylindrical die and punches (upper and lower punches). In this technique, lower
punch is placed inside the die and then powder is filled up. Then upper punch is placed at the top side of die. Finally, die and
punch assembly is pressed under uniaxial compaction. Once pressure is applied for fixed time periods, upper punch is removed
and the lower punch is used to eject the compact. Fig. 5 shows the schematic diagram of conventional die compaction. In
conventional die compaction, when pressure is applied from top and bottom punches, the process is called double-action
 Powder Metallurgy Routes for Composite Materials Production 5

Fig. 4 (a) A sketch of the density versus compaction pressure during metal powder compaction, showing key stages and (b) schematic of powder
compaction. Reproduced from (b) German, R.M., 1994. Powder Metallurgy Science, second ed. Princeton, NJ: Metal Powder Industrial Federation.

Fig. 5 Schematic of conventional die powder compaction.

pressing. On the other hand, when pressure is applied from only one punch, the process is called single action pressing. It can be
shown that in case of single pressing, pressure at any position “x” below the punch as follows:
 
4uzx
P x ¼ P exp  ð1Þ
D

where D ¼ Diameter of compact

P ¼ Pressure applied at the top of punch
Px ¼ Transmitted pressure at the position “x” below the punch
z ¼ Proportionality constant ¼ radial stress/axial stress

The derivation of equation is available elsewhere (German, 1994). The equation shows that pressure decreases with depth in
the powder bed. In uniaxial die compaction, pressure transmission decreases exponentially with height of compact. Hence, there is
variation of pressure distribution along the length and radial cross section compact. The variation of pressure results in density
gradient and it leads to variation in strength in the compact across the cross section. The height to diameter (H/D) ratio is
6 Powder Metallurgy Routes for Composite Materials Production

Fig. 6 Schematic diagram of cold isostatic compaction (CIP).

important to create uniform compact properties. Generally, when the height to diameter ratio exceeds five, die compaction is
unsuccessful. To obtain uniform density and strength of compact, cold isostatic compaction (CIP) is adopted.

Cold isostatic pressing (CIP)

For complex shape, large length to diameter ratio and to achieve uniform density and strength, CIP is a viable technique. A flexible
mold is filled with powder and pressurized isostatically using a fluid such as oil or water. As pressure is applied along all directions,
higher density can be achieved as compared to conventional die compaction. Moreover, lower density gradients are achieved and
complex shape can be compacted by cold isostatic pressing. Fig. 6 shows the schematic diagram of CIP.

Sintering
Sintering is the bonding of particles at higher temperature. It can occur below the melting point (0.7–0.8 of melting temperature)
by solid state sintering. Sintering also involves formation of liquid phase. The driving force of sintering is reduction in surface
energy. Small particles have high surface area and sinter faster than coarse particle. Sintering is thermally activated process which
occurs by atomic transport through diffusion.

Sintering mechanisms
Two types of transport mechanisms, surface transport and bulk transport occur in sintering. When sintering takes place between
two particles, a neck is formed. In surface transport mechanism, no shrinkage or densification takes place, since mass originates
and terminates at the surface. Surface diffusion and evaporation-condensation (EC) are two most important contributors during
surface transport controlled sintering. Surface diffusion dominates during low temperature sintering of metals. On the other hand,
bulk transport causes shrinkage or densification. The mass originates at the particle interior and deposits at the neck. Bulk transport
mechanism includes volume diffusion, grain boundary diffusion, plastic flow and viscous flow. Although both surface and bulk
transport processes gives neck growth, bulk shrinkage or densification occurs by bulk transport. Bulk transport generally occurs at
high temperature. Fig. 7 shows the schematic diagram of both bulk and surface transport.

Solid and liquid state sintering

Sintering can takes place both in solid state or in liquid state. Surface energy is generally small driving force for solid state sintering.
To obtain material with higher density and strength, sintering is more often enhanced. Sintering is enhanced by the formation of
liquid phase, application of external stress (pressure assisted sintering), and addition of additives (activated sintering). In liquid
phase sintering, a low melting phase is formed and this liquid phase may provide for rapid transport. There are certain criteria to
be fulfilled for liquid phase sintering. These criteria are – (1) wetting is the first requirement. There should be good wettability
between solid and liquid phase. Good wettability is fulfilled by low contact angle between solid and liquid phase, where liquid
spreading will take place over solid surface. (2) The solid must be soluble in the liquid.
Sintering has a dominant role on the properties of P/M compacts. As the degree of sintering increases, the density, strength,
ductility, thermal and electrical conductivity, corrosion resistance and other properties will improve. Sintering is a complex process
which depends on several factors like sintering time, temperature, heating rate, sintering atmosphere and also on green compact.
 Powder Metallurgy Routes for Composite Materials Production 7

E-C
SD

D VD
surface
transport X

E-C = evaporation-condensation
SD = surface diffusion
VD = volume diffusion (adhesion)

D
bulk
transport X PF GB
VD

PF = plastic flow (climb or

L o - ΔL glide)
GB = grain boundary diffusion
Lo = D VD = volume diffusion

Fig. 7 Neck growth in sintering models for spheres of diameter D. The upper drawing shows neck growth measured by neck diameter X via
surface transport mechanisms that do not produce shrinkage. The lower drawing is for bulk transport mechanism that move mass from between
the particles to allow densification. Reproduced from German, R.M., 2014. Sintering: From Empirical Observations to Scientific Principles, first ed.
United States: Elsevier-Butterworth Heinemann.

To obtain improved sintered properties, all the sintering parameters are to be optimized. Compaction at higher pressure gives
higher strength, density, contact size and dimensional control after sintering. Higher compaction pressure leads to larger net neck
sizes, however, compaction contributes at higher pressures.

Pore structure during sintering

The voids between particles generates pore in sintered product. After the initial stage of sintering, grain boundary and pore
configuration control the sintering rate. At the beginning of intermediate stage, the pore geometry is highly convoluted and
pores are located at grain boundary intersections. As sintering progresses, pore shape changes to cylindrical where densification
occurs by reduction in pore radius. In the later stage of sintering, interaction between pore and grain boundary can take in three
forms: the pore can retard grain growth, the pore can be dragged by the moving grain boundaries during grain growth or grain
boundaries can break away from the pore, leaving them isolated inside the grain. At low temperature, pores remain attached
with grain boundary and impede the movement of grain boundary. However, at higher temperature grain boundaries break
away from the pores since pores are slower moving species than grain boundary. In the final stage of sintering, pores become
spherical and isolated (German, 1994).

Fabrication of Composites by Powder Metallurgy

There are various methods by which composite materials can be fabricated. The fabrication methods depend on material system
and properties requirement of the component. The methods can be broadly classified into two categories: conventional sintering
methods and pressure assisted full density processing techniques. The conventional sintering method is followed after die com-
paction. The sintering technique is selected either solid state or liquid state sintering. On the other hand, in pressure assisted full
density processing techniques, external pressure is applied. The techniques are-
(1) Uniaxial hot pressing and hot isostatic pressing (HIP)
(2) Spark plasma sintering
(3) Microwave sintering
8 Powder Metallurgy Routes for Composite Materials Production

(4) Powder forging

(5) Powder rolling
(6) Powder extrusion
(7) Dynamic powder compaction

The various composite fabrication techniques using powder metallurgy are discussed below. Recent researches on fabrication of
composites using powder metallurgy technique are also summarized.

Conventional Pressureless Sintering

The composite powder mixture is initially compacted by using die and then the compacted mass is sintered in furnace. During
sintering, varieties of atmospheres like Ar, N2, H2, and NH3 are chosen depending on materials system. The green compacts
are sintered by solid state or liquid state. The rate of densification is lower in case of solid state sintering; hence sometimes
external additives are added for formation liquid phase. The sintering temperature is generally 0.7–0.8 of melting point
selected. The fabrication of various composites by researchers using compaction followed by pressureless sintering is
highlighted below.
Gustafsson et al. (2008) fabricated Al2O3 þ 5 vol. % SiC composite by conventional pressureless sintering. They milled Al2O3
and SiC powder and then compacted CIP and pressureless sintered in a nitrogen atmosphere at 1750 and 1780 1C. They obtained
a full density of 499% at 1780 1C. They achieved Vickers hardness and indentation fracture toughness of around 18 GPa and
2.3 MPa m1/2 respectively after sintering at 1780 1C and observed that addition of smaller additions of MgO promoted low
temperature sintering. Xu et al. (2019) studied low-temperature preparation of Al2O3–ZrO2 nanoceramics via pressureless sintering
assisted by amorphous powders. They found that Al2O3–5 mol% ZrO2 and Al2O3–10 mol% ZrO2 were almost fully densified at
temperature as low as 1350 1C and densification was attributed to the metastable state and phase transition of amorphous
powders (Al2O3–ZrO2), which acted as sintering aids. They also showed that the composites exhibited dense and homogenous
mixture of Al2O3 and ZrO2 particles with fine grain size, and the microstructure refinement further contributed to superior
mechanical properties. Wang et al. (2019) studied pressureless sintering of B4C with MoSi2 (5–30 wt%) as a sintering aid carried
out at 1600–2260 1C in vacuum. They obtained relative density, fracture toughness and hardness of the samples with 30 wt%
MoSi2 sintered at 2260 1C reach 96.5%, 3.98 MPa m1/2 and 28.1 GPa, respectively. They investigated that MoSi2 can react with B4C
to in-situ form Mo2B5 and SiC below 1600 1C. It was also noticed that Mo2B5 gradually transform to MoB2 with further increase in
temperature. Bakhsh et al. (2013) fabricated carbon nanotube reinforced alumina nanocomposites by pressureless conventional
sintering at 1600 1C under Ar gas. Their study showed that the densification can be achieved without degradation of carbon
nanotubes at elevated temperatures in the carbon nanotube–alumina nanocomposites sintered by the conventional route.
Bahaaddini et al. (2019) studied the effect of B4C additive on pressureless sintering of LPS–SiC SiC–Al2O3–Y2O3 composite. They
observed that increasing the B4C content up to 5 wt. % enhanced the strength and fracture toughness of the composite samples,
however increasing beyond 5 wt. % led to a decrease in these properties. Li et al. (2013) fabricated SiC–BN composites with a
BN content of 6 wt% by pressureless sintering at 2200 1C for 1 h and found to have 99.4% theoretical density and a high electrical
resistivity of 1.24  1010 O cm. Liu et al. (2017) fabricated TiC-NiTi/Ni cermets by pressureless sintering at 1380 1C for 1 h.
They showed that the hardness and elastic modulus of the TiC0.7–NiTi cermets were lower than for the corresponding
TiC0.95–Ni equivalent, whereas the fracture toughness and bending strength were significantly higher. They also observed that
the Ni binder exhibited a brittle fracture, whereas the NiTi binder fractured in a ductile way. Mukhopadhyay et al. (2007)
fabricated ZrO2–30 vol. % ZrB2 composites by pressureless sintering in the temperature range of 1400–1600 1C for 1 h in argon
atmosphere. They studied the influence of yttria content in the zirconia matrix, as well as the sintering temperature, on the
densification, microstructure and mechanical properties of the composites.

Uniaxial Hot Pressing and Hot Isostatic Pressing (HIP)

Uniaxial hot pressing is similar to die compaction where powder particles are consolidated generally in a graphite die using
uniaxial pressing at high temperature. Fig. 8 shows the schematic diagram of uniaxial hot pressing. Here, compaction takes place
by particle rearrangement and plastic flow (yielding at point contacts) followed by grain boundary and volume diffusion pro-
cesses. The pressing is performed under inert atmosphere or vacuum to avoid contamination. One large commercial use for
uniaxial hot pressing is in the consolidation of diamond-metal composite cutting tool.
The problem of uniaxial hot pressing is that the compact is not uniformly densified and hence uniform properties are not
achieved. To obtain uniform properties of compact, hot isostatic pressing (HIP) is preferred. In HIP, flexible dies are used with
isostatic pressurization. A deformable container is initially evacuated and degassed and then powder is filled. The consolidation of
powder container is performed in an internally heated, cold-wall pressure vessel. High pressure gas, such as Ar or N2 is sued to
transfer pressure and heat for densification. The process is similar to CIP (Fig. 6), only difference is that HIP is performed at higher
temperature but CIP is conducted at room temperature. This process is applied for the consolidation of many aerospace alloys like
Ni base superalloys, Ti and Al alloys, composites and tool steel.
 Powder Metallurgy Routes for Composite Materials Production 9

Fig. 8 Schematic diagram of uniaxial hot pressing.

Xu et al. (2015) fabricated Ti(C, N)-based cermets processed by both hot-pressing sintering and conventional pressureless
sintering. They observed that pressureless sintering present higher transverse rupture strength, fracture toughness and density than
samples fabricated by hot pressing. However, the hot pressed sintered samples possess a higher hardness. Canakci and Varol
(2014) fabricated AA7075/Al–SiC composites using powder metallurgy and hot pressing. They observed that hot pressed density
of the composites decreased with increasing amounts of Al powders and SiC content but hardness increased with increase of SiC
content. Akbarpour and Pouresmaeil (2018) fabricated Al-CNT composite by powder metallurgy and hot pressing technique. They
found that the increase of carbon nanotubes at 2 and 4 vol% increased the yield strength and compressive strength from 176 MPa
and 201–241MPa and 251 MPa and reduced the fracture strain from 420% to 4%, respectively. Gao et al. (2019) fabricated
B4Cp/6061Al composite by powder metallurgy followed by hot pressing in the temperature range of 560–600 1C. They observed
that density, yield strength and failure strain of the composites increased with increasing temperature from 560 to 600 1C.

Spark Plasma Sintering (SPS)

Spark plasma sintering is best suited for consolidation of nanoparticles or ultrafine powder, where high amperage DC pulses
current (1000 A) is passed through graphite die and powder mass. Low voltage of 5–10 V is applied through graphite die and
punches. Heating rate as high as 500–600K/min can be achieved, where sintering can be performed within 5–6 min with full
density, minimizes the chances of grain coarsening during sintering. The heat generation is internal, in contrast to conventional
hot pressing, where heat is provided by external heating elements. When spark discharge appears in the gap between the particles, a
local high temperature state occurs. This causes vaporization and melting of the surfaces of powder particles and necks are formed
around the contact area between the particles during SPS process. Fig. 9 shows the schematic diagram of SPS process. There are
certain advantages of SPS process than other conventional and pressure assisted sintering process. The advantages are:

(1) Reduced sintering time

(2) Good grain to grain bonding
(3) Clean grain boundaries
(4) Initial activation of powders by pulsed voltage
(5) Resistance sintering under pressure.

The various composites fabricated by SPS are summarized below. Leszczyńska-Madej et al. (2019) fabricated Al-SiC com-
posites reinforced with 10, 20 and 30 wt. % SiC by SPS process at 580 and 600 1C. They did not observe remarkable difference in
the microstructure of the composites reinforced with SiC particles sintered at 580 1C and 600 1C. They found that the
microstructure of the sintered compacts consists of uniform grains, the SiC strengthening phase particles locate on the grain
boundaries. The use of a higher sintering temperature had a positive effect on hardness and the bending strength of the tested
materials. Sayyadi-Shahraki et al. (2019) studied densification and mechanical properties of spark plasma sintered Si3N4/ZrO2
nano-composites consolidated at 1600 1C under the pressure of 30 MPa for 10 min. They found that the addition of Y2O3-
doped ZrO2 into the initial Si3N4 powder can noticeably facilitate densification process, decreasing sintering temperature of
10 Powder Metallurgy Routes for Composite Materials Production

Fig. 9 Schematic diagram of spark plasma sintering (SPS). Available at: https://www.substech.com.

monolithic Si3N4 ceramic from 1600 to 1420 1C through 30 vol. % YSZ utilization. The study indicated that the hardness of the
Si3N4-base composites declined from 16.6 to 13.2 GPa, whereas the fracture toughness improved from 5.8 to 7.1 MPa m1/2 by
increasing ZrO2 content from 0 to 30 vol. %. Kgoete et al. (2019) studied oxidation resistance of Ti6Al4V-TiN composites
fabricated by spark plasma sintering at 1000 1C for 6 min at 50 MPa pressure. They showed that the reinforced Ti6Al4V with TiN
significantly improved the oxidation resistance, and hardness of Ti6Al4V alloy which is compactable and beneficial for aero-
space application. They also observed that Ti-6Al-4V alloy reinforced with 5 wt. % TiN yielded better results, with improved
hardness value of 881.15 HV and less weight gain which indicates high temperature oxidation resistance. Akhlaghi et al. (2018)
fabricated TiAl–Ti3AlC2 composite by spark plasma sintering at 1000 1C for a dwell time of 15 min under an external pressure of
40 MPa in vacuum atmosphere. They achieved relative density of B95%, Vickers hardness of B4.5 GPa, fracture toughness of
11.9 MPa m1/2, and flexural strength of 336 MPa. Mallik et al. (2019) studied spark plasma sintering of Ti-diamond composites,
where they varied diamond content from 5 to 50 wt%. Sahani et al. (2016a,b) fabricated SiC-B4C-Si and SiC-B4C-Al cermets by
both pressureless and spark plasma sintering techniques and observed that SPS is more efficient densification method than
conventional pressureless sintering.

Microwave Sintering
Microwaves are electromagnetic radiation with wavelengths ranges from 1 mm to 1 m in free space and frequency varies from
300 GHz to 300 MHz respectively. It has been reported that microwave frequency of 2.45 GHz can be used for sintering of
metal and ceramic powder (Roy et al., 1999). Fig. 10 shows the schematic diagram of basic components of microwave
sintering. In microwave sintering, heating is internal, uniform and high heating rate can be obtained as compared to
conventional sintering.
Recent researches on fabrication of composites by microwave sintering are presented below. Mondal et al. (2013) studied the
sinterability of the W–Cu system consolidated in a 2.45 GHz multimode microwave furnace and also critically compared with that
processed in a radiatively heated (conventional) furnace. They found that microwave processing results in greater densification, more
homogenous distribution of the binder phase, smaller tungsten grain size, higher electrical conductivity and hardness as compared to
conventional sintering. Hong et al. (2019) fabricated Al2O3/SiC composite ceramic tool material by two step microwave sintering
(first step temp. varies from 1600 to 1700 1C and second step temp. 1100 1C) and compared with single step sintering (1600 1C).
They achieved relative density, grain size, Vickers hardness and fracture toughness of 98.37%, 0.78 7 0.31 mm, 18.40 7 0.24 GPa
and 4.97 7 0.30 MPa m1/2, respectively for the composite processed by two step and higher than single step sintering. Reddy et al.
(2016) investigated structural and mechanical properties of microwave sintered Al-Ni50Ti50 composites. Duan et al. (2019) studied
the effect of CNTs content on the microstructures and properties of CNTs/Cu composite fabricated by microwave sintering followed
by rolling. They found that electrical conductivity and relative density of microwave sintered CNTs/Cu composites decreased with
increase in CNTs content. It was also noticed that microwave sintering and subsequent rolling process enables better microstructure
and performance of sintered composites which shows tensile strength of 218 MPa, the elongation of 37.75%, and the electrical
conductivity of 498% IACS compared to pure copper. Ghasali et al. (2019) studied corrosion behavior and in-vitro bioactivity of
porous Mg/Al2O3 and Mg/Si3N4 metal matrix composites fabricated by using microwave sintering process. They performed
 Powder Metallurgy Routes for Composite Materials Production 11

Fig. 10 Schematic diagram showing main components of microwave sintering process. Reproduced from Agrawal, D., 2013. Microwave
Sintering of Metal Powders. United States: Woodhead Publishing Limited. Pennsylvanis State University.

microwave sintering at 650 1C without soaking time in a graphite bed and porosity of about 50% was measured for both sintered
composites. Yang et al. (2019) studied flexural modulus of SiC/SiC composites sintered by microwave and conventional heating in
the temperature range of 800–1100 1C. They found that microwave heating led to much lower flexural modulus of SiC/SiC
composites than conventional heating at the same sintering temperature.

Powder Rolling
In powder rolling, loose powder is gravity fed into the gap between two rolls which generate green sheet. The green sheet is then
continuously sintered and rolled to obtain a full density strip product. Fig. 11 shows the schematic diagram of powder rolling
process. Powder rolling is employed to fabricate sheet products of iron, copper, aluminum, nickel, steel, stainless steel, Mo–Cu,
NiTi, Co–Fe, Cu–Pb and composites for applications ranging from battery electrodes to wear surface. Good compressibility is
required to ensure that sufficient particle interlocking to give adequate green strip strength. The thickness of the finished strip and
particle segregation restricts the maximum particle size which can be tolerated in the powder feed to the compaction mill. The
powder must have flow smoothly and quickly through hopper with minimum tendency to stick slip or bridging.
The green strip thickness after powder rolling is calculated form the Eq. (2)

Dð1  cosaÞ
hg ¼ ð2Þ
C1

where hg is green strip thickness

D-roll diameter
a-angle of nip
C-compression ratio

From the above Eq. (2) it is found that strip thickness largely depends on roll diameter (D). Roll diameter of between 50 and
150 times the strip thickness are often required. The maximum strip thickness can be increased by increasing the ‘m’ i.e., by
roughening the rolling surface. If the air entrapped in the powder is not properly released, the strip produced will not be of
uniform density (Upadhyay, 1998).
Mo et al. (2015) studied the densification process of 10% B4C–AA2024 matrix composite strips by semi-solid powder rolling.
The gas atomized AA2024 and B4C powders were initially preheated at 300 1C. Then the mixed powders were firstly heated to 550,
585, 605, 625 1C, respectively and held for 30 min and then fed into the gap to produce strips with a width of 100 mm and a
thickness of 2.5–3 mm. They found that when the liquid phase is lower than 20%, rolling deformation is the main densification
mechanism in deformation area. When the liquid fraction is higher than 20%, the flowing and filling of liquid are the densifi-
cation mechanisms. Liu et al. (2014) also investigated microstructure evolution during semi-solid powder rolling and post-
treatment of 7050 aluminum alloy strips. They showed that the best liquid fraction to prepare a strip ranges from 45% to 65%.
12 Powder Metallurgy Routes for Composite Materials Production

Fig. 11 Schematic diagram of powder rolling process. Reprinted with permission from German, R.M., 2005. Powder Metallurgy and Particulate
Materials Processing. Princeton, NJ: Metal Powder Industries Federation, p. 330, Fig. 8.31. German, R.M., 1994. Powder Metallurgy Science,
second ed. Princeton, NJ: Metal Powder Industrial Federation.

Fig. 12 Schematic diagram showing initial pore, pore in powder forging and in HIP process respectively.

They found that flowing and filling of liquid (410%), densification by rolling and recrystallization (o10%) are the three
combination mechanisms of the semi-solid powders during rolling.

Powder Forging
Powder forging is a high strain rate deformation process, typically conducted at elevated temperature, where material has a low
strength and ductility. Conventional powder forging begins with custom-blended metal powders being fed into a die, then being
compacted into a ‘green’ shape, which is then ejected from the die. The compact, called a ‘preform’ is different from the shape of
final part will acquire after being forged. Again as in the conventional PM process, the green compact is sintered by solid state
diffusion at a temperature below the melting point of the base metal in a controlled atmosphere furnace, creating metallurgical
bonds between the powder particles and imparting mechanical strength to the preform. The heated preform is withdrawn from the
furnace, coated with lubricant, and transferred to a forging press. Forging causes plastic flow, thus reshaping the preform to its final
configuration and densifying it. Powder forging requires less handling, fewer dies and process steps as compared to conventional
forging. Conventional forging of cast material require several steps to convert a billet into the final shape. But the parts fabricated
by powder forging require only minor secondary machining and offer grater dimensional precision.
Powder forging is a combination of densification and flow under uniaxial forces. The pore collapse in forging is different from
that encountered under hydrostatic condition used in HIP. Fig. 12 shows the schematic diagram of pore closure in powder forging
and HIP process. The pore experiences higher shear in forging than in isostatic compaction. The difference in pore collapse
contributes to more shear and bonding in powder forging. Powder forging is extensively used to fabricate various automobile
components like connecting rods, cams, bearing races, off-road equipment and power tools.
 Powder Metallurgy Routes for Composite Materials Production 13

Fig. 13 Schematic diagram of powder extrusion process.

Khodabakhshi et al. (2019) fabricated AA8006-B4C nanostructured nanocomposite by accumulative fold forging process (AFF),
novel SPD process involves repetitive folding and forging steps with or without the incorporation of large fractions of nanoparticles
between aluminum foil layers. They showed the uniform dispersion of the nanoparticles with less clustering/aggregation, low fraction of
porosity, and strong bonding between the layers. They showed the refining of grain structure of aluminum matrix down to UFG range
of B200 nm and nano-sized range of B35 nm with and without the B4C nanoparticles and also improvement of modulus and
hardness. Ozerov et al. (2019) investigated evolution of microstructure and mechanical properties of Ti/TiB metal-matrix composite
produced by spark plasma sintering (SPS) at 1000 1C using a Ti-10 wt. %TiB2 powder mixture and then subjected to multiaxial
isothermal forging at 700 or 850 1C and a strain rate 103 s1. They found a considerable increase in low-temperature tensile ductility
without substantial loss in strength. Qiu et al. (2012) fabricated Ti alloy connecting rod by powder forging technique and studied
microstructure and mechanical properties. Alshammari et al. (2019) fabricated Ti–Mn alloys for biomedical applications by powder
metallurgy using powder forging. They showed that Ti–Mn alloys have mechanical properties comparable to other Ti alloys commonly
used in biomedicine such as Ti–6Al–4V or alloys being developed for dental and biomedical application such as other Ti–Mn alloy.
Kumar et al. (2017) fabricated oxide dispersion strengthened (ODS) steels containing Fe-18% Cr-2%W-0.2%Ti with 0, 0.35, 0.5, 1 and
1.5% Y2O3 for future nuclear reactors. The elemental powders were mechanically alloyed and then the powders were placed in a mild
steel can and forged in a stream of hydrogen gas at 1473K. They showed that the strength of ODS steel increased with yttria content
accompanied by a decrease in tensile elongation.

Powder Extrusion
Powder extrusion is useful for fabricating high temperature alloys like oxide dispersion strengthened Cu, Al and Ni base super-
alloys. Long shapes with a constant cross section are the main products of extrusion. Extrusion involves relatively low temperature;
hence a high level of shear is required for densification. For certain alloys and composites, the combination of temperature and
shear proves optimal with respect to microstructure control and final properties. The schematic diagram of powder extrusion
process is shown in Fig. 13.
The triaxial stress system set up in all three powder metal working processes. All three processes are related to stress, strain rate
and temperature. The ideal or theoretical pressure required for extrusion of a fully dense material is expressed as
P ¼ s0 ln ðrÞ ð3Þ

where s0 and r are yield stress and r is the extrusion ratio.

There are three varieties of powder extrusion process. These processes are mentioned below.

(1) Loose powder is placed in the heated extrusion container and extruded directly through the die. This method has been
developed for the extrusion of certain Mg alloy powder.
(2) The powder is cold compacted and then hot pressed. The hot pressed compact is then extruded as per the conventional
method. Al alloy powder billets are extruded by this method.
(3) The metal powders are placed in a metallic capsule or can, heated and extruded with the can. A green metal powder compact
may be canned or the powder may be cold pressed into a metal can under moderate pressure. The can is outgassed by
evacuation at room or elevated temperature and sealed off before the can and powder are heated for extrusion (Upadhyay
and Upadhyay, 2011).
Issa et al. (2017) fabricated amorphous nano SiO2 reinforced Al MMC by powder metallurgy and hot extrusion method. They
showed that addition of 1 wt. % silica nanoparticle to aluminum matrix increased average hardness and tensile strength of the
nano-composite by about 41.8% and 24.8%, respectively. They also observed that increasing nano-SiO2 percentage decreased the
tensile properties and ductility. Kim et al. (2019) fabricated tubular shape aluminum (Al) 6063/Al-3 vol% carbon nanotubes
(CNT)/Al3003 functionally graded materials (FGMs) by hot extrusion process. They found that FGMs has high strength of
142 MPa and high elongation of 22%. Kurinskiya et al. (2015) studied hot extrusion of Be–Ti powder in copper and steel
14 Powder Metallurgy Routes for Composite Materials Production

Fig. 14 A typical set up for the dynamic powder compaction. Reprinted with permission from German, R.M., 2005. Powder Metallurgy and
Particulate Materials Processing. Princeton, NJ: Metal Powder Industries Federation, p. 332, Fig. 8.33. German, R.M., 1994. Powder Metallurgy
Science, second ed. Princeton, NJ: Metal Powder Industrial Federation.

containers at 700 and 900 1C, respectively. They observed that processing temperature has a great influence on the metal flow
during the extrusion as well as formation of beryllide phases. Their study revealed that the brittle intermetallic phases were formed
by processing at 900 1C; while no evidence of reaction between beryllium and titanium was detected after extrusion at 700 1C.
Jiao et al. (2019) studied microstructure evolution and high-temperature tensile behavior of the 2.5 vol. % TiBw/TA15 composites
fabricated by powder extrusion.

Dynamic Powder Compaction

Dynamic powder compaction uses an accelerated mass which strikes the powder at very high velocity to supply the shock wave.
The shock wave results in metallurgical bonding and sometimes fusion of the surface of particles. Fig. 14 shows a typical set up for
the dynamic powder compaction.
The process takes place in such a short time (microsecond or less) that there is no possibility for heat to be conducted away
from the surface and thus localized melting or welding occurs. The liquid zone between the particles solidifies in the same time
scale as its formation. The rapid cooling rate (106–108 1C s1) results in solidified material with extremely fine structure and
imparts unique properties to the compact. This process allows non-equilibrium powder or powder mixture to be consolidated
with either chemical reactions or degeneration of metallurgical structures.
Mishra et al. (2007) synthesized alumina-zirconium diboride in situ composite by novel SHS dynamic compaction process and
studied the effect of addition of Ti as diluent in the reaction. They found that Vickers microhardness first increased with the addition of
5-wt. % titanium and then decreased for further additions of titanium diluent up to 20 wt. %. The maximum hardness was found as
2800 HV0.025. Mishra et al. (2014) also fabricated alumina-titanium diboride in situ composite by self-propagating high-temperature
synthesis (SHS) dynamic compaction and investigated the effect of compaction pressure on microstructure, toughness, hardness and
modulus, oxidation behavior during synthesis. They achieved high hardness (average hardness: 22.684 GPa) with reasonable toughness
(7.52 MPa m1/2) and oxidation resistance up to 900 1C temperature in Al2O3–TiB2 composite. Vorozhtsov et al. (2017) investigated
structural and mechanical properties of aluminum-based composites (Al-nanodiamonds and Al–Al2O3) processed by dynamic
shock-wave compaction processing. They observed an increase in the hardness, compressive strength and elastic modulus of the
composites after explosive compaction with the introduction of nanoparticles into the powder mixture. Atrian et al. (2015) investigated
a comparative study on hot dynamic compaction and quasi-static hot pressing of Al7075/SiCnp (0, 5, and 10 vol. % SiCnp)
nanocomposite. They obtained higher compressive strength for quasi-static hot pressed samples than those produced under dynamic
compaction. Table 2 shows the summary of various composite fabrication methods using powder metallurgy. The main features of
processing methods and density, grain structure of consolidated products of each method are shown.
Table 3 shows a comparison of SiC–TiC composites fabricated by pressureless sintering, hot pressing (HP), hot isostatic
pressing (HIP) and spark plasma sintering (SPS) (Khodaei et al., 2018). It has been observed from the table that pressureless
sintering is not capable enough to produce composite with high densification (o98%) and improved mechanical properties. It is
pressureless technique, hence some amount of residual pores are always present even sintering at comparatively higher tem-
perature (2200 1C). On the other hand, other pressure assisted sintering techniques (HP, HIP and SPS) are efficient enough to
 Powder Metallurgy Routes for Composite Materials Production 15

Table 2 Summary of various composite fabrication methods using powder metallurgy

Fabrication method Main process features Densification, grain structure of consolidated product

Conventional sintering Solid/liquid state sintering, Pressureless Low density level (max. around 90% of TD), High chance of grain
sintering, time required few hours coarsening, Cheap, simple process
Hot pressing/HIP Uniaxial pressure/isostatic pressure, Time High level of density (Max. 98%–99% TD), Chance of grain
required few hours (1–2 h) coarsening, Expensive
Spark plasma sintering (SPS) Consolidation by DC pulse, Time – few minute 99%–100% TD, Less grain coarsening, Nanostructure can be
(5–10 min), Pressure assisted retained after sintering, Highly expensive.
Microwave sintering Consolidation by microwave with Full densification, chance of grain coarsening
suitable frequency (2.45 GHz)
Powder forging Consolidation by uniaxial stress (impact force) Full densification, grains orientation along forging direction
Powder rolling Consolidated by compressive force Full densification, grains orientation along rolling direction
Powder extrusion Consolidation by shear stress Full densification, grains orientation along direction of extrusion
Dynamic powder compaction Consolidation by shock wave within few minutes Full densification, no chance of grain coarsening, rapidly solidified
non-equilibrium structure

Note: The main features of processing methods and density, grain structure of consolidated products of each method are shown.

Table 3 A comparison of SiC–TiC composite fabricated by pressureless sintering, HP, HIP and SPS techniques

Raw material Second phase Sintering Heat treatment Relative Strength Fracture toughness Hardness Ref.
method temp. (1C) density (%) (MPa) (MPa m1/2) (HV or GPa)

SiC, TiC, B, C 10 wt. % TiC Pressureless 2200 o98 – o3 o25 (Ohya et al., 1992)
SiC, TiC, B, C 10 wt. % TiC HP 2200 98 o550 o4 – (Ohya et al., 1993)
SiC, TiC 25 wt. % TiC HIP 1850 499 682 3.97 2299 HV (Shaoming et al.,
1996)
SiC, TiC 30 wt. % TiC SPS 1800 98 o650 6.25 28 (Luo et al., 2004)

Source: Khodaei, M., Yaghobizadeh, O., Baharvandi, H.R., Dashti, A., 2018. Effects of different sintering methods on the properties of SiC–TiC, SiC–TiB2 composites. International
Journal of Refractory Metals & Hard Materials 70, 19–31.

produce composite with high densification (498%) and improved mechanical properties. Among three pressure assisted sintering
techniques (HP, HIP, SPS), SPS require lowest temperature to produce composite with equivalent densification and mechanical
properties. SPS is an unique consolidation technique, where activation of powder particles, spark effect, clean grain boundaries
and minimal grain growth results in highest densification and mechanical properties even at lowest sintering temperature.

Conclusions

The article discusses about importance, relevance and uniqueness of powder metallurgy process as compared to other fabrication
processes. The basic steps of powder metallurgy like powder fabrication, mixing/blending of powder, powder compaction and
sintering are highlighted in brief. The basic principles of various composite fabrication techniques like pressureless conventional
sintering and pressure assisted full densification processes are presented. The recent researches on fabrication of composites using
various powder metallurgy processes are also summarized. Finally, a summary has been made on main features of various
processing methods and consolidated product. It has been seen that pressureless conventional sintering is simple, economical
process which consumes more time and less densification is achieved as compared to other pressure assisted sintering. On
the other hand, uniaxial hot pressing/HIP and microwave sintering are complex processes, takes less time and higher density
can be achieved than conventional sintering. SPS is best suited for consolidation of nanoparticle/ultrafine particle, where
nanostructure can be retained after consolidation with full density, since it takes very less time (5–10 min). Powder metal working
processes like powder rolling, powder extrusion and powder forging involves application of stress at higher temperature where
metals are ductile. In all three techniques, full density can be achieved where grain orientation changes with deformation direction.
In dynamic powder compaction, consolidation takes place by shock wave, generated by chemical reaction of explosive (SHS),
takes very less time. Here, rapidly solidified non-equilibrium structure is generated after consolidation.

Acknowledgment

Author would like to express his sincere gratitude to his doctoral thesis supervisors, Prof. B. K. Mishra and Prof. S. Sangal for
guiding him to start his research carrier in powder metallurgy. Like any other author of a technical book, author is grateful to
16 Powder Metallurgy Routes for Composite Materials Production

previous authors for their work on this subject, allied subjects and especially to Prof. R.M. German, pioneer in the field of powder
metallurgy. Author appreciates any suggestion or criticism about this article for further improvement.

References

Akbarpour, M.R., Pouresmaeil, A., 2018. The influence of CNTs on the microstructure and strength of Al-CNT composites produced by flake powder metallurgy and hot
pressing method. Diamond & Related Materials 88, 6–11.
Akhlaghi, M., Tayebifard, S.A., Salahi, E., Asl, M.S., 2018. Spark plasma sintering of TiAl–Ti3AlC2 composite. Ceramics International 44, 21759–21764.
Alshammari, Y., Yang, Y., Bolzoni, L., 2019. Mechanical properties and microstructure of Ti-Mn alloys produced via powder metallurgy for biomedical applications. Journal of
the Mechanical Behavior of Biomedical Materials 91, 391–397.
Atrian, A., Majzoobi, G.H., Enayati, M.H., Bakhtiari, H., 2015. A comparative study on hot dynamic compaction and quasi-static hot pressing of Al7075/SiCnp nanocomposite.
Advanced Powder Technology 26, 73–82.
Bahaaddini, M., Baharvandia, H.R., Ehsania, N., Khajehzadeha, M., Tamadon, A., 2019. Pressureless sintering of LPS-SiC (SiC–Al2O3–Y2O3) composite in presence of the B4C
additive. Ceramics International 45, 13536–13545.
Bakhsh, N., Khalid, F.A., Hakeem, A.S., 2013. Synthesis and characterization of pressureless sintered carbon nanotube reinforced alumina nanocomposites. Materials Science &
Engineering A 578, 422–429.
Canakci, A., Varol, T., 2014. Microstructure and properties of AA7075/Al–SiC composites fabricated using powder metallurgy and hot pressing. Powder Technology 268,
72–79.
Chaira, D., Karak, S.K., 2015. Fabrication of nanostructured materials by mechanical alloying. In: Aliofkhazraei, M. (Ed.), Handbook of Mechanical Nanostructuring, first ed.
Germany: Wiley-VCH Verlag GmbH & Co. KGaA, pp. 379–416.
Duan, B., Zhou, Y., Wang, D., Zhao, Y., 2019. Effect of CNTs content on the microstructures and properties of CNTs/Cu composite by microwave sintering. Journal of Alloys
and Compounds 771, 498–504.
Gao, M., Chen, Z., Kang, H., et al., 2019. Microstructural characteristics and mechanical behavior of B4Cp/6061Al composites synthesized at different hot-pressing
temperatures. Materials Science and Technology 35, 1523–1531.
German, R.M., 1994. Powder Metallurgy Science, second ed. Princeton, NJ: Metal Powder Industrial Federation.
Ghasali, E., Khiabani, A.B., Alizadeh, M., et al., 2019. Corrosion behavior and in-vitro bioactivity of porous Mg/Al2O3 and Mg/Si3N4 metal matrix composites fabricated using
microwave sintering process. Materials Chemistry and Physics 225, 331–339.
Gustafsson, S., Falk, L.K.L., Lidén, E., Carlströ, E., 2008. Pressureless sintered Al2O3–SiC nanocomposites. Ceramics International 34, 1609–1615.
Hong, D., Yin, Z., Yan, S., Xu, W., 2019. Fine grained Al2O3/SiC composite ceramic tool material prepared by two step microwave sintering. Ceramics International 45,
11826–11832.
Issa, H.K., Taherizadeh, A., Maleki, A., Ghaei, A., 2017. Development of an aluminum/amorphous nano-SiO2 composite using powder metallurgy and hot extrusion processes.
Ceramics International 43, 14582–14592.
Jiao, X., Chen, W., Yang, J., Zhang, W., Wang, G., 2019. Microstructure evolution and high-temperature tensile behavior of the powder extruded 2.5 vol% TiBw/TA15
composites. Materials Science & Engineering A 745, 353–359.
Kgoete, F.M., Popoola, A.P.I., Fayomi, O.S.I., 2019. Oxidation resistance of spark plasma sintered Ti6Al4V-TiN composites. Journal of Alloys and Compounds 772, 943–948.
Khodabakhshi, F., Gerlich, A.P., Verma, D., Haghshenasd, M., 2019. Nano-indentation behavior of layered ultra-fine grained AA8006 aluminum alloy and AA8006-B4C
nanostructured nanocomposite produced by accumulative fold forging process. Materials Science & Engineering A 744, 120–136.
Khodaei, M., Yaghobizadeh, O., Baharvandi, H.R., Dashti, A., 2018. Effects of different sintering methods on the properties of SiC–TiC, SiC–TiB2 composites. International
Journal of Refractory Metals & Hard Materials 70, 19–31.
Kim, D., Park, K., Kim, K., et al., 2019. Carbon nanotubes-reinforced aluminum alloy functionally graded materials fabricated by powder extrusion process. Materials Science &
Engineering A 745, 379–389.
Kumar, D., Prakash, Dabhade, V.V., Laha, K., Sakthivel, T., 2017. High yttria ferritic ODS steels through powder forging. Journal of Nuclear Materials 488, 75–82.
Kurinskiya, P., Leiste, H., Goraie, A.A., Mueller, S., 2015. Hot extrusion of Be–Ti powder. Fusion Engineering and Design 98–99, 1817–1820.
Li, Y., Wu, H., Yin, J., et al., 2013. High electrical resistivity of pressureless sintered in situ SiC–BN composites. Scripta Materialia 69, 740–743.
Liu, B., Huang, S., Humbeeck, J.V., Vleugels, J., 2017. Pressureless liquid-phase sintered TiCx-NiTi/Ni cermets. Ceramics International 43, 9512–9521.
Liu, Y., Luo, X., Li, Z., 2014. Microstructure evolution during semi-solid powder rolling and post-treatment of 7050 aluminum alloy strips. Journal of Materials Processing
Technology 214, 165–174.
Luo, Y., Li, S., Pan, W., Li, L., 2004. Fabrication and mechanical evaluation of SiC–TiC nanocomposites by SPS. Materials Letters 58, 150–153.
Leszczyńska-Madej, B., Garbiec, D., Madej, M., 2019. Effect of sintering temperature on microstructure and selected properties of spark plasma sintered Al–SiC composites.
Vacuum 164, 250–255.
Mallik, A.K., Das, M., Ghosh, S., Chakravarty, D., 2019. Spark plasma sintering of Ti-diamond composites. Ceramics International 45, 11281–11286.
Mishra, S.K., Gokuul, V., Paswan, S., 2014. Alumina-titanium diboride in situ composite by self-propagating high-temperature synthesis (SHS) dynamic compaction: Effect of
compaction pressure during synthesis. International Journal of Refractory Metals and Hard Materials 43, 19–24.
Mishra, S.K., Rupa, P.K.P., Das, S.K., Shcherbakov, V., 2007. Effect of titanium diluent on the fabrication of Al2O3–ZrB2 composite by SHS dynamic compaction. Composites
Science and Technology 67, 1734–1739.
Mo, Z.Q., Liu, Y.Z., Jia, H.-F., Wu, M., 2015. Densification process of 10% B4C–AA2024 matrix composite strips by semi-solid powder rolling. Transactions of Nonferrous
Metals Society of China 25, 3181–3188.
Mondal, A., Upadhyaya, A., Agrawal, D., 2013. Effect of heating mode and copper content on the densification of W-Cu alloys. Indian Journal of Materials Science.
doi:10.1155/2013/603791.
Mukhopadhyay, A., Basu, B., Bakshi, S.D., Mishra, S.K., 2007. Pressureless sintering of ZrO2–ZrB2 composites: Microstructure and properties. International Journal of
Refractory Metals & Hard Materials 25, 179–188.
Ohya, Y., Hoffmann, M., Petzow, G., 1992. Sintering of in-situ synthesized SiC–TiB2 composites with improved fracture toughness. Journal of the American Ceramic Society
75, 2479–2483.
Ohya, Y., Hoffmann, M., Petzow, G., 1993. Mechnical properties of hot pressed SiC–TiB2/TiC composites synthesized in situ. Journal of Materials Science Letters 12, 149–152.
Ozerov, M., Klimova, M., Sokolovsky, V., et al., 2019. Evolution of microstructure and mechanical properties of Ti/TiB metal-matrix composite during isothermal multiaxial
forging. Journal of Alloys and Compounds 770, 840–848.
Qiu, J.W., Liu, Y., Liu, Y.B., et al., 2012. Microstructures and mechanical properties of titanium alloy connecting rod made by powder forging process. Materials and Design
33, 213–219.
Reddy, M.P., Ubaid, F., Shakoor, R.A., Mohamed, A.M.A., Madhuri, W., 2016. Structural and mechanical properties of microwave sintered Al–Ni50Ti50 composites. Journal of
Science: Advanced Materials and Devices 1, 362–366.
 Powder Metallurgy Routes for Composite Materials Production 17

Roy, R., Agrawal, D., Cheng, J., Gedevanishvili, S., 1999. Full sintering of powdered-metal bodies in a microwave field. Nature 399, 668–670.
Sahani, P., Karak, S.K., Mishra, B., Chakravarty, D., Chaira, D., 2016a. Effect of Al addition on SiC–B4C cermet prepared by pressureless sintering and spark plasma sintering
methods. International Journal of Refractory Metals and Hard Materials 57, 31–41.
Sahani, P., Karak, S.K., Mishra, B., Chakravarty, D., Chaira, D., 2016b. A comparative study on SiC–B4C–Si cermet prepared by pressureless sintering and spark plasma
sintering methods. Metallurgical and Materials Transactions A 47, 3065–3076.
Sayyadi-Shahraki, A., Rafiaei, S.M., Ghadami, S., Nekouee, K.A., 2019. Densification and mechanical properties of spark plasma sintered Si3N4/ZrO2 nano-composites. Journal
of Alloys and Compounds 776, 798–806.
Shaoming, D., Dongliang, J., Shouhong, T., Jingkun, G., 1996. Mechanical properties of SiC–TiC composites by hot isostatic pressing. Journal of Materials Science Letters 15,
1394–1396.
Suryanarayana, C., 2001. Mechanical alloying and milling. Progress in Materials Science 46, 1–184.
Upadhyay, A., Upadhyay, G.S., 2011. Powder Metallurgy Science, Technology and Materials, first ed. Hyderabad: University Press.
Upadhyay, G.S., 1998. Powder Metallurgy Technology. United Kingdom: Cambridge International Science Publishing.
Vorozhtsov, S., Vorozhtsov, A., Kudryashova, O., Zhukov, I., Promakhov, V., 2017. Structural and mechanical properties of aluminium-based composites processed by explosive
compaction. Powder Technology 313, 251–259.
Wang, S., Gao, S.,Xing, P., et al., 2019. Pressureless liquid-phase sintering of B4C with MoSi2 as a sintering aid. Ceramics International 45, 13502–13508.
Xu, Q., Ai, X., Zhao, J., et al., 2015. Comparison of Ti(C, N)-based cermets processed by hot-pressing sintering and conventional pressureless sintering. Journal of Alloys and
Compounds 619, 538–543.
Xu, X., Yang, Y., Wang, X., Su, X., Liu, J., 2019. Low-temperature preparation of Al2O3–ZrO2 nanoceramics via pressureless sintering assisted by amorphous powders. Journal
of Alloys and Compounds 783, 806–812.
Yang, H., Li, M., Zhou, X., Wang, H., Yu, J., 2019. Flexural modulus of SiC/SiC composites sintered by microwave and conventional heating. Ceramics International 45,
10142–10148.