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Microwave sintering process is quite significant and unique in recent times for sintering
material for densification because of its intrinsic advantages such as rapid heating rates,
reduced processing times, uniform temperatures with minimal thermal gradients. Microwave
sintering process leads to substantial energy savings with higher efficiency, improved
properties, finer microstructures, environmental friendly process and with less environmental
hazards.The concept of sintering metals in microwave has been attempted by many
researchers. Though metals are known to reflect microwave radiation, researchers have
confirmed sintering of metals in powder form through microwave. In this study, sintering of
aluminium metal powder through microwave route has been attempted. The study indicated
that aluminium metal powder compacts sintered through microwave process showed better
physical, tribological and thermal properties compared to the ones sintered through
conventional sintering methods.
a-Training Division, Central Power Research Institute, Bangalore-560 080, E-mail: mgananda@cpri.in
b-Department of MME, National Institute of Technology-Karnataka, Surathkal- 575 025, E-mail: jaganmet@gmail.com
mechanical properties of the material [5, power output ranging from 1 to 6 kW in
1]. both single and multimode operations are
possible [6]. A typical microwave oven
Materials that have a high dielectric loss has either an alumina or silicon carbide
couple well with microwaves while the tube surrounded by ceramic high
poor lossy materials with no absorption at temperature insulation fibers. The primary
room temperature require initial heating function of the insulation is to preserve the
using some kind of secondary susceptors. heat in the oven. Insulation does not
For most powder metals, no susceptor is absorb microwave at the lower
needed, but it is mainly used to provide temperature range. But at higher
uniform temperature distribution temperatures there is some portion of
throughout the sample to obtain uniform power dissipation between the insulation
sintering. and the sample. Temperatures are read by
optical pyrometers or sheathed
Initially use of microwaves was to process
thermocouples placed very close to the
microwave absorbing materials such as
surface of the sample. The relative
oxide or non-oxide ceramics only, but the
temperature readings are accurate to ± 5
concept has been extended to sinter o
C. The absolute temperature monitoring
metallic powders from commercial sources
is not established to anywhere near that
using a 2.45 GHz microwave field yielding
precision. Different controlled
dense products with improved mechanical
atmospheres such as air to H2, to forming
properties compared to those sintered
gas to oxygen can be used. Typically the
conventionally. These findings were
total sintering time would be ~ 90 minutes.
surprising in view of the reflectivity of the
With the use of microwave susceptors, the
bulk metals to the microwave frequencies.
heating cycle can be rapid.
The Microwave Research Group at the
It is reported that microwave sintered
Materials Research Institute of the
ceramic reinforced aluminium composites
Pennsylvania State University, however,
have good microstructure that helps to
made the first step advance in the
produce materials with better properties
microwave sintering of many traditional
such as light weight, dense, hard, better
and advanced ceramic materials such as
engineering properties including effective
alumina, mullite and hydroxyl apatite, by
electro magnetic interference (EMI)
demonstrating rapid sintering in time
shielding and vibration damping
intervals varying from 3-20 min. leading to
properties. The composites have also been
transparency and almost full density. This
reported to give rise to significant
same step function advance in ceramic
improvements in mechanical properties
processing has been extended to other
such as high strength, high stiffness, better
commercial ceramics such as zirconia, zinc
thermal properties like low coefficient of
oxide, perovskites, and silicon nitride.
thermal expansion and lower thermal
Microwave sintering can lead to near
conductivity, better acoustic property and
theoretical densities in most materials in
damping characteristics.
less than 30 min [6].
In the conventional heat treatment, the heat
Over the past decade microwave sintering
penetrates the body from outside to inside
chambers capable of processing a variety
creating a temperature gradient; therefore
of samples with different shapes and sizes,
it is not possible to heat those samples at a
and maintaining any temperature ranges
very high heating rate. This results in long
between RT to 1500 oC has been
cycle time and makes the process energy
developed, in exceptional cases up to 1800
intensive [7]. The consolidation of metal
to 2000 oC. The microwave generators are
matrix composites has been reported to
operated at a frequency of 2.45 GHz with
give rise to significant improvements in
mechanical properties such as high on sintering of metal powder in an
strength, high stiffness, better thermal unprecedented approach, sintering of fine
properties like low coefficient of thermal metallic powders, intermetallic compounds
expansion and lower thermal conductivity, and alloys was achieved by microwave
better acoustic property and damping sintering process wherein the sintered
characteristic and EMI shielding products showed better properties.
properties. The microwave sintered Rustum Roy et al. [14] have reported that
composites are expected to yield better the ability to sinter metals with
properties compared to the composite microwaves would assist in the preparation
products that are obtained through of high-performance metal parts needed in
conventionally sintering methods. many industries, for example, in the
automotive industry and Mg–Cu
M. Gupta et al. [1] have reported the nanocomposites have been developed
enhanced overall mechanical performance using microwave assisted sintering method
of metallic materials processed using two [15].
directional microwave assisted rapid
sintering. The feasibility of densifying α Unlike bulk metals that act as reflector, it
SiC powder compacts based on a liquid is believed that in finely divided metallic
assisted sintering approach by the use of powder, multiple scattering coupled with
microwave furnaces was examined by A. eddy current loss play a significant role in
Goldstein et al. [8]. They have also microwave absorption S Das et al. [16].
reported the properties of the material. During drying of high alumina castables,
Sutton [4] observed that in addition to
Ramesh D et al. [2] studied the microwave removing of water, microwave also heated
induced reaction sintering of NiAl2O4. The the ceramics. Some microwave ovens are
anisothermal reaction condition leading to available in the temperature range of 14000
enhanced reaction kinetics of NiAl2O4 C that are lined with non-microwave
formation have been achieved by the group absorbing refractories. Hence microwave
when they carried out simultaneous energy can be used for processing full
synthesis and sintering of NiAl2O4 from scale ceramic products. Microwave
NiO + Al2O3 powder mixture in just 15 processing is observed to be faster, highly
minutes in a 2.45 GHz microwave field. cost effective and products with superior
Mulletization and Densification of powder performance can be achieved. Ananda
compacts of 3 Al2O3 and 2 SiO2 by Kumar et al. [17] have studied the physical
microwave sintering were achieved by and morphological characteristics of
Piluso et al. [3]. aluminium cenospheres composite sintered
at high temperature in microwave.
Ebadzadeh et al. [9] also reported the
microwave assisted synthesis and sintering
of ceramics like mullite. A comparative 2.0 MICROWAVE
study of microwave and conventional
processing of MgAl2O4 based spinel Microwaves can be defined as that part of
material has been reported by Idalia the electromagnetic radiation spectrum
Gomez et al. [10]. having a wavelength ranging from about 1
mm to 1 metre in free space and the
Hermann Riedel et al. [11] have studied on frequency ranging from 300 MHz to 300
the simulation of microwave sintering with GHz. However, only narrow frequency
advanced sintering models. Panneerselvam bands centered at 915 MHz and 2.45 GHz,
et al. [12] have studied on the preparation 28-30 GHz and 80-81 GHz are actually
of Si3N4SiC composite by microwave permitted for research purposes (Fig.1).
route. Gerdes et al. [13] have reported that They are coherent and polarized waves
obeying the laws of optics. Depending
upon the type of material the microwave The degree of absorption by dielectric
may get transmitted, absorbed or reflected material is related to the materials complex
by the materials [4]. permittivity ε* (F/m)) which is composed
of two components i.e. ε, (dielectric
constant) the real part and an imaginary
part ε,, (dielectric loss factor) by:
=P/(Cp ρ) …(7)
6.0 RESULTS
FIG.5 MICROWAVE SINTERING 6.1 Jet Erosion Resistance Test
FACILITY
The conventionally and microwave
sintered samples were subjected to Jet
Erosion Test to assess the erosion to 2 kg and maximum wear loss occurs at
properties of the composites as per the 3 kg loading. The conventionally sintered
guidelines of ASTM G76 -04 standard samples showed higher wear loss than the
[24] which specifies the standard test microwave sintered samples.
method for ‘Conducting Erosion Tests by
Solid Particle Impingement Using Gas Wear Loss in g
Jets’. The test was conducted in the Jet
0.19 Conventionall
Erosion test rig using silica sand particles 0.14 y sintered
for impingement on the sample surface
using gas jets supplied through an air
0.030.02 Microwave
compressor. The erosion test was carried 0.02 sintered
0.01
out at angles of 30o, 45o, 60o and 90o.
1 2 3
It can be seen from the Fig. 8, that the
Load in kg
conventionally sintered sample showed
more erosion loss compared to the Fig.9 WEAR LOSS BEHAVIOUR
microwave sintered sample. The erosion
loss is slightly lower at angle of 90o for The wear loss for the conventionally
both the samples. The erosion loss varied sintered sample was 0.02 g at 1 kg load,
from high as 0.01 g to low as 0.009 g for 0.03 g at 2 kg load and 0.19 g at 3 kg
the conventionally sintered sample and loading whereas the microwave sintered
high as 0.0085 g to low as 0.0074 g for the sample exhibited wear loss of 0.01 g at 1
microwave sintered samples. kg load, 0.02 g at 2 kg load and 0.14 g at 3
kg load which is comparatively less than
Erosion Loss the conventionally sintered sample which
0.02 is about 50 % less at 1 kg, 33.3 % less at 2
kg and 26.3 % less at 3 kg load
Conventional
0.015 respectively.
Wt.loss in g
ly sintered
0.01 Microwave
6.3 Thermal Shock Resistance Test
sintered
0.005
The conventionally and microwave
0
sintered samples were subjected to
30 45 60 90 compressive yield strength (σy). The test
Angle of Erosion was performed in the Universal Testing
Machine (UTM) of Enkay make of
FIG.8 JET EROSION TEST RESULTS
capacity 100 T. The compressive yield
strength was evaluated for the sintered
6.2 Sliding Wear behaviour samples prior to, and after the thermal
The experimental work inVol.ved studying shock resistance test. The thermal shock
the sliding wear behavior of the resistance test comprised of heating the
aluminium-cenospheres metal matrix composite samples in a laboratory make
composites system as a function of sliding resistance type muffle furnace which is
distance for a constant sliding velocity and heated with kanthal element. The samples
applied load. The wear properties of the were heated to a temperature of 500 0C and
composite samples were carried out on a held at this temperature for 15 minutes
computer interfaced Pin on Disc apparatus. soaking time. Immediately the heated
It can be seen from the Fig. 9 that the samples are quenched in water bath held at
weight loss of both the samples are low at ambient temperature. This constitutes 1
1 kg load and which progressively thermal shock cycle. The composites
increases when the load is also increased samples are then evaluated for their
compression strength after the thermal
shock cycles. The conventionally and hydraulically operated Universal Testing
microwave sintered samples were Machine of capacity 100 T. The
subjected to thermal shock resistance tests compression strength was calculated by
comprising of 5, 10 and 25 thermal shock dividing the maximum load in kN by the
cycles and the compression strength values original cross section area (cm2) of the
before and after thermal shock cycles were sample and the values are converted and
measured. given in MPa.
It can be seen from Fig.10 that for the It is seen from Fig.11 that the compression
conventionally sintered samples, the strength of the conventionally sintered
compressive yield strength of the sample samples of aluminium powder is 125.0
125.0 MPa prior to thermal shock test. kg/cm2 whereas the compression strength
The strength decreased to 123.8 MPa of the microwave sintered samples of
which is 1.0 % after 5 cycles, 121.7 MPa aluminium powder showed 140.3 kg/cm2
which is 4.9 % decrease in the strength which is higher compared to the
after 10 cycles and 120.1 MPa which is conventionally sintered ones by about 11.0
5.4% reduction in the compression %.
strength after 25 cycles.
Compression strength
Thermal shock resistance 145 140.3
Compression strength kg/cm2
145
140
140
Compression strength kg/cm2
It can be seen that for the microwave Flexural Strength also known as Modulus
sintered samples, the compressive yield of Rupture (MOR), represents the highest
strength of the sample 140.3 MPa prior to stress experienced within the material at its
thermal shock test. The strength decreased moment of rupture. The flexural test was
to 138.8 MPa which is 0.9 % after 5 carried out as per the guidelines of ASTM
cycles, 133.7 MPa which is 4.7 % D 790-15 standard [25]. Flexural Strength
reduction in strength after 10 cycles and (σf) is measured in terms of stress, here
131.1 MPa which is 5.1 % reduction in given the symbol f was calculated as
compression strength after 25 thermal follows:
shock cycles. The microwave sintered
showed 8.4 to 10.9 % less reduction in Flexural Strength σf = …(8)
compression strength after thermal shock
cycles compared to conventionally sintered Where P= the actual load at the fracture
ones. point, L is the length of the supports
holding the test specimen, B is the width
6.4 Compression strength (σc) of the test specimen and D is the depth or
thickness of the test specimen and the units
The compression strength measurements of flexural strength is kg/cm2 or MPa.
were carried out in Enkay make Flexural Strength measurements of the
composites were carried out in a laboratory
make 3 point bending machine of capacity Brinell Hardness Number
ranging from 1 to 20 kg. 46
. 32
Flexural strength
Flexural strength kg/cm2
80 71.9
70
60 52
50 Conventionally sintered Microwave sintered
40
30 Fig.13 BRINELL HARDNESS
20 NUMBER
10
0 As can be seen from Fig. 13, the BHN
Conventionally Microwave sintered value for the conventionally sintered
sintered
aluminium was 32 and for the microwave
Fig.12 FLEXURAL STRENGTH sintered sample was 46. Microwave
sintered samples showed higher BHN
value by about 30.4 % compared to
It is seen from Fig. 12 that the flexural conventionally sintered one.
strength of the conventionally sintered
samples of aluminium powder is 52.0 7.0 DISCUSSIONS
kg/cm2 whereas the flexural strength of the
microwave sintered sample of aluminium Morteza Oghbaei et al. [18] has reported
powder showed 71.9 kg/cm2 which is that microwave sintering effectively assist
higher compared to the conventionally the forward diffusion of ions which
sintered ones by about 38.2 %. accelerates the sintering. This results in
matrix densification by grain growth
6.6 Brinell Hardness Number (BHN) process. Sintering process aids re-
crystallization, grain growth and
Hardness of the composite materials was
densification at high temperatures in the
determined using Zwick Werkstoff-
body that is being sintered. This
Prufmaschinen T 3212 B Digital Hardness
densification mechanism is strongly
tester. This hardness testing machine is
dependent on diffusion of ions between the
designed according to DIN 51225 and
same sample particles. The mechanism of
ISO/R 146 for hardness testing machines
grain growth rate is assisted by the grain
with optical indentation measuring
boundary diffusion process. It has been
devices. A precision measuring
found that intense microwave field
microscope with bright field illumination
concentration is active around the particles
was used to measure the Brinell
of the sample while sintering. The power
impressions. Brinell Hardness Number
of this microwave field between the
was calculated as : particles of the sample in the bulk of the
material is about 30 times higher than the
external field and this is sufficient to
…(9) ionize the sample particles at its surface.
This accelerates ionic diffusion which
where P = load on the indenting tool (kg) promotes rapid densification of the
on the sample, D = diameter of steel ball material is promoted under microwave
(mm), d = measure diameter at the rim of sintering.
the impression (mm).
Apart from the microwave radiation, the conventionally sintered products.
surrounding electromagnetic field also Microwave sintered powder metallurgy
effectively enhances the ionic diffusion products have round edged porosities
kinetics near the grain boundaries. The which is responsible for high ductility and
kinetic energy of the ions at the grain toughness [18].
boundary increases which thereby decrease
the activation energy required for the 6.0 CONCLUSIONS
forward ion jump and in the process
increases the barrier height for the reverse 1) The aluminium powder does not get
jump. This mechanism promotes forward converted into alumina (oxide of
diffusion of the inter grain ions which aluminium) when sintered in microwave at
accelerates the grain growth during temperature of 665 0C. The microwave
sintering. sintering takes place uniformly throughout
the bulk of the material. The sintering
By microwave sintering all the properties process is rapid, has high heating rates,
of a given material are enhanced by its reduced processing times, uniform
microstructural development in which the temperature throughout with minimal
densification of the material and thermal gradients.
coarsening occurs rapidly and effectively
throughout the bulk of the material. The 2) Microwave sintered samples showed
micro structural development depends on better tribological properties such as less
the parameters such as optimized wear and erosion losses compared to the
temperature, sintering time, heating rate conventionally sintered samples. The jet
and the pressure. The rapid heating rate erosion loss varied from high as 0.01 g to
achieved by microwave heating is the key low as 0.009 g for the conventionally
to produce products with a high sintered sintered sample and high as 0.0085 g to
density for a given microstructure and low as 0.0074 g for the microwave sintered
grain size compared to slow heating for the samples. The sliding wear loss of the
same sintered density by conventional microwave sintered samples were
heating. Since microwave sintering is a comparatively lower than the
non-contact sintering technique, the heat conventionally sintered sample which is
gets transferred to the product through about 50 % less at 1 kg, 33.3 % less at 2
electromagnetic radiation. By microwave kg and 26.3 % less at 3 kg load
sintering large amount of heat can be respectively.
transferred to the material’s interior which
reduces differential sintering to a large 3) The microwave sintered showed better
extent. Hence the microwave sintered thermal shock resistance compared to the
products have finer micro-structural conventionally sintered samples.
development, with uniform grain growth Microwave sintered sample had higher
and grain size distribution coupled with compression strength by about 8.4 to 10.9
higher densification of the product thereby % after thermal shock cycles compared to
leading to enhanced engineering conventionally sintered ones.
properties.
4) The compression strength of the
The above are the reasons attributed to the conventionally sintered was 125.0 kg/cm2
microwave sintered products which yield whereas the compression strength of the
better tribolobical, mechanical and thermal microwave sintered samples of aluminium
properties in the powder pressed samples. powder showed 140.3 kg/cm2 which was
The powder pressed metal samples higher by about 11.0 %.
produces finer grain size with shape of the
porosity which is different compared to
5) The Flexural strength of the copper and nickel steel PM parts,
conventionally sintered samples of Powder Metallurgy, Vol. 48, No.1, pp.
aluminium powder was 52.0 kg/cm2 39-45, 2005.
whereas the flexural strength of the
microwave sintered sample of aluminium [7] C Lutgard, De Jonghe and N
powder showed 71.9 kg/cm2 which was Mohamed Rahaman, Sintering of
higher compared to the conventionally Ceramics, Handbook of Advanced
sintered ones by about 38.2 %. Ceramics, Chapter 4, pp. 187-253.
6) Microwave sintered samples showed [8] A Goldstein, W D Kaplan and A
higher BHN value by about 30.4 % Singurindi, Liquid assisted sintering of
compared to conventionally sintered one. SiC powders by MW (2.45 GHz)
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