Special Issue: Advances in Processing & Characterisation of Materials

Proc IMechE Part E:

Effects of nano filler powder J Process Mechanical Engineering

1–8
© IMechE 2022
during microwave-based joining Article reuse guidelines:
sagepub.com/journals-permissions
of SS304 butt joints DOI: 10.1177/09544089221107992
journals.sagepub.com/home/pie

Sony Salot1, Shankar Sehgal2 , B. S. Pabla1, Harmesh Kumar2,

Chander Prakash3 , Shashi Bahl4 and Kuldeep K Saxena5

Abstract
Filler powder plays an important role during microwave hybrid heating-based joining process. In this work, nano-size
nickel powder has been taken as filler material for preparing SS304-SS304 butt joints. Effects of size of nickel powder
on mechanical properties (strength and hardness) of joints have been investigated. Scanning electron microscope tests
show that the joints possess uniform microstructure. Energy dispersive spectroscopy tests demonstrated the presence
of elements (Chromium, iron, carbon, silicon, manganese, phosphorus) other than filler powder (Nickel) in the joint
region thereby confirming complete melting of joint region and also transfer of carbon from graphite separator sheet
to joint region during microwave processing. Micro-hardness test results showed that nano-size filler powder-based joints
are less prone to surface wear than corresponding micro-size filler powder-based joints. Micro-tensile strength of nano-
size nickel powder-based joints is also far better than micro-size filler powder-based joints.

Keywords
Butt joints, filler material, joining, microwave hybrid heating, micro-hardness, strength

Date received: 25 February 2022; accepted: 17 May 2022

Introduction tan δ indicate respectively, the capabilities of material to

Joining is a manufacturing process which helps in achieving
desired components by joining two or more sub-
components together. Conventional joining techniques
have some limitations to join metals and alloys such as
chances of having steep thermal gradients resulting into
cracks formation, poor joint-quality, non-uniform micro-
structure, energy losses, high energy consumption, environ-
mental pollution etc.1–4 These problems can be minimized
by using microwave hybrid heating (MHH) based joining
process instead of conventional joining processes. During
microwave processing, interaction of microwaves and mate-
rials takes place at molecular level; which leads to energy
conversion through dipole rotation and ionic conduction.
The dielectric properties of processed materials decide the
level of interaction of microwaves with the target materials.
Absorption of microwaves in dielectric material depends
upon the complex permittivity and loss tangent.5
ε = (ε′ − jε′′ ) (1)
store and to efficiently convert absorbed energy to heat.
Ceramics, ceramics composites and polymers are good
absorbers of microwaves. Hence they can be easily pro-
cessed through microwave processing. On the other hand,
metallic materials are very good reflectors of microwaves
because of very low skin depth.
Mechanical and micro-structural characterization of
mild steel (MS) based joints was done by Bansal et al.6
Formation of substitutional type of solid solution at inter-
face region was confirmed through X-ray diffraction
1
Department of Mechanical Engineering, National Institute of Technical
Teachers Training and Research, Chandigarh, India
2
Mechanical Engineering, UIET, Panjab University, Chandigarh, India
3
School of Mechanical Engineering, Lovely Professional University,
Phagwara, India
4
Department of Mechanical Engineering, I.K. Gujral Punjab Technical
University Hoshiarpur Campus, Hoshiarpur, India
5
Mechanical Engineering Department, GLA University, Mathura, India

ε′′ Corresponding authors:

tan δ = (2)
ε′
where ε, ε′ , j, ε′′ and tan δ are complex permittivity, abso-
lute permittivity, electrical polarizability, dielectric loss
factor and loss tangent respectively. ε′ is related to the
ability of microwaves to penetrate into material. ε′′ and
Shankar Sehgal, Mechanical Engineering, UIET, Panjab University,
Chandigarh, 160 014, India
Emails: sehgals@pu.ac.in; shankar.sehgal@alumni.iitd.ac.in
Chander Prakash, School of Mechanical Engineering, Lovely Professional
University, Phagwara
Email: chander.mechengg@gmail.com
2 Proc IMechE Part E: J Process Mechanical Engineering 0(0)
(XRD). Studies of microwave joints formed using tung-
sten carbide bearing alloy was carried out by Gupta
et al.7 Characterization results revealed fine microstruc-
ture and proper fusion of specimens when using mixture
of tungsten carbide bearing alloy (EWAC–1002 ET)
(95%) and resin (5%) as interface powder. Bansal et al.8
performed characterization of stainless steel (SS) −316
joints fabricated through MHH. Melting of filler powder
particles and formation of dense and homogenous joint
through metallurgical bonding with substrates was con-
firmed by scanning electron microscope (SEM) images.
Effects of microwave joining process parameters on
joint strength for 1018 MS specimens were investigated
by Dwivedi et al.9 They concluded that joint strength
decreases with increased rated power output. This is due
to the fact that with increase in power level, there was
an increase in rate of heat generation which resulted
into very high temperature of joint region. At such high
temperature, different gases were easily absorbed into
molten metals. But, during subsequent cooling and solidi-
fication process, such gases tend to be released thereby
leading to blow holes and porosity related issues, which
finally results in the formation of weaker joints.
Another method to increase the joint strength was to
increase the welding time and temperature. Microwave
energy was successfully utilized to achieve joining of dis-
similar metals by Bansal et al.10 They used infrared pyrom-
eter based experimental set-up and found that optimum
temperature for joining of MS and SS316 was 1360 °C.
Characterization of joints of aluminium alloy processed
through microwave joining using aluminium powder as
bonding agent was carried out by Singh et al.11 Badiger
et al.12 characterized the Inconel 625 joints processed
Figure 1. Joint dimensions.
through microwave joining. They tested microhardness at
interior of joint, joint interface and base metal. Average
microhardness at the joint interface was 395 ± 4 Hv
which was much better than that of the joint zone where
it was observed to be 360 ± 20 Hv only. Structure and prop-
erty correlations of joints of Inconel 718 processed using
microwave energy were investigated by Bansal et al.13
Recently, concept of selective hybrid carbon micro-
wave joining was proposed and implemented by Bagha
et al.14 to join SS304-SS304 using different sizes of
filler material. They used micro-size nickel powder as
interface material. Tensile strength 337 MPa, surface
hardness 238 Hv on heat affected zone (HAZ) and
356 Hv on fusion zone was observed for joints made
with 20 µm size nickel powder. It was concluded that
powder size played an important role in deciding the prop-
erties of a joint. However, during that work, size of filler
powder was limited to micro-size only. Therefore, in
order to further investigate the effect of nano-size filler
powder on joint properties, this work was carried out. In
this work, joint micro-structure has been investigated
using SEM and energy dispersive spectroscopy (EDS).
Mechanically, the joints have been tested for micro-
hardness and tensile strength. Characterization results of
nano-filler powder-based joints produced during this
work have also been compared with already published
results of micro-size powder-based joints.
Materials and methods
As shown in Figure 1, substrates with size 40 mm overall
length, 3 mm width and 5 mm thickness were cut from
SS304 plate as per ASTM designation E8/E9 standard
Salot et al.
Figure 2. Particle size distribution of filler powder.
using wire electric discharge machine Elektra make,
model no. ELCUT 234 situated at Chandigarh industrial
and tourism development corporation, Chandigarh.
Nano-size nickel powder of 99.9% purity with particle
size less than 80 nm was used as filler material. Particle
size analysis of powder is shown in Figure 2. Highest frac-
tion of particle size was 70 nm.
Schematic placement of different materials inside a
microwave applicator of 800 W working at 2.45 GHz
have been shown in Figure 3. Top face of the insulation
brick carried a slot, into which the SS304 specimens
were placed along with slurry at interface region of the
butt joint to be produced. Slurry was prepared by
mixing nickel nano-filler powder with epoxy resin
(Bisphenol-A, Blumer 1450XX) in a ratio 75:25 by
weight. Fusion zone was then covered with a graphite
sheet of 1 mm thickness. Presence of graphite sheet is
used to prevent mixing of filler powder and susceptor
material. This assembly was then covered with another
refractory brick to prevent direct contact of microwaves
with metallic parts. Upper refractory brick had a vertical
drilled hole of 10 mm diameter that acted as a charcoal
feeder. This was done to achieve the selective heating
of fusion zone.14 Vertical cavity type feeder was filled
with charcoal that acts as susceptor material. In order to
obtain good welded joints, it is pre-requisite to use
optimal processing time. The optimal processing time
was evaluated through trial experiments and found to be
360 s. Processing time less than 360 s would result in for-
mation of improper joints; while longer time duration
would result in excessive melting of portions of the speci-
mens near the joint region. After microwave switched off,
whole setup of joining process was kept for approxi-
mately 15 s for cooling.
It is quite difficult to microwave process bulk metals
because of their low skin depth. This problem was over-
come using principle of MHH, which helps in increasing
the skin depth of powder particles so that they are able to
directly couple with microwaves at high temperature.
Initially, due to interaction with microwaves, charcoal
starts burning, and heat is transferred to interface slurry
3
Figure 3. Disassembled view of experimental setup.
through graphite sheet. At higher temperature, nickel
powder particles of the slurry start direct coupling with
microwaves and absorb energy from microwaves.
Blumer gets evaporated at higher temperature and space
in fusion zone gets filled with melted powder particles
of Nickel. Transfer of energy through conduction mode
is responsible for melting the faying surfaces of substrates
up to narrow layer owing to direct contact of heated nickel
powder particles. Thus, small welded zone of melted
nickel powder particles and thin molten layer of base
material was formed. Red hot specimens immediately
after joining process have been photographed in
Figure 4(a). Specimens after air-cooling have been
shown in Figure 4(b). Homogenous and dense welded
joint was obtained through metallurgical bonding of
filler material with substrate. Then the joints were
polished as shown in Figure 4(c). Polished joints were
then characterized through physical and mechanical
testing. Microstructure of welded joints was analyzed
through SEM and EDS. Chemical composition of fusion
zone was also analyzed using SEM. Hardness tests were
conducted on Vickers hardness tester (Wilson make,
Germany VICKER’S 452 SVD model) with load of
1 Kgf for 15 s. Finally, the specimens were tested for
their tensile strength as also clear from Figure 4(d).
4 Proc IMechE Part E: J Process Mechanical Engineering 0(0)

Figure 4. Different stages of the workpieces after joining (a) red hot workpieces immediately after joining (b) workpieces after air
cooling (c) polished workpieces before hardness testing (d) workpieces after tensile testing.

Figure 5. SEM images showing (a) fusion zone, HAZ and base metal (b) fusion zone.

Results and discussion base-metal-zone. SEM images show that homogeneous

Nano-size nickel filler powder based SS304-SS304 tensile
specimens were investigated to observe their micro-
structure and mechanical properties. SEM micrographs
of various regions of the butt joint of SS304 processed
through microwave heating have been presented in
Figure 5. Well fused and fine microstructure of welded
joint of nickel powder and base materials are visible in
Figure 5(a). Three zones A, B and C are clearly visible
in Figure 5(a). Zone A refers to the melt-zone where
melting of nano-filler powder is seen. Grain formation is
observed in zone A, which is also the joint region
where nickel based filler powder is placed. Zone B
shows the region where boundary of the base metal gets
diffused with the nano powder. This zone has been
termed as a transition-zone because it represents the tran-
sition from zone A to zone C. Zone C shows the
and dense microstructure has been obtained in the
fusion zone A. Homogeneity of microstructure is attribu-
ted to uniform heating of nickel powder particles by the
microwave heating effect. Grain growth is clearly seen
in micrographs of joints from HAZ (zone B) to core of
the fusion zone (zone A). Figure 5(b) confirms complete
melting of nickel powder particles and it also shows the
formation of carbides in the joint region. Formation of
carbides is due to reaction of carbon present in the graph-
ite sheet with other elements present in the melting zone.
Presence of such carbides in zone A is expected to help in
increasing the hardness of joint region A, which was later
confirmed through micro-hardness tests also. Better hard-
ness helps in improving upon the useful life of joint
against wear-based service conditions. Microstructure of
base alloy (zone C) was also checked and as expected
Salot et al.
Figure 6. FESEM image of fractured joint.
Figure 7. EDS spectrum of joint region.
there was not any presence of carbides in the base alloy.
Absence of carbides in zone C and its presence in zone
A shows that the melting as well as joint formation
process has been successfully completed. Fractured
joints after tensile testing have been investigated
through FESEM. as shown in Figure 6. It indicates the
brittle nature of fractured joints. Presence of carbides at
grain boundaries obstructs longer deformations in the
joints. Also, intermetallics formed during higher tempera-
ture joining are responsible for further reducing the ductil-
ity of joints.
EDS spectrum of weld bead of SS304 is shown in
Figure 7. EDS spectrum of fusion zone has confirmed
5
the presence of Nickel, Iron and Chromium which deter-
mines complete inter-mixing of base metal elements and
bonding material. The increased presence of carbon in
EDS graph is attributed to graphite sheet and charcoal
powder which was used to initiate the Joining process.
Peaks of nickel in EDS spectrum is comparable with
iron peak in fusion zone which confirms the melting of
nickel powder used as interlayer between the two speci-
mens to be joined. EDS spectrum also confirms the pres-
ence of carbon in the fusion zone. The presence of
carbon in fusion zone can be attributed to the use of graph-
ite sheet placed on bottom of the vertical cavity charcoal
feeder. Graphite sheet also helps in keeping the charcoal
6 Proc IMechE Part E: J Process Mechanical Engineering 0(0)
powder and filler powder separate apart. Diffusion of
carbon from graphite sheet to the fusion zone helps in
increasing hardness of the fusion zone which is very
much needed for improving upon the surface wear proper-
ties of the joint. Melting of thin layer of substrates from
both side and their diffusion with nickel powder particles
into the interface region has also been confirmed through
the presence of small peaks of chromium and silicon ele-
ments in EDS spectrum of joints. Due to proper melting
of facing-ends of the SS specimens, chromium as well
as silicon elements also diffuse further into the fusion
zone A and thereby resulting in corresponding peaks in
the EDS spectrum of the joint region.
In order to investigate their mechanical properties, the
processed joints were tested for hardness on surface of
the joint using Vickers hardness tester under 1 Kgf load
for 15 s. Hardness testing was performed on two processed
specimens and one standard specimen of base metal. Three
measurements at each region were taken for measurement
of hardness. Average hardness of base alloy, HAZ and
fusion zone was measured to be 186, 341 and 436 Hv
respectively. Hardness of HAZ as well as fusion zone is
significantly higher than that of base metal during this
nano-filler powder-based microwave joining process.
Table 1 shows a comparison of hardness based results
of presently developed nano-filler powder based joints
Table 1. Comparison of hardness and tensile strength results with previous work.
Property Micro-powder (20 µm) based joints14
Hardness on base metal (Hv) 198
Hardness on HAZ (Hv) 238
Hardness on fusion zone (Hv) 356
Tensile strength (MPa) 337
Percent elongation (%) 1.67
Figure 8. Stress-Strain curve of SS304 unwelded specimen.
with previously published results of micro-size powder
based joints.14 In both cases, hardness of weld as well
as HAZ is higher than that of the corresponding base
alloy. Percent increase in hardness of HAZ with reference
to corresponding base alloy is 83% for the presently
developed nano-size filler powder based joints; which is
much higher than the 20% increase reported earlier for
micro-size filler powder based joints by Bagha et al.14
Moreover, hardness on weld during present work on
nano-size filler powder based joints is 2.34 times the hard-
ness of corresponding base alloy; however such increase
was only 1.8 times during previous published work with
micro-size filler powder based joints.14 Thus, hardness
results of weld as well as HAZ of nano-filler powder-
based joints are far better than their micro-size powder-
based counterparts. Overall, it is observed that hardness
of nano-filler powder-based joints is much better than
that of micro-filler powder-based joints. This is due to
the fact that in very small size nano-filler powder it is
easier for the carbon elements to enter and then further
diffuse throughout the joint region, thereby increasing
the hardness properties. However, in a region already
filled with bigger size filler powders carbon elements do
not get that easily penetrate into the joint region thereby
resulting in lesser hardness of micro-size filler powder-
based joints than the nano-powder based joints.
Nano-powder (<80 nm) based joints
186
341
436
351
1.45
Salot et al.
Figure 9. Stress-Strain curve of welded joint.
Joint strength is an important parameter while design-
ing any product. Therefore, tensile strength of the joints
was also investigated during this work. Moreover,
present tensile strength results were also compared with
previously published similar results of Bagha et al.14
The stress-strain curve for SS304 unwelded and welded
specimen is shown in Figures 8 and 9 respectively.
Yield was calculated by extension-under-load method
as per ASTM E8 at 0.2% strain. Other parameters such
as maximum force, displacement at maximum force,
maximum displacement, tensile strength, elongation,
reduction in area, yield load, yield stress were respect-
ively observed to be 11.96 kN, 9.40 mm, 11.70 mm,
797.33 MPa, 30%, 60%, 2.02 kN, 134.67 MP for
unwelded specimen; and 7.02 kN, 8.20 mm, 8.80 mm,
351 MPa, 20%, 40%, 0.86 kN and 43 MPa for welded
joint. Average tensile strength of joints was 351 MPa
which was 44.02% of the tensile strength of unwelded
specimen.
Further, Table 1 shows that the average tensile strength
of present joints is 351 MPa which is better as compared
to 337 MPa obtained earlier.14 Further, an elongation of
1.45% was achieved during present work as compared
1.67% elongation for past joints produced by using
20 µm powder. It is observed that ductility of the joints
is significantly less as compared to the other welding pro-
cesses. This is due to the addition of carbon from graphite
sheet to the fusion zone during the proposed joining
process, which makes it hard and brittle. Thus, the nano-
filler powder-based joints are stronger but less ductile than
7
their micro-size powder-based counterparts. Reduced
ductility might also have been resulted because of
increased carbon content present in nano-filler powder-
based joint compared to the micro-filler powder-based
joints. Increased carbon content in the joint region is
helpful in attaining higher hardness values but at the
same time it also results in increased brittleness or
reduced ductility of the joint.
Overall, comparison of mechanical properties of nano-
size filler powder based joints with that of the micro-size
filler powder based joints shows that the former possess
better hardness and tensile strength however it lacks in
terms of ductility of the joint. For further detailed investi-
gations in future, one can formulate a multi-objective opti-
mization problem involving maximization of hardness,
tensile strength and ductility of the MHH based processed
joints; wherein tensile strength and ductility of the joint
will appear as two conflicting objectives. Solution to
such multi-objective optimization problem will help in
identifying the optimal size of filler powder which can
be used to produce MHH based joints with optimum hard-
ness, tensile strength and ductility.
Conclusions
In the present work, use of nano-filler powder filler mater-
ial has been explored for MHH based joining of SS304
specimens. Physical and mechanical characterization of
welded joints was performed and compared with existing
literature. Major findings of this work are:
8 Proc IMechE Part E: J Process Mechanical Engineering 0(0)
• Uniform and fine microstructure has been achieved.
Clearly visible joint has been confirmed through SEM
images depicting three distinct zones, viz. melt-zone,
transition-zone and base-metal-zone. Proper fusion
between base metal and nickel powder takes place
during processing.
• For nano-filler powder-based joints, hardness of HAZ
and fusion zone is respectively 83% and 134% higher
than that of base alloy.
• Use of nano-filler-powder results in harder joints than
micro-size filler powder-based counterparts, which is
a significant achievement of this work. Hardness of
HAZ as well as weld zone of nano-filler powder-based
joints is much higher than their micro-sized based
counterparts.
• Nano-filler powder joints are stronger than micro-size
filler-powder based joints. However, the increased
tensile strength is accompanied with corresponding
decreased ductility of joint.
Declaration of conflicting interests
The author(s) declared no potential conflicts of interest with
respect to the research, authorship, and/or publication of this
article.
Funding
The author(s) received no financial support for the research,
authorship, and/or publication of this article.
ORCID iDs
Shankar Sehgal https://orcid.org/0000-0003-1874-0632
Chander Prakash https://orcid.org/0000-0003-0856-9712
Shashi Bahl https://orcid.org/0000-0001-9294-8226
Kuldeep K Saxena https://orcid.org/0000-0003-4064-5113
References
1. Pal M, Kumar V, Sehgal S, et al. Microwave hybrid heating
based optimized joining of SS304/SS316. Mater Manuf
Process 2021; 36: 1554–1560.
2. Bagha L, Sehgal S, Thakur A, et al. Low cost joining of
SS304-SS304 through microwave hybrid heating without
filler-powder. Eng Res Express 2019; 1: 1–32.
3. Pal M, Sehgal S, Kumar H, et al. Use of nickel filler powder
in joining SS304-SS316 through microwave hybrid heating
technique. Met Powder Rep 2020; 18: 45–56.
4. Pal M, Sehgal S and Kumar H. Optimization of elemental
weight % in microwave processed joints of SS304 /
SS316 using Taguchi philosophy. J Adv Manuf Syst 2020;
19: 543–565.
5. Gupta M and Leong EWW. Microwaves and metals.
Singapore: John Wiley and Sons (Asia) Pte Ltd, 2007.
6. Bansal A, Sharma AK and Das S. Metallurgical and mech-
anical characterization of mild steel-mild steel joint formed
by microwave hybrid heating process. Sadhana - Acad Proc
Eng Sci 2013; 38: 679–686.
7. Gupta P, Kumar S and Kumar A. Study of joint formed by
tungsten carbide bearing alloy through microwave welding.
Mater Manuf Process 2013; 28: 601–604.
8. Bansal A, Sharma AK, Kumar P, et al. Characterization of
bulk stainless steel joints developed through microwave
hybrid heating. Mater Charact 2014; 91: 34–41.
9. Dwivedi SP and Sharma S. Effect of process parameters on
tensile strength of 1018 mild steel joints fabricated by micro-
wave welding. Metallogr Microstruct Anal 2014; 3: 58–69.
10. Bansal A, Sharma AK, Kumar P, et al. Investigation on
microstructure and mechanical properties of the dissimilar
weld between mild steel and stainless steel-316 formed
using microwave energy. Proc Inst Mech Eng Part B J
Eng Manuf 2016; 230: 439–448.
11. Singh S, Suri NM and Belokar RM. Characterization of
joint developed by fusion of aluminum metal powder
through microwave hybrid heating. Mater Today Proc
2015; 2: 1340–1346.
12. Badiger RI, Narendranath S and Srinath MS. Joining of
inconel-625 alloy through microwave hybrid heating and
its characterization. J Manuf Process 2015; 18: 117–123.
13. Bansal A, Sharma AK, Kumar P, et al. Structure–property
correlations in microwave joining of inconel 718. JOM
2015; 67: 2087–2098.
14. Bagha L, Sehgal S, Thakur A, et al. Effects of powder size of
interface material on selective hybrid carbon microwave
joining of SS304–SS304. J Manuf Process 2017; 25: 290–295.