MICROWAVE SINTERING OF W-18CU AND

W-7NI-3CU ALLOYS
Avijit Mondal1*, Anish Upadhyaya1 and Dinesh Agrawal2
1
Department of Materials & Metallurgical Engineering
Indian Institute of Technology, Kanpur 208016, India
2
The Pennsylvania State University, University Park, PA 16802, USA
*
avijitm@iitk.ac.in

Microwave processing is emerging as an innovative and highly effective material processing

method offering many advantages over conventional methods, especially for sintering applications.
It is recognized for its various advantages, such as: time and energy saving, rapid heating rates,
considerably reduced processing cycle time and temperature, fine microstructures and improved
mechanical properties which lead to better product performance. Major constraints in conventional
sintering of refractory material such as tungsten and its alloys are high sintering temperatures and
long soaking times which cause abnormal grain growth and lead to poor mechanical properties.
They get further aggravated at smaller (submicron and nano) tungsten powder sizes. This study
describes recent research findings; W-18Cu and W-7Ni-3Cu alloys have been successfully con-
solidated using microwave heating which resulted in an overall reduction of sintering time of up
to 80%. The microwave sintered samples exhibited finer microstructure and superior mechanical
properties when compared with the conventional samples.
Submission Date: 6 August 2008
Acceptance Date: 7 January 2009
Publication Date: 16 January 2009

INTRODUCTION processed via sintering at temperatures ranging

Tungsten is a refractory metal with a melting
point of 3420°C. Because of its high melting
point, tungsten and its alloys are mostly consoli-
dated through powder metallurgy (P/M) tech-
niques, though for some specific applications
mechanical alloying and infiltration techniques
are also employed. Most commonly, liquid phase
sintering (LPS) is used for consolidating these
alloys. The technique offers the advantage of rel-
atively lower sintering temperatures, enhanced
densification, microstructural homogenization
and near theoretical density. These alloys are
Keywords: Tungsten heavy alloys, microwave sintering,
microstrutures
Guest Editor: Dr. Satoshi Horikoshi, Tokyo University of
Science, Chiba, Japan
from 1200°C to 1500°C when at least one of the
constituents melts and facilitates the sintering
process.
Depending upon the composition, these
alloys also offer a favorable combination of
high thermal conductivity, low thermal expan-
sion coefficient, high density, high strength and
ductility, good corrosion resistance and ease of
machinability. These alloys, because of their
wide range of properties, are strategically very
important and have a wide range of applications,
such as electrical contact, heat spreaders, elec-
tronic packaging, radiation-shield, counter-bal-
anced weights, and kinetic energy penetrator in
defense industry [Upadhyaya, 2001]. Because of
technological demands and strategic concerns,
there is considerable interest worldwide in con-
solidating the tungsten based alloys for thermal

International Microwave Power Institute 43-1-11

management and defense industry applications.
Each application has its own specific require-
ments as far as the properties are concerned.
In general for most of the applications, near
theoretical density, dimensional stability, high
hardness, toughness and very high ductility are
important [German, 1996].
In order to avoid thermal shock, processing
of tungsten heavy alloys in a conventional fur-
nace involves heating at a slower rate (<10°C/
min) and with an isothermal hold at intermittent
temperatures. This not only increases the process
time, but also results in significant microstruc-
tural coarsening (W grain growth) during sinter-
ing, leading to the degradation of mechanical
properties. This problem is further aggravated
when the initial powder size is extremely fine.
Hence, it is envisaged that a fast heating rate
would mitigate this problem. One of the tech-
niques to achieve fast and relatively uniform
sintering is through microwaves. Microwaves
interact with individual particulates within the
pressed compacts directly, and thereby provide
rapid volumetric and uniform heating [Clark
and Sutton, 1996]. This technique offers many
advantages over conventional methods for con-
solidation. The main advantages include rapid
sintering, fine microstructure, energy savings
and improvements in the mechanical properties
of the sintered products. Until recently, micro-
wave processing was mostly restricted to ceram-
ics, cemented carbides and ferrites [Clark and
Sutton, 1996; Gerdes et al., 1996; Agrawal et al.,
2001; Rodiger et al., 1998; Porada and Borchert,
1996-97; Tsay et al., 2001]. Applicability of
microwave sintering to metals was ignored due
to the fact that they reflect microwaves. Roy et
al. [1999] reported that particulate metals can
be heated rapidly in microwaves. This has led
to the use of microwaves to consolidate a range
of particulate metals and alloys. Researchers
have reported microstructural refinement due
to rapid heating, significant reduction in pro-
cess time, elimination of brittle intermetallic
formation and superior mechanical properties
43-1-12 Journal of Microwave Power & Electromagnetic Energy ONLINE
in microwaves [Saitou, 2006; Jain et al., 2006;
Upadhyaya et al., 2008; Mondal et al., 2008].
The present study describes the consolidation of
tungsten based alloys using microwave energy.
Conventional sintering has also been conducted
to compare the effectiveness of the microwave
process.
EXPERIMENTAL PROCEDURE
For the present study the W-18Cu powders were
supplied by Osram Sylvania, Towanda, USA.
The elemental W (d50: 4.2μm) , Ni (d50: 11.0 μm)
and Cu (d50: 47.0 μm) powders were supplied
by Kennametal-Widia India Ltd., Bangalore;
International Specialty Products (INCO), USA;
and ACu Powder International, LLC, USA re-
spectively. The detailed powder characteristics
have been reported elsewhere [Mondal et al.,
2008]. The elemental W, Ni and Cu powders
were mixed in a required proportion in a turbula
mixer for about 60 min to prepare 90W-7Ni-3Cu
(wt.%) alloy composition. Powders were pressed
in a die of 16 mm inner diameter to make the
green compacts of approximately 6 to 8 mm in
height. The pressure was applied uniaxially in a
50T hydraulic press with floating die, using zinc
stearate as a die wall lubricant. All the samples
were compressed at pressures of 200 MPa.
To study the densification behavior, the green
compacts were sintered using conventional and
microwave furnaces. The sintering temperatures
selected for the liquid phase sintering of W-18Cu
and 90W-7Ni-3Cu were 1300°C and 1450°C,
respectively. Sintering was carried out with a
constant heating rate 5°C/min in a flowing H2
atmosphere. Microwave sintering of the green
compacts was carried out using a multi-mode
cavity 2.45 GHz, 6 kW commercial microwave
furnace. The temperature of the sample was
monitored using an optical pyrometer with the
circular crosswire focused on the sample cross-
section.
The sintered density was obtained by both di-
mensional measurements as well as Archimedes’
Vol. 43, No. 1, 2009
 (a)
Figure 1. Thermal profiles of (a) W-18Cu and (b) W-7Ni-3Cu alloys sintered using conventional
and microwave furnaces.
density measurement technique. Metallographic
techniques were employed on the sintered
samples. The scanning electron micrographs of
as-polished samples were obtained by a scanning
electron microscope (model: FEI quanta, Neth-
erlands) in the secondary electron (SE) and back
scattered (BSE) mode. Phase determination and
phase evolution, if any were studied for all the
samples with the help of X-Ray Diffractometer
(Model: RICH. SEIFERT & Co., GmbH & Co.
KG, Germany). The experimental variables of
the XRD are as follows: scan rate-3°/min, tar-
get-Cu, and power-30kVx20 mA. Bulk hardness
measurements were performed on polished sur-
faces of sintered cylindrical compacts at a load
of 5 kg using Vickers hardness tester (model:
V100-C1, supplier: Leco, Japan). The load was
applied for 30 s. Micro-hardness tester (model:
Leitz 8299, Germany) was used to perform the
micro-hardness tests on the tungsten grains and
matrix phases. The loads applied for micro-hard-
ness test was 50 g for 15 s. Ten measurements
were taken at random locations for each macro
and micro-hardness test to determine statistically
accurate results.
International Microwave Power Institute
(b)
RESULTS AND DISCUSSION
Figs. 1(a) and 1(b) compare the thermal profiles
for both the compositions heated in both the
conventional and microwave furnace. It is in-
teresting to note that for both, the compositions
couple with microwaves and heat up rapidly.
The overall heating rates in the microwave fur-
nace were 15° and 22°C/min for W-18Cu and
90W-7Ni-3Cu, respectively. Taking into con-
sideration the slow heating rate (5°C/min) and
isothermal holds at intermittent temperatures in
conventional furnace, there is about a 70 to 80%
reduction in the process time during sintering of
all the compositions in the microwave furnace.
Despite such a fast heating rate, no micro- or
macro-cracking was observed in all microwave-
sintered samples. This underscores the efficacy
of volumetric heating associated with micro-
waves. Figs. 2(a) and 2(b) show the effect of
the heating mode upon the sintered density and
densification parameter for both the composi-
tions. It is noteworthy to mention that in both, a
heating mode more than 98% of its theoretical
density has been achieved. Microstructural ob-
servation was made to confirm the effect of the
heating mode on grain coarsening phenomenon
and microstructural homogeneity.
43-1-13
 Table 1. Effect of heating mode on the hardness of W-18Cu and 90W-7Ni-3Cu compacts.
Heating mode W-18Cu
Bulk hardness
Conventional 325±12
Microwave 376±15
For both the compositions, microwave sintering
results in a more refined microstructure, which
in turn, leads to enhancement of hardness.
ACKNOWLEDGMENTS
This collaborative research was done as a part of
the Center for Development of Metal-Ceramic
Composites through Microwave Processing,
funded by the Indo-US Science and Technol-
ogy Forum (IUSSTF), New Delhi. The authors
thank Dr. D. Houcke and Mr. P. Sedor of Osram
Sylvania, Towanda, USA for supplying the
powders.
REFERENCES
Agrawal, D.K., A.J. Papworth, J. Cheng, H. Jain, and
D.B. Williams (2001). “ Microstructural Examina-
tion by TEM of WC/Co Composites Prepared by
Conventional and Microwave Processes.” Proc. 15th
International Plansee seminar, v.2, G. Kneringer, P.
Rodhammer and P. wilhartitz (eds.), Plansee AG,
Reutte, Austroa, pp.677-684.
Clark, D.E and W. H. Sutton (1996). “Microwave Pro-
cessing of Materials.” Ann. Rev. Mater. Sci., 26, pp.
299-331.
Gerdes, T., M. W. Porada, K. Rodiger, and K. Dreyer
(1996). “Microwave Sintering of Tungsten Carbide
– Cobalt Hardmetals.” Mater. Res. Soc. Symp. Proc.,
430, pp.175-180.
German, R.M. (1996). Sintering Theory and Practice. J.
Wiley, New York.
Jain, M., G. Skandan, K. Martin, K. Cho, B. Klotz, R.
Dowding, D. Kapoor, D. Agarwal, and J. Chang
(2006). “Microwave Sintering: A New Approach to
Fine-Grain Tungsten-I.” International Journal of
Powder Metallurgy, 42(2), pp.45-50.
Mondal, A., D. Agarwal, and A. Upadhyaya (2008).
“Microwave Sintering of Tungsten Based Alloys.”
43-1-16 Journal of Microwave Power & Electromagnetic Energy ONLINE
90W-7Ni-3Cu
Bulk hardness Micro-hardness
W grains Matrix
301±21 445±15 333±13
328±12 442±9 312±18
International Conference on Tungsten,Refractory and
Hardmaterials VII , Washington DC, USA.
Mondal, A., and A. Upadhyaya (2008). “Phase Evolution
of Tungsten Alloys during Microwave Sintering.”
unpublished research.
Porada, M.W., and R. Borchert (1996-1997). “ Microwave
Sintering of Metal-Ceramic FGM.” Proceedings of
the 4th International Symposium on Functionally
Graded Materials, AIST Tsukuba Research Center,
Tsukuba, Japan, October 21–24, 1996-1997, pp.
349-354.
Rodiger, K., K. Dreyer, T. Gerdes, and M. W. Porada,
(1998). “Microwave Sintering of Hardmetals.” In-
ternational Journal of Refractory Metals & Hard
Materials, 16, pp.409-416.
Roy, R., D.K. Agrawal, J.P. Cheng, and S. Gedevanishvili
(1999). “Full Sintering of Powdered Metals Using
Microwaves.” Nature, 399(17), pp.668-670.
Saitou, K. (2006). “Microwave Sintering of Iron, Cobalt,
Nickel, Copper and Stainless Steel Powders.” Scripta
Materialia, 54(5), pp.875-879.
Tsay, C.Y., K.S. Liu, and I.N Lin, (2001). “Co-firing Pro-
cess Using Conventional and Microwave Sintering
Technologies for MnZn- and NiZn-Ferrites.” Journal
of European Ceramic Society, 21, pp.1937-40.
Upadhyaya, A. (2001). “Processing Strategy for Con-
solidating Tungsten Heavy Alloys for Ordnance
Applications.” Materials Chemistry and Physics,
67, pp.101-110.
Upadhyaya, A., S. K. Tiwari, and P. Mishra (2007).
“Microwave Sintering of W-Ni-Fe Alloys.” Scripta
Materialia, 56, pp.5-8.
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