Journal of Alloys and Compounds 505 (2010) 337–342
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Journal of Alloys and Compounds
journal homepage: www.elsevier.com/locate/jallcom
Nickel assisted sintering of Ti
3
SiC
2
powder under pressureless conditions
Bharat Bhooshan Panigrahi
a,∗
, N. Subba Reddy
b
, Avinash Balakrishnan
c
, Min-Cheol Chu
d
,
Seong-Jai Cho
d
, Jose J. Gracio
a
a
Center for Mechanical Technology and Automation, Department of Mechanical Engineering, University of Aveiro, Aveiro 3810-193, Portugal
b
Division of Materials Science and Engineering, Engineering Research Center, Gyeongsang National University, Chinju 660-701, Republic of Korea
c
SIMAP, CNRS, Groupe GPM2, Grenoble-INP, 38402 Saint Martin d’Heres Cedex, France
d
Division of Advanced Technology, Korea Research Institute of Standards and Science, Yuseong, Daejeon 305-340, Republic of Korea
article info
Article history:
Received 11 November 2009
Received in revised form 12 May 2010
Accepted 25 May 2010
Available online 18 June 2010
Keywords:
Cold-isostatic pressing
Sintering
Activation energy
Mechanical properties
abstract
This investigation was aimed to study the effect of nickel addition on the sintering behaviour of Ti
3
SiC
2
powder under pressureless conditions. Nearly pure bulk Ti
3
SiC
2
ceramic with relative density of ∼98.5%
was produced at 1500
◦
C by sintering of Ti
3
SiC
2
powder while using 1 wt.% nickel as a sintering aid.
The activation energy of sintering of Ti
3
SiC
2
powder was determined to be 351 ± 5 kJ/mol, which was
decreased slightly to 305 ± 10 kJ/mol when nickel (1 wt.%) was added. Sintering of Ti
3
SiC
2
powder was
found to be controlled by mixed mode of mechanisms, i.e., the interface reactions and diffusion of Si
atoms. The mechanism was changed to liquid phase sintering due to melting of Ni-based compounds in
the sample sintered with Ni. The reaction of Ni with Ti
3
SiC
2
helped to decrease the grain growth rate.
The hardness (Vickers), flexural strength and fracture toughness of the sintered Ti
3
SiC
2
–1Ni sample were
found to be 3.4 GPa, 311 ± 22 MPa and 2.8–6.4 MPa m
1/2
, respectively.
© 2010 Elsevier B.V. All rights reserved.
1. Introduction
In recent times, the ternary carbides with hexagonal structure,
known as MAX phases, have taken a considerable attention from
structural ceramists [1,2]. With a good high temperature strength,
corrosion resistant, oxidation resistant, good tribological proper-
ties, elastic stiffness, good thermal and electrical properties, they
exhibit an excellent machinability. Ti
3
SiC
2
(TSC) is the most widely
studied compound in this group which is produced using vari-
ous combinations of raw materials [3–6] including Ti, Si, C, TiC
and SiC. To enhance the purity of TSC phase, excess amount of Si,
small amounts of Al and B
2
O
3
powders were used [7–9] and the
high purity TSC powder was produced from Ti, Si and TiC powders
using 0.10–1.0 mol of extra Si [10–12]. The high density parts of
TSC were produced through hot pressing, pulse discharge sinter-
ing, spark plasma sintering and self propagating high temperature
synthesis processes [3,13–17]. There are some reports on synthesis
of TSC by pressureless sintering using Al [18–21] and B
2
O
3
[7] as
sintering aids and sintering the ball milled ultra fine powders [22];
however, the final density of over 90% could not be achieved. Pres-
sureless sintering of MAX phase powder is difficult due to its easy
decomposability at high temperatures, i.e., often subjected to the
loss of Si from TSC or Al from Ti
3
AlC
2
and Cr
2
AlC powders. Another
∗
Corresponding author. Tel.: +351 234 370830x23887; fax: +351 234 370953.
E-mail addresses: bharat@ua.pt, panigrahi14@yahoo.com (B.B. Panigrahi).
important issue during sintering of these compounds is not only the
processing atmosphere (i.e., vacuum or inert atmosphere), but the
type of furnace used, i.e., graphite heating or non-graphite heating
furnaces. High density body was produced by pressing the powder
cold-isostatically at a very high pressure of about 380 MPa, followed
by the pressureless sintering [23]. A mechanically alloyed powder
with about 80 vol.% TSC [24] and the preform prepared by tape cast-
ing of TSC powder (∼95 vol.% purity) were sintered to nearly full
density [25]. Since the sample was sintered on a graphite heating
furnace, the effect of carbon diffusion from atmosphere into the
sample was noticed; consequently the titanium carbide content in
the sintered body was increased significantly. To reduce the amount
of TiC
x
, large amount (about 10 wt.%) of Si powder was mixed with
TSC powder during sintering [25]. Recently, TSC powder with small
amounts (1 and 2 wt.%) of Si was sintered under pressureless con-
dition on a tungsten heating furnace [26]; the final product had a
very low amount of impurities. However, there is no reported study
on the sintering kinetic of TSC powder so far.
Nickel was used as a sintering aid for the metal and the ceramic
powders. Nickel is known as a fast diffuser in the metal, such as
titanium, and was found to enhance the sintering rates of titanium
[27], tungsten [28] and some ceramic powders [29]. It was also
observed that nickel suppressed the grain coarsening process up to
some extent during sintering [27]. It would be worth investigating
if sintering of TSC powder could be enhanced by nickel addition.
The present investigation has been initiated with an aim to pro-
duce high purity dense body of TSC powder by sintering under
0925-8388/$ – see front matter © 2010 Elsevier B.V. All rights reserved.
doi:10.1016/j.jallcom.2010.05.177