Reaction behavior and evolution of phases during the sintering of
TaeAl powder mixtures
Hossein Sina
a
, Srinivasan Iyengar
a, *
, Sven Lidin
b
a
Materials Engineering, Lund University, P.O. Box 118, 22100 Lund, Sweden
b
CAS Chemical Centre, Lund University, P.O. Box 118, 22100 Lund, Sweden
article info
Article history:
Received 14 July 2015
Received in revised form
7 September 2015
Accepted 12 September 2015
Available online 14 September 2015
Keywords:
Intermetallics
Powder metallurgy
Reaction synthesis
Microstructure
Thermal analysis
abstract
Intermetallic compounds based on tantalum aluminides are of considerable interest in various industrial
applications. In this work, the formation of tantalum aluminides has been studied in elemental powder
mixtures containing 25, 50 and 66.7 at% Ta. A differential scanning calorimeter (DSC) was used to heat
the samples up to 1500 K at 15 K min
À1
. Phase evolution was studied by heating a few samples to
temperatures below and above the observed DSC peaks. The heat treated samples were analyzed using
scanning electron microscopy, energy dispersive spectroscopy and X-ray diffraction. The results suggest
an exothermic reaction between tantalum particles and molten aluminum, which leads to the formation
of Al
3
Ta compound as the initial product. This reaction reached completion for the aluminum-rich
samples and the corresponding DSC peak was very broad, containing two distinct steps which indi-
cated the effect of a diffusion barrier during the reaction. In these samples, the Al
3
Ta product was stable
upon further heating. A different behavior was observed for the equiatomic and tantalum-rich samples,
an incomplete reaction with a considerable amount of unreacted tantalum. These samples were asso-
ciated with a narrower reaction peak in the DSC plots, followed by a mildly exothermic peak at higher
temperatures. The latter was found to correspond to the formation of Al
69
Ta
39
phase in the solid state,
together with minor amounts of s (Ta-rich) and 4 (near equiatomic) phases. The Al
69
Ta
39
phase showed a
tendency to disappear on prolonged heating. The s and 4 phases were observed to dominate as the
major phases in tantalum-rich and equiatomic samples, respectively.
Increasing the heating rate shifted the reaction peak for Al
3
Ta formation to higher temperatures and
the apparent activation energies were estimated as 383 ± 13 kJ mol
À1
and 439 ± 22 kJ mol
À1
for the
initial and final stages of this reaction. The heat of formation of Al
3
Ta was also estimated
as À36 ± 7 kJ mol
À1
in the interval 1050e1350 K. Studies on the effect of particle sizes of the reactants
showed that, in most cases, the reaction peak shifted to lower temperatures on decreasing the tantalum
particle size. A similar behavior was observed for aluminum in the tantalum-rich samples, while an
inverse effect was seen in equiatomic and aluminum-rich samples.
© 2015 Elsevier B.V. All rights reserved.
1. Introduction
Intermetallic compounds based on transition metal aluminides
have been regarded as suitable candidates for advanced structural
applications. These compounds exhibit an attractive combination
of properties such as high melting points and enhanced resistance
against corrosion and oxidation at elevated temperatures. This
group of materials, including AleTa compounds, offers a variety of
applications in different fields such as thin films and coatings [1,2],
microelectronics, resistors and capacitors [3,4], diffusion barriers
[5,6] and structural materials which can serve at high temperatures
[7,8]. Amorphous AleTa alloys have been employed in applications
requiring high thermal and chemical stability [1,4]. However, low
ductilities of intermetallic compounds, particularly at ambient
temperatures, may limit their use in some applications.
Despite extensive studies on the AleTa system [3,4,7e12], un-
certainties are still associated with some phase relations and the
binary phase diagram is not yet fully established. However, there
is agreement in literature on the existence, stabilities and
* Corresponding author.
E-mail addresses: Hossein.Sina@material.lth.se (H. Sina), Srinivasan.Iyengar@
material.lth.se (S. Iyengar), Sven.Lidin@chem.lu.se (S. Lidin).
Contents lists available at ScienceDirect
Journal of Alloys and Compounds
journal homepage: http://www.elsevier.com/locate/jalcom
http://dx.doi.org/10.1016/j.jallcom.2015.09.100
0925-8388/© 2015 Elsevier B.V. All rights reserved.
Journal of Alloys and Compounds 654 (2016) 103e111