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Scripta Materialia 68 (2013) 79–82

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Hot-pressed TiB2–10 wt.% TiSi2 ceramic with extremely good

thermal transport properties at elevated temperatures
(up to 1273 K)
Brahma Raju Golla and Bikramjit Basu⇑
Materials Research Center, Indian Institute of Science, Bangalore 560012, India
Received 3 August 2012; revised 7 September 2012; accepted 18 September 2012
Available online 24 September 2012

This contribution reports and analyses the high thermal transport property of hot-pressed TiB2–10 wt.% TiSi2 ceramics. Depend-
ing on the test temperature, the thermal conductivity values of the TiB2 composite (which range from 89 to 122 W m1 K1) are
determined to be 18–25% higher than that of monolithic TiB2. The thermal transport properties are analyzed in terms of electronic
and phonon contributions. The electronic contribution is the major component of the thermal conductivity of TiB2 and comparable
contributions from both electronic and phonon components are observed for the TiB2–TiSi2 composite.
Ó 2012 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Keywords: TiB2; TiSi2; Ti5Si3; Thermal diffusivity; Thermal conductivity

Among the boride ceramics, titanium diboride
(TiB2) has potential for a wide range of technological
applications including electrodes for electrodischarge
machining, cutting tools, wear-resistant parts, armor
equipment, etc. [1–4]. However, the widespread applica-
tion of monolithic TiB2 is limited due to necessity of
using high sintering temperatures (up to 2373 K), as well
as its moderate fracture toughness and low oxidation
resistance. The use of sintering additives and advanced
sintering techniques are imperative to facilitate densifi-
cation of TiB2 at low temperatures besides improving
its properties [4–9].
Recently, considerable research efforts have been de-
voted to develop materials either with very high or low
thermal conductivity in order to meet the demands of
new technological applications [10–19]. For example,
extensive studies have been performed to develop
Si3N4 with intrinsic thermal conductivity for packaging
materials and electronic devices [13,14]. On the other
hand, efforts are being made to lower the thermal con-
ductivity of materials to the lowest possible extent for
thermal barrier coating applications [17–19]. In the liter-
ature, it has been reported that microstructural features,
such as grain size, grain orientation and atomic mass
differences of phases, porosity and microcracking can
⇑ Corresponding author. Tel.: +91 8022933256; e-mail: bikram@mrc.
iisc.ernet.in
significantly affect the thermal conductivity of materials
[20–22]. The thermophysical properties are also critical
for determining the thermal stresses of materials. How-
ever, few studies are available on the thermophysical
properties of TiB2-based materials.
In the present research, an attempt has therefore been
made to study the temperature-dependent thermal con-
ductivity of TiB2 with TiSi2 (0 and 10 wt.%) as a sintering
additive. In order to understand the heat conduction
mechanisms, the thermal conductivity of TiB2–TiSi2 sam-
ples is analyzed in terms of electronic and phonon contri-
butions and the thermal conductivity is correlated with
the microstructure and the phonon mean free path as well.
A comparison is also made with the thermal properties of
other TiB2 materials, reported in the literature.
Commercially available TiB2 (Grade F, H.C. Starck,
Germany) and TiSi2 (Goodfellow Cambridge Ltd., UK)
powders in appropriate amounts were used as starting
materials to produce monolithic TiB2 and TiB2–
10 wt.% TiSi2 composite. The hot pressing of the pow-
der compacts at selected sintering temperatures (2073
and 1923 K for 1 h for the monolithic TiB2 and TiB2–
10 wt.% TiSi2 composite, respectively) were performed
with an applied pressure of 30 MPa. The densities of sin-
tered samples were measured in water according to
Archimedes’ principle. The crystalline phases of the
samples were analyzed using X-ray diffraction (XRD).
The microstructural investigation of the polished and
chemically etched surfaces of TiB2 ceramics was

1359-6462/$ - see front matter Ó 2012 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.scriptamat.2012.09.013
80 B. R. Golla, B. Basu / Scripta Materialia 68 (2013) 79–82
performed by means of scanning electron microscopy
(SEM) and the finer-scale microstructure was investi-
gated using transmission electron microscopy (TEM).
More details on the starting powders, hot pressing and
microstructural characterization of these materials were
reported elsewhere [6,7].
The thermal diffusivity of the TiB2 samples (12.2 mm
diameter  2 mm thick) was measured in the tempera-
ture range from 297 to 1273 K using the laser-flash
method (Netzsch LFA 457, Selb, Germany). Prior to
thermal diffusivity measurements, the samples were sub-
jected to metallographic polishing and were coated with
gold and carbon on both sides. It is known that gold
prevents the direct transmission of the beam and im-
proves energy transfer to the sample, while carbon in-
creases the absorption of the front surface and the
emission of the back surface. In this procedure, the front
face of the disk sample is subjected to a short duration
laser pulse and the thermal history of the opposite face
is assessed. All the experiments were carried out under
a flowing nitrogen gas atmosphere at a flow rate of
6 l h1. The thermal diffusivity (a), was calculated from
the following expression:
a ¼ 0:48ðd2 =p2  tx Þ; ð1Þ
where d is the thickness of the specimen and tx is the
time duration to initiate the pulse in the test piece.
The thermal conductivity (k) of the samples was calcu-
lated based on the measured density (q), thermal diffu-
sivity (a) and the calculated specific heat values (Cp)
according to the following equation:
k ¼ qaCp : ð2Þ
In our previous work, it was reported that monolithic
TiB2 could be densified to only 94.4% theoretical density
(qth) after hot pressing at 1923 K for 1 h [6]. However,
TiB2 could be densified to more than 98% qth with
increasing sintering temperature up to 2073 K. A com-
parison of the sintering temperatures of both the TiB2
samples reveals that addition of TiSi2 results in almost
full densification of TiB2 composite even at a relatively
lower sintering temperature and proves the usefulness
of TiSi2 as a sintering aid. Table 1 presents the densifica-
tion, microstructural characterization and grain size
data of TiB2 samples.
XRD analysis revealed the presence of Ti5Si3 as an
additional phase in hot-pressed TiB2–10 wt.% TiSi2
(see Fig. 1). The formation of such a new Ti5Si3 phase
in the TiB2 composite indicates the occurrence of sinter-
ing reactions. The details of sintering reactions and sin-
tering mechanisms are reported elsewhere [6]. A
representative SEM micrograph of chemically etched
TiB2–10 wt.% TiSi2 sample is shown in Figure 1c. The
presence of three distinct phases, namely the grey phase
(TiB2), dark phase (TiSi2) and intergranular bright
Table 1. Densification, microstructural phases and average grain size of the TiB2–TiSi2 ceramics hot pressed at various temperatures for 1 h in an
argon atmosphere.
Material composition Hot-pressing Measured bulk Relative
(wt.%) temperature (K) density, q (g cm3) density (% qth)
Monolithic TiB2 2073 4.41 98.1
TiB2–10 TiSi2 1923 4.46 99.6
(a)
-TiB2
Intensity (Arbitary unit)
-TiSi2
-Ti5Si3
(b)
20 30 40 50 60 70
Angle (2θ)
(c) (d)
TiB2
TiB2
Ti5Si3 TiSi2
TiB2
Ti5Si3
TiB2
5 µm 1 µm
TiSi2
Figure 1. XRD patterns of the hot-pressed TiB2 specimens containing
(a) 10 wt.% TiSi2 and (b) 0 wt.% TiSi2. SEM micrograph obtained
from the polished and etched surface of TiB2–10 wt.% TiSi2 (c) and the
bright-field TEM image of TiB2–10 wt.% TiSi2 (d). The corresponding
microstructural phases are marked on micrographs.
phase (Ti5Si3) could be identified. A closer look at Fig-
ure 1c reveals that the microstructure of the TiB2 com-
posite consists of bimodal TiB2 grains (typically a
large fraction of equiaxed grains varying in size from
1.5–4 lm and some coarser-faceted TiB2 grains varying
in size from 4 to 8 lm with an aspect ratio of 2.5). A
bright-field TEM image is also shown in Figure 1d.
The Ti5Si3 phase is observed to be located at the triple
pocket and surrounded by the TiB2 and TiSi2 grains.
This clearly indicates that Ti5Si3 forms as a result of
the sintering reaction between TiB2 and TiSi2.
As mentioned earlier, the thermal conductivity of the
TiB2 samples was calculated based on the measured den-
sity, thermal diffusivity and the calculated specific heat
values (Cp). The Cp values of the TiB2 composites are
calculated using the rule of mixtures formulation from
the standard Cp data of various phases and is presented
in Figure 2a. Recently, Bruls et al. proposed that the
intrinsic thermal conductivity of ceramics can be reliably
estimated on the basis of temperature-dependent ther-
mal diffusivity data [23]. The thermal diffusivity of the
TiB2 samples as a function of temperature is shown in
Figure 2b. Room temperature (RT) thermal diffusivity
values of 3.5  105 and 4.4  105 m2 s1 were mea-
sured for the monolithic TiB2 and TiB2–10 wt.% TiSi2,
respectively. The TiB2 composite exhibits relatively
higher thermal diffusivity values at all the temperatures,
when compared with monolithic TiB2. However, the
thermal diffusivity of both the TiB2 samples decreased
with temperature. The decrease in thermal diffusivity is
attributed to the phonon scattering with temperature.
XRD phase Average grain
assemblage (vol.%) size of TiB2 (lm)
TiB2 (100) 3.4 ± 0.8
TiB2 (90), TiSi2 (3.2), Ti5Si3 (6.8) 3.5 ± 0.5

1300
(a)
Specific heat (J Kg-1 K-1)
1200
1100
1000
900
800
700
600
500
0 200 400 600 800
Temperature (K)
TiB2, 98%ρth, 3.4 μm [present work]
130
Thermal conductivity (W m-1 K-1)
TiB2-10 wt.% TiSi2, 99.6%ρth, 3.5 μm [present work]
(c) TiB2, 96%ρth, 1.5 μm [12]
120
110
TiB2, 99%ρth, < 15 μm [11]
TiB2, 98%ρth, 9 μm [10]
100
90
80
70
60
50
0 200 400 600 800
Temperature (K)
Figure 2. (a) Specific heat (Cp) of TiB2 samples as a function of
temperature. The specific heat of the TiB2 samples is calculated from
the standard Cp data of TiB2, TiSi2 and Ti5Si3 phases [28,29]. (b) The
temperature-dependent thermal diffusivity and (c) thermal conductiv-
ity of hot-pressed TiB2 samples. For comparison purposes the reported
literature data on thermal conductivity, densification and average
grain size of TiB2 is also presented. (d) Average phonon mean free path
of TiB2–TiSi2 ceramics as a function of temperature.
Figure 2c shows the thermal conductivity of TiB2 sam-
ples as a function of temperature. The thermal conductivity
decreases from 122 to 89 W m1 K1 for TiB2–10 wt.%
TiSi2, while it varies from 98 to 75 W m1 K1 for mono-
lithic TiB2 with increasing temperature up to 1273 K. It
indicates that the TiB2–10 wt.% TiSi2 composite can exhi-
bit a maximum of 24.5% increase in thermal conductivity at
room temperature and more than 18% increase at elevated
temperature (up to 1273 K), when compared to the mono-
lithic TiB2. The high thermal conductivity of the TiB2
ceramics results from both the lattice and electronic contri-
bution to phonon transport [3]. Konigshofer et al. reported
that the thermal conductivity of TiB2 decreased from
94 W m1 K1 (at RT) to 72 W m1 K1 (at 1273 K)
[11]. In the case of other transition metal diborides, the
thermal conductivity also reportedly decreased from 99
to 79 W m1 K1 for ZrB2–20 vol.% SiC and from 125 to
80 W m1 K1 for HfB2–20 vol.% SiC with increasing
temperature to 1273 K [24,25].
The thermal conductivity of the presently investigated
TiB2–TiSi2 materials is also compared with the literature
data obtained with other TiB2 ceramics in order to
compare their properties (Fig. 2c). While making such
comparison, it appears that all the TiB2 materials (with
density P98% qth) exhibit a similar trend in thermal con-
ductivity with temperature. In addition, the measured
thermal conductivity of monolithic TiB2 is very similar
to the reported values of Munro and Konigshofer et al.
[10,11]. It should be noted here that all these monolithic
TiB2 ceramics were densified to more than 98% qth. How-
ever, binderless TiB2 with grain size of 1.5 lm exhibited
low thermal conductivity at all temperatures, when
compared to other TiB2 ceramics. Such a low thermal
transport behaviour of the binderless TiB2 (1.5 lm) can
be attributed to its low density (96% qth).
In order to understand the thermal transport mecha-
nisms of TiB2 samples, it is important to quantify the elec-
B. R. Golla, B. Basu / Scripta Materialia 68 (2013) 79–82 81
TiB2
5.0x10-3
(b) TiB2 tronic and phonon contributions. The electronic
Thermal diffusivity (m2s-1)
TiB2-10 wt% TiSi2
TiB2-10 wt.% TiSi2
4.0x10-3 contribution (ke) of the thermal conductivity can be esti-
3.0x10-3 mated using the Widemann–Franz law [24] based on elec-
2.0x10-3
trical conductivity (r), the absolute temperature (T) and
the Lorentz constant ðL  2:45 108 W X K2 Þ:
1.0x10-3
0.0 ke ¼ LrT: ð3Þ
1000 1200 1400 0 200 400 600 800 1000 1200
Temperature (K)
The phonon contribution (kp) to the thermal conduc-
30 tivity at elevated temperatures is difficult to predict reli-
Phonon scattering distance (μm)
28
(d) TiB2
26
24
TiB2-10 wt.% TiSi2
ably as it relies on phonon–phonon, phonon–lattice and
22
20 phonon–electron scattering. However, the phonon con-
18
16
14
tribution can be estimated by subtracting the electronic
12
10
contribution from the measured total thermal conductiv-
8
6 ity. Table 2 records the electrical conductivity of TiB2,
4
1000 1200 1400 1600
2
0
TiSi2 and Ti5Si3 and the electrical conductivity of TiB2–
0 200 400 600 800 1000 1200 10 wt.% TiSi2 composite, which is estimated from the lit-
Temperature (K)
erature data of various phases using the rule of mixtures.
The electronic contribution to thermal conductivity de-
creased from 72.8 to 59.9 W m1 K1 for TiB2 and from
67.7 to 55.6 W m1 K1 for TiB2–10 wt.% TiSi2 between
297 and 873 K. Likewise, a decrease in phonon contribu-
tion (from 25.3 to 19.7 W m1 K1 for TiB2 and from 54.5
to 41.1 W m1 K1 for TiB2–10 wt.% TiSi2 between 297
and 873 K) is evident. From this, it is clear that the ther-
mal conductivity of TiB2 samples has a significant contri-
bution from both electronic and phonon contributions.
Moreover, the electron contribution is the major compo-
nent of the thermal conductivity of TiB2, whereas it is esti-
mated that the electronic and phonon components make a
comparable contribution to the thermal conductivity of
TiB2–10 wt.% TiSi2 composite. These observations
clearly indicate that the addition of TiSi2 has a strong ef-
fect on the thermal transport behavior of TiB2.
The average phonon mean free path of TiB2 samples
is calculated from the phonon contribution (kp) of the
thermal conductivity. The resultant average phonon
mean free path ‘i’ is given by [26]:
i ¼ 3k=ðmCp Þ; ð4Þ
where k is the thermal conductivity, v is the average
sound velocity and Cp is the specific heat capacity. A
sound velocity of 9.5 km s1 (the average of the longitu-
dinal sound velocity: (11.4 km s1) and the transverse/
shear sound velocity: (7.53 km s1)) is used at all tem-
peratures for the calculation of phonon mean free path
of TiB2 samples [10]. The temperature dependence of
the average phonon mean free path in the TiB2 samples
is shown in Figure 2d. At high temperatures, the phonon
mean free path in the samples decreases and phonon
scattering increases, because of phonon–phonon scatter-
ing [27]. The phonon mean free path varies with temper-
ature from 6 to 13 lm for monolithic TiB2 and from 13
to 28 lm for TiB2–10 wt.% TiSi2 composite. Since the
phonon mean free path is considerably larger than the
grain size of TiB2 samples, it is expected that the thermal
phonons travel over more than 1.5–2 TiB2 grains for
TiB2 and 4–8 TiB2 grains for the TiB2–10 wt.% TiSi2
composite. The decrease in thermal conductivity with
temperature can therefore be partly attributed to both
the phonon–phonon scattering and phonon scattering
by grain boundaries.
In order to understand the effect of sintering additive
on the thermal conductivity of TiB2, the thermal
82 B. R. Golla, B. Basu / Scripta Materialia 68 (2013) 79–82

Table 2. Electrical conductivity, measured total thermal conductivity, electron contribution to thermal conductivity (ke) and phonon contribution to
thermal conductivity (kp) of TiB2–TiSi2 samples at different temperatures. The rule of mixture formulation was used for the electrical conductivity
calculation of TiB2 composite and the electrical conductivity data of various phases were collected from the literature [11,30,31].
Temperature Electrical conductivity Thermal Electronic contribution, Phonon
(K) (106 S m1) conductivity ke (W m1 K1) contribution, kp
(W m1 K1) (W m1 K1)
TiB2 TiSi2 Ti5Si3 TiB2–10 wt.% TiSi2 TiB2 TiB2–10 wt.% TiSi2 TiB2 TiB2–10 wt.% TiSi2 TiB2 TiB2–10 wt.% TiSi2
297 10.0 7.5 1.4 9.3 98.1 122.1 72.8 67.7 25.3 54.5
473 5.5 4.3 0.9 5.1 89.8 108.6 63.7 59.1 26.1 49.5
673 4.0 2.9 0.7 3.7 83.4 99.8 66.0 61.0 17.4 38.8
873 2.8 2.2 0.6 2.6 79.6 96.7 59.9 55.6 19.7 41.1

conductivity of the various constituent phases of TiB2
composites has to be considered. Based on the existing
literature, the reported room-temperature thermal
conductivity of various phases is as follows: TiB2 (60–
120 W m1 K1), TiSi2 (17 W m1 K1) and Ti5Si3
(11 W m1 K1) [4,30,31]. Although the thermal conduc-
tivities of the constituent secondary phases are signifi-
cantly lower than that of the matrix TiB2 phase, the
optimal amount of sintering additive addition (up to
10 wt.% TiSi2) may not adversely affect the thermal con-
ductivity of TiB2 as it resulted in almost full densification
(99.6% qth) of the TiB2–TiSi2 ceramic. Similarly, despite
the low thermal conductivity of MoSi2 (50 W m1 K1),
with the addition of 2.5 wt.% MoSi2 sinter additive, the
resultant thermal conductivity of TiB2 increased from
68 to 77 W m1 K1 due to the enhanced densification
of TiB2 [12].
Based on our research results the following conclu-
sions can be drawn:
1. The present investigation clearly shows that addition
of 10 wt.% TiSi2 is very effective in enhancing the den-
sification and thermal conductivity of TiB2. The TiB2
composite exhibits relatively higher thermal diffusiv-
ity at all temperatures compared to monolithic
TiB2. The thermal conductivity decreases from 122
to 89 W m1 K1 for TiB2–10 wt.% TiSi2, while it
varies from 98 to 75 W m1 K1 for monolithic
TiB2 with increasing temperature from 297 to
1273 K. A comparison with other TiB2 materials
establishes the highest ever thermal conductivity mea-
sured with hot-pressed TiB2–10 wt.% TiSi2.
2. The phonon mean free path varies with temperature
from 6 to 13 lm for monolithic TiB2 and from 13
to 28 lm for TiB2–10 wt.% TiSi2 composite. The
decrease in thermal conductivity with temperature
can be attributed to both phonon–phonon scattering
and phonon scattering by grain boundaries as the
phonon mean free path is considerably larger than
the grain size of TiB2 samples.
The authors gratefully acknowledge the coopera-
tion of Dr. Nurcan Calis Ackibas, Department of Materi-
als Science and Engineering, Anadolu University, Turkey
for assistance with thermal diffusivity measurements.
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