Persistent local chemical bonds in intermetallic phase formation

Physics Letters A 378 (2014) 1746–1750
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Physics Letters A
Persistent local chemical bonds in intermetallic phase formation
Yanwen Bai a , Xiufang Bian a,∗ , Xubo Qin a , Shuo Zhang b , Yuying Huang b
Key Laboratory for Liquid–Solid Structural Evolution and Processing of Materials, Ministry of Education, Shandong University, Jinan 250061, China
Shanghai Synchrotron Radiation Facilities, Shanghai Institute of Applied Physics, Chinese Academy of Sciences, Shanghai 201204, China
a r t i c l e
i n f o
Article history:
Received 21 October 2013
Received in revised form 17 April 2014
Accepted 20 April 2014
Available online 24 April 2014
Communicated by R. Wu
Liquid structure
High-temperature X-ray diffraction
Rapid solidification
a b s t r a c t
We found a direct evidence for the existence of the local chemical Bi–In bonds in the BiIn2 melt. These
bonds are strong and prevail, dominating the structure evolution of the intermetallic clusters. From the
local structure of the melt-quenched BiIn2 ribbon, the chemical Bi–In bonds strengthen compared with
those in the equilibrium solidified alloy. The chemical bonds in BiIn2 melt retain to solid during a rapid
quenching process. The results suggest that the intermetallic clusters in the melt evolve into the asquenched intermetallic phase, and the intermetallic phase originates from the chemical bonds between
unlike atoms in the melt. The chemical bonds preserve the chemical ordered clusters and dominate the
clusters evolution.
© 2014 Elsevier B.V. All rights reserved.
1. Introduction
Known as important structural materials [1,2], the excellent
physical properties, such as the superconductivity [3–5], the magnetic susceptibility [6,7], and the electrical resistivity [7], make the
intermetallic compounds attract considerable attention. Recently,
Wu and Li [8] reported the “intermetallic glasses” in the Cu–Zr
system with near-intermetallic compositions. Then Wang et al. [9]
explained the origin of these glass formers from the thermodynamics and kinetics points of view, using the melt fragility. Their
research has explored new potential applications of the intermetallic alloys.
There is no doubt that the formation of the intermetallic alloys is critical to their performance. In these studies, concerned
with the intermetallic compounds, one of the core issues is how
to synthesize them with enhanced performance. Among the various synthetic methods [10–15], the intermetallic compounds are
mostly formed in the liquid-phase reaction. Therefore, the behavior
of the intermetallic compounds in the melt is crucial to the formation and performance of the materials. For example, Singh [16]
and Prasad [17] have demonstrated that the Al3 Mg2 intermetallic
clusters in the liquid phase lead to the asymmetry in the properties of mixing of Al–Mg molten alloys. The large diversity of the
physical properties of the solid Fe–Si system with different compositions is correlated with the changing volume fraction of the
intermetallic clusters in the liquid [18]. When describing the liquid
Corresponding author. Tel.: +86 531 88392748; fax: +86 531 88395011.
E-mail address: [email protected] (X. Bian).
0375-9601/© 2014 Elsevier B.V. All rights reserved.
structure in the whole concentration range in the Fe–Si [18] and
Fe–Al [19] systems, the phase equilibrium diagrams of which are
very complex, the intermetallic clusters have also been used as the
important structural model.
Based on the above studies, since melt is the initial state when
the intermetallic compounds form, the knowledge about the structure and the formation of the intermetallic phase in the melt can
assist us in the synthesis and controlling of the intermetallic compounds in the materials. As one of the most typical intermetallic
compounds, the BiIn2 alloy is very attractive. It is known that its
solidification behavior correlates with the structures of both the
liquid and solid phases [20]. The viscosity coefficient shows the
anomalous temperature dependence [21], which was supposed to
be accompanied with concentration fluctuations in melt. In addition, the magnetic susceptibilities, electrical resistivities, and thermoelectric powers display anomaly near the concentration range
of BiIn2 [22]. It is widely accepted that the anomalous properties of the BiIn2 are due to the self-associated atomic groups in
the melt [21,23,24]. Moreover, the behaviors of these clusters can
cause the structural changes of the melt [25]. However, the studies on the formation of the intermetallic clusters and their local
structures are scarce, which are important for understanding the
behaviors of the melt structure and the anomalous properties.
In our work, by means of the high temperature X-ray diffraction [26], the liquid structure of the BiIn2 intermetallic alloy has
been detected. With the Extended X-ray Absorption Fine Structure (EXAFS) technique [27], the local structure around In atoms
of the melt-quenched BiIn2 intermetallic alloy ribbon has been
obtained. The formation and evolution of the intermetallic clusters from the melt to the as-quenched crystalline state have been
Y. Bai et al. / Physics Letters A 378 (2014) 1746–1750
Fig. 1. (a) The structure factors S ( Q ) of the pure Bi melt at 305 ◦ C [30], pure In melt at 280 ◦ C [31], and BiIn2 alloy melt from 90 to 300 ◦ C. (b) The pair distribution functions
g (r ) of the pure Bi melt at 305 ◦ C [30], pure In melt at 280 ◦ C [31], and BiIn2 alloy melt from 90 to 300 ◦ C.
revealed. The structural differences between the melt and the asquenched ribbon have been discussed, and the driven factors for
the intermetallic alloy formation have been pointed out.
2. Experiments
The ingots of the BiIn2 alloy were prepared by melting nominal amounts of pure Bi and In of 99.99% purity in a high frequency
induction furnace under Ar atmosphere. X-ray diffraction measurements were carried out using a high temperature θ –θ type X-ray
diffractometer. Mo Kα radiation (wavelength λ = 0.7089 Å) was
reflected from the free surface of the specimen and reached the
detector through a Zr monochromator in the diffraction beam.
Experiments were performed at a high purity helium (99.999%)
atmosphere of 2.0 × 10−5 Pa after the chamber was cleaned in vacuum of 1.0 × 10−3 Pa. The scanning voltage of the X-ray tube was
50 kV, the current was 40 mA, the exposure time was 5 s and the
measured scattering angle 2θ was from 5◦ to 68◦ . The scanning
step was 0.2◦ . The sample was held for 30 min to reach equilibrium every time before a new scattering scan started. The detailed
data processing can be found in Ref. [28]. The error is less than 2%
for r1 by the adopted method.
The BiIn2 intermetallic alloy ribbon was prepared by a singleroller melt-spinning technique with a circumferential speed of
27.5 m/s. The sample thickness is 40–50 μm. The In K-edge EXAFS
spectra were measured at the beamline BL14W1 of Shanghai Synchrotron Radiation Faculty. The electron beam energy was 3.5 GeV
and the maximum stored current was 300 mA. Data were collected
by a fixed-exit double-crystal Si(311) channel-cut monochromator.
The anterior ion chamber was filled with Ar, and the other with
a mixture of Ar and Kr gases. The gases were used to detect incident X-ray intensity and transmitted intensity simultaneously. The
energy resolution was 0.5 × 10−4 . The EXAFS data were analyzed
using standard procedures with IFEFFIT code [29].
3. Results and discussion
3.1. The structure of the BiIn2 intermetallic alloy melt
The structure factors S ( Q ) of the pure In melt, pure Bi melt,
and BiIn2 intermetallic alloy melt at different temperatures are
shown in Fig. 1(a). The first peaks in the S ( Q ) curves of the BiIn2
melt are asymmetrical. There is a shoulder on the high- Q side of
the first peak of the BiIn2 melt, which is similar to the S ( Q ) curves
of the pure Bi melt in Fig. 1(a) as well as in Refs. [32–34]. The
shoulder on the S ( Q ) curve is related to the interatomic potential
[32] and the covalent bonds [35,36] in the melt. Comparatively,
the intensity of the shoulder on the curve of the BiIn2 melt is
much weaker than that of the pure Bi melt. This suggests that the
Bi–Bi covalent bonds in the pure Bi melt are largely reduced in the
BiIn2 melt. Fig. 1(b) shows the pair distribution functions g (r ) of
the pure In melt, pure Bi melt, and BiIn2 alloy melt at different
temperatures. There are apparent humps between the first and the
second peaks of the three melts, as marked in the dashed rectangle region. The shoulders on the high-r side of the first peaks
can be observed clearly in the g (r ) curves of the BiIn2 melt, while
there is not any shoulder on the g (r ) curve of In. This indicates
that the structure of the BiIn2 melt is more complex, compared
with that of the In melt. In addition, the profile of the g (r ) curve
in the BiIn2 melt changes with decreasing temperature, indicating
the structure evolution of the intermetallic melt.
The structural parameters of the BiIn2 alloy melt are shown in
Fig. 2(a) and (b). From Fig. 2(a), the nearest neighbor distance r1
(i.e., the position of the first peak in the g (r )) displays an increasing trend with decreasing temperature. This is due to the thermal
contraction characteristic of In [31]. The values of r1 are from
3.18 Å to 3.20 Å. Notice that, the atomic radii of In and Bi atoms
are 1.67 Å and 1.63 Å, respectively. The r1 are smaller than the sum
of the atomic radii of In and Bi. Furthermore, r1 of the alloy melt is
smaller than that of pure In [31,33] and pure Bi [30,33] melts. The
abnormally short bond length in the intermetallic alloy melt directly confirms the unexpected strong interactions between In and
Bi atoms. Considering the nearest neighbor distances of Bi23 In77
and Bi13 In87 in Ref. [33] (which are all larger than that of the
BiIn2 melt), the increasing atomic fraction of Bi enhances the interactions between Bi–In bonds. However, the Bi23 In77 and Bi13 In87
alloys are not in the intermetallic compositions of the Bi–In system. This suggests that the Bi–In chemical bonds are tighter in the
clusters with the intermetallic compound composition. Thus in the
BiIn2 melt, these chemical Bi–In bonds maintain the chemically ordered intermetallic clusters. The atom packing of the clusters with
intermetallic compounds BiIn2 in the melt deviates from the hard
sphere random packing model [32,33].
Y. Bai et al. / Physics Letters A 378 (2014) 1746–1750
Fig. 2. (a) The nearest neighbor distance r1 and the coordination numbers N m of the first coordination shell of BiIn2 alloy melt. (b) The correlation radius rc of the cluster
and the ratio (r2 /r1 ) of the first and second peak positions of the pair distribution function g (r ) of BiIn2 alloy melt.
The coordination numbers N m fluctuate around 10 in the temperature range. Therefore, the first coordination shell in the BiIn2
melt is looser than that in the crystalline counterpart, which has
12 coordination atoms with a hexagonal structure. This is due to
the open, low-coordinated structures of the polyvalent element
Bi [30]. There is an abnormal phenomenon that N m shows a decreasing trend as r1 increases when the temperature falls, although
the variation of the values is weak. This may be caused by many
comprehensive factors, such as the discontinuous change of density
in liquid Bi as the temperature decreases [37], and the directional
Bi–In bonds in the melt. One of the most important factors is that
the evolution of the intermetallic clusters is different from the
clusters with the hard sphere random packing model. Therefore,
the relation between N m and r1 seems to be abnormal.
Fig. 2(b) shows the evolution process of the correlation radius
rc and r2 /r1 versus temperature. Interestingly, there is an unstable stage during this evolution process. From 300 ◦ C to 220 ◦ C, the
value of rc keeps almost the same. During 220 ◦ C to 200 ◦ C, rc has
a decreasing trend, indicating the small structure change. The similar phenomenon can also be found in the ratio of r2 /r1 , which has
an increasing trend except at the temperature of 220 ◦ C. In fact, the
r1 and the N m also experience the abrupt change in this temperature range. It has been reported that [20,21,25] in the temperature
range from 410 to 220 ◦ C, the SRO clusters are composed of In and
Bi atoms similar to the structure of crystalline BiIn2 . Below 220 ◦ C,
some clusters remain the same, others form the “quasi-eutectic”
structure [20]. From these structural parameters, the nearest neighbor distance r1 can be observed as a dominant factor, i.e., the
change in r1 leads to the changes in N m , rc , and r2 /r1 . Therefore,
the chemical Bi–In bonds can help maintaining the intermetallic
clusters in the melt, dominate the structure change as temperature decreases, and assist the intermetallic compound formation.
The Bi–In bonds play a decisive role in the structural evolutions of
the intermetallic clusters.
3.2. The structure of the melt-quenched BiIn2 ribbon
In order to find out how the intermetallic compound forms during the rapid quenching process, we obtained the XRD pattern in
Fig. 3(a) and EXAFS spectra for the In K-edge in Fig. 3(b) of the
as-quenched BiIn2 ribbon. From Fig. 3(a), it is known that the asquenched ribbon are totally formed into the intermetallic phase.
Fig. 3(c) displays the Fourier transform (FT) of the k2 -weighted EXAFS signals χ (k) and the corresponding fitting curve. The k-range
of the FT is from 2.7 Å−1 to 10 Å−1 , and the r-range of the fitting
is from 2.2 Å to 5 Å. The fitting is based on the model of normal BiIn2 compound [38] from Fig. 3(a), with a P63 /mmc crystal
structure. Table 1 lists the parameters from the model as well as
obtained from the fitting. The results reveal the local structure differences between the normal crystal BiIn2 intermetallic compound
model and the rapidly quenched BiIn2 intermetallic alloy ribbon. In
the model, there are 2 In atoms closed to central In atom; while
in the as-quenched ribbon, 2 Bi atoms with a distance of 3.10 Å
become the nearest atoms around In (within the fitting uncertainties). In addition, there are 2 In atoms with a distance of 3.31 Å,
and 4 Bi atoms of 3.32 Å. Compared with the model, the Bi–In
bond lengths decrease from 3.57 Å to 3.10 Å and 3.32 Å respectively; while most of the In–In bond lengths increase. It is known
that during the rapid solidification process, the chemical bond between the unlike Bi–In atoms strengthens.
If we define 3.57 Å as a boundary of the nearest coordination distance around central In atom, the coordination numbers
are about 10 (except for the 4 In atoms with a distance of 3.64 Å
from the central In). The N m in the BiIn2 alloy melt is 9–10 as
well. It can be seen that the rapid quenching process freezes the
chemical ordered cluster structure of the melt. The diffraction intensity results of both the melt and the as-quenched ribbon of
BiIn2 alloy shown in Fig. 3(d) directly confirm this. The shoulder
on the high- Q side of the alloy melt corresponds to the BiIn2 intermetallic phase. It is indicated that the intermetallic clusters with
the chemical short-range order structure persistently exist at well
above the melting, and the clusters are composed of the stoichiometry of the solid intermetallic. During the quenching process, these
intermetallic clusters evolve into the BiIn2 intermetallic phase of
the alloy ribbon. There is no doubt that the intermetallic clusters
play a very important role in the alloy melt [39]. It is known that
the clusters in the melt can be served as the crystal seeds for the
formation of the intermetallic phase in the solid state. Notice that
the average Bi–In bond length in the ribbon is similar to the distance between the nearest Bi and In atoms in the melt. Combined
the local structures of the BiIn2 melt with the as-quenched ribbon, one of the key factors keeping the intermetallic clusters is
the persistent local chemical bonds from the melt to the solid. It is
suggested that the Bi–In bonds are preserved during the quenching
process. In other word, the strong and persistent chemical bonds
dominate the whole solidification process, which finally leads to
the formation of the solid intermetallic BiIn2 phase.
Y. Bai et al. / Physics Letters A 378 (2014) 1746–1750
Fig. 3. (a) XRD pattern of the as-quenched intermetallic BiIn2 ribbon. Inset: the enlarged region from 10◦ to 36◦ . (b) EXAFS spetra of the pure In metal and the BiIn2 ribbon
for the In K-edge. Inset: the corresponding k2 -weighted EXAFS spectra. (c) Fourier transform (FT) of the k2 -weighted EXAFS signals χ (k) and the fitting curve. Inset: the
EXAFS signals χ (k) and the fitting curve. (d) Diffraction intensity curves of the BiIn2 alloy melt and the as-quenched alloy ribbon.
Table 1
Parameters from the fitting data and the normal compound model.
Bond pair
numbers N
r (Å)
1.96 ± 0.05
1.96 ± 0.05
3.92 ± 0.05
1.96 ± 0.05
3.92 ± 0.05
3.31 ± 0.02
3.42 ± 0.03
3.64 ± 0.03
3.10 ± 0.02
3.32 ± 0.03
0.003 ± 0.001
0.007 ± 0.001
4. Conclusions
In this work, the structures of both the intermetallic alloy BiIn2
melt and the as-quenched ribbon have been detected. The nearest neighbor distance r1 directly revealed the existence of chemical
Bi–In bonds in the melt, which maintain the chemically ordered intermetallic clusters and dominate the structure evolution process.
The intermetallic clusters in the melt evolve into the as-quenched
intermetallic phase. Through the EXAFS spectrum analysis, a local structure model has been proposed. The Bi–In bond lengths
decrease compared with the normal crystalline BiIn2 compound
model, but similar to the Bi–In atomic distance in the melt. The
persistent chemical Bi–In bonds play a decisive role in the formation of intermetallic phase during the rapid solidification process.
The authors would like to acknowledge financial support from
the National Natural Science Foundation of China (Grant Nos.
51241007 and 51371107), and the Natural Science Foundation of
Shandong Province, China (Grant No. ZR2013EMQ010).
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