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The formation of Fe-Cu composite based on bimetallic nanoparticles

Article  in  Vacuum · January 2019

DOI: 10.1016/j.vacuum.2018.10.078

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 Vacuum 159 (2019) 441–446

Contents lists available at ScienceDirect

Vacuum
journal homepage: www.elsevier.com/locate/vacuum

The formation of FeeCu composite based on bimetallic nanoparticles T

a,∗ a a a a a
A.S. Lozhkomoev , M.I. Lerner , A.V. Pervikov , E.V. Naidenkin , I.P. Mishin , A.B. Vorozhtsov ,
A.S. Apkariana, D.G. Eskinb
a
Institute of Strength Physics and Materials Science of Siberian Branch of Russian Academy of Sciences. 2/4, pr. Akademicheskii, Tomsk, 634055, Russia
b
Brunel Univ London, BCAST, Uxbridge, UB8 3PH, Middx, England, United Kingdom

A B S T R A C T

In this paper we suggest a new method of producing a Fe-28 wt% Cu composite by compacting and subsequent sintering of bimetallic nanoparticles made of metals
with limited mutual miscibility: iron and copper. The influence of the temperature of annealing on the structure and phase composition of consolidated composite
samples has been analyzed. It has been shown that annealing in the temperature range of 200–400 °C induces the processes of low-temperature sintering of copper
and iron. These processes are accompanied by the growth of the size of coherent scattering regions and the separation of the metallic components of nanoparticles.
During thermal treatment in the range between 400 and 600 °C, adjacent sidewalls of large particles are welded together and large pores emerge in the sample.
Further temperature increases cause the sample to shrink and the pores to become smaller. The consolidation of bimetallic nanoparticles consisting of iron and copper
and their subsequent sintering allows for obtaining volumetric composites that have homogeneous structure without distinct macroscopic separation of phases as
well as high strength characteristics.

1. Introduction nanocrystalline powders) is applied [19,20].

Mixing, compacting and subsequent sintering of nanoparticles of
Alloys consisting of mutually immiscible metals and those that have metals with differing properties allows for consolidating mutually im-
limited miscibility in equilibrium conditions are promising materials for miscible metals for fabricating volumetric composites [17,21]. How-
a range of engineering applications, thanks to their unique combination ever, the problematics of the formation of homogeneous mixtures of
of mechanical, electrical and physical properties [1–3]. In regards to nanoparticles of two different metals is a complex challenge. Due to
some of their physico-mechanical and operational properties, such their small size, nanoparticles of each of the metals possess high specific
materials may be superior to traditional alloys of similar purpose. They surface energy. This determines their high chemical activity and ability
could be used in the manufacturing of microelectronic devices, wiring to form micron-sized agglomerates [22]. Nanoparticle agglomeration
items, rocket jet nozzles, etc. [4–8]. prevents homogeneous mixing of nanopowders of different metals, and
The FeeCu system is an example of an alloy made of metals with such mixing would produce highly homogeneous mixtures of nano-
limited mutual miscibility since in equilibrium conditions iron and particles of each of the metals. According to the research, the con-
copper are virtually not intermixing because of mixing enthalpy at solidation of individual nanoparticles (specifically, such highly reactive
temperatures below 700оC [9,10]. In the meanwhile, volumetric com- metals as iron and its alloys) leads to the formation of highly non-
posites of thermodynamically immiscible FeeCu possess unique me- homogeneous microstructures [23].
chanical, electrical and magnetic properties and have a wide range of In this regard, the consolidation of composite bimetallic nano-
applications [11]. For example, nanocrystal FeeCu composites with particles consisting of such metallic phases is a promising approach to
small copper content exhibit strong magnetostrictive effects [12]. the development of alloys of immiscible metals with homogeneous
FeeCu catalysts are used to synthesize spirits [13] and to hydrogenate structures. Consolidation would ensure that the distribution of the
CO2 [14], and FeeCu alloys have high surface thermal conductivity and components in the alloy is homogeneous.
resistance to corrosion [15]. In the available literature there is no method for forming volumetric
To produce volumetric composites from mutually immiscible metals composites by sintering bimetallic nanoparticles of mutually immiscible
(or those with limited miscibility), the particle consolidation method is metals (or those with limited miscibility).
often used, and it relies on traditional approaches of powder metallurgy In this paper we present the results of the research of the structure,
[16–18]. Here, to increase mutual solubility and obtain metastable phase composition and microhardness of volumetric samples of a Fe-
phases, preliminary mechanical activation of powders (including 28 wt% Cu alloy. Those were obtained by the compaction of bimetallic

∗
Corresponding author.
E-mail address: [email protected] (A.S. Lozhkomoev).

https://doi.org/10.1016/j.vacuum.2018.10.078
Received 12 September 2018; Received in revised form 27 October 2018; Accepted 29 October 2018
Available online 30 October 2018
0042-207X/ © 2018 Elsevier Ltd. All rights reserved.
A.S. Lozhkomoev et al. Vacuum 159 (2019) 441–446

Fig. 1. A characteristic image of Fe-28 wt% Cu powders (a) and particle size distribution curve (b).

nanoparticles, depending on the temperature of annealing in vacuum. mean size of Fe/Cu nanoparticles was determined by measuring 1500
nanoparticles.
2. Experimental The phase composition of the samples was researched using a
Shimadzu XRD 6000 (Shimadzu, Japan) X-ray diffractometer with fil-
2.1. The synthesis of bimetallic nanoparticles tered СuКа radiation at 40 kV and 30 mA in the scanning mode in the
2θ angle range from ∼40 to 80° and with a step of 0.02°. The quali-
Bimetallic nanoparticles were synthesized by the electrical explo- tative analysis was performed using the PDF-2 Release 2014 database.
sion of two intertwined wires (copper and iron). The general schematics The microhardness of the consolidated samples was determined
of the synthesis workflow are provided in Ref. [24]. This method allows using a PMT-3 microhardness tester with the indenter load of 100 g.
for obtaining nanopowders where the content of impurities is de- The microhardness of each sample was determined from at least 20
termined by the composition of the exploded wires and the impurities measurements.
in the gas medium surrounding the wires. To synthesize bimetallic The relative density of the compacted samples (ρ/ρ0) was de-
nanoparticles, Fe wires (with the diameter of 0.3 mm and iron content termined from the apparent density that was measured while taking
of 99.0 wt. %) and Cu wires (with the diameter of 0.2 mm and copper into account the geometry and mass of the samples. The apparent
content of 99.9 wt. %) were used. The wires were destructed by an density was based on the calculated theoretical density of the materials
incoming pulse of current with the density of 5 × 107 A/cm2. The ex- (8.35 g/cm3) while taking into account the chemical composition
plosion took place in argon atmosphere (99.99 vol%) at the pressure of (73 wt.% Fe and 27 wt.% Cu). The mass of the obtained samples was
2 × 105 Pa. The content of copper and iron in the 28Cu/72Fe wt.% measured using an Acculab ALC-210d4 (Sartorius, USA) analytical
powders depended on the diameter of the wires that had identical balance with the accuracy of 0.0001 g.
length. After the powder had been obtained, it was passivated by slow
air flow into the unit for 48 h.
3. Results and discussion

2.2. The consolidation of bimetallic nanoparticles and subsequent annealing Fig. 1 shows a characteristic image of Fe-28 wt% Cu nanoparticles
of the samples obtained by the electrical explosion with the particle size distribution
curve. As seen from Fig. 1, the particles mostly have spherical shape
Nanoparticle consolidation was performed by pressing in a hy- and their distribution by size is close to log-normal. Average particle
draulic press with a cylindrical die with the hob diameter of 20 mm 2 g size is ∼66 nm. Also, individual particles may be as large as
nanopowder batches were poured into the die and then compacted at 200–300 nm.
the pressure of 3 t/cm2 for 10 min at room temperature. After that, the The research of the elementary composition of Fe-28 wt% Cu
compacted material was extracted from the die. The thermal treatment powder samples has shown that all the researched particles contain iron
of the consolidated samples was performed in the temperature range of and copper. The particles are mostly Janus-type structures (Fig. 2a,
200–1000 °C using a Nabertherm R 120/1000/13/B180 (Nabertherm, particle 1) and core-shell structures (Fig. 2a, particle 2). Such structures
Germany) furnace, and the roughing pump provided the pressure of at are characteristic for bimetallic nanoparticles obtained by this method
least 10−2 mm Hg. [24].
Fig. 3 shows a raster image of the surface of a Fe-28 wt% Cu com-
2.3. The analysis of the characteristics of bimetallic nanoparticles and posite obtained by nanoparticle consolidation and the elementary
composites based on them composition of its surface. As seen from Fig. 3a, the sample mainly
comprises nanosize particles, and large particles sized > 0.5 μm are
Electron microscopy analysis and the elementary analysis of bime- probably agglomerates of smaller particles. It ensues from Fig. 3b and c
tallic nanoparticles and consolidated samples was conducted using a that the metals (iron and copper) have highly homogeneous distribu-
JEM 2100 transmission electron microscope (JEOL, Japan) with X-max tion throughout the samples volume.
(an integrated EDS system by Oxford Instruments, United Kingdom) Fig. 4 shows the results of X-ray diffraction analysis of the con-
and a Quanta 200 3D (FEI, USA) scanning electron microscope with solidated Fe-28 wt% Cu samples depending on the annealing tempera-
Pegasus (an integrated system of elementary and structural analysis by ture. The initial sample at 25 °C contains the copper phase and α- and γ-
EDAX, USA). phases of iron as well as ferric oxide Fe2O3. It is probable that high
Particle size distribution of Fe/Cu nanoparticles was obtained from temperature γ-Fe is formed at over 1200 °C because of the high cooling
image analysis of TEM micrographs at a magnification of 50,000. The rate of the disperse phase that is formed from the gas-plasma state [25].

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A.S. Lozhkomoev et al. Vacuum 159 (2019) 441–446

Fig. 2. TEM (а) and EDS (b, c) images of bimetallic Fee28Cu wt.% nanoparticles: 1 – Janus nanoparticle, 2 – core-shell nanoparticle.

The parameter of the copper lattice determined from the locations be observed in a FeeCueO system if liquid copper interacts with iron
of Bragg maxima is 3.608 Å. According to Vegard's rule, it corresponds oxide that is formed in the oxidized surface layer of nanoparticles with
to a copper-based solid solution with the content of iron about 2.4 at. % iron shell (Fig. 2).
[26]. Thus, when bimetallic particles are produced by electrical ex- Increasing annealing temperature to 800 °C does not result in a
plosion, non-equilibrium phases are formed, as in the case with the significant increase in the values of dcsr and ε. For iron we observe an
mechanical activation of powders. The areas of coherent scattering increase in dcsr and a decrease in ε. Here the peak corresponding to iron
were evaluated at 38 and 25 nm for iron and copper, respectively oxide disappears and the maximum corresponding to copper oxide in-
(Fig. 5a). We can note that the sum of these values is close to the creases (Fig. 4). This suggests that iron oxide has been fully reduced by
average size of bimetallic nanoparticles (66 nm). copper.
Heating the compacted sample to 200 °C leads to the decomposition Fig. 6 shows an evolution of the microstructure of consolidated
of the copper-based solid solution and an γ-α phase transition in iron. samples when they are sintered in vacuum in the temperature range of
The lattice parameter takes the standard value of 3.615 Å. We observe 200–800 °C. Because of the lower coefficient of reflection of electrons
an insignificant increase in the size of the areas of coherent scattering of by iron, the areas saturated with copper look lighter in Fig. 6c and d and
iron dcsr (Fig. 5a) and a decrease in lattice microstains ε (Fig. 5b). Such therefore can be easily identified.
changes may be a consequence of a decreased defects density and the At 200 °C (Fig. 6a), as compared to the initial sample (Fig. 3а), no
relaxation of the crystalline lattice. significant changes in the microstructure are visually observed. How-
Heating the samples to 400 °C leads to a significant increase in dcsr of ever, the relative density of the sample p/p0 (Fig. 7) is increasing. The
both copper and iron and a decrease in ε of iron. Such changes in the density increase can probably be attributed to low-temperature sin-
diffraction diagram can speak in favor of sintering process start. This tering of copper nanoparticles as copper has a lower melting tem-
process leads to more intense migration of sub-boundaries and to the perature than iron. The effect of low-temperature sintering and melting
coalescence of crystallites while the sizes of dcsr increase. In accordance of nanoparticles is well-known [29,30] and is attributed to their surface
with Bochvar rule [27], copper (at 140÷270°С) and iron (at energy [31] which is determined by a high density of defects and the
270÷450°С) are characterized by the development of recrystallization curvatures of nanoparticles surface [32]. It is also shown in Ref. [33]
that results in the formation of crystallites with a more equilibrium that sintering of Cu nanoparticles (average size of 20 nm) obtained by
(defectless) structure. the electrical explosion of copper wire takes place in the temperature
When a sample is heated to 600°С, a drastic decrease in dcsr and ε for range of 170–270 °C. According to [34], sintering of copper nano-
copper is observed. These results suggest that at 600°С, copper and iron particles (with the average size of 23 nm and covered in ∼1 nm carbon
crystallites with more equilibrium structure are formed. In the tem- shell) obtained by the electrical explosion of copper wire was observed
perature range of 200–600°С, ferric oxide Fe2O3 is observed in the already at ∼ 200°С.
samples. At 600–800 °C, we see peaks that correspond to copper oxide The analysis of the relative density of the samples has shown that
in the sample, Cu2O (Fig. 4). As shown in Ref. [28], such a reaction can after sintering in the temperature range of 200–400 °C, the relative

Fig. 3. An SEM image of the surface of consolidated samples of bimetallic Fe-28 wt.% Cu particles (a) and the distribution of copper (b) and iron (c) according to the
SEM-EDS analysis in the mapping mode. All bars 2 μm.

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A.S. Lozhkomoev et al. Vacuum 159 (2019) 441–446

copper and iron particles sintering is taking place more intensely. As a

result, the density of the sample increases (Fig. 7). At 600 °C the
structure of the sample significantly differs from the structure of the
samples obtained at lower temperatures (Fig. 6с). In the sample, we see
separated areas of copper and iron that are in contact with each other.
Here, areas saturated with iron normally have round shape and are
2–5 μm in size; they are surrounded by areas of copper that are lighter-
colored and spread along the boundaries (Fig. 6). Also, there are large
irregularly shaped pores in the sample. Based on the fact that at 600 °C,
the value of dcsr for both copper and iron is less than thatat 400 °C, we
can suppose that in the temperature range of 400–600 °C, material
consolidation will take place through the liquid phase. Inside large
micron-sized areas saturated with iron, light-colored round-shape areas
of copper depositions are observed. Those are less than 1 μm in size
(Fig. 6c and d), and this resembles what we see in Ref. [35] happening
with a Cu80Fe20 alloy in areas saturated with iron (СFe∼77%). This also
confirms that a liquid-phase separation of copper and iron is taking
place in the specified conditions.
After annealing at 800 °C, further compaction of the sample during
sintering takes place (Fig. 7). As a result, pore size is significantly de-
creased. In the material we mostly see isolated pores with a shape that
is close to sphere (Fig. 6d). The separation of metallic phases becomes
more apparent. In the meanwhile, despite the fact that in the initial
powders there is less copper than iron, the areas that contain iron are
normally surrounded with areas containing copper. Here, the value of ε
for the iron component continues decreasing. In our opinion, this means
that at 800 °C rebuilding of the crystalline structure of iron grains is not
completed. According to data in Ref. [36], the growth of the relative
density of the samples produced from iron nanoparticles with the initial
size of 38 nm continues up to 900 °C. Annealing of the samples obtained
by particle consolidation at 800 °C and above leads to the formation of a
stable Fe-28 wt% Cu composite with even distribution of the compo-
nents throughout the volume (Fig. 8).
A measurement of the microhardness of the compact samples has
shown that it significantly increases (from 0.5 to 2.6 GPa) after an-
nealing in the range of 200–600°С (Fig. 9). As it has been shown above,
in this temperature range, copper and iron sintering processes are de-
veloping. Also, there is a linear dependency when the relative density of
the composite is increasing along with the temperature (Fig. 7). The
Fig. 4. The diffraction diagrams of the consolidated Fee28Cu wt.% samples microhardness attained after annealing at 600 °C is close to the value
depending on the temperature. observed in Ref. [37] for an alloy of similar composition (Fe-15% Cu)
with a nanocrystalline structure (d∼15 nm). That alloy has been ob-
density continues increasing. The size of the particles in the sample tained by high-pressure torsion that caused high degree of deformation
obtained at 400 °C is significantly higher than the size of the grains in (e > 100). In the above referenced paper, as well as in our research, at
the sample obtained at 200 °C (Fig. 6b), which suggests that nano- this temperature (600 °C) noticeable roughing of the structure is ob-
particles merge (create agglomerates) when the temperature grows. served. However, the size of Cu and Fe particles remains significantly
In the range of annealing temperatures (400–600 °C), the process of smaller (150–200 nm). Despite a significantly larger size of the

Fig. 5. The dependences of the sizes of coherent scattering areas (dcsr) and microstrains of the crystalline lattice (ε) in the consolidated samples on the temperature.

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A.S. Lozhkomoev et al. Vacuum 159 (2019) 441–446

Fig. 6. SEM images of consolidated samples after sintering in vacuum at 200 °C (a), 400°С (b), 600°С (c) and 800°С (d); samples (c) and (d) have been obtained in the
reflected electrons mode.

consolidated samples in the temperature range of 200–400 °C, the

processes of low-temperature sintering of copper and iron are devel-
oping. When the annealing temperature increases to 600 °C, two phe-
nomena are observed: liquid-phase separation of copper and iron and
the formation of areas saturated with iron that are separated by areas
containing copper along the separation boundaries. Inside the areas
saturated with iron, round-shaped depositions of copper with the size
below 1 μm are found. Such a hierarchically arranged structure remains
stable when the annealing temperature is below 800°С. This, in com-
bination with the deposition of iron and copper oxides, promotes a
significant increase in the strength properties of the Fe-28 wt% Cu
composite. Throughout the entire range of annealing temperatures that
we analyzed, a linear increase in the relative density (i. e. a decrease in
the porosity) of the composite is observed when the temperature is
increased.
Fig. 7. The dependency of the relative density of consolidated Fe-28 wt% Cu
samples on the sintering temperature: p – measured density, p0 – theoretical
density. 4. Conclusion

structural elements, high strength properties of the composite obtained In this research paper, we suggest a new method of producing a Fe-
from bimetallic particles can be the result of the formation of a het- 28 wt% Cu composite by compacting and subsequent sintering bime-
erogeneous structure. Further increase in the annealing temperature up tallic nanoparticles made of metals of limited mutual miscibility (iron
to 800°С leads to an insignificant decrease in the microhardness of the and copper) and obtained by the electrical explosion of two intertwined
analyzed material (Fig. 9). wires. It has been shown that as a result of such treatment, a Fe-28 wt%
Thus, our research has shown that as a result of the compaction of Cu composite with the homogeneous distribution of elements
bimetallic nanoparticles obtained by electrical explosion, a Fe-28 wt% throughout its volume is formed. Heating the consolidated samples in
Cu composite is formed, in which the elements are homogeneously the temperature range of 200–400 °C induce the processes of low-
distributed throughout the volume. As a result of annealing of the temperature sintering of copper and iron. When the temperature is
increased to 600 °C, two phenomena are observed: liquid-phase

445
A.S. Lozhkomoev et al. Vacuum 159 (2019) 441–446

Fig. 8. The elementary composition of the surface of the Fe-28 wt% Cu sample after annealing at 800 °C: a – an image of the sample's structure, b – Cu, c – Fe. All bars
2 μm.

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