Synthesis, crystal structure, electric and magnetic properties of new UNiSi₂ splat
We explored the crystal structure, magnetic and transport properties of UNiSi₂ material, which was prepared by rapid solidification—splat cooling. The UNiSi₂ splat is mostly single phase, the refinement of crystal structure indicated orthorhombic CeNiSi₂-type structure (space group Cmcm) with lattic...
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| Cite this: | Synthesis, crystal structure, electric and magnetic properties of new UNiSi₂ splat / Z. Molčanová, M. Mihalik, M. Mihalik Jr., M. Rajňák, M. Zentková, M. Huráková, V. Kavečanský, M. Paukov, L. Havela, M. Cieslar, K. Milianchuk // Физика низких температур. — 2017. — Т. 43, № 8. — С. 1224-1228. — Бібліогр.: 18 назв. — англ. |
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Molčanová, Z. Mihalik, M. M. Mihalik Jr. Rajňák, M. Zentková, M. Huráková, M. Kavečanský, V. Paukov, M. Havela, L. Cieslar, M. Milianchuk, K. 2021-01-30T18:40:27Z 2021-01-30T18:40:27Z 2017 Synthesis, crystal structure, electric and magnetic properties of new UNiSi₂ splat / Z. Molčanová, M. Mihalik, M. Mihalik Jr., M. Rajňák, M. Zentková, M. Huráková, V. Kavečanský, M. Paukov, L. Havela, M. Cieslar, K. Milianchuk // Физика низких температур. — 2017. — Т. 43, № 8. — С. 1224-1228. — Бібліогр.: 18 назв. — англ. 0132-6414 PACS: 75.50.–y, 75.50.Tt https://nasplib.isofts.kiev.ua/handle/123456789/175141 We explored the crystal structure, magnetic and transport properties of UNiSi₂ material, which was prepared by rapid solidification—splat cooling. The UNiSi₂ splat is mostly single phase, the refinement of crystal structure indicated orthorhombic CeNiSi₂-type structure (space group Cmcm) with lattice parameters a = 4.0082 Å, b = 16.0813 Å and c = 4.0064 Å. Also SEM analysis revealed the morphology exhibiting dendritic grains in the matrix. TEM images indicate mixed structure formed by crystalline particles embedded into amorphous or nanocrystalline matrix. Magnetic and electrical properties of the splat resemble properties of samples, which were prepared by conventional methods, exhibiting a ferromagnetic transition at about 91 K and similar temperature dependence of resistivity. The coercive field of μ₀Hc = 2.25 T is much enhanced due to the magnetic anisotropy introduced by the sample preparation technique. Barkhausen jumps were observed on the hysteresis loop. Magnetization of the sample does not saturate in magnetic fields up to μ₀H = 18 T. This work was supported by project ERDF EU, Nos. ITMS26220120005 and VEGA 2/0010/16. en Фізико-технічний інститут низьких температур ім. Б.І. Вєркіна НАН України Физика низких температур Low dimensionality and inhomogeneity effects in quantum matter Synthesis, crystal structure, electric and magnetic properties of new UNiSi₂ splat Article published earlier |
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Synthesis, crystal structure, electric and magnetic properties of new UNiSi₂ splat |
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Synthesis, crystal structure, electric and magnetic properties of new UNiSi₂ splat Molčanová, Z. Mihalik, M. M. Mihalik Jr. Rajňák, M. Zentková, M. Huráková, M. Kavečanský, V. Paukov, M. Havela, L. Cieslar, M. Milianchuk, K. Low dimensionality and inhomogeneity effects in quantum matter |
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Synthesis, crystal structure, electric and magnetic properties of new UNiSi₂ splat |
| title_full |
Synthesis, crystal structure, electric and magnetic properties of new UNiSi₂ splat |
| title_fullStr |
Synthesis, crystal structure, electric and magnetic properties of new UNiSi₂ splat |
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Synthesis, crystal structure, electric and magnetic properties of new UNiSi₂ splat |
| title_sort |
synthesis, crystal structure, electric and magnetic properties of new unisi₂ splat |
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Molčanová, Z. Mihalik, M. M. Mihalik Jr. Rajňák, M. Zentková, M. Huráková, M. Kavečanský, V. Paukov, M. Havela, L. Cieslar, M. Milianchuk, K. |
| author_facet |
Molčanová, Z. Mihalik, M. M. Mihalik Jr. Rajňák, M. Zentková, M. Huráková, M. Kavečanský, V. Paukov, M. Havela, L. Cieslar, M. Milianchuk, K. |
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Low dimensionality and inhomogeneity effects in quantum matter |
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Low dimensionality and inhomogeneity effects in quantum matter |
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2017 |
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English |
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Физика низких температур |
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Фізико-технічний інститут низьких температур ім. Б.І. Вєркіна НАН України |
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Article |
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We explored the crystal structure, magnetic and transport properties of UNiSi₂ material, which was prepared by rapid solidification—splat cooling. The UNiSi₂ splat is mostly single phase, the refinement of crystal structure indicated orthorhombic CeNiSi₂-type structure (space group Cmcm) with lattice parameters a = 4.0082 Å, b = 16.0813 Å and c = 4.0064 Å. Also SEM analysis revealed the morphology exhibiting dendritic grains in the matrix. TEM images indicate mixed structure formed by crystalline particles embedded into amorphous or nanocrystalline matrix. Magnetic and electrical properties of the splat resemble properties of samples, which were prepared by conventional methods, exhibiting a ferromagnetic transition at about 91 K and similar temperature dependence of resistivity. The coercive field of μ₀Hc = 2.25 T is much enhanced due to the magnetic anisotropy introduced by the sample preparation technique. Barkhausen jumps were observed on the hysteresis loop. Magnetization of the sample does not saturate in magnetic fields up to μ₀H = 18 T.
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0132-6414 |
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https://nasplib.isofts.kiev.ua/handle/123456789/175141 |
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Synthesis, crystal structure, electric and magnetic properties of new UNiSi₂ splat / Z. Molčanová, M. Mihalik, M. Mihalik Jr., M. Rajňák, M. Zentková, M. Huráková, V. Kavečanský, M. Paukov, L. Havela, M. Cieslar, K. Milianchuk // Физика низких температур. — 2017. — Т. 43, № 8. — С. 1224-1228. — Бібліогр.: 18 назв. — англ. |
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2025-11-26T21:41:32Z |
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| fulltext |
Low Temperature Physics/Fizika Nizkikh Temperatur, 2017, v. 43, No. 8, pp. 1224–1228
Synthesis, crystal structure, electric and magnetic
properties of new UNiSi2 splat
Z. Molčanová1, M. Mihalik1, M. Mihalik, Jr.1, M. Rajňák1, M. Zentková1, M. Huráková1,
V. Kavečanský1, M. Paukov2, L. Havela2, M. Cieslar2, and K. Milianchuk2,3
1Institute of Experimental Physics SAS, Watsonova 47, 040 01 Košice, Slovakia
2Charles University, Faculty of Mathematics and Physics, Ke Karlovu 5, 121 16 Prague 2, Czech Republic
3Ivan Franko National University of Lviv, 1 Universytetska Str., Lviv 79000, Ukraine
E-mail: zentkova@saske.sk
Received January 31, 2017, published online June 26, 2017
We explored the crystal structure, magnetic and transport properties of UNiSi2 material, which was prepared
by rapid solidification — splat cooling. The UNiSi2 splat is mostly single phase, the refinement of crystal struc-
ture indicated orthorhombic CeNiSi2-type structure (space group Cmcm) with lattice parameters a = 4.0082 Å,
b = 16.0813 Å and c = 4.0064 Å. Also SEM analysis revealed the morphology exhibiting dendritic grains in the
matrix. TEM images indicate mixed structure formed by crystalline particles embedded into amorphous or
nanocrystalline matrix. Magnetic and electrical properties of the splat resemble properties of samples, which
were prepared by conventional methods, exhibiting a ferromagnetic transition at about 91 K and similar tempera-
ture dependence of resistivity. The coercive field of μ0Hc = 2.25 T is much enhanced due to the magnetic anisot-
ropy introduced by the sample preparation technique. Barkhausen jumps were observed on the hysteresis loop.
Magnetization of the sample does not saturate in magnetic fields up to μ0H = 18 T.
PACS: 75.50.–y Studies of specific magnetic materials;
75.50.Tt Fine-particle system; nanocrystalline materials.
Keywords: magnetic anisotropy, Barkhausen jumps, magnetic hysteresis, UNiSi2 splat.
1. Introduction
Research of strongly correlated electron systems is very
attractive part of the physics of condensed matter. Materi-
als with strongly correlated electrons, originating in open
d- or f-shells, have often unusual electrical and magnetic
properties [1,2]. In the case of actinides there are mainly
uranium-based intermetallic compounds, exhibiting diverse
exotic types of effects, as unconventional type of mag-
netism or superconductivity [3], often accompanying by
heavy fermion behavior [4–7]. On the other hand, the study
of uranium compounds is stimulated by the practical use of
nuclear energy (nuclear fuel or waste) [8–10].
The splat cooling technique can facilitate stabilization
of selected polymorphous modifications. It was successful-
ly used for retention of high-temperature γ-uranium phase
to room temperature [11]. It can be expected that the rapid
solidification can stimulate preparation of single phase
from in-congruently melting materials, e.g., UNiSi2.
The uranium compound UNiSi2 melts incongruently,
however single crystals of this compound were grown by the
Czochralski method [12] and in a gallium flux [13]. This
compound crystallizes in the orthorhombic CeNiSi2-type
layered structure (space group Cmcm) [14], which is con-
structed from deformed fragments of the CeGa2Al2 and
α-ThSi2 structures. UNiSi2 exhibits ferromagnetism with
local uranium moments below the Curie temperature TC =
= 95 K [15–17], while a Kondo lattice behavior was report-
ed at higher temperatures [13,15,16]. The residual resist-
ance can be enhanced by high pressure of about 5.5 GPa [13].
A strong magnetic anisotropy was observed on the single
crystal with the easy magnetization direction in the ac
plane [12]. The electronic coefficient γ is small in compar-
ison with uranium heavy fermion compounds [16]. In the
present paper we report on synthesis, characterization, elec-
trical and magnetic properties of samples with nominal com-
positions UNiSi2, which were prepared by the splat cooling
technique and we compare our results with previous re-
© Z. Molčanová, M. Mihalik, M. Mihalik, Jr., M. Rajňák, M. Zentková, M. Huráková, V. Kavečanský, M. Paukov, L. Havela, M. Cieslar, and
K. Milianchuk, 2017
Synthesis, crystal structure, electric and magnetic properties of new UNiSi2 splat
sults, which were obtained on polycrystalline materials and
single crystals [12–17].
2. Experimental results
In the first step, polycrystalline sample of UNiSi2 was
prepared by arc melting from the starting constituents in Ar
atmosphere. For better homogeneity, the sample was several
times turned over and re-melted. The obtained ingot was
subsequently placed into the high vacuum splat cooling
system. In this technique, an alloy is melted by electrical
arc under Ar atmosphere. The molten drop then falls through
a hole in a copper crucible, triggering an infrared photo-
electric switch that initiates movement of two massive cop-
per anvils, which hit the drop producing a splat, which is
a foil of irregular shape and typical thickness 0.1 mm. X-ray
powder diffraction (XRPD) measurements were performed
by Rigaku Ultima IV diffractometer in Bragg Brentano
configuration and as a source we used CuKα1,α2 doublet
radiation (λKα1 = 0.154060 nm, λKα2 = 0.1544430 nm).
Additional analysis was performed by TESCAN VEGA3
scanning electron microscope (SEM) using secondary elec-
trons and back scattered electrons imaging as well energy
dispersive x-ray (EDX) analysis and transmission electron
microscopy (TEM) using a JEOL JEM 2000 FX micro-
scope equipped with a thin-window x-ray energy disper-
sive analyser (EDX).
The magnetic measurements were carried out by the
SQUID magnetometer in MPMS and in applied magnetic
field up to 5 T in the temperature range 2–300 K. High
magnetic field experiments were performed on the Cryo-
gen Free High Field Measurement System (Cryogenic Ltd.)
operating in magnetic field up to 18 T. The electrical resis-
tivity was measured by ac transport method in the tempera-
ture range 5–380 K by the PPMS.
3. Results and discussion
XRPD measurements from both the surface of splat and
the powdered splat revealed that UNiSi2 contains only
small traces of spurious phases. The XRPD patterns were
fitted using Le Baill method and using orthorhombic,
CeNiSi2-type structure as a starting model [14].
The refined lattice parameters are a = 4.0082 Å, b =
= 16.0813 Å and c = 4.0064 Å. We have also detected the
presence of a secondary phase (Fig. 1), however we were
unable to determine the chemical composition of this phase
due to very low contribution from this phase to the total
XRPD pattern.
The SEM analysis from the surface of the polished
UNiSi2 rapidly cooled samples (splats) indicates that the
average composition corresponds to the nominal one. Also
Fig. 1. (Color online) X-ray diffraction pattern of the UNiSi2
splat are shown together with Bragg’s position for main phase
UNiSi2. The secondary phase is indicated by arrows.
Fig. 2. SEM image was taken from the surface in secondary (left) and backscattered (right) electrons.
Low Temperature Physics/Fizika Nizkikh Temperatur, 2017, v. 43, No. 8 1225
Z. Molčanová, et al.
the morphology exhibits dendritic grains, which are nickel-
depleted due to quenching (Fig. 2). The TEM revealed
mixed structure formed cylindrical or spherical nanocrys-
talline particles which are embedded into amorphous or
nanocrystalline matrix with very fine nanoparticles (Fig. 3).
The cylindrical particles have average size of about
20×10 nm. The remaining part of splat contains large crys-
talline blocks with the partially distorted crystal structure.
The results of ac susceptibility measurements suggest
that the UNiSi2 polycrystalline sample has magnetic transi-
tion at 91 K (Fig. 4) as it is evident from pronounced broad
maxima in both real and imaginary part of ac susceptibil-
ity. This temperature shifts somewhat to 90.5 K and the
maximum broadens by the fast cooling synthesis indicating
that fast cooling does not affect the temperature of magnet-
ic phase transition very much. The temperature dependence
of magnetization shows step increase of magnetization be-
low 100 K which we associate with magnetic phase transi-
tion (Fig. 5). The temperature dependence of inverse sus-
ceptibility can be fitted above 180 K to a Curie–Weiss
(CW) law giving the effective moment μeff = 2.82 μB and
θp = 14.3 K for the splat (Fig. 5). The positive value of θp
indicates the ferromagnetic interaction in the sample. The
effective moment is smaller than expected one for free
uranium ion (3.6 μB), but higher than the moment of poly-
crystalline sample or single crystal. The value of θp is
much smaller than in those cases [12,15,17].
Measurements of hysteresis loops indicate ferromagnet-
ic behavior (Fig. 6). The magnetization does not saturate
even at 18 T. Very large coercive field μ0Hc = 2.25 T,
which is comparable with measurements along magnetic
hard axis on single crystal [17], is characteristic feature for
the hysteresis loops of the UNiSi2 splat (Fig. 6). Such en-
hancement of coercive field can be attributed to preferred
orientation of crystallites along the hard magnetic axis or
to pinning of domain walls on additional defects, which
were introduced by rapid solidification, in the conditions of
high anisotropy, producing very narrow domain walls. The
coercive field is nearly the same for measurement with
magnetic field applied along the splat and perpendicular to
the surface of the splat which excluded preferential crystal-
lization of crystals in the sample and large coercive force
due to magneto-crystalline anisotropy. The huge coercive
force can be in this manner attributed to pinning of narrow
domain walls. Remnant magnetization and saturated mag-
netization both depend on applied magnetic field indicating
shape anisotropy. The steps on the hysteresis loops for 2 K
indicate magnetization processes in ferromagnetic material,
which can be related to Barkhausen jumps. The hysteresis
Fig. 4. (Color online) ac susceptibility for polycrystalline is com-
pared with ac susceptibility of splat.
Fig. 5. (Color online) Temperature dependence of magnetization
is plotted together with the inverse susceptibility. Fig. 3. TEM image of the UNiSi2 splat shows mixture structure
consisting of well-defined crystals embedded into the amorphous
or very fine nanocrystalline matrix.
20 nm
1226 Low Temperature Physics/Fizika Nizkikh Temperatur, 2017, v. 43, No. 8
Synthesis, crystal structure, electric and magnetic properties of new UNiSi2 splat
loop becomes smaller with increasing temperature; coer-
cive force and remnant magnetization are reduced. Like-
wise Barkhausen jumps disappear with rising temperature.
We wanted to study magnetic anisotropy in more details
and that is why we compared measurements of hysteresis
loop on the splat and powdered sample and the results are
presented on Fig. 7. In the case of powdered sample the
powder was fixed by glue to ensure that the magnetic field
will not orient powder along easy magnetic axis. As can be
seen (Fig. 7) the shape of hysteresis loops as well magnetic
characteristics like coercive force and remnant magnetiza-
tion are similar only the remnant and saturated magnetiza-
tion at 18 T are higher for splat. The major difference is in
Barkhausen jumps. In the case of splat there are several
jumps on the loop in compare with only two main
Barkhausen jumps on powdered splat.
The temperature dependence of the relative electrical
resistivity, R/R300(T) is shown in Fig. 8. The resistivity
curve resembles the resistivity curves of polycrystalline
material [12,14]. The irregular shape of the sample did not
allow the determination of absolute values of resistivity.
The steep decrease of resistivity below 91 K we associate
with transition to the magnetically ordered state. The low
temperature part of the curve can be fitted by an expres-
sion, containing an exponential term, attributed to electron-
magnon scattering:
2
0
300
exp ,R R cT
R T
∆ = + −
(1)
where 0R is dimension-less relative zero-temperature resist-
ivity parameter and c has dimension [K–2] used for fitting
the relative resistivity data in temperature interval 2–33 K
gives value Δ = 19.3 K. This is somewhat smaller than the
value determined on a polycrystalline material [13,15].
Weakly decreasing resistivity at high temperatures, also
observed in [13], is generic for a broad class of U com-
pounds with sizeable magnetic moments. They lead to a large
spin-disorder resistivity, amounting to weak localization
phenomena [18].
4. Conclusions
UNiSi2 material has been for first time synthetized by
the high vacuum splat cooling technique. The prepared splat
beside the parent compound UNiSi2 contains small amount
of spurious phase as it was detected by XRPD, SEM and
TEM techniques. The TEM revealed that majority of mate-
rial consists of mixed structure formed by cylindrical or
spherical nanocrystalline particles which are embedded into
amorphous or nanocrystalline matrix with very fine nano-
particles. The remaining part of splat contains large crys-
talline blocks with the partially distorted crystal structure.
Rapid solidification of the UNiSi2 splats did not affect the
magnetic transition but resulted in very high coercive force.
Such enhancement of coercive force can be attributed to
Fig. 6. (Color online) Hysteresis loops which were measured on a
splat at various temperatures. Black pattern represents the meas-
urement for transversal direction of magnetic field.
Fig. 7. (Color online) Hysteresis loops which were measured on
a splat and on powdered splat.
Fig. 8. (Color online) Temperature dependence of resistivity for
the UNiSi2 splat. The line represents the fit due to Eq. (1).
Low Temperature Physics/Fizika Nizkikh Temperatur, 2017, v. 43, No. 8 1227
Z. Molčanová, et al.
pinning of domain walls on additional defects, which were
introduced by rapid solidification, in the conditions of high
anisotropy, producing very narrow domain walls. The steps
on the hysteresis loops for 2 K indicate magnetization pro-
cesses in ferromagnetic material, which can be related to
Barkhausen jumps. Temperature of magnetic transition de-
termined value of Δ resembles magnetic and electrical prop-
erties of from magnetization and resistivity measurements
and the polycrystalline UNiSi2 sample.
Acknowledgement
This work was supported by projects ERDF EU,
No. ITMS26220120005 and VEGA 2/0010/16.
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1228 Low Temperature Physics/Fizika Nizkikh Temperatur, 2017, v. 43, No. 8
1. Introduction
2. Experimental results
3. Results and discussion
4. Conclusions
Acknowledgement
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