Сhanges in the structural state and properties of vacuum-arc coatings based on high-entropy alloy TiZrHfNbTa under the influence of nitrogen pressure and bias potential at deposition
Complex studies have been carried out on the effect of nitrogen pressure and the negative bias potential on the structure and properties of vacuum-arc nitride coatings based on the high-entropy alloy TiZrHfNbTa. It is defined that the change in pressure during deposition (in the range 0.01...4 mTo...
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| Опубліковано в: : | Вопросы атомной науки и техники |
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| Дата: | 2018 |
| Автори: | , , , , , , , , , |
| Формат: | Стаття |
| Мова: | Англійська |
| Опубліковано: |
Національний науковий центр «Харківський фізико-технічний інститут» НАН України
2018
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| Назва журналу: | Digital Library of Periodicals of National Academy of Sciences of Ukraine |
| Цитувати: | Сhanges in the structural state and properties of vacuum-arc coatings based on high-entropy alloy TiZrHfNbTa under the influence of nitrogen pressure and bias potential at deposition / O.V. Sobol’, A.A. Andreev, R.P. Mygushchenko, V.F. Gorban’, V.A. Stolbovoy, A.A. Meylekhov, V.V. Subbotina, D.V. Kovteba, A.V. Zvyagolsky, A.E. Vuets // Вопросы атомной науки и техники. — 2018. — № 5. — С. 109-115. — Бібліогр.: 26 назв. — англ. |
Репозитарії
Digital Library of Periodicals of National Academy of Sciences of Ukraine| _version_ | 1859627706216349696 |
|---|---|
| author | Sobol’, O.V. Andreev, A.A. Mygushchenko, R.P. Gorban’, V.F. Stolbovoy, V.A. Meylekhov, A.A. Subbotina, V.V. Kovteba, D.V. Zvyagolsky, A.V. Vuets, A.E. |
| author_facet | Sobol’, O.V. Andreev, A.A. Mygushchenko, R.P. Gorban’, V.F. Stolbovoy, V.A. Meylekhov, A.A. Subbotina, V.V. Kovteba, D.V. Zvyagolsky, A.V. Vuets, A.E. |
| citation_txt | Сhanges in the structural state and properties of vacuum-arc coatings based on high-entropy alloy TiZrHfNbTa under the influence of nitrogen pressure and bias potential at deposition / O.V. Sobol’, A.A. Andreev, R.P. Mygushchenko, V.F. Gorban’, V.A. Stolbovoy, A.A. Meylekhov, V.V. Subbotina, D.V. Kovteba, A.V. Zvyagolsky, A.E. Vuets // Вопросы атомной науки и техники. — 2018. — № 5. — С. 109-115. — Бібліогр.: 26 назв. — англ. |
| collection | DSpace DC |
| container_title | Вопросы атомной науки и техники |
| description | Complex studies have been carried out on the effect of nitrogen pressure and the negative bias potential on the
structure and properties of vacuum-arc nitride coatings based on the high-entropy alloy TiZrHfNbTa. It is defined
that the change in pressure during deposition (in the range 0.01...4 mTorr) mainly affects the nitrogen atoms content
in the coating. The feed of a negative bias potential to the substrate (Ub = -50...-250 V) makes it possible to control
the content of the metallic component using the effect of selective sputtering of atoms in the formation of coatings.
Determined, that as the pressure increases the structural state associated with the predominant growth orientation
(axial texture) of the crystallites changes. The texture changes in the sequence [311] → [311] + [111] → [111] with
increasing pressure for a six-element (TiZrHfVNbTa)N nitride and the texture state changes in the sequence
[110] → [110] + [111] → [111] for a five-element (TiZrHfNbTa)N nitride. It is shown that the presence of a bitextured state in the coating makes it possible to achieve an ultrahard state with a hardness exceeding 50 GPa.
Проведено комплексні дослідження щодо впливу тиску азоту і негативного потенціалу зміщення на
структуру і властивості вакуумно-дугових нітридних покриттів на основі високоентропійного сплаву
TiZrHfNbTa. Визначено, що зміна тиску при осадженні (в інтервалі 0,01 ... 4 мТорр) в основному впливає на
вміст атомів азоту в покритті, а подача негативного потенціалу зміщення на підкладку (Ub = -50...-250 В)
дозволяє управляти вмістом металевої складової використовуючи ефект селективного розпилення атомів
при формуванні покриття. Встановлено, що зі збільшенням тиску відбувається зміна структурного стану,
пов'язаного з переважною орієнтацією зростання (аксіальної текстури) кристалітів. Для шестиелементного
нітриду (TiZrHfVNbТа)N зі збільшенням тиску відбувається зміна текстури в послідовності
[311] → [311] + [111] → [111], а для пʼятиелементного нітриду (TiZrHfNbТа)N текстурний стан змінюється в
послідовності [110] → [110] + [111] → [111]. Показано, що наявність бітекстурного стану в покритті
дозволяє досягти надтвердого стану з твердістю понад 50 ГПа.
Проведены комплексные исследования по влиянию давления азота и отрицательного потенциала
смещения на структуру и свойства вакуумно-дуговых нитридных покрытий на основе высокоэнтропийного
сплава TiZrHfNbTa. Определено, что изменение давления при осаждении (в интервале 0,01…4 мТорр) в
основном влияет на содержание атомов азота в покрытии, а подача отрицательного потенциала смещения на
подложку (Ub.= -50…-250 В) позволяет управлять содержанием металлической составляющей c
использованием эффекта селективного распыления атомов при формировании покрытия. Установлено, что с
увеличением давления происходит изменение структурного состояния, связанного с преимущественной
ориентацией роста (аксиальной текстуры) кристаллитов. Для шестиэлементного нитрида (TiZrHfVNbТа)N с
увеличением давления происходит изменение текстуры в последовательности [311] → [311] + [111] → [111],
а для пятиэлементного нитрида (TiZrHfNbТа)N текстурное состояние изменяется в последовательности
[110] → [110] + [111] → [111]. Показано, что наличие битекстурного состояния в покрытии позволяет
достигнуть сверхтвердого состояния с твердостью, превышающей 50 ГПа.
|
| first_indexed | 2025-11-29T13:26:10Z |
| format | Article |
| fulltext |
ISSN 1562-6016. ВАНТ. 2018. №5(117) 109
CHANGES IN THE STRUCTURAL STATE AND PROPERTIES
OF VACUUM-ARC COATINGS BASED ON HIGH-ENTROPY
ALLOY TiZrHfNbTa UNDER THE INFLUENCE OF NITROGEN
PRESSURE AND BIAS POTENTIAL AT DEPOSITION
O.V. Sobol’
1
, A.A. Andreev
2
, R.P. Mygushchenko
1
, V.F. Gorban’
3
, V.A. Stolbovoy
2
,
A.A. Meylekhov
1
, V.V. Subbotina
1
, D.V. Kovteba
2
, A.V. Zvyagolsky
1
, A.E. Vuets
1
1
National Technical University «Kharkiv Polytechnic Institute», Kharkov, Ukraine
E-mail: sool@kpi.kharkov.ua;
2
National Science Center “Kharkov Institute of Physics and Technology”, Kharkov, Ukraine
E-mail: aandreev@kipt.kharkov.ua;
3
Frantsevich Institute for Problems of Materials Science, Kyiv, Ukraine
Complex studies have been carried out on the effect of nitrogen pressure and the negative bias potential on the
structure and properties of vacuum-arc nitride coatings based on the high-entropy alloy TiZrHfNbTa. It is defined
that the change in pressure during deposition (in the range 0.01...4 mTorr) mainly affects the nitrogen atoms content
in the coating. The feed of a negative bias potential to the substrate (Ub = -50...-250 V) makes it possible to control
the content of the metallic component using the effect of selective sputtering of atoms in the formation of coatings.
Determined, that as the pressure increases the structural state associated with the predominant growth orientation
(axial texture) of the crystallites changes. The texture changes in the sequence [311] → [311] + [111] → [111] with
increasing pressure for a six-element (TiZrHfVNbTa)N nitride and the texture state changes in the sequence
[110] → [110] + [111] → [111] for a five-element (TiZrHfNbTa)N nitride. It is shown that the presence of a bi-
textured state in the coating makes it possible to achieve an ultrahard state with a hardness exceeding 50 GPa.
PACS: 81.07.Bc, 61.05.сp, 68.55.jm, 61.82.Rx
INTRODUCTION
Structural engineering has become a basic method
for achieving the necessary functional properties of
materials [1, 2]. Through the use of structural
engineering, it was possible to create new materials
[3, 4] or stabilize [5] metastable structural states.
Separate direction of structural engineering is the
creation of artificial materials (i. e., materials that are
not identified in nature and are created by specially
developed algorithms) based on multilayer [6] or multi-
element composites [7]. For example, when creating
multilayer composites, the algorithm determines the
thickness of the layers, as well as the required elemental
and phase composition. Such artificial materials have
uniquely high functional characteristics [8]. A
particularly large increase in the functional
characteristics was observed in materials with a
nanostructured state, when the formation was carried
out under strongly nonequilibrium conditions [9]. Such
materials include ion-plasma condensates [10]. Among
methods for the formation of such materials, the greatest
degree of ionization can be achieved by using the
vacuum-arc method [11]. This made it possible to
obtain high-density coatings with high hardness and
wear resistance [12]. The highest mechanical properties
were achieved for multilayer composites based on
transition metal nitrides [13, 14].
In recent years, special attention has been paid to
coatings based on multi-element (high-entropic) alloys
[15]. This is due to the fact that high-entropy alloys
have a unique ordering property in the metal lattice at
high temperatures [16]. The ordering is due to the fact
that in the high-entropic alloys, as a result of the
intensive mixing effect, the contribution of the entropy
factor increases, which stabilizes the formation of a
solid solution with a simple crystal structure.
As is well known, using Boltzmann’s conjecture on
the relationship between entropy and system complexity
[17], the configuration change in entropy, ΔSconf, when
forming a solid solution of n elements with equiatomous
content, can be calculated by the following formula:
1
ln ln( ),confS R R n
n
where R is the ideal gas constant, and n is the number of
mixing elements. At n = 5, ΔSconf = 1.61R, which
approaches the fusion entropy size of most
intermetallides (in the range of values R...2R). This
indicates that only a solid solution of the same type,
namely a solid solution based on face-centered cubic
(fcc), body-centered cubic (bcc), or fcc + bcc crystalline
lattices, is formed mostly in high entropy alloys
[18, 19].
In addition, large lattice distortions caused by the
replacement of several metal elements with different
atomic dimensions lead to a decrease in the diffusion
rate of atoms increasing the effect of the formation and
stabilization of the solid solution, and also contribute,
due to large distortions, to a decrease in the crystallite
growth rate, thereby causing the formation of a
nanoscale and even an amorphous structure. As a result
of high entropy of mixing of such alloys and
deformation of the lattice, solid-solution phases with a
simple face-centered cubic (fcc) or body-centered (bcc)
structure, rather than double or triple intermetallic
compounds, are formed.
Transition metals (Ti, Zr, Hf, Nb, Ta) with a high
heat of nitride formation were used in this paper as base
mailto:sool@kpi.kharkov.ua
mailto:aandreev@kipt.kharkov.ua
110 ISSN 1562-6016. ВАНТ. 2018. №5(117)
elements of high-entropy alloys to obtain coatings with
high hardness, low friction coefficient, good adhesion to
the substrate. The aim of the paper is to determine the
efficiency of using the vacuum-arc deposition method to
obtain materials with high mechanical properties from
composites containing strong nitride-forming
components. The nitrogen atmosphere pressure and the
bias potential were varied during deposition.
SAMPLES AND RESEARCH METHODS
The coatings were deposited by the vacuum-arc
method using upgraded “Bulat-6” unit [11]. A cathode
of the required composition was pre-fabricated by
vacuum-arc remelting of a multicomponent mixture of
pure metal powders. As initial components, metals with
a purity of not less than 99.9% were used. A non-
consumable tungsten cathode was used for remelting.
The crystallized ingot was removed from the
crystallizer, turned over and placed again in a
crystallizer. The melt was melted again and the
procedure was repeated 7 times to obtain the most
homogeneous structure (The technology is developed at
the Institute of Problems of Material Sciences NAS of
Ukraine). The ingot in the form of a cylinder (diameter
~ 45 mm, height ~ 30 mm) was extracted from the
crystallizer and soldered to a titanium cathode using
solder. Thus, target cathodes based on the
Ti+Zr+Nb+Hf+V+Ta system were fabricated (also five-
element Ti+Zr+Nb+Hf+Ta target cathodes were
fabricated), which were used to prepare nitride coatings.
The average composition of the six-element cathode
(at.%): Ti – 18, Zr – 18, Nb – 18, Hf – 15, V – 12,
Ta –19. The composition of the five-element cathode
(at.%): Ti – 27, Zr – 19, Nb – 20, Hf – 14, Ta – 20. The
reactive gas was nitrogen. The deposition parameters
are given in Table.
Samples with size (15x15x2.5 mm) made of
12Х18Н9Т steel (Ra = 0.09 μm) were chosen as the base
for the coatings deposition. The application time was
1.5 hours, coatings thickness was ~ 8.0 μm.
The morphology of the cross section of multi-period
structures was studied with a scanning electron
microscope JEOL JSM840. For electron-microscopic
studies, coatings were deposited on copper substrates
0.2 mm thick. The study of the coatings elemental
composition was carried out by analyzing the spectra of
characteristic X-ray radiation generated by an electron
beam in a scanning electron microscope.
The phase-structure state was studied on a DRON-
3M diffractometer in Cu-Kα-radiation. A graphite
monochromator was used to monochromatize the
detected radiation and was installed in a secondary
beam (in front of the detector). The study of the phase
composition, structure (texture, substructure) was
carried out using traditional X-ray diffractometry
techniques by analyzing the position, intensity, and
shape of the diffraction reflection profiles. The
substructural characteristics (medium microdeformation
<ε> and crystallite size, L) were determined by the two-
order approximation of reflections from planes {111}.
Coatings hardness was measured by the
microindentation method. Microindentation was carried
out at the Micron-gamma unit [20–22] with a load up to
F = 0.5 N using a Berkovich diamond pyramid with
cutting angle of 65
о
, with automatic loading and
unloading for 30 s.
Physico-technological parameters of coatings deposition
Se-
rial
No
Coatings
Ia,
A
If,
А
Ub, V
Р,
Torr
1 (TiZrHfVNbТа)N 90 0.4 150 2·10
-4
2 (TiZrHfVNbТа)N 90 0.4 150 5·10
-4
3 (TiZrHfVNbТа)N 90 0.4 150 7·10
-4
4 (TiZrHfVNbТа)N 90 0.4 150 2·10
-3
5 (TiZrHfVNbТа)N 90 0.4 150 4·10
-3
6 (TiZrHfNbTa)N 110 0 50 1·10
-5
7 (TiZrHfNbTa)N 110 0.5 150 2·10
-4
8 (TiZrHfNbTa)N 110 0.5 150 7·10
-4
9 (TiZrHfNbTa)N 110 0.5 150 1·10
-3
10 (TiZrHfNbTa)N 110 0.5 150 4·10
-3
11 (TiZrHfNbTa)N 110 0.5 50 4·10
-3
12 (TiZrHfNbTa)N 110 0.5 100 4·10
-3
13 (TiZrHfNbTa)N 110 0.5 200 4·10
-3
14 (TiZrHfNbTa)N 110 0.5 250 4·10
-3
RESULTS AND DISCUSSION
Fig. 1 shows that as the pressure of the nitrogen
atmosphere increases, the content of the drop phase in
the nitrides coatings of high-entropy alloys decreases. It
should be noted that as it was stated earlier [23], the
drop phase mainly consists of a metal alloy (in this case
a high-entropy alloy TiZrHfNbTa with a bcc crystal
lattice) with a predominant content of low-melting
metallic constituents. It can be seen that at a low
pressure of 2.5∙10
-4
Torr (see Fig. 1,a), the drop phase is
largely present both in the bulk and on the surface of the
coating, and the size of the droplets varies in a wide
range: from a micron fraction to several units micron.
The increase in pressure leads to a qualitative change in
the content of the drop phase. Fig. 1,b shows that the
presence of a drop phase in the coating volume is not
observed in coatings obtained at a pressure of
1.5∙10
-3
Torr, and individual droplets of a small
(submicron) size are detected on the surface.
The decrease in the content of the drop phase with
increasing Ub can be explained by the fact that the
droplet component, like any other cluster of atoms
placed in the plasma, acquires a negative (floating)
potential and is repelled by a surface on which a
negative potential (in this case, the substrate surface) is
fed.
ISSN 1562-6016. ВАНТ. 2018. №5(117) 111
a
а b
Fig. 1. Morphology of the coatings cross section and coatings surface obtained at pressures 2.5∙10
-4
Torr (а)
and 1.5∙10
-3
Torr (b)
To Energy-dispersive elemental analysis was carried
out on the cross sections of the coatings. This made it
possible to avoid errors while determining the elemental
composition due to the inhomogeneous distribution of
elements on the surface (droplets and other
inhomogeneities). A typical EDX spectrum is shown in
Fig. 2 and the distribution maps of the elements in
Fig. 3.
a
b
Fig. 2. Energy dispersion spectra of coatings obtained
at pressures 2.5∙10
-4
Torr (а)
and 1.5∙10
-3
Torr (b)
Fig. 3 shows that a uniform distribution of all
elements constituting the high-entropic alloy nitride is
observed on the coatings surface obtained at the
nitrogen atmosphere pressure of 1.5∙10
-3
Torr.
Fig. 3. Maps of the
elements distribution on the
coating surface obtained at
a pressure of 1.5∙10
-3
Torr
112 ISSN 1562-6016. ВАНТ. 2018. №5(117)
In this case, a microelement analysis of the nitrogen
content in the coatings (Fig. 4) showed that the increase
in the nitrogen content is especially seen at pressures
0.4...2.0 mTorr. It is to be noted that the atomic
concentration of nitrogen in the coating, taking into
account the mass composition of the metallic
component, is in the range 37...52 at.%. Thus, according
to the absolute value at the maximum pressure of
5.7 mTorr, the atomic nitrogen content exceeds the
content of the metallic component making such coatings
superstoichiometric considering the nitrogen
component.
1 10
40
45
50
,
a
t.
%
Р, mTorr
Fig. 4. Dependence of nitrogen content in coatings on
the nitrogen atmosphere pressure for a six-component
system (Ub = -150 V)
When the displacement potential is changed, the
nitrogen content changes less significantly from
49.84 at.% and Ub = -50 V to 45.77 at.% and
Ub = -250 V.
0,0 0,5 1,0 1,5 2,0 2,5
5
10
15
20
25
30
35
Ta
Hf
ZrNb
V
Р, mTorr
С
M
e ,
a
t.
%
Ti
a
0 50 100 150 200 250 300
10
15
20
25
30
35
Ta
Hf
Zr
Nb
-U
b
, V
С
M
e ,
a
t.
%
Ti
b
Fig. 5. Dependences of the metallic elements content
in coatings obtained: a – at different pressures
(Ub = -150 V) and b – at different bias potentials
(PN = 2 mTorr)
The influence of the nitrogen atmosphere pressure
during deposition has a lesser effect on the ratio change
of the metallic elements in the coating (Fig. 5,a). With
increasing pressure, a small redistribution of elements
takes place. As a result of the redistribution in the
coating, the content of strong nitride-forming elements
increases (mostly Ti, less Ta) and the relative content of
relatively weak (with the lowest gain of free energy
during the formation of nitride) of nitride-forming
elements (V, Nb) decreases. Note that for large P the
content of Hf decreases. The reason for this, apparently,
is the large scattering of the most heavy atoms of
hafnium by their own atoms because of the most
effective energy loss for particles of equal masses.
The feeding of a negative bias potential affects
mostly the change in the elemental composition (see
Fig. 5,b). At a pressure of 2 mTorr, an increase in the
displacement potential leads to a decrease in the content
of the lightest metallic element (Ti) and an increase in
the heavy metal content (Ta and Hf). This clearly
indicates that selective secondary sputtering of atoms is
the determining factor in the formation of the elemental
coating composition. This allows makes it possible to
control the content of the metallic component using the
effect of selective sputtering of atoms in the formation
of coatings. Thus, the content of the lightest element of
titanium decreases almost 2-fold with an increase in Ub
from 50 to 250 V.
The revealed patterns in the elemental composition
indicate that the secondary ballistic sputtering from the
growth surface is the determining effect of the metal
atoms considering feeding Ub [24]. The content of
lightnitrogen gas atoms decreases with increasing Ub.
Also, the content in the titanium atoms coating with a
strong Ti–N bond decreases (the negative formation
heat is 336 kJ/mol [25]). The results obtained make it
possible to assert that the formation process of stable
nitrides is carried out directly in the near-surface growth
layers. In this case, the sputtering process is decisive in
the formation of the composition.
It should be noted that the revealed patterns of
elemental composition control with selective sputtering
in the deposition process broadens the possibilities of
structural engineering by feeding Ub.
The XRD method was used to study the phase
composition and structure. Fig. 6 shows the XRD
spectra of coatings obtained at different pressures of the
working atmosphere (nitrogen gas).
30 40 50 60 70 80
0
2000
4000
6000
8000
10000
12000
14000
5
4
3
2
(2
2
2
)
(3
1
1
)
(2
0
0
)
I,
a
rb
.
u
n
.
2 deg.
(1
1
1
)
1
Fig. 6. XRD-spectra nitride coatings of a six-element
alloy (TiZrHfVNbTa)N, obtained at Ub = -150 V and at
pressure PN, mTorr: 1 – 0.25; 2 – 0.5; 3 – 0.7;
4 – 2.0; 5 – 4.5
ISSN 1562-6016. ВАНТ. 2018. №5(117) 113
It can be seen that a texture [311] is formed at low
pressure, which is sufficiently resistant to radiation
defect formation [26]. This texture is maintained up to a
relatively high pressure of 2 mTorr. At higher pressures,
a bi-texture state with a basic growth texture [111] (see
Fig. 6, spectrum 5) is formed. However, the degree of
perfection of such a texture is not large, which can be
associated with the disorienting effect of atoms of
different sizes in the lattice sites of the metal
components.
The appearance of the plane having preferential
orientation of the crystallites (200) at a relatively low
nitrogen atmosphere pressure (see curves 1–3, Fig. 6)
indicate a mobility increase in the deposited particles
[14] as a result of relatively low energy loss to collisions
under reduced pressure.
An alloy on the basis of a simple bcc lattice (Fig. 7,
spectrum 1) is formed in nitrile coatings based on a five-
element alloy (the absence in the vanadium composition
in contrast to the coatings, the spectra for which are
shown in Fig. 6) at the lowest pressure of 1.5∙10
-5
Torr.
20 30 40 50 60 70 80 90
0
500
1000
1500
2000
2500
3000
3500
4000
4500
5000
(2
2
2
)f
c
c
(3
1
1
)f
c
c
(2
2
0
)f
c
c
(2
0
0
)f
c
c
(1
1
1
)f
c
c
(2
1
1
)b
c
c
(2
0
0
)b
c
c
I,
a
rb
.
u
n
.
2 deg.
5
4
3
2
1
(1
1
0
)b
c
c
Fig. 7. XRD-spectra nitride coatings of a five-element
alloy (TiZrHfNbTa)N, obtained at Ub = -150 V
and at pressure PN, mTorr:
1 – 0.01; 2 – 0.25; 3 – 0.7; 4 – 1.5; 5 – 4
Nitride is formed on the basis of the fcc metal
sublattice (structural type NaCl) with increasing
pressure. However, in contrast to the previous series, a
texture with an axis [110] (see spectrum 2, Fig. 7) is
formed in this series of coatings. The difference in the
axis of the formed texture (from the series in Fig. 6) can
be related to the increasing influence of the radiation
factor due to the higher specific content of heavy
elements. When the pressure (2.5...7)∙10
-4
Torr is
relatively low, then a range of particles without energy
loss for collisions is small. This leads to high-energy
bombardment and the formation of a radiation-
stimulated texture with an axis [110]. Such a texture has
a smaller reticular density in the plane of the surface
(for example, in comparison with [111]).
At a pressure of more than 1 mTorr, as for the series
in Fig. 6, the predominant orientation of crystallite
growth with the axis [111] is observed.
The influence of the bias potential also affects the
structural state. Fig. 8 shows the diffraction spectra of
coatings obtained with different Ub (-50 to -250 V). It
can be seen that in all cases a single-phase state is
formed. Almost untextured state is formed at Ub = -50 V
(see Fig. 8, spectrum 1). A noticeable intensification of
the diffraction peaks intensity from the plane {111}
systems appears at Ub = -100 V (see Fig. 8, spectrum 2),
which determines the preferential orientation of the
crystallites with the axis [111] perpendicular to the
growth surface. With an increase in Ub to -200 V (see
Fig. 8, spectrum 3) and -250 V (see Fig. 8, spectrum 4),
the relative intensity of the {111} peaks increases,
indicating an increase in texture perfection [111]. In this
case, the position of the peaks shifts toward smaller
angles (as shown in Fig. 8 by an arrow) and at θ–2θ the
imaging scheme corresponds to the increase in the
macrostresses of compression in the coating [2].
20 30 40 50 60 70 80 90
0
2000
4000
6000
8000
10000
(2
2
2
)
(3
1
1
)
(2
0
0
)
I,
a
rb
.
u
n
.
2, deg.
1
2
3
4
(111)
Fig. 8. XRD-spectra of coatings deposited at Ub, V:
1 – 50; 2 – 100; 3 – 200; 4 – 250
The most important mechanical characteristics for
most application ranges of coatings is their hardness.
The results of microhardness measurements,
generalized in Fig. 9 depending on pressure, show that
coatings obtained at the pressure range 0.7...2 mTorr
have the greatest hardness.
0 1 2 3 4
0
10
20
30
40
50
60
2
Р, mTorr
H
,
G
P
a
1
Fig. 9. Dependence of coatings microhardness
on the pressure value during their deposition:
1 – for coating based on a six-element
(TiZrHfVNbTa)N high-entropy alloy; 2 – for coating
based on a five-element (TiZrHfNbTa)N high-entropy
alloy
The structural state of such coatings is characterized
by the presence of a bi-texture state ([311] + [111] for
the first series and [110] + [111] for the second series).
As can be seen, the appearance of the texture [110]
results in a relatively lower hardness due to the
radiation-stimulated effect.
The high hardness of coatings based on the 6-
element alloy (compared to the 5-element alloy) which
114 ISSN 1562-6016. ВАНТ. 2018. №5(117)
precipitated at a low pressure of 0.2 mTorr is
determined by the greater deformation of the crystalline
fcc lattice (distortion). This effect is based on the overall
greater discrepancy between the atomic radii for
different elements in the 6-element alloy compared with
the 5-element alloy. The deformation of the crystal
lattice (caused by such a mismatch) makes it difficult to
move dislocations and increases the strength.
The presence of monotexture [111] at a high
pressure of 4 mTorr leads from 35 to 38 GPa typical for
vacuum-plasma condensates of transition metal nitrides
(for this texture type).
This is indicated by the hardness data for coatings
obtained at a pressure of 4 mTorr (when the texture
[111] is formed), but with different displacement
potentials. With increasing Ub (and, correspondingly, at
the structural level, an increase in the degree of texture
perfection [111]), the hardness of coatings increases:
18.7 GPa (Ub = -50 V), 30.1 GPa (Ub = -100 V),
32.6 GPa (Ub = -200 V) up to a value of 40.2 GPa at
Ub = -250V.
CONCLUSIONS
1. Vacuum-arc evaporation of high-entropy alloys in
the nitrogen atmosphere makes it possible to obtain
high-strength nitride coatings.
2. A single-phase state is formed based on the fcc
metal sublattice (structural type NaCl) in
(TiZrHfVNbTa)N and (TiZrHfNbTa)N coatings.
3. The change in pressure during deposition mainly
affects the content of nitrogen atoms in coating, and the
feeding of a negative bias potential to the substrate
makes it possible to control the content of the metallic
component.
4. As the pressure increases, the structural state
associated with the predominant orientation of
crystallite growth changes. The texture changes in the
sequence [311] → [311] + [111] → [111] with
increasing pressure for a six-element (TiZrHfVNbTa)N
nitride, and the texture state changes in the sequence
[110] → [110] + [111] → [111] for a five-element
nitride (TiZrHfNbTa)N.
5. The presence of a bi-textured state in the coating
makes it possible to achieve a superhard state of a
hardness exceeding 50 GPa.
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Статья поступила в редакцию 19.04.2018 г.
ИЗМЕНЕНИЯ СТРУКТУРНОГО СОСТОЯНИЯ И СВОЙСТВ ВАКУУМНО-ДУГОВЫХ
ПОКРЫТИЙ НА ОСНОВЕ ВЫСОКОЭНТРОПИЙНОГО СПЛАВА TiZrHfNbTa
ПОД ВЛИЯНИЕМ ДАВЛЕНИЯ АЗОТА И ПОТЕНЦИАЛА СМЕЩЕНИЯ
ПРИ ОСАЖДЕНИИ
О.В. Соболь, А.А. Андреев, Р.П. Мигущенко, В.Ф. Горбань, В.А. Столбовой, А.А. Мейлехов,
В.В. Субботина, Д.В. Ковтеба, А.В. Звягольский, А.Е. Вуец
Проведены комплексные исследования по влиянию давления азота и отрицательного потенциала
смещения на структуру и свойства вакуумно-дуговых нитридных покрытий на основе высокоэнтропийного
сплава TiZrHfNbTa. Определено, что изменение давления при осаждении (в интервале 0,01…4 мТорр) в
основном влияет на содержание атомов азота в покрытии, а подача отрицательного потенциала смещения на
подложку (Ub.= -50…-250 В) позволяет управлять содержанием металлической составляющей c
использованием эффекта селективного распыления атомов при формировании покрытия. Установлено, что с
увеличением давления происходит изменение структурного состояния, связанного с преимущественной
ориентацией роста (аксиальной текстуры) кристаллитов. Для шестиэлементного нитрида (TiZrHfVNbТа)N с
увеличением давления происходит изменение текстуры в последовательности [311] → [311] + [111] → [111],
а для пятиэлементного нитрида (TiZrHfNbТа)N текстурное состояние изменяется в последовательности
[110] → [110] + [111] → [111]. Показано, что наличие битекстурного состояния в покрытии позволяет
достигнуть сверхтвердого состояния с твердостью, превышающей 50 ГПа.
ЗМІНИ СТРУКТУРНОГО СТАНУ І ВЛАСТИВОСТЕЙ ВАКУУМНО-ДУГОВИХ
ПОКРИТТІВ НА ОСНОВІ ВИСОКОЕНТРОПІЙНОГО СПЛАВУ TiZrHfNbTa
ПІД ВПЛИВОМ ТИСКУ АЗОТУ І ПОТЕНЦІАЛУ ЗМІЩЕННЯ ПРИ ОСАДЖЕННІ
О.В. Соболь, А.А. Андрєєв, Р.П. Мигущенко, В.Ф. Горбань, В.О. Столбовий, А.О. Мейлехов,
В.В. Суботіна, Д.В. Ковтеба, О.В. Зв`ягольський, О.Є. Вуєць
Проведено комплексні дослідження щодо впливу тиску азоту і негативного потенціалу зміщення на
структуру і властивості вакуумно-дугових нітридних покриттів на основі високоентропійного сплаву
TiZrHfNbTa. Визначено, що зміна тиску при осадженні (в інтервалі 0,01 ... 4 мТорр) в основному впливає на
вміст атомів азоту в покритті, а подача негативного потенціалу зміщення на підкладку (Ub = -50...-250 В)
дозволяє управляти вмістом металевої складової використовуючи ефект селективного розпилення атомів
при формуванні покриття. Встановлено, що зі збільшенням тиску відбувається зміна структурного стану,
пов'язаного з переважною орієнтацією зростання (аксіальної текстури) кристалітів. Для шестиелементного
нітриду (TiZrHfVNbТа)N зі збільшенням тиску відбувається зміна текстури в послідовності
[311] → [311] + [111] → [111], а для пʼятиелементного нітриду (TiZrHfNbТа)N текстурний стан змінюється в
послідовності [110] → [110] + [111] → [111]. Показано, що наявність бітекстурного стану в покритті
дозволяє досягти надтвердого стану з твердістю понад 50 ГПа.
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| id | nasplib_isofts_kiev_ua-123456789-147672 |
| institution | Digital Library of Periodicals of National Academy of Sciences of Ukraine |
| issn | 1562-6016 |
| language | English |
| last_indexed | 2025-11-29T13:26:10Z |
| publishDate | 2018 |
| publisher | Національний науковий центр «Харківський фізико-технічний інститут» НАН України |
| record_format | dspace |
| spelling | Sobol’, O.V. Andreev, A.A. Mygushchenko, R.P. Gorban’, V.F. Stolbovoy, V.A. Meylekhov, A.A. Subbotina, V.V. Kovteba, D.V. Zvyagolsky, A.V. Vuets, A.E. 2019-02-15T17:41:39Z 2019-02-15T17:41:39Z 2018 Сhanges in the structural state and properties of vacuum-arc coatings based on high-entropy alloy TiZrHfNbTa under the influence of nitrogen pressure and bias potential at deposition / O.V. Sobol’, A.A. Andreev, R.P. Mygushchenko, V.F. Gorban’, V.A. Stolbovoy, A.A. Meylekhov, V.V. Subbotina, D.V. Kovteba, A.V. Zvyagolsky, A.E. Vuets // Вопросы атомной науки и техники. — 2018. — № 5. — С. 109-115. — Бібліогр.: 26 назв. — англ. 1562-6016 PACS: 81.07.Bc, 61.05.сp, 68.55.jm, 61.82.Rx https://nasplib.isofts.kiev.ua/handle/123456789/147672 Complex studies have been carried out on the effect of nitrogen pressure and the negative bias potential on the structure and properties of vacuum-arc nitride coatings based on the high-entropy alloy TiZrHfNbTa. It is defined that the change in pressure during deposition (in the range 0.01...4 mTorr) mainly affects the nitrogen atoms content in the coating. The feed of a negative bias potential to the substrate (Ub = -50...-250 V) makes it possible to control the content of the metallic component using the effect of selective sputtering of atoms in the formation of coatings. Determined, that as the pressure increases the structural state associated with the predominant growth orientation (axial texture) of the crystallites changes. The texture changes in the sequence [311] → [311] + [111] → [111] with increasing pressure for a six-element (TiZrHfVNbTa)N nitride and the texture state changes in the sequence [110] → [110] + [111] → [111] for a five-element (TiZrHfNbTa)N nitride. It is shown that the presence of a bitextured state in the coating makes it possible to achieve an ultrahard state with a hardness exceeding 50 GPa. Проведено комплексні дослідження щодо впливу тиску азоту і негативного потенціалу зміщення на структуру і властивості вакуумно-дугових нітридних покриттів на основі високоентропійного сплаву TiZrHfNbTa. Визначено, що зміна тиску при осадженні (в інтервалі 0,01 ... 4 мТорр) в основному впливає на вміст атомів азоту в покритті, а подача негативного потенціалу зміщення на підкладку (Ub = -50...-250 В) дозволяє управляти вмістом металевої складової використовуючи ефект селективного розпилення атомів при формуванні покриття. Встановлено, що зі збільшенням тиску відбувається зміна структурного стану, пов'язаного з переважною орієнтацією зростання (аксіальної текстури) кристалітів. Для шестиелементного нітриду (TiZrHfVNbТа)N зі збільшенням тиску відбувається зміна текстури в послідовності [311] → [311] + [111] → [111], а для пʼятиелементного нітриду (TiZrHfNbТа)N текстурний стан змінюється в послідовності [110] → [110] + [111] → [111]. Показано, що наявність бітекстурного стану в покритті дозволяє досягти надтвердого стану з твердістю понад 50 ГПа. Проведены комплексные исследования по влиянию давления азота и отрицательного потенциала смещения на структуру и свойства вакуумно-дуговых нитридных покрытий на основе высокоэнтропийного сплава TiZrHfNbTa. Определено, что изменение давления при осаждении (в интервале 0,01…4 мТорр) в основном влияет на содержание атомов азота в покрытии, а подача отрицательного потенциала смещения на подложку (Ub.= -50…-250 В) позволяет управлять содержанием металлической составляющей c использованием эффекта селективного распыления атомов при формировании покрытия. Установлено, что с увеличением давления происходит изменение структурного состояния, связанного с преимущественной ориентацией роста (аксиальной текстуры) кристаллитов. Для шестиэлементного нитрида (TiZrHfVNbТа)N с увеличением давления происходит изменение текстуры в последовательности [311] → [311] + [111] → [111], а для пятиэлементного нитрида (TiZrHfNbТа)N текстурное состояние изменяется в последовательности [110] → [110] + [111] → [111]. Показано, что наличие битекстурного состояния в покрытии позволяет достигнуть сверхтвердого состояния с твердостью, превышающей 50 ГПа. en Національний науковий центр «Харківський фізико-технічний інститут» НАН України Вопросы атомной науки и техники Физика радиационных и ионно-плазменных технологий Сhanges in the structural state and properties of vacuum-arc coatings based on high-entropy alloy TiZrHfNbTa under the influence of nitrogen pressure and bias potential at deposition Зміни структурного стану і властивостей вакуумно-дугових покриттів на основі високоентропійного сплаву TiZrHfNbTa під впливом тиску азоту і потенціалу зміщення при осадженні Изменения структурного состояния и свойств вакуумно-дуговых покрытий на основе высокоэнтропийного сплава TiZrHfNbTa под влиянием давления азота и потенциала смещения при осаждении Article published earlier |
| spellingShingle | Сhanges in the structural state and properties of vacuum-arc coatings based on high-entropy alloy TiZrHfNbTa under the influence of nitrogen pressure and bias potential at deposition Sobol’, O.V. Andreev, A.A. Mygushchenko, R.P. Gorban’, V.F. Stolbovoy, V.A. Meylekhov, A.A. Subbotina, V.V. Kovteba, D.V. Zvyagolsky, A.V. Vuets, A.E. Физика радиационных и ионно-плазменных технологий |
| title | Сhanges in the structural state and properties of vacuum-arc coatings based on high-entropy alloy TiZrHfNbTa under the influence of nitrogen pressure and bias potential at deposition |
| title_alt | Зміни структурного стану і властивостей вакуумно-дугових покриттів на основі високоентропійного сплаву TiZrHfNbTa під впливом тиску азоту і потенціалу зміщення при осадженні Изменения структурного состояния и свойств вакуумно-дуговых покрытий на основе высокоэнтропийного сплава TiZrHfNbTa под влиянием давления азота и потенциала смещения при осаждении |
| title_full | Сhanges in the structural state and properties of vacuum-arc coatings based on high-entropy alloy TiZrHfNbTa under the influence of nitrogen pressure and bias potential at deposition |
| title_fullStr | Сhanges in the structural state and properties of vacuum-arc coatings based on high-entropy alloy TiZrHfNbTa under the influence of nitrogen pressure and bias potential at deposition |
| title_full_unstemmed | Сhanges in the structural state and properties of vacuum-arc coatings based on high-entropy alloy TiZrHfNbTa under the influence of nitrogen pressure and bias potential at deposition |
| title_short | Сhanges in the structural state and properties of vacuum-arc coatings based on high-entropy alloy TiZrHfNbTa under the influence of nitrogen pressure and bias potential at deposition |
| title_sort | сhanges in the structural state and properties of vacuum-arc coatings based on high-entropy alloy tizrhfnbta under the influence of nitrogen pressure and bias potential at deposition |
| topic | Физика радиационных и ионно-плазменных технологий |
| topic_facet | Физика радиационных и ионно-плазменных технологий |
| url | https://nasplib.isofts.kiev.ua/handle/123456789/147672 |
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