Durability of the multicomponent nitride coatings based on TiN and (Ti,Al)N deposited by PIII&D method
The multicomponent nitride coatings based on TiN and (Ti, Al)N with small additions of Y, Re, Ni, Cr, Si, Mo, Fe synthesized by the PIII&D method from the filtered cathodic-arc plasma. The crystalline nitride phase in all coatings is of the cubic structure of NaCl type. All investigated coatings...
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Національний науковий центр «Харківський фізико-технічний інститут» НАН України
2015
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| Цитувати: | Durability of the multicomponent nitride coatings based on TiN and (Ti,Al)N deposited by PIII&D method / V.V. Vasyliev, V.S. Goltvyanytsya, S.K. Goltvyanytsya, A.A. Luchaninov, V.G. Marinin, E.N. Reshetnyak, V.E. Strel'nitskij, G.N. Tolmachоva // Вопросы атомной науки и техники. — 2015. — № 2. — С. 130-138. — Бібліогр.: 35 назв. — англ. |
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irk-123456789-824542015-05-30T03:02:16Z Durability of the multicomponent nitride coatings based on TiN and (Ti,Al)N deposited by PIII&D method Vasyliev, V.V. Goltvyanytsya, V.S. Goltvyanytsya, S.K. Luchaninov, A.A. Marinin, V.G. Reshetnyak, E.N. Strel'nitskij, V.E. Tolmachоva, G.N. Физика радиационных и ионно-плазменных технологий The multicomponent nitride coatings based on TiN and (Ti, Al)N with small additions of Y, Re, Ni, Cr, Si, Mo, Fe synthesized by the PIII&D method from the filtered cathodic-arc plasma. The crystalline nitride phase in all coatings is of the cubic structure of NaCl type. All investigated coatings were characterized with the hardness of 23…36 GPa and Young's modulus of 324…436 GPa. The addition of dopants reduces the average rate of cavitation and abrasive wear of the coatings. The best durability demonstrated coating deposited from the cathode of the Ti₀.₄₉Al₀.₅₀Y₀.₀₀₆Re₀.₀₀₀₅ composition. This coating also demonstrated high thermal stability. Многокомпонентные нитридные покрытия на основе TiN и (Ti, Al)N с малыми добавками Y, Re, Ni, Cr, Si, Mo, Fe синтезированы PIII&D-методом из фильтрованной катодно-дуговой плазмы. Во всех исследованных покрытиях обнаружена кристаллическая нитридная фаза с кубической структурой типа NaCl. Покрытия характеризуются твердостью 23…36 ГПа и модулем Юнга 324…436 ГПа. Добавка примесных элементов приводит к уменьшению средней скорости кавитационного и абразивного износа покрытий. Наилучшую стойкость и термостабильность показало покрытие, осажденное из катода состава Ti₀.₄₉Al₀.₅₀Y₀.₀₀₆Re₀.₀₀₀₅. Багатокомпонентні нітридні покриття на основі TiN й (Ti, Al)N з малими домішками Y, Re, Ni, Cr, Si, Mo, Fe синтезовані PIII&D-методом з фільтрованої катодно-дугової плазми. У всіх досліджених покриттях виявлено кристалічну нітридну фазу з кубічною структурою типу NaCl. Покриття характеризуються твердістью 23…36 ГПа та модулем Юнга 324…436 ГПа. Додавання домішкових елементів призводить до зменшення середньої швидкості кавітаційного та абразивного зносу покриттів. Найліпшу стійкість та термостабільність має покриття, осаджене з катоду складу Ti₀.₄₉Al₀.₅₀Y₀.₀₀₆Re₀.₀₀₀₅. 2015 Article Durability of the multicomponent nitride coatings based on TiN and (Ti,Al)N deposited by PIII&D method / V.V. Vasyliev, V.S. Goltvyanytsya, S.K. Goltvyanytsya, A.A. Luchaninov, V.G. Marinin, E.N. Reshetnyak, V.E. Strel'nitskij, G.N. Tolmachоva // Вопросы атомной науки и техники. — 2015. — № 2. — С. 130-138. — Бібліогр.: 35 назв. — англ. 1562-6016 http://dspace.nbuv.gov.ua/handle/123456789/82454 539.21:621.793 en Вопросы атомной науки и техники Національний науковий центр «Харківський фізико-технічний інститут» НАН України |
| institution |
Digital Library of Periodicals of National Academy of Sciences of Ukraine |
| collection |
DSpace DC |
| language |
English |
| topic |
Физика радиационных и ионно-плазменных технологий Физика радиационных и ионно-плазменных технологий |
| spellingShingle |
Физика радиационных и ионно-плазменных технологий Физика радиационных и ионно-плазменных технологий Vasyliev, V.V. Goltvyanytsya, V.S. Goltvyanytsya, S.K. Luchaninov, A.A. Marinin, V.G. Reshetnyak, E.N. Strel'nitskij, V.E. Tolmachоva, G.N. Durability of the multicomponent nitride coatings based on TiN and (Ti,Al)N deposited by PIII&D method Вопросы атомной науки и техники |
| description |
The multicomponent nitride coatings based on TiN and (Ti, Al)N with small additions of Y, Re, Ni, Cr, Si, Mo, Fe synthesized by the PIII&D method from the filtered cathodic-arc plasma. The crystalline nitride phase in all coatings is of the cubic structure of NaCl type. All investigated coatings were characterized with the hardness of 23…36 GPa and Young's modulus of 324…436 GPa. The addition of dopants reduces the average rate of cavitation and abrasive wear of the coatings. The best durability demonstrated coating deposited from the cathode of the Ti₀.₄₉Al₀.₅₀Y₀.₀₀₆Re₀.₀₀₀₅ composition. This coating also demonstrated high thermal stability. |
| format |
Article |
| author |
Vasyliev, V.V. Goltvyanytsya, V.S. Goltvyanytsya, S.K. Luchaninov, A.A. Marinin, V.G. Reshetnyak, E.N. Strel'nitskij, V.E. Tolmachоva, G.N. |
| author_facet |
Vasyliev, V.V. Goltvyanytsya, V.S. Goltvyanytsya, S.K. Luchaninov, A.A. Marinin, V.G. Reshetnyak, E.N. Strel'nitskij, V.E. Tolmachоva, G.N. |
| author_sort |
Vasyliev, V.V. |
| title |
Durability of the multicomponent nitride coatings based on TiN and (Ti,Al)N deposited by PIII&D method |
| title_short |
Durability of the multicomponent nitride coatings based on TiN and (Ti,Al)N deposited by PIII&D method |
| title_full |
Durability of the multicomponent nitride coatings based on TiN and (Ti,Al)N deposited by PIII&D method |
| title_fullStr |
Durability of the multicomponent nitride coatings based on TiN and (Ti,Al)N deposited by PIII&D method |
| title_full_unstemmed |
Durability of the multicomponent nitride coatings based on TiN and (Ti,Al)N deposited by PIII&D method |
| title_sort |
durability of the multicomponent nitride coatings based on tin and (ti,al)n deposited by piii&d method |
| publisher |
Національний науковий центр «Харківський фізико-технічний інститут» НАН України |
| publishDate |
2015 |
| topic_facet |
Физика радиационных и ионно-плазменных технологий |
| url |
http://dspace.nbuv.gov.ua/handle/123456789/82454 |
| citation_txt |
Durability of the multicomponent nitride coatings based on TiN and (Ti,Al)N deposited by PIII&D method / V.V. Vasyliev, V.S. Goltvyanytsya, S.K. Goltvyanytsya, A.A. Luchaninov, V.G. Marinin, E.N. Reshetnyak, V.E. Strel'nitskij, G.N. Tolmachоva // Вопросы атомной науки и техники. — 2015. — № 2. — С. 130-138. — Бібліогр.: 35 назв. — англ. |
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Вопросы атомной науки и техники |
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130 ISSN 1562-6016. ВАНТ. 2015. №2(96)
UDC 539.21:621.793
DURABILITY OF THE MULTICOMPONENT NITRIDE COATINGS
BASED ON TiN AND (Ti, Al)N DEPOSITED BY PIII&D METHOD
V.V. Vasyliev*, V.S. Goltvyanytsya**, S.K. Goltvyanytsya**, A.A. Luchaninov*,
V.G. Marinin*, E.N. Reshetnyak*, V.E. Strel'nitskij*, G.N. Tolmachоva*
*National Science Center “Kharkov Institute of Physics and Technology”,
Kharkov, Ukraine;
**Real Ltd., Ukraine
The multicomponent nitride coatings based on TiN and (Ti, Al)N with small additions of Y, Re, Ni, Cr, Si, Mo,
Fe synthesized by the PIII&D method from the filtered cathodic-arc plasma. The crystalline nitride phase in all
coatings is of the cubic structure of NaCl type. All investigated coatings were characterized with the hardness of
23…36 GPa and Young's modulus of 324…436 GPa. The addition of dopants reduces the average rate of cavitation
and abrasive wear of the coatings. The best durability demonstrated coating deposited from the cathode of the
Ti0.49Al0.50Y0.006Re0.0005 composition. This coating also demonstrated high thermal stability.
INTRODUCTION
Doping the nitride coatings with small amounts of B,
Si, Cr, V, Nb, Y, Hf and other elements that are
traditionally added to the heat-resistant alloys can
significantly improve their wear and heat resistance [1–
14]. It enables to develop new multicomponent
nanostructured coatings used for protection the tools
and machine components that undergo extreme
environmental conditions.
The PIII&D (plasma immersion ion implantation
and deposition) method combined with FVAD (filtered
vacuum arc deposition) is powerful tool for fabricating
the wide range of high quality coatings [15]. Among the
factors which affect the mechanical and functional
properties of the nitride coatings the chemical
composition and energy of ions deposited (adjusted by
the substrate potential) were examined. However, other
deposition process parameters should be taken into
consideration too, for example, plasma gas composition
(or the partial pressure of nitrogen and argon) also plays
an important role [16–19]: nitrogen (N2) being the
reactive gas for nitride synthesis and argon (Ar) gas is
widely used for improving operation stability of the
vacuum-arc sources.
Present work is a logical continuation of our earlier
investigations [20, 21], where the structure and
properties of the TiN, (Ti, Al)N and (Ti, Al)N coatings
doped with Y were studied. We use the developed
method of the nitride coatings deposition for search new
perspective coatings of novel elemental compositions.
Futhermore in the present experiments Ar pressure was
varied as an important parameter of the technological
deposition process, because different cathode materials
need different Ar pressure values for supplying stable
vacuum arc source operation as it follows from the
experiment.
The main goal of the present work was development
novel multicomponent nitride coatings by PIII&D
method using filtered vacuum-arc plasma source and as-
cast Ti-based and TiAl-based cathodes with additions of
Cr, Si, Y, Re, Ni, Mo, Fe in various combinations and
comparative estimation of their functional properties.
The influence of doping elements and deposition
process parameters on the composition, structure,
mechanical characteristics and functional properties of
the multicomponent nitride coatings was investigated.
We tested the doped coatings on the cavitation and
abrasion resistance as well as their oxidation resistance.
1. EXPERIMENTAL METHODS
The nitride coatings of Ti-N and Ti-Al-N systems
doped with small additions of Cr, Si, Y, Re, Ni, Mo, Fe
were produced by vacuum-arc method. The straight
magnetoelectric filter was used for removing the
macroparticles from the plasma stream [22]. The
scheme of the installation used for coatings deposition
was presented elsewhere [20]. The alloys of
Ti0.49Al0.50Y0.01, Ti0.86Si0.13Y0.01, Ti0.48Al0.50Ni0.01Cr0.01,
Ti0.88Mo0.11Fe0.01Y0.002, Ti0.49Al0.50Y0.006Re0.0005,
Ti0.49Al0.50Y0.01Re0.001 elemental composition produced
via vacuum-arc remelting in argon atmosphere (by Real
Ltd., Zaporozhye, Ukraine) were used as cathode
materials in vacuum-arc plasma source. The coatings
with the thickness in the range of 6…8 μm were
deposited on stainless steel substrates with geometry
17×20×0.6 mm. The distance from the filter outlet to the
specimens was of 180 mm. A glow discharge in argon
at pressure of PAr = 4 Pa and pulsed substrate bias
potential of 2.5 kV amplitude relative to the vacuum
chamber was used for cleaning the substrates surface.
Coatings were deposited at an arc current of 100 A.
Partial nitrogen and argon pressure in the vacuum
chamber were in the ranges 0.1…0.2 and 0.01…0.02 Pa
accordingly. The pulsed potential of negative polarity
with the amplitude of 1.5…2.5 kV, pulse duration 5 μs
and repetition frequency 24 kHz was applied to the
substrate. In the time intervals between the pulses the
substrate was at “floating” potential of 3…15 V.
Additional magnetic focusing of the plasma flow in the
vacuum chamber ensured a high deposition rate of
12…16 μm/h. Coating deposition duration was 30 min.
The elemental composition of the coatings was
measured by X-ray fluorescence analysis (XRA) with
the vacuum scanning crystal diffraction spectrometer
SPRUT. The concentration of Ti, Al and doping
elements was calculated without taking into account the
nitrogen content. It is well known that in some cases,
ISSN 1562-6016. ВАНТ. 2015. №2(96) 131
when the characteristic lines intensity depends on the
thickness of thin film, the values of the elements
concentration determined by the XRA spectrometer
requires correction for the thickness [23]. In the present
experiments correction on the coating thickness was
applied only for measurements concentrations in the
coatings which contained Y, Re and Mo elements.
The X-ray diffraction (XRD) measurements were
performed on a DRON-3 diffractometer in the filtered
Cu-Kα radiation on (θ-2θ) configuration. Judging by the
position of the nitride diffraction lines of a cubic NaCl-
type structure the value of the crystal lattice parameter
in the direction of the normal to the film surface was
determined. The size of the crystal grains (coherent
scattering zone) of nitride films was calculated using the
Scherrer relation, in which the full width at half
maximum (FWHM) was taken from the (111) or (220)
peaks in XRD patterns.
The hardness (H) and reduced Young’s modulus (E)
of the coatings was measured with a G200 nanoindenter
in CSM (continuous stiffness measurement) mode. The
H and E values were taken at the depth of indentation,
equal to 10% of the film thickness.
The erosion under the action of cavitation in distilled
water at room temperature was studied in the facility
with an ultrasonic vibrator [21]. The mass loss was
measured with an accuracy of 0.015 mg. As a rule the
tests lasted until visually watched open-ended pores in
the coating began to form, but for all of these the depth
of erosive defects did not reach 5…6 μm. Owing to such
restriction only the coating material loss was measured
in the test, not the substrate one. The average wear rate
was used as a criterion for the coating durability.
The abrasive wear of the coatings was determined
by the gravimetric method using the scheme “plane
specimen rotating abrasive disk” at linear velocity of
4.38 m/s and normal load of 2.2 N. The test duration
was 40 min. Coatings adhesion was evaluated on the
results of the Rockwell indenter test.
The oxidation resistance of the coatings was studied
with a thermal analyzer (Netzsch STA 449 F Jupiter) in
the range of 20…1000 °C at a heating rate of 20 K/min
in a mixture of dry nitrogen (80 vol.%) and oxygen
(20 vol.%) with a flow rate of 70 ml/min.
2. RESULTS AND DISCUSSION
2.1. STRUCTURE AND PROPERTIES OF THE
MULTICOMPONENT TiN-BASED AND
(Ti, Al)N-BASED NITRIDE COATINGS DOPED
WITH Cr, Si, Y, Ni, Mo, Fe
The coatings described in this section were
deposited under identical process parameters: nitrogen
partial pressure 0.1 Pa, argon partial pressure 0.01 Pa,
the substrate bias potential amplitude of 1.5 kV [20].
The cathodes compositions and characteristics of the
multicomponent nitride coatings are listed in Table 1.
For comparison the characteristics of the TiN and
(Ti0.5Al0.5)N coatings deposited at the same process
parameters are shown too. On the results of XRA
measurements the concentration of the doping elements
in the coatings approximately equals to that in the
cathode materials. The only exception is Si
concentration in the coating of the specimen #2 which is
three times lower than that in the cathode material. Such
effect was reported too by the authors of the works [24,
25].
The X-ray diffraction patterns of the
multicomponent nitride coatings are shown in Fig. 1. It
was revealed the only crystalline nitride phase in the
films, namely a cubic NaCl-type structure. The only
exception is the specimen #3 (the coating deposited
using the Ti0.88Mo0.11Fe0.01Y0.002 cathode), which
included another phase, probably Mo9Ti4. Two phases
were also revealed in vacuum-arc nitride coatings of
Mo-N system deposited at high substrate bias [26].
Table 1
The results of the XRD analysis and mechanical properties of the multicomponent nitride coatings produced
with use of the cathodes of various composition (amplitude of pulse substrate bias potential 1.5 kV; partial pressure
of the gas mixture: nitrogen – 0.1 Pa and argon – 0.01 Pa)
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2 Ti0.86Si0.13Y0.01 0.4283 8 (hh0) 1900 32.1 387
3 Ti0.88Mo0.11Fe0.01Y0.002 0.4296 6 (hh0) 1078 28.5 374
4 Ti0.5Al0.50 0.4212 7 (hh0) 1702 31.4 436
5 Ti0.48Al0.50Ni0.01Cr0.01 0.4208 6 (hh0) 370 25.8 324
6 Ti0.49Al0.50Y0.01 0.4209 9 (hh0) 6160 35.8 418
132 ISSN 1562-6016. ВАНТ. 2015. №2(96)
Table 2
Deposition parameters and characteristics of the coatings deposited with use of Ti0.49Al0.50Y0.01 cathode
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7 2.5 0.1 0.01 Ti0.51Al0.48Y0.01N (hh0) 2184 30.1 380 12.5 12 2.7
8 2.5 0.1 0.015 Ti0.51Al0.48Y0.01N (h00) 1400 27.5 364
9 2.5 0.1 0.018 Ti0.54Al0.41Y0.01N (hhh) 630 32.5 378 1.7 8 7.6
10 2.5 0.2 0.018 Ti0.52Al0.47Y0.01N (h00) 850 22.9 325 1.7 8 2.9
6 1.5 0.1 0.01 Ti0.49Al0.50Y0.01N (hh0) 6160 35.8 418 3.7 12 3.8
11 1.5 0.1 0.015 Ti0.54Al0.45Y0.01N (hhh) 270 30.1 360 5.0 4 9.7
12 1.5 0.2 0.018 Ti0.52Al0.47Y0.01N (h00) 900 31.1 383 3.3 4 2.0
The nitride phase in all coatings has a strong texture
with a preferred orientation of the (hh0) crystallographic
planes parallel to the surface of the coating. The (220)
peak is dominant in all XRD patterns, but its intensity
for different coatings differs greatly. At the same time
width of the (220) peak is close enough for all coatings.
This fact indicates that the grain size of crystallites in all
coatings is nearly of the same value which does not
exceed 13 nm (see Table 1).
For the films fabricated from the cathodes based on
Ti0.5Al0.5 alloy with different dopants (specimens #46),
a nitride crystal lattice period amounts to about
0.421 nm. This value is considerably lower than that for
the films deposited from the cathodes based on Ti with
dopants (specimens #13): 0.428…0.430 nm. All
investigated coatings were characterized by hardness of
26…36 GPa and Young’s modulus of 324…436 GPa.
Hardness of the Ti0.97Si0.03Y0.02N coating was
32.1 GPa, that is slightly higher than that of the TiN one
(specimen #1) produced using the same process
parameters. This result agrees well with the well known
fact of increase in hardness of the TiN coating in case Si
doping [24]. On the contrary, addition of
Mo0.08Fe0.01Y0.005 resulted in decrease in hardness of the
coating to 28.5 GPa. The Ti0.49Al0.47Ni0.03Cr0.01N coating
was characterized by lower hardness (25.8 GPa) than
the Ti0.5Al0.5N one (31.4 GPa).
The results of cavitation tests of specimens with the
coatings of various compositions are presented in Fig. 2.
The dependencies of the mass losses show that all
investigated coatings are characterized by low cavitation
wear, much lower than that of the substrate (austenite
stainless steel). Fig. 3 shows the micrographs of the
surface of the coatings after the test.
It can be seen that the TiN coating has the worst
cavitation resistance. Few pits are observed on its
surface which reach the substrate during the first 1.5 h
period of the test because of strongly pronounced
columnar structure of the coating [21].
The nitride coatings with additions of Ni, Cr, Si, Mo, Fe
show better cavitation resistance than TiN one. They
withstood cavitation impact for 2, 3 h before the wear
rate began increased sharply. A sufficiently large
number of defects in form of small pits and cracks on
the surface of these coatings are visible after all
cavitation tests (see Fig. 3,b). The Ti0.5Al0.5N coating,
doped with Y, demonstrated the best cavitation
resistance. It stood the 12 hours testing. The wear rate of
this coating was lower than that of the rest, and the
number of defects on the eroded surface was little (see
Fig. 3,c). This coating is also characterized by the
highest hardness of about 36 GPa. The results of
abrasive wear tests of coatings are shown in Fig. 4. The
abrasive wear rate of the doped coatings does not
exceed 7∙10
-3
mg/min. It is three orders of magnitude
lower than that of uncoated stainless steel and an order
of magnitude lower than the wear rate of the TiN
coating. The TiN coatings doped with Mo, Fe (specimen
#3) and the (Ti, Al)N coatings doped with Y (specimen
#6) were the most abrasion resistant. Thus, the coatings
fabricated from Ti0.49Al0.50Y0.01 cathode have good
promise as resistant material against both types of wear.
The search for correlations between the cavitation
erosion resistance and properties of materials remains
up to now the issue of great importance [2730]. Our
observations did not reveal correlation between the
cavitation erosion resistance and hardness of
multicomponent nitride coatings. However, the
experiment shows clearly that the addition of impurities
improves durability. This may be due to suppression the
columnar structure in coating during its growth because
of the doping [4, 21].
An important characteristic of the coatings is also
the quality of the adhesion to the substrate. We used the
Rockwell indenter test for evaluation the adhesion level.
In Fig. 5 the photographs of the indenter prints on the
coating surface after testing are presented.
ISSN 1562-6016. ВАНТ. 2015. №2(96) 133
a
b
Fig. 1. XRD scans of the nitride coatings, deposited
using the cathodes of different elemental composition
(amplitude of pulse substrate bias potential 1.5 kV;
partial pressure of the gas mixture:
N2 – 0.1 Pa and Ar – 0.01 Pa):
a – Ti-based cathodes;
b – Ti0.5Al0.5-based cathodes
Fig. 2. Kinetic curves of the cavitation wear of the
TiN-based and (Ti, Al)N-based coatings doped with the
different elements (amplitude of pulse substrate bias
potential 1.5 kV; partial pressure of the gas mixture:
N2 – 0.1 Pa and Ar – 0.01 Pa)
a
b
c
Fig. 3. Surface images of the TiN-based and
(Ti, Al)N-based coatings doped with different elements
after cavitation test (amplitude of pulse substrate bias
potential 1.5 kV; partial pressure of the gas mixture:
N2 – 0.1 Pa and Ar – 0.01 Pa): a – TiN;
b – TiN+Si+Y (specimen #2);
c – (Ti,Al)N+Y (specimen #6)
There is an evident difference in adhesion levels of
the TiN-based and (Ti, Al)N-based coatings.
Delamination of the TiN+Si+Y and TiN+Mo+Fe+Y
coatings in their contact with the Rockwell indenter
indicates poor adhesion of these coatings to the
substrate. On the contrary, the (Ti, Al)N+Ni+Cr and
(Ti, Al)N+Y coatings do not break down and not peel
off from the substrate showing a fairly good adhesion.
There are no radial cracks at the edges of the prints on
the surface of these coatings. So, the best mechanical
characteristics along with good adhesion and durability
demonstrated the (Ti, Al)N+Y coating. The results of
detailed investigations of the coatings of this system are
presented in the next section.
134 ISSN 1562-6016. ВАНТ. 2015. №2(96)
Fig. 4. Abrasive wear rate of the TiN-based and
(Ti, Al)N-based coatings doped with different elements
(amplitude of pulse substrate bias potential 1.5 kV;
partial pressure of the gas mixture:
N2 – 0.1 Pa and Ar – 0.01 Pa)
2.2. INFLUENCE OF THE DEPOSITION
PARAMETERS ON THE STRUCTURE
AND WEAR RESISTANCE OF THE (Ti, Al)N
COATINGS DOPED WITH Y
This section presents the results of studies of the
effect of the partial pressure of gases (nitrogen, argon)
and the amplitude of the high-voltage pulsed bias
potential on the characteristics of the coatings produced
using the Ti0.49Al0.50Y0.01 cathode. Table 2 shows the
deposition parameters, structural and mechanical
characteristics of the coatings and the results of
cavitation and abrasion tests.
Cubic solid solution is the sole nitride phase, which
is detected by X-ray analysis in the studied (Ti,Al)N
coatings doped with Y. However, it should be noted that
some of the coatings may have an amorphous-
crystalline (heterophasic) structure, i. e. contain a
substantial amount of amorphous phase. This is
evidenced by the extremely low intensity of the
reflections in its XRD patterns. Thus the width of the
diffraction peaks is not very different. The grain size of
such nitride coatings is in the range of 6…8 nm.
It is well known that the integrated intensity of the
diffraction lines of the crystalline phase is proportional
to its content in the irradiated volume [31]. It is
decreased greatly with increase in Ar content in gas
mixture (see Table 2). At the same time the changes of
the preferred orientation of nitride grains occur.
Quantitative description of the texture was done by
calculations of the texture coefficients for reflections
(111), (200) and (220). The texture coefficient was
defined in accordance with [32].
Dependence of the texture coefficient on argon
partial pressure for specimens #79 deposited at pulsed
bias potential amplitude of 2.5 kV and nitrogen partial
pressure of 0.1 Pa is shown in Fig. 6. With increase in
argon pressure in the range of 0.01…0.018 Pa the
change in the preferred orientation of the crystallites in
the coatings occurs in the following sequence:
(hh0)→(h00)→(hhh). The preferential grain orientation
in the other investigated nitride coatings shown in
Table 2.
a
b
c
d
Fig. 5. Fragments of the Rockwell imprints on the
surface of TiN-based and (Ti, Al)N-based coatings
doped with the different elements: a TiN+Si+Y;
b TiN+Mo+Fe+Y; c (Ti,Al)N+Ni+Cr;
d (Ti, Al)N+Y. Insertions are the common view
of the imprints
It can be seen that for coatings deposited at a lower
bias potential of 1.5 kV (specimens #6, 11) such change
in orientation from (hh0) to (hhh) is observed at a lower
argon pressure – 0.015 Pa. Thus, with increase in the
argon partial pressure the crystal structure of the nitride
coatings is changed from crystalline to an amorphous-
crystalline heterophasic one and preferred orientation
from (hh0) to (hhh). Changing the preferred orientation
ISSN 1562-6016. ВАНТ. 2015. №2(96) 135
of the grains in the vacuum arc nitride coatings as a
result of adding argon to the gas phase was also
observed by the authors of [18, 33].
It is well known that the ion bombardment
significantly affects the microstructure of films growing
from the vapor phase [34]. In general, two main effects
occur by increasing the argon ion bombardment during
deposition. (1) A rapid increase in the number of
secondary nuclei and discontinuance of columnar
growth. (2) Increase in strain energy of the film due to
increase in energy of arrival ions and its sub-
implantation. In our case, influence of the ions
bombardment becomes stronger at higher argon partial
pressure and higher substrate bias voltage.
Fig. 6. Effect of the partial pressure of Ar on texture
coefficients of the coatings obtained using the
Ti0.49Al0.50Y0.01 cathode (amplitude of pulse substrate
bias potential 2.5 kV, partial pressure of N2 in the gas
mixture of 0.1 Pa)
The texture evolution of a film was predicted by the
authors of the work [18] in frames of minimization the
overall energy of the film, which includes the surface
free energy, interface energy and strain energy. When
the films were grown under low-stress conditions (low
argon pressure and bias potential), the strain energy
should not dominate the overall energy of the films, and
(100) or (110) orientations would be the preferred these
because they possess the lowest surface energy
compared to the (111) one for the TiN films. Vice versa,
when the films were grown under the high stress, the
strain energy determines the overall energy of the films,
the (111) orientation became preferred one because it
has the lowest strain energy [35].
Our studies have shown that if a high voltage pulse
bias potential is applied to a substrate, the wear
resistance of vacuum-arc deposited nitride coatings
depends greatly on the argon content in N2+Ar gas
mixture because of the structural changes caused in the
coating by argon ion bombardment. Thus, increase in
argon content in the gas mixture significantly
deteriorates the cavitation resistance of the deposited
coatings (see Table 2).
Fig. 3,c represents typical for all the coatings image
of eroded surface with some small enough pits. The
observed average wear rate correlates with the
cavitation defects density. The results indicate that the
coatings obtained at elevated partial pressure of argon
are characterized with both enhanced density of erosion
defects on the surface and increased speed of deepening
the erosion pits under the cavitation impact.
To explain these results it should be noted that an
important factor which determines the crystalline
structure and properties of the coatings is their
elemental composition, which can be varied to some
extent by changing parameters of the deposition
process. The XRA data on the ratio of the metal
components in the coating which are presented in
Table 2 show that with increasing partial pressure of
argon the content of aluminum in the coating is reduced.
This may be due to selective sputtering of light elements
atoms from the surface under argon ion bombardment
during the deposition of the coatings [19]. With increase
in argon pressure the intensity of bombardment is
increased, and the concentration of aluminum in the
coating decreased. All of the above can be fully
attributed to the lightest coating component – nitrogen.
It is very likely that the amorphous-crystalline
structure in the coatings deposited at higher partial
pressure of argon (specimens #9, 11) arises in
consequence of deviation from stoichiometric nitride
composition. XRD data on the structure of the coatings
deposited at increased to 0.2 Pa nitrogen partial pressure
(specimens #10, 12) confirm this assumption. More
nitrogen in the gas mixture promotes formation of more
crystalline nitride phase and stoichiometric composition.
Indeed, in these coatings the aluminum concentration is
of 47% and the degree of crystallinity is increased, and
the preferred orientation (h00) returns. As a result,
cavitation resistance of the coating is improved.
Concerning the abrasion resistance, all coatings are
characterized by rather low values of the abrasive wear
rate. However, low abrasive wear does not guarantee
high cavitation resistance of the coating (specimens #9,
10). There was not observed unambiguous correlation
between the hardness and wear resistance of the
coatings. The rates of cavitation and abrasive wear of
the specimen #6 with hardness value of 36 GPa are
higher than these of the specimen #10 with hardness
value of 23 GPa. These results are in line with the
findings of our previous work [21], where it was shown
that the cavitation and abrasive wear resistance of
coatings was determined by a complex variety of factors
including hardness, crystallite size and its preferred
orientation, surface roughness and residual stress level.
2.3. PROPERTIES OF THE (Ti, Al)N-BASED
COATINGS SIMULTANEOUSLY DOPED WITH
Y AND RE
The (Ti, Al)N coatings simultaneously doped with Y
and Re, whose characteristics are given in Table 3,
show the same basic structural features and properties as
the (Ti, Al)N coating doped with Y alone. Increase in
partial pressure of argon during deposition leads to a
reduction in the aluminum content in the coating,
alteration structure from the predominantly crystalline
onto the amorphous-crystalline one and deterioration of
their durability. Specimen #13 (cathode composition
Ti0.49Al0.50Y0.006Re0.0005) demonstrated the best
resistance against cavitation and abrasive wear among
all specimens investigated in our experiments. Fig. 7
illustrates the effect of doping with Y and Re on the
136 ISSN 1562-6016. ВАНТ. 2015. №2(96)
cavitation wear of the (Ti, Al)N coatings, deposited
under optimum gas mixture parameters (nitrogen and
argon partial pressure of 0.1 and 0.01 Pa accordingly).
For the (Ti, Al)N coating, simultaneously doped with Y
and Re, formation of open-ended defects under
cavitation lasts 14 h, and the rate of cavitation wear is
reduced noticeably.
Table 3
Deposition parameters and characteristics of (Ti,Al)N coatings, doped with Y and Re
S
p
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Cavitation tests
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N2 Ar
13 1.5 0.1 0.01 Ti0.53Al0.46Y0.006Re0.0005N (h00) 1000 28.2 354 1.7 14 2.0
14 1.5 0.1 0.016 Ti0.53Al0.46Y0.01Re0.001N (hhh) 252 29.4 341 5 8 13.8
15 2.5 0.1 0.016 Ti0.57Al0.42Y0.01Re0.001N (hhh) 510 29.4 355 1.7 10 4.1
As for amorphous-crystalline coatings deposited at a
higher partial pressure of argon (specimens #14, 15)
using the Ti0.49Al0.50Y0.01Re0.001 cathode, their cavitation
resistance is substantially lower than that for the
specimen #13 with predominantly crystalline structure.
At that, hardness and Young’s modulus of these
coatings are close within the measurement error.
Fig. 7. Effect of doping the (Ti, Al)N coating with Y and
Re on the kinetic curves of cavitation wear (amplitude
of pulse substrate bias potential 1.5 kV, partial pressure
of the gas mixture: N2 – 0.1 Pa and Ar – 0.01 Pa)
Another important characteristic for technical
applications of the coatings is their resistance to
oxidation. Fig. 8 shows the thermogravimetric curves of
the specimens with the (Ti, Al)N coatings doped with Y
and Re. It can be seen that adding any of used additions
to the base elemental composition (Ti, Al)N improves
the oxidation resistance, but to a variable degree. The
thermal stability of the specimen #13, which showed the
best wear resistance, is also maximal. Its oxidation onset
temperature is 950 °C and the weight gain at 1000 °C is
minimal (0.01%). These characteristics are close to the
values obtained previously for the Ti0.49Al0.50Y0.01N
coating [20]. Specimen #14, synthesized at a higher
partial pressure of argon, begins to oxidize slightly
earlier, that is at 810 °C, but after some time the
oxidation rate is decreased dramatically, and its mass
gain at 1000 °C substantially coincides with that for the
specimen #13.
Fig. 8. Thermogravimetric curves of specimens with the
(Ti, Al)N coating and these, doped with Y and Re,
deposited at partial pressure of N2 in the gas mixture of
0.1 Pa and various values of pulsed substrate bias
potential amplitude and argon partial pressure:
1 (Ti, Al)N (amplitude of 1.5 kV, Ar pressure of
0.01 Pa); 2 (Ti, Al)N+Y+Re (amplitude of 1.5 kV,
Ar pressure of 0.01 Pa); 3 (Ti, Al)N+Y+Re
(amplitude of 1.5 kV, Ar pressure of 0.016 Pa);
4 (Ti, Al)N+Y+Re (amplitude of 2.5 kV, Ar pressure
of 0.016 Pa)
Apparently, an oxide film is formed on a specimen
surface and therefore prevents further intensive
oxidation. Also, it can be seen that increase in the
substrate bias potential during deposition leads to the
deterioration of the oxidation resistance. Specimen #15,
deposited at pulsed bias potential with amplitude of
2.5 kV, begins to oxidize even before the (Ti, Al)N
coating, at a temperature of 625 °C, however, its
oxidation rate is 2.5 times lower.Thus, specimen #13
showed all-time high durability against various
deleterious factors simultaneously: thermal oxidation,
ISSN 1562-6016. ВАНТ. 2015. №2(96) 137
abrasive and cavitation wear. The role of yttrium and
rhenium additions is still largely unclear, but the results
of the tests show promising possibilities in improving
the protective properties of the multicomponent nitrides
deposited by the PIII&D method.
CONCLUSIONS
The structure and properties of the multicomponent
TiN and (Ti, Al)N coatings with small additions of Y,
Re, Ni, Cr, Si, Mo, Fe, synthesized by the PIII&D
method from the filtered cathodic arc plasma were
investigated. It was established that crystalline nitride
phase in all coatings is of the cubic structure of the
NaCl type, but its quantity and the preferred orientation
of the crystallites depends on the elemental composition
of the gas phase and the amplitude of the high voltage
pulsed substrate bias potential. All investigated coatings
were characterized by relatively high hardness of
23…36 GPa and Young’s modulus of 324…436 GPa.
The cavitation and abrasion wear resistance of the
nitride multicomponent TiN-based and (Ti, Al)N-based
coatings were investigated. The addition of dopants
reduced the average rate of both types of wear. The
most efficient was the doping of the (Ti, Al)N coatings
with small amounts of Y and Re. The best durability
demonstrated coating produced using the cathode
Ti0.49Al0.50Y0.006Re0.0005, at pulsed substrate bias
potential amplitude of 1.5 kV and partial pressure of
nitrogen of 0.1 Pa and argon of 0.01 Pa. This coating
demonstrated high thermal stability, as well.
It was found that the structure and mechanical
properties of the coatings are very sensitive to the
parameters of the deposition process. Increase in the
partial pressure of argon in the range of 0.01…0.018 Pa
and pulsed substrate bias potential amplitude from 1.5
to 2.5 kV during deposition of the (Ti, Al)N coatings
doped with Y and Re results in formation the
amorphous-crystalline structure with less amount of
crystalline phase, characterized by significantly worse
cavitation and oxidation resistance. Both cavitation and
abrasive resistance of the amorphous-crystalline
coatings with (hhh) orientation are significantly worse
than that of predominantly crystalline coatings with
(hh0) or (h00) orientation.
Thus, the multicomponent nitride coatings with
close elemental composition and mechanical properties
can fundamentally differ in their durability and thermal
oxidation resistance because of the peculiarities of its
crystal structure.
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Статья поступила в редакцию 22.01.2015 г.
ИЗНОСОСТОЙКОСТЬ МНОГОКОМПОНЕНТНЫХ НИТРИДНЫХ ПОКРЫТИЙ
НА ОСНОВЕ TiN И (Ti, Al)N, ОСАЖДЕННЫХ МЕТОДОМ PIII&D
В.В. Васильев, В.С. Голтвяница, С.К. Голтвяница, А.А. Лучанинов, В.Г. Маринин, Е.Н. Решетняк,
В.Е. Стрельницкий, Г.Н. Толмачева
Многокомпонентные нитридные покрытия на основе TiN и (Ti, Al)N с малыми добавками Y, Re, Ni, Cr,
Si, Mo, Fe синтезированы PIII&D-методом из фильтрованной катодно-дуговой плазмы. Во всех
исследованных покрытиях обнаружена кристаллическая нитридная фаза с кубической структурой типа
NaCl. Покрытия характеризуются твердостью 23…36 ГПа и модулем Юнга 324…436 ГПа. Добавка
примесных элементов приводит к уменьшению средней скорости кавитационного и абразивного износа
покрытий. Наилучшую стойкость и термостабильность показало покрытие, осажденное из катода состава
Ti0.49Al0.50Y0.006Re0.0005.
ЗНОСОСТІЙКІСТЬ БАГАТОКОМПОНЕНТНИХ НІТРИДНИХ ПОКРИТТІВ НА ОСНОВІ TiN
ТА (Ti, Al)N, ОСАДЖЕНИХ МЕТОДОМ PIII&D
В.В. Васильєв, В.С. Голтв’яниця, С.К. Голтв’яниця, О.А. Лучанінов, В.Г. Маринін, О.М. Решетняк,
В.Є. Стрельницький, Г.М. Толмачова
Багатокомпонентні нітридні покриття на основі TiN й (Ti, Al)N з малими домішками Y, Re, Ni, Cr, Si,
Mo, Fe синтезовані PIII&D-методом з фільтрованої катодно-дугової плазми. У всіх досліджених покриттях
виявлено кристалічну нітридну фазу з кубічною структурою типу NaCl. Покриття характеризуються
твердістью 23…36 ГПа та модулем Юнга 324…436 ГПа. Додавання домішкових елементів призводить до
зменшення середньої швидкості кавітаційного та абразивного зносу покриттів. Найліпшу стійкість та
термостабільність має покриття, осаджене з катоду складу Ti0.49Al0.50Y0.006Re0.0005.
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