Ion beam-assisted deposition technology as a method of nanocrystalline coating formation
This scientific paper describes the structure, phase composition and mechanical properties of nanocrystalline coatings obtained using the ion beam-assisted deposition technology. The results of computer simulation of IBAD processes for different energy values of bombarding ions and for relationships...
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Національний науковий центр «Харківський фізико-технічний інститут» НАН України
2014
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| Цитувати: | Ion beam-assisted deposition technology as a method of nanocrystalline coating formation / A.G. Guglya, I.G. Marchenko // Вопросы атомной науки и техники. — 2014. — № 2. — С. 125-136 — Бібліогр.: 31 назв. — англ. |
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irk-123456789-799452015-04-10T03:02:40Z Ion beam-assisted deposition technology as a method of nanocrystalline coating formation Guglya, A.G. Marchenko, I.G. Физика радиационных и ионно-плазменных технологий This scientific paper describes the structure, phase composition and mechanical properties of nanocrystalline coatings obtained using the ion beam-assisted deposition technology. The results of computer simulation of IBAD processes for different energy values of bombarding ions and for relationships between the densities of ion fluxes and metal deposition rates is given. The data of electron-microscope analysis of the initial stages of film structure formation (of 5 nm thick and more) is presented. And finally we demonstrate the influence produced by the ion energy and ion current density on the formation of nanocrystalline structure and its correlation with tribological properties of coatings. Дается описание структуры, фазового состава и механических характеристик нанокристаллических покрытий, полученных с использованием технологии ионно-стимулированного осаждения (IBAD method). Приводятся результаты компьютерного моделирования IBAD процесса для различных энергий бомбардирующих ионов и различных соотношений между скоростью осаждения покрытий и плотностью ионных потоков. Представлены данные электронно-микроскопических исследований начальной стадии формирования нанокристаллических структур (толщиной 5 нм и больше). И наконец, продемонстрированы влияние энергии ионов и плотности ионных потоков на формирование нанокристаллических структур и их корреляция с трибологическими свойствами покрытий. Приводиться опис структури, фазового складу та механічних характеристик нанокристалічних покриттів, які здобуваються з використанням технології іонно-стимульованого осадження (IBAD method). Приводяться результати комп’ютерного моделювання IBAD процесу для різних енергій бомбардуючих іонів та різних співвідношень між швидкостями осадження покриттів та щільністю іонних потоків. Представлені також дані електронно-мікроскопічних досліджень початкової стадії формування нанокристалічних структур (товщиною 5 нм и вище). В останньому розділі продемонстровано вплив енергії іонів та щільності іонних потоків на формування нанокристалічних структур та їх кореляція з трибологічними властивостями покриттів. 2014 Article Ion beam-assisted deposition technology as a method of nanocrystalline coating formation / A.G. Guglya, I.G. Marchenko // Вопросы атомной науки и техники. — 2014. — № 2. — С. 125-136 — Бібліогр.: 31 назв. — англ. 1562-6016 PACS: 81.15Jj;81.07Bc;61.20Ja http://dspace.nbuv.gov.ua/handle/123456789/79945 en Вопросы атомной науки и техники Національний науковий центр «Харківський фізико-технічний інститут» НАН України |
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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 Guglya, A.G. Marchenko, I.G. Ion beam-assisted deposition technology as a method of nanocrystalline coating formation Вопросы атомной науки и техники |
| description |
This scientific paper describes the structure, phase composition and mechanical properties of nanocrystalline coatings obtained using the ion beam-assisted deposition technology. The results of computer simulation of IBAD processes for different energy values of bombarding ions and for relationships between the densities of ion fluxes and metal deposition rates is given. The data of electron-microscope analysis of the initial stages of film structure formation (of 5 nm thick and more) is presented. And finally we demonstrate the influence produced by the ion energy and ion current density on the formation of nanocrystalline structure and its correlation with tribological properties of coatings. |
| format |
Article |
| author |
Guglya, A.G. Marchenko, I.G. |
| author_facet |
Guglya, A.G. Marchenko, I.G. |
| author_sort |
Guglya, A.G. |
| title |
Ion beam-assisted deposition technology as a method of nanocrystalline coating formation |
| title_short |
Ion beam-assisted deposition technology as a method of nanocrystalline coating formation |
| title_full |
Ion beam-assisted deposition technology as a method of nanocrystalline coating formation |
| title_fullStr |
Ion beam-assisted deposition technology as a method of nanocrystalline coating formation |
| title_full_unstemmed |
Ion beam-assisted deposition technology as a method of nanocrystalline coating formation |
| title_sort |
ion beam-assisted deposition technology as a method of nanocrystalline coating formation |
| publisher |
Національний науковий центр «Харківський фізико-технічний інститут» НАН України |
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2014 |
| topic_facet |
Физика радиационных и ионно-плазменных технологий |
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http://dspace.nbuv.gov.ua/handle/123456789/79945 |
| citation_txt |
Ion beam-assisted deposition technology as a method of nanocrystalline coating formation / A.G. Guglya, I.G. Marchenko // Вопросы атомной науки и техники. — 2014. — № 2. — С. 125-136 — Бібліогр.: 31 назв. — англ. |
| series |
Вопросы атомной науки и техники |
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AT guglyaag ionbeamassisteddepositiontechnologyasamethodofnanocrystallinecoatingformation AT marchenkoig ionbeamassisteddepositiontechnologyasamethodofnanocrystallinecoatingformation |
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2025-07-06T03:52:09Z |
| last_indexed |
2025-07-06T03:52:09Z |
| _version_ |
1836868100174118912 |
| fulltext |
ISSN 1562-6016. ВАНТ. 2014. №2(90) 125
Раздел четвертый
ФИЗИКА РАДИАЦИОННЫХ
И ИОННО-ПЛАЗМЕННЫХ ТЕХНОЛОГИЙ
ION BEAM-ASSISTED DEPOSITION TECHNOLOGY AS A METHOD
OF NANOCRYSTALLINE COATING FORMATION
Review article
A.G. Guglya, I.G. Marchenko
National Science Center “Kharkov Institute of Physics and Technology”, Kharkov, Ukraine
E-mail: guglya@kipt.kharkov.ua
This scientific paper describes the structure, phase composition and mechanical properties of nanocrystalline
coatings obtained using the ion beam-assisted deposition technology. The results of computer simulation of IBAD
processes for different energy values of bombarding ions and for relationships between the densities of ion fluxes
and metal deposition rates is given. The data of electron-microscope analysis of the initial stages of film structure
formation (of 5 nm thick and more) is presented. And finally we demonstrate the influence produced by the ion
energy and ion current density on the formation of nanocrystalline structure and its correlation with tribological
properties of coatings.
PACS: 81.15Jj;81.07Bc;61.20Ja
INTRODUCTION
Perennial attempts made by the researchers in
different countries of the world, who work in the field
of production and application of thin-films, to develop
technologies that would improve the structure-phase
stability of such thin films resulted in the development
of physical vapor deposition methods (PVD). The
success achieved in this field can in many respects be
attributed to the creation of different plasma plants and
accelerated ion sources in the early sixties. It has been
established that an increase in the ion component in the
flux of deposited metal atoms and molecules results in a
considerable change in the structure and properties of
produced films. The use of nitrogen, carbon and boron
ions as charged particles allowed for the formation of
coatings made of nitrides, carbides and borides whose
performance characteristics considerably surpassed
those of metals.
An ever-increasing demand for the extension of the
resource of articles operating under high mechanical
loads, elevated temperatures and corrosion media
promoted the development of such coating deposition
technologies that allow for the formation of a coating
structure by intensive bombardment with ions of
> 100 eV. The purpose of ion bombardment is to
provide controllable variation of the progress rate of
diffusion processes, grain nucleation and growth
conditions and also an increase in chemical activity of
atoms. To produce such coatings nowadays solely no
equilibrium technologies are used that include the
stimulation bombardment of a deposited material with
gas ions whose energy ranges from several tens of eV to
tens of keV (Table). These methods include traditional
PVD methods including unbalanced magnetron
sputtering (UBM) and ion beam-assisted deposition
(IBAD).
Physical phenomena that occur in the depth and on
the surface of the material exposed to ion bombardment
differ for different technologies. Fig. 1 schematically
shows most of those processes.
PVD and UMS methods usually deal with processes
that occur on the film surface. As for the IBAD method
the depth pass of gas ions reaches 100nm. Therefore
their influence on the structure and phase composition is
not limited by the film surface region; it captures
approximately the same film thickness (Fig. 1). The
main processes that take place on the film surface in this
connection are as follows: surface diffusion promotion
and the creation of surface defects that are the major
centers of grain nucleation and also maintenance of the
high flow of radiation defects, which provides the
formation of stoichiometric Me-(N,O,C) compounds
and highly dispersed structure stabilization. While
comparing the parameters of technological processes
given in Table the attention should be paid to the first
two, in particular accelerating potential (ion energy) and
working gas pressure in the chamber. It is seen that the
IBAD method differs by high ion energy and low gas
pressure in the process chamber. High energy provides
good coating adhesion due to the ballistic mixing of
condensed atoms with substrate atoms. PVD and UMS
methods employ high process temperature for the
mixing. The IBAD method requires no high temperature
maintenance, which allows for the formation of the film
structure in no equilibrium conditions. Particularly at
such conditions the nucleation and growth of ultrafine
grains of 5 to 10 nm (nano grains) take place. It should
be noted that in the case of the IBAD method the
structure formation is not ended at the nucleation stage.
The film material is exposed to the gas ion beam until
the thicknesses of ~100 nm is reached; this provides
stabilization both of component composition and grain
size. The advantage of low pressure inside the process
chamber is that the formed coatings have low porosity
and low pollution with gas impurities. And finally, in
the case of the IBAD technology metal evaporators and
gas ion sources are spaced and this provides an
opportunity to independently control each parameter of
the ion-assisted deposition process and have stable
impact on the coating structure. Fig. 2 gives diagrams of
two the most spread configurations of the IBAD
method.
126 ISSN 1562-6016. ВАНТ. 2014. №2(90)
PVD, UMS and IBAD methods performances
PVD UMS IBAD
E, Ud, (V) 20-300 0-200 500-50000
Gas pressure, Pа 0.05…8.0 0.05…1.0 10-2…10-3
T, оС 200…600 100…400 20…200
Working gas N2 Ar + N2 Ar or N2
Damages, eV/at. 10…102 1.0…10 102…104
Depth of the damaged zone, nm 1…5 <1 10…100
Fig. 1. Surface and in-depth physical phenomena of the IBAD process
a
b
Fig. 2. The main variants of IBAD technology
realisation:
а – e-beam metal evaporation + ion bombardment;
b – ion-beam metal sputtering + ion bombardment
The option given in Fig. 2,a has more opportunities
for the rate control of metal evaporation and therefore it
is employed by industrial ion beam-assisted deposition
plants.
1. COMPUTER SIMULATION OF THE ION
BEAM-ASSISTED DEPOSITION
To simulate the process of ion beam –assisted
deposition we used a computer SRIM program of atom
–atom collisions [1]. A peculiar feature of this method is
that the portion of ions is reflected from the surface
reducing thus total ion flux during the bombardment of
deposited film with ions. The interaction of ions with
the surface results in the sputtering of deposited film
and the rate of its growth is reduced. In the steady-state
mode the film boundary moves at a rate V along the
“x”-axis. In time t the profile of interstitial atoms
),( txg shifts together with the boundary of a growing
film. During time t the concentration of interstitial
atoms at a point x will change by a value of
∫=Δ
t
i dttxgjxc
0
),()( , where ij is the flux density of
incident ions. We consider the stationary process of film
growth and therefore )0,(),( Vtxgtxg −= . It means
that the profile of an implanted dopant is simply shifted
with time. The concentration at a point x can be found
through the integration.
ISSN 1562-6016. ВАНТ. 2014. №2(90) 127
∫
−
=
x
Vtx
i duug
V
jxC )()( , (1)
On elapse of some time stt the stationary nitrogen
distribution )(xCst should be established, which in the
future shifts together with the surface. Its value can be
derived if characteristics of atomic and ion flows are
known.
s
ia
ii
st Sjj
j
V
jC ργγ
−
−
=
−
=
)1()1(
, (2)
Where γ is the ion reflection coefficient; S is the
integral sputtering ratio; ij is the ion current density,
aj is the flux density of deposited atoms, sρ is the
near-surface atomic density of synthesized film
material.
In the general case the film growth rate is a function
of time and can be derived from the balance between the
flow of deposited atoms aj and sputtered near-surface
atoms:
sia SjjV ρ/))1(( −⋅+= , (3)
Fig. 3 shows the dependance of nitrogen
concentration in the substrate and deposited chrome
film on time during the implantation of ions of 15 and
30 keV at room temperature, when the diffusion
mobility of implanted dopant is low [2].
a
b
Fig. 3. Distribution of nitrogen in the depth of growing
Cr film under N2
+ bombardment. The ion flux –
1014 ion/cm2·s, the film growth rate – 8 nm/min;
a – E = 15 keV and b – E = 30 keV. Different curves
correspond to the different thickness of the deposited
film (- - – 15 nm; · · · – 30 nm; ·-·-· – 60 nm;
··-··- – 75 nm; -- – 100 nm; … – 150 nm) [2]
At the beginning of the deposition an abrupt increase
in nitrogen concentration in the substrate is observed.
Afterwards the dopand concentration reaches a
maximum value stc , which corresponds to the steady-
state concentration in the depth of deposited film. The
distance of nitrogen ion penetration is longer in case of
the radiation with ions of 30 keV. Accordingly, the
substrate-film mixing zone is also larger.A stationary
stage of the IBAD process is also characterised by the
availability of the region on the growing film surface
whose nitrogen concentration varies from a maximum
value to zero. It implies the existance of unformed
zone. The higher the ion energy the wider this zone.
The width of mixing zone and that of underformed
zome depends not only on the energy of bombarding
ions but also on substrate and deposited film materials.
Fig. 4 shows the nitrogen distribution at the stationary
stage of the IBAD process for the cases of chrome-on-
chrome and aluminium-on-aluminium deposition [2]. It
is seen that the penetration depth of nitrogen ions into
the aluminium substrate exceeds that for the chrome
substrate (a mixing zone is larger). At the same time the
width of the underformed zone of chrome coating is
smaller in comparison with that for alunimium coating.
Fig. 4. Sample thickness change of nitrogen
concentration during deposition of aluminum and
chrome onto substrates made of the same material at
simultaneous bombardment with nitrogen ions of 30 keV
during 1800 s, j =1014 ion/сm2/s [2]
To study the processes of a change in chemical
composition of the near-surface region during the ion-
assisted deposition taking into consideration diffusion
processes the following diffusion equation can be used:
)()( xgC
x
VC
x
D
xt
C
+
∂
∂
−
∂
∂
∂
∂
=
∂
∂
, (4)
where ),( txCC = is the nitrogen concentration, D is
the diffusion coefficient, )(xg is the concentration of
nitrogen imbedded per time unit. The x coordinate is
normal to the sample surface. The addend in the left
side of equation is defined by the choice of coordinate
system, which moves together with the solid body
surface.
Fig. 5 shows the sample depth change of the
concentration of implanted nitrogen as the diffusion
coefficient is increased. Different curves correspond to
different nitrogen diffusion coefficients.
128 ISSN 1562-6016. ВАНТ. 2014. №2(90)
Fig. 5. Sample thickness change in nitrogen
concentration during the aluminum deposition onto the
substrates made of the same metal at simultaneous
bombardment with nitrogen ions of 30keV during 3600 s
1 – 0.01 nm2/s; 2 – 1.0 nm2/s; 3 – 10.0 nm2/s
Figure shows that the mixing zone thickness is
increased with an increase in diffusion mobility. The
nitrogen concentration at the growing film front is
increased due to the migration of implanted nitrogen
from the maximum position of occurrence to the film
surface. It can also be seen that at high temperatures of
the IBAD-process (D-10) the nitrogen concentration in
the film depth fails to reach a stationary value during the
estimated time (3600 s) of film deposition.
To check the compliance of the results of computer
simulation with experimental data using the secondary
ion spectroscopy we investigated nitrogen distribution
in the Cr-N-coating on the Al-substrate (Fig. 6). Zero
coordinate corresponded to the aluminum substrate
surface.
Fig. 6. Data on a change in relative nitrogen
concentration in the aluminum substrate and Cr-N film
obtained using the SIMP method (marker-drawn), a
dashed curve shows computer simulation data. The left
ordinate axis is related to the design data. The ion
current density is 25 μА/cm2, the deposition rate is
0.1 nm/s, and the temperature is 300 оС
Figure shows that nitrogen concentration in a film
reached constant stationary value, because the film
thickness exceeded the thickness of the transition zone.
Our attention is focused on an abrupt increase in
nitrogen concentration at the film-substrate boundary
and the concentration curve bent for aluminum at a
depth of 25 nm. This Figure also gives computation
data shown by the dashed line. Computation results fit
well experimental data and reproduce special features of
a nitrogen concentration curve. At the same time the
mismatch of the design and experimental data is
observed near the film surface. A higher nitrogen
content revealed on the surface confirms the results that
were published earlier on the investigation of the phase
composition of Cr-N composite at the initial stage of its
formation in the ion irradiation environment [3]. The
electron microscopy showed that chrome nitrides CrN
and Cr2N are formed at process temperatures exceeding
250 оС. The estimated nitrogen content in the film
should not exceed 25%. Experimental investigations
that were carried out testify that an increased value of
nitrogen concentration at the growing film front can be
related to the uptake of nitrogen from a residual
atmosphere and formation of deposited metal nitrides
within the chamber volume.
2. PECULIARITIES OF THE FILM
STRUCTURE FORMATION AT THE
INITIAL STAGE OF THE IBAD PROCESS
The results of computer simulation of a coating
deposition process in the gas ion bombardment
environment that are given in the next chapter show that
the concentration of implanted ions and the amount of
defects created by them change at different process
stages. Therefore the conditions at which the coating
structure is nucleated and formed will be different. This
becomes especially topical for the deposition of
coatings using the ion beam-assisted technology
because the control over coating deposition processes at
the initial stage defines in the long run the formation of
the substrate-coating transition zone structure and a
coating adhesion.
The previous papers that delved into the studies of
the initial stage of coating formation [4, 5] studied
mainly the influence produced by the bombardment
with inert gas ions on the nucleation of a coating
structure. It has been shown that the ion bombardment
results in the promotion of the coalescence of grain
nuclei and formation of coatings with an explicit
texture.
While creating nitride coatings nitrogen ions
should inevitably be used as bombarding particles
since their presence must influence not only the
structure of condensates but also their phase
composition. The analysis of curves in Figs. 3 and 4
showed that the component composition and structure
of films can continuously be changed until the
thickness of 60 to 80 nm is reached. This happens
due to the implantation of nitrogen ions and an
increase in the amount of radiation defects created by
them.
While studying the initial stages of the structure
formation, for example, nitride coatings exposed to the
ion bombardment attention should be paid to the
nitrogen affinity to a definite material, i.e. to a value of
Gibbs free energy of the given nitrides. The papers
[6, 7] showed that the amount of nitrogen that can be
adsorbed by the metal surface depends on the value of
Gibbs free energy of appropriate nitrides.
In particular Fig. 7,a gives theoretical relationships
of N/Me ratio taken from the paper [7] for the series of
nitrides exposed to the bombardment with argon ions in
ISSN 1562-6016. ВАНТ. 2014. №2(90) 129
nitrogen environment as a function of their Gibbs
energy. Fig. 7,b gives data taken from the paper [8],
which show that using the same parameters for the
irradiation of titanium whose nitride has low Gibbs
energy with nitrogen ions its content in the material
cardinally depends on nitrogen pressure.
The irradiation up to a maximum tested dose of
1017 ion/cm2 at nitrogen pressure of 1·10-4 Pa results
in 90% nitrogen saturation and the pressure of
1·10-3 Pa provides 100 percent saturation and
irradiation dose-independent saturation occurs at
2·1016 ion/сm2. For comparison the diagram gives
data for iron whose free energy of nitride formation is
much higher than that of titanium, in particular
8.5 kcal/mole. It is seen that a change in nitrogen
pressure by two and a half orders actually results in
no change of its content in iron.
-100 -80 -60 -40 -20 0
0,0
0,2
0,4
0,6
0,8
1,0
ZrN
HfN TiN
YN
VN0.465
Nb
2
N
TaN
NbN
VN
Cr
2
N
CrN
Mo2N Fe2N
R
at
io
, N
/M
e
Gibbs energy, kcаl/mоl
0 2 4 6 8 10
0,0
0,1
0,2
0,3
0,4
0,5
0,6
0,7
0,8
0,9
1,0
1,1
Ti, 5.10-6 Pа
Ti, 1.10-4 Pа
Ti, 1.10-3 Pа
Fe, 5.10-6 Pа
Fe, 1.10-3 Pа
N
/M
e
Dose, N+, ion/cm2,х1016
а b
Fig. 7. Relation between the saturation surface nitrogen-to-metal ratio and:
a – Gibbs energy of nitride formation at 298 K for various metals bombarded with 8 keV Ar+ ions at 4 µA·cm-2
in nitrogen at 10-3 Pа [7]; b – dose nitrogen ion irradiation (E=6 keV) at different nitrogen pressure [8]
We performed electron microscopy of initial
stages of the formation of vanadium and chrome-
nitride films that possess different Gibbs energy in
conditions of ion-assisted deposition [9]. Figs. 8, 9
give distribution histograms of film grains whose
effective thickness is in the range of 5 to 20 nm.
0 1 2 3 4 5 6 7 8 9 10 11
0
15
30
45
%
nm
0 1 2 3 4 5 6 7 8 9 10 11
0
15
30
45
%
nm
0 1 2 3 4 5 6 7 8 9 10 11
0
10
20
%
nm
0 1 2 3 4 5 6 7 8 9 10 11
0
10
20
30
%
nm
5 nm 10 nm 15 nm 20 nm
Fig. 8. Histograms of size distribution of grains in four CrN films [9]
0 5 10 15 20 25 30 35 40 45 50
0
5
10
15
20
25
30
35
%
nm
0 5 10 15 20 25 30 35 40 45 50
0
5
10
15
20 %
nm
0 5 10 15 20 25 30 35 40 45 50
0
2
4
6
8
10
12
14
16
18 %
nm
0 10 20 30 40 50
0
5
10
15
20
25 %
nm
5 nm 10 nm 15 nm 20 nm
Fig. 9. Histograms of size distribution of grains in four VN films [9]
The analysis of histograms of CrN grain distribution
for different deposition time showed that the material
structure at the given stage corresponds to the grain
nuclei system whose distribution function changes with
an increase in the deposition time and irradiation dose.
The first two films show uniform-sized distribution with
sufficiently narrow peak for the size range of
≈ 2…3 nm, however starting from the third film the
origination of nuclei of ≈ 5…8 nm is observed. This
tendency is explicitly manifested in the fourth film.
It should be noted that an increase in the average
size of nuclei occurs due to the appearance of the
second peak in the region of large sizes, and not because
of peak displacement on the distribution curve. The
amount of small-size nuclei remains actually
unchanged. This is indicative of the progress of
coalescence process with simultaneous nucleation of
130 ISSN 1562-6016. ВАНТ. 2014. №2(90)
new grain population on vacant substrate sections.
Vanadium grain size distribution curves have one
maximum which shifts on the size scale from 15 to
25 nm as the film thickness is increased. Further
deposition results in no shift of the given peak toward
large sizes. In addition, an increase in the amount of
small –size grains is observed, which occurs due to their
origination on triple and quadruple grain junctions, not
in the substrate plane. Due to the fact that the new grain
population shades the space of intergranular junctions
the formation process of a solid coating turns out to be
incomplete. As a result the formed coating contains
many pores of ~ 10 nm.
The diffraction analysis of chrome films showed that
starting from the lowest thicknesses the formation of the
crystalline structure of CrN occurs. Thereat, with an
increase in the thickness of films their crystalline
orientation is changed. The sequential orientation
transition [211] → [211] + [100] → [100] is observed.
A change in the structure of V films differs from that of
Cr films. At low thicknesses a film consists of fully
disoriented grains whose diffraction reflections form an
annular electron-diffraction pattern. As the coating
deposition time increases the texture formation in the
direction (001) occurs. The film structure corresponds to
the fcc phase of vanadium nitride VN1-х. The attention is
arrested by the fact that the vanadium nitride grain
nuclei density does not exceed the value of 1.2·1011 cm-2,
while for chrome nitride the nuclei density varied in the
range of 6·1011…2·1012 cm-2.
Thus, we can state that in conditions of the
irradiation with nitrogen ions during the chrome
deposition a fine-crystalline dense structure is formed.
The vanadium deposition in the same conditions results
in the formation of a larger-grain messy structure. And
finally, in spite of the fact that the estimated value of
N+/Cr,V ratio does not exceed 0.08 at the initial stage of
coating formation (for thicknesses of 20 nm) the nitride
phase is formed in both cases. The differences in
formation processes of CrN1-х and VN1-х coatings can be
explained within the framework of nitride formation
thermodynamics. Fig. 7,a shows that for vanadium
nitride the Gibbs energy is considerably lower in
comparison with that of chrome nitride. Hence, nitrogen
will react with vanadium more actively during the
formation of nitride coatings by the ion-assisted
deposition.
The deposition of vanadium and chrome occurs in
conditions of continuous adsorption of nitrogen
molecules by the substrate surface. The nitrogen
dissociation energy is rather high and it reaches
205.8 kcal/mole, and therefore nitrogen fails to
dissociate on the substrate at 200 °С. Its dissociation
seems to be more feasible in ion-assisted process
conditions. This mechanism can take place if specificity
of the statement of IBAD experiments is taken into
consideration. For this technology a vacuum space right
before the substrate is in the effective area of
bombarding ions. At such a configuration the
probability of the dissociation of molecular nitrogen in
the chamber volume is rather high. This may result in
the formation of chemical compounds both in the
chamber and on the substrate surface. It means that this
method of coating deposition allows for the formation
of compounds at the initial stage in two ways, in
particular on the substrate due to the surface diffusion of
metal and nitrogen atoms and due to the formation of
nitride molecules in space, their deposition and
diffusion.
A criterion of applicability of either mechanism for
ion-assisted technology can be a degree of nitrogen
affinity to metal. The fact that nitrogen reacts easier
with vanadium in comparison with chrome allows us to
assume that major portion of stable VN molecules is
formed at the earliest stage of the process, i.e. during
spatial interaction of dissociated vanadium and nitrogen
molecules. On the contrary the formation of chrome
nitride mainly occurs after the deposition of metal onto
the substrate surface.
In the paper [9] we substantiated that vanadium
nitride molecules have a longer lifetime while
depositing on the substrate surface and display higher
diffusion mobility in comparison with individual
chrome and nitrogen atoms. Therefore, while forming a
coating by combining clusters into stable nuclei, the
distribution density of those nuclei should be lower than
the density of structures formed due to the atom
merging. In the case of chrome nitride the nuclei density
is defined by the diffusion mobility both of chrome
atoms and nitrogen atoms and by the time of their
existence on the substrate. Each of these parameters will
be lower than those for VN clusters that were formed
prior to their appearance on the substrate. Due to this
fact the chrome nitride structure should be more fine-
grained than that of vanadium nitride as the experiment
showed.
3. STRUCTURE AND PHASE
CHARACTERISTICS OF “THICK” FILMS
AND COATINGS
It was mentioned above that the reactive gas used for
the IBAD technology enters a formed coating by two
channels, in particular in the form of accelerated ions
and adsorbed molecules. In spite of low pressure of a
working gas in the vacuum chamber and taking into
account relatively low deposition rates used for this
method that range from -0.1 to 1.0 nm/s the amount of
gas absorbed during the deposition can considerably
exceed the number of deposited metal atoms. Therefore,
the phase composition and coating structure depend
directly on the amount and final state of gas present in
the metal lattice, to be more exact to what extent
specific material reacts with gas being used.
Use of the IBAD technology allowed for more
detailed analysis of a Cr-N compound. In particular,
Ensinger et al. [10] showed that coatings with different
phase composition (Fig. 10) can be obtained by varying
evaporation rate and ion current density. In order to
form a stoichiometric CrN compound it is necessary to
use low deposition rate of 0.1 to 0.3 nm/s and high ion
current densities. However, all X-ray pictures show the
reflection from the chrome lattice even at high densities.
In contrast to chrome transient metals of the fourth
group, such as Ti, Hf, Zr have high affinity to reactive
gases, therefore in conditions of ion-assisted deposition
ISSN 1562-6016. ВАНТ. 2014. №2(90) 131
it is possible to obtain nitrides that contain no metal
component (Fig. 10,b) [11].
As it was mentioned above the ion bombardment
during metal deposition contributes to an increase in the
concentration of grain nucleation places and diffusion
mobility both of individual atoms and Me-(N,C,O)
compounds. This results in a change of the formation
mechanism of grain nuclei. The grains become equiaxed
and the content of gas impurities is decreased. The
diffusion mobility of atoms is defined not so much by
the substrate temperature as by ion current density. The
nucleating structure is characterized by high grain
density, small size (in nanorange) and narrow peak in
the grain size distribution.
20 40 60 80 100 120 140 160 180 200
0,0
0,1
0,2
0,3
0,4
0,5
0,6
0,7
0,8
0,9
1,0
0
CrN
Cr2N,CrN
Cr,Cr2N
Cr
E
va
po
ra
tio
n
ra
te
, n
m
/s
Ion beam density, μA/cm2
(Cr)
(Cr)
0,0 0,5 1,0 1,5 2,0
0
100
200
300
400
500
600
700
800
900
1000
1100
1200
α
α+ε+δ
ε+δ
Io
n
cu
rr
en
t d
en
si
ty
, m
A
/c
m
2
Evaporation rate, nm/s
0
δ
I/A-ratio
α-Ti
ε-Ti2N
δ-TiN
a b
Fig. 10. Regions of existence of different phases in the deposition rate/ion irradiation intensity diagram.
a – Cr-N [10], b – Ti-N [11]. Ion energy – 30 keV
To stabilize the nanocrystalline structure and to
improve consequently tribological characteristics the
IBAD process is complemented with the evaporation or
sputtering of the second metal, i.e. the three-component
compounds are created [12]. A simultaneous deposition
of two components requires the creation of appropriate
conditions for the formation of nanocrystalline solid
nitride phase surrounded by the second phase. In order
to provide phase separation were selected metals that
form no triple alloy Me1Me2N in their equilibrium state
[13, 14]. The creation of nanocomposite structure is
controlled by the process temperature and gas ion
density. Nitrogen ions provide the formation of a solid
nitride phase on the basis of one metal and a
temperature provides diffusion of the second metal to
the boundaries of nitride grains [14]. This configuration
allows for the creation of composite structures with
different phase ratio by varying metal percentage,
substrate temperature, and energy density imparted by
the ion beam. As a rule, such materials demonstrate the
highest hardness and acceptable tribological
characteristics when the size of their grains approaches
5 to 10 nm [12-14]. In such cases the intergranular
space is filled very often with amorphous or crystalline
boundary region.
0 5 10 15 20 25
0
2
4
6
8
10
12
14
16
18
G
ra
in
si
ze
, (
nm
)
Ni (at.%)
400oC
RT
0 5 10 15 20 25
0
1
2
3
A
m
or
ph
ou
s p
ha
se
th
ic
kn
es
s,
nm
Ni (at.%)
400oC
RT
a b
Fig. 11. a – the grain size as a function of Ni content in the Ti-Ni-N coating. b – normalized average intergranular
distance between TiN grains as a function of Ni content [14]
Fig. 11,a gives the relationships of grain sizes of the
Ti-Ni-N film as a function of Ni content [14]. It is seen
that in the absence of nickel the grain size is higher for
the deposition at 400 °С. This means that the governing
factor is the mobility of titanium and titanium nitride
atoms. The addition of nickel results in its segregation at
the nuclei boundaries of TiN grains and the blocking of
their growth. As a result the grain size is decreased. The
132 ISSN 1562-6016. ВАНТ. 2014. №2(90)
radiation-assisted nickel diffusion and not temperature
becomes the basic factor that defines the grain size. As
the nickel content is increased actually the same
increase in thickness of amorphous nickel layer between
the grains occurs at room temperature and 400 °С (see
Fig. 11,b).
4. TRIBOLOGICAL CHARACTERISTICS
It is believed that coatings with high tribological
characteristics should meet three basic requirements, in
particular the portion, which is contiguous with the
article, should possess a good article adhesion and the
external portion of a coating should sustain loadings to
which the article is exposed during the operation and an
interim region must damp these loadings. In the classic
case to solve this problem it is necessary to apply a
three-layer coating in which each layer fulfills the
required function. Naturally, the main parameter that
defines the quality of transition zones between the
layers will be a temperature of a coating deposition
process. In the IBAD technology the function of
temperature is fulfilled by the flow density of gas ions
and their energies.
For example, W. Ensinger et al. [15] analyzed the
quality of TiN coatings applied onto AlSI 52100 and
aluminum alloy AlCuMg2 using the IBAD method. It
has been shown that structural and tribological
characteristics of a coating are mainly defined by the
ion beam energy and density. For the range of mean and
high energies of 10 to 20 keV the coatings that were
obtained using the IBAD method demonstrate higher
tribological characteristics, in particular adhesion, wear-
resistance and hardness in comparison with those that
were deposited using traditional PVD methods.
4.1. MICROHARDNESS
It is known that the hardness of polycrystalline
structures is defined by their microstructure. In order to
have an increased hardness the structure should be able
to suppress the formation and motion of dislocations
and microcracks. This problem can be solved in many
ways, in particular grain crushing, cold deformation,
alloying and so on. However, these methods are not
applicable to the case of nanocrystalline objects since
the alloying ions leave the grain volume and segregate
on its boundaries and the dislocations are not formed at
all. Therefore, the microhardness of films obtained in
ion bombardment conditions is defined by process
parameters and a possibility to alloy the grain
boundaries of a single-phase material by the second
phase.
The papers [16-19] studied the influence produced
by the ion energy and ion current density on
microhardness of Cr-N coatings (Fig. 12). Lower values
of microhardness were obtained in the paper [17] that
used high densities of ion streams of 100 to
120 μA/cm2; as a result the coating structure was a
mixture of Cr + Cr2N. The transition to lower intensities
of ion current [18] results in the formation of CrN phase
and an increase in microhardness. The increase was
insignificant, possibly due to the large size of a coating
grain, i.e. 200 nm. The papers [16, 19] used higher
energies that defined an increase in microhardness up to
18…30 GPa. The highest increase was demonstrated by
coatings with the smallest grain size of 5 to 8 nm [16].
0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 32
8
10
12
14
16
18
20
22
24
26
28
30
N
an
oh
ar
dn
es
s,
G
Pa
Ion energy, keV
Fig. 12. Dependences of microhardness of CrN coatings
on the energy of bombardment ions.
● – [16]; ▲ – [17]; ▼ – [19]; ■ – [18]
The data given above with regard to the influence
produced by experimental parameters of the IBAD-
process on microhardness of a Cr-N coating show that
not only the phase composition influences this value but
also the grain size. It was noted time and again that the
Hall-Patch formula cannot be applied to nanocrystalline
structures with the size grain of < 10 to 20 nm (for
example 20, 21) and the microhardness value can
exceed the estimated value by a factor of 4 to 5. Today
many models are available that could explain the
observed effect. It is known, for example, that
availability of a large amount of low-angle boundaries
in a fine-grained structure creates conditions for the
appearance of a stressed state in films [22]. As a rule,
metal films deposited without ion stimulation
experience tensile internal stresses that crave for the
compensation of porosity that occurs at grain
boundaries. The deposition of chrome in the ion-
bombardment conditions cardinally changes the
situation. As a rule an increase in the amount of energy
introduced by the ion beam results in the change of the
stress sign replacing tensile stresses by compressive
ones [23-25].
0 1 2 3 4
0
10
20
30
40
Cohesion
Adhesion
C
ri
tic
al
lo
ad
in
g,
N
Ratio N/Cr
Fig. 13. Dependence of a critical load of CrN coating
separation on N/Cr ratio value [26]
Fig. 13 shows the relationships of stress values in
Cr-N coatings as a function of N/Cr ratio [26]. Such a
trend of curves correlates with an increase in the CrN
phase and decrease in the grain size revealed in the
ISSN 1562-6016. ВАНТ. 2014. №2(90) 133
same work. That is, an increase in microhardness of
CrN films with a decrease in the grain size is explained
by an increase in compressive stresses. The grain value
is just a parameter convenient for the comparison of
different data [27].
4.2. ADHESION
The adhesion characteristics of coatings applied
using ion bombardment technologies are defined by
many factors, in particular careful preparation of the
substrate surface, substrate-coating mixing zone depth,
the formation efficiency of chemical compounds in the
transition zone and also by the absence of both
increased stresses and segregation of gas mixtures in
this zone. The ion bombardment during the deposition
ambiguously affects each factor mentioned above.
The papers [26, 28] studied the influence of the ion
energy on the adhesion value of the Cr-N coating. The
authors did not manage to establish direct interrelation
between the energy of nitrogen ions and the adhesion
value [28]. On the contrary, the increase in energy from
20 to 40 keV resulted in a decreased adhesion.
For additional improvement of adhesion
characteristics of coatings we used the method of
stimulation of mutual substrate-coating mixing through
the preliminary implantation of nitrogen ions into the
substrate with energy of 30 keV to reach doses at which
the substrate surface layer is saturated with nitrogen up
to the concentration of Me/N = 1. The process
temperature is not high and reaches 200 °С. Then the
irradiation is continued and the metal is deposited using
the electron -beam evaporation technique, i.e. a duplex
IBAD process [29]. The coating thickness is 130 nm.
Fig. 14 gives Cr and Nb distribution curves depending
on the depth for the case of ordinary IBAD process (a)
and for the case of duplex treatment, i.e. implantation
+IBAD process (b).
0 50 100 150 200
Nb
50
40
30
20
10
0
Nb
Cr
I,
ar
b.
u
n.
Depth, nm
a b
Fig. 14. Cr and Nb distribution in a coating-substrate combination for the ordinary
IBAD process (a) and for the duplex process, implantation 3.5·1017 cm-2 + IBAD (b) [29]
It is seen that in spite of relatively low temperature
of the experiment, the high flaw level peculiar for the
IBAD technology contributes to the intensive progress
of diffusion processes and formation of rather broad
mixing zone. A preliminary ion bombardment
stimulates this process even more.
4.3. FRICTION COEFFICIENT AND WEAR
Comprehensive study of the friction coefficient and
wear-resistance of CrN and TiN coatigs applied onto
AlSI H13 steel was done in the paper [30]. It has been
shown that the friction coefficient of CrN coatings
applied on corundum at a relative humidity (RH) of 50
and 85% was about 0.3, slightly higher than that of TiN
coatings. At RH < 10% , it is a little bit higher but still
has a low value before complete wear of CrN coatings,
whereas TiN coatings exhibit the high coefficient of
friction of about 0.8. In addition, a volumetric loss of
CrN coatings during their friction is smaller in
comparison with that of TiN coatings, especially at low
RH.
The influence of Cr/N ratio and the energy of
nitrogen ions on the wear of CrN coating applied onto
AISI 52100 steel were studied in the paper [16]. It has
been shown that the fraction of Cr2N phase is increased
in the coating with an increase in Cr/N ratio and the
wear is also cardinally increased (Fig. 15). A three-fold
increase in the ion energy produces actually no impact
on the wear-resistance.
0
5
10
W
ea
r
am
ou
nt
(m
m
2 )
Cr/N arrival ratio Acceleration voltage
1/2 1/1 2/1 10 kV 30 kV
Fig. 15. Wear of Cr-N coating after 200 test cycles as a
function of Cr/N arrival ratio and ion energy [16]
0 50 100 150 200
SubstrateCoating
50
40
30
20
10
0
Nb
Cr
I,
ar
b.
u
n.
Depth, nm
Nb
134 ISSN 1562-6016. ВАНТ. 2014. №2(90)
Studying the influence produced by the basic
parameters of the IBAD process (the ion energy and
beam current density) on tribological characteristics of
CrN coating showed that the friction coefficient slightly
depends on both parameters [18]. The wear-resistance is
significantly increased in coated steel. The range of
currents’ densities embracing 8 to 32 µА/cm2 and
energies of 4 to 12 keV has been studied. The most
optimal are energy values of 12 keV and minimal values
of current density are 8 µА/cm2.
0 200 400 600 800 1000
0
10
20
30
N
an
oh
ar
dn
es
s (
G
Pa
)
Bombarding energy (eV)
a
0 200 400 600 800
0.0
0.2
0.4
0.6
0.8
1.0
1.2
1.4
1x10-8
1x10-7
1x10-6
1x10-5
1x10-4
1x10-3
Fr
ic
tio
n
co
ef
fic
ie
nt
Bombarding energy (eV)
5N load
W
ea
r
ra
te
(m
m
3 /N
m
)
b
Fig. 16. Nanohardness (a), friction coefficient and wear
(b) of TiBN synthesized at different bombardment
energy [31]
The deposition of a three-component TiBN coating
in conditions of low-energy radiation [31] showed that
the change in the ion energy in the range of 0 to 800 eV
cardinally changes hardness, friction coefficient and
wear-resistance (Fig. 16). It is seen that the most
acceptable values are reached at different energy values:
a maximum hardness is reached at 400 eV and a
minimum wear and friction coefficients are observed at
150 eV. The structure of TiBN composite consists of
nanocrystals TiB2 and TiN surrounded by a soft h-BN
phase. At such a configuration the best tribological
characteristics are obtained at optimum mixing of
nanograins in the soft phase. An increase in hardness
with an energy increase can be explained by that the rise
in the ion energy up to 400 eV and higher results in the
preferred sputtering of lighter coating components B
and N. As a result the share of a harder component of
TiN is increased and this contributes to an increase in
hardness of TiN coatings at high energies. At lower
energies a softer h-BN phase defines tribological
properties to a large extent.
CONCLUSIONS
The research done in the field of nanostructured
material science over the last few years showed that
materials with ultrafine grain have great prospects for
the heavy-duty operation. The production of such
materials is impossible using equilibrium technologies,
Therefore the interest in nanocrystalline materials
stimulated the development of technologies based on
nonequilibrium processes. In particular ion assisted
deposition technologies are widely used for the
formation of thin-film structures. High operating
performances of the obtained coatings are defined by
that the ion bombardment in combination with the
deposition of atomic-&- molecular flows give an
opportunity to design their structure on the atomic level.
The intensive irradiation with heavy charged particles in
combination with the deposition of overheated metal
vapors onto the “cold” substrate creates conditions for
the formation of structures with the grain size less than
10 nm. By varying such parameters as ion current
density, ion energy, nitrogen/boron/carbon/oxygen
content and metal component concentration we can
create structures whose tribological characteristics can
vary in wide ranges.
An additional advantage of the ion beam-assisted
technology is that it can be used for the deposition of
protective coatings onto the material with low melting
temperature. Also is very important that the evaporation
of metals with different affinity to active gases allows
for the purposeful design of multicomponent structures
that include both metal nanocrystalline grains and
amorphous/ crystalline nitride (boride and carbide)
phases.
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Статья поступила в редакцию 29.01.2014 г.
136 ISSN 1562-6016. ВАНТ. 2014. №2(90)
ИОННО-СТИМУЛИРОВАННАЯ ТЕХНОЛОГИЯ – МЕТОД СОЗДАНИЯ
НАНОКРИСТАЛЛИЧЕСКИХ ПОКРЫТИЙ
Обзор
А.Г. Гугля, И.Г. Марченко
Дается описание структуры, фазового состава и механических характеристик нанокристаллических
покрытий, полученных с использованием технологии ионно-стимулированного осаждения (IBAD method).
Приводятся результаты компьютерного моделирования IBAD процесса для различных энергий
бомбардирующих ионов и различных соотношений между скоростью осаждения покрытий и плотностью
ионных потоков. Представлены данные электронно-микроскопических исследований начальной стадии
формирования нанокристаллических структур (толщиной 5 нм и больше). И наконец, продемонстрированы
влияние энергии ионов и плотности ионных потоков на формирование нанокристаллических структур и их
корреляция с трибологическими свойствами покрытий.
ІОННО-СТИМУЛЬОВАНА ТЕХНОЛОГІЯ – МЕТОД СТВОРЕННЯ
НАНОКРИСТАЛІЧНИХ ПОКРИТТІВ
Огляд
О.Г. Гугля, І.Г. Марченко
Приводиться опис структури, фазового складу та механічних характеристик нанокристалічних покриттів,
які здобуваються з використанням технології іонно-стимульованого осадження (IBAD method).
Приводяться результати комп’ютерного моделювання IBAD процесу для різних енергій бомбардуючих іонів
та різних співвідношень між швидкостями осадження покриттів та щільністю іонних потоків. Представлені
також дані електронно-мікроскопічних досліджень початкової стадії формування нанокристалічних
структур (товщиною 5 нм и вище). В останньому розділі продемонстровано вплив енергії іонів та щільності
іонних потоків на формування нанокристалічних структур та їх кореляція з трибологічними властивостями
покриттів.
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