Formation of Nanostructured Relief of TiN—Fe Heterostructures in Hybrid Helicon-Arc Plasma Reactor
The features of the physical mechanisms of controlled ion-plasma formation of the new functional nanomaterials are investigated. The technological regimes of formation of functional nanostructured materials under combined impact of several plasma sources are investigated; the structural and electric...
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Інститут металофізики ім. Г.В. Курдюмова НАН України
2015
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| Cite this: | Formation of Nanostructured Relief of TiN—Fe Heterostructures in Hybrid Helicon-Arc Plasma Reactor / E. M. Rudenko, I. V. Korotash, D. Y. Polotskiy, L. S. Osipov, M. V. Dyakin, T. A. Prikhna, A. P. Shapovalov // Металлофизика и новейшие технологии. — 2015. — Т. 37, № 4. — С. 499-508. — Бібліогр.: 8 назв. — рос. |
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irk-123456789-1118932017-01-16T03:03:17Z Formation of Nanostructured Relief of TiN—Fe Heterostructures in Hybrid Helicon-Arc Plasma Reactor Rudenko, E.M. Korotash, I.V. Polotskiy, D.Y. Osipov, L.S. Dyakin, M.V. Prikhna, T.A. Shapovalov, A.P. Металлические поверхности и плёнки The features of the physical mechanisms of controlled ion-plasma formation of the new functional nanomaterials are investigated. The technological regimes of formation of functional nanostructured materials under combined impact of several plasma sources are investigated; the structural and electrical properties of the obtained TiN films are studied. The structures of films are studied with scanning tunnelling microscope JSPM-4500/4610 interlocked with an atomic force microscope. As shown, the optimized helicon-arc reactor demonstrates the unique properties and provides controlled low-temperature formation of the dense regular TiN nanostructures with the sizes from a few to tens of nanometres. Вивчено особливості фізичних механізмів керованого йонно-плазмового формування нових функціональних наноматеріялів. Відпрацьовано технологічні режими формування функціональних наноструктурованих матеріялів за спільної роботи кількох джерел плазми; вивчено структурні та електрофізичні особливості одержаних плівок TiN. Структури плівок досліджено на сканівному тунельному мікроскопі JSPM-4500/4610, зблокованому з атомним силовим мікроскопом. Встановлено, що оптимізований гелікон-дуговий реактор демонструє унікальні властивості і забезпечує кероване низькотемпературне формування щільних упорядкованих наноструктур TiN з розмірами від одиниць до десятків нанометрів. Изучены особенности физических механизмов управляемого ионно-плазменного формирования новых функциональных наноматериалов. Отработаны технологические режимы формирования функциональных наноструктурированных материалов при совместной работе нескольких источников плазмы; изучены структурные и электрофизические особенности полученных плёнок TiN. Структуры плёнок исследованы на сканирующем туннельном микроскопе JSPM-4500/4610, сблокированном с атомным силовым микроскопом. Установлено, что оптимизированный геликонно-дуговой реактор демонстрирует уникальные свойства и обеспечивает управляемое низкотемпературное формирование плотных упорядоченных наноструктур TiN с размерами от единиц до десятков нанометров. 2015 Article Formation of Nanostructured Relief of TiN—Fe Heterostructures in Hybrid Helicon-Arc Plasma Reactor / E. M. Rudenko, I. V. Korotash, D. Y. Polotskiy, L. S. Osipov, M. V. Dyakin, T. A. Prikhna, A. P. Shapovalov // Металлофизика и новейшие технологии. — 2015. — Т. 37, № 4. — С. 499-508. — Бібліогр.: 8 назв. — рос. 1024-1809 PACS: 52.50.Dg, 52.50.Qt, 61.46.Bc, 68.35.Ct, 68.35.Dv, 81.16.Rf, 82.33.Xj http://dspace.nbuv.gov.ua/handle/123456789/111893 en Металлофизика и новейшие технологии Інститут металофізики ім. Г.В. Курдюмова НАН України |
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English |
| topic |
Металлические поверхности и плёнки Металлические поверхности и плёнки |
| spellingShingle |
Металлические поверхности и плёнки Металлические поверхности и плёнки Rudenko, E.M. Korotash, I.V. Polotskiy, D.Y. Osipov, L.S. Dyakin, M.V. Prikhna, T.A. Shapovalov, A.P. Formation of Nanostructured Relief of TiN—Fe Heterostructures in Hybrid Helicon-Arc Plasma Reactor Металлофизика и новейшие технологии |
| description |
The features of the physical mechanisms of controlled ion-plasma formation of the new functional nanomaterials are investigated. The technological regimes of formation of functional nanostructured materials under combined impact of several plasma sources are investigated; the structural and electrical properties of the obtained TiN films are studied. The structures of films are studied with scanning tunnelling microscope JSPM-4500/4610 interlocked with an atomic force microscope. As shown, the optimized helicon-arc reactor demonstrates the unique properties and provides controlled low-temperature formation of the dense regular TiN nanostructures with the sizes from a few to tens of nanometres. |
| format |
Article |
| author |
Rudenko, E.M. Korotash, I.V. Polotskiy, D.Y. Osipov, L.S. Dyakin, M.V. Prikhna, T.A. Shapovalov, A.P. |
| author_facet |
Rudenko, E.M. Korotash, I.V. Polotskiy, D.Y. Osipov, L.S. Dyakin, M.V. Prikhna, T.A. Shapovalov, A.P. |
| author_sort |
Rudenko, E.M. |
| title |
Formation of Nanostructured Relief of TiN—Fe Heterostructures in Hybrid Helicon-Arc Plasma Reactor |
| title_short |
Formation of Nanostructured Relief of TiN—Fe Heterostructures in Hybrid Helicon-Arc Plasma Reactor |
| title_full |
Formation of Nanostructured Relief of TiN—Fe Heterostructures in Hybrid Helicon-Arc Plasma Reactor |
| title_fullStr |
Formation of Nanostructured Relief of TiN—Fe Heterostructures in Hybrid Helicon-Arc Plasma Reactor |
| title_full_unstemmed |
Formation of Nanostructured Relief of TiN—Fe Heterostructures in Hybrid Helicon-Arc Plasma Reactor |
| title_sort |
formation of nanostructured relief of tin—fe heterostructures in hybrid helicon-arc plasma reactor |
| publisher |
Інститут металофізики ім. Г.В. Курдюмова НАН України |
| publishDate |
2015 |
| topic_facet |
Металлические поверхности и плёнки |
| url |
http://dspace.nbuv.gov.ua/handle/123456789/111893 |
| citation_txt |
Formation of Nanostructured Relief of TiN—Fe Heterostructures in Hybrid Helicon-Arc Plasma Reactor / E. M. Rudenko, I. V. Korotash, D. Y. Polotskiy, L. S. Osipov, M. V. Dyakin, T. A. Prikhna, A. P. Shapovalov // Металлофизика и новейшие технологии. — 2015. — Т. 37, № 4. — С. 499-508. — Бібліогр.: 8 назв. — рос. |
| series |
Металлофизика и новейшие технологии |
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| fulltext |
499
PACS numbers:52.50.Dg, 52.50.Qt,61.46.Bc,68.35.Ct,68.35.Dv,81.16.Rf, 82.33.Xj
Formation of Nanostructured Relief of TiN—Fe Heterostructures
in Hybrid Helicon-Arc Plasma Reactor
E. M. Rudenko, I. V. Korotash, D. Y. Polotskiy, L. S. Osipov,
M. V. Dyakin, T. A. Prikhna*, and A. P. Shapovalov*
G. V. Kurdyumov Institute for Metal Physics, N.A.S. of Ukraine,
36 Academician Vernadsky Blvd.,
UA-03680 Kyiv, Ukraine
*V. Bakul Institute for Superhard Materials, N.A.S. of Ukraine,
2 Avtozavodska Str.,
04074 Kyiv, Ukraine
The features of the physical mechanisms of controlled ion-plasma formation
of the new functional nanomaterials are investigated. The technological re-
gimes of formation of functional nanostructured materials under combined
impact of several plasma sources are investigated; the structural and electri-
cal properties of the obtained TiN films are studied. The structures of films
are studied with scanning tunnelling microscope JSPM-4500/4610 inter-
locked with an atomic force microscope. As shown, the optimized helicon-arc
reactor demonstrates the unique properties and provides controlled low-
temperature formation of the dense regular TiN nanostructures with the siz-
es from a few to tens of nanometres.
Вивчено особливості фізичних механізмів керованого йонно-плазмового
формування нових функціональних наноматеріялів. Відпрацьовано тех-
нологічні режими формування функціональних наноструктурованих ма-
теріялів за спільної роботи кількох джерел плазми; вивчено структурні та
електрофізичні особливості одержаних плівок TiN. Структури плівок до-
сліджено на сканівному тунельному мікроскопі JSPM-4500/4610, збло-
кованому з атомним силовим мікроскопом. Встановлено, що оптимізова-
ний гелікон-дуговий реактор демонструє унікальні властивості і забезпе-
чує кероване низькотемпературне формування щільних упорядкованих
наноструктур TiN з розмірами від одиниць до десятків нанометрів.
Изучены особенности физических механизмов управляемого ионно-
плазменного формирования новых функциональных наноматериалов.
Отработаны технологические режимы формирования функциональных
наноструктурированных материалов при совместной работе нескольких
источников плазмы; изучены структурные и электрофизические особен-
Металлофиз. новейшие технол. / Metallofiz. Noveishie Tekhnol.
2015, т. 37, № 4, сс. 499—508
Оттиски доступны непосредственно от издателя
Фотокопирование разрешено только
в соответствии с лицензией
2015 ИМФ (Институт металлофизики
им. Г. В. Курдюмова НАН Украины)
Напечатано в Украине.
500 E. M. RUDENKO, I. V. KOROTASH, D. Y. POLOTSKIY et al.
ности полученных плёнок TiN. Структуры плёнок исследованы на скани-
рующем туннельном микроскопе JSPM-4500/4610, сблокированном с
атомным силовым микроскопом. Установлено, что оптимизированный
геликонно-дуговой реактор демонстрирует уникальные свойства и обес-
печивает управляемое низкотемпературное формирование плотных упо-
рядоченных наноструктур TiN с размерами от единиц до десятков нано-
метров.
Key words: TiN films, plasma, nanostructures, helicon-arc reactor.
(Received December 19, 2014)
1. INTRODUCTION
Nanoscale materials have unique physical, chemical, and biological
properties that are significantly different from those at macro- and
microscale. This allows us to develop new applications, for example, to
create specific materials, devices, and functional systems.
Recently carbon nanotubes (CNTs) became of great interest. Pro-
spects for application of CNTs and other carbon-based nanostructures
in micro- and nanoelectronics are caused by peculiarities of their elec-
tronic properties as systems with reduced dimensionality, e.g., CNT is
quasi-one-dimensional (quasi-1D) structure. The long-term implemen-
tation of the ballistic electron-transport regime in such systems could
lead to ultralow levels of an electrical resistance. That is why CNTs
could be one of the fundamental building blocks for nanoelectronics
[1, 2].
It should be noted that for the date an activated plasma-enhanced
chemical vapour deposition (PECVD) is the only deterministic CNT
growth technology, which allows us to control a position, size, shape,
and structure of CNTs at a certain extent and synthesize CNTs at lower
temperatures [3—5]. Main technological operations in PECVD process
to provide high-quality CNT synthesis are: 1) deposition of diffusion
barrier sublayer; 2) formation of nanostructured films of metal cata-
lyst; 3) synthesis of CNTs. Ni, Fe, Co, and their combinations are
commonly used as catalysts [6]. However, if Si single-crystal is used as
a substrate, then deposition of a passivation (protective) layer, for ex-
ample, TiN, is necessary in order to prevent chemical interaction be-
tween Si substrate and a catalyst layer. In addition, a nanostructured
relief must be formed at a catalytic layer, which provides creation of
CNT with a regular structure for the needs of electronics. The possibil-
ity to create CNTs with a regular structure at nanostructured relief is
demonstrated in investigations of CNT synthesis on the catalytic Fe
layer formed on the single-crystal Si substrate [7].
The object of these investigations is a study of formation of
nanostructured relief in TiN—Fe heterostructure at n-Si(100) sub-
FORMATION OF NANOSTRUCTURED RELIEF OF TiN—Fe HETEROSTRUCTURES 501
strate. The solution of this problem can be helpful for creation of tech-
nological bases for the usage of CNTs for the needs of electronics.
2. EXPERIMENTAL
The new hybrid ion-plasma reactor based on helicon and magneto-
activated vacuum-arc (MAVA) sources (created in Institute for Metal
Physics, N.A.S.U.) is used to develop the physical foundations of the
new technology of synthesis of nanostructured materials [8]. The tech-
nological chamber (see Fig. 1) consists of the discharge chamber of the
helicon source (with the diameter and the length of 20 cm) and the drift
chamber (with the diameter of 35 cm and the length of 25 cm) docked to
it. The discharge in argon, in reactive gases (O2, and C2Cl2H4, SiH4 in
gaseous states) under a pressure of 7—8 mTorr is excited by the planar
antenna with the diameter of 11 cm, which is plugged in by the inter-
face unit to the RF (radio frequency) generator with the frequency of
13.56 MHz and the power of 1 kW. The magnetic system of the helicon
plasma source consisted of two parts. The solenoid, which covers the
discharge chamber and provides the discharge excitation and plasma
generation in the right mode. The control magnetic system with the
independent power supply allows us to adjust the magnetic field in the
drift chamber with no significant change in its discharge chamber.
Two modules of MAVA sources are docked to the drift chamber that
allowed us to deposit film heterostructures with different chemical
Fig. 1. The technology chamber with the helicon and plasma-arc sources.
502 E. M. RUDENKO, I. V. KOROTASH, D. Y. POLOTSKIY et al.
composition. Figure 1 shows the right MAVA reactor (the second
MAVA reactor is located symmetrically leftward). The substrate hold-
er is placed at the bottom of the drift chamber, where the electric po-
tential in the range of 0—200 V is applied.
The reactor in the single vacuum cycle could carry out the following
technological operations: 1) sample surface treatment by plasma of
helicon sources at different potentials applied to the substrate in dif-
ferent working gaseous environments; 2) film deposition with using
MAVA sources at different potentials applied to the substrate. For
these investigations, the experimental samples of TiN-films on silicon
substrates were obtained by the following technological scheme. The
first stage consisted of clearing and activating the surface of the sili-
con substrate by the helicon source plasma (with RF power of 300 W) in
the argon atmosphere under the pressure of 2 Pa for 15—20 minutes
until the electrode current in the substrate holder will not fall to
2.3 mA. The second stage consisted of forming the TiN film layer by
the cyclic procedure (10 cycles in total) at two different stages: 1) TiN
film deposition by MAVA source with the titanium oxide cathode in
the nitrogen atmosphere (under the pressure of 0.6 Pa and the arc cur-
rent of 40 A) during 20 seconds; 2) treatment by helicon plasma source
(with RF power of 300 W) in argon atmosphere under pressure of 1 Pa
during 40 seconds. The potential at the substrate holder was a variable
parameter. In addition to the above mentioned technological stages in
formation of TiN-film layer, Fe-film deposition by MAVA source with
the iron cathode in the argon atmosphere was carried out at the final
stage for 30 seconds (under the pressure of 0.6 Pa and the arc current
of 45 A) to generate TiN—Fe heterostructures on Si substrates.
3. RESULTS AND DISCUSSION
The effect of technological conditions (related to formation of Si—TiN-
film structures on Si substrates obtained in a hybrid helicon-arc reac-
tor) on the surface morphology of the films is investigated by atomic
force microscopy (AFM). The structural studies were targeted to opti-
mize the formation regimes of nanostructured topography of the
films. The results of the studies of a surface topography for the film
structures obtained by various technological parameters are shown in
Fig. 2—4: the surface topography of the film structures is shown at dif-
ferent magnifications in Fig. 2—4 (a and b), and the numerical calcula-
tions of the data are shown in Fig. 2—4 (c and d). In Figures 2—4, the
surface roughness values Rpv and Rms are given under the figures of the
surface topography (Fig. 2—4, a and b). The latter parameter (Rms) de-
scribes the standard deviation of height values for the surface relief.
The essential feature of the formation regime of these film structures
is the cyclic impact of the argon ion flow generated in the helicon plas-
FORMATION OF NANOSTRUCTURED RELIEF OF TiN—Fe HETEROSTRUCTURES 503
ma source of hybrid helicon-arc reactor. As known, the condensate
formation on the substrate surface causes simultaneous adsorption,
diffusion, desorption, and energy relaxation of surface atoms, and
formation of atomic and chemical bonds. However, all these processes
will be affected significantly by the density and the average ion energy
of plasma flow along with the substrate temperature and flow density.
As one can see from Fig. 2, for the average ion energy in the flow
about 90 eV, the dense nanostructured film structure is formed with
the average crystallite size of 5—20 nm and the surface roughness pa-
rameters Rpv 48 Å and Rms 4.3 Å. Under these technological condi-
tions, the formation process of a nanostructured surface relief in films
probably occurs with a predominance of desorption over adsorption of
atoms. The energy relaxation of surface ions goes to the level of the
equilibrium temperature of a condensate against the background of
intense surface energy disturbance and therefore this energy relaxa-
tion has negligible influence on formation of atomic and chemical
bonds.
a b
c d
Fig. 2. Surface topography of Si—TiN-film structures obtained under cyclic
exposures of ion beams with the energy of 90 eV on the film surface.
504 E. M. RUDENKO, I. V. KOROTASH, D. Y. POLOTSKIY et al.
For the low ion energy (10 eV), the more developed nanoscale film
structure (Fig. 2) forms with the average crystallite size of 20—40 nm.
The corresponding surface roughness values are equal to Rpv 138 Å
and Rms 13.5 Å. Formation of nanostructured relief of film’s surface
under these technological conditions takes place with the predomi-
nance of adsorption over desorption of atoms. The energy relaxation of
surface ions goes to the nearly equilibrium conditions. Such quasi-
equilibrium conditions favour the structure flattening followed by ap-
proach to its uniform distribution over the surface.
For the low ion energy (200 eV) (Fig. 4), which is significantly
higher than the self-sputtering threshold, the islet film structures
with the average crystallite size of 100 nm form against the back-
ground of the nanosize structures. The corresponding surface rough-
ness values are equal to Rpv 550 Å and Rms 50.5 Å. Formation of
nanostructured relief of film’s surface under these technological con-
ditions takes place with substantial predominance of desorption of at-
oms. A far more non-equilibrium energy distribution appears in the
condensate, and the ion energy is sufficient for destruction of existing
a b
c d
Fig. 3. Surface topography of Si—TiN-film structures obtained under cyclic
exposures of ion beams with the energy of 10 eV on the film surface.
FORMATION OF NANOSTRUCTURED RELIEF OF TiN—Fe HETEROSTRUCTURES 505
atomic and chemical bonds with scattering of condensate atoms. Scat-
tering of substrate atoms is also possible.
The results of investigations obtained by scanning tunnelling mi-
croscopy (STM) are consistent with those obtained by AFM. STM mi-
crographs (Fig. 5) show that nanostructure of iron films (Fig. 5, b) ad-
equately reflects the morphology of the transition layer of titanium
nitride (Fig. 5, a). The three-dimensional image of the resulting struc-
ture of the catalytic iron layer intended for further synthesis of CNTs
is shown in Fig. 6.
Structure analysis of the films formed for the different ion energies
shows the presence of the monotonous relationship between the size of
nanoclusters (ranging from 5 to 100 nm) and the ion energy (from 10—
20 to 90—100 eV).
Thus, the controlled formation of nanostructured relief in the range
of 10—100 nm is shown to be possible and dependent on the technologi-
cal conditions of formation of TiN—Fe-film heterostructures. The as-
sisted cyclical effect of plasma fusion reactor creates such non-
equilibrium condensation of atoms adsorbed on the surface that facili-
a b
c d
Fig. 4. Surface topography of Si—TiN-film structures obtained under cyclic
exposures of ion beams with the energy of 200 eV on the film surface.
506 E. M. RUDENKO, I. V. KOROTASH, D. Y. POLOTSKIY et al.
tates creation of the regular surface structure of nanoclusters.
The formation of nanostructured relief of films is based on competi-
tive adsorption and desorption of atoms, and formation and destruc-
tion of existing atomic and chemical bonds with the energy relaxation
a b
Fig. 5. Nanostructured films on (001)Si: (a) TiN and (b) Fe/TiN for the sub-
strate holder potential of 90 V.
Fig. 6. Three-dimensional STM images of the resulting structures of the cata-
lytic iron layer.
FORMATION OF NANOSTRUCTURED RELIEF OF TiN—Fe HETEROSTRUCTURES 507
of surface ions to the equilibrium condensate temperature. Then, the
energy change of plasma flow significantly affects mechanisms of the
nanoscale surface relief of the produced film structures. However, it
should be noted that investigations of the combined effect of other fac-
tors (e.g., a substrate temperature, an ion flow density and a material
flow density) on formation of the nanoscale surface relief on film
structures are necessary for the choice of the more optimal technologi-
cal parameters. AFM data indicate the possibility of controlled for-
mation of the nanoscale surface relief on the obtained film structures.
4. CONCLUSIONS
Structure analysis of the films formed for the different ion energies
elucidates the presence of the monotonous relationship between the
nanocluster sizes (in the range of 5 to 100 nm) and the ion-flow energy
(in the range from 10—20 to 90—100 eV). The controlled formation of
the nanostructured relief with the roughness in the range of 10—
100 nm is shown to be possible and dependent on the technological con-
ditions of formation of TiN—Fe-film heterostructures. The assisted cy-
clical effect of the plasma fusion reactor creates such nonequilibrium
condensation of atoms adsorbed on the surface that facilitates creation
of the regular surface structure of nanoclusters. The formation of
nanostructured relief of films is based on competitive adsorption and
desorption of atoms, and formation and destruction of existing atomic
and chemical bonds with the energy relaxation of surface ions to the
equilibrium condensate temperature. Then, the energy change of
plasma flow significantly affects the mechanisms of the nanoscale sur-
face relief of the obtained film structures. However, it should be noted
that investigations of the combined effect of other factors (the sub-
strate temperature and the material flow density) on formation of the
nanoscale surface relief on the film structures are necessary for the
choice of the more optimal technological parameters.
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/NLD (Gebruik deze instellingen om Adobe PDF-documenten te maken die zijn geoptimaliseerd voor prepress-afdrukken van hoge kwaliteit. De gemaakte PDF-documenten kunnen worden geopend met Acrobat en Adobe Reader 5.0 en hoger.)
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/ENU (Use these settings to create Adobe PDF documents best suited for high-quality prepress printing. Created PDF documents can be opened with Acrobat and Adobe Reader 5.0 and later.)
>>
/Namespace [
(Adobe)
(Common)
(1.0)
]
/OtherNamespaces [
<<
/AsReaderSpreads false
/CropImagesToFrames true
/ErrorControl /WarnAndContinue
/FlattenerIgnoreSpreadOverrides false
/IncludeGuidesGrids false
/IncludeNonPrinting false
/IncludeSlug false
/Namespace [
(Adobe)
(InDesign)
(4.0)
]
/OmitPlacedBitmaps false
/OmitPlacedEPS false
/OmitPlacedPDF false
/SimulateOverprint /Legacy
>>
<<
/AddBleedMarks false
/AddColorBars false
/AddCropMarks false
/AddPageInfo false
/AddRegMarks false
/ConvertColors /ConvertToCMYK
/DestinationProfileName ()
/DestinationProfileSelector /DocumentCMYK
/Downsample16BitImages true
/FlattenerPreset <<
/PresetSelector /MediumResolution
>>
/FormElements false
/GenerateStructure false
/IncludeBookmarks false
/IncludeHyperlinks false
/IncludeInteractive false
/IncludeLayers false
/IncludeProfiles false
/MultimediaHandling /UseObjectSettings
/Namespace [
(Adobe)
(CreativeSuite)
(2.0)
]
/PDFXOutputIntentProfileSelector /DocumentCMYK
/PreserveEditing true
/UntaggedCMYKHandling /LeaveUntagged
/UntaggedRGBHandling /UseDocumentProfile
/UseDocumentBleed false
>>
]
>> setdistillerparams
<<
/HWResolution [2400 2400]
/PageSize [612.000 792.000]
>> setpagedevice
|