Annealing Effect on the Microstructure and Mechanical Properties of a Thin Titanium Nitride Film
Titanium nitride (TiN) films were deposited by the D.C. magnetron sputtering process on a SUS 304 steel substrate. The effect of postdeposition annealing on the microstructure and mechanical properties of thin TiN films was studied in detail using atomic force microscopy, a potentiostat and na...
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| Date: | 2014 |
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| Format: | Article |
| Language: | English |
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Інститут проблем міцності ім. Г.С. Писаренко НАН України
2014
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| Online Access: | https://nasplib.isofts.kiev.ua/handle/123456789/112717 |
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| Journal Title: | Digital Library of Periodicals of National Academy of Sciences of Ukraine |
| Cite this: | Annealing Effect on the Microstructure and Mechanical Properties of a Thin Titanium Nitride Film / S.C. Her, C.L. Wu // Проблемы прочности. — 2014. — № 2. — С. 66-72. — Бібліогр.: 21 назв. — англ. |
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Digital Library of Periodicals of National Academy of Sciences of Ukraine| _version_ | 1859638067063685120 |
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| author | Her, S.C. Wu, C.L. |
| author_facet | Her, S.C. Wu, C.L. |
| citation_txt | Annealing Effect on the Microstructure and Mechanical Properties of a Thin Titanium Nitride Film / S.C. Her, C.L. Wu // Проблемы прочности. — 2014. — № 2. — С. 66-72. — Бібліогр.: 21 назв. — англ. |
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| container_title | Проблемы прочности |
| description | Titanium nitride (TiN) films were deposited by
the D.C. magnetron sputtering process on a SUS
304 steel substrate. The effect of postdeposition
annealing on the microstructure and mechanical
properties of thin TiN films was studied in detail
using atomic force microscopy, a potentiostat
and nano-indentation tests. The TiN films were
annealed at temperatures ranging from 100 to
300C. Surface roughnesses of TiN films estimated
by atomic force microscopy decreased
from 3.83 to 2.43 nm as the annealing temperatures
increased from 100 to 300°C. The
corrosion rates of the films measured by a
potentionstat in a 0.5-molar H₂SO₄ solution decreased
from 8.57•10⁻² to 4.59•10⁻² mmPY as
the annealing temperatures increased from 100
to 300°C. An increase in corrosion resistance
was attributed to an increase in hardness and a
modulus of the film with the annealing temperature.
Atomic force microscopy images of the film
revealed fine-grained morphology for TiN films
annealed at higher temperature. Experimental results
show that the mechanical properties of TiN
films could be significantly improved by annealing.
The control of the annealing process was
proved to be critical for the improvement of TiN
film properties.
Методом магнетронного напыления при постоянном токе на стальную подложку SUS 304
наносили нитрид-титановые пленки. Детально исследовано влияние отжига после нанесения
пленок на микроструктуру и их механические свойства с помощью метода атомно-силовой
микроскопии, стабилизатора напряжения и наноиндентирования. Нитрид-титановые пленки
обжигали при температуре 100…300С. Шероховатость их поверхности, исследуемая методом атомно-силовой микроскопии, уменьшилась с 3,83 до 2,43 нм при повышении температуры отжига в интервале 100…300°С. Скорость коррозии пленок, измеренная с помощью
стабилизатора напряжений в 0,5%-ном молярном растворе H₂SO₄, снизилась с 8,57•10⁻² до 4,59•10⁻² мм, тогда как температура отжига повысилась с 100 до 300°С. Рост коррозионной стойкости зависит от увеличения твердости и модуля упругости пленки с температурой отжига. Исследование пленки посредством метода атомно-силовой микроскопии
показало, что нитрид титана, который обжигался при более высокой температуре, имеет
мелкозернистую структуру. Установлено, что механические свойства нитрид-титановых
пленок можно значительно улучшить путем отжига. Получил подтверждение тот факт,
что контроль процесса отжига крайне необходим для усовершенствования свойств нитридтитановых пленок.
Методом магнетронного напилення під дією постійного струму на стальну підкладку
SUS 304 наносили нітрид-титанові плівки. Детально досліджено вплив відпалу після
нанесення плівок на мікроструктуру та їх механічні властивості за допомогою методу
атомно-силової мікроскопії, стабілізатора напруги і наноіндентування. Нітрид-титанові плівки випалювали за температури 100...300C. Шорсткість їхньої поверхні, що
досліджувалася методом атомно-силової мікроскопії, зменшилася з 3,83 до 2,43 нм із
підвищенням температури відпалу в інтервалі 100...300°С. Швидкість корозії плівок,
яку вимірювали за допомогою стабілізатора напруги в 0,5%-ному молярному розчині
H₂SO₄, зменшилася з 8,57•10⁻² до 4,59 •0⁻² мм, у той час як температура відпалу підвищилась із 100 до 300°C. Зростання корозійної стійкості залежить від збільшення твердості і модуля пружності плівки з температурою відпалу. Дослідження
плівки за допомогою методу атомно-силової мікроскопії показало, що нітрид титану,
який випалювався за більш високої температури, має дрібнозеренну структуру. Установлено, що механічні властивості нітрид-титанових плівок можна значно покращити шляхом відпалу. Отримав підтвердження той факт, що контроль процесу
відпалу необхідний для удосконалення властивостей нітрид-титанових плівок.
|
| first_indexed | 2025-12-07T13:18:21Z |
| format | Article |
| fulltext |
UDC 539.4
Annealing Effect on the Microstructure and Mechanical Properties of a Thin
Titanium Nitride Film
S. C. Her
1
and C. L. Wu
Department of Mechanical Engineering, Yuan Ze University, Chung-Li, Taiwan
1 mesch@saturn.yzu.edu.tw
ÓÄÊ 539.4
Âëèÿíèå îòæèãà íà ìèêðîñòðóêòóðó è ìåõàíè÷åñêèå ñâîéñòâà òîíêîé
íèòðèä-òèòàíîâîé ïëåíêè
Ø. ×. Õåð
1
, ×. Ë. Âó
Ôàêóëüòåò ìàøèíîñòðîåíèÿ, Óíèâåðñèòåò Þàíü Çå, ×óíã-Ëè, Òàéâàíü
Ìåòîäîì ìàãíåòðîííîãî íàïûëåíèÿ ïðè ïîñòîÿííîì òîêå íà ñòàëüíóþ ïîäëîæêó SUS 304
íàíîñèëè íèòðèä-òèòàíîâûå ïëåíêè. Äåòàëüíî èññëåäîâàíî âëèÿíèå îòæèãà ïîñëå íàíåñåíèÿ
ïëåíîê íà ìèêðîñòðóêòóðó è èõ ìåõàíè÷åñêèå ñâîéñòâà ñ ïîìîùüþ ìåòîäà àòîìíî-ñèëîâîé
ìèêðîñêîïèè, ñòàáèëèçàòîðà íàïðÿæåíèÿ è íàíîèíäåíòèðîâàíèÿ. Íèòðèä-òèòàíîâûå ïëåíêè
îáæèãàëè ïðè òåìïåðàòóðå 100…300�Ñ. Øåðîõîâàòîñòü èõ ïîâåðõíîñòè, èññëåäóåìàÿ ìåòî-
äîì àòîìíî-ñèëîâîé ìèêðîñêîïèè, óìåíüøèëàñü ñ 3,83 äî 2,43 íì ïðè ïîâûøåíèè òåìïåðà-
òóðû îòæèãà â èíòåðâàëå 100…300�Ñ. Ñêîðîñòü êîððîçèè ïëåíîê, èçìåðåííàÿ ñ ïîìîùüþ
ñòàáèëèçàòîðà íàïðÿæåíèé â 0,5%-íîì ìîëÿðíîì ðàñòâîðå Í2SO4, ñíèçèëàñü ñ 8,57 10 2� � äî
4,59 10 2� � ìì, òîãäà êàê òåìïåðàòóðà îòæèãà ïîâûñèëàñü ñ 100 äî 300�Ñ. Ðîñò êîððî-
çèîííîé ñòîéêîñòè çàâèñèò îò óâåëè÷åíèÿ òâåðäîñòè è ìîäóëÿ óïðóãîñòè ïëåíêè ñ òåìïå-
ðàòóðîé îòæèãà. Èññëåäîâàíèå ïëåíêè ïîñðåäñòâîì ìåòîäà àòîìíî-ñèëîâîé ìèêðîñêîïèè
ïîêàçàëî, ÷òî íèòðèä òèòàíà, êîòîðûé îáæèãàëñÿ ïðè áîëåå âûñîêîé òåìïåðàòóðå, èìååò
ìåëêîçåðíèñòóþ ñòðóêòóðó. Óñòàíîâëåíî, ÷òî ìåõàíè÷åñêèå ñâîéñòâà íèòðèä-òèòàíîâûõ
ïëåíîê ìîæíî çíà÷èòåëüíî óëó÷øèòü ïóòåì îòæèãà. Ïîëó÷èë ïîäòâåðæäåíèå òîò ôàêò,
÷òî êîíòðîëü ïðîöåññà îòæèãà êðàéíå íåîáõîäèì äëÿ óñîâåðøåíñòâîâàíèÿ ñâîéñòâ íèòðèä-
òèòàíîâûõ ïëåíîê.
Êëþ÷åâûå ñëîâà: ìàãíåòðîííîå íàïûëåíèå, íèòðèä-òèòàíîâûå ïëåíêè, îòæèã, íàíî-
èíäåíòèðîâàíèå.
Introduction. In recent years, titanium nitride (TiN) films have been widely used for
many industrial applications, e.g., for improvement of corrosion resistance and wear
protection of cutting tools [1] and machine components [2], because TiN possesses high
hardness, thermal stability, low friction coefficient, corrosion and erosion resistance [3].
TiN with sufficient biocompatibility is also considered as an important biomaterial [4–7].
Hadad et al. [8] reported that the addition of up to 30% of titanium nitride to silicon nitride
matrix led to an improvement of wear resistance of migration of metal atoms from the
interconnects into adjacent dielectric [9]. TiN is one of the most widely used diffusion
barrier materials [10]. TiN films grown by physical vapor deposition (PVD) on a substrate,
will inevitably have residual stress after the process is complete. The residual stress is also
a significant factor on influencing preferred orientation, adhesion, and hardness of the film
[11]. An excessive stress can lead to cracking of the film in the case of tensile stress and to
buckling in the case of compressive stress. Machunze and Janssen [12] deposited TiN films
© S. C. HER, C. L. WU, 2014
66 ISSN 0556-171X. Ïðîáëåìû ïðî÷íîñòè, 2014, ¹ 2
on silicon substrate using unbalanced magnetron sputter. They found that the average film
stress is highly compressive in thin films and less compressive in thicker ones. Lee et al.
[13] investigated the effect of TiN coating on electrochemical behavior of Ti alloys. The
wear resistance of TiN is often attributed to the high hardness as well as to good chemical
stability. The achievement of high hardness and high toughness ought to be linked to the
large number of internal interfaces, which act as sites of energy dissipation and crack
deflection. Carvalho and De Hosson [14] described the results of an investigation to
determine the relationship between microstructure, deformation mechanisms, and mechanical
properties of TiN/(Ti,Al)N multilayers subjected to nanoindentation. Wittling et al. [15]
investigated the influence of coating thickness and substrate type on the hardness and
deformation of TiN films on high-speed steel, silicon and sapphire substrates through
nanoindentation with a Berkovich indenter. Sun and co-workers [16, 17] used the finite
element analysis to investigate the plastic behavior of various TiN coating/substrate
systems for a range of different substrates with different properties. Ma et al. [18] studied
the deformation mechanisms of a range of TiN coatings with different thicknesses
deposited on the V820 steel substrate. The performance of tribological coatings depends
greatly on the adhesion strength between the coatings and substrates. Liu et al. [19]
investigated the influence of the ion implantation energy of nitrogen on the adhesion and
surface properties of TiN deposited on aluminum substrate.
Magnetron sputtering provides a wide variation of the deposition parameters which
affect the microstructure and morphology of the films and, consequently, their properties.
In this work, TiN thin films were deposited by D.C. magnetron sputtering process on the
SUS 304 steel substrate. The effects of annealing temperature on the morphology and
mechanical properties of the TiN films were investigated. The microstructure and surface
roughness of the TiN films were examined using atomic force microscopy. The elastic
modulus and hardness are the key parameters in the study of wear and adhesion of thin
films to the substrates and their responses to the mechanical loads. Since the mechanical
properties of the nanomaterials may be significantly different from those of bulk materials,
there is a need to study the mechanical properties of the thin film at the nanoscale. Various
techniques have been developed for evaluating the mechanical properties of thin films.
Among them, nano-indentation [20, 21] has become the most widely adopted technique in
the study of the mechanical properties, such as hardness and elastic modulus, on small scale
or near surfaces. In this study, nanoindentation tests were employed to determine hardness
and the elastic moduli of TiN films with different annealing temperatures. The effects of
annealing temperature on the corrosion behavior were investigated using the electrochemical
method.
Film Preparation. A series of TiN films were prepared by D.C. magnetron sputtering
system (ULVAC MB06-4703) on the SUS 304 steel substrate. The target was a titanium
disk (2 inch diameter) with a purity of 99.995%. The distance between the target and
substrate was approximately 15 cm. The target was sputtered in high-purity argon
(99.999%) and nitrogen (99.999%) plasma. Prior to deposition, the substrates were cleaned
in soap solution, submerged into acetone and ethanol solutions and in an ultrasound bath
for 10 min after rinsing with distilled water. Then the substrates were dried in an oven at
the temperature of 50�C for 30 min before the application of deposition. The chamber was
equipped with a rotary vane pump and a turbo pump. After the pumping period of two
hours, the chamber was evacuated down to a base pressure of 8 10 4� � Pa. Before the
application of deposition, the Ti target and substrate were sputter-cleaned to remove the
oxide and contaminant. TiN films were deposited at the operation pressure of about
6 10 1� � Pa with the duration of 80 min for all the prepared samples. The as-prepared films
were post-annealed at different temperatures in air to investigate the effect of annealing
temperature on the microstructure and mechanical properties. The annealing was performed
at temperatures of 100, 200, and 300�C for 80 min. Then, the samples were allowed to cool
Annealing Effect on Microstructure and Mechanical Properties ...
ISSN 0556-171X. Ïðîáëåìû ïðî÷íîñòè, 2014, ¹ 2 67
down to the room temperature in their environment. The thicknesses of TiN films were
measured by the surface profiler (KLA Tencor P16). To obtain the film thickness, a small
tape was placed at the substrate prior to deposition to get a step on the sample surface. The
step height was measured in different points on the sample surface, and the film thickness
was taken as the average of these values. The thicknesses of TiN films annealed at different
temperatures of 100, 200, and 300�C, are 195, 181, and 174 nm, respectively. One can see
that the film thickness decreases with the increase of annealing temperature.
Microstructure and Surface Topography. The microstructure and surface topography
of TiN films were examined using atomic force microscopy (Seiko Instruments Inc. SPA
400). The AFM was operated in the tapping mode. The AFM images depicted in Fig. 1
show that the films annealed at high temperature of 200 and 300�C have relatively smooth
surface and compact structure. The surface roughness decreased with the increase of the
annealing temperature as shown in Table 1. More energy was supplied to the molecules at
higher temperatures resulting in the higher migration mobility, which in turn favored the
formulation of a smoother and denser film. This observation was in agreement with the
surface roughness and film thickness listed in Table 1.
Nanoindentation Test. The mechanical properties (hardness and elastic modulus) of
TiN films were characterized using nanoindentation techniques. Oliver and Phar [20, 21]
developed the most comprehensive method for determining the hardness and modulus from
load–indention curve. The results were analyzed according to the equation
S aE E Ar r� �2
2�
�
, (1)
S. C. Her and C. L. Wu
68 ISSN 0556-171X. Ïðîáëåìû ïðî÷íîñòè, 2014, ¹ 2
T a b l e 1
Surface Roughness and Thickness of TiN Film with Various Annealing Temperatures
Annealing temperature (�C) 100 200 300
Surface roughness RMS (nm) 3.83 2.94 2.43
Film thickness (nm) 195 181 174
Fig. 1. AFM images of TiN films with annealing temperature 100�C.
where a is the contact radius and A is the projected contact area, whereas � is used to
account for the geometric shape of different indenters. For a Berkovich indenter �� 1 034. .
Here S is the contact stiffness corresponding to the slope of the load–indention curve at
the beginning of the unloading. Er is the reduced modulus expressed in terms of the
elastic modulus E and Poisson’s ratio � of the indenter and the indented material as
follows:
1 1 12 2
E E Er
s
s
i
i
�
�
�� �
, (2)
where subscripts i and s represent the indenter and substrate, respectively. For a diamond
Berkovich indenter Ei � 1140 GPa and � i � 0 07. .
The hardness was determined using the equation
H
P
Ac
�
max
, (3)
where Ac is the area of the indentation at the maximum applied load Pmax . By knowing
precisely the geometry of the indenter, Ac can be expressed in terms of the indentation
depth h directly determined from measurements.
In this study, the nanoindentation tests were performed using the Mico Material Co.
Nano Test. Indentation was made using a Berkovich indenter calibrated with a standard
silica specimen. A typical load–displacement curve consists of three segments: loading to a
peak load, holding at the peak and unloading back to the zero load. A holding period of at
least 5 s was applied to allow the time-dependent effects to diminish. TiN films annealed at
different temperatures were examined by nanoindentation. Figure 2 represents the load–
displacement curves of TiN films annealed at 100�C. There are three curves in the figure
corresponding to three different indentation depths. By using the continuous stiffness
measurement mode, nanoindenter allows the hardness and modulus to be determined as a
function of indentation depth.
The hardness and elastic modulus of TiN films with different annealing temperatures
(versus normalized indentation depth) are presented in Figs. 3 and 4, respectively. It can be
ISSN 0556-171X. Ïðîáëåìû ïðî÷íîñòè, 2014, ¹ 2 69
Annealing Effect on Microstructure and Mechanical Properties ...
Fig. 2. Load versus displacement of TiN film with annealing temperature 100�C.
observed that both the hardness and elastic modulus increase with the increase of annealing
temperature. This increase is attributed largely to the effects of fine-grained morphology of
the film annealed at higher temperature. The measured hardness and elastic modulus values
were found to depend on the indentation depth. As shown in Figs. 3 and 4, both hardness
and elastic modulus drop with the increase of indentation depth.
Corrosion Test. The corrosion behavior of TiN films was investigated using a
potentostat (Solartron 1285 potentostat) in 0.5 molar H2SO4 solution at room temperature.
Electrochemical measurements were carried out with conventional three-electrode
configuration consistent with a platinum counter electrode, a saturated calomel reference
electrode and a working electrode. The corrosion potential
corr was swept from the
initial potential of �1V to the final potential of 1V with a sweep rate of 10 mV/s for all
specimens. The corrosion current density J corr can be obtained from the polarization
curves using the Tafel extrapolation. The corrosion potential, corrosion current density and
corrosion rate of TiN films with various annealing temperatures are listed in Table 2. The
corrosion rate of TiN film measured by a potentionstat in 0.5 molar H2SO4 solution
decreased from 8 57 10 2. � � to 4 59 10 2. � � mmPY as the annealing temperature increasing
from 100 to 300�C. The increase in the corrosion resistance is attributed to the increase of
hardness and modulus of the film with higher annealing temperature.
Conclusions. The microstructure and mechanical properties of TiN films annealed at
different temperatures were investigated in this paper. Experimental results show that
annealing temperature plays an important role in modifying the morphology and mechanical
properties of TiN films. More energy was supplied to the molecules at higher temperatures
70 ISSN 0556-171X. Ïðîáëåìû ïðî÷íîñòè, 2014, ¹ 2
S. C. Her and C. L. Wu
Fig. 3. Hardness versus indentation depth for TiN films with various annealing temperatures.
Fig. 4. Elastic modulus versus indentation depth for TiN films for various annealing temperatures.
Fig. 3 Fig. 4
T a b l e 2
Corrosion Potential, Corrosion Current Density, and Corrosion Rate of TiN Film
with Various Annealing Temperatures
Annealing
temperature (�C)
Corrosion
potential (V)
Corrosion current
density (A/cm2)
Corrosion rate
(mmPY)
100 517 10 1. � � 8 27 10 6. � � 8 57 10 2. � �
200 4 44 10 1. � � 710 10 6. � � 7 34 10 2. � �
300 4 63 10 1. � � 4 42 10 6. � � 4 59 10 2. � �
resulting in the higher migration mobility and nucleation density, which in turn favored the
formulation of a smoother and denser film. Consequently, surface roughness and film
thickness decreased with the increase of annealing temperature. Enhancement in the
hardness and elastic modulus of TiN films with the increase of annealing temperature was
attributed to the fine grain morphology. The corrosion resistance of TiN films also
improved with the annealing temperature increase.
Acknowledgment. The authors gratefully acknowledge the financial support provided
by National Science Council of R.O.C. under grant No. NSC 101-2622-E-155-015-CC3 for
this work.
Ð å ç þ ì å
Ìåòîäîì ìàãíåòðîííîãî íàïèëåííÿ ï³ä 䳺þ ïîñò³éíîãî ñòðóìó íà ñòàëüíó ï³äêëàäêó
SUS 304 íàíîñèëè í³òðèä-òèòàíîâ³ ïë³âêè. Äåòàëüíî äîñë³äæåíî âïëèâ â³äïàëó ï³ñëÿ
íàíåñåííÿ ïë³âîê íà ì³êðîñòðóêòóðó òà ¿õ ìåõàí³÷í³ âëàñòèâîñò³ çà äîïîìîãîþ ìåòîäó
àòîìíî-ñèëîâî¿ ì³êðîñêîﳿ, ñòàá³ë³çàòîðà íàïðóãè ³ íàíî³íäåíòóâàííÿ. ͳòðèä-òèòà-
íîâ³ ïë³âêè âèïàëþâàëè çà òåìïåðàòóðè 100...300�C. Øîðñòê³ñòü ¿õíüî¿ ïîâåðõí³, ùî
äîñë³äæóâàëàñÿ ìåòîäîì àòîìíî-ñèëîâî¿ ì³êðîñêîﳿ, çìåíøèëàñÿ ç 3,83 äî 2,43 íì ³ç
ï³äâèùåííÿì òåìïåðàòóðè â³äïàëó â ³íòåðâàë³ 100...300�Ñ. Øâèäê³ñòü êîðî糿 ïë³âîê,
ÿêó âèì³ðþâàëè çà äîïîìîãîþ ñòàá³ë³çàòîðà íàïðóãè â 0,5%-íîìó ìîëÿðíîìó ðîç÷èí³
H2SO4, çìåíøèëàñÿ ç 8 57 10 2, � � äî 4 59 10 2, � � ìì, ó òîé ÷àñ ÿê òåìïåðàòóðà â³äïàëó
ï³äâèùèëàñü ³ç 100 äî 300�C. Çðîñòàííÿ êîðîç³éíî¿ ñò³éêîñò³ çàëåæèòü â³ä çá³ëü-
øåííÿ òâåðäîñò³ ³ ìîäóëÿ ïðóæíîñò³ ïë³âêè ç òåìïåðàòóðîþ â³äïàëó. Äîñë³äæåííÿ
ïë³âêè çà äîïîìîãîþ ìåòîäó àòîìíî-ñèëîâî¿ ì³êðîñêîﳿ ïîêàçàëî, ùî í³òðèä òèòàíó,
ÿêèé âèïàëþâàâñÿ çà á³ëüø âèñîêî¿ òåìïåðàòóðè, ìຠäð³áíîçåðåííó ñòðóêòóðó. Óñòà-
íîâëåíî, ùî ìåõàí³÷í³ âëàñòèâîñò³ í³òðèä-òèòàíîâèõ ïë³âîê ìîæíà çíà÷íî ïîêðà-
ùèòè øëÿõîì â³äïàëó. Îòðèìàâ ï³äòâåðäæåííÿ òîé ôàêò, ùî êîíòðîëü ïðîöåñó
â³äïàëó íåîáõ³äíèé äëÿ óäîñêîíàëåííÿ âëàñòèâîñòåé í³òðèä-òèòàíîâèõ ïë³âîê.
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Received 22. 11. 2013
72 ISSN 0556-171X. Ïðîáëåìû ïðî÷íîñòè, 2014, ¹ 2
S. C. Her and C. L. Wu
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| id | nasplib_isofts_kiev_ua-123456789-112717 |
| institution | Digital Library of Periodicals of National Academy of Sciences of Ukraine |
| issn | 0556-171X |
| language | English |
| last_indexed | 2025-12-07T13:18:21Z |
| publishDate | 2014 |
| publisher | Інститут проблем міцності ім. Г.С. Писаренко НАН України |
| record_format | dspace |
| spelling | Her, S.C. Wu, C.L. 2017-01-26T19:07:15Z 2017-01-26T19:07:15Z 2014 Annealing Effect on the Microstructure and Mechanical Properties of a Thin Titanium Nitride Film / S.C. Her, C.L. Wu // Проблемы прочности. — 2014. — № 2. — С. 66-72. — Бібліогр.: 21 назв. — англ. 0556-171X https://nasplib.isofts.kiev.ua/handle/123456789/112717 539.4 Titanium nitride (TiN) films were deposited by the D.C. magnetron sputtering process on a SUS 304 steel substrate. The effect of postdeposition annealing on the microstructure and mechanical properties of thin TiN films was studied in detail using atomic force microscopy, a potentiostat and nano-indentation tests. The TiN films were annealed at temperatures ranging from 100 to 300C. Surface roughnesses of TiN films estimated by atomic force microscopy decreased from 3.83 to 2.43 nm as the annealing temperatures increased from 100 to 300°C. The corrosion rates of the films measured by a potentionstat in a 0.5-molar H₂SO₄ solution decreased from 8.57•10⁻² to 4.59•10⁻² mmPY as the annealing temperatures increased from 100 to 300°C. An increase in corrosion resistance was attributed to an increase in hardness and a modulus of the film with the annealing temperature. Atomic force microscopy images of the film revealed fine-grained morphology for TiN films annealed at higher temperature. Experimental results show that the mechanical properties of TiN films could be significantly improved by annealing. The control of the annealing process was proved to be critical for the improvement of TiN film properties. Методом магнетронного напыления при постоянном токе на стальную подложку SUS 304 наносили нитрид-титановые пленки. Детально исследовано влияние отжига после нанесения пленок на микроструктуру и их механические свойства с помощью метода атомно-силовой микроскопии, стабилизатора напряжения и наноиндентирования. Нитрид-титановые пленки обжигали при температуре 100…300С. Шероховатость их поверхности, исследуемая методом атомно-силовой микроскопии, уменьшилась с 3,83 до 2,43 нм при повышении температуры отжига в интервале 100…300°С. Скорость коррозии пленок, измеренная с помощью стабилизатора напряжений в 0,5%-ном молярном растворе H₂SO₄, снизилась с 8,57•10⁻² до 4,59•10⁻² мм, тогда как температура отжига повысилась с 100 до 300°С. Рост коррозионной стойкости зависит от увеличения твердости и модуля упругости пленки с температурой отжига. Исследование пленки посредством метода атомно-силовой микроскопии показало, что нитрид титана, который обжигался при более высокой температуре, имеет мелкозернистую структуру. Установлено, что механические свойства нитрид-титановых пленок можно значительно улучшить путем отжига. Получил подтверждение тот факт, что контроль процесса отжига крайне необходим для усовершенствования свойств нитридтитановых пленок. Методом магнетронного напилення під дією постійного струму на стальну підкладку SUS 304 наносили нітрид-титанові плівки. Детально досліджено вплив відпалу після нанесення плівок на мікроструктуру та їх механічні властивості за допомогою методу атомно-силової мікроскопії, стабілізатора напруги і наноіндентування. Нітрид-титанові плівки випалювали за температури 100...300C. Шорсткість їхньої поверхні, що досліджувалася методом атомно-силової мікроскопії, зменшилася з 3,83 до 2,43 нм із підвищенням температури відпалу в інтервалі 100...300°С. Швидкість корозії плівок, яку вимірювали за допомогою стабілізатора напруги в 0,5%-ному молярному розчині H₂SO₄, зменшилася з 8,57•10⁻² до 4,59 •0⁻² мм, у той час як температура відпалу підвищилась із 100 до 300°C. Зростання корозійної стійкості залежить від збільшення твердості і модуля пружності плівки з температурою відпалу. Дослідження плівки за допомогою методу атомно-силової мікроскопії показало, що нітрид титану, який випалювався за більш високої температури, має дрібнозеренну структуру. Установлено, що механічні властивості нітрид-титанових плівок можна значно покращити шляхом відпалу. Отримав підтвердження той факт, що контроль процесу відпалу необхідний для удосконалення властивостей нітрид-титанових плівок. The authors gratefully acknowledge the financial support provided by National Science Council of R.O.C. under grant No. NSC 101-2622-E-155-015-CC3 for this work. en Інститут проблем міцності ім. Г.С. Писаренко НАН України Проблемы прочности Научно-технический раздел Annealing Effect on the Microstructure and Mechanical Properties of a Thin Titanium Nitride Film Влияние отжига на микроструктуру и механические свойства тонкой нитрид-титановой пленки Article published earlier |
| spellingShingle | Annealing Effect on the Microstructure and Mechanical Properties of a Thin Titanium Nitride Film Her, S.C. Wu, C.L. Научно-технический раздел |
| title | Annealing Effect on the Microstructure and Mechanical Properties of a Thin Titanium Nitride Film |
| title_alt | Влияние отжига на микроструктуру и механические свойства тонкой нитрид-титановой пленки |
| title_full | Annealing Effect on the Microstructure and Mechanical Properties of a Thin Titanium Nitride Film |
| title_fullStr | Annealing Effect on the Microstructure and Mechanical Properties of a Thin Titanium Nitride Film |
| title_full_unstemmed | Annealing Effect on the Microstructure and Mechanical Properties of a Thin Titanium Nitride Film |
| title_short | Annealing Effect on the Microstructure and Mechanical Properties of a Thin Titanium Nitride Film |
| title_sort | annealing effect on the microstructure and mechanical properties of a thin titanium nitride film |
| topic | Научно-технический раздел |
| topic_facet | Научно-технический раздел |
| url | https://nasplib.isofts.kiev.ua/handle/123456789/112717 |
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