Functional protective ZrN coatings on implants for trauma surgery
The nano-crystalline films of zirconium nitride have been synthesized on implants for trauma surgery made of AISI 316 L stainles steel by using vacuum-arc deposition under RF-biasing mode in “Bulat” type device. Structure examinations – X-ray diffraction analysis (XRD), X-ray fluoriscent analysis (X...
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| Опубліковано в: : | Вопросы атомной науки и техники |
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| Дата: | 2020 |
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Національний науковий центр «Харківський фізико-технічний інститут» НАН України
2020
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| Назва журналу: | Digital Library of Periodicals of National Academy of Sciences of Ukraine |
| Цитувати: | Functional protective ZrN coatings on implants for trauma surgery / V.S. Taran, I.E. Garkusha, A.V. Taran, R.M. Muratov, P.M. Vorontsov, Yu.P. Gnidenko, H.M. Herasimov, V.V. Starikov, A.A. Baturin, S.P. Romaniuk // Problems of atomic science and tecnology. — 2020. — № 6. — С. 115-118. — Бібліогр.: 13 назв. — англ. |
Репозитарії
Digital Library of Periodicals of National Academy of Sciences of Ukraine| _version_ | 1860163611967619072 |
|---|---|
| author | Taran, V.S. Garkusha, I.E. Taran, A.V. Muratov, R.M. Vorontsov, P.M. Gnidenko, Yu.P. Herasimov, H.M. Starikov, V.V. Baturin, A.A. Romaniuk, S.P. |
| author_facet | Taran, V.S. Garkusha, I.E. Taran, A.V. Muratov, R.M. Vorontsov, P.M. Gnidenko, Yu.P. Herasimov, H.M. Starikov, V.V. Baturin, A.A. Romaniuk, S.P. |
| citation_txt | Functional protective ZrN coatings on implants for trauma surgery / V.S. Taran, I.E. Garkusha, A.V. Taran, R.M. Muratov, P.M. Vorontsov, Yu.P. Gnidenko, H.M. Herasimov, V.V. Starikov, A.A. Baturin, S.P. Romaniuk // Problems of atomic science and tecnology. — 2020. — № 6. — С. 115-118. — Бібліогр.: 13 назв. — англ. |
| collection | DSpace DC |
| container_title | Вопросы атомной науки и техники |
| description | The nano-crystalline films of zirconium nitride have been synthesized on implants for trauma surgery made of AISI 316 L stainles steel by using vacuum-arc deposition under RF-biasing mode in “Bulat” type device. Structure examinations – X-ray diffraction analysis (XRD), X-ray fluoriscent analysis (XRF), scanning electron microscopy (SEM) with microanalysis (EDX), nanoidentation method – were performed to study phase and chemical composition, surface morphology, microstructure and nanohardness of ZrN coatings. The corrosion resistance of coatings has been tested in 0.9% quasiphysiological NaCl solution.
Нанокристалічні плівки нітриду цирконію були синтезовані на імплантах для травматології, які виготовлені з нержавіючої сталі AISI 316 L, за допомогою вакуумно-дугового осадження в режимі ВЧ-зміщення в установці типу «Булат». Структурні дослідження – рентгенівський дифракційний аналіз (XRD), рентгенівський флуоресцентний аналіз (XRF), скануюча електронна мікроскопія (SEM) з мікроаналізом (EDX), метод наноідентифікації – були виконані для вивчення фазового та хімічного складів, морфології поверхні, мікроструктури та нанотвердості покриттів ZrN. Корозійну стійкість покриттів було досліджено в 0,9% квазіфізіологічному розчині NaCl.
Нанокристаллические пленки нитрида циркония были синтезированы на имплантах для травматологии, изготовленных из нержавеющей стали AISI 316 L, с использованием вакуумно-дугового напыления в режиме ВЧ-смещения в установке «Булат». Структурные исследования – рентгеноструктурный анализ (XRD), рентгенофлуоресцентный анализ (XRF), сканирующая электронная микроскопия (SEM) с микроанализом (EDX), метод наноидентификации – были выполнены для изучения фазового и химического составов, морфологии поверхности, микроструктуры и нанотвердости покрытий ZrN. Коррозионная стойкость покрытий исследовалась в 0,9% квазифизиологическом растворе NaCl.
|
| first_indexed | 2025-12-07T17:55:50Z |
| format | Article |
| fulltext |
ISSN 1562-6016. ВАНТ. 2020. №6(130)
PROBLEMS OF ATOMIC SCIENCE AND TECHNOLOGY. 2020, № 6. Series: Plasma Physics (26), p. 115-118. 115
https://doi.org/10.46813/2020-130-115
FUNCTIONAL PROTECTIVE ZrN COATINGS ON IMPLANTS FOR
TRAUMA SURGERY
V.S. Taran
1
, I.E. Garkusha
1,3
, A.V. Taran,
1
R.M. Muratov
1
, P.M. Vorontsov
2
,
Yu.P. Gnidenko
3
, H.M. Herasimov
3
, V.V. Starikov
4
, A.A. Baturin
4
, S.P. Romaniuk
5
1
Institute of Plasma Physics NSC “Kharkov Institute of Physics and Technology”, Kharkiv, Ukraine;
2
Sytenko Institute of Spine and Joint Pathology, NAMS, Kharkiv, Ukraine,
3
V.N. Karazin Kharkiv National University, Kharkiv, Ukraine;
4
National Technical University “Kharkiv Polytechnic Institute”, Kharkiv, Ukraine;
5
Kharkiv Petro Vasylenko National Technical University of Agriculture, Kharkiv, Ukraine
E-mail: avtaran@ukr.net
The nano-crystalline films of zirconium nitride have been synthesized on implants for trauma surgery made of
AISI 316 L stainles steel by using vacuum-arc deposition under RF-biasing mode in “Bulat” type device. Structure
examinations – X-ray diffraction analysis (XRD), X-ray fluoriscent analysis (XRF), scanning electron microscopy
(SEM) with microanalysis (EDX), nanoidentation method – were performed to study phase and chemical
composition, surface morphology, microstructure and nanohardness of ZrN coatings. The corrosion resistance of
coatings has been tested in 0.9 % quasiphysiological NaCl solution.
PACS: 81.40.-z
INTRODUCTION
Metallic biomaterials such as Ti6Al4V alloys, 316L
stainless steel and Co-Cr alloys are being used as
artificial joints, dental abatements, orthopedic fixation,
and stents bone fixation devices [1-3]. Ti6Al4V alloy has
excellent mechanical properties, corrosion resistance and
super plasticity. However, Ti6Al4V contains aluminum
and vanadium which are toxic elements and very harmful
to human bodies. AISI 316 L stainless steel (SS) does not
have the required level of bioinerticity due to high nickel
content whereas Co in long term Co-Cr alloys has
cancerogenic effect [4-6]. Low mechanical properties and
stress corrosion have been reported for implants
fabricated from AISI 316 L [7]. All biomaterials have to
satisfy various criteria, such as strength, high corrosion
resistance, bioadhesion, biocompatibility, high wear
resistance, and low friction coefficient [8].
Non-corrosive behavior in tissue-material interface is
one of the most important criteria for bio-metallic
implants [9]. The implanted material is exposed to body
fluids, such as intercellular fluid and blood depending on
the surrounding tissue. Body fluid consists of inorganic
ions (Na
+
, Cl
-
, etc), amino acids, proteins, and organic
acids [9].
Manufacturing of implants from medical stainless
steel with additional biocompatible coatings based on
composite materials, titanium, zirconium and their
nitrides, oxides, allows to significantly reducing the
occurrence of infiltrates in the human body. Bioinertness
of structures from such elements is four times better than
that of medical stainless steel. Among these ZrN is also
considered as biocompatible coating for various implants
and coatings for surgical instruments.
Zirconium nitride (ZrN) ceramic with cubic structure
has high wear, fatigue and corrosion resistance properties
and is widely used as hard, refractory and bioinert coating
in industry and medicine. It was reported that ZrN
coating showed better corrosion resistance then TiN
coating [10, 11]. Stoichiometric ZrN has only stable
phase with a gold-like color due to its metallic band
structure.
Plasma based PVD coatings have favorable residual
stresses, higher density and better adhesion compared to
other techniques. PVD technology modifies the surface
properties of tools without changing the underlying
material properties and biomechanical functionality. One
of the drawbacks of this method is formation of
macroparticles by the ejected molten droplets from the
hot cathode spot by higher plasma pressure within the
cathode spot. The composition of these particles being
completely different from the rest of the coatings, these
particles also offer the local source of variation in
physical and mechanical properties. It was shown in our
experiments [12, 13] that the utilization of vacuum-arc
evaporation with RF discharge allows applying coatings
onto dielectrics and thermo-liable instrument at room
temperature decreasing the amount of macro-particles
emitted from plasma flow.
In the present research, the nano-crystalline films of
zirconium nitride have been synthesized on implants for
trauma surgery made of AISI 316 L stainless steel. The
corrosion resistance of coatings has been tested in 0.9 %
quasiphysiological NaCl solution.
1. EXPERIMENTAL SETUP
ZrN coatings were synthesized on plates for
osteosynthesis made of AISI 316 L SS by using the
vacuum-arc method with RF discharge in a “Bulat-6”
type device (Fig.1). Bias potential was applied to the
sample holder from the RF generator operated at 5 MHz.
Chemically pure zirconium (at purity 99.999 %) was used
as cathode material. Nitrogen (99.99%) was used as an
active gas. Before deposition, the substrates were pre-
mailto:avtaran@ukr.net
116 ISSN 1562-6016. ВАНТ. 2020. №6(130)
cleaned in an ultrasonic bath for 10 min. Surface cleaning
(substrate degreasing and removing impurities) in the RF
discharge was carried out in an argon plasma for 15 min
(Ubias = 1 kV, P(A) = 0.6 Pa). A Zr buffer layer of 20 nm
thickness was deposited before the nitride coating to
improve coating adhesion, using Iarc = 110 A, U (RF)
bias = -200 V, base pressure P = 5∙10
–3
bar and deposition
time was 20 min.
Fig.1. Scheme of the experimental equipment:
1 – plasma source; 2, 3 – electromagnetic coils;
4 – sample holder; 5 – vacuum chamber
The surface topography of the coating was studied
using JEOL JSM-6390LV scanning electron microscope
(SEM) with an accelerating voltage of 20 kV. Elemental
composition was examined using EDX analysis. X-ray
diffraction (XRD) analyses were performed using
DRON-3M device, under Cu–Kα radiation. Energy-
dispersive spectrometer SPRUT-K (AO Ukrrentgen,
Ukraine) was used for X-ray fluorescent analysis. Film
thickness was determined by XRF examinations and
comprised ~2.2 µm. The measurement of nonohardness
was carried out with a Nanoindenter G200 nanoindentor
from the USA, using Berkovich diamond triangular
pyramid. 7 probes were applied on the sample at a
distance of 15 μm from each other and the results were
averaged.
The electrochemical activity (corrosion properties) of
the ZrN coatings was determined by the values of their
electrode potentials (reference electrode: AgCl). The
measurements were carried out in an electrochemical cell
filled with 0.9 % w/w aqueous NaCl (quasi-physiological
solution).
2. RESULTS AND DISCUSSION
2.1. SURFACE MORPHOLOGY AND CHEMICAL
COMPOSITION
The images of ZrN coated implants are shown in
Fig. 2. The surface morphology of ZrN coated samples
was examined by using light optical and scanning
electron microscopy (Figs. 3, 4). The surface of the
coating is cellular with so-called “honey-comb” type
structure with a cell size of 0.2...2 μm with low amount
of macroparticles.
In Fig. 4,b, SEM cross-section revealed the
formation of dense structure with columnar grain
growth, typical for transition metal nitrides such as TiN,
ZrN, and CrN. Thin Zr buffer layer is also clearly
distinguished in Fig. 4,b.
Fig. 2. General views of implants (plates) for trauma
surgery with ZrN coatings
Fig. 3. Light optical image of ZrN coating on implant
under magnification, × 100
a
b
Fig. 4. SEM image (a) and cross-section (b) of ZrN
coating on implant made of 316 L SS
A typical XRD pattern of ZrN coating is presented
in Fig. 5. All angles of diffraction peaks were indexed
as ZrN phase with a crystal structure of B1 NaCl cubic
lattice type (according to ICDD 96-101-1362,
ISSN 1562-6016. ВАНТ. 2020. №6(130) 117
a = 0.4577 nm lattice parameter). The average grain size
calculated from the full-width-at-half-maximum
(FWHM) intensity was 16 nm confirming the formation
of nano-crystalline structure.
Fig. 5. XRD pattern for ZrN coating grown on stainless
steel implant
According to the EDX data the relative contents of
elements in the coatings were 78 wt.% Zr, and
16 wt.% N, 2...3 wt.% O and 5 wt.% C. The presence of
a small amount of oxygen and carbon is due both to
residual gas incorporated in the chamber walls and to
the contamination during sample handling in open
atmosphere before the composition analysis.
2.2. MECHANICAL PROPERTIES
The results of studies of the hardness and elastic
modulus of ZrN coatings are shown in Table. The
average value of hardness and modulus of elasticity
was: H = 29 GPa; E = 319 GPa. Plasticity index H/E
and the ratio H
3
/E*
2
(where E* = E / (l – μ
2
) – the
effective elastic modulus; μ – Poisson's ratio) are
qualitative comparative characteristics of material
plastic deformation resistance. The shear modulus (G)
and yield stress (σT) are defined as: G = E/2 × (1 + μ)
and σT = Hμ/3.
The results of ZrN coating mechanical test
№ Е, GPa Н, GPa Н/Е Н
3
/Е
*2
G, GPa
σT,
GPa
1 335 31 0.092 0.233 210.19 10.36
2 333 31 0.095 0.249 208.42 10.53
3 289 26 0.090 0.188 180.38 8.70
4 301 25 0.088 0.182 188.77 8.88
5 317 30 0.092 0.218 197.73 9.73
6 332 29 0.088 0.198 207.29 9.71
7 338 32 0.095 0.254 210.77 10.68
319 29 0.092 0.217 200.506 9.798
The increase in the hardness of coatings obtained by
deposition uner RF biasing mode is related, first of all,
to the grinding of the grain structure of the coatings (the
Hall-Petch rule). The factor of compressive internal
stresses that always occur in coatings deposited at low
substrate temperatures under such deposition conditions
cannot be excluded. We also speculate that a pulsed
plasma is not only a source of substance and energy, but
also under certain conditions, it manifests itself as a
powerful matter structurizer.
2.3. CORROSION PROPERTIES
The electrode potential of the pure implant was –
34 mV (Fig. 6, curve 1). The ZrN coating passivates the
surface and increases the potential to a value of +25 mV
(see Fig. 6, curve 2). This means that there are no
through pores in the coating confirming good
passivation properties. We assume that application of Zr
buffer layer can also alter adhesion and may interrupt
the pinhole connection through the coating surface to
the underlying substrate, therefore reducing the
exposure area of the substrate to the electrolyte.
Fig. 6. Corrosion tests in 0.9 % quasiphysiological
NaCl solution
CONCLUSIONS
1. ZrN coatings have been deposited onto AISI 316
L implants for trauma surgery by using vacuum-arc
deposition under RF biasing mode.
2. XRD data revealed the formation of
stoichiometric ZrN phase of cubic modification with
average grain size of 16 nm.
3. The average value of nanohardness comprised
29 GPa with elastic modulus 319 GPa.
4. The electrode potential of the coated implant was
significantly improved than that of the uncoated
stainless steel implant confirming good passivation
properties.
5. The Zr buffer layer improves mismatch of the
ZrN coating and the stainless steel substrate and may
interrupt the pin-hole corrosion.
6. The obtained results would be perspective for
applying functional protective ZrN coating on implants
to reduce Ni induced corrosion.
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Article received 15.09.2020
ФУНКЦИОНАЛЬНЫЕ ЗАЩИТНЫЕ ПОКРЫТИЯ ZrN НА ИМПЛАНТАХ
ДЛЯ ТРАВМАТОЛОГИИ
В.С. Таран, И.E. Гаркуша, A.В. Taран, Р.М. Муратов, П.М. Воронцов, Ю.П. Гниденко,
Г.Н. Герасимов, В.В. Стариков, A.A. Батурин, С.П. Романюк
Нанокристаллические пленки нитрида циркония были синтезированы на имплантах для травматологии,
изготовленных из нержавеющей стали AISI 316 L, с использованием вакуумно-дугового напыления в
режиме ВЧ-смещения в установке “Булат”. Структурные исследования – рентгеноструктурный анализ
(XRD), рентгенофлуоресцентный анализ (XRF), сканирующая электронная микроскопия (SEM) с
микроанализом (EDX), метод наноидентификации – были выполнены для изучения фазового и химического
составов, морфологии поверхности, микроструктуры и нанотвердости покрытий ZrN. Коррозионная
стойкость покрытий исследовалась в 0,9 % квазифизиологическом растворе NaCl.
ФУНКЦІОНАЛЬНІ ЗАХИСНІ ПОКРИТТЯ ZrN НА ІМПЛАНТАХ
ДЛЯ ТРАВМАТОЛОГІЇ
В.С. Taран, І.Є. Гаркуша, А.В. Таран, Р.М. Муратов, П.М. Воронцов, Ю.П. Гніденко,
Г.М. Герасимов, В.В. Старіков, A.A. Батурин, С.П. Романюк
Нанокристалічні плівки нітриду цирконію були синтезовані на імплантах для травматології, які
виготовлені з нержавіючої сталі AISI 316 L, за допомогою вакуумно-дугового осадження в режимі
ВЧ-зміщення в установці типу “Булат”. Структурні дослідження – рентгенівський дифракційний аналіз
(XRD), рентгенівський флуоресцентний аналіз (XRF), скануюча електронна мікроскопія (SEM) з
мікроаналізом (EDX), метод наноідентифікації – були виконані для вивчення фазового та хімічного складів,
морфології поверхні, мікроструктури та нанотвердості покриттів ZrN. Корозійну стійкість покриттів було
досліджено в 0,9 % квазіфізіологічному розчині NaCl.
|
| id | nasplib_isofts_kiev_ua-123456789-194656 |
| institution | Digital Library of Periodicals of National Academy of Sciences of Ukraine |
| issn | 1562-6016 |
| language | English |
| last_indexed | 2025-12-07T17:55:50Z |
| publishDate | 2020 |
| publisher | Національний науковий центр «Харківський фізико-технічний інститут» НАН України |
| record_format | dspace |
| spelling | Taran, V.S. Garkusha, I.E. Taran, A.V. Muratov, R.M. Vorontsov, P.M. Gnidenko, Yu.P. Herasimov, H.M. Starikov, V.V. Baturin, A.A. Romaniuk, S.P. 2023-11-28T12:24:19Z 2023-11-28T12:24:19Z 2020 Functional protective ZrN coatings on implants for trauma surgery / V.S. Taran, I.E. Garkusha, A.V. Taran, R.M. Muratov, P.M. Vorontsov, Yu.P. Gnidenko, H.M. Herasimov, V.V. Starikov, A.A. Baturin, S.P. Romaniuk // Problems of atomic science and tecnology. — 2020. — № 6. — С. 115-118. — Бібліогр.: 13 назв. — англ. 1562-6016 PACS: 81.40.-z https://nasplib.isofts.kiev.ua/handle/123456789/194656 The nano-crystalline films of zirconium nitride have been synthesized on implants for trauma surgery made of AISI 316 L stainles steel by using vacuum-arc deposition under RF-biasing mode in “Bulat” type device. Structure examinations – X-ray diffraction analysis (XRD), X-ray fluoriscent analysis (XRF), scanning electron microscopy (SEM) with microanalysis (EDX), nanoidentation method – were performed to study phase and chemical composition, surface morphology, microstructure and nanohardness of ZrN coatings. The corrosion resistance of coatings has been tested in 0.9% quasiphysiological NaCl solution. Нанокристалічні плівки нітриду цирконію були синтезовані на імплантах для травматології, які виготовлені з нержавіючої сталі AISI 316 L, за допомогою вакуумно-дугового осадження в режимі ВЧ-зміщення в установці типу «Булат». Структурні дослідження – рентгенівський дифракційний аналіз (XRD), рентгенівський флуоресцентний аналіз (XRF), скануюча електронна мікроскопія (SEM) з мікроаналізом (EDX), метод наноідентифікації – були виконані для вивчення фазового та хімічного складів, морфології поверхні, мікроструктури та нанотвердості покриттів ZrN. Корозійну стійкість покриттів було досліджено в 0,9% квазіфізіологічному розчині NaCl. Нанокристаллические пленки нитрида циркония были синтезированы на имплантах для травматологии, изготовленных из нержавеющей стали AISI 316 L, с использованием вакуумно-дугового напыления в режиме ВЧ-смещения в установке «Булат». Структурные исследования – рентгеноструктурный анализ (XRD), рентгенофлуоресцентный анализ (XRF), сканирующая электронная микроскопия (SEM) с микроанализом (EDX), метод наноидентификации – были выполнены для изучения фазового и химического составов, морфологии поверхности, микроструктуры и нанотвердости покрытий ZrN. Коррозионная стойкость покрытий исследовалась в 0,9% квазифизиологическом растворе NaCl. en Національний науковий центр «Харківський фізико-технічний інститут» НАН України Вопросы атомной науки и техники Low temperature plasma and plasma technologies Functional protective ZrN coatings on implants for trauma surgery Функціональні захисні покриття ZrN на імплантах для травматології Функциональные защитные покрытия ZrN на имплантах для травматологии Article published earlier |
| spellingShingle | Functional protective ZrN coatings on implants for trauma surgery Taran, V.S. Garkusha, I.E. Taran, A.V. Muratov, R.M. Vorontsov, P.M. Gnidenko, Yu.P. Herasimov, H.M. Starikov, V.V. Baturin, A.A. Romaniuk, S.P. Low temperature plasma and plasma technologies |
| title | Functional protective ZrN coatings on implants for trauma surgery |
| title_alt | Функціональні захисні покриття ZrN на імплантах для травматології Функциональные защитные покрытия ZrN на имплантах для травматологии |
| title_full | Functional protective ZrN coatings on implants for trauma surgery |
| title_fullStr | Functional protective ZrN coatings on implants for trauma surgery |
| title_full_unstemmed | Functional protective ZrN coatings on implants for trauma surgery |
| title_short | Functional protective ZrN coatings on implants for trauma surgery |
| title_sort | functional protective zrn coatings on implants for trauma surgery |
| topic | Low temperature plasma and plasma technologies |
| topic_facet | Low temperature plasma and plasma technologies |
| url | https://nasplib.isofts.kiev.ua/handle/123456789/194656 |
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