The study of the oxide coating effect on bone–implant interface formation by means of electron microscopy method with energy dispersive x-ray analysis
The experimental results of the measurement of the tissue constituent elements distribution, as well as impurity elements in the tissues around a Ti-implant with protective TiO₂ oxide coating are presented. Study of morphology, qualitative and quantitative analysis were carried out by means of scann...
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| Cite this: | The study of the oxide coating effect on bone–implant interface formation by means of electron microscopy method with energy dispersive x-ray analysis / A.A. Gudakova, S.N. Danilchenko, L.F. Sukhodub, V.V. Luk'yanchenko, A.V. Zykova, V.I. Safonov // Вопросы атомной науки и техники. — 2007. — № 1. — С. 145-147. — Бібліогр.: 7 назв. — англ. |
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Gudakova, A.A. Danilchenko, S.N. Sukhodub, L.F. Luk'yanchenko, V.V. Zykova, A.V. Safonov, V.I. 2017-01-04T20:10:09Z 2017-01-04T20:10:09Z 2007 The study of the oxide coating effect on bone–implant interface formation by means of electron microscopy method with energy dispersive x-ray analysis / A.A. Gudakova, S.N. Danilchenko, L.F. Sukhodub, V.V. Luk'yanchenko, A.V. Zykova, V.I. Safonov // Вопросы атомной науки и техники. — 2007. — № 1. — С. 145-147. — Бібліогр.: 7 назв. — англ. 1562-6016 PACS: 87.68.+z https://nasplib.isofts.kiev.ua/handle/123456789/110583 The experimental results of the measurement of the tissue constituent elements distribution, as well as impurity elements in the tissues around a Ti-implant with protective TiO₂ oxide coating are presented. Study of morphology, qualitative and quantitative analysis were carried out by means of scanning electron microscopy method with energy dispersive X-ray analysis. The results show weak migration of Ti into the bone tissue near the interface and protective role of the oxide coatings. Представлено експериментальні результати дослідження розподілу елементів, що входять до складу кісткової тканини та слідів елементів у тканинах навколо титанового імплантату з захисним покриттям ТiO₂. Дослідження морфології, кількісний та якісний аналіз проводили за допомогою методу скануючої електронної мікроскопії з рентгенівським мікроаналізом. Результати показали слабку міграцію титану в кісткову тканину біля інтерфейсу та біосумісність оксидних покриттів. Представлены экспериментальные результаты исследования распределения элементов, составляющих костную ткань и примесей элементов в тканях вокруг титанового имплантата с защитным покрытием ТiO₂. Изучение морфологии, количественный и качественный анализ проводили с помощью метода сканирующей электронной микроскопии с рентгеновским микроанализом. Результаты показали слабую миграцию титана в костную ткань возле интерфейса и биосовместимость оксидных покрытий. We thank T.G. Kalinichenko and P.A. Pavlenko for electron microscopy and X-ray microanalysis. en Національний науковий центр «Харківський фізико-технічний інститут» НАН України Вопросы атомной науки и техники Low temperature plasma and plasma technologies The study of the oxide coating effect on bone–implant interface formation by means of electron microscopy method with energy dispersive x-ray analysis Дослідження впливу оксидного покриття на формування інтерфейсу кість-імплантат методом скануючої електронної мікроскопії з рентгеноспектральним мікроаналізатором Исследование влияния оксидного покрытия на формирование интерфейса кость-имплант методом сканирующей электронной микроскопии с рентгеноспектральным микроанализатором Article published earlier |
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Digital Library of Periodicals of National Academy of Sciences of Ukraine |
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DSpace DC |
| title |
The study of the oxide coating effect on bone–implant interface formation by means of electron microscopy method with energy dispersive x-ray analysis |
| spellingShingle |
The study of the oxide coating effect on bone–implant interface formation by means of electron microscopy method with energy dispersive x-ray analysis Gudakova, A.A. Danilchenko, S.N. Sukhodub, L.F. Luk'yanchenko, V.V. Zykova, A.V. Safonov, V.I. Low temperature plasma and plasma technologies |
| title_short |
The study of the oxide coating effect on bone–implant interface formation by means of electron microscopy method with energy dispersive x-ray analysis |
| title_full |
The study of the oxide coating effect on bone–implant interface formation by means of electron microscopy method with energy dispersive x-ray analysis |
| title_fullStr |
The study of the oxide coating effect on bone–implant interface formation by means of electron microscopy method with energy dispersive x-ray analysis |
| title_full_unstemmed |
The study of the oxide coating effect on bone–implant interface formation by means of electron microscopy method with energy dispersive x-ray analysis |
| title_sort |
study of the oxide coating effect on bone–implant interface formation by means of electron microscopy method with energy dispersive x-ray analysis |
| author |
Gudakova, A.A. Danilchenko, S.N. Sukhodub, L.F. Luk'yanchenko, V.V. Zykova, A.V. Safonov, V.I. |
| author_facet |
Gudakova, A.A. Danilchenko, S.N. Sukhodub, L.F. Luk'yanchenko, V.V. Zykova, A.V. Safonov, V.I. |
| topic |
Low temperature plasma and plasma technologies |
| topic_facet |
Low temperature plasma and plasma technologies |
| publishDate |
2007 |
| language |
English |
| container_title |
Вопросы атомной науки и техники |
| publisher |
Національний науковий центр «Харківський фізико-технічний інститут» НАН України |
| format |
Article |
| title_alt |
Дослідження впливу оксидного покриття на формування інтерфейсу кість-імплантат методом скануючої електронної мікроскопії з рентгеноспектральним мікроаналізатором Исследование влияния оксидного покрытия на формирование интерфейса кость-имплант методом сканирующей электронной микроскопии с рентгеноспектральным микроанализатором |
| description |
The experimental results of the measurement of the tissue constituent elements distribution, as well as impurity elements in the tissues around a Ti-implant with protective TiO₂ oxide coating are presented. Study of morphology, qualitative and quantitative analysis were carried out by means of scanning electron microscopy method with energy dispersive X-ray analysis. The results show weak migration of Ti into the bone tissue near the interface and protective role of the oxide coatings.
Представлено експериментальні результати дослідження розподілу елементів, що входять до складу кісткової тканини та слідів елементів у тканинах навколо титанового імплантату з захисним покриттям ТiO₂. Дослідження морфології, кількісний та якісний аналіз проводили за допомогою методу скануючої електронної мікроскопії з рентгенівським мікроаналізом. Результати показали слабку міграцію титану в кісткову тканину біля інтерфейсу та біосумісність оксидних покриттів.
Представлены экспериментальные результаты исследования распределения элементов, составляющих костную ткань и примесей элементов в тканях вокруг титанового имплантата с защитным покрытием ТiO₂. Изучение морфологии, количественный и качественный анализ проводили с помощью метода сканирующей электронной микроскопии с рентгеновским микроанализом. Результаты показали слабую миграцию титана в костную ткань возле интерфейса и биосовместимость оксидных покрытий.
|
| issn |
1562-6016 |
| url |
https://nasplib.isofts.kiev.ua/handle/123456789/110583 |
| citation_txt |
The study of the oxide coating effect on bone–implant interface formation by means of electron microscopy method with energy dispersive x-ray analysis / A.A. Gudakova, S.N. Danilchenko, L.F. Sukhodub, V.V. Luk'yanchenko, A.V. Zykova, V.I. Safonov // Вопросы атомной науки и техники. — 2007. — № 1. — С. 145-147. — Бібліогр.: 7 назв. — англ. |
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Problems of Atomic Science and Technology. 2007, 1. Series: Plasma Physics (13), p. 145-147 145
THE STUDY OF THE OXIDE COATING EFFECT ON BONE–IMPLANT
INTERFACE FORMATION BY MEANS OF ELECTRON MICROSCOPY
METHOD WITH ENERGY DISPERSIVE X-RAY ANALYSIS
A.A. Gudakova, S.N. Danilchenko, L.F. Sukhodub, V.V. Luk'yanchenko1,
A.V. Zykova2, V.I. Safonov2
Institute of Applied Physics, NASU, Sumy, Ukraine, e-mail: sukhodub@ipfcentr.sumy.ua;
1N.I. Sitenko Orthopedy and Trauma Surgery Institute Design Bureau, Kharkov, Ukraine;
2Institute of Surface Engineering, Kharkov, Ukraine, e-mail: ais@kharkov.ua
The experimental results of the measurement of the tissue constituent elements distribution, as well as impurity
elements in the tissues around a Ti-implant with protective TiO2 oxide coating are presented. Study of morphology,
qualitative and quantitative analysis were carried out by means of scanning electron microscopy method with energy
dispersive X-ray analysis. The results show weak migration of Ti into the bone tissue near the interface and protective
role of the oxide coatings.
PACS: 87.68.+z
1. INTRODUCTION
Metal orthopedic implants have been applied widely
and successfully for various types of bone
reconstructions [1]. Titanium and its alloys show
excellent biocompatibility, good implant fixation due to
the surface oxide, high degree of mechanical strength
and corrosion resistance [2]. TiO2 titanium dioxide is
widely used in biomedical application because its high
blood compatibility and negative surface charge in
physiological solution [3]. Surface treatments such as
anodic oxidation, thermal vacuum deposition, chemical
vapor deposition, plasma spraying and magnetron
sputtering are commonly employed to modify surface
properties and enhance interaction between implants and
adjacent tissues [4]. The implant material degradation and
metal ion dissolution from the metal materials remains the
major factor limiting the longevity of total joint
replacements [2]. Since interaction between tissues and
titanium implants occurred at their interfaces, protective
characteristics of titanium should be essential [5,6]. That is,
the key factors should involve properties of surface TiO2
films and their change in biological environment. The
protective properties of Ti based materials and oxide
coatings play the most important role because of their
ability to prevent the detrimental element penetration to
surrounding bone tissue on the bone - implant interface [7].
2. MATERIALS AND METHODS
The electrochemical treatment of titanium samples in
salt solution of disubstititued sodium sulphate medium at
different stabilize voltage values from 10 to 100 V in DC
regime was made.
The structural and morphological properties of the
interface bone-implant and diffusion of elements into the
bone tissue were characterized by the scanning electron
microscope REMMA-102, equipped with the
multichannel wave-dispersive and energy dispersive
X-ray spectrometers manufactured by JSC “SELMI”
(Sumy, Ukraine). The X-ray energy dispersive
spectrometer, equipped with the semi-conductor Si (Li)
detector, had the power resolution 200 eV. The
accelerating voltage for an electronic probe was 20 kV,
when the current of the probe was 3 nA. The time of the
spectrum acquisition in each point was 200 seconds.
To prevent the accumulation of surface electrostatic
charge, during electron probe microanalysis, the sample
was covered with thin layer of aluminum in the special
vacuum equipment.
The Ti holders with investigated coatings were
implanted in medial surface of the proximal metaphyse of
rabbit cannon bone. The samples were extracted after the
implantation into the bone during four months tests
duration. The reparative regeneration of the bone tissue
and focal reaction of connective tissue under the condition
of bone defect reparation by means of Ti implant with
oxide coating in vivo test was observed.
The content of base elements of substrate material and
coating in bone tissue and the weight ratio Ca/P in the
bone zone near the interface was measured (see Table).
Quantities of Ti, P, Ca on the interface bone tissue -
implant (obtained by using X-ray microanalysis) in areas
of analysis (1-4) (see Fig. 1)
3. RESULTS AND DISCUSSION
In the present study the qualitative and quantitative
analysis of the interface bone-implant and material
degradation degree estimation were made. The sample
was titanium implant, with protective oxide coating TiO2,
deposited by electrochemical method in salt solution of
disubstititued sodium sulphate medium at potential 70V.
It was extracted after the implantation into the cannon
bone of rabbits in vivo test.
P Ca Ti Ca/P,
weight,%
Ca/P, at.,%
1 3,7644 7,6524 0 2,03329 1,572051
2 3,2062 6,8926 0,0242 2,14969 1,662046
3 2,0606 4,2082 0,043 2,042342 1,579049
4 4,3094 9,0894 0,0302 2,109264 1,63079
mailto:sukhodub@ipfcentr.sumy.ua
mailto:ais@kharkov.ua
146
0 5 10 15 20 25 30
0
10
20
30
40
50
60
70
C
on
ce
nt
ra
tio
n,
%
d
ry
w
ei
gh
t
Distance, microns
Ti
Ca
P
The place of tight contact of the implant with the bone
tissue and the horizontal area of bone tissue under Ti-
implant were selected for study by scanning electron
microscopy. The obtained micrograph of the bone tissue,
which formed in cavities and convexities of implant is
given below (Fig. 1).
In the Fig. 1 we marked the points of analyses which
were studied at magnification x500 and accelerating
voltage 20 kV.
.
Fig.1. Micrograph of the area of bone tissue which was in
tight contact with the Ti implant
Micrographs which show morphology of the bone
tissue under the Ti-implant are given in the Fig. 2 (a-d).
a b
c d
Fig.2. Micrographs of bone tissue horizontal surface
which was under Ti-implant obtained at magnification
x500: (a, b)1 and 2 points of analyses;
(c, d) 3 and 4 points of analyses
The reaction of the living tissue on the introduced
implant was estimated by Ca/P ratio in the bone tissue.
X-ray microanalysis was carried out using SEM
(REMMA-102) with x-ray analyzer.
The results of the qualitative and quantitative analysis
are given in the Table above. The concentration of
elements was calculated directly from the spectrum.
The obtained results show, that quantity of Ti is rather
small, close to the detection limit of device. The weight
ratio Ca/P (1,9-2,03) which is typical for HA
(hydroxyapatite) observed in the bone zone near the
interface region correlate with the ratio for the real bone.
As it is shown at the graph in Fig. 3, first three points
were at the surface of implant, where content of Ti was
maximal but there was no Ca and P. Then, at the fourth
point the quantity of Ti decreases (interface implant-bone
tissue), but the quantity of Ca and P increases greatly
(which connected with the bone tissue formation).
Further, the concentrations of this elements are nearly at
the same level.
Fig. 3. The Ti, Ca, P concentrations depending on the
distance in the zone implant-bone
In the Fig. 4, the Ti concentration at the distances
more than 10 µm from the implants are given in the
narrower concentration range.
Fig. 4. Dependence Ti concentration
(% dry weight) on distance (microns)
At the distance of 10 µm from implant concentration
of Ti is low, which is related with the loss of electron
beam in the connective tissue. At the points 10, 12, 14 we
can see the sudden change of Ti concentration. It could be
explained by the presence of connective tissue, in which
the distribution of Ti is irregular. At the rest of the points
the concentration of Ti gradually decreases with the
increase of the distance from the implant.
10 15 20 25 30 35
0,0
0,2
0,4
0,6
0,8
1,0
1,2
C
on
ce
nt
ra
tio
n,
%
d
ry
w
ei
gh
t
Distance, microns
Ti
147
4. CONCLUSIONS
1. The results show the weak migration of Ti into the
bone tissue near the interface. Also, the normal weight
ratio Ca/P (1,9-2,03) which is typical for HA
(hydroxylapatite) was observed in bone zone near the
interface region.
2. These data suggest the major importance of oxide
coating deposition for further implant biocompatibility,
ingrowth and osteointegration. The oxide coatings form
the reliable barrier to the toxicity of metal ion
dissolution and keep the normal ratio Ca/P in zone
near the bone-implant interface.
ACKNOWLEDGEMENTS
We thank T.G. Kalinichenko and P.A. Pavlenko for
electron microscopy and X-ray microanalysis.
REFERENCES
1. A.M. Ektessabi, T. Otsuka, Y. Tsuboi et al.
Preliminary experimental results on mapping of the
elemental distribution of the organic tissues
surrounding titanium-alloy implants // Nuclear
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v. 109/110, p. 278-283.
2. Eva Palsgard, Carina Johansson, Gang Li et al. Bone
growth and bone development in the presence of
implants or after induced leg-lengthening studied using
the Oxford Scanning Proton Microprobe // Nuclear
Instruments and Methods in Physics Research B. 1997,
v. 130, p. 431-438.
3. C. Lin., S. Yen. Characterization of electrolytic TiO2
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modifications for titanium implants // European Cells
and Materials . 2001, v. 1, Suppl. 2, p. 22-27.
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Characterization of surface oxide films on titanium and
adhesion of osteoblast //Biomaterials. 2003, v. 24,
p.4663-4670.
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using of modern pulsed ion-plasma
technology//Problems of Atomic Science and
Technology. 2003, N1, p. 137-141.
7. A.V. Zykova, V.V. Luk’yanchenko, V.I.Safonov,
V.M.Rashkovan. The corrosion properties of implanted
materials with various protective coatings//Proceeding
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Canada, 4-10 April, 2005, N IS –73.
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