Fabrication and characterization of sol-gel

hydroxyapatite-forsterite-bioactive glass
nanocomposite coating for biomedical applications
M. Mazrooei Sebdani*, M.H. Fathi
Biomaterials Group, Department of Materials Engineering,
Isfahan Universityof Technology,
Isfahan, 84156-83111, Iran.
E-mail:m.mazrooei@ma.iut.ac.ir







AbstractFabrication and characterization of hydroxyapatite-
forsterite-bioactive glass nanocomposite coating was the aim of
this work. The sol-gel technique was used to perform
hydroxyapatite-forsterite-bioactive glass nanocomposite coating
on 316L stainless steel (SS). The X-ray diffraction (XRD),
scanning electron microscopy (SEM) and energy dispersive X-ray
analysis (EDX) techniques were used to investigate the
microstructure and morphology of the coating. Results show that
the suitable temperature for calcination was 600 C. At this
temperature, the homogenous and crack-free coating could
attach to the 316L SS substrate. The result of EDX analysis of
hydroxyapatite-forsterite-bioglass coated 316L SS surface
indicated the consisting elements of prepared hydroxyapatite-
forsterite-bioglass nanocomposite coating and the substrate.
Hydroxyapatite-forsterite-bioactive glass nanocomposite coating
might be a good candidate for biomedical application.
Keywords-component; nanocomposite coating
I. INTRODUCTION
During the last years, advances in many special bioactive
ceramics such as hydroxyapatite and bioactive glasses have
improved the quality of human life [1]. These bioactive
ceramics are widely used in numerous ways due to their
appropriate properties such as biocompatibility, chemical
stability, high wear resistance and low density and for calcium
phosphates, mainly for their compositional similarity to
mineral phase of bone [2]. Among which, a great deal of
research has been focused on hydroxyapatite owing to its
closed resemblance to bones and teeth [3, 4]. The usage of
hydroxyapatite has been studied in the form of powders [5],
coatings [6] or composites [7, 8]. However, the poor
mechanical properties such as the inherent brittleness are the
major limitation associated with the use of hydroxyapatite at
high load bearing conditions [5]. There have been several
attempts to combine hydroxyapatite with other ceramics, in
order to produce composites with improved mechanical and
bioactive properties [9]. Composite coatings could be a subject
of interest in order to achieve a combine of properties of
coating and substrate and overcome the main limitation of
hydroxyapatite [10]. So, researches have been focused on. In
experimental studies, it has been observed that the
incorporation of glasses within the CaO-SiO
2
-P
2
O
5
system is
the suitable choice for improving its properties. Glass added
hydroxyapatite composite is able to bond to both soft and hard
tissue without an intervening fibrous layer and as a result,
exhibits greater biological activities than commercial
hydroxyapatite [11, 12]. However, similar to hydroxyapatite,
these glasses could not be used in load-bearing applications
and consequently, these composites have not achieved the
superior mechanical properties [13]. Therefore, it is expected
that the incorporation of other ceramics with better mechanical
properties such as forsterite (Mg
2
(SiO
4
)) might improve the
mechanical properties of hydroxyapatite-bioactive glass
composite coating. In contrast to hydroxyapatite and bioglass,
forsterite ceramics show considerable fracture toughness and
hardness. The fracture toughness of forsterite ceramics is 2.4
MPa.m
1/2
superior to the lower limit reported for bone
implants and hydroxyapatite ceramics (0.6-1MPa.m
1/2
) [14].
Moreover, it is expected that addition of these ceramics with
reduced grain size lower than 100nm improves the mechanical
properties [15]. So, it is expected that hydroxyapatite-
forsterite-bioactive glass nanocomposite coatings have better
mechanical properties than single hydroxyapatite and
hydroxyapatite-bioactive glass nanocomposite coatings.
Among the several methods, solgel synthesis is rapidly
popularized because of inherent suitable properties such as
availability, commercial technique and ability to produce thin
coating. At this method, precursors are mixed at the molecular
978-1-4244-7484-4/10/$26.00 2010 IEEE
Proceedings of the 17th Iranian Conference of Biomedical Engineering (ICBME2010), 3-4 November 2010
level and variously shaped materials may be formed at much
lower temperatures than it is possible by traditional methods
of preparation. The morphology and the composition of the
thin films and powders can be relatively easy to be controlled
by sol-gel processing parameters such as annealing for
crystallization temperature [16] and addition of auxiliary
chemical reagents [17].
The aim of this work was fabrication and evaluation of
novel hydroxyapatite-forsterite-bioactive glass nanocomposite
coating via a sol-gel method.
II. MATERIALS AND METHODS
A. Preparation and characterization of coating samples
The phosphoric pentoxide (P
2
O
5
, Merck), nitrate calcium
tetrahydrate (Ca (NO
3
)
2
.4H
2
O, Merck), ethanol (Merck,
99.9%purity), oxalic acid, forsterite nanopowder [18] and 45S
bioactive glass nanopowder [19] were used for preparing a sol
which contains hydroxyapatite, forsterite and bioactive glass;
20mm10mm2mm of stainless steel plates (SS316L) were
selected as a substrate and polished to grade #1200 and then
cleaned in an ultrasonic bath. Hydroxyapatite-forsterite-
bioactive glass composite coatings were prepared by dipping
substrates in a sol containing hydroxyapatite as a matrix, oxalic
acid, bioactive glass nanopowder and forsterite nanopowders
with 10wt% total amount and withdrawing at a rate of
5cm/min. After aging at ambient temperature for 24h, samples
were placed in an oven and dried at 80 C for 24h and then,
were heat treated at 600 C with 1 C/min. The composite
coatings at different temperatures were subjected to X-ray
diffraction (XRD, Philips XPert-MPD) technique using a
CuK radiation generated at 40kV and 30mA in order to
determine the phase composition. The microstructure and
morphology of prepared coatings was observed using scanning
electron microscopy (SEM, Phillips XL30). The composition
of prepared coatings was estimated by energy dispersive X-ray
analysis (EDX).
III. RESULTS AND DISCUSSION
A. XRD analysis
Fig. 1 shows an XRD pattern of prepared composite
coating. The XRD of composite coating showed the presence
of hydroxyapatite and forsterite peaks in accordance with No:
09-0432 and No: 34-0189 files, confirming it to be free of
additional crystalline phases. Fig. 2 shows XRD patterns of
composite coatings at different temperatures. As shown, as the
sintering temperature increased to 700 C and above,
hydroxyapatite decomposes into the additional crystalline
phases (-TCP and CaO). Therefore, the desired temperature
was determined to be 600 C. The suggested reaction is:
Ca
10
(PO
4
)
6
(OH)
2
=3Ca
3
(PO
4
)
2
+CaO+H
2
O (1)









Figure 1. XRD pattern of the prepared hydroxyapatite-forsterite-bioactive
glass nanocomposite coating.






Figure 2. XRD patterns the prepared nanocomposite coating sinterred at
different temperatures.
B. SEM evaluation and EDX analysis
Fig. 3 shows the SEM micrograph of hydroxyapatite-
forsterite-bioactive glass composite coating. The crack-free
and homogeneous hydroxyapatite-forsterite-bioactive glass
composite coating was observed with no observable defects.
Fig. 4 shows the SEM micrograph of a cross-section view of
prepared coating on the 316L SS substrate. The thickness of
prepared composite coating was about 20-30m.
The result of EDX analysis of prepared coating is shown in
Fig. 5. The peaks of O, Si, P and Ca belong to the consisting
elements of prepared coating and the peaks of Fe, Cr and Ni
belong to 316 L SS.




Figure 3. SEM micrograph of the prepared nanocomposite coating on the
316L SSsubstrate.









Figure 4. SEM micrograph of a cross-section view of the prepared
nanocomposite coatingon the 316L SS substrate.







Figure 5. Energy dispersive X-ray analysis (EDX) of the hydroxyapatite-
forsterite-bioactive glass coated 316L SS sample.
IV. CONCLUSION
Hydroxyapatite-forsterite-bioactive glass nanocomposite
coating was prepared by sol-gel technique. The prepared
coating could attach to the 316L SS substrate and homogenous
and crack-free coating could be performed. Hydroxyapatite-
forsterite-bioactive glass nanocomposite coating can be used
for biomedical application (as dental and orthopedic implants).
ACKNOWLEDGMENT
THE AUTHORS THANK FOR SUPPORT OF THIS RESEARCH BY
ISFAHAN UNIVERSITY OF TECHNOLOGY.
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