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The evaluation of the wettability and surface characterization of titanium

implant coated by electrophoretic deposition technique

Conference Paper · February 2017

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 9th National Conference of Mechanical Engineering-NCME2017
Islamic Azad University, Khomeinishahr Branch, Iran
February 2017

The evaluation of the wettability and surface characterization of titanium

implant coated by electrophoretic deposition technique

Amirsalar Khandan1* , Ebrahim Karamian2, David Ogbemudia3

*
Corresponding author: [email protected]

Abstract Keywords
The long-term success of any dental implants largely depends on how rapid the Nanocomposite,
healing process takes place as well as how safe the integration process with the Coating, Orthopedic
jaw bone will be. The aim of this current study is to characterize the wettability of Implant, Wettability,
orthopedic implant coated with the electrophoretic deposition technique. The Surface Modification
novel Hydroxyapatite-Diopside (HA-DI) nanocomposite coats were fabricated via
electrophoretic deposition technique. The reactions of the coats that were
incubated in the simulated body fluid (SBF) solution were studied to investigate
the wettability, and growth of apatite of the coats. The results showed that the
bioactivity and wettability values of obtained composite coatings enhanced with
increase in DI amounts by up to 30%. The results of the wettability and
thermogravimetric analysis (thermal decomposition) of nanocomposite might be
an important factor in dental coating applications. The pore volume indicates an
increasing trend with higher temperature which is suitable for osseointegradation
of prosthesis inside the body. Wettability is an important parameter, and the
porous films usually displays a highly hydrophobic character due to the
hydrophobic polymer matrix and the air entrapped inside the pores, which
results in an increased surface roughness.

1
Young Researchers and Elite Club, Khomeinishahr Branch, Islamic Azad University, Isfahan, Iran
2
Advanced Materials Research Center, Department of Materials Engineering, Najafabad Branch, Islamic Azad
University Najafabad, Iran
3
Mechanical Engineering Department, Eastern Mediterranean University, North Cyprus, Gazimağusa, TRNC,
Mersin 10, Turkey
 2

1. Introduction (bioinorganics) into the calcium silicate structures.

The trace elements such as magnesium (Mg2 +), zinc
There are different types of metallic implants used (Zn2 +), titanium (Ti4 +) and zirconium (Zr4 +) have
in human body; these are mostly made up of been incorporated into the Ca Si structure. The
medical-metallic grade like titanium-based (Ti) [1]. resulting minerals, namely CaMgSi 2O6 (diopside)
One of the advantages of Ti implants over the other [20-25], Ca3ZrSi2O9 (baghdadite) [16],
types of implant is the formation of a fibrous layer Ca2MgSi2O7 (akermanite) [17-18] and have already
between the metallic part and surrounding tissue been tested in vitro and in vivo, and indicate
[2]. Ti implants are the most commonly used significant improvement in comparison to simple
metallic materials which remain in the body after calcium silicate [25-27]. The use of eggshell as the
the bone heals and can be there for long time [2-3]. calcium source in producing bioceramics has been
Thus, various intricate surgical procedures can lead reported in previous researches [23-27]. The
to higher cost for people and patients that require application of hydroxyapatite (HA) has been
replacement with permanent implants [4-6]. discovered in various forms like coatings, powders,
Therefore, this revision is one of the major reasons and nanocomposites. Unfortunately, the HA
for replacing the conventional metals like stainless samples are limited due to their brittleness, high
steel 316 L with Ti-6Al-4V implant [6-8]. By prices, high dissolution and difficult synthesising
considering the serious health problems i.e. bone method. Therefore, discovering cheap second
degradation and tumor disorder, it is crucial to phases has been a huge challenge in creating HA
obtain a composite that meets predictable that has high performance with excellent quality at
performance [9-11]. Wound healing around a dental low cost. The modification of calcium silicates by
implant that is placed into a prepared osteotomy metal ions improved their biological and
follows three stages of repair- the first is the mechanochemical performance. Diopside (DI) is a
formation of a blood clot that takes place through suitable choice because of its easy preparation
the process of biochemical activation [12-13]; this technique unlike other additives that use
is followed by a cellular activation and finally, the mechanical activation (MA) method [23-25].
third phase is the cellular response. Bioactivity, Meanwhile, additives that enhance the bioactivity
wettability rate and mechanical properties may all of pure HA, and improves nanocopmposite coats in
depend on the chemical and physical nature of the SBF or ringer solution. Fluorine doped
material including the extent of its crystallinity, hydroxyapatite (F-HA; Ca10 (PO4)6(OH)2−xF x has
crystallite size, processing condition and porosity. been revealed to be a viable alternative to bone
However, the excellent properties of Ti, leads to an because of its good biocompatibility, low solubility,
appropriate choice for clinical usage of Ti alloys, and also high thermal and chemical stability [28].
which needs to be addressed before and after Pure fluorapatite (FA; Ca10 (PO4)6 F2) is known to
surgical implantation. There are some important have a much lower solubility in biological fluids
parameters that required for highlighting them than HA, because FA has a greater stability
while conducting the biomaterials/biomedical compared to HA, both chemically and structurally
investigations. Several surface modifications have [22-28]. The bios activate material serves as a
been developed and are currently being used with scaffold for new bone formation and increase the in
the aim of enhancing clinical performance, growth of osteoprogenitor cells, capillaries, and
including turned, blasted, acid-etched, porous per vascular tissue from the recipient
sintered, oxidized, plasma-sprayed [3, 14, 20] and bed. Biomaterials should participate in the
hydroxyapatite-coated surfaces, as well as the continuous process of bone remodeling, and the
combinations of these procedures. Enhancing the implanted biomaterial should be gradually replaced
bioactivity and wettability of Ti alloys is possible at a rate that is comparable to that of the in growth
via different coating methods that will be used on of newly formed bone. Nowadays, FeO3 ceramics
the bone implant. Several types of coating like: have been the target of attention of researchers due
Electrophoretic Deposition (EPD) [1, 22-24], to their useful properties in various applications
plasma spray [3, 20-25], and sol-gel [17, 25] are ranging from solid oxide fuel cells, sensors, and
used to coat the implants. Characterization and environmental catalysts to magnetic materials [29].
investigations on the applications of these silicate Besides, high domain-wall velocity as well as the
materials in bone repair research are growing existence of Bloch lines makes them applicable in
rapidly due to production new types of biomaterials magneto-optical data storage devices. The
[12]. Recently, several novel bioceramics that have biomaterials containing calcium and silicates have
been introduced to modify dental implant surface good bioactivity, and are able to bond with living
like apatite/wollastonite [13], wollastonite [14], tissues when implanted [30]. Therefore, DI
akermanite [15], baghdadite [16], akermanite [17], bioceramics have been considered as a material to
forsterite [18], and bioglasses [14, 19] have been achieve suitable biological and mechanical
seen to bond with the bone. As a successful method properties by adding to HAs, which are prepared
for improving the orthopedic application, one can due to the the incorporation of the second phases
refer to the incorporation of trace elements
 9th
National Conference of Mechanical Engineering-NCME2017

such as TiO2 [28], Al2O3, ZrO2 and ZrSiO4, and DI of DI in 90, 80, 70wt. % of NHA were prepared and
powder into HA microstructure. The surface mixed with Iso-propanol (99.9%, Merck).
properties and modification such as wettability, Suspensions of the obtained nanocomposite at a
roughness, bioactivity, surface charge, and porosity concentration of 10/100 (g/mL) were prepared in
play a significant role in the enhancing the Iso-propanol, in an ultrasonic bath for 30 min and
biomedical implants [31]. Hydrophobicity is an stirred with a magnetic stirrer for 120 min. The
important surface property, because it often plays a surface treatment samples were ultrasonically
dominant role in the physical interactions that takes washed with distilled water and then dried in an
place between components in an aqueous oven. Deposition was carried out on substrates of
environment. And also, It may influence the 10 mm×10 mm×2 mm. A Ti cathode (−) sample
adhesion of biological parts on the protein surface. and a graphite anode (+) electrode were also used.
In other to evaluate the influence of DI powder with
2. Materials and methods NHA on its bioactivity and wettability, the changes
in the reaction at the surface of the obtained
2.1. Sample Preparation nanocomposite after the predicted time of contact
with SBF were investigated. The solution was
The titanium implant specimen’s was selected prepared following the procedure described by
as a substrate, as it is commonly used for Kokubo. Coated samples were soaked in the falcon
biomedical applications. The Ti substrate were
for predicated time 1, 7, 14 and 21days at 37C
cleaned thoroughly with acetone, ultrasonically and
with the pH=7.4, without refreshing the soaking
dried in the oven at temperature 110°C for about 2
medium. The process is shown schematically,
min. The synthesis procedure to synthesis DI is
where the powders were carried out at 850°C with 3
called mechanical activation (MA). The amount of
h for NHA and at 1350°C for 10 for Di powder,
starting raw materials required for synthesis of 10 g
fabrication of composite, ball milling, and sintering
DI powder was as follow: talc (Merck 99% purity),
process (see Fig. 1).
calcite (Merck 99% purity) and silica (Merck 99%
purity) 4.74 wt%., 3.76 wt. %, 1.5 wt. %,
2.4. Coatings Characterization
respectively. Then, the blend of this compound was
sintered for 10 h at 1350C in the atmospheres 2.4.1. Characterization of Dental Implants
furnace. The matrix for composite contains NHA as
the starting materials synthesized and described in Contact angle measurements were performed to
the previous work as shown in the Figure 1[3, 21]. evaluate the materials wettability. The sessile drop
method was used to measure the contact angle by
2.2. Fabrication of Composite depositing ultrapure water (3μl; Milli-Q; Millipore,
USA) on the surfaces of the polymer films using a
The composites with different amounts of DI contact angle measurement system (OCA 20;
(10 wt%, 20 wt% and 30 wt.%), pure DI, was Dataphysics, GmbH, Germany). Contact angle
mechanically activated (MA) through high energy analysis will be carried out by sessile drop of SBF
ball milling (HEBM) process. HEBM was chosen using optical measurements, CCD camera. The
to avoid segregation of oxides under a BPR of 10 theoretical contact angle was calculated as the
and a vial velocity of 400 rpm for 10 h. Mechanical following equation:
milling, is one of the widely used techniques to
produce nanoparticles. It is feasible for large-scale Cos (Ɵ)=( γ -γ )/γ
SV SL LV (Eq.1)

which γ , γ γ
nanoparticle production; however, it is a simple and
low cost technique. It is a complex process and In SV SL and LV are respectively
requires optimization of a few parameters to obtain interfacial surface tensions of solid–gas, solid–
the required phase, absence of residues and control liquid and V liquid–gas. Thermogravimetric
of particle size. These features are relevant for analysis (TGA) and differential scanning
current biomedical applications of magnetic calorimetric (DSC) analysis were use for thermal
nanoparticles, most of which requires characterization of bioceramic powders. The BET
biocompatible magnetic nanoparticle with small specific surface area of the calcined powder was
particle size [20, 21, 23, 29]. obtained by N2 adsorption–desorption (Model
ASAP 2010, Micro meritics, Norcross, GA) with
2.3. Coating Technique the multiple point’s method. Sintered densities of
the pellets were measured by the Archimedes
EPD technique was used according to our previous method in distilled water (three pellets were
work as the best method for coating HA on Ti measured every time).Instruments are applied for
implant [22, 24]. The coating technique was carried analyzing the experimental results for samples
out at room temperature (37±1°C). The four type containing different percentages of powders.
coatings with different amounts of DI
nanocomposite sample with 0, 10, 20, and 30 wt. %
 4

2.4.2. Thermal Analysis between 200 and 450°C, followed by the last W.L
in the range 500-900°C caused by combustion of
TGA is carried out by increasing the temperature the organic materials in the composite. The total
slowly and plotting weight against temperature. weight loss of the DI powder was 24%. It is very
Observations of the thermogravimetric (Isfahan interesting to introduce bone-like apatite to produce
University, IUT, and Iran) were carried out dry at a chemical bonding between the nanocomposite,
heating ramp rate of 20°C/min, from 30 to 1350°C. hard/soft tissue and matrix [26]. In fact, a non-
In this study, TGA was conducted on DI powder to biodegradable NHA/DI made hybridization
assess its water loss temperature. The heat flow indicated higher strength than conventional NHA.
within the samples pan was compared to that of the Generally, these apatite formations both decrease
reference pan DSC, which was performed in the DI the corrosion rate of the substrate and increase the
nanopowders. The pore volume and surface area in vitro bioactivity of the implants. The apatite
indicate an increasing trend with higher formation mechanism on the surface of coats shows
temperature. that the silanol (Si-OH) groups which exist in DI
structures are effective for creating heterogeneous
nucleation. Although, the apatite formation of NHA
changes the shape of surface of the sample
containing 30% Di powder. An increase in
agglomeration was also observed to be the result of
an increase in NHA content. The EDS spectra
showed that these spherical nanoparticles consist of
calcium, silica and phosphorus. The surface area
indicated a decrease of 8% up to 4 h, while the pore
volume indicated a decrease of 28%. Milling
process for 10 h showed a surface area decrease of
55%. Although the calcinations performed at
1350°C for 10 h indicated a decrease in surface area
Figure (1) the process is shown schematically in to14 m2/g (Fig. 3).
which powders were carried out at 850°C for 3 h in
the NHA and at 1350°C for 10h in the Di powder,
Fabrication of composite, ball milling, and sintering
process.

3. Results and Discussions

3.1. Thermal Analysis
Figure 2 shows the thermal decomposition curve of
DI powders. The profiles indicates three different
weight losses, related to three processes caused by
the high temperature , according to the thermal
cycle graph which is performed from 50°C to
1100°C.
Figure (3) BET surface area (m2/g), Pore size (nm)
of synthesized DI powders.

3.2. Wettability Results

Furthermore, the Ca, Na, P and Cl precipitated from

the SBF solution can also be monitored. This
mineralization occurred in the coated sample with
30% DI powder. Due to mineralization of samples
and SBF wettability with SBF solution improved.
From the shown equation it can be seen and
introduced that a circular groove leads to an upward
increase in contact angle (ϴ) which leads to a
Figure (2) TGA vs. DSC curve of synthesized DI decrease in its wettability. The ability of
and NHA powders [24]. a coated surface in the sample 30%
First drop in weight loss was seen at 50-150°C to decrease the surface-tension of SBF
which was due to the evaporation (weight loss, in contact with it such that it spreads over the
W.L) of water, then the second W.L happened coated surface and wets the surface. It is obvious
 9th
National Conference of Mechanical Engineering-NCME2017

that higher surface energy leads to good wettability amount of 30% DI powder along with higher
and adhesion (see Fig. 4) [20-21]. It is true that low porosity. Compared to other bioceramics with SiO2,
surface energy had a non-wetting test surface. A such as akermanite (Ca2MgSi2O7) [17-20] and
good wettability or hydrophilic due to high surface bredigite (Ca7MgSi4O16) [30] ceramics, diopside
energy and small contact angle (less than 90°) nanopowder possessed great improved mechanical
occurred. Implant surface properties are likely to be and biological properties. Such porosity allowed the
of particular relevance to the chemical and liquids to diffuse into the implant which facilitated
biological interface processes in the early healing the corrosion attack. DI powder reinforced NHA
stages after implantation. composites, exhibited significant improvements in
biological properties, such as bioactivity and
wettability. To our knowledge, the fabrication and
preparation of NHA/DI composite coated on Ti
substrate, have not been reported to be associated
with mechanical activation as synthesis and coating
EPD process. Razavi et al. [31] worked on bredigite
coating that was prepared on a biodegradable
magnesium alloy. The bredigite coating enhanced
the corrosion resistance of magnesium alloy. The
surface wettability and adhesive behaviors (see
Fig.4-5), as important properties of porous
materials, have been given more attention due to
new function development, such as photoelectric
Figure (4) Wettability test of nanocomposite conversion antireflection and cell adhesion. Many
sample calculated by surface tension formula. artificial surfaces with special wettability and
adhesion have been prepared, for example
Hydroxyapatite, (HA), is a calcium phosphate vertical-aligned multiwalled carbon nanotubes
(CaP) bio-ceramic material which has an almost and an artificial biomimic polymer film
identical chemical composition to that of the duplicated by a rose petal surface. In this field,
mineral component of teeth and bone. It is well- our group also reported a high-adhesive ordered
known that the bioceramic materials, such as HA, porous structure surface fabricated with EPD
can integrate well with living bone tissues by technique. The surface adhesive force of the as-
spontaneously forming a biologically active bone- prepared film can be effectively adjusted by
like apatite layer on their surfaces. HA is changing the pore sizes. However, the wettability
manufactured in many forms and can be prepared and adhesion regulation on the conductive
as a dense ceramic, powder, ceramic coating that is polymer porous material surface by the external
required for a particular application. In addition, voltage has generated fewer reports.
adding of DI nanopowders to the NHA leads to an
improved wettability and bioactivity [22-25]. It
also showed a high degree of swelling in water, and
an elastic nature which can closely simulate natural
tissue so that it can be readily accepted by the
body [26]. Additionally, data showed that the
decrease in porosity of the nanocomposite with
higher percentages of DI nanopowders of up to
20% in their microstructure, caused to some extent,
an enhancement of the mechanical properties like
micro-hardness; however, it was neutralized with
the effect of particle accumulation along with the
increase of DI powder content. Therefore, the Figure (5) The wettability and bioactivity feature
nanocomposite NHA with 30% DI is preferred of the nanocomposite wetted with the SBF liquid.
because great amount of DI powder reinforcing
agent helps the procedure to have better porosity for
scaffolds composites and bone osseointegradation. Wettability is an important parameter, and porous
Also, it enhances the wettability and chemical films usually display a highly hydrophobic
properties compared to the pure NHA coatings. character due to the hydrophobic polymer matrix
Therefore, the effect of different percentages of DI and the air entrapped inside the pores, which
powders on the porosity, microstructure, and increases the surface roughness [20, 3].
hydrophilicity of the created scaffolds were
4. Conclusion
examined. It is noticeable that higher wettability
This work was written with the aim of synthesizing
and bioactivity happened in the sample with the nanostructured diopside by utilizing the facile
 6

method from eggshell powder as the source of implants by electrophoretic deposition of

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