dental

materials
Dental Materials 19 (2003) 188±198
www.elsevier.com/locate/dental

In vitro corrosion behavior of bioceramic, metallic, and bioceramic±

metallic coated stainless steel dental implants
M.H. Fathi a,*, M. Salehi a, A. Saatchi a, V. Mortazavi b, S.B. Moosavi b
a
Department of Materials Engineering, Isfahan University of Technology, Isfahan 84154, Iran
b
School of Dentistry, Isfahan University of Medical Sciences, Isfahan, Iran
Received 4 July 2001; revised 26 November 2001; accepted 18 December 2001

Abstract
Objectives: The most common metals and alloys used in dentistry may be exposed to a process of corrosion in vivo that make them
cytotoxic. The biocompatibility of dental alloys is primarily related to their corrosion behavior. The aim of this work was to evaluate the
corrosion behavior and thus the biocompatibility of the uncoated and coated stainless steels and compare the effect of type of coatings on
corrosion behavior.
Methods: Three types of coatings, hydroxyapatite (HA), titanium (Ti), and a double-layer HA/Ti on AISI 316L stainless steel were made.
HA coating was produced using plasma-spraying technique and Ti coating was made using physical vapor deposition process. In order to
perform a novel double-layer composite coating, a top layer of HA was plasma-sprayed over a physical vapor deposited Ti layer on AISI
316L stainless steel. Structural characterization techniques including XRD, SEM and EDX were used to investigate the microstructure,
morphology and crystallinity of the coatings. Electrochemical potentiodynamic tests were performed in physiological solutions in order to
determine and compare the corrosion behavior of the coated and uncoated specimens as an indication of biocompatibility.
Results: Double-layer HA/Ti coating on AISI 316L SS had a positive effect on improvement of corrosion behavior. The decrease in
corrosion current densities was signi®cant for these coated specimens and was much lower than the values obtained for uncoated and single
HA coated specimens. Ti coating on AISI 316L SS also has a bene®cial effect on corrosion behavior. The results were compared with the
results of corrosion behavior of HA coated commercially pure titanium (cpTi) and uncoated cpTi.
Signi®cance: These results demonstrated that the double-layer HA/Ti coated 316L SS can be used as an endodontic implant and two goals
including improvement of corrosion resistance and bone osteointegration can be obtained simultaneously.
q 2003 Academy of Dental Materials. Published by Elsevier Science Ltd. All rights reserved.
Keywords: AISI 316L stainless steel; Corrosion; HA coating; Ti coating

1. Introduction biocompatibility of dental alloys is primarily related to

Biocompatibility is the ability of a material to perform
with an appropriate host response in a speci®c application
[1]. This means that the tissue of the patient that comes into
contact with the materials does not suffer from any toxic,
irritating, in¯ammatory, allergic, mutagenic, or carcino-
genetic action [2±5]. Since the oral environment is particu-
larly favorable for the biodegradation of metals due to its
ionic, thermal, microbiological, and enzymatic properties, it
can be presumed that the patient is exposed to a certain
extent to the products of the corrosion process [6]. The
* Corresponding author. Tel.: 198-311-8912750; fax: 198-311-
8912752.
E-mail addresses: fathi@cc.iut.ac.ir, fathimoh@yahoo.com
(M.H. Fathi).
0109-5641/03/$30.00 + 0.00 q 2003 Academy of Dental Materials. Published by Elsevier Science Ltd. All rights reserved.
PII: S01 09- 5641( 02) 0002 9-5
their corrosion behavior [7]. The higher the corrosion of
an alloy, the more its elements will be released and the
risk of unwanted reactions in the oral tissues may be
increased. These unwanted reactions include unpleasant
tastes, irritation, allergy or other reaction [7].
Surgical implants are usually made of metallic materials,
such as austenitic stainless steel, cobalt±chromium alloys,
and titanium and its alloys. Among all the metallic materi-
als, the austenitic stainless steels are the most popular
materials because of their relatively low cost, ease of fabri-
cation and reasonable corrosion resistance [8]. However, the
austenitic stainless steels are prone to localized attack in
long-term applications due to the aggressive biological
effects. The corrosion products include iron, chromium,
nickel and molybdenum, etc. Ions can accumulate in tissues
surrounding the implant or be transported to distant parts of
 M.H. Fathi et al. / Dental Materials 19 (2003) 188±198 189

Fig. 1. XRD patterns of the coatings: (a) plasma-sprayed HA coating on cpTi; (b) plasma-sprayed HA coating on 316L SS; (c) double-layer HA/Ti coating on
316L SS.

the body [9]. It has been demonstrated that metallic ions
resulting from the in vitro corrosion of austenitic stainless
steels cause alteration of the expression of human lympho-
cyte-surface antigens and inhibit the immune response as
assessed by lymphocyte proliferation [10]. The presence of
these ions in vivo not only causes toxic effects in mouse
testicular seminiferous epithelium but also alterations in the
spleen cellular population [11].
A number of investigations have demonstrated that metal
ions can be released from metallic materials as the result of
190 M.H. Fathi et al. / Dental Materials 19 (2003) 188±198
Fig. 1. (continued)
corrosion [2,3,8±10,12±14]. Local adverse tissue reactions
or elicit allergy reactions caused by metallic implants
originate from the release of metal ions. This release of
ions depends upon the corrosion rate of the alloy and the
solubility of the ®rst formed corrosion products [15]. Inten-
sive investigations have been carried out on biomaterials in
order to study their corrosion behavior, ion release and its
effects [14,16±25], and toxicity and immunity of alloys
[6,16±18,26±29]. The studies have been more intensive
for stainless steels due to their corrosion behavior [14,19±
29]. It has been suggested that metal ions associated with
316L stainless steel are toxic to osteogenic cells, affecting
their proliferation and differentiation [19]. Stainless steel
corrosion products above certain concentrations may disturb
the normal behavior of osteoblast-like bone marrow cell
cultures [20±22,25]. Advanced techniques have been used
for determining toxicity and tissue reaction around metal
implants [24,27,29]. For this purpose, in vivo animal tests
have been performed [28].
Ion release rates in vitro can be used to determine the
proportionality of release in vivo [30±32] but long-term in
vivo studies have been made and results indicate that metal
ion release increases with the exposure time [33,34].
Release of metal ion in vivo analysis did not demonstrate
any consistent differences in the concentrations of metallic
elements next to stressed and nonstressed miniplates and
screws of stainless steels [35].
A previous in vivo study by the present authors has shown
that the type of metallic implants had signi®cant effects on
the clinical success, bone tissue response and histopatho-
logical results of hydroxyapatite coated/uncoated metallic
implants in animals [36]. In this previous work, endodontic
implants consisting of plasma-sprayed HA coated and
uncoated substrates of various materials, namely 316L
stainless steel and Co±Cr±Mo alloy, were prepared. These
implants were subsequently implanted in the mandibular
canine of cats. After a healing period of 4 months, osteo-
integration evaluation and histopathological interpretation
were carried out by using scanning electron microscopy
(SEM). The results showed that different substrates had
pronounced effects on the histopathological response to
different HA coated implants [36].
The aim of the present work was to evaluate the corrosion
behavior and therefore biocompatibility of the uncoated and
coated stainless steels. In order to design and produce
a desired coating for improvement of histopathological
response, tissue reaction and bone osteointegration around
dental implants, the effects of three types of coatings on the
behavior of substrates were compared.
2. Materials and methods
2.1. Substrates and coatings
Commercially pure titanium (cpTi) and AISI 316L stain-
less steel were used as substrates. The composition (wt%) of
stainless steel was C 0.03, Si 0.80, Mn 1.2, Cr 17.55, Ni
13.65, Mo 3.1, P # 0.040, S # 0.030 and Fe as the balance.
The composition (wt%) of cpTi was Ti . 99.5%.
 M.H. Fathi et al. / Dental Materials 19 (2003) 188±198 191

Fig. 2. SEM micrograph of the coatings: (a) plasma-sprayed HA coating surface showing partially melted with some porosity and microcracks; (b) the top
layer of a double-layer HA/Ti coating shows some porosity and microcracks; (c) a physical vapor deposited Ti coating on a 316L SS.

Ti coating (3±7 mm thickness) was made using physical
vapor deposition process on AISI 316L stainless steel. Crys-
talline hydroxyapatite coatings with 40±60 mm were pro-
duced using plasma-spraying technique on two types of
substrate, i.e. AISI 316L stainless steel and commercially
pure Ti. A double-layer composite coating composed of a
hydroxyapatite top layer (40±60 mm thickness) and a Ti
under layer (3±5 mm thickness) was prepared using a
plasma-spraying and a physical vapor deposition process,
respectively, on AISI 316L stainless steel.
2.2. Experimental procedure
X-ray diffraction (XRD) technique (Philips X'Pert-MPD
System with a Cu ka wavelength of 1.5418 A Ê ) was used to
analyze the crystalline structure and phases present in the
coatings. This technique was also used to estimate the
percentage of the crystallinity of the HA coating. SEM
and energy dispersive X-ray analysis (EDX) techniques
(Philips XL 30) were used to study the microstructure and
morphology of the coatings. EDX analysis was utilized to
estimate the ratio of Ca/P of the HA coating and the compo-
sition of the coatings.
Commercially pure titanium (cpTi) and AISI 316L stain-
less steel (316L SS) were selected as the sample materials.
Coupons of two types of alloys were cut and surface
preparations were carried out by wet grinding with a series
of SiC papers to 4000-grit followed by thorough cleaning in
distilled water, degreasing with acetone and air drying.
An electrochemical corrosion polarization test cell was
used for in vitro potentiodynamic corrosion tests in physio-
logical solutions. Graphite was used as the counter electrode
and saturated calomel electrode (SCE) as the reference elec-
trode. The physiological solutions were the Ringer's solu-
tion and physiological normal saline (0.9 wt% NaCl) and
the potentiodynamic corrosion tests were performed at
37 ^ 1 8C. Dynamic polarization curves were recorded at a
potential scanning rate of 0.5 mV s 21 initiated at 2250 mV
192 M.H. Fathi et al. / Dental Materials 19 (2003) 188±198
Fig. 3. SEM EDX of the coatings: (a) HA coating, desirable Ca/P is obtained; (b) and (c) HA layer and Ti layer, respectively, of a double-layer HA/Ti coating.
below the open circuit potential and the atmosphere was
open to air. Five replicate tests of each group of specimens
were performed.
To compare the corrosion behavior between the uncoated
and HA coated cpTi, the uncoated 316L SS, HA coated
316L SS and double-layer HA/Ti coated 316L SS, speci-
mens were dynamically polarized in two different types
of physiological solutions. Potentiodynamic polarization
curves were determined at 37 ^ 1 8C using a EG and G
model 263A potentiostat/galvanostat interfaced with a
computer and a recorder. The tests were started after a
steady open-circuit potential was attained (not more than
^5 mV drift in 5 min). The anodic and cathodic polariza-
tion curves were obtained for each specimen and corrosion
potentials and corrosion current densities were determined
by Tafel extrapolation and linear polarization methods. The
mean value and standard deviations of the results were
calculated.
It is noticeable that two kinds of electrochemical tests
were utilized in this investigation. The ®rst test was referred
to as a potentiodynamic anodic polarization-scan because it
is dynamic or continuous. It represented a pro®le of the
behavior of the alloy when scanned in a forward direction
from anodic to cathodic potential and spans a range of 1 V
or more. The straight line segments of these scans are iden-
ti®ed by the Tafel equation. DE ˆ b log…i=I0 †: The expanded
form of this equation shows linearity where b is slope and
log i0 is the Y intercept. The scans are plotted as potential, E
(mV, SCE), vs. log current density, log i (mA cm 21), and are
often referred to as Evans Diagrams. The reverse scan was
obtained by reversing the direction of the scan, thus obtain-
ing a reverse Evans Diagram. Curve shape, potentials at
current discontinuities and absolute values are all important
in characterizing corrosion behavior. The second test
involved potentiodynamic or continuous scanning but over
a much smaller potential range than anodic polarization.
Typically, a scan is started 10 mV anodic to the corrosion
potential and terminates 10 mV cathodic to it. The scan is
plotted directly as E vs. i and is referred to as a linear
polarization plot. The slope of the linear segment of the
DE vs. Di plot is expressed by the formula:
…DE=Di†DE!0 ˆ RP ˆ B=icorr
where RP is polarization resistance (kV cm 2), (DE/Di) is
slope (mV cm 2/mA) and
B…constant† ˆ b a bc =2:3…ba 1 bc †
where ba and bc are Tafel slopes for the anodic and cathodic
pro®les, respectively. One way to ®nd the value of the equa-
tion involves the determination of Tafel bc and ba from
 M.H. Fathi et al. / Dental Materials 19 (2003) 188±198
Fig. 3. (continued)
potentiodynamic polarization curves and calculation of the
resulting value of B.
3. Results
3.1. Structural characterization
The XRD patterns of the plasma-sprayed HA coatings on
cpTi and 316L SS are shown in Fig. 1(a) and (b), respec-
tively. In the plot of intensity vs. 2u , there are numerous
sharp peaks and a low background indicative of highly crys-
talline HA coating. Fig. 1(c) also shows the XRD pattern of
a double-layer HA/Ti coating on 316L SS which is very
similar to the XRD pattern of HA coating on 316L SS.
The SEM micrograph showing a typical plasma-sprayed
HA coating on a metallic substrate is shown in Fig. 2(a). The
structure appears to be partially melted and porous and
microcracks can be observed scattered throughout the struc-
ture, probably as a result of a very rapid cooling rate during
the deposition process. Fig. 2(b) is a SEM micrograph show-
ing a typical double-layer HA/Ti coating on 316L SS
substrate which also shows that the coating consists of a
193
porous surface and some microcracks. Fig. 2(c) is a SEM
micrograph showing a physical vapor deposited Ti coating
on a 316L SS. The porosity of the coating is less than HA
coating but microcraks cannot be seen.
The result of EDX analysis of HA coating surface is
shown in Fig. 3(a). The Ca/P ˆ 2 is the desired ratio. Fig.
3(b) and (c) show EDX analysis of HA layer and Ti layer of
double-layer HA/Ti coating.
3.2. Corrosion behavior
The potentiodynamic polarization curves of the uncoated,
HA coated, Ti coated, double-layer HA/Ti coated 316L SS
and HA coated/uncoated cpTi in the normal saline solution
are shown in Fig. 4. The similar curves that are obtained in
Ringer's solution are plotted in Fig. 5. These curves are
selected because their extracted data were the most nearest
to the mean values of the current densities of each group of
specimens.
The corrosion current densities of various specimens
were determined from the potentiodynamic polarization
curves (Figs. 4 and 5) by Tafel extrapolation method.
These results align with corrosion potentials, summarized
194 M.H. Fathi et al. / Dental Materials 19 (2003) 188±198
Fig. 3. (continued)
in Tables 1 and 2 in normal saline solution and Ringer's
solution, respectively. The standard deviations of the corro-
sion current densities are shown in parentheses in Tables 1
and 2. The corrosion current densities as determined by
linear polarization method are also shown in Tables 1 and 2.
According to Table 1 and Fig. 4, the uncoated 316L SS
possesses lower corrosion resistance and thus higher corro-
sion current density (icorr ˆ 265 nA cm 22) in the normal
saline solution. The similar trend can be observed in the
Ringer's solution (Table 2). The HA coating decreased the
corrosion current density of the HA coated 316L SS
(icorr ˆ 68 nA cm 22) and HA coated cpTi (icorr ˆ 43
nA cm 22). The double-layer HA/Ti coating had a sig-
ni®cant effect on the corrosion behavior of 316L SS so
that the corrosion current density of HA/Ti coated 316L
SS decreased (icorr ˆ 44 nA cm 22) and was exactly similar
to single HA coated cpTi (icorr ˆ 43 nA cm 22) in normal
saline solution. The Ti coating could decrease the corrosion
current density of the Ti coated 316L SS in both types of the
physiological solutions (Table 1 and 2).
4. Discussion
The single HA coating had a positive effect on corrosion
resistance of metallic substrate, i.e. 316L SS and cpTi and
decreased the corrosion current density of each type of
coated metallic substrate. The polarization curve, (b) in
Fig. 4, of the HA coated 316L SS was shifted to the left
upper area, compared with curve (a), which is the uncoated
316L SS specimen. It means that the HA coated 316L SS
(Ecorr ˆ 2105 mV, icorr ˆ 68 nA) was more corrosion resis-
tant than the uncoated 316L SS (Ecorr ˆ 2174 mV,
icorr ˆ 265 nA). The corrosion behavior of the HA coated
cpTi (Ecorr ˆ 2256 mV, icorr ˆ 43 nA) was better than
uncoated cpTi (Ecorr ˆ 2334 mV, icorr ˆ 72 nA) up to
200 mV, as manifested by a shift of the polarization curve
(f) to the left upper of the uncoated cpTi curve (e). A similar
trend can be observed in the Ringer's solution (Fig. 5,
curves (a), (b), (e) and (f), Table 2). Therefore, single HA
coating on metallic substrate caused signi®cant changes on
corrosion behavior of substrate. This result was in agree-
ment with the results of the other researchers [37].
Single HA coating could decrease the corrosion current
density of 316L stainless steel substrate in physiological
solutions (Tables 1 and 2 and Figs. 4 and 5) but this effect
was not adequately complete. This was due to the fact that
the structure and surface morphology of single HA coating
consists of a porous surface and some microcracks (Fig. 2)
and could not act as a barrier to the release of metal ions
 M.H. Fathi et al. / Dental Materials 19 (2003) 188±198 195

Fig. 5. Potentiodynamic polarization curves of: (a) the uncoated; (b) HA

Fig. 4. Potentiodynamic polarization curves of: (a) the uncoated; (b) HA
coated; (c) Ti coated; (d) double-layer HA/Ti coated 316L SS; (e) the HA
coated cpTi; (f) uncoated cpTi in the normal saline solution (0.9 wt% NaCl)
at 37 8C.
from metallic implant to physiological solutions and
corrosive environment. The HA coating acted simply as a
semi-mechanical barrier. The corrosion rate in this case was
drastically reduced, although in the microcracks and pores
of the HA coating the substrate came into contact with the
solution and some corrosion occurred.
Earlier work by the present authors showed that the histo-
coated; (c) Ti coated; (d) double-layer HA/Ti coated 316L SS; (e) the HA
coated cpTi; (f) uncoated cpTi in the Ringer's solution at 37 8C.
pathological responses to uncoated 316L SS and uncoated
vitallium were not acceptable [36]. These results are in
agreement with the studies that have been carried out on
endodontic implants [16,17]. Vitallium was originally
used but its biocompatibility was questioned when it was
shown to undergo surface corrosion. This is an important
factor in the success of an endodontic implant. Stainless
steel and vitallium have generally lost acceptance and are

Table 1 Table 2
Mean values (standard deviation) of corrosion current densities and corro- Mean values (standard deviation) of corrosion current densities and corro-
sion potentials in normal saline solution (0.9 wt% NaCl) at 37 8C sion potentials in Ringer's solutions at 37 8C

Material Ecorr (mV) Icorr (nA/cm 2) Material Ecorr (mV) Icorr (nA/cm 2)

Tafel Linear Tafel Linear

Uncoated 316L SS 2174(20) 265 (16) 194 (16) Uncoated 316L SS 2195(20) 218 (17) 181 (20)
Uncoated cpTi 2334(11) 72 (7) 63 (9) Uncoated cpTi 2303(5) 71 (6) 61 (6)
HA coated 316L SS 2105(10) 68 (2) 52 (1) HA coated 316L SS 2110(21) 57 (3) 49 (1)
HA coated cpTi 2256(10) 43 (6) 34 (7) HA coated cpTi 2215(14) 40 (4) 29 (3)
HA/Ti coated 316L SS 2153(15) 44 (5) 32 (3) HA/Ti coated 316L SS 2182(20) 43 (5) 32 (4)
Ti coated 316L SS 288(20) 27 (5) 26 (5) Ti coated 316L SS 261(15) 24 (5) 26 (2)
196 M.H. Fathi et al. / Dental Materials 19 (2003) 188±198
Fig. 6. Periapical tissue response to HA coated 316L SS: (a) in¯ammatory
connective tissue can be observed ( £ 25); (b) the same picture ( £ 100).
no longer available for clinical use as endodontic implants
[16,17].
On the other hand, earlier work showed that the type of
metallic substrates which were HA plasma-sprayed coated
and used for endodontic implants in animals had signi®cant
effects on histopathological response [36]. Statistical analyses
of the signi®cance of the differences between histopathologi-
cal response to single HA coated vitallium and single HA
coated 316L SS were carried out by Kruskal±Wallis method.
More tissue damage, in¯ammation and irritation have been
observed around single HA coated 316L SS (Fig. 6) in
comparison with single HA coated vitallium [36]. This was
owing to the inability of the single HA coating to act as a
barrier to the release of metal ions to animal's body on the
316L SS implants. The bone osteointegration around single
HA coated vitallium alloy and single HA coated 316L SS
were almost the same and from the point of the clinical
success and osteointegration no signi®cant difference were
observed [36]. This result is also in agreement with the
other researchers [38]. It has been observed that there are no
differences between osteointegration when stainless steel is
used instead of Ti alloy as metallic substrate, con®rming
that bone responds primarily to coating [38].
Many attempts have been made for improvement and
optimization of implant surface conditions by creating a
bioceramic coating on implant surface [39±43]. In this
case, double- or multi-layer coatings have been recently
considered by a number of researchers' works [37,44±46]
for improvement of biomedical applications and offering
potential clinical bene®ts in orthopedic and dental surgery.
Bioceramic coatings such as Al2O3, TiO2 and ZrO2 on 316L
SS have already been considered to increase corrosion resis-
tance [43,47±49].
The in vitro electrochemical polarization corrosion test
results indicated that novel double-layer HA/Ti coating
have a bene®cial and desired effect on corrosion behavior
of 316L SS. This can improve the corrosion resistance (Figs.
4 and 5 and Tables 1 and 2) and subsequently can decrease
the release of metallic ions and deleterious effects. There-
fore, two goals could be obtained simultaneously by the
formation of the double-layer HA/Ti coating. First, the
improvement of 316L SS corrosion resistance and decreas-
ing of ion release and consequently prevention of tissue
damages, in¯ammation and irritation and obtain desirable
histopathological response. The second improvement is in
terms of bone osteointegration and bone bonding with the
coated implant.
The Ti coating had a positive effect on corrosion resis-
tance of 316L SS. The polarization curve, (c) in Fig. 4, of
the Ti coated 316L SS was shifted to the left upper
area, compared with curve (a), which is the uncoated
316L SS specimen. The Ti coated 316L SS (Ecorr ˆ 288
mV, icorr ˆ 30 nA) was more corrosion resistant than the
uncoated 316L SS. The type of physiological solution had
no effect on this trend.
It is noticeable that the passive current density (ip) of the
Ti coated 316L SS (curve (c) in Figs. 4 and 5) was similar to
HA/Ti coated 316L SS (curve (d) in Figs. 4 and 5). This
means that the Ti responded primarily to environment and
corrosion reaction was essentially between Ti and solution.
5. Conclusion
Double-layer HA/Ti coating can have a bene®cial and
desired effect on corrosion behavior of 316L SS and
decrease the corrosion current density that is a distinct
advantage for prevention of ion release. Corrosion current
density of double-layer HA/Ti coated 316L SS was similar
and equal to single HA coated cpTi and it suggests that
double-layer HA/Ti coated 316L SS can be used as endo-
dontic implant.
Acknowledgements
The authors are grateful for the support of this research by
Isfahan University of Technology.
 M.H. Fathi et al. / Dental Materials 19 (2003) 188±198
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