Biomaterials 23 (2002) 1995–2002

Influence of fluoride content and pH on the corrosion resistance of

titanium and its alloys
Nicolas Schiffa,*, Brigitte Grosgogeata, Michele Lissaca, Francis Dalardb
a
School of dentistry, University Claude Bernard of Lyon 1, Rue Guillaume Paradin, 69372 Lyon Cedex 08, France
b
Electrochemical and Physico-Chemical Laboratory of Materials and Interfaces, Polytechnic Institut of Grenoble, UMR 5631,
"
INPG-CNRS, Rue de la piscine 38042, Saint Martin D’heres Cedex, France
Received 30 January 2001; accepted 21 September 2001

Abstract

In the last decade, new titanium alloys have been developed in different areas of dentistry, such as TiAl6V4 and NiTi.
Concurrently, treatments using fluoride supplementation, such as odontology fluoride containing gels, have also been widely used in
odontology.
The aim of this study was to compare the NiTi, NiTiCo and TiAl6V4 alloys with the titanium, regarding the corrosion resistance
in Fusayama Meyer artificial saliva with different pH and fluoride contents. In the experimental methods, the corrosion potential
was measured over time, then a linear sweep voltametric analysis measured the polarization resistances and corrosion currents.
Our results have shown that TiAl6V4 alloys have a good corrosion resistance as good as that of titanium in Fusayama Meyer
saliva and acid salivary solution, except NiTi and NiTiCo alloys.
Conversely, we noticed, as for the titanium, a remarkable localized corrosion phenomenon of those new alloys in fluoride and
acid–fluoride salivary solutions. The fluoride ions could cause the breakdown of the protective passivation layer that normally exists
on the titanium and its alloys, leading to pit corrosion. r 2002 Published by Elsevier Science Ltd.

Keywords: Titanium; Corrosion; Titanium alloys; Fluoride; pH; Salivary media

1. Introduction The purpose of the present study is therefore to

compare the electrochemical properties of the TiAl6V4,
Titanium and the titanium-based alloy TiAl6V4 are NiTi and NiTiCo alloys with those of pure titanium, as
chosen for dental implantology because of their a function of the pH and fluoride content of the
resistance to corrosion and their biocompatibility [1–3]. medium.
Similarly, in orthodontics, NiTi memory alloys are
also widely used since they can create a less traumatic
force while still producing very good results [4–7].
2. Materials and methods
In parallel to these practices, fluoride therapy is now
recognized as being one of the principal methods in
2.1. Materials
preventing dental caries.
While numerous studies have been carried out on the
The origin and composition of the titanium, titanium
electrochemical corrosion of titanium and titanium-
alloy and nickel titanium alloys studied are shown in
based alloys, few have rarely taken into account the
Table 1.
influence of fluoride and pH on pure titanium [8–15],
The four samples were selected from metal already
and to our knowledge, the electrochemical behavior of
prepared for implantology and orthodontics use. The
TiAl6V4 and NiTi in a fluoridated medium has never
samples were shaped into a cylindrical form, as shown in
been investigated.
Fig. 1, in order to constitute the cap of a rotating disk
electrode.
*Corresponding author. Tel.: +33-476-86-19-63. The metal part was inserted in a polytetrafluoroethy-
E-mail address: nicolas.schiff@wanadoo.fr (N. Schiff). lene (PTFE) ring, adaptable to the working electrode.

0142-9612/02/$ - see front matter r 2002 Published by Elsevier Science Ltd.

PII: S 0 1 4 2 - 9 6 1 2 ( 0 1 ) 0 0 3 2 8 - 3
1996 N. Schiff et al. / Biomaterials 23 (2002) 1995–2002

Table 1
Origin and composition of materials

Material Composition (wt%) Supplier

Pure titanium grade 2 Ti: base, O: 0.18, N: 0.05, STRAUMANN

C: 0.06, H: 0.013 St Ismier, Switzerland
TiAl6V4 Ti: base, Al: 6, V: 4 CEZUS
Ugine, France
NiTi Sentalloy Ni: 50.4, Ti: 49.6 G.A.C
Tours, France
NiTiCo (experimental alloy) Ni: 51.7, Ti: 45, Co: 3.3 ENSCP
Paris, France

Table 2
Metal P.T.F. E. pH and fluoride concentration of different test media

pH Fluoride
content
Resin Medium 1: Fusayama Meyer saliva 5.3 F
Medium 2: acidified saliva 2.5 F
Medium 3: fluoridated saliva 5.3 1 g/l
Fig. 1. Rotating disk electrode. Medium 4: fluoridated–acidified saliva 2.5 1 g/l

In order to prevent infiltration of the electrolyte, the
space between the metal and the PTFE was filled with a
resin having inert electrochemical properties.
The exposed surface of the metal disk constituted the
working electrode (the areas concerned were 0.158 cm2
for pure titanium and TiAl6V4, 0.005 cm2 for NiTi
Sentalloy, and 0.036 cm2 for NiTiCo).
The samples were mechanically cleaned with abrasive
strips (BF03 0.3 mm, Tacussel, Villeurbanne, France).
2.2. Test solutions
(1). The electrolyte reference used was Fusayama
Meyer artificial saliva. All the ingredients were supplied
by Sigma Chemical Company, St. Louis, USA. The
composition of this solution, which closely resem-
bles natural saliva, is KCl (0.4 g/l), NaCl (0.4 g/l),
CaCl2
2H2O (0.906 g/l), NaH2PO4
2H2O (0.690 g/l),
Na2S
9H2O (0.005 g/l), Urea (1 g/l). The pH was
measured with an XC601 type glass electrode (Radio-
meter Analytical, Villeurbanne, France) convected to a
PHM 220 type pH meter (Radiometer, Analytical,
Villeurbanne, France). The pH of this reference saliva
corresponding to our first test medium was 5.3.
(2). The second medium used had the same contents
as the first, but the pH was lowered by adding lactic acid
(Prolabo, Paris, France). This acid was chosen in order
to obtain conditions that were as close as possible to the
clinical reality since this acid is naturally released by
bacteria in the buccal cavity [16]. The pH was fixed
arbitrarily at 2.5, knowing that the pH of the
commercially available fluoridated odontological gels
(e.g., Fluogel, Dentoria, Le Plessis-Robinson, France
and Fluocaril, Synthelabo, Le Plessis-Robinson,
France) is about 4, and that after a meal, the buccal
cavity pH can fall below this value in confined
zones [17]. We, therefore, chose the most unfavorable
situation.
(3). The third medium was identical to the reference
medium but was enriched with fluoride ions (Prolabo,
Paris, France) with a concentration of 0.1% (i.e., 1 g/l or
1000 ppm), which corresponds to the average fluoride
concentration of the odontological gels mentioned
above. The pH was still around 5.3.
(4) The last medium was both fluoridated and at
the same time acidified: 0.1 g/l of fluoride ions and
pH 2.5.
Each of the four materials, described above, titanium,
TiAl6V4, NiTi and NiTiCo, was tested in the four
different media. Fluoride ions concentrations and pH
are shown in Table 2.
2.3. Electrochemical setup
We used a glass electrochemical cell (Roucaire,
Courtaboeuf, France), with the thermostat set (Bio-
block, Illkirch, France) at 37.070.11C. The cover of the
cell was pierced with openings to facilitate the insertion
of different electrodes (Radiometer Analytical, Villeur-
banne, France): TC 100 type satured calomel electrode
(SCE), platinium counter electrode and a working EDI
101 type rotating disk electrode. The entire three-
electrode assembly was placed in a Faraday cage to
limit noise disturbance, and was then connected to an
EG&G PAR 273 A type computer controlled potentio-
stat (Perkin Elmer, Evry, France).
 N. Schiff et al. / Biomaterials 23 (2002) 1995–2002 1997

In our investigation, a rotating electrode, with a FUSAYAMA MEYER SALIVA

rotating speed of 500 rpm was used. ACIDIFIED SALIVA
FLUORIDATED SALIVA
0.2 FLUORIDATED-ACIDIFIED SALIVA
2.4. Technique for studying corrosion resistance 0

Corrosion potential was measured over time, then the -0.2

E(V/SCE)
polarization curves (i ¼ f ðEÞ) were plotted once the -0.4
potential had stabilized in order to determine the
-0.6
corrosion resistance of the titanium and titanium alloys
in different media [18]. -0.8
The corrosion potential was measured for a period of
-1
24 h. Voltametry was then performed at a scanning rate 0 5 10 15 20 25
Time(h)
of 0.25 mV/s in a potential range of 800–1200 mV/
SCE. Fig. 2. Corrosion potential evolution against time for Titanium in
Since the surface areas of our four samples were different media.
different, the results are presented according to unit
area. The densities of corrosion current values are given
in A/cm2. Table 3
The polarization curves were used to determine, by Corrosion potentials (mV/SCE) of the samples in different media after
24 h
the Stern–Geary method, the density of corrosion
current (icorr) and the polarization resistance Corrosion potential Ti gr 2 TiAl6V4 NiTi NiTiCo
(Rp ¼ ðDE=DiÞ) at the end of corrosion potential mV/SCE (Ecorr)
exposure after 24 h. The polarization resistance values Fusayama Meyer saliva 25 0 100 420
are given in kO cm2. Acidified saliva 80 50 250 880
The different experimentations ensured a perfect Fluoridated saliva 300 370 300 410
Fluoridated–acidified saliva 850 800 525 410
control of the physicochemical parameters. This permits
the duplication under identical experimental conditions,
therefore leading to comparable and reproducible
results with a maximum error of 10–15% for the values. potential indicated the passivation of the pure titanium
In order to confirm the influence of fluoride, the grade 2 in this medium [20–23].
current density was monitored over time for the pure In the acidified medium, the shape of the Ti gr 2 curve
titanium grade 2 sample by applying a potential of changed very little and the potential obtained was only
100 mV/SCE for 2 h in Fusayama Meyer saliva with very slightly negative (Fig. 2), suggesting that the
different fluoride concentrations. material retained its protective passive layer [24].
In the fluoridated medium, the potential of the pure
2.5. Surface analysis titanium grade 2 decreased, reaching 300 mV/SCE after
24 h (Fig. 2). This suggested that the characteristics of
Two of the alloys, NiTi and NiTiCo, were observed the passive film change in this medium, leading to a
using a LAECA CAMBRIDGE LTD-type scanning reduced corrosion resistance [25].
electron microscope. The samples were then subjected to Finally, in the fluoridated–acidified medium, the
chronoamperometry at a constant potential of 100 mV/ corrosion potential of the pure titanium grade 2
SCE for 5 h in two different media: Fusayama Meyer dropped sharply to a value of approximately 850 mV/
saliva and fluoridated–acidified medium. SCE (Fig. 2), suggesting the complete disappearance of
the protective passive layer and a consequent reduction
of the material corrosion resistance properties [10,15].
3. Results and discussion All the values are reported in Table 3.
Thus, the chronoamperometric examinations per-
3.1. Measurement of corrosion potential of the different formed on the pure titanium grade 2 enabled us to
materials determine the induction time prior to the current density
increase for different fluoride concentrations in Fusaya-
3.1.1. Pure titanium grade 2 ma Meyer saliva. We found that the higher the fluoride
We noted that the corrosion potential of the pure concentration in the medium, the shorter is the
titanium grade 2 stabilized at 25 mV/SCE in Fusayama induction time. This effect can be seen from the results
Meyer saliva medium (Fig. 2). This value is similar to shown on a semi-logarithmic scale in Fig. 3.
that obtained by Grosgogeat [19] in the same experi- These results confirmed the negative influence of
mental conditions. The continued increase in corrosion fluoride on the electrochemical behavior of pure
1998 N. Schiff et al. / Biomaterials 23 (2002) 1995–2002

1% FLUORIDATED SALIVA FLUORIDATED-ACIDIFIED SALIVA

2% FLUORIDATED SALIVA FLUORIDATED SALIVA
5 10
-7 ACIDIFIED SALIVA
0 FUSAYAMA MEYER SALIVA
-7
4 10 -0.1

E(V/SCE)
-0.2
i(A/cm²)

-7
3 10

-7
-0.3
2 10
-0.4
1 10-7
-0.5
0
-2.5 -2 -1.5 -1 -0.5 0 -0.6
0 5 10 15 20 25
Log(t)
TIME(h)
Fig. 3. Current evolution against time for titanium, in different
fluoride concentration media, at 100 mV/ECS (semi-logarithmic scale). Fig. 5. Corrosion potential evolution against time for NiTi Sentalloy
in different media.

FUSAYAMA-MEYER SALIVA FLUORIDATED-ACIDIFIED SALIVA

FLUORIDATED-ACIDIFIED SALIVA FLUORIDATED SALIVA
FLUORIDATED SALIVA ACIDIFIED SALIVA
0.2 ACIDIFIED SALIVA -0.2 FUSAYAMA MEYER SALIVA
-0.3
0
-0.4
-0.2
-0.5
E(V/SCE)

E(V/SCE)

-0.4 -0.6
-0.7
-0.6
-0.8
-0.8
-0.9
-1 -1
0 5 10 15 20 25 0 5 10 15 20 25
TIME(h)
TIME(h)
Fig. 4. Corrosion potential evolution against time for TiAl6V4 alloy in Fig. 6. Corrosion potential evolution against time for NiTiCo alloy in
different media.
different media.

titanium grade 2, as previously demonstrated by
Toumelin–Chemla [15], Boere [8] and Reclaru [12].
We, therefore, decided to compare this metal to
titanium-based alloys tested in the same conditions.
3.1.2. TiAl6V4
For the TiAl6V4 alloy, the shape of the corrosion
potential curves over time was the same (Fig. 4). In
Fusayama Meyer saliva, the corrosion potential was
approximately 0 mV/SCE (Table 3), a value similar to
that obtained by Grosgogeat [19], Khan [26] and
Ricardo [25], also indicating that the metal underwent
passivation.
In the other three media, the results and conclusions
were the same as for pure titanium grade 2.
than pure titanium grade 2 and TiAl6V4, confirming the
results of Rondelli [30–31] who obtained a value of
160 mV/SCE in the same experimental conditions.
In acidified saliva medium, this alloy is deteriorated,
with a corrosion potential of 250 mV/SCE (Table 3),
suggesting an increase in the corrosion rate of the
material in this medium.
In a fluoridated saliva medium, the alloy also
deteriorated, reaching a potential of approximately
300 mV/SCE (Table 3), which was roughly the same
as in the case of pure Ti gr 2 and TiAl6V4.
In the fluoridated–acidified saliva medium, the
potential dropped sharply, as observed for pure Ti gr
2 and the TiAl6V4 alloy, reaching a value of 550 mV/
SCE (Table 3).

3.1.3. NiTi 3.1.4. NiTiCo

For the NiTi alloy, the shape of the curve in
Fusayama Meyer saliva also indicated that a passive
layer formed on the metal [27–29] (Fig. 5), even though
the corrosion potential was negative: 100 mV/SCE
(Table 3). This result indicates that NiTi is less noble
Lastly, the shape of the curve obtained for the NiTiCo
alloy (Fig. 6) and the very negative corrosion potential
value of 400 mV/SCE (Table 3) after 24 h corrosion in
Fusayama Meyer saliva medium suggested a poorer
corrosion resistance [32]. The metal became less noble,
 N. Schiff et al. / Biomaterials 23 (2002) 1995–2002
suggesting that the characteristics of the passive film
change. This result is contrary to the findings of Chern
[33] who reported a more noble behavior for this
material. This difference may be due to the machining
of the sample and in particular the heat treatment.
Then, in acidified saliva medium, the NiTiCo alloy
deteriorated even more, with the value dropping to
880 mV/SCE (Table 3).
The fluoridated saliva medium was found to have the
same influence on corrosion (410 mV/SCE) (Table 3)
as in the case of the other alloys.
On the other hand, this was the alloy on which the
effect of the fluoridated–acidified saliva medium seemed
to be the least negative (400 mV/SCE) (Table 3),
though we should bear in mind that the corrosion
resistance of this alloy was supposed to be considerably
poorer in Fusayama Meyer saliva medium than in those
of the other samples.
3.2. Polarization curves
3.2.1. Pure titanium grade 2 and TiAl6V4
Similar polarization curves were obtained for pure
titanium grade 2 and the TiAl6V4 alloy (Figs. 7 and 8).
The values given in Table 4 suggested that densities of
corrosion currents of these two materials increased,
indicating that their corrosion resistance decreased with
medium changes: acidified, fluoridated or fluoridated–
acidified.
The polarization resistance values in Table 5 indicate
an inversely proportional change: as the medium
changed to acidified, then to fluoridated and then to
fluoridated–acidified, the values decreased, showing an
increase in corrosion rate.
These different results are confirmed by different
studies [8,10,12] performed on pure titanium in Fusaya-
ma Meyer saliva and acid–fluoridated saliva media.
Fig. 7. Polarization curves for titanium in different media.
1999
Fig. 8. Polarization curves for TiAl6V4 alloy in different media.
To the best of our knowledge, no studies have been
performed on TiAl6V4 in fluoridated medium.
3.2.2. NiTi and NiTiCo
The results obtained for NiTi and NiTiCo alloys were
different from those obtained with pure titanium and
TiAl6V4 (Figs. 9 and 10). As summarized in Table 4, the
corrosion current density obtained in Fusayama Meyer
saliva, fluoridated saliva and acidified saliva media
is higher, suggesting an insufficient electrochemical
resistance.
However, it is interesting to note that these two alloys
seem to be less affected by the fluoridated–acidified
saliva medium than were pure titanium and TiAl6V4:
the corrosion current densities were also lower and the
polarization resistance values were of a similar magni-
tude (Tables 4 and 5). These findings confirm our first
results, namely, that in Fusayama Meyer saliva and
acidified saliva media, the corrosion resistance of the
NiTi and NiTiCo alloys was low compared with that of
pure titanium and TiAl6V4.
On the other hand, in fluoridated saliva and
fluoridated–acidified saliva media, the polarization
resistance values of NiTi and NiTiCo alloys did not
drop as sharply as they did in that of pure titanium and
the TiAl6V4 alloy.
3.3. Surface analysis
It was decided to perform surface analyses on the
NiTi and NiTiCo alloys since they displayed the highest
risk of corrosion. The samples were observed using
scanning electron microscopy (SEM)[34]. The surface
micrographs obtained are shown in Figs. 11–14.
They show a general change in the surface of the NiTi
and NiTiCo in Fusayama Meyer saliva medium, while
2000 N. Schiff et al. / Biomaterials 23 (2002) 1995–2002

Table 4
Densities of corrosion currents values (106 A/cm2) of the samples in different media determined by the Stern–Geary method

icorr (106 A/cm2) Ti grade 2 TiAl6V4 NiTi NiTiCo

Fusayama Meyer saliva 170.2 1.570.2 2072 1572

Acidified saliva 370.3 3.570.3 4574 3073
Fluoridated saliva 10.572 970.2 5075 6075
Fluoridated–acidified saliva 500755 480750 250730 300725

Table 5
Polarization resistance values (kO cm2) of the samples in different media determined by the Stern–Geary method

Rp (O cm2) Ti grade 2 TiAl6V4 NiTi NiTiCo

Fusayama Meyer saliva 500745 430745 6076 7078

Acidified saliva 300735 350730 4575 4075
Fluoridated saliva 6075 4574 2073 1572
Fluoridated–acidified saliva 170.2 270.3 570.5 370.3

Fig. 9. Polarization curves for NiTiCo Sentalloy in different

media.
Fig. 11. SEM photomicrograph  1000 of NiTiCo alloy after
chronoamperometry in Fusayama Meyer saliva.

in the much more aggressive fluoridated–acidified saliva

medium the metal is characterized by localized pitting.
These results confirm those of Grimsdottir [16] who also
observed surface degradation of NiTi alloys in the form
of localized pitting corrosion.

4. Conclusion

The results of the present study have made it possible

Fig. 10. Polarization curves for NiTiCo alloy in different media.
to classify the different titanium alloys currently used in
Odontology according to their corrosion resistance, with
pure titanium grade 2 used as the reference.
The electrochemical tests performed using poten-
tiometric and voltametric techniques revealed an
 N. Schiff et al. / Biomaterials 23 (2002) 1995–2002
Fig. 12. SEM photomicrograph  1000 of NiTi Sentalloy after
chronoamperometry in Fusayama Meyer saliva.
Fig. 13. SEM photomicrograph  1000 of NiTiCo alloy after
chronoamperometry in fluoridated–acidified saliva.
interaction between the fluoride ions and titanium,
which caused changes to the protective passive layer of
the metal.
Patients wearing dental prosthetic reconstructions or
who have titanium implants should therefore be advised
not to use fluoridated odontological gels.
The corrosion rates of the TiAl6V4 alloy were found
to be similar to those of the reference sample.
In the case of NiTi and NiTiCo alloys, corrosion
resistance was lower than that of the other alloys,
especially in neutral and acid saliva media. Further
studies are now needed to investigate these phenomena
in more detail.
2001
Fig. 14. SEM photomicrograph  1000 of NiTi Sentalloy after
chronoamperometry in fluoridated–acidified saliva.
In the meantime, it would be advisable to limit the use
of fluoridated gels or mouth rinces for young people
wearing orthodontic braces with NiTi wires. Thus,
nickel is known to cause toxic and allergic reactions in
the body, and concerns have been expressed regarding
the biocompatibility of material.
In all cases, fluoride was found to have a negative
effect on pure titanium and the titanium-based alloys
and this information should be widely diffused to all
dental practitioners.
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