Degradation Characteristics of Poly-tetrafluoroethylene

Coatings on Stainless Steel Orthodontic Wires Immersed

in Tuna Fish Derived Products
MADALINA NICOLETA MATEI1, KAMEL EARAR1*, LUCIA CARMEN TRINCA2*, DANIEL MARECI3, LENUTA FOTEA2,
CATALINA ANISOARA PEPTU3, CRISTINA BICA4
1
Dunarea de Jos University of Galati, Medicine and Pharmacy Faculty, Department of Dentistry, 47 Domneasca Str., 800008, Galati,
Romania
2
Ion Ionescu de la Brad University of Agricultural Sciences and Veterinary Medicine, Faculty of Horticulture, 3 Mihail Sadoveanu
Alley, 700490, Iasi, Romania
3
Gheorghe Asachi Technical University of Iasi, Faculty of Chemical Engineering and Environmental Protection, 73 D. Mangeron
Blvd., 700050, Iasi, Romania
4
University of Medicine and Pharmacy of Tirgu Mures, Faculty of Dentistry, 38 Gheorghe Marinescu Str., Tirgu Mures, Romania

This paper objective was to evaluate the degradation characteristics of polytetrafluoroethylene (PTFE)
coatings on stainless steel orthodontic wires with memory shape while immersed in tuna fish derived
products. EIS was the major investigative technique, since it has the potential to discover new information
on the processes occurring, while not interfering significantly with the mechanism operating. The spectra of
uncoated and coated orthodontics stainless steel wires were recorded, and the data were analyzed in order
to evaluate the equivalent circuit (EC) parameters and subsequently the degradation characteristics of each
material. The corresponding corrosion morphologies after polarization test was also observed using scanning
electron microscopy (SEM). Comparison of the electrochemical behaviour, in the condition of exposure to
aggressive media, for stainless steel orthodontic wires with memory shape, coated with a PTFE porous
layer versus the uncoated alloy sample was done. The coatings stainless steel orthodontic wires samples
exhibited more positive zero current potential, higher breakdown potential, and lower anodic current densities
than the uncoated ones. Impedance spectra were interpreted in terms of a duplex film, with corrosion
resistance arising mainly due to the thin inner layer as the outer layer being more porous was less sealed.
Pseudo-capacitive behaviour and high corrosion resistance were registered for the coated stainless steel
alloy, in the medium to low frequency ranges. This paper results are valuable for estimation of coated and
uncoated stainless steel orthodontic wires corrosion resistance and for anticipation of their effect upon
biochemical events in oral cavity.
Keywords: stainless steel dental alloy, memory shape, polytetrafluoroethylene coatings, tuna fish products,
EIS, SEM

Metal alloys are the main materials of orthodontics wires

and arch [1]. Formerly, the alloys used in orthodontics were
gold-based alloys. Their high costs and low mechanical
properties determined their replacement with more
economical materials like NiTi alloys and stainless steel.
In the actual socio-economical conditions, the dental
physician should select with discernment from the rich
offer of alternative orthodontics materials existing currently
on the market.
Currently, orthodontic materials with the inner ability of
transforming between the two phases (austenite/
martensite) begin to be of interest for clinical testing, the
more so as, the use of metal alloys with shape memory
property may reduce the time of treatment in daily practice.
Stainless steels are substantially used in many countries
as main materials of orthodontic wires and arches. Among
them, AISI 316L stainless steels presented, in vitro, the
same corrosion behaviour after immersion in
electrochemical media that simulates the inner human
body physiological state versus pathological one [2].
However, the performance of an orthodontic wire is
conditioned by its corrosion behavior in the oral
environment, an aggressive and complex electrolytic
medium [3]. Ion leaching and corrosion processes trigger

the releasing of the materials different component

particles, depending on solubility, pH, wear induced by
biomechanical forces, electrochemical processes at the
interface and outer factors. The investigations focusing
corrosion and using different in vitro models may contribute
to the selection of an alloy with enhanced properties [415], or a special coated layer as coating is one of the most
widely used method for reducing biomaterials corrosion.
The electrochemical techniques for evaluation of corrosion
resistance are rapid, reproducible, reliable, and also provide
information about corrosion mechanism involved [22-24].
The increased consumption of refined products derived
of fruits, vegetables, milk, meat and fish [16-20], raised
the prevalence of orthodontic wires corrosion in the mouth,
especially in the last years. However, the paucity of reported
studies on the corrosion behaviors of orthodontic wires in
refined products, explains the limited information regarding
the corrosion behavior of stainless steel orthodontic wires
in fish derived products [21].
This work presents the electrochemical study of
polytetrafluoroethylene (PTFE) coatings on stainless steels
orthodontic wires in contact with derived fish products.
The electrochemical behaviour of each stainless steel
orthodontic wire was evaluated by potentiodynamic

* email: erar_dr.kamel@yahoo.com; lctrinca@uaiasi.ro; Tel.: 0040745320134

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REV.CHIM.(Bucharest) 67No. 4 2016

Fig. 1. EDX spectra

measured at the
surface of the coated
orthodontics stainless
steel

Fig. 2. EDX spectra

measured at the
surface of the uncoated
orthodontics stainless
steel

polarization and electrochemical impedance spectroscopy

(EIS) after different immersion time in derived fish
products.
EIS was the major investigative technique, since it has
the potential to discover new information on the processes
occurring, while not interfering significantly with the
mechanism operating. The spectra of uncoated and coated
orthodontics stainless steel wires were recorded, and the
data were analyzed in order to evaluate the equivalent
circuit (EC) parameters and subsequently the degradation
characteristics of each material. The corresponding
corrosion morphologies after polarization test was also
observed using scanning electron microscopy (SEM).
The obtained data are valuable for estimation of coated
and uncoated stainless steel orthodontic wires corrosion
resistance and for anticipation of their effect upon
biochemical events in oral cavity.
Experimental part
Materials and methods
Materials
Tow different uncoated and coated with PTFE
orthodontics stainless steel, both manufactured by
Dentsply Gac International Inc. (Bohemia NY, USA), were
considered in this investigation. The chemical compositions
has been determined by EDX analysis using a scanning
electron microscope (SEM) Quanta 3D Model AL99/D8229
(FEI, Hillsboro, OR, USA) operating with beam energy 30
kV. The chemical compositions of uncoated and coated
with PTFE orthodontics stainless steel are presented in
figures 1-2.
Differential scanning calorimetry (DSC)
The stainless steel orthodontic wires were examined
with DSC technique in order to determine the
accompanying transformations with temperature.
The sample was placed in an aluminum crucible, and
sealed. An empty aluminum crucible served as a reference
during the DSC measurements with DSC Model 1Mettler
Toledo. Nitrogen gas (120 mL/min) was used in order to
prevent condensation of water vapors and oxidation of
REV.CHIM.(Bucharest)67 No. 4 2016

stainless steel orthodontic wires. The temperature of the

crucible was scanned from -40 to + 50 oC at 15 oC/min.
Electrochemical media
Electrochemical tests were performed in two different
media: the first medium used was the fish paste obtained
by mixing (with a blender) the content of a tuna filet in
sunflower oil can, that consisted in sliced tuna filet in
sunflower oil, having 185g net weight, 140 drained weight,
and containing Skipjack tuna (Katsuwonus Pelamis),
sunflower oil and salt as ingredients. The pH of the paste
obtained from tuna filet in sunflower oil was 5.79.
The second medium, was the paste resulted by mixing
(with a blender) the content of tuna filet in brine can,
consisting in sliced Skipjack tuna steak (Katsuwonus
Pelamis) in brine, having 195g net weight, 150 drained
weight, and containing tuna steak, water and salt as
ingredients. The pH of the paste obtained from tuna filet in
brine was 5.83.
Both types of tuna filet cans (Nixe, Ecuador) were
obtained from supermarket.
Biochemical freshness and proximate composition
parameters were determined in order to evaluate the
main variations of both electrochemical mediums
containing the tuna fish paste (in sunflower oil / in brine),
during 8 h storage at room temperature.
The pH was determined on homogeneous solution of
sample and distilled water (1:10, w:v), using a InoLab 730
pH metre. Also, moisture, protein, colagen, lipid and salts
contents, as the main proximate composition parameters
were determined by NIRS Near Infrared Spectrophotometer
Food Check Bruins.
Electrochemical measurements
A three-electrode corrosion flow cell kit (C145/170,
Radiometer, France) with platinum as counter electrode
and saturated calomel reference electrode (SCE) as
reference electrode was employed for both electrochemical measurements. The electrochemical cell
contained a freely adjustable Luggin capillary that housed
the reference electrode. The sample surface of the

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801

uncoated and coated stainless steel orthodontic wires

exposed to the electrolyte testing was 0.05 cm2 . All
potentials in this paper are referred to the SCE. All
electrochemical measurements were carried out on a
Princeton Applied Research potentiostat Model PARSTAT
4000 (Princeton Applied Research, Princeton, NJ, USA). The
instrument was controlled by a personal computer and
specific software (Versa Studio, PAR, Princeton, NJ, USA).
Electrochemical impedance spectroscopy (EIS)
measurements were also performed using the same
instrumentation. The perturbation amplitude was 10 mV
and the frequency ranged down from100 kHz to 10 mHz.
Five points were recorded for each frequency decade. The
EIS spectra were obtained at different times: 1 hour, 2 h ,
and 8 h after electrode immersion in tuna filet paste in
sunflower oil, and in brine. The EIS experimental data were
analyzed in terms of equivalent circuits (EC) using
ZSimpWin 3.22 software [25]. Measurement of
potentiodynamic polarization curves (PPC) was initiated
after 8 hours exposure to the test.
Scanning electron microscopy (SEM) of corroded surfaces
In order to observe the surface morphology the
polarization tested samples have been analyzed by
scanning electron microscopy (SEM) using a HITACHI-SU
1510 microscope.
Results and discussions
DSC analysis of the uncoated and coated stainless steel
orthodontic wires
The DSC heating and cooling curves of the uncoated
and coated stainless steel orthodontic wires are shown in
figures 3 and 4, respectively. The endothermic peaks
appear to be constant at 11-12 oC. Such type of endothermic
peaks are attributed to the transformation of martensite to
austenite due to presence of alloy intermetallic phases.
The endothermic peak from the heating curve of the
uncoated and coated stainless steel orthodontic wires is
the austenite corresponding transformation temperature
while the exothermic peak from the cooling curves is
considered as the corresponding martensite transformation
temperature.

Fig. 4. The DSC thermogram of the coated stainless steel

orthodontic wires

The experimental impedance data measured at the

open-circuit potential of both the uncoated and coated
stainless steel orthodontic wires immersed for different
periods of time in both type of derived tuna fish products,
at 37 oC are presented as Nyquist diagrams in figures 5-6.
Nyquist plots showed that the impedance of the
materials decreased with the elapse of time, more

Electrochemical analysis
When an alloy is placed in the oral cavity environment,
it takes place an electrochemical interaction (i.e., corrosion
process).

Fig. 5. Nyquist plots of the impedance spectra measured for:

(a) coated and (b) uncoated stainless steel orthodontic wires as
Fig. 3. The DSC thermogram of the uncoated stainless steel
a function of immersion time in the paste of tuna filet in
orthodontic wires
sunflower oil
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Fig. 6. Nyquist plots of the impedance spectra measured for: (a)

coated and (b) uncoated stainless steel orthodontic wires as a
function of immersion time in the paste of tuna filet in brine

pronounced for the uncoated material. All the spectra

exhibit a capacitive loop (open arc). The diameter of the
open arc provided an estimation of the polarization
resistance. The decrease in diameter indicated a reduction
of the corrosion resistance.
Bode plots of the two materials immersed for different
periods of time in fish products are shown in figures 7-8.
The advantage of the Bode plot is that the data for all
measured frequencies are shown and also a wide range of
impedance values are displayed.
The frequency dependence of the phase angle indicates
the number of time constants presented in the system and
can be used to determine the parameters values in the
equivalent circuit. Two peaks were observed in the Bodephase plots determined for the coated stainless steel
orthodontic wires, whereas only one was observed for the
uncoated stainless steel orthodontic wires. This indicates
the involvement of two time constants in the open circuit
potential for the coated stainless steel orthodontic wires
immersed in both type fish products. The rather high
impedance values (of the order of 104 cm2), registered
in the medium to low frequencies domaine, revealed the
presence of the corrosion resistance of the coated stainless
steel orthodontic wires in the fish products used as
electrochemical medium.
The impedance modulus (|Z|) of stainless steel
orthodontic wires slowly decreased with the time of sample
immersion. All the spectra showed that in the higher
frequency region, log |Z| tends to become constant. This
is a typical response for the resistive behavior and
corresponds to the solution resistance, Rsol. In the medium
frequency range, a linear relationship between log |Z| and
log f was observed in all cases, though with different slopes
(always less than 1), whereas the maxima in the phase
REV.CHIM.(Bucharest)67 No. 4 2016

Fig. 7. Bode plots of the impedance spectra measured for:

(a) coated and (b) uncoated stainless steel orthodontic wires as a
function of immersion time in the paste of tuna filet in
sunflower oil

Fig. 8. Bode plots of the impedance spectra measured for: (a)

coated and (b) uncoated stainless steel orthodontic wires as a
function of immersion time in the paste of tuna filet in brine

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Table 1
ELECTROCHEMICAL PARAMETERS RESULTED FROM EIS SPECTRA BY USING
THE SELECTED EC FOR THE PTFE COATED STAINLESS STEEL ORTHODONTIC
WIRES AFTER DIFFERENT IMMERSION TIME IN THE PASTE OF TUNA FILET IN
SUNFLOWER OIL AT OPEN CIRCUIT POTENTIAL

Fig. 9. Equivalent circuits used for fitting the

measured impedance spectra

Table 2
ELECTROCHEMICAL
PARAMETERS RESULTED
FROM EIS SPECTRA USING
THE SELECTED EC FOR THE
UNCOATED STAINLESS
STEEL ORTHODONTIC
WIRES AFTER DIFFERENT
IMMERSION TIME
IN THE PASTE OF TUNA
FILET IN BRINE AT OPEN
CIRCUIT POTENTIAL

angle plots are smaller than 90o, indicating that the both
stainless steel orthodontic wires were not completely
capacitive.
For the interpretation of the electrochemical behavior
of a system from EIS spectra, an appropriate physical model
of the electrochemical reactions occurring on the
electrodes is necessary. The electrochemical system may
be represented by an equivalent circuit (EC). In the case of
the uncoated stainless steel orthodontic wires, the spectra
could be satisfactorily simulated using the simplified EC
circuit shown in figure 9a. The occurrence of a second
overlapping wave in the phase shift response of the
stainless steel orthodontic wires indicated that the spectra
cannot be explained by the simple equivalent circuit based
on a single parallel combination of a resistance and a
constant phase element, as shown in figure 9a. Therefore,
fitting of the impedance was done with the EC depicted in
figure 9b using a series combination of the solution
resistance, Rsol (7510 W cm2), with two RQ parallel
combinations: Rsol (R1Q1) (R2Q2). The proposed EC give the
electrical representation of two-layer surface films
consisting of a barrier-type inner layer and a relatively porous
coated outer layer [26 28].
Very good agreement between the simulated and
experimental data was obtained. The values of the

impedance parameters determined from the fits are

presented in tables 1 and 2 for the uncoated and coated
stainless steel orthodontic wires, respectively.
For the uncoated and coated stainless steel orthodontic
wires, the parameters R1 and Q1 account for the reactions
at the stainless steel orthodontic wires layer/solution
interface and determine the impedance behavior in the
high frequency range of the spectrum. The constant phase
element Q 1 represents the double layer pseudocapacitance of the stainless steel layer, as shown by the
high value of the n1 exponent [29].
Corrosion may occur in pores as the result of the directly
metal expose to the aggressive attack of the electrolyte.
Pores in the coating layer may act as paths for the
electrolyte attack to the substrate.
Therefore for coated stainless steel orthodontic wires,
the parameters R2 and Q2 describe the properties of the
PTFE layer.
As immersion time increases from 1 hour to 8 h , the
resistance (R2) of the PTFE coated layer decreases slowly.
However, the values of R2 are about 10 times bigger than
those of R1 for all time exposures, which revealing that
PTFE coated layer provides most of the corrosion protection
to the stainless steel orthodontic wires. Therefore, the
performance of the PTFE coated stainless steel orthodontic

Table 3
pH AND PROXIMATE
COMPOSITION VALUES
OF THE PASTE FROM TUNA
FISH MEAT CANS SAMPLES
DURING 8 HOURS STORAGE

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REV.CHIM.(Bucharest) 67No. 4 2016

wires in the both fish products was superior to that of the

uncoated material.
Therefore, both type (coated and uncoated) of stainless
steel orthodontic wires presented higher corrosion
resistance values in the paste of tuna filet in sunflower oil.
In the case of fish product containing tuna meat and
sunflower oil, the formation (hypothetically) of a fully
covered oil film would prevent corrosion [30-31] of the
stainless steel surface by separating the water phase, salt
and the others main biochemical compounds of the tuna
fish meat (table 3) Practically, when the paste of tuna fish
in oil was prepared by well blending the cans content, the
water phase was embedded into the oil phase, and the
resulted stable emulsion, that showed non significant
changes of the proximate composition during 8 hours
storage (table 3) exerted an inhibitory effect on the
corrosion process [32-33].
In the case of the paste of tuna filet in brine, the smaller
corrosion resistance values registered for both type of
stainless steel orthodontic wires can be explained by the
enhanced corrosive effect of sodium chloride [34] and citric
acid from the brine aqueous solution [30].
Semi-logarithmic plots between -1000 mV and 1000
mV vs. SCE of the uncoated stainless steel wires in both
tunafish derived products are displayed in figures 10-11.
The zero current potential (ZCP) and corrosion current
(jcorr) values were determined by Tafel analysis of both the
anodic and cathodic branches of the polarization plots. The
ZCP is defined as the potential at which the current reaches
a minimum during the for ward potentiodynamic

polarization scan. As a result of the coated samples, the

zero-current potential of the uncoated stainless steel
orthodontic wires was shifted towards a more noble value
in both paste of tuna filet products.
The corrosion current is representative for the
degradation degree of each sample. The average values of
ZCP and jcorr determined from the polarization curves are
presented in tables 4 and 5.
Corrosion may occur in pores as the result of the metal
being directly exposed to the aggressive attack of the
electrolyte. Data from figures 10-11 reveals an evident
decrease of the anodic current for the coated stainless
steel orthodontic wires as compared with the uncoated
ones. This fact proves that the coated sample has a greater
corrosion resistance compared to uncoated sample, which
determine the correspondently smaller measured values
of the corrosion current densities. Low corrosion current
density values were obtained from the potentiodynamic
polarization curves of investigated samples in the paste of
the tuna filet in sunflower oil. These results are in agreement
with EIS data.
The susceptibility of an alloy to pitting corrosion in a
certain medium [35] can be characterized in terms of the
breakdown potential (Ebd) relative to the zero-current
potential value (ZCP). The potential range situated
between ZCP and Ebd represents the passivity zone in which
the corrosion rate is low or even insignificant. As the
difference between Ebd and ZCP becomes smaller, the alloy
is expected to become more susceptible to pitting

Fig. 10. Potentiodynamic polarization curves for coated and

uncoated stainless steel orthodontic wires in the paste of tuna filet
in sunflower oil

Fig. 11. Potentiodynamic polarization curves for coated and

uncoated stainless steel orthodontic wires in the paste of tuna filet
in brine

Table 4
THE MEAN VALUES OF
ELECTROCHEMICAL
PARAMETERS MEASURED
AND CALCULATED
FOR THE PASTE OF TUNA
FILET IN SUNFLOWER OIL
(37 OC)
Table 5
THE MEAN VALUES OF
ELECTROCHEMICAL
PARAMETERS MEASURED
AND CALCULATED
FOR THE SAMPLES IN TUNA
FILET IN BRINE (37 OC)

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805

Fig. 12. Surface attack morphology

after potentiodynamic polarization of
the uncoated stainless steel
orthodontic wires in the paste of tuna
filet : (a) in brine, and (b) in
sunflower oil

Fig. 13. Surface attack morphology

after potentiodynamic polarization
for the coated PTFE stainless steel
orthodontic wires in the paste of
tuna filet: (a) in brine, and (b) in
sunflower oil

corrosion. Also, the area of hysteresis loop (Qhysteresis) reflects

the susceptibility to localized corrosion.
The analysis of the potentiodynamic polarization curves
proved that the uncoated stainless steel alloy exhibited a
more area of hysteresis loop and a more negative
breakdown potential value than coated stainless steel
orthodontic wires. These results indicating that uncoated
stainless steel orthodontic wires exhibited a greater
susceptibility to localized corrosion, are consistent also with
the conclusions derived from Qhysteresis presented above.
A comparison with other published is not applicable in
this case, since the corrosion and anodic current densities
of stainless steel orthodontic wires depend on potential
scanning rate, surface preparation or exposure time.
However, our results sustain the recommendation of
caution against consumption of products derived from
tuna filet in brine for patients with stainless steel orthodontic
wires.
The surface morphologies of coated and uncoated
stainless steel orthodontic wires polarized at +1 V in the
paste of tuna filet in sunflower oil and in brine were
examined by scanning electrochemical microscopy (SEM).
The analysis of figures 12-13 indicated the appearance
of localized corrosion at the surface of coated and uncoated
stainless steel orthodontic wires. The localized corrosion
at surface of both coated and uncoated stainless steel
orthodontic wires was evident, even the morphology of
the electrochemically polarization tests was extremely
irregular.
Conclusions
Low corrosion current densities of the potentiodynamic
polarization curves for the coated stainless steel
orthodontic wires showed more positive zero current (ZCP)
and breakdown (Ebd) potentials than the uncoated stainless
steel orthodontic wires. However, the PTFE protective layers
from the surface of stainless steel orthodontic wires are
prone to localized breakdown in both tuna filet products as
characterized by the measurement of pitting corrosion
potential chloride-containing solutions. The EIS spectra of
the coated stainless steel samples in the paste of tuna filet
exhibited two time constants: the first accounting for the
characteristic reactions at the stainless steel layer/solution
806

interfaces, and the second corresponding to the PTFE

coated layer . The experimental potentiodynamic
polarization curves, EIS diagrams, and the equivalent circuit
parameters showed that the coated stainless steel
orthodontic wires in both tuna filet products presented good
electrochemical corrosion resistance .
Acknowledgements: This work was supported by the Romanian
National Authority for Scientific Research, CNCS-UEFISCDI (project
number PN-II-IDPCE-2011-3-0218).

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Manuscript received: 3.10.2015

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