ONLINE ONLY

Martensitic transformation of austenitic stainless

steel orthodontic wires during intraoral exposure
Paula P. Izquierdo,a Ronaldo S. de Biasi,b Carlos N. Elias,b and Lincoln I. Nojimaa
Rio de Janeiro, Brazil

Introduction: Our purpose was to study the mechanical properties and phase transformations of orthodontic
wires submitted to in-vivo exposure in the mouth for different periods of time. Methods: Stainless steel wires
were tied to fixed orthodontic appliances of 30 patients from the orthodontics clinic of Universidade Federal do
Rio de Janeiro School of Dentistry in Brazil. According to the duration of the clinical treatment, the patients
were divided into 3 groups. After in-vivo exposure, the samples were studied by mechanical testing
(torsion) and ferromagnetic resonance. Statistical analyses were carried out to evaluate the correlation
between time of exposure, mechanical properties, and austenite-to-martensite transformation among the
groups. Results: The results were compared with as-received control samples. The torque values
increased as time in the mouth increased. The increase in torque resistance showed high correlations with
time of exposure (P 5 0.005) and austenite-martensite phase transformation. Conclusions: The resistance
of stainless steel orthodontic wires increases as the time in the mouth increases; this effect is attributed to
the austenite-to-martensite transformation. (Am J Orthod Dentofacial Orthop 2010;138:714.e1-714.e5)

A
ustenitic stainless steels are known to undergo
a partial transformation to martensite when
subjected to plastic deformation.1,2 This
transformation has been shown to be a function of
temperature, microstructure, chemical composition,
cumulative strain, and strain rate.3 However, as far as
we know, partial transformation to martensite as a conse-
quence of exposure to the oral environment during
orthodontic treatment has not been investigated. Aus-
tenitic stainless steels have been used for some decades
in orthodontic wires and appliances because of their
good combination of mechanical properties and
biocompatibility. Orthodontic treatment consists of
using and controlling forces acting on teeth and adjacent
tissues. Such forces are clinically induced by orthodon-
tic appliances such as wires, brackets, elastics, and
springs.4 Orthodontic treatment results depend on the
a
Graduate student, Departamento de Ortodontia, Universidade Federal do Rio
de Janeiro, Rio de Janeiro, Rio de Janeiro, Brazil.
b
Professor, Instituto Militar de Engenharia, Rio de Janeiro, Rio de Janeiro,
Brazil.
The authors report no commercial, proprietary, or financial interest in the
products or companies described in this article.
Based on a thesis submitted by Paula P. Izquierdo to the graduate faculty of
Universidade Federal do Rio de Janeiro in partial fulfillment of the requirements
for the master of science degree. Supported by CNPq and CAPES Brazilian
Government (Process 472449/2004-4, 400603/2004-7 e 500126/2003-6) and
FAPERJ (Process E-26/151. 970/2004).
Reprint requests to: Carlos N. Elias, Laboratório de Biomateriais, Departamento
de Engenharia Mecânica e de Materiais, Instituto Militar de Engenharia, Praça
General Tibúrcio, 80, Praia Vermelha, 22290-270 Rio de Janeiro, Rio de Janeiro,
Brazil; e-mail, elias@ime.eb.br.
0889-5406/$36.00
Copyright Ó 2010 by the American Association of Orthodontists.
doi:10.1016/j.ajodo.2010.05.015
control of the applied force.5 Consequently, when de-
signing and preparing each appliance, a clinician must
be able to predict its response during treatment. How-
ever, the materials are subjected to mechanical actions
and the environment in which they function for varying
time periods; these can influence clinical behavior.5
Stainless steels are iron-based alloys that contain chro-
mium and nickel. Chromium improves corrosion resis-
tance, forming a thin, adherent, passive surface
chromium oxide layer. When deprived of this protec-
tion, stainless steel can suffer strong corrosive attacks.
Nickel is responsible for austenite stabilization at
room temperature, which increases steel’s toughness.
The mechanical properties of materials that must with-
stand the oral environment are also of concern. Bending
the wires into a desired shape causes plastic deformation
and induces work hardening, resulting in preferential
areas for stress concentration. Complex loading derived
from engaging activated wires into bracket slots and
masticatory loads is known to exert heavy stresses on
the material.6
Some reports show that retrieved archwires had
much higher fracture incidence than expected from lab-
oratory experiments, which suggested that the archwires
would be almost unbreakable.7,8 This can be due to
several factors, including intraoral aging of wires.
This evidence suggests that research approaches with
in-vitro methodologies might not adequately model
in-vivo phenomena.9 Despite much evidence from or-
thodontic materials research, an in-vitro methodology
cannot accurately reproduce the complex oral environ-
ment. Retrieval analyses provide critical information
714.e1
714.e2 Izquierdo et al
Fig 1. Model of stainless steel sample tied in the ortho-
dontic appliance.
derived from investigating the performance of the mate-
rial in vivo.6 The aim of this study was to characterize
the effects of increasing the time of in-vivo exposure
in the oral cavity on the mechanical properties of stain-
less steel archwires.
MATERIAL AND METHODS
We selected for this study a stainless steel type 304
orthodontic archwire (batch number 0540017, TP Ortho-
dontics, LaPorte, Ind). The wires were straight, 180-mm
long, and retangular with an 0.018 3 0.025-in (0.45 3
0.625 mm) cross section. A sample specimen was created
by using 40 mm of as-received wire and bending a loop
stop about halfway in its length. The height of the loop
was 3 mm. The sample was reproduced by using Vision
software (Microsoft Corporation, Redmond, Wash) and
printed as a real-size template for standardizing the shape
of 35 specimens (Fig 1). Part of the wire more susceptible
to phase transformation was about 1.0 cm from the cen-
tral loop; the excess length at the edges allowed for clin-
ical adjustments while tying it to a patient’s appliances.
All samples were taken from the same batch of
wires and prepared by the same operator (P.P.I) using
the same pliers. The 35 specimens were separated in 4
groups (1 control and 3 experimental groups). The con-
trol group consisted of 5 specimens of the same size, and
equal loop stops and shapes as the experimental ones of
as-received wires, having no interaction with the oral
environment throughout the trial period. The experi-
mental group consisted of 30 wire specimens that
were subjected to the oral environment of 30 patients
randomly chosen from the orthodontics clinic of the
Universidade Federal do Rio de Janeiro in Brazil. This
American Journal of Orthodontics and Dentofacial Orthopedics
December 2010
Fig 2. Orthodontic appliance in a patient’s mouth.
group was divided into 3 subgroups according to the
time of exposure in the mouth: 1, 2, or 3 months. The
patients were allocated at random to each subgroup.
All participants were undergoing corrective orthodontic
treatment, which allowed for specimens to be tied by
their edges to the patient’s fixed appliances by using
stainless steel 0.010-in (0.24 mm) ligatures and ligature
cutters (Fig 2). In all participants, the specimens were
placed by the same author (P.P.I.) in the maxillary
arch on the right side. This research proposal was
approved by the Research Ethics Committee of the
Universidade Federal do Rio de Janeiro (number 87/
2007). An informed consent form was signed by all
30 patients or their legal representatives. At the end of
the clinical period, each experimental specimen was re-
moved with a ligature cutter and tweezers, and placed
on a sterile tray with the inner surface that had been
turned to the teeth facing up. Before mechanical testing
in the laboratory, all experimental and control speci-
mens were placed in an ultrasound cleaner with enzyme
detergent Endozyme (DFL, Petrópolis, Rio de Janeiro,
Brazil) for 20 minutes. This substance proved ineffec-
tive in removing gross debris from the specimens, so
the procedure was repeated with a multiuse detergent
(Amway, Ada, Mich) for 1.5 hours. After in-vivo
clinical time, all samples were subjected to mechanical
torque testing.
Torque testing is a simple mechanical test. The test
consists of twisting a specimen at a defined rate to
a prescribed strain or twist, to failure or angle. Figure 3
shows the torque testing device developed by our research
team.10,11 This apparatus held a specimen by both ends,
with 5 mm of wire from the central loop. One end was
fixed, and the other was free to rotate, connected to
a universal testing machine with a load cell of 50 N
(DL10.000, EMIC, Sao José dos Pinhais, Paraná,
American Journal of Orthodontics and Dentofacial Orthopedics Izquierdo et al 714.e3
Volume 138, Number 6

Fig 3. Device for toque testing.

Brazil). The force required to twist specimen by 15
in Table. Torque and FMR results for all groups
torsion was measured. The twist was done at a constant Minimum Maximum Average FMR line
speed of 100 rpm. A 10-cm long rectangular stainless torque torque torque intensity
steel wire with a cross section of 0.018 3 0.025 in (0.45 Group (gf.mm) (gf.mm) (gf.mm) (A.U.)
3 0.625 mm) was fixed to the rotating axis, serving as Control (n 5 5) 738 779 755 4.5
a pointer. A conventional protractor was scanned, Experimental 1 (n 5 10) 749 810 768 5.0
printed, and positioned behind the experimental setup; as Experimental 2 (n 5 10) 765 863 810 6.0
testing began, the pointer turned, and the test was Experimental 3 (n 5 10) 825 980 905 9.0
stopped after a 15
displacement, when force readings A.U., arbitrary units.
were taken in gram-force (gf) units. The output data was
force (gf) against twist. But, in principle, the torsion test
data are torque-twist curves. To convert the results to tor- RESULTS
que (gf.mm), the force (gf) readings were multiplied by The torque needed to produce a 15
rotation on the
the radius of the rotating axis (5 mm) and registered in a Mi- wires in the control group ranged from 738 to 779
crosoft Excel spreadsheet (Microsoft) in gf per millimeter gf.mm, with an average of 755 gf.mm. In experimental
units (gf.mm). group 1 (wires in the mouth for 1 month), results ranged
The torsion test simulated the most common clinical from 749 to 810 gf.mm, with an average of 767.5
situation, when we apply torque in a rectangular ortho- gf.mm. In group 2 (wires in the mouth for 2 months), re-
dontic archwire during the last treatment phase. The sults ranged from 765 to 863 gf.mm, with an average of
orthodontic arch of the last stage has loop or omega in 810 gf.mm. In group 3 (wires in the mouth for 3
the region of molars. The tested samples were fixed in months), results ranged from 825 to 980 gf.mm, with
the region of the molars of the orthodontic appliances. an average of 905 gf.mm. These results are shown in
The sample design simulated the region of the archwire, the Table; the statistical analysis results between torque
which normally receives torque in the final stage of and time of exposure was P 5 0.01.
orthodontic treatment. Typical FMR spectra of samples in the control group
In this study, complete data of all parameters, includ- and the 3 experimental groups are shown in Figure 4.
ing descriptive statistics and statistical models, were The FMR line intensity increased with the time of expo-
evaluated. The mechanical and magnetic properties sure in the mouth. The intensity values shown in the
results were analyzed with SPSS statistical software Table are the averages for the same samples used in
(version 13, SPSS, Chicago, Ill). An alpha level of the torsion tests; the FMR spectra were recorded before
0.05 was chosen to determine the statistical significance. the torsion tests. Figure 5 shows the correlation between
Post-hoc multiple comparisons were performed by using torque and martensite volume fraction (FMR line inten-
Bonferroni adjustments for significant tests. sity) after wire exposure in the mouth for different
First-derivative ferromagnetic resonance (FMR) periods of time.
spectra were recorded at room temperature and 9.50
GHz by using a Varian E-12 spectrometer with
100-kHz field modulation (Varian, Inc., Santa Clara, DISCUSSION
Calif). FMR line intensity was computed by double in- Three of the most frequently used materials for
tegration of the first derivative absorption spectrum. orthodontic treatment with fixed appliances are
714.e4 Izquierdo et al
Fig 4. FMR spectra of samples of the control group and
3 experimental groups: a, control group (as received);
b, experimental group 1; c, experimental group 2;
d, experimental group 3.
stainless steel, beta-titanium (also known as titanium-
molybdenum alloy), and nickel-titanium alloys.
More than 120 different compositions of stainless
steel are available for many applications and in various
fields. The alloy of stainless steel most frequently used
in medical practice is a modified American Iron and
Steel Institute (AISI) type 316L. According to the
standards of the American Society for Testing and
Materials, F138, the modified AISI type 316L alloy,
contains chromium, nickel, molybdenum, and small
amounts of phosphorous and sulfur. The change in the
chemical composition of F138 stainless steel increases
its resistant to pit corrosion, which is higher than AISI
type 304 used for orthodontic materials. The F138 and
304 alloys are austenitic stainless steels.
Austenitic stainless steels are susceptible to mar-
tensitic transformation by plastic deformation, subzero
cooling, subzero deformation, hydrogen charging, ion
implantation, and magnetron sputtering.1-3 Metastable
austenitic steels (for example, AISI 301, 302, 304,
304L, 316, and 316L) might form martensites 3
(hexagonal close packed, paramagnetic) and a0 (body
centered cubic, ferromagnetic), and stable steels (eg,
AISI 310) might form only martensite 3 induced by
plastic deformation. The a0 martensitic transformation
increases the work-hardening rate during deformation.
When the orthodontic appliance is made of austenitic
American Journal of Orthodontics and Dentofacial Orthopedics
December 2010
Fig 5. Torque and FMR intensity as functions of the time
of exposure in the mouth. The straight lines are only
guides to the eye.
steel and the austenite phase transforms to the martensite
phase, the appliance’s mechanical properties change
also. Despite a lack of information, stainless steel is
the considered a reference material for orthodontic
wire alloys. The amount of martensite a0 formed in an
austenitic stainless steel can be measured by x-ray
diffraction and magnetic measurements. In this study,
we used the FMR method to analyze the influence of de-
formation on martensite a0 transformation in stainless
steel orthodontic wires during orthodontic treatment.
The results show that the torque needed for a 15
rotation
increases with the exposure time in the mouth: control
group, 755 gf.mm \ group 15 767 gf.mm \ group
2 5 810 gf.mm \ group 3 5 905 gf.mm. As a result,
a decrease in ductility can be expected; this is in often
undesirable and might be accompanied by a tendency
to fracture. In a study of 304-stainless steel, martensite
formation was observed at room temperature.12 This
phase has increased hardness when compared with
austenite; this would explain the increase in torque resis-
tance. Another finding that would point toward martens-
itic transformation is the observation of magnetic
behavior after exposure to the oral environment. Clini-
cians should bear in mind that used materials might
have different mechanical behavior than as-received
specimens. It is not yet fully understood how an increase
in the archwire exposure could explain the higher resis-
tance provided by the wires in torque. Perhaps changes
occurring on the wire structure act as barriers to form-
ability, similar to those in cold-worked metal specimens.
The effects of aging on mechanical properties are not
well established and seem to vary according to the meth-
odology applied. Studies indicate that using topical fluo-
ride agents with beta titanium and stainless steel wires
could decrease the functional unloading mechanical
American Journal of Orthodontics and Dentofacial Orthopedics
Volume 138, Number 6
properties of the wires and potentially contribute to pro-
longed orthodontic treatment.13 It was observed that
used nickel-titanium orthodontic wires have lower
fatigue fracture resistance than as-received wires.14 In
contrast, another study showed that despite the obvious
alteration of the surface through pitting corrosion on re-
trieved nickel-titanium wire surfaces, no major effects
on the mechanical properties of the wires were identified
clinically.7,15 Ferromagnetic resonance measurements
also suggest an austenite-to-martensite transformation,
since the intensity of the resonance line, which is propor-
tional to the volume fraction of martensite, increases
with the time of exposure in the mouth.16 When FMR
line intensity and torque are plotted in the same graph
as functions of the time of exposure in the mouth
(Fig 4), one sees similar trends. Future research should
continue to approach in-vivo methodologies, further
addressing the potential changes in the mechanical prop-
erties of intraorally aged materials.
CONCLUSIONS
The behavior of stainless steel 304 orthodontic wires
during intraoral exposure was investigated by using
torque testing and magnetic measurements. The results
showed that (1) the stainless steel wire resistance to torque
increases with the time of intraoral exposure, (2) the FMR
line intensity increases with the time of exposure in the
mouth, and (3) both results suggest that resistance to twist
increases because the volume fraction of martensite
increases with the time of exposure in the mouth.
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