d e n t a l m a t e r i a l s 2 5 ( 2 0 0 9 ) 1039–1043

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Nanoindentation of orthodontic archwires: The effect of

decontamination and clinical use on hardness, elastic
modulus and surface roughness

Joseph P. Alcock a , Michele E. Barbour b , Jonathan R. Sandy a , Anthony J. Ireland a,∗

a Division of Child Dental Health, Bristol Dental School, University of Bristol, Bristol, UK
b Biomaterials Science, Bristol Dental School, University of Bristol, Bristol, UK

a r t i c l e i n f o a b s t r a c t

Article history: Objectives. The purpose of this research was to investigate the effects of decontamination and
Received 18 August 2008 clinical exposure on the elastic moduli, hardness and surface roughness of two frequently
Received in revised form used orthodontic archwires, namely 0.020 in. × 0.020 in. heat activated (martensitic active)
19 February 2009 nickel titanium archwires and 0.019 in. × 0.025 in. austenitic stainless steel archwires.
Accepted 10 March 2009 Method. This study was a prospective clinical trial in which 20 consecutive patients requiring
an archwire change as part of their course of orthodontic fixed appliance therapy, had either
a nickel titanium or stainless steel archwire fitted as deemed clinically necessary. The effect
Keywords: of clinical use was determined by comparing distal end cuts of the “as received” archwires
Orthodontics before and after decontamination, with the same retrieved archwires following clinical use
Archwires and decontamination. Hardness, elastic modulus and surface roughness were determined
Nickel titanium using an atomic force microscope (AFM) coupled with a nanoindenter.
Stainless steel Results. The results showed that the decontamination regimen and clinical use had no sta-
Atomic force microscopy tistically significant effect on the nickel titanium archwires, but did have a statistically
Nanoindentation significant effect on the steel archwires. Decontamination of the steel wires significantly
increased the observed surface hardness (p = 0.01) and reduced the surface roughness
(p = 0.02). Clinical use demonstrated a statistically significant increase in the observed elastic
modulus (p < 0.001) and a decrease in surface roughness (p = 0.001).
Significance. At present it is difficult to predict the clinical significance of these statistically
significant changes in archwire properties on orthodontic tooth movement.
© 2009 Published by Elsevier Ltd on behalf of Academy of Dental Materials.
All rights reserved.

1. Introduction main choice for the orthodontist, when assessing mechanical

Historically orthodontic archwires have mainly comprised
austenitic stainless steel, the mechanical properties of which
are largely determined by the manufacturer. This can be
through minor changes in the constituent alloy or by the
processes of heat treatment and, or work hardening. The
mechanical properties might vary to a small degree, but the
properties for use during treatment, is based on cross-
sectional shape and size of the wire. Since the 1980s nickel
titanium alloys have predominated for all but the latter
stages of treatment with orthodontic fixed appliances, and
three types are available, namely: martensitic stable (clas-
sic), austenitic active (super or pseudo elastic) and martensitic
active (thermally active or heat activated). Although the

∗
Corresponding author. Tel.: +44 117 928 4355.
E-mail address: Tony.Ireland@bristol.ac.uk (A.J. Ireland).
0109-5641/$ – see front matter © 2009 Published by Elsevier Ltd on behalf of Academy of Dental Materials. All rights reserved.
doi:10.1016/j.dental.2009.03.003
1040 d e n t a l m a t e r i a l s 2 5 ( 2 0 0 9 ) 1039–1043
orthodontist can still choose wires with differing cross-
sectional shapes and dimensions, mechanical properties vary
greatly with alloy composition and heat treatment during
manufacture. This is to the degree that variable modulus
orthodontics is now practised rather than just variable shape
and dimension [1]. Elastic modulus determines archwire stiff-
ness and hence strength, springiness and range. This, along
with other variables including surface hardness and rough-
ness will affect frictional forces between the archwire and
bracket, and hence tooth movement [2]. Surface roughness
will also influence corrosion [3,4], biocompatibility [4,5] and
the appearance of the wire [6].
The more recently introduced thermally active nickel tita-
nium wires undergo phase transformations over a useable
and specified temperature range, or transition temperature
range (TTR). The crystal structure changes from austenitic
to martensitic on heating and cooling and the force per unit
deflection of the wire therefore changes with temperature. In
addition to the orthodontist utilising this property to facilitate
wire engagement, when the TTR is around mouth tempera-
ture, everyday eating and drinking activities by the patient will
also affect crystal structure and therefore the force applied by
the wire. Some of these effects can be prolonged rather than
precise and predictable short term events [7], which may have
implications for the long term use of such wires.
Traditionally the mechanical and physical properties of
archwires have been measured separately using a variety of
techniques, including three-point bend tests, tensile tests,
Rockwell and Vickers hardness test methods. Surface rough-
ness has been assessed using surface profilometry, various
optical methods and by atomic force microscopy (AFM).
However, it is possible to measure all three properties simul-
taneously using an AFM, if combined with a nanoindenter.
Nanoindentation simply being an indentation test in which
the depth of the indent is in the order of nanometres (m10−9 ).
This technique allows simultaneous quantitative measure-
ments of hardness and elastic modulus [8] and when coupled
to an AFM, surface roughness is also recorded. Nanoindenta-
tion as a means of characterising orthodontic archwires is a
relatively new technique and was first reported by Alcock et
al. [9].
If predictable forces are to be delivered to the teeth by
orthodontic archwires then clinicians should be aware of any
effect that clinical exposure might have on both the physical
and mechanical properties of orthodontic archwires. To date
the effect of temperature variation on the properties of nickel
titanium archwires has been confined to the laboratory set-
ting. The aim of this pilot clinical study was to determine the
effect of intraoral exposure on the physical and mechanical
properties of stainless steel and heat activated nickel titanium
archwires. In particular the elastic modulus, surface hardness
and surface roughness.
2. Materials and methods
Prior to starting patient recruitment for this research project,
ethical committee approval was obtained from the Salisbury
and South Wiltshire Local Research Ethics Committee (REC
number 06/Q2008/26). Twenty consecutive patients who ful-
filled the inclusion criteria were asked to participate in this
study. The inclusion criteria were as follows:
Patients undergoing upper and lower fixed appliance ther-
apy using 0.022 in. preadjusted edgewise appliances and who
required the insertion of either of the following wires:
• 0.019 in. × 0.025 in. stainless steel
• 0.020 in. × 0.020 in. heat activated nickel titanium
At the appointment where the archwire was to be fit-
ted this was done as per normal clinical practice. The
wire samples consisted of one randomly selected packet of
0.020 in. × 0.020 in. heat activated nickel titanium and one
packet of 0.019 in. × 0.025 in. stainless steel. Each packet con-
tained ten archwires from a single batch. In the case of each
patient, where these wires were fitted, the excess wire at the
distal end was retained, cataloged and placed into a plastic
bag at room temperature for storage until testing. Ten dis-
tal end cuts from the preformed 0.019 in. × 0.025 in. stainless
steel archwires (GAC International, Bohemia, NY, USA) and ten
distal end cuts from the preformed 0.020 in. × 0.020 in. nickel
titanium orthodontic archwires (GAC International, Bohemia,
NY, USA) were collected in this way.
Following clinical exposure of the remainder of the wire
(minimum 49 days, maximum 204 days, average 91 days), the
inserted archwires were retrieved, cataloged and also placed
into plastic bags, again at room temperature, prior to testing.
Once collected the end cuts and the clinically exposed arch-
wires were decontaminated using the following regimen:
• Immersion in a 2% solution of sodium dodecyl sulphate
(SDS) while placed in an ultrasonic water bath for 5 min.
• Wiped for 1 min with cotton buds soaked in SDS.
• Rinsed with distilled water for 20 s.
• Immersed in a 70% solution of ethanol for 2 min.
• Air dried.
The purpose of this decontamination regimen was to
remove any biofilm contaminants prior to placement in the
AFM. The distal end cuts were tested in the AFM, both before
and after exposure to the same decontamination regimen, in
order to determine the effect on the mechanical and physical
properties.
Incisor sections (the length of archwire between 0 mm and
8.5 mm from the midline) were cut from the clinically retrieved
archwires for testing. Previous work [10] had found there to be
little variation in measured properties throughout individual
archwires. These clinically used sections and the correspond-
ing distal end cut specimens were then glued to AFM stubs
and mounted in the AFM for testing.
Nanoindentation was performed in air under ambient con-
ditions (room temperature ranged between 28 ◦ C and 32 ◦ C)
using a Berkovich nanoindentation tip (TI-039, Hysitron Inc.,
Minneapolis, MN, USA) attached to a Hysitron Triboscope
nanoindenter (Hysitron, Minneapolis, MN, USA) which was
mounted on a Nanoscope IIIa AFM (Digital Instruments, Santa
Barbara, CA, USA). The Berkovich tip had a tip angle of 142◦
and a tip radius of approximately 100–200 nm. The precise
shape of the tip was calibrated prior to use by using a mate-
rial of known elastic modulus, namely fused quartz. The load
 d e n t a l m a t e r i a l s 2 5 ( 2 0 0 9 ) 1039–1043 1041

Table 1 – Results for hardness (GPa).

Wire Treatment Obs Mean Median SD Min Max 95% CI of median Shapiro-Wilks W

NiTi Predecontamination 50 2.36 2.26 0.51 1.05 4.19 2.23–2.40 0.014

Postdecontamination 50 2.42 2.5 0.84 0.33 3.67 2.15–2.79 0.038
Post-treatment 50 2.61 2.62 1.08 0.57 6.03 2.43–2.76 0.011

Steel Predecontamination 50 4.13 4.14 1.18 1.74 6.53 3.76–4.43 0.890

Postdecontamination 50 5.11 5.21 2.10 1.26 9.78 4.27–6.05 0.435
Post-treatment 50 5.96 5.90 1.58 1.38 9.72 5.44–6.68 0.732

cycle was carried out over 50 s and comprised a constant speed
loading segment (400 ␮N/s, 20 s), a hold segment at the peak
load (8000 ␮N, 10 s) and a constant speed unloading segment
(400 ␮N/s, 20 s).
Each wire section, i.e. used incisor sections following
decontamination and unused distal ends both before and after
decontamination, was indented five times at widely separated
intervals (>1 mm spacing between indents). No indentations
were made near the cut ends in case sectioning had affected
mechanical properties. Data from exposed incisor sections
and unexposed end cut sections were compared in order to
determine whether decontamination and also clinical expo-
sure had altered the nanomechanical properties of these
archwires. The wire surface was imaged using the nanoin-
denter tip before each indentation in order to ensure that the
surface was free from debris. In order to do this, the AFM was
operated in contact scanning mode and using the Berkovich
tip rather than a conventional AFM tip. The image obtained
was therefore a convolution of the surface features of the wire
and the triangular shape of the tip. Although the resolution
is lower than that which would be offered by a conventional
AFM tip, it allows the user to obtain a clear image of the sur-
face at and surrounding the indent site, and to check for debris,
surface cracks or scratches. In the rare event that debris was
observed, the area was not indented and the tip was relocated
to a clean area of the wire.
Hardness and reduced elastic modulus were calculated
using the Hysitron software [8] and the average surface
roughness (Ra ) was calculated using SPIPTM v.4.7.2 software
(Nanoscience Instruments, Inc., Phoenix, AZ, USA).
3. Results
The data were analyzed using Stata Version 10 (Stata Corp, Col-
lege Station, Texas) with a predetermined level of significance
of ˛ = 0.05. Summary data for hardness, elastic modulus and
surface roughness are illustrated in Tables 1–3. In all cases the
residuals were tested for normality using the Shapiro–Wilks
W test and in virtually all instances were not found to
be normally distributed. The data were subsequently ana-
lyzed using the Kruskal Wallis one way analysis of variance,
Mann Whitney tests and boxplots. As this was a pilot study
no formal power calculation was used to determine sample
size.
When considering the effect of the decontamination reg-
imen and also clinical usage on the heat activated nickel
titanium wire, there was no significant effect on the measured
hardness (p = 0.22), elastic modulus (p = 0.24) or on the surface
roughness (p = 0.71) when analyzed using the Kruskal Wallis
one way analysis.
In the case of the stainless steel wires, there were sig-
nificant effects of decontamination and usage on hardness
(p < 0.001), elastic modulus (p < 0.001) and surface roughness
(p < 0.001).
With respect to observed surface hardness the Mann Whit-
ney test demonstrated the decontamination regimen to have
a statistically significant effect on stainless steel (p = 0.01),
whereas clinical use had no statistically significant effect on
hardness (p = 0.06). The summary data (Table 1) and the box-
plot (Fig. 1) indicate an increase in surface hardness with
decontamination which continued, albeit to a lesser degree,
with clinical use.
The Mann Whitney test indicated no statistically signif-
icant effect on the elastic modulus of stainless steel as a
result of the decontamination regimen (p = 0.08), but a statis-
tically significant effect as a result of clinical use (p < 0.001).
Consideration of the summary data (Table 2) and the boxplot
(Fig. 2) would suggest the decontamination regimen reduces
the observed elastic modulus measured at the surface of the
wire, but that clinical use increases the elastic modulus.
Finally, the Mann Whitney test indicated statistically sig-
nificant reductions in the measured surface roughness (Ra )
following both decontamination (p = 0.02) and clinical use

Table 2 – Results for modulus of elasticity (GPa).

Wire Treatment Obs Mean Median SD Min Max 95% CI of median Shapiro-Wilks W

NiTi Predecontamination 50 71.46 69.55 13.29 36.3 99.1 67.25–75.40 0.465

Postdecontamination 50 67.08 67.6 11.65 37.3 93.9 63.21–72.59 0.642
Post-treatment 50 68.36 69.05 13.01 37.9 102.3 64.93–71.9 0.438

Steel Predecontamination 50 229.36 212.35 54.25 149.7 371.6 203.44–225.46 0.002

Postdecontamination 50 207.22 203.9 53.28 107.4 397.9 184.28–223.49 0.021
Post-treatment 50 260.53 250.2 45.09 184.1 385.1 241.97–266.65 0.074
1042 d e n t a l m a t e r i a l s 2 5 ( 2 0 0 9 ) 1039–1043

Table 3 – Results for surface roughness (Ra ).

Wire Treatment Obs Mean Median SD Min Max 95% CI of Median Shapiro-Wilks W

NiTi Predecontamination 50 41.93 38.2 17.96 16.4 91.9 32.72–44.43 0.001

Postdecontamination 50 39.33 34.55 18.53 14.3 114 29.86–39.09 0.001
Post-treatment 50 42.69 37.35 24.18 14.3 151 30.75–43.53 0.001

Steel Predecontamination 50 25.76 25.05 7.95 13.5 49.8 21.32–29.6 0.032

Postdecontamination 50 22.38 21.9 9.58 6.67 57.8 17.73–25.5 0.001
Post-treatment 50 16.48 15.85 5.96 6.24 28.7 14.65–18.3 0.346

Fig. 1 – Boxplot of hardness of nickel titanium and

stainless steel wires (GPa), prior to decontamination Fig. 3 – Boxplot of surface roughness (Ra ) of nickel titanium
unused (1), postdecontamination unused (2) and and stainless steel wires prior to decontamination unused
post-clinical use and postdecontamination (3). (1), postdecontamination unused (2) and post-clinical use
and postdecontamination (3).

(p = 0.001) of the stainless steel. This is illustrated by the sum-

mary data in Table 3 and the boxplots (Fig. 3).
4. Discussion
In order to determine the true effect of clinical exposure
on archwire properties, the effect of the decontamination
Fig. 2 – Boxplot of elastic modulus of nickel titanium and
stainless steel wires (GPa), prior to decontamination
unused (1), postdecontamination unused (2) and
post-clinical use and postdecontamination (3).
regimen alone was investigated. Previous work has shown
intra-archwire variations in the properties of hardness, elastic
modulus and surface roughness of as received orthodon-
tic wires to be statistically insignificant [10]. Therefore any
observed differences in mechanical properties between the
control group (distal end cuts) and the retrieved specimens
(incisor section from the same archwire) can be assumed to
have occurred as a result of either the decontamination regi-
men, clinical exposure or the combination of the two.
The decontamination regimen was found to have the
following effects on the nickel titanium archwires; mean hard-
ness was found to have increased by 2.49% (from 2.36 GPa to
2.42 GPa), elastic modulus reduced by 6.12% (from 71.46 GPa
to 67.08 GPa) and surface roughness decreased by 6.18% (from
41.93 nm to 39.33 nm). All of these relatively small changes
were found to be statistically insignificant. This agrees with
previous work by Buckthal and Kusy [11] who also detected no
statistically significant changes in the mechanical properties
and surface topography of Nitinol and Titanal archwires fol-
lowing disinfection using three different regimens, namely 2%
glutaraldehyde, chlorine dioxide and iodophor.
In the present study, after intraoral exposure and sub-
sequent decontamination, the mean hardness of the nickel
titanium wires was found to have increased by 12.73% (from
2.36 GPa to 2.61 GPa), elastic modulus reduced by 4.32% (from
71.46 GPa to 68.36 GPa) and surface roughness increased by just
1.83% (from 41.93 nm to 42.69 nm). Once again these changes
 d e n t a l m a t e r i a l s 2 5 ( 2 0 0 9 ) 1039–1043
were not statistically signifcant and concur with previous in
vitro research by Sung Ho Lee et al. [12], but are contrary to
the results of an in vivo experiment by Kapila et al. [13]. In
the former study, following 4 weeks of immersion in artificial
saliva, all three nickel titanium wire types tested showed no
statistically significant differences in tensile strength, elonga-
tion rates or modulus of elasticity. In the latter study, following
8 weeks of clinical use and subsequent cold sterilisation (2%
acidic gluteraldehyde for 10 h), the mechanical properties of
martensitic stable (classic) and austenitic active nickel tita-
nium archwires (super elastic) were affected to a statistically
significant degree. The authors however left the clinical signif-
icance of the very small, yet statistically significant, changes
open to question.
Perhaps somewhat unexpectedly, and in contrast to
the nickel titanium archwires, the stainless steel arch-
wires showed statistically significant changes following both
decontamination and clinical exposure. In particular with
decontamination there was a mean increase in the surface
hardness of 23% (from 4.13 GPa to 5.11 GPa) and a decrease in
the surface roughness of 13.15% (from 25.76 nm to 22.38 nm).
It is surprising that what was initially thought would be a
relatively inocuous decontamination regimen, turned out to
have such an effect. After all, the purpose of the decontami-
nation was only to remove any acquired biofilm and thus avoid
contaminating the nanoindenter.
With clinical use the elastic modulus increased by 13.58%
(from 229.36 GPa to 260.53 GPa) whereas the surface roughness
decreased by 36.03% (from 25.76 nm to 16.48 nm). Certainly the
statistically signifcant increase in elastic modulus is perhaps
not so surprising, as there may be some work hardening as a
result of clinical use, which on average for the steel wires was
90 days.
It must be remembered that the observed changes in elas-
tic moduli and hardness may not be representitive of similar
changes throughout the thickness or bulk of the archwires.
Overall, bulk changes may be either greater or smaller than
those observed at the surface. With decontamination alone
it is unlikely that anything other than just surface properties
have been altered. Work hardening of the archwire, secondary
to repeated bending during clinical use, may account for the
observed increase in elastic modulus with the steel wires.
Once again this may have been either a surface or a bulk effect.
Even if the changes in surface topgraphy, hardness and elastic
modulus are localized to the surface of the wires then this may
have a significant effect on orthodontic tooth movement. This
is because orthodontic tooth movement will be dictated to a
large degree by surface, as a well as bulk interactions, between
the archwire and associated orthodontic brackets and tubes.
5. Conclusions
Whereas the nickel titanium archwires remained uneffected
by the decontamination regimen and clinical use, some
1043
of the the surface properties of stainless steel archwires
were altered by both. Probably the most signicant find-
ings are the increased elastic modulus and the decreased
surface roughness with stainless steel wires, as a result
of clinical use. However, at present it is difficult to deter-
mine the likely clinical significance of these observed
changes.
references
[1] Burstone CJ. Variable-modulus orthodontics. Am J Orthod
1981;80:1–16.
[2] Wichelhaus A, Geserick A, Hibst R, Sander FG. The
effect of surface treatment and clinical use on
friction in NiTi orthodontic wires. Dent Mater
2005;21:938–45.
[3] El Medawar L, Rocher P, Hornez JC, Traisnel M, Breme J,
Hildebrand HF. Electrochemical and cytocompatibility
assessment of nitinol memory shape alloy for orthodontic
use. Biomol Eng 2002;19:153–60.
[4] Es-Souni M, Es-Souni M, Fischer-Brandies H. On the
properties of two binary NiTi shape memory alloys. Effects
of surface finish on the corrosion behaviour and in vitro
biocompatibility. Biomaterials 2002;23:2887–94.
[5] Kappert HF, Jonas I, Liebermann M, Rakosi T.
Korrosionsverhatten Verschiedener Orthodontischer Drahte.
Fortschritte der Kieferorthopadie 1988;49:358–67.
[6] Bourauel C, Fries T, Drescher D, Plietsch R. Surface
roughness of orthodontic wires via atomic force microscopy,
laser specular reflectance, and profilometry. Eur J Orthod
1998;20:79–92.
[7] Meling TR, Odegaard J. The effect of short-term temperature
changes on superelastic nickel–titanium archwires activated
in orthodontic bending. Am J Orthod Dentofac Orthop
2001;119:263–73.
[8] Oliver WC, Pharr GM. An improved technique for
determining hardness and elastic modulus using load
displacement sensing indentation experiments. J Mater Res
1992;7:1564–83.
[9] Alcock JP, Ireland AJ, Barbour ME, Sandy JR. Nanoindentation
of orthodontic archwires: variation of elastic modulus and
hardness within a stainless steel wire. Int J Nano Biomater
2007;1:128–37.
[10] Alcock JP, An investigation into the mechanical properties of
orthodontic archwires. DDS dissertation, University of
Bristol 2008.
[11] Buckthal JE, Kusy RP. Effects of cold disinfectants on the
mechanical properties and the surface topography of
nickel–titanium arch wires. Am J Orthod Dentofac Orthop
1988;94:117–22.
[12] Sung Ho Lee, Chang YII. Effects of recycling on the
mechanical properties and the surface topography of
nickel–titanium alloy wires. Am J Orthod Dentofac Orthop
2001;120:654–63.
[13] Kapila S, Reichhold G, Anderson S, Watanabe L. Effects of
clinical recycling on mechanical properties of
nickel–titanium alloy wires. Am J Orthod Dentofac Orthop
1991;100:428–35.