JIOS

10.5005/jp-journals-10021-1073
ORIGINAL ARTICLE
Effects of Intraoral Ageing on Ultimate Tensile Strength and Surface Topography of Superelastic NiTi Wires

Effects of Intraoral Ageing on Ultimate Tensile

Strength and Surface Topography of
Superelastic NiTi Wires from Two Different
Manufacturers: A Comparative in vivo Study
1
A Pravin Devaprasad, 2TR Chandrasekaran

ABSTRACT

Aim: The purpose of this study was to evaluate and compare the ultimate tensile strength/fracture resistance of superelastic NiTi wires
from two manufacturers 3M Unitek and American orthodontics in as received condition, after 3 months and 6 months of intraoral use. The wires
would also be evaluated for surface characteristics under a scanning electron microscope.
Materials and methods: Superelastic NiTi wires of 0.016" from 3M Unitek were categorized as group I and from American orthodontics as group
II. The subgroup A of groups I and II consisted of 10 unused samples. The subgroups B of groups I and II consisted of wires retrieved after 3 months
of clinical use. The subgroup C of groups I and II consisted of wires retrieved after 6 months of intraoral use.
Results: The results showed that the ultimate tensile strength of the unused wires of both groups I and II were significantly higher than the used
wires of the same group. The unused wires of 3M Unitek were found to have superior ultimate tensile strength than the unused wires from American
orthodontics and the difference was statistically significant. Likewise, the ultimate tensile strength of 3M Unitek wires which were unused was
significantly higher than used wires at 3 months and 6 months of intraoral use, American orthodontics wires which were unused were also found
to have statistically higher ultimate tensile strength that the intraorally placed wires after 3 months and 6 months. The 3M Unitek wires retrieved
after 3 months and 6 months of intraoral use showed statistically increased ultimate tensile strength than American orthodontic wires of comparative
use. Even the surface topography of 3M Unitek wires which were unused and after 3 and 6 months of exposure to intraoral environment showed
less pitting, decrease in indentations and less surface roughness.
Conclusion: Super elastic NiTi wires from 3M Unitek were found to be superior to the wires from American orthodontics in as received condition,
after 3 months of clinical use and 6 months of clinical use. The surface topography of 3M Unitek wires was found to have less pitting and indentations
than American orthodontic wires of comparable use. Wires from both manufactures were found to undergo degradation after clinical use. During
the study, it was found that 3M Unitek NiTi superelastic wires had better ultimate tensile strength and surface topography than superelastic NiTi
from American orthodontics.
Keywords: Ageing, Ultimate tensile strength, Superelastic NiTi.

How to cite this article: Devaprasad AP, Chandrasekaran TR. Effects of Intraoral Ageing on Ultimate Tensile Strength and Surface Topography
of Superelastic NiTi Wires from Two Different Manufacturers: A Comparative in vivo Study. J Ind Orthod Soc 2012;46(3):119-125.

INTRODUCTION newer wires and their ability to preferentially orient elastic

A bewildering array of arch wires is available today for
orthodontic use, ranging from stainless steel to different
innovations with NiTi wires to Timolium. The paradigm shift
from variable cross-section orthodontics to variable modulus
orthodontics has reduced the number of arch wires needed for
alignment because of the decreased load deflection rate of the
1,2
Reader
1
Department of Orthodontics and Dentofacial Orthopedics, SRM
Kattankulathur Dental College, Kanchipuram, Tamil Nadu, India
2 wire and depending on these studies, conclusions were drawn
Department of Orthodontics and Dentofacial Orthopedics, Raja
Muthiah Dental College, Chidambaram, Tamil Nadu, India
Corresponding Author: Pravin Deva Prasad, Reader, F-2, Star Saffire
Apartments, H-1586, 6th Street, 11th Main Road, Annanagar, West Chennai-
600040, Tamil Nadu, India, e-mail: pravindevaprasad@ yahoo.co.in
Received on: 13/11/11
Accepted after Revision: 20/3/12
deflection.1
An orthodontic archwire which seats in the bracket slot
with minimum patient discomfort, during the aligning stages, is
considered superior initial wire.2 The physical behavior of the
NiTi wire has been described as unique and radically different
from conventional wires. This is due to its property of shape
memory, greater spring back and flexibility allowing large elastic
deflections and thus recognized as a better aligning wire.3
A number of in vitro and in vivo studies have been carried
out to determine the mechanical and physical properties of the
on the clinical efficiency of the arch wire material.4,5 The effect
of intraoral ageing on the archwires requires further research to
establish the true spectrum of effects that might influence the
surface characteristics and the mechanical properties of the
wire.
Exposure of orthodontic materials to the oral environment
is associated with a nonspecific ageing pattern characterized

The Journal of Indian Orthodontic Society, July-September 2012;46(3):119-125 119

A Pravin Devaprasad, TR Chandrasekaran
by calcification of the adsorbed complexes of ions and
proteinaceous matter. This effect, coupled with a variety and
potency of several other factors making up the environmental
conditions of the oral cavity, might alter the morphologic,
structural and compositional characteristics, thereby the
mechanical properties of the orthodontic alloy. The material in
the oral cavity might not perform identical to their as received
or in vitro aged counterparts, in that their properties might
deviate from those specified by the manufacturer. Clinicians
should understand the limitations on the properties of the
materials arising from intraoral ageing, modifying their
expectations and monitoring treatment progress accordingly.
Therefore, it is essential to identify the changes in the material
especially those used for an extended period to maximize the
clinical efficiency of the material.6 It has been established that
the intraoral exposure of NiTi wires alters the topography and
structural characteristics of the alloy through surface attacks
by way of pitting, crevice corrosion or formation of
integuments.7
It has been hypothesized that the sporadic failure of NiTi
wires is due to corrosion induced by pitting as well as surface
defects present on the alloy surface. The long term use of a
NiTi arch wire in the oral cavity is associated with degradation
in performance, notably in the limit of the elasticity and
eventually affecting ultimate tensile strength.
AIMS AND OBJECTIVES
The aims and objectives of the study are as follows:
1. To evaluate and compare the intraoral ageing induced
surface topographic changes on 3M Unitek and American
orthodontics superelastic NiTi wires.
2. To evaluate and compare the fracture resistance (ultimate
tensile strength) of superelastic NiTi wires from 3M Unitek
and American orthodontics in as received condition, after
3 months of intraoral use and after 6 months of intraoral use.
MATERIALS AND METHODS
This study was conducted at the Department of Orthodontics
and Dentofacial Orthopedics, Meenakshi Ammal Dental
College and Hospital, Chennai. In this study two different
groups of nickel titanium superelastic archwires from
manufacturer 3M Unitek and American orthodontics (AO)
were used to evaluate the ultimate tensile strength and surface
topography. The wires from both manufacturers were standard
orthoform III arch form of the lower arch. Each group
comprised of 30 samples of wires.
Group I superelastic, NiTi, 0.016" 30 3M Unitek; group II
superelastic NiTi, 0.016" 30; American orthodontics.
Each main group comprised of three subgroups namely as
follows:
• Subgroup A: As received group or the control group—
comprised of 10 wires in as received condition.
• Subgroup B: Comprise of 10 wires retrieved after 3
months after placement in the patient’s mouth.
120
• Subgroup C: Comprises of 10 wires retrieved after 6
months of placement in the patient’s mouth.
The experimental wires were placed in patients undergoing
treatment that involved aligning and leveling. The wires were
placed only in the lower arch for each patient.
The patients were randomly selected from a pool of
participants established with the following criteria:
• Age range of 14 to 25 years
• No medication or other intraorally administered
substances
• Similarity in gross malocclusion parameters such that there
was lower anterior crowding greater than 4 mm and
required extraction of all first premolars.
All the patients were bonded with PEA 0.022" slot Roth
prescription appliance.
The patients were given standard instructions toward the
maintenance of the appliance. Modules were changed at monthly
intervals.
In the subjects, the wires were removed such that the area
closer to the midline was not handled with any instrument. The
collected archwires were rinsed with deionized water to detach
any loosely bound precipitates. The wires were placed in paper
sterilization pouches and taken to be tested for the ultimate
tensile strength and surface characteristics.
The ultimate tensile strength of the unused wires and the
retrieved wires after 3 and 6 months of the two groups were
measured with a Universal Testing Machine. Archwire insertion
and retrieval appointments were monitored by means of retrieval
protocol consisting of the following variables, such as date of
archwire placement, archwire subgroup.
METHOD OF STUDY
Tensile Testing
The tensile properties were measured with universal testing
machine (Model 4301, Instron Corp, Canton, Mass) at IIT,
Chennai, Tamil Nadu. A full scale load of 1000N was set in the
machine.
The machine was operated in tensile mode with a cross-
head speed of 5 mm/min. Each specimen was cut in the midline
and placed in the jaws of the machine. The span of the wire
between the cross-heads was standardized as 20 mm. The load
taken to break the wire was noted.
The tensile strength of specimen was calculated by the
following formula:
Ultimate tensile strength
Load taken to break the wire (Newtons)
= ———————————————————
Cross-sectional area of the specimen
Surface Topography
Scanning electron microscopy was used to study the surface
topography of the wires used. The microscope used was JEOL,
Model No: JSM 5610: Low vacuum and the SEM study was
done at Annamalai University, Chidambaram, Tamil Nadu.
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Effects of Intraoral Ageing on Ultimate Tensile Strength and Surface Topography of Superelastic NiTi Wires

Ultimate tensile strength = 0.016 inch NiTi archwire from The formula used for one-way ANOVA was:
the experimental and control group was assessed qualitatively
with the SEM at three different magnifications. For the SEM
 k 2– 
  N i (x i – x)  (k  1)
evaluation, 7 mm of the wire was cut from the midline in the
F =  i k1 
unused wire, retrieved wire sample after 3 and 6 months. The
wire segment was stuck to adhesive pad which was then placed  
  (N i – 1)Si  (N  k)
2
on the metallic pellet which is used as a platform for the scanning
 i 1 
electron microscopy (SEM). The surface was scanned and
viewed on the monitor at different magnifications and the Ni
representative micrographs of the studied sample were obtained.  (x ij – x i )2
The magnifications used in this study were: 250×, 500× and Where Si2 j1
=
1000× magnification. Ni – 1
xij is the jth observation in the ith group, xi is the mean of obser-
Statistical Analysis vations in the ith group and Ni is the number of observations in
the ith group, x is the overall mean of the entire observations.
Mean and standard deviation were estimated from the sample
In the present study, p < 0.05 was considered as the level of
for each study group. Mean values were compared between
statistical significance.
different study groups by student’s unpaired t-test.
The results were statistically analyzed using the following
statistical analysis. RESULTS
i. Student independent ‘t’ test or The results on critical analysis showed that the ultimate tensile
ii. One-way analysis of variances (ANOVA) with multiple strength of the unused wires of both groups I and II were
range test by Tukey-Honestly significantly difference significantly higher than used wires of the same group. The
(HSD) procedure appropriately: unused wires of 3M Unitek were found to have superior ultimate
x1 – x 2 tensile strength (Tables 1 and 2) than the unused wires from
t= American orthodontics and the difference was statistically
Sp2 Sp2
 significant.
n1 n2 There was a statistically significant decrease in the ultimate
tensile strength value between the unused wire of both groups.
(n1 – 1)S12  (n 2 – 1)S22 Comparing the mean values of ultimate tensile strength retrieved
Where Sp2 =
n1  n 2 – 2 after 3 month between the two groups (IB and IIB) (Figs 1 and 2)
showed a statistically significant decrease of ultimate tensile
x1–x2 are the sample means. S12 and S22 are the sample
variances. n1 and n2 are the sample sizes in two independent
Table 1: Mean, standard deviation and test of significance of mean
groups. values of ultimate tensile strength between different study groups

Groups compared Mean ± SD (MPa) p-value*

Sample mean may be calculated as:
IA 1169.7 ± 9.2 <0.0001 (sig)
x– = x + x + … + x =
1 2 x /n
n  i IIA 1080.7 ± 5.3
i 1
IB 1051.7 ± 7.0 <0.0001 (sig)
IIB 960.7 ± 24.2
n
 (xi – x)2– IC
IIC
970.8 ± 19.2
843.9 ± 27.8
<0.0001 (sig)
and SD  S = i 1
n 1 Sig: Significant

Table 2: Comparison of percentage difference in ultimate tensile strength between

subgroups A, B and C of groups I and II

Ultimate tensile strength

Subgroup (A) Subgroup (B) Subgroup (C) Difference Difference Difference
mean ± SD mean ± SD mean ± SD A and B (%) B and C (%) A and C (%)
(MPa) (MPa) (MPa)

Group I 1169 ± 9.8 1051.7 ± 7.0 970.8 ± 19.2 10.03 7.7 16.95
Group II 1080 ± 5.6 960.7 ± 24.2 843.9 ± 27.8 11.1 12.1 21.9

The Journal of Indian Orthodontic Society, July-September 2012;46(3):119-125 121

A Pravin Devaprasad, TR Chandrasekaran
Fig. 1: Deposits of plaque, pitting and thin indentations
Fig. 2: Increased pitting with great depth and
prominent indentations
Fig. 3: Increased plaque accumulation with increase in
number and depth of indentation
Fig. 4: Increased surface roughness with deep crevices
122
strength value for group II. Comparing the mean values of
ultimate tensile strength retrieved after 6 month between the
two groups (IC and IIC) (Figs 3 and 4) showed a statistically
significant decrease of ultimate tensile strength value for
group II (Table 2). There was a significant percentage of
difference between retrieved wire from 3 to 6 months period
for groups I and II, indicated an increased degradation of ultimate
tensile strength in group II compared to group I (Tables 1 and 2).
DISCUSSION
Optimal wire used for treatment of orthodontic applications
is nickel-titanium. There are innumerable wire brands currently
available in the market and sometimes these products are offered
without specifying their mechanical properties. Even when
revealed these properties cannot be properly compared with
those of similar products because the measuring conditions
and specifications differ from one manufacturer to another.8
Taking this fact into consideration, two brands (3M
Unitek—group I and American orthodontics—group II) of
nickel-titanium superelastic wires that are commonly used in
our department were compared. NiTi archwires are
predominantly used during the initial stages of aligning and
leveling. During this extended period of alignment, the
superelastic NiTi wires undergo a number of alterations within
the oral cavity which affects the further performance of the
wire. It is essential to determine these age changes and
understand the effect of these changes on the clinical
efficiency of the wires which helps in managing the clinical
situation better and improve the effectiveness of the treatment.
Here, we have evaluated the ultimate tensile strength and
surface characteristics of superelastic NiTi wires, which seem
to undergo changes in vivo.9
Superelastic NiTi was used in this study due to its
advantage of pseudoelasticity and smooth surface.1,10,11 For
this study, cases with lower anterior crowding greater than 4
mm which needed long-term placement of initial aligning wires
were segregated.
The ultimate tensile strength of the unused and retrieved
wires was studied using the Universal Instron Testing Machine.
The values were converted to MPa units. A number of
researches have focused on the detailed study of mechanical
properties, and phase transformation changes of the wire under
in vitro conditions.1 There is a scarcity of information on the
effect of the intraoral environment on the structural and
compositional alterations. Studies have been conducted
simulating the oral environment too.12 Despite the abundance
of evidence produced by orthodontic material research, the
laboratory configuration and setup used to simulate intraoral
condition are strikingly different to the actual oral environment.
The main factor that distinguishes the oral cavity from
in vitro media is the presence of oral flora and their byproducts
as well as accumulation of plaque on the material. The
multifaceted intraoral environmental milieu cannot be
simulated with currently available in vitro simulated research
methodologies most of which involve exposure of materials to
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Effects of Intraoral Ageing on Ultimate Tensile Strength and Surface Topography of Superelastic NiTi Wires
various electrolytes, artificial saliva, water and other media.
Thus, there is a notable lack of evidence regarding the intraoral
ageing pattern of orthodontic wires and the associated cohort
of phenomena, such as surface alterations, structural changes
and variation of mechanical properties.
The lack of relevant evidence may derive from the noted
inability of in vitro research to simulate in vivo conditions
reliably. This has been due to the multiplicity and potency of
factors present in the oral cavity, such as extreme pH and
temperature variations and the complex oral flora and its by
products. Therefore, although there are a number of studies
done with in vivo simulation, their conclusions do not carry
great clinical significance.13
The issue of interest is in vivo alteration of the material
due to the long period of performance with possible effects
on mechanical properties, the main focus being the alterations
induced on orthodontic wires.14 During the extended phase of
alignment, the surface characteristics and mechanical
properties undergo changes.15
The results of our study indicates an alteration in the surface
texture and mechanical properties over a period of 6 months.
Our results were in concordance with the studies done by Edie
and Anderson,15 Eliades et al.13
Ultimate tensile strength is the maximum stress the wire
can withstand before fracture. This mechanical property is
generally affected due to the manufacturing defects and/or
the intraoral ageing process. The manufacturer’s contribution
may be due to the compositional differences leading to
creviced wires or due to the defects during the drawing
process.12,13,16 Comparing the ultimate tensile strength, there
is a gradation from the unused sample to 6 month retrieved
wires with the 3 months retrieved wire showing intermediate
values.
Previously, Eliades et al13 reported delamination, pitting
and crevice corrosion defects as well as reduction in alloy
grain size in the retrieved NiTi wires after 6 months. The age
changes of NiTi wires have been studied and the ageing effects
are elaborated as adsorption and calcification of the biofilm,
increased porosity and roughness.17 The potential mechanical
effects is the decreased ultimate tensile strength and clinically
reported as superelastic properties not being expressed and
fracture resistance of the wire decreased. The results of our
study are in concordance with the above-mentioned literature.
Our study shows significant decrease of 5% in the ultimate
tensile strength between the unused wire and the 6-month
retrieved wire of the two groups. These values suggest that
the degradation of the wire in the intraoral environment is more
prominent. The results also clearly indicate that there is a
significant change in the mechanical properties of the wire as
the period of intraoral ageing is increased. The surface structure
of orthodontic wire is an essential feature known to influence
esthetic result, the resistance to corrosion and the biocom-
patibility of the wire.
Profilometer has been one of the methods to study the
surface texture. Due to the increasing demands for
The Journal of Indian Orthodontic Society, July-September 2012;46(3):119-125
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nondestructive or noncontact technique the development of
number of optical methods like integrated scatter, diffuseness,
angular scattering distributions, speckle ellipsometry and
inferometry have become popular.
However, we used scanning electron microscopy which is
yet another popular method for the evaluation of the surface
properties. A number of studies have been done using SEM as
a reliable method to evaluate the surface characteristics of
the NiTi wires.13,18,19,20
In our study, SEM evaluation of the unused wire, the
retrieved NiTi wire after 3 and 6 months of the two groups
were done. SEM analysis of unused wire subgroup IA showed
smooth finish at 250X magnification and pitting that was
obvious only in the 500X and 1000X magnification. The
unused wire subgroup IIA showed thin indentation and round
and oval pitting with certain areas of rough and irregular surface
at 500× and 1000× magnification.
In a study conducted by Lee and Chang et al 21 on surface
topography of wires, the indentations seen in the wires are
mostly due to the drawing process during the manufacturing.
These surface irregularities and indentations caused by the
manufacturing process on the NiTi wire could predispose the
wire to corrosive attack in the mouth.14,15,22
The retrieved wire of subgroup IB showed deposits of
plaque, pitting and thin indentations. The surface irregularity
is minimal. The retrieved wire of subgroup IIB showed
increased pitting with greater depth, accumulation of the
integuments and the indentations were more prominent in
higher magnification than the subgroup IB. The retrieved wire
of subgroup IC showed increased plaque accumulation with
increase in number and depth of indentations. The retrieved
wire of subgroup IC displayed decreased integuments with
abrading residues. The indentations were thicker and more
prominent. Deep cracks were more frequently seen.
When assessing the quality of archwires, surface quality
should be, as it determines corrosion resistance, biocom-
patibility and friction characteristics. Comparing the surface
characteristics of the unused wire of groups I and II, subgroup
IA shows superior finish compared to subgroup IIA.
The surface of the alloy influencing the working charac-
teristics and corrosion potential was analyzed by Kusy and
Whitley.23 Most published data referring to the properties of
superelastic NiTi wires are limited to the wire in a dry
environment whereas the clinician uses the wire under various
stress and strain. In the corrosive environment of the oral
cavity, the superelastic NiTi wire has been advocated to use.
In this study we have compared the wires in vivo to determine
accurately the surface structure and ultimate tensile strength
after 3 and 6 months.
It has been shown that oral exposure of superelastic NiTi
wires alters the topography in the form of pitting, crevice
corrosion and formation of integuments.24 Retrieved super-
123
A Pravin Devaprasad, TR Chandrasekaran
elastic NiTi demonstrated signs of corrosion after 2 months
of service and signs of pitting and corrosion were detected
after 6 months of oral exposure.25 In our 6 months in vivo
evaluation deep crevices with increased integuments were
identified in both groups. The subgroup IIC had relatively more
surface roughness which makes it more susceptible to crevice
corrosion. Subgroup IC displayed less indentation and hence
it is less prone to crevice corrosion.
The alteration in the surface texture is due to a combination
of intraoral conditions and also loading attributed to the
engagement of the archwire into the slot. The described
alterations of the retrieved wires profoundly altered the reactivity
of the wire making it more susceptible to corrosion and decrease
in the fracture resistance of the archwire. Although superelastic
NiTi wires are unbreakable in vitro, it seems that intraorally
exposed NiTi wires, do break more frequently than expected. In
cases which require extended use of aligning wire, fracture of
the initial wire was one of the commonly encountered
problems.19 Every surface damage could become a start of a
fracture.26 Therefore, the retrieved superelastic NiTi wires after
6 months of intraoral ageing with deep crevices and indentations
display a reduction in fracture resistance leading to a decrease
in the gradation of ultimate tensile strength from 3 to 6 months.
These wires were vulnerable to fracture.9,14 Recycling of NiTi is
done by 52% of orthodontist of those who use NiTi wires
routinely.27 The most common reason for recycling being the
expense. As the properties of NiTi are altered due to intraoral
ageing it is not advisable to reuse the NiTi wires that have been
previously used for an extended alignment or has been exposed
to the intraoral environment for a period of 6 months. Our study
is in concordance with results of Harris et al19 which evaluated
the long-term use of superelastic NiTi wire and associated the
ageing effects to decreased performance. Fracture of aligning
wires could cause discomfort to the patient in the form of a wire
prick and the sliding of the remaining wire. This also may could
undesirable tooth movement.
It is therefore essential to understand the effects of intraoral
ageing of the superelastic NiTi wires and use these wires
according to the clinical effectiveness. Considering the above
results 3M Unitek wires exhibited better properties than
American orthodontic wires especially in cases requiring an
extended alignment.
Similarly in cases requiring the extended alignment, it would
be better to change the superelastic NiTi wire preferably within
a period of 3 months, there by using two sets of 0.016
superelastic NiTi wire for the initial aligning and leveling and
would lead to less chance of fracture.
CONCLUSION
Retrieval analyses have gained interest in biomaterials research
because of the critical information derived from investigating
the performance of the material in the environment in which
it was intended to function. The main factor that distinguishes
the in vivo environment from various storage media is the
presence of complex oral flora and their by products, which
along with local microenvironmental variables, could form
124
specific conditions, which cannot be simulated under current
in vitro research methodological approaches. The enhanced
deterioration of the wire surface coming in contact with the
oral environment has been illustrated and explained on the basis
of development of comprehensive forces and surface morpho-
logies.
The surface topography and ultimate tensile strength
evaluation of the unused and retrieved wire presents a decrease
in the performance in both groups due to intraoral ageing effects.
The 3M Unitek wire displayed better tolerance to the intraoral
ageing effects.
The fracture resistance was decreased in both groups after
3 months. The fracture resistance was decreased more in both
groups after 6 months with greater percentage difference in
the American orthodontics wires compared to the 3M Unitek
wires.
The results of this study should not be viewed as
conclusive evidence in comparing the commercial superelastic
NiTi archwires, since variations in clinical situation and various
other properties which are not taken in this study are still
inconclusive.
Clinicians should understand the limitations of materials
arising from ageing, modifying their expectations and monitoring
treatment progress accordingly.
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