Basic Research—Technology
Fatigue Resistance of Nickel-titanium
Instruments Exposed to High-concentration
Hypochlorite
Xiangya Huang, DDS, PhD,*† Ya Shen, DDS, PhD,†‡ Xi Wei, DDS, PhD,*
and Markus Haapasalo, DDS, PhD†
Abstract
Introduction: The purpose of this study was to intro-
duce a new fatigue test model that simulates the clinical
situation for evaluating the corrosion effect of 5.25% so-
dium hypochlorite (NaOCl) on nickel-titanium (NiTi) files
and to evaluate the effect of 3 different temperatures
(22 C, 37 C, and 60 C) on the cyclic fatigue of these
files. Methods: Three NiTi files (size 25/.04), K3 (Sybro-
nEndo, Orange, CA), K3XF (SybronEndo), and Vortex
(Dentsply Tulsa Dental Specialties, Tulsa, OK), were sub-
jected to cyclic fatigue tests inside a novel artificial
ceramic canal with a curvature of 60 and a 5-mm
radius. A 19-mm-long file segment from the tip was
introduced into the canal and immersed in water or
5.25% NaOCl at 3 different temperatures, and the num-
ber of revolutions to fracture (Nf) was recorded. The
fracture surface of all fragments was examined by a
scanning electron microscope. Data were analyzed using
univariate analysis of variance with the significance
level at 0.05. Results: The Nf of Vortex files was the
highest followed by K3XF and K3 (P < .05) at all condi-
tions. The Nf of all files was highest at 22 C and lowest
at 60 C (P < .05). However, no difference in Nf was de-
tected in Vortex files between 22 C and 37 C. The Nf of
all files in 5.25% NaOCl was shorter than that in water
although there was no statistically significant difference.
No pitting or crevice corrosion was observed on the frac-
ture surface. Conclusions: NaOCl, 5.25%, does not
significantly affect the fatigue behavior of NiTi files.
The fatigue resistance should be tested under specific
temperature conditions. The austenite finish tempera-
ture of a file is important in determining the fracture
risk at body temperature. (J Endod 2017;43:1847–1851)
Key Words
Ceramic canal, corrosion, fatigue resistance, nickel-
titanium instrument, sodium hypochlorite, temperature
From the *Department of Conservative Dentistry and Endodontics, Guanghua School of Stomatology, Guangdong Province Key Laboratory of Stomatology, Sun
Yat-Sen University Guangzhou, China; †Division of Endodontics, Department of Oral Biological and Medical Sciences, Faculty of Dentistry and ‡Department of Materials
Engineering, The University of British Columbia, Vancouver, Canada.
Address requests for reprints to Prof Markus Haapasalo, Division of Endodontics, Department of Oral Biological and Medical Sciences UBC Faculty of Dentistry, 2199
Wesbrook Mall, Vancouver, BC, Canada V6T 1Z3. E-mail address: markush@dentistry.ubc.ca
0099-2399/$ - see front matter
Copyright ª 2017 American Association of Endodontists.
http://dx.doi.org/10.1016/j.joen.2017.06.033
JOE — Volume 43, Number 11, November 2017
D espite their popularity,
a concern with the use
of nickel-titanium (NiTi)
Significance
NaOCl, 5.25%, does not significantly affect the fa-
tigue behavior of NiTi files. The fatigue resistance
rotary files is the possibility
should be tested under specific temperature con-
of unexpected separation.
ditions.
Two different mechanisms
may lead to NiTi rotary
fracture: cyclic fatigue and torsional fracture (1–3). When a rotary file undergoes
repeated compression and extension in a curved canal, this can cause work
hardening of the metal, which causes cyclic fatigue and an increased risk of fracture.
NiTi file failures in the clinic are mainly caused by cyclic fatigue (2–4). The fatigue life
of a file can be expressed as the number of loading cycles required to initiate a fatigue
crack and to propagate the crack to critical size (5, 6). Fatigue crack growth rates in
NiTi alloys have been reported to be significantly greater than in other metals of
similar strength (7). Therefore, it is not surprising that several studies have been
published in recent years with a focus on the fatigue resistance of different NiTi files
(4–6,8–12). All of these studies have attempted to simulate the rotation of the
instrument within a curvature to determine how long it lasts before the fracture occurs.
Root canal instrumentation is recommended to be performed with sodium hypo-
chlorite (NaOCl) as an irrigant in the canal(s) and a reservoir in the pulp chamber.
NaOCl has antimicrobial and tissue-dissolving activity (13, 14), but it can also cause
the corrosion of metals. NiTi instruments come into contact with NaOCl during
instrumentation, which raises the question of the impact of such short-term contact
on the integrity of the files. The events potentially leading to complete separation of
file fragments begin on the file surface as crack initiation. Because environmental con-
ditions are also known to affect crack initiation, a role possibly played by a corrosive
irrigating solution, NaOCl is of interest. Surface corrosion starting as pitting and crevice
corrosion could have an impact on the file’s ability to withstand fatigue stress. NaOCl is
commonly used in concentrations between 0.5% and 6%. Although the corrosive
behavior of NaOCl on NiTi instruments has been studied (15–21), the fatigue test
was performed after a passive exposure of the instruments to NaOCl for different
time periods (15–18) or while instruments were immersed in a low concentration
of NaOCl (ie, 1.2%) (19–21) to avoid the corrosion of the test models, which
typically are or contain metallic parts such as stainless steel. Zirconia found in
nature is a highly hard material that has been given the nickname ‘‘ceramic steel’’
(22). The interest in using zirconia dioxide as a biomaterial is based on its mechanical
NiTi Instruments and High-concentration Hypochlorite 1847
Basic Research—Technology
strength as well as its chemical and dimensional stability and elastic

284.17  38.54b

293.06  62.45b
609.72  77.59c
modulus similar to stainless steel (22).
The use of only low-concentration NaOCl in a real-time corrosion

60 C
test may give a too optimistic picture of the effect of NaOCl on NiTi in-
struments. Hence, a fatigue test model allowing high NaOCl concentra-
tions would be useful to mimic the clinical situation for examining the
fatigue behavior of NiTi instruments under various conditions.
Currently, 2 studies (12, 23) have found that the temperature
influenced the fatigue life of NiTi files in water. Therefore, the aims of
this study were to introduce a new fatigue test (in zirconium oxide)

505.56  73.28ac
348.33  72.00b
model that better simulates the clinical situation for the evaluation of

1098.61  90.65f
5.25% NaOCl
the corrosion effect of 5.25% NaOCl on NiTi files and to evaluate the
effect of 3 different temperatures (22 C, 37 C, and 60 C) on the

37 C
cyclic fatigue life of conventional superelastic and heat-treated NiTi files.

Materials and Methods

Three nickel-titanium rotary instruments (size 25/.04), K3 (Syb-
ronEndo, Orange, CA), K3XF (SybronEndo), and Vortex (Dentsply
Tulsa Dental Specialties, Tulsa, OK), were subjected to cyclic fatigue

884.72  242.69d
tests inside a novel ceramic artificial canal model. The ceramic artificial

433.33  57.89ab

1197.92  64.76f
canals were milled in an InCoris ZI zirconium oxide disc (Dentsply Si-
rona, Bensheim, Germany) using the inLab MC X5 Digital computer-

22 C
aided design and computer-aided manufacturing (CAD/CAM) System
(Dentsply Sirona). The size of the artificial canal was 30/.06 with a cur-
vature of 60 and a 5-mm radius (24). The model was fixed in a glass

TABLE 1. The Number of Revolutions until Fracture of Files in Water and Sodium Hypochlorite (NaOCl) at 22 C, 37 C, and 60 C
container filled with 300 mL 5.25% NaOCl (The Clorox Company,
Brampton, Ontario, Canada) or distilled water. To achieve the desired
temperatures, the glass container was placed on a hot plate until the wa-
ter temperature was stabilized at the room temperature (22 C  1 C),
body temperature (37 C  1 C), or high temperature (60 C  1 C);

328.75  47.87b

325.00  30.77b
638.89  64.48c
during all tests, the temperature was measured with an infrared ther-
60 C
mometer (Sper Scientific Ltd, Scottsdale, AZ). A 19-mm-long segment
from the tip of the instrument was introduced into the ceramic canal
and immersed in the liquid medium during the test. Each group
included 12 instruments. K3 was rotated at 300 rpm, and K3XF and Vor-
tex were allowed to rotate at 500 rpm as recommended by the manu-
facturer until fracture. The fatigue life of the time to break (seconds)
was recorded and multiplied by the number of rotations per minute
603.47  112.45c
413.75  46.37ab

to obtain the total number of cycles to failure (Nf). After the test, the de-
1102.78  84.93f
Distilled water

tached fragments were collected and rinsed briefly with deionized wa-
Different superscript letters indicate statistically significant differences between groups (P < .05).

ter, and the length of the fragment was measured using a

37 C

stereomicroscope at 10 (Microdissection; Zeiss, Bernried, Ger-

many). The fractured instruments (ie, 3 files randomly selected from
each group) were further cleaned in an ultrasonic bath in absolute
alcohol, and the fractured surfaces were faced upward for fractographic
examination using a scanning electron microscope (Helios NanoLab
650; FEI, Eindhoven, Netherlands) operating at 3 kV.
The data for the Nf were verified with the Kolmogorov-Smirnov test
914.58  215.30d
1356.94  126.87e
501.54  70.46ac

for the normality of the distribution and the Levene test for the homo-
geneity of variances. The data were analyzed statistically using univariate
22 C

analysis of variance (SPSS for Windows 11.0; SPSS, Chicago, IL). Post
hoc multiple comparison (the Tukey test) was used to isolate and
compare the means of the results. All analyses were performed at a sig-
nificance level of a = 0.05.

Results
Heat treated

The Nf of the Vortex files was the highest followed by K3XF and K3
Traditional

both in water and NaOCl at all 3 temperatures (P < .01) (Table 1). All 3
Vortex
K3 XF

files had the highest Nf at 22 C and the lowest at 60 C (P < .001). There
File

K3

was no difference (NaOCl) or a smaller difference (water) in the Nf of

Vortex files at 22 C and 37 C, whereas the fatigue resistance of K3 and

1848 Huang et al. JOE — Volume 43, Number 11, November 2017

K3XF was significantly reduced at 37 C compared with 22 C. The Nf of
all 3 files was significantly lower at 60 C than at 37 C. There was no
statistically significant difference between files tested in water and
NaOCl. The length of the broken fragments was 4.14–5.13 mm.
The scanning electron microscopic appearance of the fracture
surfaces of all 3 files showed typical features of cyclic fatigue, including
1 or 2 crack initiation areas, the presence of fatigue striations, and a fast
fracture zone with dimples (Fig. 1A–F). None of the tested files showed
pitting or crevice corrosion in water or 5.25% NaOCl as evaluated under
scanning electron microscopy (Fig. 1).
Discussion
Zirconia is provided to dental laboratories in blocks of different
sizes, which can be milled into single-unit copings or multiple-unit fixed
bridge frameworks. CAD/CAM dentistry is a field of dentistry that uses
CAD/CAM to improve the design and creation of dental restorations
and fixed dental prostheses. Using CAD/CAM technology, the model is
milled or created with stereolithography using a computer-controlled
Figure 1. The fracture surface of (A and B) K3, (C and D) K3XF, and (E and F) Vortex files after the fatigue test in 5.25% NaOCl at 60 C. A high-magnification view
of the crack ignition in B, D, and F. The arrows point toward the crack initiation points. No signs of corrosion can be seen on the files.
JOE — Volume 43, Number 11, November 2017
Basic Research—Technology
system. The tolerances are in the microns, making these models
extremely accurate. The higher strength and higher hardness of the
ceramic materials yield superior wear and abrasion resistance as well
as corrosion resistance. The device for the fatigue testing in the present
study was milled in a zirconium dioxide block using the CAD/CAM sys-
tem. Thus, the model is custom-made, size-matched artificial canals in a
noncorrosive biomaterial (25). This allowed standardized evaluation of
the fatigue resistance of NiTi files in the potentially corrosive environ-
ment of concentrated NaOCl, which will mimic clinical conditions better
than earlier models. To our knowledge, the present study is the first one
to simulate the fatigue resistance of NiTi files in the continuous presence
of a high concentration of NaOCl.
Testing in 5.25% NaOCl resulted in a slightly shorter but statisti-
cally insignificant fatigue life in all 3 types of files compared with water
in the present study. This result is contradictory to the general belief that
a high concentration of NaOCl is expected to have a negative effect on the
fatigue behavior as a result of an increased amount of available chlorine
that attacks the metal (26). Cheung et al (19) found that even with 1.2%
NaOCl the fatigue life of ProFile (Dentsply Tulsa Dental Specialties) was
NiTi Instruments and High-concentration Hypochlorite 1849
Basic Research—Technology
shorter than in water. In the present study, all files failed in the low-cycle
(Nf <104) fatigue region where the test was performed to simulate the
clinical situation. In such a relatively short period in which the material
can withstand the low number of load cycles, there is little time for the
corrosive attack, and, hence, the absolute number of revolutions until
fracture did not differ much between the 2 conditions (ie, water and
5.25% NaOCl). This was also supported by findings in the scanning elec-
tron microscopic specimens of the fractographic appearance of the
fracture surfaces in which no pitting by corrosion was detected, and
no difference was observed in files that had been in water or NaOCl.
Several studies (27, 28) have shown that warming NaOCl to 60 C
significantly increases the rate and effectiveness of tissue dissolution. It
has also been shown that NaOCl solutions were stable for 4 hours when
heated to 37 C (29). Sirtes et al (28) found that 1%, 2.62%, and 5.25%
solutions had an unchanged quantity of available chlorine for 1 hour at
45 C and 60 C, respectively. Therefore, in the present study, the NaOCl
solution was changed into a fresh one every 3 files to exclude the pos-
sibility of reduced activity of NaOCl during the experiment at higher tem-
peratures. One study (30) found that the temperature of a solution
preheated to 66 C decreased in vivo from 56.4 C to 45.4 C in 5 sec-
onds, to 37 C in 60 seconds, and to 35.7 C after 240 seconds. One of
the purposes of the present study was to evaluate the corrosion effects of
NaOCl on different NiTi files at high temperature. The constant temper-
ature was kept in each group during the experimental process to mini-
mize the effect of confounding factors. Therefore, conclusions from the
results must be drawn with caution. However, it seems clear that 1 area
requiring particular focus in future file manufacturing is the relation-
ship of the austenite start (As) temperature, the austenite finish (Af) tem-
perature, and body temperature. High transformation temperatures
may mean a smaller decrease in file fatigue resistance at body temper-
ature, as found in the present study with the Vortex files.
In agreement with previous findings (8, 10), the present results
showed that the fatigue life of heat-treated NiTi files (Vortex and K3XF)
was longer than non–heat-treated files (K3), which is likely to be a
consequence of greater flexibility caused by the heat treatment. Ther-
momechanical treatment of NiTi files has a high impact on their trans-
formation behavior (10–12). Proprietary heat treatments increase the
so-called As and Af temperatures, which indicate the temperatures
where transformation of the metallic structure from martensite to
austenite starts and is completed (finished). In short, increasing the
Af by heat treatment extends the temperature range in which the files
are still at the more flexible martensite phase. Although most conven-
tional superelastic NiTi files have an Af temperature at room temper-
ature or below, heat-treated files usually have an Af between 30 C and
55 C (31, 32). Differential scanning calorimetry analyses have shown
that the Af for the Vortex, K3XF,and K3 files are approximately 54 C,
25 C, and 18 C, respectively (31, 32). In other words, both K3 and
K3XF have an austenite structure, whereas Vortex has a mostly
martensite structure at body temperature. Indeed, there was no
significant difference in the fatigue resistance of Vortex files between
room and body temperatures in the present study, whereas the
fatigue life of K3 and K3XF at body temperature was significantly
shorter than at room temperature. Interestingly, De Vasconcelos
et al (12) and Plotino et al (23) reported shortened Nf for Vortex
Blue files (Dentsply Tulsa Dental Specialties) at body temperature.
Vortex Blue files are made from M-Wire and have design features
similar to Vortex files; however, the proprietary heat treatment process
is different. The Af temperature of Vortex Blue is 33 C, which is much
lower than the 54 C Af temperature of Vortex files (31). Under the
relationship of the file’s Af temperature and the temperature at the
site, the fatigue resistance of the Vortex file decreased when the tem-
perature was increased to 60 C.
1850 Huang et al.
Within the limitations of this study, the ceramic model used in this
study allowed the examination of the fatigue resistance of NiTi files un-
der a potentially highly corrosive environment at different temperatures.
The fatigue life of NiTi files in 5.25% NaOCl was only slightly shorter than
in water, with no statistically significant difference. Vortex files with a
reported Af temperature of over 50 C showed only slight reduction of
cyclic fatigue resistance at body temperature, whereas at 60 C the fa-
tigue resistance was greatly reduced. Contrary to the Vortex file, the fa-
tigue resistance of K3 and K3XF files decreased clearly at body
temperature. The future emphasis in new files should be directed to
the relationship of the As and Af temperatures to body temperature.
Acknowledgments
Xiangya Huang and Ya Shen contributed equally to this study.
The authors thank SybronEndo for donating the files used in
this study.
Supported in part by the Guangdong Medical Science and
Technology Research Foundation (#B20111118) and the Canada
Foundation for Innovation (CFI fund # 32623).
The authors deny any conflicts of interest related to this study.
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