doi:10.1111/iej.
12924
REVIEW
New thermomechanically treated NiTi alloys – a
review
€fer2
J. Zupanc1, N. Vahdat-Pajouh1 & E. Scha
1
Department of Periodontology and Operative Dentistry, Westphalian Wilhelms-University, M€
Interdisciplinary Ambulance in the School of Dentistry, M€
Abstract
Zupanc J, Vahdat-Pajouh N, € fer E.
Scha
thermomechanically treated NiTi alloys
International Endodontic Journal, 51, 1088–1103, 2018.
In the past 10 years, several proprietary processing
procedures for nickel titanium (NiTi) alloy were devel-
oped to improve the mechanical properties of NiTi
endodontic instruments. Beside specific thermal and
mechanical treatments, manufacturers introduced
several machining procedures (e.g. twisting, electrical
discharge machining), as well as techniques for final
surface finishing. NiTi alloys used for endodontic
instruments can be subdivided into instruments that
mainly contain the austenite phase (austenitic: con-
ventional NiTi, M-Wire, R-Phase) and those mainly
containing the martensite phase (martensitic: CM
Wire, Gold and Blue heat-treated NiTi). Thermome-
chanically treated NiTi alloys have been reported
to be more flexible with improved cyclic fatigue
Introduction
Nickel titanium (NiTi) endodontic instruments have
been reported to be more flexible with an increased
torsional fracture resistance when compared to stain-
less steel instruments (Walia et al. 1988). These
enhanced characteristics allowed a substantial
improvement in engine-driven endodontic instru-
ments (Fife et al. 2004). Though, fracture of rotary
NiTi instruments remains an inadvertent incident
Correspondence: Edgar Sch€ afer, Central Interdisciplinary
Ambulance, Waldeyerstr. 30, D-48149 M€ unster, Germany
(fax: + 251/834 3749; e-mail: eschaef@uni-muenster.de).
1088 International Endodontic Journal, 51, 1088–1103, 2018
unster; and 2Central
unster, Germany
resistance and greater angle of deflection at failure
when compared to conventional NiTi. These
New
enhanced properties may be attributed to a modified
– a review.
phase composition containing varying amounts of R-
phase and martensite. Endodontic instruments made
of austenitic alloys possess superelastic properties
because of stress-induced martensite transformation
and consequently tend to spring-back to their original
form after deformation. In contrast, the martensitic
instruments can easily be deformed due to the reori-
entation of the martensite variants and show a shape
memory effect when heated. The use of martensitic
alloy results in more flexible instruments, with an
increased cyclic fatigue resistance compared with aus-
tenitic alloy.
Keywords: austenitic NiTi alloy, controlled
memory, martensitic NiTi alloy, metallurgical proper-
ties, thermomechanical treatment.
Received 21 December 2017; accepted 16 March 2018
during clinical use (Pruett et al. 1997, Gutmann &
Gao 2012). Beside variations in the design of NiTi
instruments, manufacturers have introduced several
proprietary manufacturing procedures including ther-
mal, mechanical and surface treatment to improve
the mechanical properties of NiTi alloys, in order to
produce instruments with enhanced resistance to
fracture and increased flexibility.
Preparation errors during canal instrumentation
(e.g. zips, ledges, perforations or canal transporta-
tions) can occur. Both, stainless steel and NiTi
endodontic instruments tend to straighten within a
curved root canal resulting in a lateral force upon the
root canal wall. To minimize this lateral force and to
ensure a centred preparation, great flexibility is a
© 2018 International Endodontic Journal. Published by John Wiley & Sons Ltd

fundamental requirement of endodontic instruments
(Craig et al. 1968, Viana et al. 2010). It has been
shown that root canal preparation with engine-driven
NiTi endodontic instruments results in significantly
less canal transportation and fewer preparation errors
compared with stainless steel hand instruments (Glos-
sen et al. 1995, Short et al. 1997, Sch€ afer 2001,
Sch€afer & Lohmann 2002).
Fracture of NiTi endodontic instruments
In spite of the advanced flexibility of NiTi alloy com-
pared with stainless steel, fracture of NiTi endodontic
instruments remains a problem in clinical practice
(Pruett et al. 1997, Sattapan et al. 2000, Bergmans
et al. 2001, Gutmann & Gao 2012). Fracture of
rotary NiTi instruments occurs in different ways: due
to torsional failure or due to cyclic fatigue (Sattapan
et al. 2000). The total cyclic life of NiTi endodontic
instruments can be divided into two stages: starting
with crack initiation in which microcracks form and
start to grow preferentially along specific crystallo-
graphic planes or grain boundaries followed by crack
propagation until final fracture (Gao et al. 2010).
Cyclic fatigue resistance is usually measured by the
time until fracture occurs or by the number of cycles
to fracture (NCF). Fracture due to torsion occurs
when the tip or another part of the instrument binds
within the canal whilst the handpiece keeps turning
resulting in the elastic limit of the NiTi endodontic
instrument being exceeded (Martın et al. 2003). It is
important to mention that torsional stress occurs dur-
ing every cutting action in the canal. Torsional tests
of endodontic instruments are carried out by measur-
ing the maximum torque and angle of rotation during
fracture.
Numerous studies have examined the resistance to
fracture of NiTi files. Beside variations in the experi-
mental design, and testing model, many studies have
not considered the intracanal temperature, even
though a change in environmental temperature pro-
foundly affects the mechanical properties of NiTi
endodontic instruments. Recently it was shown that
increasing the environmental temperature from room
to intracanal temperature significantly decreases cyc-
lic fatigue resistance (de Vasconcelos et al. 2016,
Dosanjh et al. 2017, Grande et al. 2017, Plotino et al.
2017). It is important to mention that in addition
to the specific alloy the mechanical properties of
endodontic instruments are affected by the design and
diameter of the instruments as well as the working
© 2018 International Endodontic Journal. Published by John Wiley & Sons Ltd
Zupanc et al. Thermomechanically treated NiTi alloys
motion (rotary or reciprocation). The maximum tor-
que increases with greater instrument diameter,
whilst flexibility decreases (Melo et al. 2008, Ninan &
Berzins 2013). Cyclic fatigue resistance decreases as
the maximum tensile strain amplitude on the surface
of the instruments increases, which occurs at the
maximum bending point during shaping of a curved
root canal (Melo et al. 2008). Because the tensile
strain amplitude on the surface of an instrument
increases with diameter, small instruments with little
taper have increased cyclic fatigue resistance com-
pared with large and greater tapered instruments
(Bahia & Buono 2005). Reciprocal motion revealed
an enhanced cyclic fatigue resistance compared with
rotary motion (Pedull a et al. 2013, Perez-Higueras
et al. 2013).
Metallurgical and mechanical
characteristics of NiTi alloy
NiTi alloy was developed by the Naval Ordnance Lab-
oratory (White Oak, MD, USA) (Buehler et al. 1963).
It was named Nitinol; an acronym for nickel (ni), tita-
nium (ti) and Naval Ordnance Laboratory (nol).
NiTi alloy used in endodontic instruments contain
approximately 56 wt% nickel and 44 wt% titanium
resulting in a nearly one-to-one atomic ratio (equia-
tomic) (Thompson 2000). This equiatomic NiTi alloy
can exist in two different temperature-dependent crys-
tal structures named austenite (high-temperature or
parent phase, with a cubic B2 crystal structure) and
martensite phase (low-temperature phase, with a mon-
oclinic B190 crystal structure) (Shen et al. 2013a) and
possesses typical characteristics which are superelastic-
ity (SE) and shape memory effect (SME) (Table 1).
These properties occur as a result of the austenite-to-
martensite transition (martensitic transformation),
which can be induced by stress or temperature (Fig. 1).
Under certain conditions (e.g. ageing at temperatures
Table 1 Definition of the martensitic transformations
Superelasticity (SE) = Complete recoverable elastic
pseudoelasticity deformation up to 8% strain due
to phase transformation between
stable austenite and stress-induced
martensite phase (Fig. 1)
Shape memory Ability of deformed NiTi to recover
effect (SME) its original shape when heated
due to phase transformation of
stable deformed martensite to
stable austenite phase (Fig. 1)
International Endodontic Journal, 51, 1088–1103, 2018 1089
 Thermomechanically treated NiTi alloys Zupanc et al.

Figure 1 Martensitic transformations. (a) Superelasticity (SE) at ambient temperature above austenite finish temperature (Af).
(b) Shape memory effect (SME). For the martensite reorientation (MR), less stress is required than for stress-induced martensite
(SIM) transformation. (Ms = martensite start temperature).

around 400 °C to cause the precipitation of Ti3Ni4

phase, substitution of a third element (iron, alu-
minium) or heat treatment after cold working to create
rearranged dislocation structures), a rhombohedrally
distorted phase (R-phase) may appear prior to the
transformation to martensite (Miyazaki & Otsuka
1986). This R-phase transformation is established as a
martensitic transformation itself that competes with
the subsequent martensitic transformation (Otsuka &
Ren 2005). The stress occurring during this cubic
(austenite) to rhombohedrally (R-phase), respectively,
monoclinic (martensite) lattice transformation is
released by twinning of the new phase structure
Figure 2 Temperature hysteresis diagram of NiTi alloy. (Ms)
(twinned R-phase or martensite) (Fig. 1). Martensite
martensite start temperature, (Mf) martensite finish tempera-
exhibits a lower elastic modulus (about 30–40 GPa)
ture, (As) austenite start temperature, (Af) austenite finish
than austenite (about 80–90 GPa) (Ammon 2014),
temperature.
and the elastic modulus of the R-phase is even lower
than that of martensite (Kuhn & Jordan 2002).
The phase composition and consequently the Hence, a change in the transformation tempera-
mechanical properties of NiTi alloy are dependent on tures (Ms, Mf, As, Af; Fig. 2) of the utilized NiTi alloy,
the ambient temperature and whether the alloy is which can be achieved by thermal and mechanical
cooled or heated to this temperature (Fig. 2). If the treatment or variation in the chemical composition
temperature is above austenite finish temperature (Miyazaki & Otsuka 1986, Alapati et al. 2009, Kim
(Af), the alloy is in austenitic state, that is, it is stiff, et al. 2010), is the most important tool for manufac-
hard and possesses superior superelastic properties turers to alter the phase composition and conse-
(Zhou et al. 2013). If the temperature is below quently the mechanical properties of the NiTi alloy.
martensite finish temperature (Mf), the NiTi alloy is in The transformation temperatures are usually exam-
martensitic state, that is, it is soft, ductile, can easily ined by DSC (differential scanning calorimetry) analy-
be deformed and possesses the shape memory effect sis. Concerning the phase constitution, other
(Zhou et al. 2013). Because of the reorientation techniques such as XRD (X-ray diffraction), metallo-
capacity of the twinned phase structure, martensite graphic examination and SEM (scanning electron
has a superior cyclic fatigue resistance compared with microscopy) are needed to confirm the findings of the
austenite (Shen et al. 2013a,b). DSC analysis (Zhou et al. 2013).

1090 International Endodontic Journal, 51, 1088–1103, 2018 © 2018 International Endodontic Journal. Published by John Wiley & Sons Ltd
 Zupanc et al. Thermomechanically treated NiTi alloys

NiTi raw wires are provided by manufacturers in a
cold-worked state. Cold working significantly increases
the incidence of crystal lattice defects in NiTi alloy and
results in a microstructure that contains residual
martensite in an austenitic matrix with an impeded
mobility of the martensite twin boundaries (Zinelis et al.
2007). Heat treatment of the cold-worked NiTi alloy in a
temperature range around 450–550 °C is able to release
the internal stresses and reduces the defects of the crys-
tal lattice by giving the atoms enough thermal energy to
rearrange themselves (Zinelis et al. 2007). Conse-
quently, heat-treated NiTi alloy has significantly
increased cyclic fatigue resistance and higher transfor-
mation temperatures than not heat-treated NiTi alloy
(Zinelis et al. 2007, 2010). Additionally to the heat
treatment procedure, the superelastic properties of NiTi
alloy can be trained by thermal cycling under mechani-
cal stress (usually in a cold bath at about 0–10 °C and a
hot bath at about 100–180 °C under constraint elonga-
tion at 1–4%) (Berendt 2007), resulting in an easier
formation of the ‘trained’ martensite upon loading
(Otsuka & Ren 2005). The mechanical properties,
transformation temperatures and phase compositions of
NiTi endodontic alloy are mainly influenced by the
unknown, proprietary thermomechanical treatment
rather than the elemental composition (Zinelis et al.
2010).
A modified phase composition due to changed trans-
formation temperatures is the main difference between
thermomechanically treated and conventional NiTi
alloy. Whilst conventional NiTi alloy contains austenite
(Thompson 2000), thermomechanically treated NiTi
alloy additionally contains varying amounts of R-phase
and martensite under clinical conditions (Shen et al.
2011a, Pereira et al. 2012, Iacono et al. 2017). These
modifications are supposed to lead to more flexible
endodontic instruments with an advanced resistance to
fracture (Table 2).
Austenitic NiTi alloy
To utilize the superelasticity of NiTi alloy, NiTi
endodontic instruments should mainly consist of
austenite phase (Zhou et al. 2013). Austenite can be

Table 2 Overview of NiTi alloy used for the manufacture of endodontic instruments

Alloy Phase composition/properties NiTi system

Conventional NiTi alloy Austenitic: Mtwo

OneShape
• superelastic ProFile
ProTaper Universal
Electropolishing RaCe, BioRaCe, iRace
F360, F6 Skytaper
R-phase Austenitic: Twisted File
Twisted File Adaptive
• superelastic K3XF (not twisted)
• twisted
M-Wire Austenitic with small amounts of R-phase and martensite: ProFile Vortex
ProFile GT Series X
• superelastic ProTaper Next
• two stage stress-induced transformation Reciproc
through an R-phase WaveOne
CM Wire Martensitic with varying amounts of austenite and R-phase: Hyflex CM
THYPOON Infinite Flex NiTi Files
• controlled memory effect V-Taper 2H
• deformable, pseudoplastic Hyflex EDM
Gold heat-treated • shape memory effect ProTaper Gold
Blue heat-treated • superior flexibility WaveOne Gold
• enhanced cyclic fatigue resistance ProFile Vortex Blue
• greater angle of rotation at fracture Reciproc Blue

• lower maximum torque

MaxWire Martensitic (20 °C), austenitic (35 °C): XP-endo Finisher
XP-endo Shaper
• shape memory effect
• superelastic

© 2018 International Endodontic Journal. Published by John Wiley & Sons Ltd International Endodontic Journal, 51, 1088–1103, 2018 1091
 Thermomechanically treated NiTi alloys Zupanc et al.
transformed to martensite by stress (e.g. insertion of
the instrument into a curved root canal). This effect
is called stress-induced martensite (SIM) transforma-
tion (Fig. 1). The transformation of the austenitic
cubic crystal lattice to the martensitic monoclinic
crystal lattice allows a complete recovery of the defor-
mation up to 8% strain (Thompson 2000). Because
the stress-induced martensitic state is not stable at
the present temperature, unloading of the endodontic
instrument (e.g. withdrawal of an instrument out of a
curved root canal) leads to retransformation to the
austenite phase and therefore to a spring-back of the
endodontic instrument to its original shape (Fig. 1).
In addition to superelasticity, NiTi alloy possesses a
lower elastic modulus compared with stainless steel
resulting in an advanced flexibility of NiTi endodontic
instruments (Viana et al. 2010).
Conventional NiTi alloy
Conventional NiTi endodontic instruments approxi-
mately contain 56 wt% nickel and 44 wt% titanium
(Thompson 2000). The austenite finish temperature is
below body temperature (Brantley et al. 2002, Pereira
et al. 2012). Hence, conventional NiTi endodontic
instruments mainly consist of the austenite phase and
possess superelastic properties (Thompson 2000).
These instruments have to be grinded rather than
twisted (Thompson 2000). The grinding process may
lead to defects on the surface of the NiTi instruments,
which are supposed to have negative effects concerning
fracture resistance, cutting efficiency and resistance to
corrosion (Thompson 2000, Kuhn et al. 2001, Ander-
son et al. 2007, Cheung et al. 2007, Lopes et al. 2010).
Electropolishing
Electropolishing (EP) is an established final surface
finishing process for metal workpieces that allows for
a controlled electrochemical removal of surface mate-
rial leading to a smoother surface with increased gloss
(Bonaccorso et al. 2008a, Lopes et al. 2016, 2017).
During manufacturing of NiTi endodontic instru-
ments, EP is used to remove surface irregularities,
cracks and residual stress that are caused by the pre-
vious grinding process. This is supposed to improve
fracture resistance, cutting efficiency and resistance to
corrosion (Kuhn et al. 2001, Bonaccorso et al. 2008a,
Bui et al. 2008).
Several studies revealed that the presence of micro-
cracks, surface debris and milling grooves can be
1092 International Endodontic Journal, 51, 1088–1103, 2018
reduced by EP (Tripi et al. 2006, Anderson et al.
2007, Bonaccorso et al. 2008b), although EP is not
able to inhibit the development of microfractures
(Herold et al. 2007). Most studies indicated an
advanced resistance to cyclic fatigue of electropolished
versus nonelectropolished instruments (Anderson
et al. 2007, Condorelli et al. 2010, Lopes et al. 2010,
2016, Praisarnti et al. 2010). In accordance with
these findings, SEM analysis of fractured surfaces
revealed that the cracks of nonpolished instruments
run along the machining grooves, whilst electropol-
ished instruments exhibited a fine irregular zigzag
crack pattern (Lopes et al. 2010). Only Bui et al.
(2008) found that EP significantly reduces the resis-
tance to cyclic fatigue whilst increasing the angle of
deflection at failure. Maximum torque at failure was
not affected by EP (Bui et al. 2008).
M-Wire
With the aim to produce a more flexible NiTi alloy with
enhanced cyclic fatigue resistance, Sportswire LLC
(Langley, OK, USA) developed a proprietary thermome-
chanical manufacturing procedure in 2007. The newly
developed NiTi alloy was named M-Wire (Gambarini
et al. 2008a). The starting material for the heat treat-
ment of M-Wire is a Nitinol composition consisting of
55.8  1.5 wt% nickel (Ni), 44.2  1.5 wt% titanium
(Ti) and trace elements less than 1 wt% (Berendt
2007). The austenite finish temperature of M-Wire was
found to be around 43–50 °C (Alapati et al. 2009,
Shen et al. 2011a, Pereira et al. 2012, Ye & Gao 2012,
Braga et al. 2014) and consequently well above Af of
conventional NiTi and body temperature, indicating
that M-Wire is not completely composed of austenite
under clinical conditions. According to this, various
metallurgical laboratory techniques (e.g. DSC, XRD,
and SEM) revealed that M-Wire contains austenite
phase with small amounts of martensite and R-phase
at body temperature (Alapati et al. 2009, Pereira et al.
2012, Ye & Gao 2012). Hence, M-Wire maintains a
superelastic state (Johnson et al. 2008).
M-Wire exhibits greater flexibility than convention-
ally processed NiTi wire (Montalv~ ao & Alcßada 2011,
Gao et al. 2012, Pereira et al. 2012, 2013). It is known
that the elastic moduli of martensite and R-phase are
lower than that of austenite. Thus, improved flexibility
of M-Wire could be attributed to the presence of these
two phases. Additionally, Pereira et al. (2012, 2013)
found that the stress-strain curve of M-Wire exhibits a
distinctive yielding phenomenon (Fig. 3), indicating
© 2018 International Endodontic Journal. Published by John Wiley & Sons Ltd

Figure 3 Schematic stress-strain diagram of conventional
NiTi (black) and M-Wire (red) displaying the yielding phe-
nomenon (YP) resulting in a lower initial elastic modulus of
M-Wire (ΔE1) compared with conventional NiTi (ΔE2). The
stress-plateau occurs due to stress-induced martensite (SIM)
transformation.
that a stress-induced R-phase formation occurs prior to
SIM transformation. As a result, M-Wire possesses a
lower initial elastic modulus compared with conven-
tional NiTi which can be seen by an initial lower incli-
nation of the loading curve (Pereira et al. 2012, 2013).
Furthermore, the stress-strain diagram shows that less
stress is required to induce martensite transformation
in M-Wire than in conventional NiTi (Pereira et al.
2012, 2013).
Whilst maintaining comparable torsional properties
(Johnson et al. 2008, Kramkowski & Bahcall 2009,
Gao et al. 2012), M-Wire was found to be signifi-
cantly more resistant to cyclic fatigue compared with
conventional NiTi alloy (Johnson et al. 2008, Larsen
et al. 2009, Al-Hadlaq et al. 2010, Gao et al. 2010,
2012, Pereira et al. 2013, Braga et al. 2014). The
Figure 4 Stress-strain-temperature diagram showing the shape memory effect of martensitic NiTi instruments (e.g. Hyflex CM).
The stress-plateau occurs due to martensite reorientation (MR).
© 2018 International Endodontic Journal. Published by John Wiley & Sons Ltd
Zupanc et al. Thermomechanically treated NiTi alloys
improved fatigue resistance could be explained by an
enhanced resistance to fatigue-crack initiation
because of the better reorientation capability of the
martensitic variants (Fig. 4) (Gao et al. 2010).
R-phase
In 2008, shortly after the introduction of M-Wire,
SybronEndo (Orange, CA, USA) developed another
manufacturing process to create a new rotary NiTi
system named twisted file (TF). The manufacturing
procedure of TF includes three new methods: R-phase
heat treatment, twisting of the metal wire and a spe-
cial surface conditioning (Larsen et al. 2009). The
twisting process is conducted by transforming a raw
NiTi wire in austenitic state through a proprietary
thermal process into R-phase. R-phase possesses a
lower shear modulus, and its transformation strain is
less than one-tenth of that of the martensite transfor-
mation (Wu et al. 1990, Otsuka & Wayman 1998).
Consequently, less stress is required to cause a plastic
deformation in R-phase allowing the twisting process
(Hou et al. 2011). After twisting, TF is converted back
to austenite by additional thermal procedures to
maintain its new shape (Hou et al. 2011). Meanwhile,
two more NiTi systems with proprietary R-phase tech-
nology were introduced (K3XF, TF Adaptive; Sybro-
nEndo). In contrast to TF and TF Adaptive (TFA), the
K3XF instruments are manufactured by traditional
grinding process with a post-machining R-phase heat
treatment. The twisted TFA instruments are used in a
new adaptive motion technology allowing for either a
rotary or reciprocating movement of the file depend-
ing on the intracanal torsional forces.
International Endodontic Journal, 51, 1088–1103, 2018 1093
 Thermomechanically treated NiTi alloys Zupanc et al.
DSC analysis revealed that the austenite finish tem-
perature of R-phase instruments is around 18–25 °C
(Hou et al. 2011, Shen et al. 2011a, 2013c, Braga
et al. 2013) indicating that these instruments mainly
contain superelastic austenite in the oral environment
(Hou et al. 2011).
In several studies, R-phase instruments revealed
superior resistance to cyclic fatigue (Gambarini et al.
2008a, Larsen et al. 2009, Kim et al. 2010, Pedull a instrument. Twinned martensite can be plastically
et al. 2011, 2012, Rodrigues et al. 2011, Bhagabati
et al. 2012, Bouska et al. 2012, Perez-Higueras et al.
2013, Bulem et al. 2013, Aminsobhani et al. 2015,
Ersoy et al. 2016) and superior flexibility compared
with conventional NiTi without heat treatment (Gam-
barini et al. 2008b,c, Hou et al. 2011, Shen et al.
2013c, Choi et al. 2016). The load-deflection curve of
TF instruments displays a narrower stress hysteresis
including a lower plateau on loading than conven-
tional NiTi (Hou et al. 2011, Shen et al. 2013c),
implying that less stress is required to induce SIM for-
mation whilst more austenite can be transformed to
martensite (Liaw et al. 2007). As a result of the
enhanced flexibility, the use of R-phase instruments
allows a more centred canal preparation with less
transportation than conventional NiTi rotary systems
(El Batouty & Elmallah 2011, Hashem et al. 2012,
Reddy et al. 2014, Rejula et al. 2017). R-phase
instruments reveal similar cyclic fatigue resistance in
comparison with those made of M-Wire (Bouska et al.
2012, Higuera et al. 2015). Concerning torsional
fracture, the R-phase instruments have a greater
angle of deflection at failure but a decreased maxi-
mum torque compared with M-Wire and conventional
NiTi instruments (Casper et al. 2011, Wycoff & Ber-
zins 2012, Choi et al. 2016, Elsaka et al. 2017).
Martensitic NiTi alloy
Martensite NiTi alloy is softer and more ductile than
austenite. Additionally, it can easily be deformed and
exhibits the shape memory effect when heated. The
fatigue-crack growth resistance of the martensite phase
was found to be superior to that of the stable austenite
(McKelvey & Ritchie 2001). Shen et al. (2013a) con-
sidered that a hybrid (austenite-to-martensite) phase
composition with a certain proportion of martensite is
more likely to have favourable fatigue resistance.
To produce endodontic instruments mainly contain-
ing the martensite phase, the transformation tempera-
tures of the NiTi alloy have to be raised (e.g. by
thermomechanical treatment). At a temperature
1094 International Endodontic Journal, 51, 1088–1103, 2018
above, the austenite finish temperature NiTi endodon-
tic instruments consist of austenite. Upon cooling, a
successive austenite-to-martensite transformation
occurs beneath the martensite start temperature. The
stress occurring during this cubic (B2) to monoclinic
(B190 ) lattice transformation is released by twinning
of the developed martensite (twinned martensite)
without macroscopic form changes of the endodontic
deformed under stress, leading to detwinning of the
lattice structure (deformed martensite). This transfor-
mation from twinned to deformed martensite is called
martensite reorientation (MR). Similar to SIM, the MR
enables deformation up to 8% strain without signifi-
cant increase of stress (Kaack 2002). By heating the
deformed instrument beyond the austenite finish tem-
perature (e.g. autoclaving), it will regain its original
shape by returning to the primary austenitic state
(Fig. 4). Thus, martensitic instruments are pseudo-
plastic and exhibit the shape memory effect upon
heating.
CM Wire
Controlled memory (CM) Wire which was introduced
in 2010 is the first thermomechanically treated NiTi
endodontic alloy that does not possess superelastic
properties at neither room nor body temperature
(Zhou et al. 2012). Because of a modified phase com-
position, CM Wire instruments can be deformed
because of reorientation of the martensite variants
(Shen et al. 2013a). Thus, in contrast to austenitic
NiTi files, CM Wire instruments do not tend to fully
straighten during the preparation of curved root
canals (Fig. 5). According to the manufacturer, this
controlled memory effect is supposed to reduce the
Figure 5 (a) Spring-back effect of austenitic NiTi alloys (b)
controlled memory effect of martensitic NiTi alloys.
© 2018 International Endodontic Journal. Published by John Wiley & Sons Ltd

incidence of preparation errors (Hyflex, http://www.
hyflex.info/fileadmin/dam/DATEN/HyFlex-CM/down
loads/allgemein/6846_05-13_HyFlex_CM_EN.pdf).
However, a reduced root canal transportation for
Hyflex CM (Coltene/Whaledent, Altst€atten, Switzer-
land) compared with superelastic NiTi instruments
(conventional NiTi, R-phase, M-Wire) was not con-
firmed in several studies (Kumar et al. 2013, B€ urklein
et al. 2014, Marceliano-Alves et al. 2015, Rubio et al.
2015, Saber et al. 2015). Only compared to Revo-S
(Micro-Mega, Besancßon, France), ProTaper Next
(Dentsply Sirona Endodontics, Ballaigues, Switzerland)
and Reciproc (VDW, Munich, Germany) Hyflex CM
have significantly less root canal straightening
(B€urklein et al. 2014, Marceliano-Alves et al. 2015,
Saber et al. 2015).
DSC analysis revealed that the austenite finish tem-
perature of CM Wire instruments is above intracanal
temperature (around 47–55 °C) (Shen et al. 2011a,
2013b). Iacono et al. (2017) found that unused
Hyflex CM instruments exhibit Af temperatures
around 32–37 °C, whilst the Af temperature for used
Hyflex CM instruments is about 54–61 °C. However,
XRD analysis of Hyflex CM and Typhoon CM (Clini-
cian’s Choice Dental Products, New Milford, CT, USA)
revealed that both new and used CM Wire instru-
ments are a mixture of austenite and martensite
structure with small amounts of the R-phase at room
temperature (Shen et al. 2011a, 2013b, Iacono et al.
2017).
CM Wire instruments have greater flexibility than
M-Wire and conventional NiTi instruments (Testarelli
et al. 2011, Pongione et al. 2012, Ninan & Berzins
2013, Santos Lde et al. 2013, Pereira et al. 2015,
Goo et al. 2017, Soares et al. 2017). The improved
flexibility is mainly be attributed to the fact that the
critical stress to induce martensite reorientation
(twinned to deformed martensite) in martensitic
instruments is much lower than the critical stress to
induce SIM transformation (austenite to deformed
martensite) in austenitic instruments (Fig. 1) (Zhou
et al. 2012). Despite increased flexibility, which is
considered to affect cutting efficiency negatively,
Hyflex CM instruments have an enhanced cutting effi-
ciency in lateral action compared to electropolished
and conventional NiTi instruments (Morgental et al.
2013, Peters et al. 2014).
CM Wire instruments have a significantly enhanced
cyclic fatigue resistance compared with M-Wire and
conventional NiTi instruments (Shen et al. 2011b,
2012, Plotino et al. 2014a, Capar et al. 2015, Goo
© 2018 International Endodontic Journal. Published by John Wiley & Sons Ltd
Zupanc et al. Thermomechanically treated NiTi alloys
et al. 2017, Soares et al. 2017, AlShwaimi 2018),
which might be attributed to their martensitic state.
CM Wire instruments exhibited a greater angle of
deflection at failure than M-Wire and conventional
NiTi, but the maximum torque was nearly equal (Cas-
per et al. 2011, Peters et al. 2012, Chang et al.
2016).
Electrical discharge machining (Hyflex EDM)
Coltene/Whaledent has introduced Hyflex EDM,
which is another rotary NiTi system manufactured
from CM Wire. Hyflex EDM is the first endodontic
instrument that is manufactured via an electrical dis-
charge machining (EDM) process (Pirani et al. 2016).
According to the manufacturer, this innovative
machining process should harden the surface of the
NiTi file, resulting in an improved fracture resistance
and superior cutting efficiency (Hyflex EDM, https://
www.coltene.com/fileadmin/Data/EN/Products/Endod
ontics/Root_Canal_Shaping/HyFlex_EDM/31328A_
HyFlexEDM_Brochure_US.pdf).
EDM is a well-known noncontact machining proce-
dure that allows precise material removal via pulsed
electrical discharge (Bojorquez et al. 2002, Danesh-
mand et al. 2013). For EDM, both the machining tool
(electrode) and the workpiece have to be electrically
conductive (Daneshmand et al. 2013). Embedded in a
dielectric liquid, the machining tool is moved towards
the workpiece until the gap is small enough so that
the applied voltage is able to ionize the dielectric liq-
uid (Bojorquez et al. 2002). The resulting spark
vaporizes small particles from the workpiece, which
resolidify in the dielectric liquid and are subsequently
flushed away (Fig. 6) (Bojorquez et al. 2002), EDM
does not require direct contact with the workpiece,
which eliminates the chance of mechanical stress as
in the traditional grinding process (Singh et al. 2004).
EDM produces a crater-like surface, which seems not
to compromise the integrity of the instrument even
after multiple clinical applications (Pirani et al. 2016).
Uslu et al. (2018) examined the surface topographies
of intact Hyflex CM and EDM files before and after
root canal preparation using three-dimensional optical
profilometry. Whilst the increase in surface roughness
values in the Hyflex EDM group was not significant,
Hyflex CM had significantly higher surface alterations
compared with Hyflex EDM after preparation of
severely curved root canals (Uslu et al. 2018).
The transformation temperatures Ms, As and Af for
new Hyflex EDM instruments were found to be higher
International Endodontic Journal, 51, 1088–1103, 2018 1095
 Thermomechanically treated NiTi alloys Zupanc et al.
Figure 6 Electrical discharge machining. (1) Ionization of
the dielectric liquid (2) Spark (3) Vaporization of a small par-
ticle (4) Resolidification.
than for Hyflex CM indicating a changed phase com-
position (Iacono et al. 2017). Optical metallographic
analysis of Hyflex EDM revealed a microstructure
mainly composed of lenticular grains (assumed to be
martensite) alternating with large flat grains (as-
sumed to be austenite) (Pirani et al. 2016). In con-
trast, XRD analysis revealed that Hyflex EDM consists
of martensite and substantial amounts of R-phase,
whilst Hyflex CM was a mixture of martensite and
austenite (Iacono et al. 2017). It is known that the R-
phase occurs in aged NiTi alloy with Ti3Ni4 precipita-
tion (Otsuka & Ren 2005), which could be detected
in Hyflex EDM instruments (Iacono et al. 2017). The
absence of austenite in Hyflex EDM files could be
explained by its increased austenite start temperature
(As  42 °C) compared with Hyflex CM (As  21 °C)
preventing the formation of austenite at either room
or body temperature (Shen et al. 2013b, Iacono et al.
2017).
In accordance with these findings, several studies
proved that Hyflex EDM exhibits a significantly
increased cyclic fatigue resistance compared with
Hyflex CM, M-Wire and conventional NiTi instru-
ments (Kaval et al. 2016, Pedull a et al. 2016, Pirani
et al. 2016, Goo et al. 2017, G€ undo € urek
gar & Ozy€
2017, Iacono et al. 2017). The flexibility of Hyflex
EDM was found to be similar to other CM Wire
instruments (Goo et al. 2017, Iacono et al. 2017).
Hyflex EDM has been reported to create a centred root
canal preparation, respecting the original root canal
€ urek et al. 2017, Pinheiro et al. 2018,
anatomy (Ozy€
Venino et al. 2017). In addition, Hyflex EDM instru-
ments revealed a greater angle of rotation at fracture
1096 International Endodontic Journal, 51, 1088–1103, 2018
but a lower torque to fracture than M-Wire instru-
a et al. 2016).
ments (Pedull
Despite reduced austenite phase, Hyflex EDM instru-
ments exhibited a higher hardness than conventional
manufactured CM Wire files (Iacono et al. 2017), con-
sequently proving the surface hardening effect of
EDM. At the moment, there is no study available that
confirms a superior cutting efficiency of Hyflex EDM.
Gold and Blue heat-treated instruments
In 2011, Dentsply Tulsa Dental (Tulsa, OK, USA)
introduced ProFile Vortex Blue, which was the first
endodontic instrument possessing a distinctive blue
colour. There are now two Gold and two Blue heat-
treated NiTi systems available. Two of them are used
in a rotary (ProFile Vortex Blue; ProTaper Gold,
Dentsply Sirona Endodontics), and two of them are
used in a reciprocating motion (Reciproc Blue, VDW;
WaveOne Gold, Dentsply Sirona Endodontics). These
instruments also exhibit a controlled memory effect
and can be deformed (Plotino et al. 2014b). The main
difference between CM Wire and the Gold, respec-
tively, Blue heat-treated instruments is that these files
are ground before they go through a proprietary post-
machining heat treatment (Pereira et al. 2015).
For Vortex Blue instruments, it is known that a vis-
ible titanium oxide layer is responsible for the distinc-
tive blue colour that remains on the surface as a
result of the post-machining heat treatment (Hu et al.
2014). The austenite finish temperature for Vortex
Blue was found to be around body temperature
(38.5 °C), whilst the martensite start temperature is
approximately 31 °C (Shen et al. 2015). Blue heat-
treated instruments exhibited less Vickers surface
hardness than M-Wire instruments (Gao et al. 2012,
De-Deus et al. 2017). Considering the controlled
memory behaviour of the Blue heat-treated file, it can
be assumed that despite lower transformation temper-
atures these instruments contain a greater amount of
stable martensite than M-Wire, leading to a softer
and more ductile NiTi alloy. At the moment, there
are no studies available examining the phase compo-
sition by XRD, metallographic examination or SEM to
confirm this assumption. For Gold heat-treated instru-
ments, a surface layer may also be responsible for the
distinctive colour. DSC analysis of ProTaper Gold
revealed approximately 50 °C for austenite finish tem-
perature (Hieawy et al. 2015), indicating that these
instruments also mainly contain martensite or R-
phase under clinical conditions.
© 2018 International Endodontic Journal. Published by John Wiley & Sons Ltd

All Gold and Blue heat-treated files demonstrated
enhanced flexibility and fatigue resistance compared
with conventional NiTi and M-Wire instruments (Gao
et al. 2012, Nguyen et al. 2014, Plotino et al. 2014b,
2017 Duke et al. 2015, Hieawy et al. 2015, Elnaghy
& Elsaka 2016a, 2017a, Kaval et al. 2016, Ozy€ € urek
2016, Uygun et al. 2016, Adıg€ uzel & Capar 2017,
De-Deus et al. 2017, Keskin et al. 2017, Topcßuo glu
et al. 2017, Topcßuo glu & Topcßuoglu 2017), which
might be attributed to their martensitic state.
Only Hyflex EDM files have a significantly increased
cyclic fatigue resistance compared with ProTaper
Gold, WaveOne Gold and Reciproc Blue (Kaval et al.
2016, G€ undo € urek 2017). All four Gold and
gar & Ozy€
Blue heat-treated NiTi systems create well-centred
preparation even in severely curved root canals (Elna-
ghy & Elsaka 2016b, Silva et al. 2016, Duque et al.
€ urek et al. 2017, Pinheiro et al. 2018).
2017, Ozy€
Kaval et al. (2016) reported that ProTaper Gold had a
significantly higher maximum torque than Hyflex
EDM and ProTaper Universal (Dentsply Sirona
Endodontics), whilst Hyflex EDM had an increased dis-
tortion angle. ProTaper Gold was found to be more
effective in lateral cutting action than ProTaper
Universal (Vasconcelos et al. 2018). This could be
explained by the relatively harder surface layer of the
Gold and Blue heat-treated instruments that might
compensate the decreased microhardness (Gao et al.
2012).
MaxWire
Recently, FKG Dentaire introduced another proprietary
thermomechanically treated NiTi alloy named Max-
Wire (Martensite-Austenite-electropolish-fileX), which
is the first endodontic NiTi alloy that combines both
shape memory effect and superelasticity in clinical
application. At the moment, there are two instruments
available that are made of MaxWire; the XP-endo Sha-
per and XP-endo Finisher (both FKG Dentaire). Whilst
these instruments are relatively straight in their M-
phase (martensitic state) at room temperature, they
change to a curved shape when exposed to intracanal
temperature due to a phase transformation to A-phase
(austenitic state) (XP-endo Finisher, http://www.fkg.
ch/sites/default/files/201610_fkg_xp_endo_finisher_b
rochure_v2_en_web_0.pdf.). Thus, these instruments
exhibit a shape memory effect when inserted into the
root canal (M-phase to A-phase) and possess superelas-
ticity during preparation. The curved shape is claimed
to enable a preparation of complex root canal
© 2018 International Endodontic Journal. Published by John Wiley & Sons Ltd
Zupanc et al. Thermomechanically treated NiTi alloys
morphologies with the potential to adapt to canal irreg-
ularities.
The XP-endo Shaper revealed significantly
increased cyclic fatigue resistance compared with
Hyflex CM, Vortex Blue and iRaCe (FKG Dentaire)
(Elnaghy & Elsaka 2017b, Silva et al. 2018), but had
less torsional resistance compared with Vortex (Dents-
ply Tulsa) and FlexMaster (VDW) (Elnaghy & Elsaka
2018, Silva et al. 2018). It is important to mention
that the special low taper design (0.01) of the XP-
endo Shaper instrument profoundly affects its cyclic
and torsional resistance. It is well known that a smal-
ler diameter increases the cyclic fatigue and reduces
the torsional resistance of NiTi rotary instruments
(Melo et al. 2008, Ninan & Berzins 2013). Because of
the comparison of instruments with very different
diameters, these studies might be of low evidence
when comparing the mechanical properties of Max-
Wire to other NiTi alloy. At the moment, there are
no studies available examining the transformation
temperatures, phase composition and flexibility of
MaxWire instruments.
Conclusion and consequences for clinical
practice
Thermomechanical treatment of NiTi alloy allows a
change in the phase composition leading to the
appearance of martensite or R-phase under clinical
conditions. Whilst M-Wire and R-phase instruments
maintain an austenitic state, CM Wire, as well as the
Gold and Blue heat-treated instruments, is composed
of substantial amounts of martensite.
The austenitic instruments possess superelastic
properties and reveal high torque values at fracture.
Thus, these files are appropriate to shape straight or
slightly curved root canals. Additionally, the use of
austenitic alloy in pathfinding instruments may com-
pensate for the decreased torque resistance caused by
the smaller diameter of these files.
Due to an increased amount of the martensite
phase, martensitic instruments are more flexible with
an enhanced resistance to cyclic fatigue and reveal a
greater angle of rotation but lower torque at fracture.
Cyclic fatigue is known to occur more likely in com-
plex curvatures and root canal anatomies. Thus,
martensitic instruments should be preferred in cases
of severely curved root canals or those with a double
curvature. Moreover, martensitic instruments are
prebendable, which can be useful when trying to
bypass ledges.
International Endodontic Journal, 51, 1088–1103, 2018 1097
 Thermomechanically treated NiTi alloys Zupanc et al.
Conflict of interest
The authors have stated explicitly that there are no
conflict of interests in connection with this article.
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