journal of the mechanical behavior of biomedical materials 29 (2014) 295308

Available online at www.sciencedirect.com

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Review Article

Thermal cycling for restorative materials:

Does a standardized protocol exist in laboratory
testing? A literature review

Anna Lucia Morresia, Maurizio DAmarioa,n, Mario Capogrecoa,

Roberto Gattob, Giuseppe Marzob, Camillo DArcangeloc, Annalisa Monacob
a
Unit of Restorative Dentistry, Oral Pathology, Department of Life, Health and Environmental Sciences,
School of Dentistry, University of L'Aquila, L'Aquila, Italy
b
Department of Life, Health and Environmental Sciences, School of Dentistry, University of L'Aquila, L'Aquila, Italy
c
Unit of Restorative Dentistry, Department of Oral Science, Nano and Biotechnology, G. D'Annunzio
University of Chieti, Italy

art i cle i nfo ab st rac t

Article history: In vitro tests continue to be an indispensable method for the initial screening of dental
Received 12 July 2013 materials. Thermal cycling is one of the most widely used procedures to simulate the
Received in revised form physiological aging experienced by biomaterials in clinical practice. Consequently it is
15 September 2013 routinely employed in experimental studies to evaluate materials performance.
Accepted 21 September 2013 A literature review aimed to elucidate test parameters for in vitro aging of adhesive
Available online 27 September 2013 restorations was performed. This study aims to assess whether or not a standardized

Keywords: protocol of thermal cycling has been acknowledged from a review of the literature.

Aging An exhaustive literature search, examining the effect of thermal cycling on restorative

Dental restorations dental materials, was performed with electronic database and by hand. The search was

In vitro tests restricted to studies published from 1998 to August 2013. No language restrictions were

Standardization applied. The search identied 193 relevant experimental studies. Only twenty-three

Thermal cycling. studies had faithfully applied ISO standard. The majority of studies used their own
procedures, showing only a certain consistency within the temperature parameter
(555 1C) and a great variability in the number of cycles and dwell time chosen. A wide
variation in thermal cycling parameters applied in experimental studies has been
identied. The parameters selected amongst these studies seem to be done on the basis
of convenience for the authors in most cases. A comparison of results between studies
would appear to be impossible. The available data suggest that further investigations will
be required to ultimately develop a standardized thermal cycling protocol.
& 2013 Elsevier Ltd. All rights reserved.

n
Correspondence to: Unit of Restorative Dentistry. Oral Pathology, Department of Life, Health and Environmental Sciences, School
of Dentistry, University of L'Aquila, Via Vetoio, Delta 6, 67010 Coppito, L'Aquila, Italy. Tel.: 39 862 434 785; fax: 39 0862 434 978.
E-mail address: mauriziodamario@gmail.com (M. D'Amario).

1751-6161/$ - see front matter & 2013 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.jmbbm.2013.09.013
296 journal of the mechanical behavior of biomedical materials 29 (2014) 295 308

Contents

1. Introduction. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 296
2. Materials and methods . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 296
2.1. Study inclusion and exclusion criteria . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 296
3. Results . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 297
4. Thermal cycling . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 297
4.1. Temperature . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 298
4.2. Dwell times. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 299
4.3. Number of cycles . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 299
5. Conclusions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 302
References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 302

1. Introduction valuable in predicting biomaterials clinical performance when

Over the last few decades, signicant improvements have been
made in the eld of dental materials, so actually modern resto-
rative dentistry can count on a wide range of materials used for
dental rehabilitations.
The long term success of modern dental restoratives is
limited by their durability in the oral environment (Freeman
et al., 2012). Longevity and efciency are characteristics that
should ideally be provided from each product; however, these
properties are still goals to be achieved.
Restorative materials must withstand a harsh environ-
ment, which varies from patient to patient. Mastication
forces, occlusal habits, dietary factors, humidity and tem-
perature uctuations all contribute to uncontrollable factors
that may affect materials longevity (Cavalcanti et al., 2007).
For the evaluation of dental materials, well-conducted rando-
mized controlled clinical trials are considered the best method to
evaluate the quality of new systems; nevertheless there are
many limitations that do not allow this kind of study to be
routinely employed (Nikaido et al., 2002; Rocha et al., 2007;
Koyuturk et al., 2008). First, factors such as operator variability,
substrate differences, patient compliance and recall failure make
these tests complicated and their standardization impossible
(Nikaido et al., 2002). Second, clinical trials are costly and time-
consuming, so in adopting the view that dental materials evolve
rapidly, it is very important to understand that their clinical
success must be estimated in an easy, rapid and realistic way
(Koyuturk et al., 2008; Naumann et al., 2009).
In vitro simulations can be useful to predict the longevity
of dental materials, evaluating their mechanical and struc-
tural decay characteristics during clinical aging.
Although laboratory evaluation and in vitro studies cannot
exactly simulate conditions in the oral cavity, such as the
clinical environment, moisture and stresses inicted on teeth
and restorations alike, they can, to some extent, simulate the
oral cavity environment through aging procedures of teeth
and/or restorations. As a result, it appears that experimental
studies are, as far as possible, similar to the outcomes
obtained in clinical situations under complex occurrences in
the oral cavity (Khoroushi and Mansoori, 2012).
Many researchers are agreed, that while static tests can
obtain data over a longer time scale than that of mastication, it
can be a source of misleading results. Dynamic tests appear to
better mimic the cyclic masticatory loading to which dental
composites are clinically subjected which could be extremely
working under the cyclic solicitations generated by the human
body's physiological movements (Mesquita and Geis-Gerstorfer,
2008; Mazzitelli et al., 2012).
In the eld of laboratory research, out of the currently
available systems able to reproduce dynamic stresses, ther-
mal cycling is one the most widely used procedures that is
also widely accepted in international literature.
Many experimental studies have been published that use
thermal cycling regimes to test dental materials character-
istics (Doerr et al., 1996; Schuckar and Geurtsen, 1997; Wegner
et al., 2002; Bedran-de-Castro et al., 2004b; D'Amario et al.,
2010), following the publication of Gale and Darvell's review
over ten years ago (Gale and Darvell, 1999). The aim of the
subsequent review is to assess whether or not there is a
standardized protocol for thermal cycling processes, through
the appraisal of specic experimental studies published in
the last fteen years.
2. Materials and methods
The following review was conducted using the following search
strategy: MEDLINE database (via PubMed) was searched between
January 1998 and August 2013 by a single reviewer. Key words
used were: (thermal cycling OR thermocycling OR aging system)
AND (dentistry OR restorative dentistry). In addition, the follow-
ing journals were manually searched between January 1998 and
August 2013: Operative Dentistry, Journal of Prosthetic Dentistry,
Dental Materials, Journal of Dentistry, Journal of Endodontics,
Journal of Applied Oral Science, Journal of Adhesive Dentistry. No
language restriction was applied.
2.1. Study inclusion and exclusion criteria
One reviewer performed the study selection process in three
phases. In the rst stage, the studies were analyzed on the
basis of the title and abstract. Only studies of general interest
for the review were admitted to the next phase. In the second
phase, the studies were analyzed according to the following
inclusion criteria (A):
A.1 Experimental studies.
A.2 Studies involving materials used in restorative
dentistry.
A.3 Available abstract.
 journal of the mechanical behavior of biomedical materials 29 (2014) 295 308
Only studies that fullled all the inclusion criteria (A) were
admitted to the third phase, which consisted in analysis of
the preselected studies according to the following exclusion
criteria (B):
B.1 Studies reporting less than two thermal cycling
parameters.
B.2 Simultaneous use of different aging systems on the
same samples tested.
3. Results
A total of 2377 potentially relevant titles and abstracts were
found during the electronic and manual searches. During the
rst stage of study selection, 1754 publications were excluded
on the basis of evaluation of the title and abstract. During the
second phase, the complete full-text articles of the remaining
623 publications were evaluated. A total of 163 articles were
excluded because they did not fullled the inclusion criteria
(A). 267 full-text articles of the remaining 460 publications
were excluded because they met one or more of the exclusion
criteria (B). Finally, a total of 193 studies were included in the
present review. A owchart for the study selection process is
shown in Fig. 1.
4. Thermal cycling
Thermal cycling has been commonly employed in dental
research since 1952, when it was observed that chilled, restored
Fig. 1 Flowchart of the search strategy.
297
teeth produced an exudates from restoration margins when
the teeth were warmed (Youngson and Barclay, 2000). This
system is conventionally used to simulate the in vivo aging of
restorative materials by subjecting them to repeated cyclic expo-
sures to hot and cold temperatures, in a water baths in a bid to
reproduce thermal changes occurring in the oral cavity (El-Araby
and Talic, 2007; Catalbas et al., 2010; zel Bektas et al., 2012).
It stresses the bond between resin and tooth and, depend-
ing on the adhesive system, it may affect bond strength
(Helvatjoglu-Antoniades et al., 2004a; El-Araby and Talic,
2007); furthermore, it can affect the marginal integrity of
the restoration, causing the microleakage phenomenon that
may lead to staining, marginal breakdown, hypersensitivity
and development of pulpal pathology (Cenci et al., 2008).
Over the years, several studies have used this procedure to
test a wide number of dental materials with contradictory results
(Rossomando and Wendt, 1995; Schuckar and Geurtsen, 1997;
Hakimeh et al., 2000; Pazinatto et al., 2003; Kenshima et al., 2004),
probably due to differences in technical procedures and due to
the lack of a standardized methodology.
The consensus however is that the effects of thermal cycling
procedures might be related to the varieties of materials tested
and/or cavity design and/or the different test methods and/or the
properties of the hard tissues (Erdilek et al., 2009). Additionally, it
is well known that there is a wide range of temperature extr-
emes, transfer times between baths and dwell times to analyze
(Pazinatto et al., 2003).
Therefore the importance to determine a more realistic
thermal cycling regime, which is as close as possible to the
physiology of the oral cavity, is evidently necessary.
298 journal of the mechanical behavior of biomedical materials 29 (2014) 295 308
Three important factors to analyze, to better understand
the true validity and the eventual limits presented by
thermal cycling are: temperature, dwell time and number of
cycles.
4.1. Temperature
The measurement of temperature at specic sites within the
human oral cavity has been reported for well over a century.
Sublingual temperature is routinely used as an indicator of oral
temperature, and when measured under specic conditions it
approximates 37 1C for most individuals. It cannot, however, be
assumed that this represents the true resting temperature for all
sites within the oral cavity (Moore et al., 1999).
Temperature changes in the oral cavity are dynamic in
nature, so it's very hard to dene the range of temperature
closest to the physiology of the mouth.
It is essential to consider as many variables as possible
that could inuence the temperature of the teeth. The main
sources equilibrating temperature in the mouth are cheek,
tongue and periodontal tissue surrounding the teeth, which
acted as physical barriers, regulating the temperature dis-
tribution (Youngson and Barclay, 2000; Ernst et al., 2004).
Another important external factor is breathing. Many
authors suggest that air temperature, humidity and air
velocity when breathing can also radically alter the resting
mouth temperature, although, it seems this has only a slight
effect and mainly affects the front teeth of the upper jaw
(Gale and Darvell, 1999; Bishara et al., 2003; Ernst et al., 2004).
The foremost factor that leads to temperature change is the
intake of food and uids of various temperatures (Moore
et al., 1999; Ernst et al., 2004). Many authors suggest that
temperature uctuations during meals are frequent and
variable and that alterations in oral temperature occur
rapidly while the return to baseline temperature occurs more
slowly (Michailesco et al., 1995; Moore et al., 1999).
Fluids can be drunk within a range of 0100 1C but cooked
foods and frozen solids could provide temperatures to the
oral cavity outside of this range. The range of temperatures
that an individual can tolerate is likely to vary amongst the
population and may be affected by variables such as,
the number of teeth, the amount of exposed dentin present,
the degree of keratinization of the oral mucosa and the age
and the sex of the patient (Barclay et al., 2005).
Table 1 Intraoral temperature ranges measured during in vivo studies.
First author Min temp- Max temp (1C)
Moore et al. (1999) 5.658.5 1C (incisor sites)
7.954 1C (premolar sites)
Youngson and Barclay (2000) 15.468 1C
Ernst et al. (2004) 13.752.8 1C
Barclay et al. (2005) 070 1C
Mair and Padipatvuthikul (2010) 060/65 1C
Whatever the main contributing factor, it can be agreed that
each time the temperature changes, the teeth undergo thermal
stress.
Similarly, dental restoratives are also subjected to constant
and extreme changes in the oral environment brought about by
uctuations in temperature and pH (Wahab et al., 2003). Thermal
cycling, through temperature parameter, simulates the entrance
of hot and cold substances in the oral cavity, and shows the
relationship of linear coefcient of thermal expansion between
tooth and restorative material (Cenci et al., 2008).
The articial aging effect induced by thermal cycling can
be two-fold. Firstly hot water may accelerate hydrolysis of
non-protected collagen and extract poorly polymerized resin
oligomers, secondly due to the higher thermal contraction/
expansion coefcient of the restorative material (as com-
pared to that of tooth tissue), repetitive contraction/expan-
sion stresses are generated at the tooth-biomaterial interface.
This may result in cracks that propagate along bonded
interfaces, and once a gap is created, changing gap dimen-
sions can cause in and out ow of pathogenic uids, a
process known as percolation (De Munck et al., 2005).
Historically the principle difculty was to understand which
extreme values were to be used during simulated physiological
aging of biomaterials in the oral cavity. In fact a too extreme
range of temperature could overstress the material; in contrast,
a temperature range too limited could understress the material,
resulting in the production of clinically decient materials into
the dental community (Palmer et al., 1992).
In contrast with the temperature regime of 555 1C pro-
posed in ISO 11405 recommendations (International Standards
Organization, 1994), Gale and Darvell (1999), through an
extensive review of available data, concluded that the tem-
peratures commonly chosen by investigators were too
extreme to provide a representative simulation of temperature
uctuations in vivo. They opted instead for temperatures of
15 1C and 45 1C as their extreme values, and as the reference
resting temperature they opted for 35 1C, proposing the follow-
ing regime: 35 1C for 28 s., 15 1C for 2 s., 35 1C for 28 s., 45 1C
for 2 s.
In the last 15 years, a limited number of studies that
investigate the range of intraoral temperatures during function
have been published (Table 1), considering that thanks to the
buffering effect of the oral environment, the temperatures at the
tooth surface may never reach the actual temperatures of
ingested hot and cold uids (Li et al., 2002; Cenci et al., 2008).
Thermal cycling protocol proposed
No data
65 1C for 5 s.
45 1C for 25 s.
35 1C for 30 s.
10 1C for 5 s.
25 1C for 25 s.
35 1C for 30 s.
No data
No data
No data
 journal of the mechanical behavior of biomedical materials 29 (2014) 295 308
4.2. Dwell times
Dwell time is the period of time that the specimen is immersed
in a bath of a particular temperature (Schmid-Schwap et al.,
2011).
It corresponds to a latency period, which is required by the
oral capacity to reach its normal temperature again, after
consuming hot or cold food and drink.
Unfortunately, the choice of dwell times in experimental
studies appears arbitrary and no effect of dwell time on results
has been clearly established (Helvatjoglu-Antoniades et al.,
2004a; Kenshima et al., 2004; De Munck et al., 2005; Cavalcanti
et al., 2007).
Amaral et al. (2007) suggested that patients would not
tolerate direct contact of a vital tooth with extremely hot or
cold substances for extended period of time. For this reason,
several studies proposed to use shorter dwell times (10 s or
15 s), which may simulate more faithfully the abrupt changes
of temperature that occur in the oral cavity (Li et al., 2002;
Helvatjoglu-Antoniades et al., 2004a; Ernst et al., 2004). Doerr
et al. (1996) even decided to use a shorter dwell time (5 s) in
their experimental study. According to this proposed shorter
dwell time protocol, recently Schmid-Schwap et al. (2011)
suggested that in vivo maximum exposure time of a tooth to
an extremely hot or cold temperature, respectively, could be
considered 25 s, after which the tooth returns to the oral
temperature.
4.3. Number of cycles
The biggest problem has always been how to estimate the
number of cycles that correspond to one year of physiological
aging in the oral cavity. There are still no reports that have been
found about the number of thermal cycles per unit time in vivo.
Historically, every author who tried to suggest a specic
number of cycles for thermal cycling regimen, did not base
their conclusion on researched data, therefore the choice of
this parameter, in many studies, is widely dissimilar and
seems to be selected by convenience.
In other terms, the number of cycles is usually randomly set
which makes it difcult to compare published results (Amaral
et al., 2007).
Although the International Organization for Standardization
(International Standards Organization, 1994), in 1994 considered
a protocol of 500 cycles as appropriate in simulating the aging of
biomaterials, many studies suggest that 500 cycles are a limited
number to represent an adequate aging time (Gale and Darvell,
1999; Amaral et al., 2007; Stewardson et al., 2010).
Stewardson et al. (2010), for example, claimed that the 500
cycles would only correspond to the number of cycles esti-
mated to occur in less than 2 months in the mouth.
Michailesco et al. (1995) suggested 30 thermocycles occur
during each meal, which at three meals per day, equates to
about 33,000 thermocycles per year.
Gale and Darvell (1999) postulated that approximately
10,000 thermal cycles correspond to 1 year of clinical func-
tion. This estimate is based on the hypothesis that such
cycles might occur 20 to 50 times a day and it is accepted by
many authors (De Munck et al., 2005; Amaral et al., 2007;
Ulker et al., 2010; Xie et al., 2010; zel Bektas et al., 2012).
299
Ehrenberg and Weiner (2000) proposed a different system,
using thermalcycling and mechanical loading to simulate clinical
condition in the oral cavity. He hypothesized that 50,000 cycles
of occlusal loading and 8000 cycles of thermal cycling simulate
68 weeks of function in the oral cavity.
Bayne (2012) recently suggested that temperature of food
and liquids, quantities of them, and frequency of consump-
tion vary among individuals. If one should drink 100 ounces
of water per day, the potential for cold cycling per year is
50.000 cycles. If we are interested in the 10-year service life of
a restoration, then thermal cycling probably should be con-
ducted for 500.000 cycles or more.
The following table (Table 2) shows thermal cycling pro-
tocols applied in experimental studies published since 1998,
leaving out those published before that date, already included
in the previous review by Gale and Darvell (1999).
On the basis of the main thermal cycling protocols pro-
posed in the last twenty years by International Standards
Organization (1994) and by Gale and Darvell (1999) (Table 3),
only twenty-three studies have faithfully applied ISO standard
in their experimental protocols (Table 2). Four other studies
used only in part the previous protocol, adopting a shorter
dwell time (15 s) (Loguercio et al., 2002a,b; Amra et al., 2007).
However, there is no study that followed exactly the protocol
more recently introduced by Gale and Darvell (1999). The
majority of authors have used their own protocols and vari-
ables, in most cases, on the basis of convenience.
Temperature was the only parameter to show, over the
years, a constant use during the in vitro tests. According to
ISO standard, several studies reported temperatures of 5 1C
and 55 1C to test dental materials, considering these values as
the closest to the physiology of the oral cavity (Table 2).
However some authors have opted for a thermal cycling
regime that used more than 2 values of temperature:
Helvatjoglu-Antoniades et al. (2000, 2004a, 2004b) (53755
37 1C); Aguilar et al. (2002) (537 1C/3755 1C); Barclay et al.
(2002) (5225022 1C); Ghring et al. (2005) (5505 1C); Li et al.
(2002) (545 1C72 1C/555 1C72 1C); Upadhyay and Rao (2011)
(4376072 1C); Mathew et al., (2001) (6375437 1C); Staninec
et al. (2008) (53755 1C).
The choice of dwell time, instead, seems to be rather
arbitrary, showing a great variability in the different studies.
Popular dwell times of exposure to each temperature extreme
have ranged between 10 s, 15 s, 30 s, 55 s, 60 s, 2 min and 3 min
(Table 2).
Regarding the number of cycles determined by authors,
the choice was equally varied and not very well explained.
The number of cycles used in experimental studies published
in the last 15 years, have been ranged between 100 cycles
(Mathew et al., 2001; Stojanac et al., 2009) and 100.000 cycles
(Moreau et al., 2012). A small group of authors have followed
the principle that 10,000 cycles correspond to one year of
physiological aging in the oral cavity, as claimed by Gale and
Darvell (1999), Hatanaka et al. (2006), De Munck et al. (2005),
Saboia et al. (2009), Stewardson et al. (2010), Xie et al. (2010),
zel Bektas et al. (2012). Some studies selected an increased
number of cycles in their experimental protocols, to deter-
mine if there was a direct relation with properties modica-
tion of tested materials (Table 2). In any case, most of the
authors decided to apply a number of cycles less than the
300 journal of the mechanical behavior of biomedical materials 29 (2014) 295 308

Table 2 Thermal cycling regimens and experimental conditions.

First Author Number of Dwell Temperature

cycles time

Miyazaki et al. (1998) 3.00010.000 No 560 1C

30.000 data
Xalabarde et al. (1998), Wahab et al. (2003), Idriss et al. (2003), Deliperi et al. (2004), 500 30 s 555 1C
Cenci et al. (2004), Aysegl et al. (2005), Wattanawongpitak et al. (2006), Salim et al. (2006),
Deliperi et al. (2007), De V Habekost et al. (2007), Ferreira and Vieira (2008), Rajbaran et al.
(2009), Schmoldt et al. (2011), Rttermann et al. (2013)
Toledano et al. (1999) 1.000 30 s 660 1C
Fraunhofer et al. (2000) 5.000 1 min 555 1C
Helvatjoglou-Antoniades et al. (2000) 3000 15 s 53755
37 1C
Drfer et al. (2000) 1000 No 560 1C
data
Hakimeh et al. (2000) 2.880 1 min 460 1C
Stoll et al. (2000), Rosin et al. (2002), Gharizadeh et al. (2007), Erdilek et al. (2009) 2.000 30 s 555 1C
Kawano et al. (2001) 5.00010.000 1 min 460 1C
20.000
Chuang et al. (2001) 1.500 No 560 1C
data
Manhart et al. (2001), Sensi et al. (2005), Duarte et al. (2009b), Al-Saleh et al. (2010), 1.000 30 s 555 1C
Cehreli et al. (2010), Kasraei et al. (2011), Freeman et al. (2012), Poptani et al. (2012),
Khoroushi et al. (2013), Shaei et al. (2013),
Kubo et al. (2001), Kubo et al. (2003), Kubo et al. (2004a), Kubo et al. (2004b) 5.000 15 s 560 1C
Raskin et al. (2001) 250500 30 s 555 1C
Yoshida et al. (2001) 5000 1 min 460 1C
Yoshikawa et al. (2001) 300 30 s 460 1C
Medina Tirado et al. (2001) 2000 30 s 36072 1C
Mathew et al. (2001) 100 30 s 63754
37 1C
Wegner et al. (2002) 37.500 No 555 1C
data
Aguilar et al. (2002) 3.000 1 min 537 1C/37
55 1C
Loguercio et al. (2002a), Loguercio et al. (2002b), Amra et al. (2007) 500 15 s 555 1C
Neme et al, (2002), Brackett et al. (2004), Kenshima et al. (2004), Magalhes et al. (2005), 1.000 1 min 555 1C
Nalcaci and Ulusoy (2007), Lodovici et al. (2009)
Besnault and Attal (2002) 2.000 10 s 555 1C
Li et al. (2002) 5001.500 15 s 545 1C72 1C
5-55 1C72 1C
Ernst et al. (2002), Akili et al. (2002), Akili et al. (2003), Bitter et al. (2006), Janda et al. (2006), 5.000 30 s 555 1C
Papacchini et al. (2007), Ozcan et al. (2007), Kitayama et al. (2007), Monticelli et al. (2007),
Ernst et al. (2008), Koenraads et al. (2009), D'Arcangelo et al. (2009), Schmage et al. (2009),
Souza et al. (2010), Rinastiti et al. (2011), Sampaio et al. (2011), Dimitrouli et al. (2012),
Kuroda et al. (2012), Schmage et al. (2012), Bauer and Ilie (2013), Arslan et al. (2013)
Barclay et al. (2002) 3.000 55 s 52250
22 1C
Bedran de Castro et al., 2002 1500 60 s 55572 1C
Nikaido et al. (2002) 1256251.250 30 s 555 1C
2.000
Cardoso et al. (2002), Poskus et al. (2004) 700 1 min 555 1C
Aguiar et al. (2002), Aguiar et al. (2003), Purton et al. (2003) 3.000 1 min 555 1C
Drummond and Bapna (2003) 6.000 30 s 763 1C
Bishara et al. (2003), Bishara et al. (2007), Shaei and Memarpour (2009), Fabianelli et al. 500 20 s 555 1C
(2010), Pires et al. (2013)
Kim et al. (2003) 5.000 30 555 1C
35 s
Pazinatto et al. (2003) 5001.000 15 s 555 1C72 1C
2.5005.000
Civelek et al. (2003), Bedran-de-Castro et al. (2004a, 2004b, 2004c, 2004d), Lee et al. (2004) 2.000 No 555 1C
data
Tezvergil et al. (2003), Tezvergil et al. (2005) 6.000 30 s 555 1C72 1C
Cavalcante et al. (2003), Mitsui et al. (2006), Owens et al. (2006) 1.000 1 min 555 1C72 1C
Huang et al. (2004) 5001.000 15 s 555 1C
2.0003.000
Keski-Nikkola et al. (2004), Meri and Ruyter (2007) 12.000 30 s 555 1C
 journal of the mechanical behavior of biomedical materials 29 (2014) 295 308 301

Table 2 (continued )

First Author Number of Dwell Temperature

cycles time

Yazici et al. (2004) 200 1 min 460 1C

Helvatjoglu-Antoniades et al. (2004a) 5.000 15 s 537555 1C
Helvatjoglu-Antoniades et al. (2004b) 3.000 15 s 537555 1C
Ghring et al. (2005) 3.000 No 5505 1C
data
Ziskind et al. (2005) 750 1 min 46072 1C
Smisson et al. (2005) 9.000 20 s 555 1C
Naughton and Latta (2005) 850 1 min 555 1C
Dos Santos et al. (2005) 500 1 min 455 1C
De Munck et al. (2005), Senawongse et al. (2011) 20.000 30 s 555 1C
Fennis et al. (2005), Bell et al. (2005), Ozcan et al. (2005), Ozcan et al. (2006), Ovul et al. (2011) 6.000 30 s 555 1C
Martinhon and Vieira (2005), Corona et al. (2005), Do Nascimento et al. (2008), Ebrahimi et al. 500 1 min 555 1C
(2013)
Guders et al. (2006) 800 30 s 555 1C
Suzuki et al. (2006) 5000 20 s 455 1C
Kwon et al. (2006) 2000, 5000, 30 s 460 1C
10.000
Amano et al. (2006), Asaka et al. (2007) 10.00020.000 No 560 1C
data
Asaka et al. (2006) 10.000 30 s 560 1C
Hatanaka et al. (2006) 20.000 1 min 555 1C
Abdalla et al. (2007) 5.000 3 min 555 1C
El-Araby and Talic (2007), Shimizu et al. (2009) 10.000 1 min 555 1C
Nakata et al. (2007) 1.0002.000 30 s 555 1C
3.000
Knobloch et al. (2007), Sadeghi and Lynch (2009), Feitosa et al. (2010), Mortazavi et al. (2012), 1.500 30 s 555 1C
Davari et al. (2013)
Rocha et al. (2007) 2.000 1 min 555 1C
Stavridakis et al. (2007) 3.000 2 min 550 1C
Nam et al. (2007) 1000 30 s 055 1C
Frankenberger et al. (2007) 2500 No 555 1C
data
D'Arcangelo et al. (2007a, 2007b, 2007c), D'Arcangelo et al. (2008a) 10.000 30 s 555 1C
Elekdag-Turk et al. (2008) 2.0005.000 30 s 555 1C
Koyuturk et al. (2008), Ulker et al. (2010) 10.000 30 s 55572 1C
Cenci et al. (2008) 5001.000 30 555 1C
60 s
Staninec et al. (2008) 1000 520 53755 1C
5s
Saboia et al. (2009) 60.000 No 555 1C
data
Almeida et al. (2009) 500 1 min 55572 1C
Ikeda et al. (2009) 10.000 No 555 1C
data
Latta et al. (2009) 6000 20 s 555 1C
Stojanac et al. (2009) 100 60 s 45872 1C
Gaspar Junior Ade et al. (2009) 5000 15 s 55572 1C
Ritter et al. (2009) 1800 30 s 555 1C
Mazzoni et al. (2009) 40.000 30 s 555 1C
Duarte et al. (2009a) 20.000 15 s 560 1C
Stewardson et al. (2010) 10.000 30 s 1050 1C
Catalbas et al. (2010) 5.00010.000 30 s 555 1C
15.00020.000
Yuasa et al. (2010) 6.000 No 555 1C
data
Xie et al. (2010) 5.00010.000 30 s 555 1C
Korkmaz et al. (2010) 500 No 555 1C
data
Geerts et al. (2010), Geerts et al. (2012) 800 No 555 1C
data
Al-Boni and Raja (2010), Hosseini et al. (2012) 200 30 s 555 1C
Monteiro et al. (2011) 500 15 s 55573 1C
Upadhyay and Rao (2011) 250 30 s 437
6072 1C
302 journal of the mechanical behavior of biomedical materials 29 (2014) 295 308

Table 2 (continued )

First Author Number of Dwell Temperature

cycles time

Jiang et al. (2011) 1.000 15 s 555 1C

Umer et al. (2011) 200 60 s 55572 1C
Mazzitelli et al. (2012) 5.000 30 s 550 1C
zel Bektas et al. (2012) 1.0005.000 30 s 555 1C
10.000
Kimyai et al. (2012) 500 30 s 55575 1C
Singla et al. (2012a) 200 1 min 555 1C
Singla et al. (2012b) 250 30 s 56072 1C
Kim and Shin (2012) 10.000 15 s 555 1C
Joulaei et al. (2012) 5000 No 55575 1C
data
Ghandehari et al. (2012) 3000 20 s 555 1C
Poggio et al. (2012) 1000 60 s 560 1C
Moreau et al. (2012) 105 15 s 560 1C
Taha et al. (2012) 5000 20 s 555 1C
Jafari Navimipour et al. (2012) 500 30 s 55572 1C
Poggio et al. (2013) 1500 60 s 560 1C
Schlueter et al. (2013) 8500 30 s 555 1C

time and intervals between baths hinder in the comparison

Table 3 Main thermal cycling protocols proposed in the
last twenty years.
Thermal cycling protocol
ISO TR 11405 (1994) - Number of cycles: 500 cycles
- Temperature: 555 1C
- Dwell time: Z20 s.
Gale and Darvell (1999) - Number of cycles: 10.000
- Temperature and Dwell time:
35 1C for 28 s.
15 1C for 2 s.
35 1C for 28 s.
45 1C for 2 s
10,000 cycles suggested by Gale and Darvell (1999), showing to
not share the idea that this number of cycles correspond to
one year of aging in vivo (Table 2).
5. Conclusions
In vitro tests still remain an indispensable method for initial
screening of dental materials and, between the available
protocols, thermal cycling seems to be a valid in vitro method
to accelerate the aging of restorative materials (Amaral et al.,
2007; Cenci et al., 2008).
Unfortunately, although this aging method is, together
with the cyclic loading, the most widely used and necessary
to evaluate dental materials properties there is an apparent
lack of a standardized protocol evident from our comparison
across different studies. The choice of parameters for thermal
cycling (temperature, dwell time, number of cycles) seems to
be commonly chosen on the basis of convenience.
Authors in their experimental studies rarely give a thor-
ough explanation for the choice of temperature and time
conditions. The varied number of cycles, temperatures, dwell
of results across studies. Consequently, results obtained from
thermal cycling are contradictory (Amaral et al., 2007).
Taking everything into consideration, we can only propose
that further investigations are absolutely necessary in order
to develop a standardized and a reliable thermal cycling
protocol, so that the results of different studies can be
compared and effectively analyzed.
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