Vol. 132 (2017) ACTA PHYSICA POLONICA A No.

3-II

Special issue of the 3rd International Conference on Computational and Experimental Science and Engineering (ICCESEN 2016)

Nanomechanical Comparison of Commonly Used Dental

Crown Cements to a Newly Developed One
E. Kalea , Z. Arslanoğlub , H. Altanc , F. Bilgiçd , M. Tuzlalia , A. Köroğlua,e,∗
and S. Özarslanf
a
Mustafa Kemal University, Faculty of Dentistry, Department of Prosthodontics, Hatay, Turkey
b
Mustafa Kemal University, Faculty of Dentistry, Department of Paediatric Dentistry, Hatay, Turkey
c
Gaziosmanpaşa University, Faculty of Dentistry, Department of Paediatric Dentistry, Tokat, Turkey
d
Mustafa Kemal University, Faculty of Dentistry, Department of Orthodontics, Hatay, Turkey
e
Mustafa Kemal University, Faculty of Dentistry, Department of Periodontology, Hatay, Turkey
f
Mustafa Kemal University, Department of Physics, Hatay, Turkey
The main goal of nanoindentation tests is to obtain elastic modulus and hardness of the specimen material from
load-displacement measurements. With this study, it was aimed to establish a quantitative relationship between the
nanomechanical properties of commonly used dental cements in comparison to a newly developed crown cement and
to predict its performance potential. Nanomechanical properties of polycarboxylate cement (PCC), glass-ionomer
cement (GIC), dual-cure self-adhesive cement (SAC) and a newly developed glass-carbomer cement (GCC) were
investigated by nanoindentation tests. All samples were fabricated according to their respective manufacturer’s
instructions. Available damage on the surface due to manipulation was removed by grinding with 1200, 2400 and
4000 grit sandpaper, and then polishing on 6, 3, and 1 µm diamond-lap-wheel was performed. Nano-mechanical
measurements were done using nanoindenter machine with resolution less than 1 nN and displacement resolution
of 0.04 nm. Berkovich diamond indenter tip was used for the nanoindentation tests. For each indentation, a set
of nanoindentation tests at least on 6 different locations per specimen surface were performed to obtain more
representative mean results. Indentation test load-displacement curves were analysed using Oliver-Pharr method,
and one-way ANOVA or Kruskal-Wallis test, following Kolmogorov-Smirnov and Shapiro-Wilk, was used to compare
the results. Nanohardness (Hnano ) values were 0.52±0.25, 0.45±0.18, 1.03±0.82 and 0.43±0.18 GPa for GIC, GCC,
PCC, and SAC, respectively. Reduced elastic modulus (Er ) values were 9.51 ± 6.17, 11.77 ± 5.04, 27.37 ± 20.61,
10.33 ± 5.08 GPa for GIC, GCC, PCC, and SAC, respectively. There was no statistical difference between the
tested materials. PCC was the hardest, and GIC was the least hard material, whereas the newly developed GCC
was the second, in terms of Hnano , before SAC. PCC also had the highest Er mean, compared to the other dental
crown cements, suggesting lower elastic properties. SAC was more elastic than GCC and less elastic than GIC.
GCC had the second highest Er , standing closer to SAC and GIC. Within the limitations of the current study,
it can be concluded that the newly developed glass-carbomer cement is comparable to the other tested commonly
used dental crown cements, regarding Hnano and Er .
DOI: 10.12693/APhysPolA.132.954
PACS/topics: 62.20.–x, 62.20.Qp, 62.20.de

1. Introduction undergo setting through an acid-base reaction between

an ion-leachable glass and aqueous polyacid and can che-
Dental cements are widely used luting agents for fix-
mically bond to enamel and dentin [4]. Moreover, they
ation of dental crowns and other fixed dental prostheses
have an ability to release fluoride with superior physi-
in dentistry. There is a wide range of cements available
cal and mechanical properties [1, 5, 6]. Self-adhesive re-
on the market from conventional water-based to contem-
sin cements are the latest of the contemporary resin ce-
porary resin-based cements [1]. Today, among the most
ments [7]. They contain specific adhesive monomers that
commonly used dental cements are zinc-polycarboxylate
are sufficiently acidic to produce their self-adherence to
cement, glass-ionomer cement and self-adhesive resin
dental hard tissue [7].
cement [1].
Classical polycarboxylate cement was the first ce- Despite their clinically acceptable success, all these
ment system developed with a potential for adhesion materials have some clinical limitations, such as a pro-
to tooth structure [2]. Conventional glass-ionomer ce- longed setting time, moisture sensitivity during initial
ments were developed based on the favourable properties setting, dehydration and rough surface characteristics,
of both silicate and polycarboxylate cements [3]. They which can potentially reduce their mechanical resis-
tance [8, 9]. In the last few years, a new type of dental ce-
ment has been introduced to the market – class-carbomer
cement – that has been claimed by its manufacturer
∗ corresponding author; e-mail: [email protected] to overcome the negative properties of glass-ionomer
cements, due to its improved physical properties [10].

(954)
 Nanomechanical Comparison of Commonly Used Dental Crown Cements. . . 955

This new material contains nano-sized glass particles and force on nano-scale, by measuring the depth of indention
fluor-apatite, as filler, and sets chemically while being op- in microns. These tests are based on new technology that
timized for heat curing [10]. allows for precise and controlled indentation forces along
While any cement has its advantages, dentists must with precise measurement of the indentation depths [15].
carefully consider which is the most suitable for an in- Measurement procedures consist of pressing the indenter
dividual case, depending on the material and substrate into surface with constant load or strain rate, recording
to be bonded [11, 12]. Successful cement should be easy indenter displacement as a function of load during loa-
to use, excellent in adhesion with mechanical properties ding/unloading, and of finally, calculating the hardness
to withstand masticatory or parafunctional forces, and from the load-displacement curve and elastic modulus of
a long-term stability in the warm and wet oral environ- the material from the unloading curve [15]. The main
ment, it should also be aesthetic and biocompatible [11]. goal of nanoindentation tests is to easily determine elas-
The real difference in the performance of dental crown tic modulus and hardness, as basic mechanical properties
cements can be established by means of long-term cli- of newly developed materials from load-displacement me-
nical evidence-based data. However, before starting an asurements.
extensive research, basic mechanical properties of new The purpose of this study was to establish a quantita-
materials on the market can easily be compared to those tive relationship between the nanomechanical properties
of materials that have been on sale for a long time and of commonly used dental cements in comparison to a ne-
have had the privilege to be observed and studied clini- wly developed crown cement in terms of nanohardness
cally for a while. Hnano and reduced elastic modulus Er , and to predict
Hardness as a physical property of a solid is the resis- its performance potential, based on previously published
tance to potential penetration of the mass by any har- dental literature, regarding materials present on the mar-
der material or the resistance of the tested material to ket for a longer time. The null hypothesis was that there
wear, scratching, cutting and plastic deformation [13]. would be no difference in tested mechanical properties be-
It covers several properties like resistance to deforma- tween commonly used and newly developed dental crown
tion, friction and abrasion. It combines elastic and plas- cements.
tic properties and can be understood as some measure of
resistance to surface contact deformation [13, 14]. Inden- 2. Materials and methods
tation hardness, as a principal parameter for mechanical
characterization of solid materials, has been commonly Four different dental crown luting cements were tested
used as a technique to measure the mechanical properties in this study (n = 6). Specimens consisted of conventio-
of dental materials [14]. It is defined in macro-, micro- nal glass-ionomer cement (GIC), newly developed glass-
or nano-scale according to the indentation forces applied carbomer cement (GCC), classic polycarboxylate cement
and the displacement of the indenter observed. Nanoin- (PCC) and contemporary dual-cure self-adhesive cement
dentation tests measure hardness by using indentation (SAC) (Table I).

TABLE I
Brand name, lot number, specification and manufacturer information of the luting cements tested in the study.

Material type
Material brand Material manufacturer
(Lot number)
Glass-Ionomer Cement
Voco Meron VOCO, Germany
(liquid: 1305047; powder: 1309554)
Glass-Carbomer Cement
GCP Glass Crown Cement GCP Dental, Netherlands
(7302245)
Zinc-Polycarboxylate Cement
Adhesor Carbofine Spofa Dental, Czech Republic
(liquid/powder: 2480086-2)
Self-Adhesive Resin Composite Cement
Panavia SA Cement (Automix) Kuraray, Japan
(2J0002)

Four 10 mm-thick parallel-edged polymethylmethacry- block was randomly filled with one of the test materials.
late (PMMA) cylinder blocks with diameter of 50 mm All the materials were applied strictly in accordance with
were fabricated with 7 cavities of 2 mm depth and dia- the manufacturer’s instructions.
meter of 10 mm on one of the flat surfaces of each. A Blue light of 1400 mW/cm2 was used for 20 s (VALO
thin layer of cyanoacrylate adhesive was applied to the LED; Ultradent, USA) for the curing procedure of group
inner surface of the cavities and each of seven cavities per SAC. Capsule mixer (10 s) (GCP CarboMIX; GCP Den-
956 E. Kale et al.

tal, Nederland), capsule applicator (GCP CarboCAP; the topographic images of the indents, the nanoinden-
GCP Dental) and light-heat-curing (1400 mW/cm2 for ter was also operated in scanning probe mode (Fig. 3).
60 s) device (GCP CarboLed Lamp; GCP Dental) was Indentation test load-displacement curves were analysed
used for the application and curing of GCC group. Sam- using Oliver-Pharr method [15–17].
ples were stored at 100% humidity environment in room
temperature for 24 hours after preparation.

Fig. 1. Prepared samples inside PMMA cylinders, for Fig. 3. Morphological topography of an indent (arrow)
each group. (B), and computation of indent depth and contact dis-
tance (A).

In the current model, contact area (Ac ) and nanohard-

ness (Hnano ) were computed with the following formula,
Pmax
Ac = 24.5h2c Hnano = ,
A
where Pmax is the maximum test load and Ac is the pro-
jected contact area at Pmax . The reduced elastic modulus
Er was computed with the following formula,
√
π S
Er = √ ,
2 24.5hc
where S is the contact stiffness, acquired from the initial
slope on the unloading curve at Pmax .
Kolmogorov-Smirnov and Shapiro-Wilk methods were
Fig. 2. Samples in nanoindenter machine.
used to assess the homogeneity of variance of nanoin-
dentation test results and one-way ANOVA along with
Prior to testing, material surfaces were aligned flat to Kruskal-Wallis tests were used accordingly by means
the surface of their corresponding carrying PMMA cylin- of statistical software (Statistical Package for the So-
ders to ensure parallelism between samples, using 1200, cial Sciences v.15; SPSS, USA) at a level of significance
2400 and 4000 grit (SiC) sandpaper discs and 6, 3 and α = 0.05.
1 µm diamond-lap-wheels, consecutively, on a mechani-
cal device (Fig. 1). Nanomechanical measurements were 3. Results
done using nanoindenter machine (TI 950 TriboIndenter; Kolmogorov-Smirnov and Shapiro-Wilk tests have re-
Hysitron, USA) with resolution less than 1 nN and dis- vealed normal distribution for Hnano but not for Er . The
placement resolution of 0.04 nm (Fig. 2). Berkovich dia- results from one-way ANOVA for Hnano and Kruskal-
mond indenter tip was used for Hnano and reduced elastic Wallis for Er did not show any statistical difference bet-
modulus Er tests. The tip was calibrated using a fused ween the tested materials. Detailed data of the evaluated
quartz reference sample. One of the specimens on each physical properties of the luting cements, regarding mea-
PMMA cylinder was also used for calibration purposes surements, calculations and statistical analyses, are given
before the test start in each group. For an indentation, in Table II trough Table V. The obtained indentation test
a set of nanoindentation tests, at least on six different load-displacement curves are shown in Fig. 4.
locations per specimen surface, with maximum load of Among the tested dental crown luting cements, PCC
6000 µN under a loading/unloading rate of 1200 µN s−1 , was the hardest, and GIC was the least hard, whereas the
with load held at maximum value for 2 s, were performed newly developed GCC was the second in terms of Hnano
to obtain more representative mean results. To record before SAC (Fig. 5). PCC also had the highest mean Er
 Nanomechanical Comparison of Commonly Used Dental Crown Cements. . . 957

TABLE II
Mean ± standard deviation (SD), standard error (SE), me-
dian and minimum-maximum range of Er for the tested
materials (GPa). Specimen number: 6.

Mean
Group SE Med Min Max
(SD)
GIC 9.51
2.52 6.72 4.81 20.70
(Glass-Ionomer Cement) (6.17)
GCC 11.77
2.06 11.24 6.36 18.36
(Glass-Carbomer Cement) (5.04)
PCC 27.37
8.42 18.98 9.61 58.93
(Polycarboxylate Cement) (20.61)
SAC 10.33
2.07 8.71 6.46 20.46
(Self-Adhesive Cement) (5.08)

TABLE III Fig. 4. Indentation test load versus indentation depth

for the tested materials.
Mean ± standard deviation (SD), standard error (SE),
median and minimum-maximum range of Hnano for the
tested materials (GPa). Specimen number: 6. compared to others, suggesting lower elastic properties.
SAC was more elastic than GCC and less elastic than
Mean GIC (Fig. 6). GCC had the second highest Er standing
Group SE Min Max
(SD) closer to SAC and GIC.
GIC 0.52
0.10 0.21 0.85
(Glass-Ionomer Cement) (0.25)
GCC 0.45
0.07 0.27 0.77
(Glass-Carbomer Cement) (0.18)
PCC 1.03
0.34 0.15 2.02
(Polycarboxylate Cement) (0.82)
SAC 0.43
0.07 0.27 0.74
(Self-Adhesive Cement) (0.18)

TABLE IV
Kruskal-Wallis results for Er (P < 0.05). Specimen num-
ber: 6.

Mean Chi Asymp. sig.

Group df
rank square P (α = 0.05)
GIC Fig. 5. Box-plot comparison diagrams of Hnano for tes-
8.33 3 7.380 0.061 (NS) ted materials.
(Glass-Ionomer Cement)
GCC
12.33
(Glass-Carbomer Cement)
PCC
18.83
(Polycarboxylate Cement)
SAC
10.50
(Self-Adhesive Cement)
NS: non-significant.

TABLE V
One-way ANOVA results for Hnano (P < 0.05).

Source of Sum of Mean

df F P (α = 0.05)
variation squares square
Between groups 1.443 3 0.481 2.394 0.099 (NS)
Within groups 4.019 20 0.201
Total 5.462 23 Fig. 6. Box-plot comparison diagrams of Er for tested
NS: non-significant. materials.
958 E. Kale et al.

4. Discussion is somewhere between GIC, PCC and SAC in terms of

Hnano and Er , comments for dental crown cement with
The nanomechanical comparison in terms of Hnano and
reliable mechanical properties. Glass-ionomer, polycar-
Er of the common dental crown cements (GIC, PCC and
boxylat and resin cements are well documented in the
SAC) to the newly developed one (GCC) used in this
literature with acceptable long-term performance ability
study had shown no statistical differences between each
[11, 12]. The results of the current study suggest an
other, therefore the null hypothesis set up at the begin-
acceptable performance potential, considering the GCC
ning of the study was accepted. dental crown luting agent. Further investigations are
The main limitation of the current study was the low encouraged.
number of specimens per group. Although, a mean of at
least 6 indentations per specimen was considered while
testing in each group, other parameters, like standard de- 5. Conclusions
viation, for example, remained undefined regarding these
Within the limitations of the current study, it can be
mean values. This deficiency eradicated the chance of im-
concluded that the newly developed glass-carbomer ce-
plementation of a power analysis to the statistical evalu-
ment is comparable to the other tested, commonly used,
ation and limited the indentation test number to 6 (num-
dental crown cements, regarding Hnano and Er .
ber of specimens per group), whereas the number of in-
dentations per group was actually 6×6 = 36. This should
be taken into account before generalizing from the results Acknowledgments
of the present study.
Authors express sincere appreciation to Dr. Osman
Glass-carbomer cement is relatively new on the market
ŞAHİN for his kind cooperation during the preparation of
and is very scarcely represented in dental literature [17],
this work for presentation at the (3th) ICCESEN-2016 in
whereas there are quite a lot of studies investigating me-
Antalya, and Prof. Dr. Tacettin İNANDI for performing
chanical properties of glass-ionomer, polycarboxylate and
the statistics of this article.
resin cements [8, 9, 11]. Rosenstiel et al. have reviewed
the mechanical properties of different dental luting ce-
ments and have ordered the materials, considering the References
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