B. Kuter*, E. Eden*, H.
Yıldız** Keywords Command set; Glass-ionomer cement;
* Ege University, Faculty of Dentistry, Department of Pediatric
Dentistry, IZMIR, TURKEY
** Ege University, Engineering Faculty, Department of
Mechanical Engineering, IZMIR / TURKEY
e-mail: bernakuter@yahoo.com
The effect of heat
on the mechanical
properties of glass
ionomer cements
abstract
Aim The objective of this study was to assess the effect
of heat application on the mechanical properties of glass
ionomer cements.
Materials and methods Study design: experimental
design. The effect of heat on glass ionomer cements during
their setting was evaluated by measuring compressive
strength, flexural strength and microhardness. Moroever,
temperature changes from one surface of the glass
ionomer cement specimens 2, 4, and 6 mm thick to
the other surface were measured. A condensable glass
ionomer cement (Fuji IX) and a ceramic-reinforced glass
ionomer cement (Amalgomer CR) were used as test
materials. Heat was applied with soldering iron for 2
minutes at 80±2oC. All mechanical tests were carried out
24 hours after the setting of glass ionomer cements.
Results No significant differences in compressive
strength were found between the control groups and
the heated groups. There were no statistically significant
differences in the flexural strength value for both groups
of Fuji IX. On the contrary, when heat was applied to
Amalgomer, its mean flexural strength reached a
value that was higher than that of Amalgomer control.
Significant differences in microhardness were found
between the control groups and the heated groups
and between Fuji IX and Amalgomer CR. Temperature
rising in both glass ionomer cements was also noted.
Statistics: two-way ANOVA was used where appropriate
and independent samples t-test was used in case of
interaction.
Conclusion It is established that heat application
improved the surface mechanical properties of
conventional glass ionomer cements.
90
Heat; Mechanical strength.
Introduction
Glass ionomer cements (GICs ) were developed in the
early 1970s by McLean and Wilson [Wilson and Mclean,
1998]. The material was based on the hardening
reaction among aluminosilicate glass powders and
aqueous solutions of polymers and copolymers of acrylic
acid [Wilson and Kent, 1972]. GICs have been usually
preferred as restorative materials in paediatric dentistry
due to their low sensitivity to moisture, good adhesion
ability [Kilpatrick, 1996], and high fluoride content [Croll,
1990]. However, insufficient mechanical properties limit
the use of the material and numerous researches have
been carried out in attempts to improve the longevity
and the success of the restorations [Woolford, 1994;
Towler et al., 2001; Kleverlaan et al., 2004; Algera et al.,
2005; Skrinjaric et al., 2008; Yan et al., 2007].
Besides the new additives, Woolford [1994]
investigated the effect of heat activation on the GICs
and found that rising the temperature of the surface
of the cements to a maximum of 60 °C significantly
improved the early surface hardness of the cement after
24 h compared to cements which had not been heat
treated. Towler et al. [2001] showed that the application
of ultrasound to GICs improved the short-term surface
mechanical properties. The initial setting obtained
by the application of ultrasound provides improved
surface hardness, particularly within the first 24 hours
after setting. Kleverlaan et al. [2004] investigated
the influence of externally applied command
setting applications on the mechanical properties
of conventional GICs. Significant temperature rise
in the GICs was observed with ultrasonic excitation,
so it was hypothesized that its effect on the setting
of GICs may partially be explained by the increase in
temperature. Algera et al. [2005] investigated the
influence of heat and ultrasound application on the
setting reaction of GICs and determined that the heat
curing (70±2) and ultrasound accelerated the setting
reaction. Furthermore, in that study ıt was shown
that mechanical properties could be improved with
ultrasound and heat. Ultrasound especially affected
glass ionomer cements properties by producing
heat. Skrinjaric et al. [2008] showed that the heating
procedure during setting of GICs sealants can not be
recommended as routine treatments in clinical practice.
Yan et al. [2007] investigated the dimensional changes
caused by thermal stimuli of GICs with different
glass matrix ratios and showed that water loss from
conventional GICs with different power/liquid (P/L)
ratios compensated for thermal expansion and resulted
European Journal of Paediatric Dentistry vol. 14/2-2013

in a minimal dimensional change. It was shown
that under wet conditions glass ionomer cements
maintained their original dimensions upon heating.
Rafeek [2008] showed that heat treatment of
conventional GICs seemed to have no significant effect
on the compressive strength, fluoride release and
modulus on stress relaxation characteristics.
O’Brıen et al. [2010] investigated the effects of
various energy sources on the upper and lower surface
hardness of a setting GIC and showed that preheating
GIC capsules prior to mixing resulted in superior
hardness values.
Thermal response of glass ionomer cements when
heated is a very important clinical implication for the
longevity of the restored tooth [Yan et al., 2007].
The objective of this study was to assess the effect
of heat application on the mechanical properties and
microstructure of conventional GICs. It was also the
subject of this study to analyse the heat transfer degree
through the specimens.
Materials and methods
Fuji IX (GC, Japan), a condensable glass ionomer
cement, and Amalgomer CR (AHL, England), a ceramic-
reinforced glass ionomer cement, were used as test
materials. The information about some characteristics
of the test materials are summarized in Tables 1 and 2.
The materials were mixed according to the
manufacturers’ instructions and Fuji varnish was
applied after the initial setting time (Table 1) for both
glass ionomer cements. The study was carried out at
room temperature (23±1°C) and relative humidity of
50%±10 as stated in the ISO Standard 9917-1:2003
(E) for glass polyalkeonate cements. The stainless steel
molds were preheated to 37°C and the cement surface
was covered with a single cellulose acetate sheet in
order to obtain a smooth surface. The other molds
were placed on top of the cellulose sheet to give the
specimen a flat surface and GICs samples were kept in
Product Manufacturer Lot
Amalgomer CR AHL, ENGLAND Powder 020615-1
Liquid 040522-7
Fuji IX GC, JAPAN Powder 0411051
Liquid 0411051
tabLE 1 Materials tested.
Element Al Si Ca Na P F
Amalomer CR 15.8 18.7 7.1 5.5 1.6
Fuji IX 17.9 13.7 0 1.0 2.2
European Journal of Paediatric Dentistry vol. 14/2-2013
Heat application on glass ionomer cements
the incubator during initial setting time of the cement.
Heat was applied with a soldering iron (Lötstation MLS-
48, McVoice, Verzeuge, Germany). The active tip of
the soldering iron was 5 mm in diameter. The soldering
iron was set to 80±2°C and applied on one surface of
the specimens in the study group for 2 minutes. The
samples were kept in distilled water at 37°C and all
tests were carried out 24 hours after the setting of glass
ionomer cements. Eighty specimens were prepared
and then divided into 4 groups. The effect of heat on
the mechanical properties of conventional GICs was
evaluated by measuring compressive strength, flexural
strength, microhardness and temperature rising in the
test materials was also measured and noted.
Compressive strength
Cylindrical specimens were prepared in stainless steel
molds [ISO] of 4 mm in diameter and 6 mm in height.
Heat was applied only on the circular surface of the
cylinder, and a universal testing machine (Shımadzu
AG-IS 100kN Autograph, Japan) was used on the
heated surface for compressive strength test at a
loading rate of 0.5 mm/min.
Flexural strength
For testing flexural strength, the prepared specimens
dimensions were 25x2x2 mm. Heat was applied on
the square surface of 2x2 mm. The flexural strength
of these materials was determined using a three-
point bending machine with Autograph (the distance
between supports was set to 20 mm) (Shımadzu AG-IS
100kN Autograph, Japan).
Microhardness
Vickers Hardness Testing Machine (HMV-2 Shımadzu
Kyoto, Japan) was used to test microhardness of these
materials. Disc-shaped specimens of 5 mm diameter
and 2 mm height were prepared in a plastic mold. A
load of 300 g was applied to the heated surface of
the specimens. The load was applied for 10 s and the
application was repeated 5 times.
Component Initial Setting Time
Powder: Glass, Polyacrylic acid, 3 min, 30 s
tartaric acid, zirconium oxide
Liquid: polyacrylicacid, water
Powder: Glass, polyacrylic acid, 2 min, 20 s
tartaric acid
Liquid: polyacrylic acid
Sr La tabLE 2 Weight percentage
12.9 0 0 composition of GICs.
10.2 19.9 0
91
Kuter B., Eden E. and Yıldız H.

70
275
250 60
Compressive strength (Mpa)

225

Flexural strength (Mpa)

200 50
175
40
150
125
30
100
75 20
50
25 10
0
0
Fuji Cntr. Fuji healed Arrig. Cntr. Arrig. healed
Fuji Cntr. Fuji healed Arrig. Cntr. Arrig. healed

Fig. 1 Compressive strength of Fuji IX and Amalgomer CR. Fig. 2 Flexural strength of Fuji IX and Amalgomer CR.

Thickness 2 mm 4 mm 6 mm
105 Fuji IX 33.3 ±2.6ºC 32.5 ± 2.0ºC 31.5 ± 1.0ºC
Amalgomer CR 37.3 ± 1.0ºC 34.5 ± 1.6ºC 31.9 ± 0.9ºC
90

75 tabLE 3 Temperatures measured at the bottom of the

Microhardness (VHN)

specimens after heat application from the top (ºC).

60

45 Results

30 The results of the compressive strengths and the

statistical analysis between groups are shown in Figure
1. No significant (ANOVA) differences in compressive
15
strength were reported between Fuji IX and Amalgomer
CR. Moreover, no significant differences in compressive
0 strength were found between control group and heated
Fuji Cntr. Fuji healed Arrig. Cntr. Arrig. healed group, as well.
The flexural strengths of the materials with and
without heat application are shown in Figure 2. No
Fig. 3 Microhardness of Fuji IX and Amalgomer CR. significant differences in flexural strength among Fuji
IX and Amalgomer CR were found in the study. When
heat was applied to the Fuji IX, no significant differences
Heat Application on GICs (independent samples t-test) in flexural strengths were
In this case were used 20 disc-shaped specimens of 5 mm found between control and heated groups. When
diameter and thickness of 2, 4 and 6 mm. Temperature the heat source was applied to the Amalgomer, the
increase due to heat application from the top surface of mean flexural strengths were higher than that of the
the specimens to bottom was measured by thermocouple corresponding control group and significant differences
(Thermometer HD 8605, Delta OHM, Italy). were found (p<0.05).
The mean surface hardness of Fuji IX was 66.5
Statistical analysis (±11.4) VHN. When heat was applied to the surface
Statistical analysis was done using two-way ANOVA of the Fuji IX, the mean surface hardness was found
where appropriate and independent samples t-test was to be 84.8(±7.5) VHN. The mean surface hardness of
used when there was interaction. Amalgomer was 60.1(±16.4) VHN. When heat source

92 European Journal of Paediatric Dentistry vol. 14/2-2013


was applied to the surface of the Amalgomer, the mean
surface hardness was measured as 65.4(±8.5) VHN.
Significant differences in micro-hardness were found
between control and heated groups (p<0.05) (Fig 3).
Temperatures measured at the bottom of the
specimens after heat application on the top surface are
shown in Table 3 and it can be seen that temperature
rising in both materials was inconsiderable.
Discussion
The effect of heat on the setting reaction is likely
to make the polyalkenoic acid more active [Woolford,
1994]. When the acid gets in contact with the surface
of the glass, it is able to break down the surface of
the glass more readily. It increases the rate at which
the ions are leached and released from the glass. The
total effect of all these accelerated reactions produces
a more rapid formation of the calcium polyalkeonate
matrix. Gu and Fu [2004] showed thar particle size
of GICs increases after heat application. This is due
to particle agglomeration, coalescence and growth at
high temperatures. Particle size distribution influenced
the mechanical properties of glass ionomer cements
significantly [Gu et al., 2004].
The thermal behaviour of GICs is different because of
interaction with water from the environment [Carrick
and McCabe, 2007]. Thermal behaviour may be
affected by the original P/L ratio and the structure of
the set cement [Yan et al., 2007]. The matrix of GICs
contains loosely bound water as well as tightly bound
water [Wilson and McLean, 1998]. Depending on
the environment, loosely bound water is easily lost or
gained, depending on the level of moisture/humidity in
the wet or dry environment. Wilson et al. [1998] showed
that the water content and especially the loosely bound
water in GICs depends on the P/L ratio and the storage
method. A great amount of mass loss was observed
in GICs after heating in a dry environment [Yan et
al., 2007]. The mass loss of GICs in wet conditions is
significantly lower.
Yan et al. [2007] showed that all the GICs tested
in their study lost weight during the heating process
and the greatest P/L ratios produced the lowest
final weight loss. The lowest P/L ratio produced the
greatest contraction after heating. The water content
and ıts relative mobility in the GICs matrix have been
considered as major factors in determining the thermal
response behaviour of GICs. The ratio of reinforcing
glass-core and matrix affects the diffusion of water in
the glass ionomer matrix [Davies et al., 1993]. When
GICs are mixed at a high initial P/L ratio, the ratio of
reinforcing glass core in the matured cement matrix is
increased. Decreasing the P/L ratio reduces the amount
of the reinforcing fillers in the matrix [Fleming et al.,
2003]. The ratio of reinforcing glass core in the matured
European Journal of Paediatric Dentistry vol. 14/2-2013
Heat application on glass ionomer cements
cement matrix was increased in the SEM evaluation
[Kuter et al., 2010] this was particularly evident at SEM
on the heated specimens.
Algera et al. [2005] showed that heat may contribute
to acceleration of the reaction by de-clustering
glass particles and enhancing the diffusion of the
reaction components. SEM evaluation did not show
de-clustering of the glass particles or a reduction of
porosity in that study [Algera et al., 2005]. Kuter et
al. [2010] showed that the portion of GICs specimens
closer to the heat were affected to a greater extent.
In that study the top part where heat was applied had
a better and more meaningful differentiation. The
bottom part had a lesser differentiation after the heat
treatment. Voids decreased, texture became denser
and there were particles with larger sizes with the heat
applied. These results showed that application of heat
affected the top portion where heat was applied more
than the lower portion and for this reason, mechanical
strength of heated GICs specimens highly increased
only microhardness.
Kleverlaan et al. [2004] showed that an increase in
compressive strength of the Fuji IX was found with
the heat and ultrasonic application. No significant
differences in compressive strengths of the Fuji IX heat
and control groups were found 24 hours later, in this
study. However, Kleverlaan et al. [2004] stored the
samples in lubricants, in order to prevent dehydration,
and the glass ionomer cement was placed between
two heated metal elements for 5 minutes. Algera et
al. [2005] showed that materials cured in oil reached
a significantly higher compressive strength compared
to storage in water. Jones et al. [2007] showed that
the temperature rise on the samples lubricated with
oil were greater than samples lubricated with water.
For this reason, the results of our study did not show a
similarity with that study, since all of the samples in our
study were stored in water according to ISO [ISO] and
heat was applied for 2 minutes from one surface of the
glass ionomer cement.
When Rafeek [2008] carried out his study with
samples stored in water, like in our study, he showed
that compressive strength values between the control
and the heat-treated conventional GICs specimens were
not statistically different.
There were no statistically significant differences
in flexural strengths of Fuji IX in both groups. On the
contrary, when the heat was applied to the Amalgomer,
its mean flexural strength reached a value that was
higher than that of Amalgomer control, and this time
significant differences were noted. When temperature
is high, the P/L ratio can increase due to evaporation
of the liquid, which results in high strength of materials
[Kleverlaan et al., 2004]. Increasing the P/L ratio can
improve the mechanical properties of the glass ionomer
cements. Fuji IX is a condensable glass ionomer cement,
but Amalgomer CR is a ceramic-reinforced glass ionomer
93
Kuter B., Eden E. and Yıldız H.
cement and Fuji IX has higher P/L ratio. Thus, Fuji IX that
further increasing P/L ratio, due to the heat application,
did not lead to higher flexural strength values.
When a temperature of 700C was applied on the
glass ionomer cement (Fuji IX Fast) with soldering
iron, the temperature in the pulp chamber showed a
maximum rise of 2.50C after 60 seconds [Algera et al.,
2005]. Kleverlaan et al. [2004] showed that when a
temperature of 700C was applied on the glass ionomer
cement (Fuji IX) for 5 minutes on both surfaces, the
temperature of the glass ionomer rose from 34.60C to
45.30C. When the temperature of 80±20C was applied
on one surface on the GICs 2, 4, or 6 mm thick (Fuji IX
and Amalgomer CR) for 2 minutes at room temperature
(23±1°C), temperature rising of both glass ionomer
cements was inconsiderable through the glass ionomer
cement.
On the other hand, significant differences in
microhardness were reported between the control and
the heated groups of Fuji IX and Amalgomer CR. Wang
and Darvell showed the Amalgomer CR was sensitive to
moisture and the same caused a deterioration by surface
degradation [Wang and Darwell, 2009]. However, it
has been shown in this study that application of heat
improved the strength of the GICs, at least the surface
strengths of the cement. As heat transfer in this study
can not be conducted all the way through the specimens,
the significant improvements in microhardness were
obtained in the areas that were adjacent to the surfaces
where heat was applied, whereas no increase in
compressive strength of GICs was observed. Kuter et al.
[2010] also showed that the top parts where heat was
applied had a better and more significant differentiation
and the bottom parts had less differentiation in the SEM
evaluation. Increasing microhardness with heat yields
higher abrasion resistance values and less retention
zones on the GICs surfaces. It could be strongly thought
that heat application could be an alternative in the
prevention of harmful effects of oral liquids on the
outer surface of GICs which are sensitive to moisture for
a period of 24 hours. Since it is very difficult to prevent
saliva contamination on application area, especially in
children, heat application on the glass ionomer cements
may be useful in paediatric dentistry.
Conclusion
We can conclude that the application of heat may
improve the characteristics of GICs, especially on the
surface. Therefore, it may be easily expected that the
application of heat increases greatly the microhardness
of GICs, whereas the application of heat increases the
flexural strength to a relatively lower extent. Heat should
be applied on the surface of the glass ionomer cements
to avoid contact with oral liquid, particularly after initial
setting time and to provide higher abrasion resistance
94
and less retention areas on the glass ionomer cements.
However, further research is necessary to establish the
potential effect of heat and long-term results of the
restorations.
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