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Dental Materials (2004) 20, 133141

http://www.intl.elsevierhealth.com/journals/dema

Morphology and properties of denture acrylic resins


cured by microwave energy and conventional
water bath
C.-P. Laia, M.-H. Tsaia, M. Chena,*, H.-S. Changb, H.-H. Tayb
a

Institute of Materials Science and Engineering, National Sun Yat-Sen University, Kaohsiung 80424,
Taiwan, ROC
b
Dental Department, Veterans General Hospital-Kaohsiung, Kaohsiung 813 Taiwan, ROC
Received 7 March 2002; received in revised form 1 January 2003; accepted 12 March 2003

KEYWORDS
Denture; Poly(methyl
methacrylate);
Microwave; Morphology;
Transmission electron
microscopy

Summary Objectives. This study examined the influence of microwave energy levels
on the morphology and properties of an impact resistant denture material poly(methyl
methacrylate) with a thickness of 10 mm.
Methods. A microwave flask containing two resin blocks was processed at 80, 160,
240, and 560 W for 15, 10, 7, and 2 min, separately. Each Flask was then turned over,
and cured for an additional 2 min at 560 W. The process using conventional methods
was carried out at 70 8C for 9 h. The blocks were tested for hardness, porosity, flexural
properties, solubility, and molecular weight. The morphology of the specimens after
staining with osmium tetroxide was examined by transmission electron microscope.
Results. The changes in temperature with time were recorded during microwave
heating at 80, 160, and 240 W, respectively. A significantly large difference in the
curing temperature was observed when comparing these two processing methods.
There was little difference in the mean values of surface hardness and the weight
percents of the insoluble parts. The mean domain size and the volume fraction of the
rubber phase favor of the water-bath method. However, the porosity in the waterbath-cured specimens was much less than that in the microwave-cured specimens.
Thus, the conventionally cured specimens showed better flexural strength and flexural
modulus than the microwave-cured specimens.
Significance. This study has shown that microwave energy can efficiently polymerize
denture base polymer. Highly statistical differences in morphology and flexural
properties favor of the water-bath method. Choice of a suitable microwave power and
polymerization time is important in order to reduce porosity to a minimum level and
increase the domain size and volume of the rubber phase.
Q 2003 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Introduction
*Corresponding author. Tel.: 886-7-5252000x4062; fax:
886-7-525-4099.
E-mail address: mingchen@mail.nsysu.edu.tw

Acrylic resins have been used for denture fabrication


for over 60 years. The most popular denture base
material is heat-cured poly(methyl-methacrylate)

0109-5641/$ - see front matter Q 2003 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.
doi:10.1016/S0109-5641(03)00084-8

134

(PMMA). In addition to homo-PMMA, impact resistant


resins have been developed.1 Virtually all dentures
are constructed from these materials using the
conventional polymer/monomer dough molding
process and cured using a water-bath system. Since
the introduction of acrylic resins for denture
construction, there has been a continual search for
modified procedures to process the resin. Nishii2 first
reported the use of microwave energy to polymerize
denture base materials in 1968. Kimura et al.3
reported that it was possible to cure acrylic resin
in a very short time using this technique. In 19844 and
1985,5 the light fiber-reinforced plastic (FRP) flask
was substituted for the heavy brass flask and
compress, and the water-bath curing tank gave
way to a microwave oven.
Methyl methacrylate (MMA) is a polar liquid at
room temperature. The microwaves cause the MMA
molecules within the acrylic resin to orient themselves in the electromagnetic field at a frequency of
2450 MHz, and numerous polarized molecules are
flipped over rapidly and generate heat due to
molecular friction. Initiating radicals are then
able to react with monomers to start polymerization. Microwave heating is independent of thermal
conductivity, therefore, curing cycles involving the
application of rapid heat may be used without the
development of a high exothermic temperature.
The major advantages of microwave heating over
conventional heating are: (1) the inside and outside
of substance are almost equally heated, and (2)
temperature rises rapidly. Peyton6 reviewed the
curing methods and concluded, that when all
factors were considered it was doubtful that any
of these methods had any real advantage over the
water-bath method and the important factor for
consideration was the careful control of the
temperature during processing.
Reitz et al.5 compared porosity, hardness, and
transverse strength of microwave and water-bath
cured specimens and found no significant differences. The frequency and size of porosity in thick
specimens could be reduced to 30% by a longer
polymerization time at a lower wattage. Hayden7
compared the flexural strength of three acrylic
resins cured by water-bath and microwave energy.
The microwave-cured acrylic did not absorb as
much energy before fracture as the water-bath
cured acrylic. Shlosberg et al.8 also tested transverse strength and hardness. No statistical differences were noted when microwave or water-bath
curing were used. Smith et al.9 investigated hardness, transverse strength, modulus of elasticity,
and Izod impact strength of seven resins cured using
a water bath, microwave energy, or by visible
light. Microwave curing improved the modulus of

C.-P. Lai et al.

elasticity of two resins, decreased the impact


strength of one, and had little effect on the
properties of the other two resins.
In the literature, some data on the morphology of
acrylic resins was found. The purpose of this study
was to establish the time and temperature required
for the complete conversion of monomer to polymer and to determine if denture bases processed by
microwave energy varied significantly in morphology from those processed by the conventional
water-bath curing method. Finally, the size and the
distribution of rubber phase were correlated with
the heating methods, microwave power, the physical properties and mechanical properties.

Materials and methods


Experimental materials. The Optilon-399 (Coltene/
Whaledent Inc., Ohio, USA) used in this study is a
PMMA denture base polymer of Hygenic brand
marketed as two parts, powder and liquid. The
powder contains mainly PMMA modified with graft
copolymer and a small percentage of benzoyl
peroxide as initiator, titanium dioxide, and cadmium pigments. Principle ingredients of liquid are
MMA monomer and ethylene glycol dimethacrylate
as the crosslinking agent. The proportion of powder
to liquid was 30 10 ml.
Specimen preparation. The domestic microwave
oven used in this study was a Samsung model MW3190T (Korea) with a full power of 800 W. For
production of specimens using the microwave
technique, a special dental FRP flask (Acron MC
microwave flask, GC America Inc.) was used. Mold
separation (alginate solution), packing and clamping procedures followed standard practice. While
the resin was in dough stage, it was packed into two
molds (65 mm 15 mm 10 mm). These two molds
were 52 mm apart which were geometrically
equivalent with respect to the flask. The halves of
the flask were pressed together in a pneumatic
press (Kavo EWL 5414, Germany). The pressure was
increased up to 40,000 N in several steps in order to
remove excess resin. The packed FRP flasks were
used for temperature measurement and specimen
preparation.
For the water-bath cured specimens, the preparation procedures were the same as for the
microwave-specimens except that conventional
metal dental flasks (Brass flask, Kavo EWL,
Germany) were used. Acrylic resins were processed
in a water-bath curing tank at 70 8C for 9 h, and then
the dental flasks were cooled to room temperature.

Morphology and properties of denture acrylic resins

135

Measurement of temperature change


and microwave curing

the volume fraction of rubber phase domains


were measured using Optimas software.

Two thermocouples went through the holes on the


upper part of the FRP flask, and located at the
center position of each denture base resins mold.
The turntable of the microwave oven was removed
during the temperature measurement (models 3711
and 3712, LR4100 recorders, Yokogawa Electric
Co.). Ideally, the FRP flask was placed in the center
of the oven cavity, and at the same height as the
turntable by putting the flask on two blocks of cured
resin. The changes in temperature with time were
recorded during the microwave heating at 80, 160,
and 240 W, respectively. The measurement of 10
blocks of resin molds was made for each power
condition. It was found that the temperature
tended toward an approximately constant value,
and the time required to reach this temperature
was selected to cure acrylic resins for each power
condition.
Microwave curing was carried out in a microwave
oven equipped with a turntable. The microwave
flask containing two of the same size resin blocks
was processed at 80, 160, 240, and 560 W for 15, 10,
7, and 2 min, separately. Then each flask was
turned over, and cured for an additional 2 min at
560 W. Ten blocks were prepared for use in each
condition and cooled to room temperature before
deflasking. A total of 50 blocks of cured acrylic resin
were thus prepared, 40 in the FRP flasks and 10 in
the brass flasks. These blocks were tested for
hardness, porosity, flexural properties, solubility,
and molecular weight in sequence.

Hardness

Transmission electron microscopy


Slices of 1 mm 15 mm 10 mm were cut from
the center part of the cured blocks using a slow
cutter (Minitom, Struers). The center sections of
the slices were sharpened into a cross-section
of about 0.01 mm2 across the transverse direction
of the thickness. Specimens of 30 50 nm thick
were cut from the sharpened section using an
ultramicrotome (Ultra cutter, Reichert-Jung) and
mounted on formvar-carbon 200 mesh copper
grids (Ted Pella, Inc.). The ultra thin specimens
were stained with 2% OsO4 (Osmium tetroxide,
Ted Pella, Inc.) for 48 h. The morphology was
observed under a JEOL (JEM-200CX) transmission
electron microscope (TEM) using an accelerating
voltage of 160 kV. To quantitatively determine
the domain size, at least 360 rubber phase
domains (or 10 TEM pictures) were examined
for each condition. The size, the distribution, and

The specimens were polished on both surfaces using


0.5 mm aluminum oxide grit. The final thickness was
less than 10 mm. Their hardness was determined in
a Shimadzu hardness tester (HMV-2000) with a load
of 300 g loading time of 30 s. Measurements of 15
areas along uniformly selected points of both
surfaces were made for each water-bath cured
resin. A total of 150 VHN (Vickers hardness) values
were obtained for 10 specimens. In each condition
of microwave method, at least six areas were
measured per specimen and a total of 46 VHN values
were obtained for eight specimens. An average of
150 or 46 VHN values was performed in each group
to determine if the variables of curing methods had
any statistically significant effect on the hardness.

Porosity
The pulse echo C-scans were performed with the
Testech ultrasonic tester (model VI-100). The
polished blocks were inspected at a test frequency
of 10 MHz using a 25.4 mm (1 in.) element transducer with approximately a 38.1 mm (1.5 in.) focal
length in the coupling medium (water), and were
scanned along the top surface at a speed of
0.2 mm/s. The interface delay was measured and
converted into a gray scale value on a C-scan image.

Flexural test
The mechanical test used was the three-pointbending test with a span-to-thickness ratio s=t of
4:1. Six to eight blocks of each condition were
tested at room temperature on a MTS dynamic
tensile testing machine (Model 810) at a crosshead
speed of 1.25 mm/min. The deflection reading as a
function of the applied load was recorded during
the entire test until the applied load dropped
substantially, as a result of internal damage in the
specimens.

Solubility
A sample from the fracture surface was cut into a
piece of about 0.2 g. It was then refluxed with
150 ml of tetrahydrofuran (THF) in a round-bottomed flask at a cycle of about 45 min. This
procedure continued for 25 26 h to ensure that all
soluble PMMA in the cuttings was extracted into
solution. The insoluble part was dried and then
weighed to determine its percentage. Three

136

C.-P. Lai et al.

confidence, and difference between means was


significant if P value was less than 0.05.

Results

Figure 1 Specimen temperature versus time for microwave power at 80, 160 and 240 W, respectively.

samples were taken from each group for the


solubility analysis. The sol parts were used for the
molecular weight determinations.

Gel permeation chromatography (GPC)


The analysis was performed on a Waters 150CV GPC.
THF was used as the mobile phase at a flow rate of
1.0 ml/min with two Styragelw HT columns in series
at 40 8C. The system was calibrated with eight
standard samples of polystyrene (PS) of known
molecular weight. A PS molecule has an average
of length in THF at ambient
weight of 41 for each A
temperature. The Q -factor for PS is therefore 41.
PMMA has an approximate Q -factor of 23 under the
same condition. Q -factor method was used to
estimate the molecular weights of the sol parts of
cured PMMA resins.

Statistics
Means and standard deviations were calculated for
each measurement or property. A one-way analysis
of variance (ANOVA) was conducted on the data of
domain size, hardness, and flexural properties
seeking statistically significant difference between
one water-bath and four microwave cured specimens. Means were compared at the 95% level of

Fig. 1 shows the average temperature changes of 10


measurements during PMMA polymerization when
heated by microwave power at 80, 160 and 240 W,
respectively. The temperature of the specimens
cured at high power increased more rapidly and
reached a constant value more quickly than that at
lower ones. In the case of 240 W (open triangles),
the temperature of the resins began to increase
rapidly to 97 ^ 16 8C after irradiation for 5 min. The
temperature tended towards 120 8C with a standard
deviation of 5.6 8C at 7, 4.3 8C at 8 min, and finally
3 8C from 9 to 15 min. The variation of temperature
with time for acrylic resin cured at 160 W is plotted
as open circles. In the first 1 min, the temperature
rose at almost the same rate as that at
240 W. Beyond 1 min, the temperature increments
became slower and it was 75 ^ 8 8C at 6 min. After
the specimens were irradiated for 6 min, the
temperature rose more rapidly to 107 ^ 7 8C at
9 min, then to a final temperature of 111 ^ 3 8C
from 10 to 15 min. The same trend was seen when
the output power was 80 W (filled squares). The
plateau of temperature was 109 ^ 4 8C when the
specimens had been irradiated at 80 W for 14
20 min. This plot reveals the effect of decreasing
the output power, i.e. lower the field strength,
lower the heating rate, and lower the level off
temperature.
Fig. 2a and b depicts the typical morphology of a
specimen cured in a water-bath. This cured acrylic
resin may be considered to comprise three components: a plastic phase that is continuous, a
dispersed graft copolymer, and an effective rubber
phase that is also dispersed. The gray or white
phase represents PMMA (circle C). Circle B
illustrates the dispersed stained phase with a
diameter of about 0.1 mm. Circle A in Fig. 2a
represents the effective rubber phase (domain) with
a diameter between 0.24 and 0.67 mm. A close-up

Figure 2 TEM micrographs of denture base resins cured in conventional water-bath (a) overall view and definition of
domains, (b) close view.

Morphology and properties of denture acrylic resins

137

Table 1 Statistical analysis of the domain size of the effective rubber phase.
Number of
domains

Water-bath curing
Microwave power

Overall
80 W
160 W
240 W
560 W

383
2485
685
756
675
369

Mean domain
size (mm)

0.395
0.373
0.379
0.378
0.370
0.354

of a typical circle A is shown in Fig. 2b where


PMMA was trapped in a large rubber phase and some
small stained rubber phases were also dispersed in
it. The number of domains, means, standard
deviations, and the bounds of 95% confidence
level for the statistical analysis of the effective
rubber phase are listed in Table 1. As shown in the
first row, the mean domain size was
0.395 ^ 0.068 mm, and 95% confidence level ranged
from 0.388 to 0.402 mm for the water-bath cured
specimens. The domain size distribution was 1.042
(see Fig. 4a), and the volume fraction of the
effective rubber phase was 10.3%.
The TEM micrographs in Fig. 3a d show the
specimens cured at a microwave power of 80, 160,
240, or 560 W, respectively. The domain size ranges
from 0.18 to 0.62 mm, and their means are
0.379 ^ 0.060, 0.378 ^ 0.070, 0.370 ^ 0.072, and
0.354 ^ 0.062 mm, respectively (see Fig. 4b, and
rows 3 6 of Table 1). The corresponding distributions are 1.038, 1.048, 1.051, and 1.044.
The occupied area (or the volume fraction) of

Std. dev.
(mm)

0.068
0.067
0.060
0.070
0.072
0.062

95% Confidence
interval (mm)

Water-bath vs. microwave

Lower
bound

Upper
bound

P-value

P , 0:05

0.388
0.370
0.375
0.373
0.365
0.347

0.402
0.375
0.384
0.383
0.375
0.360

1.346 1027
8.926 1025
1.101 1024
2.985 1028
1.576 10217

Yes
Yes
Yes
Yes
Yes

the effective rubber phase decreased from 8.44,


7.99, 7.80 to 7.50%, i.e. the effective rubber phase
decreased with increasing microwave power. For
the overall microwave-cured specimens, the distribution is plotted in Fig. 4a, and is compared with
the water-bath cured specimens. As shown in the
last two columns of Table 1, ANOVA revealed
significant difference P , 0:05 of the mean
domain size between the overall microwave cured
specimens, or the microwave specimens cured at
each energy level, and the water-bath cured
specimens.
Table 2 compares the solubility, porosity, molecular weights, and polydispersity for the specimens cured in the water-bath and in the microwave
oven at four different powers. The insoluble wt% of
all the specimens is shown in Table 2, along with the
standard deviations. Mean values were found to be
60.6 ^ 2.2 wt% for the water-bath method and
60.0 68.0 wt% for the specimens cured in a microwave oven. The resin blocks showed the least
amount of porosity, 0 10%, compared to when

Figure 3 TEM micrographs of denture base resins cured by microwave power at (a) 80, (b) 160, (c) 240, and (d) 560 W,
respectively.

138

C.-P. Lai et al.

Figure 4 Domain size distribution for denture base


resins cured by (a) water-bath versus microwave
methods, (b) Microwave power at 80, 160, 240, and
560 W, respectively.

cured in the water-bath. The blocks cured at 80 and


160 W had a similar amount of porosity, 60 and 65%,
respectively. The blocks showed large amounts of
porosity, 80%, when cured at 560 W. Compared with
all the blocks for the microwave method, the blocks
cured at 240 W were considered to have markedly
decreased porosity (40%). The molecular weight
 n ; together with the peak M
 p ;
 w =M
distribution M

 w averages, are listed in


 n and weight M
number M
Table 2. All of the sol parts of the cured resins had
average molecular weights in the order of 6 104
 n ; of 105 for M
 w and M
 p : The molecular weight
for M
distributions were between 2.37 and 2.75.
The mean Vickers hardness is shown in Table 3,
along with the standard deviations, and 95%
confidence interval. The overall microwave cured
specimens showed a small but significantly lower
(17.38 ^ 0.33 VHN) value than the water-bath
cured specimens (17.62 ^ 0.78 VHN) for mean
hardness P , 0:05: Specimens 160 and 560 W also
showed a small but significantly lower value,
17.20 ^ 0.27 and 17.25 ^ 0.32 VHN, respectively.
However, specimens 80 and 240 W had values of
17.41 ^ 0.28 and 17.65 ^ 0.27 VHN, and showed no
statistical difference P . 0:05 when compared
with the water-bath cured specimens.
From the load/displacement curves, the flexural
strength and flexural modulus were calculated by
using the equations of homogeneous beam theory.
Fig. 5 shows the flexural strength and the displacement for the specimens cured by different
methods. The mean flexural strength was found to
be 144 ^ 17 MPa and the mean displacement value
was 0.83 ^ 0.17 for the specimens cured in waterbath. The results of the statistical analysis of
flexural strength and displacement are listed in
Tables 4 and 5, respectively. ANOVA exhibited
highly significant differences between the two
processing methods. The flexural strength of the
specimens cured by microwave showed a strength
of 89 92% of water-bath cured ones. Discernible
differences were evident in a comparison of the
flexural displacement and the flexural modulus.
The flexural displacement was 2.3 2.4 mm for the
microwave cured specimens, which was at least 2.8
times that cured in the water-bath. In contrast, the
flexural modulus was one-third. Examination of Fig.
5, Tables 4 and 5 revealed there was little
difference among the microwave cured specimens

Table 2 Solubility, porosity, molecular weights, and polydispersity.


Water-bath curing

Insoluble wt%
Porosity
Molecular weights
n
M
w
M
n
 w =M
M
p
M
a

Microwave power
80 W

160 W

240 W

560 W

60.6 (2.2)a
0 10%

65.2 (2.8)
60%

60.0 (7.9)
65%

68.0 (1.8)
40%

62.7 (1.8)
80%

64400 (1350)
171500 (1630)
2.75
153,500

68600 (4600)
170300 (4260)
2.48
141,800

59500 (3140)
163000 (7120)
2.74
140,700

65300 (2690)
154900 (6400)
2.37
129,400

66900 (1230)
167200 (8470)
2.50
130,500

The number inside the parentheses is the standard deviation.

Morphology and properties of denture acrylic resins

139

Table 3 Statistical analysis of Vickers hardness (VHN).


Data points
(# of specimens)

Water-bath curing
Microwave power

Overall
80 W
160 W
240 W
560 W

150 (10)
184 (32)
46 (8)
46 (8)
46 (8)
46 (8)

Mean

17.62
17.38
17.41
17.20
17.65
17.25

Std. dev.

0.78
0.33
0.28
0.27
0.27
0.32

for the mean values of flexural strength and


displacement. The statistical analysis for significance confirms this observation (P . 0:05; as shown
in the last two columns of Tables 4 and 5).

Discussion
Microwave polymerization is affected by the random availability of benzoyl peroxide, and the
variation in duration and magnitude of exothermic
reaction, etc.10,11 The half-lives of benzoyl peroxide initiator are 7.3, 1.4 h, and 19.8 min at 70,
85, and 100 8C, respectively.12 The higher the
power applied to the system, the more the resin
temperature rises,13 the faster the benzoyl peroxide decomposes, and the more rapid is the
polymerization reaction. In these experiments,
the temperatures rose rapidly in the center of the
resin blocks. Because a microwave oven has almost
no thermal inertia, the response is effective and
almost instantaneous. From the half-lives of benzoyl peroxide, it is clear that the time required for
substantial conversion of monomer to polymer
would be impractically long at temperatures much
below 100 8C.14 To avoid porosity especially in the
thick parts of dentures, polymerization must be
conducted at a relatively low temperature (70 8C)
and slowly (9 h) in a hot-water bath. When
comparing both heating methods, quite a large
difference in the curing temperature was observed.
This study has shown that microwave energy can
efficiently polymerize denture base polymer. Microwave processing has a potential for saving a great
amount of time in processing dentures.
Microwaves acted initially on the MMA monomers
inside the resin blocks, therefore MMA absorbed
much energy in the beginning of polymerization.
After initiation of polymerization and a period of
conversion of MMA monomers, the resulting exotherm raised the heating rate.10 The standard
deviation of the final equilibrium temperature was

95% Confidence interval

Water-bath vs.
microwave

Lower bound

Upper bound

P-value

P , 0:05

17.49
17.33
17.33
17.12
17.57
17.15

17.75
17.43
17.50
17.29
17.73
17.34

1.820 1024
0.0825
5.070 1024
0.815
1.961 1023

Yes
No
Yes
No
Yes

less than 4 8C in all cases, as shown in Fig. 1.


However, the standard deviation was 13 16 8C
when the resin blocks were irradiated at 240 W for
2 6 min, and it was 11 17 8C at 80 W for 6 12 min.
It means that at the position of the thermocouple
some resin blocks have absorbed more than average
energy in the beginning and the initial stage of
polymerization is very efficient. The other blocks
may absorb more energy at a later stage, and then
there is a rapid rise in the resin temperature and the
rate of polymerization that continues until substantial conversion of monomer is achieved.
One would normally expect the polymerization
rate and the temperature to fall rapidly with time in
the final stages due to a decrease in the thermal
motion of polar monomers as a result of polymerization and crosslinking. In the De Clercks studies,10
the polymer did not become hot in the microwave
oven because PMMA has a glass transition temperature Tg at 105 8C. Since the polar ester side group
was not involved in curing, the dipolar relaxation of
the cured PMMA did not disappear completely. The
relaxation time of the orientation movement of
such groups (b relaxation) is shorter than the
relaxation time of main-chain segments (a relaxation), allowing them to retain their mobility below
Tg ; so that the resin blocks could be heated and

Figure 5 Flexural strength and flexural displacement


for specimens cured in water-bath and microwave oven.

140

C.-P. Lai et al.

Table 4 Statistical analysis of flexural strength.


Number of
specimens

Water-bath curing
Microwave power

Mean
strength (MPa)

Std. dev.
(MPa)

95% Confidence interval


(MPa)

Water-bath vs.
micsrowave

Lower bound

Upper bound

P-value

P , 0:05

0.011

Yes

0.861
(Microwave-vs.
microwave-)

No

Overall
80 W
160 W
240 W

6
30
7
8
8

144
130
128
128
132

17
10
9
12
10

126
126
120
118
124

161
134
136
138
140

560 W

131

11

120

142

maintained at a high temperature that depended on


the microwave power. Because of the merging of
the a and the b relaxations in PMMA at frequencies
. 10 kHz, the critical temperature of PMMA at
2.45 GHz is 185 8C.15 In these experiments, the
final temperature was below 185 8C. It suggested
that the microwave energy absorbed by the resin
blocks was in equilibrium with the energy conducted away from the resin blocks. This is important because a form of self-regulation of the curing
program takes place. This temperature must be
controlled accurately and the timing must be
correct. Therefore, 7, 10, and 15 min were selected
to cure acrylic resins at 240, 160, and 80 W,
respectively. Then the microwave flask was turned
over, and cured for an additional 2 min at 560 W in
order to make the curing complete.
Since the initial size of the dispersed graft
copolymer was very small, 0.1 mm, the possible
effect of the initial size (circle B) on the toughness
of denture resins can be neglected. For the waterbath specimens, the volume fraction of the effective rubber phase increased up to 10.3% with a
mean domain size of 0.395 mm. For the microwave
cured specimens, the volume fraction of the
effective rubber phase decreased from 8.44 to
7.50% with an increasing microwave power from 80
to 560 W. The mean domain size also decreased

from 0.379 to 0.354 mm with a P value of


2.65 1029 (, 0.05) among these four power
levels. The mean domain size and the volume
fraction of the rubber phase are in favor of the
water-bath method. A highly significant difference
in morphology indicated that it was important to
choose a suitable power and curing (or polymerization) time.
The results of the temperature measurement
and the solubility analysis indicated that a microwave oven for curing resin was much faster than a
conventional water-bath, and the degree of curing
also increased a little. The sol part of water-bath
 p ; whereas the
 w and M
specimens had the highest M
sol part of the resins after curing at 240 W had the
 p : It may be related to the weight
 w and M
lowest M
percent of soluble part, 39.4 for the former ones
versus 32.0 for the latter. Based on the lack of
consistency in the molecular weight analysis, an
advantage cannot be claimed for either method of
curing. Though the curing time of resins could be
remarkably shortened by the use of the microwave,
hardness for the microwave cured specimens is very
close to that of the water-bath cured specimen.
Microwave processing temperatures beyond
100.3 8C caused vaporization of the monomer and
produced porosity. Compared with the specimens
cured in the microwave oven, the water-bath cured

Table 5 Statistical analysis of displacement.


Number of
specimens

Water-bath curing
Microwave power

Displacement,
mean (mm)

Std. dev.
(mm)

95% Confidence interval


(mm)

Water-bath vs. microwave

Lower bound

Upper bound

P-value

P , 0:05

1.576 10217

Yes

0.947
(Microwave-vs.
microwave-)

No

Overall
80 W
160 W
240 W

6
30
7
8
8

0.83
2.36
2.33
2.34
2.35

0.17
0.35
0.22
0.21
0.40

0.65
2.23
2.13
2.16
2.02

1.01
2.49
2.54
2.51
2.69

560 W

2.43

0.54

1.94

2.93

Morphology and properties of denture acrylic resins

141

resin is considered to have markedly decreased


porosity. Porosity became inevitable with thicker
specimens whose voids might be formed by shrinkage in the inner portion. The blocks cured at 240 W
seemed to be superior to other microwave cured
blocks because of little porosity and their sufficiently cured state.

89-2216-E-110-027 from the National Science


Council, ROC.

Conclusions
A significantly large difference in the curing
temperature was observed upon comparing these
two processing methods. This study has shown that
microwave energy can efficiently polymerize and
cure denture base polymer from the results of
insoluble weight percent and the curing temperature. Highly statistical differences in morphology
and flexural properties were evident in a comparison of processing methods. The size and the volume
fraction of the rubber phase are in favor of the
water-bath method. However, the amount of
porosity increased with an increase in microwave
energy level. Thus, the water-bath cured specimens
showed better flexural strength and flexural modulus than the microwave-cured specimens. There
were no significant differences in the surface
hardness and the domain size distribution of the
effective rubber phase. It has been stated that
choice of a suitable power and polymerization time
is important in order to reduce porosity to a
minimum level. Microwave processing has a potential for saving time in processing dentures.

Acknowledgements
This work was partially supported by grant
VGHNSU88-01 from the Veterans Affairs Commission, Executive Yuan, ROC, and by grant NSC

References
1. Craig RG. Restorative dental materials, 7th ed. St Louis: CV
Mosby Co; 1985. p. 362.
2. Nishii M. Studies on the curing of denture base resins with
microwave irradiation: with particular reference to heatcuring resins. J Osaka Dent Univ 1968;2:2340.
3. Kimura H, Teraoka F, Ohnishi H, Saito T, Yato M. Applications
of microwave for dental technique (Part 1): dough-forming
and curing of acrylic resins. J Osaka Univ Dent Sch 1983;23:
439.
4. Kimura H, Teraoka F, Saito T. Applications of microwave for
dental technique (Part 2): adaptability of cured acrylic
resins. J Osaka Univ Dent Sch 1984;23:439.
5. Reitz PV, Sanders JL, Levin B. The curing of denture acrylic
resins by microwave energy: physical properties. Quint Int
1985;8:54751.
6. Peyton FA. Packing and processing denture base resins. J Am
Dent Assoc 1950;40:5216.
7. Hayden WJ. Flexural strength of microwave-cured denture
baseplates. Gen Dent 1986;34:36771.
8. Shlosberg SR, Goodacre CJ, Munoz CA, Moore BK, Schnell RJ.
Microwave energy polymerization of poly(methyl methacrylate) denture base resin. Int J Prosthodont 1989;2:4538.
9. Smith LT, Powers JM, Ladd D. Mechanical properties of new
denture resins polymerized by visible light, heat, and
microwave energy. Int J Prosthodont 1992;5:31520.
10. De Clerck JP. Microwave polymerization of acrylic resins
used in dental prostheses. J Prosthet Dent 1987;57:6508.
11. Huggett R, Brooks SC, Bates JF. The effect of different curing
cycles on levels of residual monomer in acrylic resin denture
base materials. Quint Dent Technol 1984;8:36571.
12. Odian G. Principles of polymerization, 2nd ed. New York:
Wiley; 1981. p. 196.
13. Chen M, Siochi EJ, Ward TC, McGrath JE. Basic ideas of
microwave processing of polymers. Polym Engng Sci 1993;33:
1092109.
14. Al Doori D, Huggett R, Bates JF, Brooks SC. A comparison of
denture base acrylic resins polymerized by microwave
irradiation and by conventional water bath curing systems.
Dent Mater 1988;4:2532.
15. Chen M, Siochi EJ, Ward TC, McGrath JE. The dielectric
behavior of glassy amorphous polymers at 2.45 GHz. Polym
Engng Sci 1993;33:111021.