Original article

Bond strength of denture teeth to acrylic resin: effect of

thermocycling and polymerisation methods

Debora Barros Barbosa, Valentim Adelino Ricardo Barão, Douglas Roberto Monteiro, Marco
Antonio Compagnoni and Juliê Marra
Department of Dental Materials and Prosthodontics, Araçatuba Dental School, São Paulo State University (UNESP), São Paulo, SP, Brazil

doi:10.1111/j.1741-2358.2008.00218.x
Bond strength of denture teeth to acrylic resin: effect of thermocycling and polymerisation methods
Background: Failure of bonding between acrylic resin teeth and denture base material is a considerable
problem for patients who wear complete dentures.
Objective: The purpose of this study was to evaluate the bond strength between acrylic resins and resin
denture teeth with different thermocycling and polymerisation methods.
Materials and methods: Microwave-polymerised (Onda-Cryl), heat-polymerised (Clássico) and auto-
polymerising (Jet) acrylic resins and resin denture tooth (Biotone) were used. The acrylic resins were
polymerised according to the following: (A) microwave – fast cycle, Onda-Cryl; (B) microwave – long cycle,
Onda-Cryl; (C) microwave – manufacturer’s cycle, Onda-Cryl; (T) water bath – long cycle, Clássico; and (Q)
bench polymerisation cycle, Jet. Twenty specimens were prepared for each polymerisation method. Ten
were thermocycled, and 10 did not receive thermocycling. For the purpose of the study, a shear test was
used. Data were analysed with the Kruskal–Wallis test and Dunn’s multiple comparisons test (p = 0.05).
Results: Cycles B, C and T were similar (p > 0.05), and had statistically higher bonding values than cycles
A and Q (p < 0.05) for the thermocycled and non-thermocycled groups. For all cycles, there were no
statistically significant differences between thermocycled and non-thermocycled groups (p > 0.05), except
for cycle Q (p = 0.0038).
Conclusion: Thermocycling decreased the bond strength, but not significantly for microwave and heat-
polymerised cycles. Regarding the bond strength of denture teeth to acrylic resin, the fast microwave
polymerisation cycle should be avoided when polymerising Onda-Cryl acrylic resin. In addition, Jet acrylic
resin is not adequate for use in denture repair.

Keywords: acrylic resins, bonding, shear strength, denture bases, tooth, artificial, thermocycling.

Accepted 9 December 2007

debonding of acrylic teeth from the acrylic resin

Introduction
The most common reason for the elderly to seek
dental treatment is for the replacement of missing
teeth1. Although the number of edentulous people
has decreased, there are still many patients needing
treatment that require complete dentures2.
Various materials and fabrication techniques
have been used to prepare dentures1. An acrylic
resin denture base material has been available to
the dental profession for over 60 years, and
although materials with superior properties have
been on the market for the same time, it still
remains the most popular choice3. However,
 2008 The Authors
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denture base continues to present problems1,4.
The failure rate of acrylic resin dentures resulting
from fracture has been reported to be unacceptably
high5, with the most common type of failure
encountered being debonding or fracture of the
teeth6. According to Huggett et al.7, approximately
30% of all denture repairs received by commercial
dental laboratories involved faults attributed to
failed bonding between the teeth and the denture
base resin. Several factors affect this bond, such as
wax remaining on the ridge lap area of the teeth,
careless application of the separating medium
during processing8, insufficient available monomer
237
238 D.B. Barbosa et al.
during processing8 and the polymerisation method
used in the processing of denture base resins9.
Intraoral temperature changes are produced
from routine eating10, drinking11 and breathing12,
and can change the interface between the
acrylic resin teeth and acrylic resin denture
base. Laboratory simulations of clinical service
are often performed because clinical trials are
costly and time-consuming13. Thermocycling is
an in vitro process used to simulate in vivo
events and is often represented in these studies.
However, the regimens used vary considerably
between studies and, with few exceptions14, are
always proposed without reference to in vivo
observations13.
The bond strength between two types of acrylic
resin denture teeth and a pour-type denture base
resin after thermocycling was examined by Chai
et al.15 Thermocycling significantly decreased the
bond strength of the two types of resin teeth.
These results were in agreement with the findings
of Amin16, who compared the bond strength of
heat-polymerised and autopolymerising acrylic
resin to acrylic denture teeth after storage in water
and thermocycling. The deterioration in bond
strength was attributed to leaching of monomer
and water sorption resulting in some interfacial
separation.
The method of denture base resin polymerisation
might also influence the adhesion between acrylic
teeth and the acrylic resin denture base9. Poly-
merisation by microwave energy is an alternative
to conventional water-bath processing17,18, pre-
senting the principal advantage of greatly reducing
the polymerisation time of the denture base resin19.
However, there is the difficulty of controlling the
rising temperature of the exothermic polymerisa-
tion reaction20, such that a rise above the boiling
point of the monomer leads to the formation of
porosities18.
Polyzois and Zissis21 found inferior bonding be-
tween acrylic teeth and denture base material
polymerised by microwave energy compared to hot
water-bath polymerisation. Porosities can reduce
the strength properties of the denture base mate-
rial22,23, with the formation of porosities at the
interface between the artificial teeth and denture
base resin as a probable explanation for the bond
failure after microwave polymerisation24. The same
results were found by Schneider et al.19 and Ta-
kahashi et al.25 The higher bond strengths to the
tested denture teeth were obtained with the con-
ventional heat-polymerised acrylic resin than with
the microwave-polymerised acrylic resin. However,
in another study, the bond strength of microwave-
Journal compilation  2008 The Gerodontology Association and Blackwell Munksgaard Ltd, Gerodontology 2008; 25: 237–244
polymerised acrylic resins to denture teeth was
greater than that of conventional heat-polymerised
acrylic resins26.
Differences in types of denture teeth, acrylic re-
sin and the experimental technique used might
explain the variation in reported results27.
Depending on the study, the load mode was
tensile16,19,28–33, shear3,26,34–37, peel7,24, compres-
sive25,29 and transverse three-point3,35–39 or four-
point bending40.
In the literature, most of the bond strength
studies used conventional heat-polymerised den-
ture base materials and autopolymerising acrylic
resins7,27,34,38,39. Studies of microwave-polymer-
ised denture base materials 25,26 and the effect of
thermocycling15,16,32 on bond strengths are more
rare, especially when denture base resins are
polymerised by microwave energy and thermally
cycled19.
If the problem of debonding teeth were solved,
the elderly population would benefit by avoiding
repeated repair of their dentures1. The purpose of
this study was to evaluate the bond strength be-
tween three types of acrylic resin and resin denture
teeth with different thermocycling and polymeri-
sation methods. On the basis of the limited data
available, the null hypothesis was that neither
thermocycling nor polymerisation methods would
affect the shear bond strength between the acrylic
resin and the artificial tooth.
Materials and methods
A representative brand of resin cross-linked den-
ture teeth, composed of poly-methylmethacrylate,
ethylene glycol dimethacrylate, mineral pigments
and fluorescent organic pigment (Biotone, Dents-
ply Ind. e Com., Rio de Janeiro, RJ, Brazil) was
chosen for bonding three types of acrylic resins: a
heat-polymerised resin, a microwave-polymerised
resin and an autopolymerising resin. The acrylic
resins are listed in Table 1 with the polymerisation
methods used in this study. Twenty specimens
were prepared for each polymerisation method;
ten were thermocycled, and 10 were not thermo-
cycled.
The ridge-lap surfaces of the denture teeth were
ground using 320, 400 and 600-grit wet/dry sand-
paper (Norton; Saint-Gobain Abrasivos Ltd, Vin-
hedo, SP, Brazil) in a polishing machine (Arotec
Ind. e Com. Ltd, Cotia, SP, Brazil) at 300 r.p.m.
until flat. Flattering this surface does not affect the
cross linking within the teeth, since the cross
linking is part of the matrix of the acrylic resin
polymer tooth42. The cross-linked polymer matrix
 2008 The Authors
 Bond strength of denture teeth to acrylic resin 239

Table 1 Acrylic resins and polymerisation methods used in the study.

Acrylic resin Polymerisation method Manufacturer Mixing ratio

Onda-Cryl (microwaveable Cycle A – microwave: Artigos Odontológicos Clássico Ltd, 1.097 g/0.5 ml
denture resin) 500 W/3 min41 São Paulo, SP, Brazil
Onda-Cryl (microwaveable Cycle B – microwave: Artigos Odontológicos Clássico Ltd, 1.097 g/0.5 ml
denture resin) 90 W/13 min + 500 W/90 s41 São Paulo, SP, Brazil
Onda-Cryl (microwaveable Cycle C – microwave: Artigos Odontológicos Clássico Ltd, 1.097 g/0.5 ml
denture resin) 320 W/3 min + 0 W/4 min + São Paulo, SP, Brazil
720 W/3 mina
Clássico (conventional Cycle T – water bath: Artigos Odontológicos Clássico Ltd, 1.097 g/0.5 ml
thermopolymerised 74C/9 h41 São Paulo, SP, Brazil
denture resin)
Jet (autopolymerising Cycle Q – bench Artigos Odontológicos Clássico Ltd, 1.097 g/0.5 ml
acrylic resin) polymerisation at 23C São Paulo, SP, Brazil
a
Cycle recommended by Onda-Cryl manufacturer.

of a proprietary tooth is usually not evenly
distributed in the tooth structure, with the gingival
ridge-lap area not as highly cross-linked as the
incisal area of the tooth42.
Each denture tooth was embedded in an auto-
polymerising polymer (PMMA) using an embed-
ding machine (Arotec Ind. e Com. Ltd), which
heats a polymer above its glass transition temper-
ature. After cooling, the denture tooth was firmly
embedded into the polymer (Fig. 1) and the pro-
jecting ridge-lap surface of each embedded denture
tooth was ground flat with 320, 400 and 600-grit
wet/dry sandpaper. The specimens were then
cleaned with water.
A silicone rubber mould frame (Zetalabor; Zher-
mack S.p.A., Rovigo, Italy), with a cavity approxi-
mately 5 mm diameter and 2.5 mm deep, was
used to control the bonding area15,43. The micro-
wave, heat and auto-polymerising acrylic resins
were packed into the mould and polymerised
(Fig. 2) 3,29.
The silicone mould was fixed on the embedded
tooth with an adhesive (Super Bonder; Loctite
Henkel Ltd, Diadema, SP, Brazil). Tracing com-
pound (Kerr Corporation, Orange, GA, USA) was
then melted and packed into the hole of the sili-
cone rubber mould. The silicone rubber mould and
embedded tooth were invested with dental stone
(Gesso-Rio; Orlando Antonio Bussioli-ME, Rio
Claro, SP, Brazil) into a denture flask. After the
dental stone had set, the flask was opened and the
tracing compound was removed from the mould.
The tooth surface was carefully cleaned with a
small brush and distilled water to remove any
impurities. The microwave and water bath-poly-
merised resins were mixed according to the man-
ufacturer’s recommendations (Table 1) and were
then polymerised.
The autopolymerising acrylic resin was mixed
according to the manufacturer’s instructions, with
the dough resin packed directly into the hole of
the silicone mould. Resin processing for these
specimens was not performed in the denture
flask. The silicone mould, embedded tooth and
autopolymerising acrylic resin were kept on the
bench until the polymerisation was completed

Figure 1 Denture tooth in the poly-

mer after the embedding process.
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240 D.B. Barbosa et al.

Figure 2 Sample specimen and method for determination of shear bond strength. Diameter /1 and /2 were 5.0 mm
(approximately) and 2.5 mm for the acrylic resin polymer processed on the surface tooth15,43.

and the silicone mould was then carefully re- Table 3 Dunn’s multiple comparison test among cycles
moved. according to each situation.
The completed specimens were deflasked after
the final polymerisation and flask cooling. All Non-thermocycling Thermocycling
specimens were stored at 37C for 50 ± 2 h in
distilled water. Half of the specimens were then B C T Q B C T Q
thermocycled between 4 and 60C with 30 s dwell A * ** ** ns * * * ns
times for 5000 cycles. B – ns ns * – ns ns ***
The apparatus that was used to test shear bond C – ns *** – ns ***
strength, which allowed the application of force T – ** – ***
0.50 ± 0.02 mm from the joint surface, is repre- Q – –
sented in Fig. 2. The specimen was adjusted and
ns, nonsignificant difference (p > 0.05).
fixed for shear testing, with all tests performed on a *Significant difference (p < 0.05).
Universal testing machine (EMIC-DL 3000; EMIC **Significant difference (p < 0.01).
Equip. e Sist. de Ensaios Ltd, Curitiba, PR, Brazil) ***Significant difference (p < 0.001).
using a crosshead speed of 1 mm/min43. The load at
fracture was recorded.
Mean values for all the groups tested were adhesive failure patterns at the acrylic resin/den-
analysed using Kruskal–Wallis test. The variables ture tooth interface.
were polymerisation method and thermocycling.
Dunn’s post hoc multiple comparisons test was
Results
computed to identify those groups which were
significantly different at p < 0.05. SPSS for Win- Mean shear bond strength and standard deviation
dows was used for data analysis (SPSS Inc., (SD) values for the groups and the Dunn’s
Chicago, IL, USA). test are illustrated in Tables 2 and 3. They list
The fracture sites were evaluated with a scanning the post hoc analysis according to each cycle,
electronic microscope (SEM) (Scanning Microscope where the groups and cycles were compared.
Jeol JSM-T330a; JEOL Ltd, Tokyo, Japan) at a For all cycles, no significant differences were
magnification of 350 to determine cohesive and found between the thermocycling and non-

Table 2 Mean shear bond strength (MPa) and standard deviation for each group.

Polymerisation cycles

Groups A B C T Q

Non-thermal 4.57 ± 1.18 9.1 ± 2.78 10.18 ± 2.45 9.74 ± 1.50 4.22 ± 1.22
Thermal 3.43 ± 1.98 8.70 ± 2.20 9.32 ± 2.92 8.34 ± 1.26 1.66 ± 0.47

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Journal compilation  2008 The Gerodontology Association and Blackwell Munksgaard Ltd, Gerodontology 2008; 25: 237–244

(a)
Figure 3 (a) Scanning electronic
microscope (SEM) view of adhesive
acrylic resin surface failure. (b) SEM
view of adhesive acrylic resin surface (c)
failure, with surface topography
appearing to be the polymer matrix
with bead exposition. (c) SEM view
of mixed adhesive-cohesive surface
failure within acrylic resin. (d) SEM
view of mixed adhesive-cohesive
surface failure within denture tooth.
Original magnification ·350,
bar = 50 lm.
thermocycling groups (p > 0.05), except for cycle
Q (p = 0.0038).
There were no significant differences in the bond
strengths between the non-thermocycling and
thermocycling groups for cycles A and Q
(p > 0.05). The highest significant values were
found for cycles B, C and T (p < 0.01), with no
significant differences between the cycles (Table 3).
Following shear bond testing, the fracture inter-
faces of specimens were evaluated with SEM.
Adhesive failures were observed for the thermo-
cycling groups, regardless of the polymerisation
cycle (Fig. 3a,b). Adhesive failures were relatively
common for the non-thermocycling groups,
although mixed cohesive-adhesive failures also
occurred in cycles B and C (Fig. 3c,d).
Discussion
The original research hypothesis was rejected. In
this study, thermocycling and polymerisation
methods influenced the bond strength between
acrylic resin and artificial teeth. The 5000 30-s
thermocycles between 4 and 60C decreased the
bond strength of all polymerisation methods.
However, only the Q polymerisation method
exhibited significantly reduced strength values
when comparing thermocycling and non-thermo-
cycling groups. In addition, the thermocycled
group failed adhesively, while the non-thermo-
cycled group showed mixed cohesive and adhesive
failures. An explanation for the lower bond
strength values and the adhesive fractures of ther-
mocycling groups might be mechanical stresses
 2008 The Authors
Journal compilation  2008 The Gerodontology Association and Blackwell Munksgaard Ltd, Gerodontology 2008; 25: 237–244
Bond strength of denture teeth to acrylic resin 241
(b)
(d)
induced by differential thermochanges, inducing
crack propagation through bonded interfaces15.
The results of this study are in general agreement
with previous bonding studies involving thermo-
cycling15,44. Nevertheless, Clancy et al.32 found that
this did not affect the adhesion between acrylic
resins and denture teeth. The differences in the
thermocycling protocol most probably accounted
for the variations found among the studies. Chai
et al.15 and Saavedra et al.44 performed 10 000 and
12 000 thermocycles, respectively, whereas Clancy
et al.32 used 1000 cycles.
However, it has been observed that there is no
concrete evidence that bonding failures in clinical
practice occur as a result of thermostress13. Whe-
ther failures occur because of flowing in one or
another layer in the bonded structure is un-
known13. According to Gale and Darvell13, layer
flow must be dependent on the glass transition
temperatures of the bonded materials. These au-
thors supposed that such flow would lead to
collapse in a truly static test, at a stress below the
ordinary static strength.
The test results from the current and other
studies15,32,44 cannot discriminate these issues by
thermocycling. The type of denture tooth and
acrylic resin could account in part for the incon-
sistency of bonding strength results.
Regarding the polymerisation methods, the
microwave-polymerised cycles B and C, and the
conventional water bath-polymerised cycle (T)
exhibited higher bond strengths. Cycle A, which
represents a fast microwave polymerisation
method, and cycle Q achieved the lowest shear
242 D.B. Barbosa et al.
bond strength values. This result might suggest
that these cycles resulted in less monomer pene-
tration into the tooth and acrylic resin polymer
networks. The bond strength depends on the de-
gree of penetration of the monomer and the
strength of the interwoven polymer network
formed thereafter25. Moreover, unpolymerised
acrylic resin was in contact with the tooth surface
for a longer period in cycles B, C and T than for
the other cycles19.
The findings of Polyzois and Dahal24 disagree
with the current results. The bond strength with
microwave-polymerised denture base resin showed
higher values than water bath-polymerised resin,
except for cycle A, where the bond strength was
significantly lower than that observed for cycle T.
In cycle A, a rise in the temperature above the
boiling point of the monomer might have occurred.
More energy at the beginning of the polymerisation
reaction could have led to a rapid rise in resin
temperature18,45, resulting in the formation of
porosities at the tooth–denture base resin inter-
face18.
The differences in bond strength values in the
literature might be explained by the size and shape
of the specimens or the method and magnitude of
loading used during the test34. In this respect, a
universal testing technique might be required to
replace the many methods of determining tooth-
acrylic resin bond strength in use around the
world. A universal technique would facilitate
standardised testing and allow direct comparison of
results31.
The limitation of this study is that only one brand
of microwaveable denture base resin, conventional
heat-polymerised resin, and acrylic resin denture
tooth were tested. Further research is necessary to
determine the influence of different mechanical
and chemical treatments of denture teeth before
acrylic resin processing. In addition, the presence of
wax remaining on the ridge lap surface of the
artificial teeth or the careless application of sepa-
rating medium during processing should be evalu-
ated regarding bond strength. To overcome the
limitations of in vitro tests, the bonding between
denture teeth and acrylic resins should be evalu-
ated intraorally.
The clinical implication of this study is that the
microwave polymerisation method of acrylic resin
using longer microwave cycles could reduce the
bonding failures between the artificial tooth and
denture base resin. Intraoral temperature changes
may reduce the bond strength of denture teeth
repaired with autopolymerised acrylic resin. Fur-
thermore, to decrease the adhesive failures, the
Journal compilation  2008 The Gerodontology Association and Blackwell Munksgaard Ltd, Gerodontology 2008; 25: 237–244
tooth bond surface may be mechanically treated by
grinding39 or chemically treated with methyl
methacrylate monomer44.
Conclusion
Within the limitations of this in vitro study, the
following conclusions were drawn.
1. Thermocycling insignificantly decreased the
bond strength of all polymerisation methods, ex-
cept for microwaveable cycle Q, which was statis-
tically significantly decreased.
2. The polymerisation methods affected the bond
strength of the thermocycling and non-thermocy-
cling groups.
3. The conventional water bath cycle (T) and
microwaveable cycles B and C produced the high-
est bond strength values.
Acknowledgements
This study was supported by the FAPESP (grant
number 04/11250-9), FUNDUNESP (grant number
850/04-DFP) and PIBIC/Reitoria UNESP. The au-
thors thank Raphael Freitas de Souza for the sta-
tistical analysis, and Jeremy Matis for the English
review.
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Correspondence to:
Debora Barros Barbosa, Department of Dental
Materials and Prosthodontics, Faculdade de
Odontologia de Araçatuba, UNESP, José Bonifácio,
1193, Araçatuba, São Paulo, SP, Brazil 16015-050.
Tel./fax: (55) 18 3636 3245
E-mail: debora@foa.unesp.br
 2008 The Authors