Clinical Ma terials 12 (1993) 117-120 The Use of Microwave Energy to Cure Denture Acrylic Resins Randa IDiwan, E. C. Combe & A. A. Grant Department of Restorative Dentistry, University Dental Hospital of Manchester, Higher Cambridge Street, Manchester M 15 6FH, UK (Received 2 December 1991; sent for revision 9 March 1992; accepted 10 April 1992) Abstract: Experiments have been carried out on the curing of poly(methy1 methacrylate) denture base material in a microwave oven, using conventional dental flasks and flask clamps. It has been shown that it is important (a) to maintain sufficient pressure on the materials, (b) to avoid gaseous porosity by not heating too rapidly initially, and (c) to ensure that all metal is protected from exposure to microwaves. When the appropriate conditions of polymerisation were used, microwave-cured samples had satisfactory physical and mechanical properties according to American Dental Association specification number 12. INTRODUCTION Since the introduction of acrylic resin into the dental field for the constructi on of denture bases, several techniques have been employed for its fabri cation. One option is to use injection mould- ing,l though the most widely used technique is compression moulding of an acryl ic resin dough which consists of a mixture of poly(methy1 meth- acryiate) together with monomeric methyl meth- acrylate and an initiator such as benzoyl peroxide. This d ough is polymerised in a two-part metallic flask, either using a water bath or dry heat oven at typically 72 “ C for up to 14 h. Use of such a method to obtain a denture base that is free of porosity and has satisfactory physical and mechanic al properties consumes much time and energy. More rapid heat curing cycles have been explored by Jerolimov et cd2 can be used for curing denture acrylic resins.4s5 A technique using microwave energy has been re- ported in which a conventional denture base resin was cured in specially desig ned non-metallic flasks, for example, made of glass-fibre reinforced poly- ester resin flasks with polycarbonate bolts.5-11 Porosity of the resin was a potential problem, particularly for thicker sections of material. This work was undertaken to explore microwave techniques of curing, to see to wh,at extent this would be feasible using conventional dental flasks and materials, and to determi ne the necessary conditions for the production of porosity- free specimens with suitable mechanical properties. MATERIALS AND METHODS The chemical ly activated (self-curing) materials, containi ng a tertiary amine activator, require less energy but the resu ltant resin has a relatively high residual mon omer content, high creep values, lower strength and stiffness, poorer colour stability, and is not usually free of porosity.3 This work was carried out with a hea&-cured resin; this was an unpi gment ed materiatl, to enable assessment of porosity to be undertaken readily. A polymer/mono mer ratio of 2.5/l by weight was employed. The moulds were prepared from Kaffir D dental stone, mix ed at a water/powder ratio of 0.3. It has been sugg ested that microwave energy The microwave oven was an AEG Mi cromat 11 7 Ciinical Materids 0267-6605/ 93/ $06.00 0 1993 Elsevier Science Publishe rs Ltd, England 10-2
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The Use of Microwave Energy to Cure DentureAcrylic Resins
Randa IDiwan, E. C. Com be & A. A. GrantDepartment of Restorative Dentistry, University Dental Hospital of Manchester, Higher Cambridge Street,Manchester M 15 6FH, UK
(Received 2 December 1991; sent for revision 9 March 1992; accepted 10 April 1992)
Abstract: Experiments have been carried out on the curing of poly(methy1methacrylate) denture base material in a microwave oven, using conventionaldental flasks and flask clamps. It has been shown that it is important (a) tomaintain sufficient pressure on the materials, (b) to avoid gaseous porosity by notheating too rapidly initially, and (c) to ensure that all metal is protected fromexposure to microwaves. When the appropriate conditions of polymerisation wereused, microwave-cured samples had satisfactory physical and mechanicalproperties according to American D ental Association specification number 12.
INTRODUCTION
Since the introduction of acrylic resin into thedental field for the construction of denture bases,several techniques have been employed for itsfabrication. One option is to use injection mould-ing,l though the most widely used technique iscompression moulding of an acrylic resin doughwhich consists of a mixture of poly(methy1 meth-acryiate) together with monomeric methyl meth-acrylate and an initiator such as benzoyl peroxide.This dough is polymerised in a two-part metallicflask, either using a water bath or dry heat oven attypically 72 “C for up to 14 h. Use of such a methodto obtain a denture base that is free of porosity andhas satisfactory physical and mechanical propertiesconsumes much time and energy. More rapid heatcuring cycles have been explored by Jerolimovet cd2
can be used for curing denture acrylic resins.4s5 A
technique using microwave energy has been re-ported in which a conventional denture base resinwas cured in specially designed non-metallic flasks,for example, made of glass-fibre reinforced poly-ester resin flasks with polycarbonate bolts.5-11Porosity of the resin was a potential problem,particularly for thicker sections of material.
This work was undertaken to explore microwavetechniques of curing, to see to wh,at extent thiswould be feasible using conventional dental flasksand materials, and to determine the necessaryconditions for the production of porosity-freespecimens with suitable mechanical properties.
MATERIALS AND METHODS
The chemically activated (self-curing) materials,containing a tertiary amine activator, require lessenergy but the resultant resin has a relatively highresidual monomer content, high creep values, lowerstrength and stiffness, poorer colour stability, and is
not usually free of porosity.3
This work was carried out with a hea&-cured resin;this was an unpigmented materiatl, to enableassessment of porosity to be undertaken readily. Apolymer/monomer ratio of 2.5/l by weight wasemployed. The moulds were prepared from KaffirD dental stone, mixed at a water/powder ratio of
0.3.It has been suggested that microwave energy The microwave oven was an AEG Micromat
117C i i n i c a l M a t e r i d s 0 2 6 7 -6 6 0 5 / 9 3 / $ 0 6 . 00 01993 Elsevier Science Publishers Ltd, England 10-2
which operates at a frequency of 2450 MHz. Themaximum power was 650 W. The apparatusenabled different power settings to be selected: inthis work these ranged from 10 % to 100 % of theavailable power, thus enabling different rates of
polymerisation to be studied.In initial work, the moulds were designed to give
acrylic specimens of rectangular cross-section, ofdimensions 65 mm x 40 mm x 7 mm. Preliminaryexperiments were carried out under different con-ditions without using a conventional dental flask,because of the inadvisability of exposing metallicobjects to microwaves. Techniques were thenevolved, as detailed below, which permitted the useof dental flasks. Subsequently, specimens wereprepared under a wide range of polymerisationconditions, and examined visually for porosity.When optimum curing conditions had been found,some properties of the cured resin were determinedby the methods of American ental Association(ADA) specification number 12. These includedtransverse deflection, water sorption and solubility,and colour stability. Finally, dentures were made inthe unpigmented resin, to assess the practicalviability of the suggested curing technique
RESULTS AND DISCUSSION
Preliminary experiments
The first test was carried out at 100% power for10 min in moulds without any means of applyingpressure to the material, to determine if gypsumcould transmit microwaves to the resin. It wasobserved that the acrylic mass expanded after about7 min. At the end of the test, the gypsum was
Fig. 1. Porous acrylic specimens produced in a gypsum mouldwith pressure applied by G-clamps.
10 min then 50 %100 % power for
from the vo~at~~~satio~ of ~~~o~~~---.-~~ uncuring, leading to excessive residual ~~r~~~~~~r n
ower with visual ~bse~vati~~ of tspecimens after I 60 min it -was
hat this power setting was insucient ~~ly~e~~sati5~. At 2.0 %
findings were essentially similar. Thirty and 40 %power for 60 min gave ised bnt porous
was that cracking ofn observed. Attempts
essnre to gypsum mogauze were also often ~~s~~~essf~~~ n sc9me experi-
ments, a V-shaped pattern of porosity wasobserved owing ts uneven ~~~~~~~t~~~. f pressure
place.Following this, an ex
with the stonekept in its metal flask; wmetal discs removed, onmicrowaves could pass thrto reach the acrylic dough.the flask clamp waspressure could be a
Table 1 . Relation between curing cycle and porosity
Cur ing cyc let i m e a n d p o w er
(% I
Poros i ty oft h i n s p e ci m e n s
Poros i ty oft h i c k s p e ci m e n s
1 0 min at 10%60 min at 40 % Clear, non-porous10 min at 100%10 min at 1 0%90 min at 40 % Clear, non-porous
5 min at ‘100%10 min at 1 0%90 min at 40 % Clear, non-porous15 min at 100%
Clear with a singletiny central pore
Clear, non-porous
Clear, non-porous
10min at 10%100 min at 40 % 1
Clear, non-porous
20 min at 110% Incomplete40 min at 50 % polymerisation20min at IO%
1Won-porous, quite
50 min at 50 % transparent
Incompletepolymerisation
Slight porosity incentre of specimen
A few pores incentre of specimen
Slight porosity incentre of specimen
Did not polymerise
20 min at 1.0%60 min at 5 0 % 1 Clear, non-porous
20min at 10%90 min at 50% }
Clear, non-porous
20min at 10%30 min at 60% !-
Did not polymerise
20min at 10%30 min at 60% Clear, non-porous
Porosity in centre
5 min at 1 00%with branch shape
20min at 10%40 min at 60 %
IClear, non-porous Porosity in centre
20min at 10%45 min at 60% ?
Clear, non-porous Porosity in centre
Clear, non-porous
processed at 20 % power for 10 min, 50 % powerfor 10 min and full power for 10 min. Porousspecimens resulted, possibly because the gypsumwas not ex.erting sufficient pressure on the flask withthe acrylic dough. Also, the odour of monomercould be detected, suggesting that polymerisationwas incomplete.
In the next experiment, two flasks were used inthe clamp, and a longer curing time was adopted.The upper flask contained gypsum only, and the
Fig. 2. Dentures produced in an unpigmented resin by amicrowave technique.
lower one contained the dough. As before, this flaskwas used without its upper or lower metal discs.Curing was carried out at 20 %, 50 % and 100 %power consecutively, at 20 min for each powersetting. The specimens contained a small amount ofporosity.
On the assumption that this porosity was of thegaseous type, the above experiment was repeated,using a longer curing time, namely, 10 % power for20 min, 40 % for 40 min, 60 % for 10 min, then100 % for 10 min. This yielded apparently sat-isfactory specimens.
Table 2. Physical and mechanical properties of microwave-cured acrylics
Effect of curing cycle
Following this, many specimens were cured underdifferent conditions, and examined for porosity.Table 1 shows the observations for thick specimens(7 mm as above) and thin specimens (3 mm).
S a m p l e Deject ion (mm ) , for loads”1 .5-3 .5 kg 1 .5-H kg
Wa t e rsorp t ion’(m glcm’)
Wa t e rso lubi l i tyb(mglcm ”)
Col’ours tab i l i ty
Microwave cured :10 min at 10%90 min at 40% >15 min at 100%ADA specification
1.48 ( f 0.28) 3.24 ( f 0.44) 0.75 0.005
max. 2.5 min. 2.0max. 5.5
max. 0.8 max. 0.04 Slight change
Slight changein colour
a Mean of five determinations as required by specification.b Mean of two determinations as required by specification.
Table 2 shows data for microwave cured specimens,tested according to the ADA specification number12. It appears that satisfactory acrylic specimens
can be produced by this technique.Full upper and lower dentures were prepared in
the microwave oven using an unpigmented resin toenable observation of porosity, if any, to be carriedout. Figure 2 shows dentures cured at 10% powerfor 10 min, followed by 40 % power for 90 min,then 100 % power for 15 min. It can be seen that thetechnique appears to have been satisfactory.
CONCLUSIONS
Acrylic denture materials can be cured usingmicrowave energy. Conventional dental equipmentcan be used, provided care is taken to preventexposure of metal to microwaves. The techniqueoffers the potential of ensuring adequate curingwith minimal consumption of energy. Because ofthe potential of this system, further studies arebeing conducted on the effect of curing conditionson residual monomer and mechanical properties.
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