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Objectives. To evaluate the initial bonding properties of recently and previously introduced
soft relining materials to denture base polymers with different polymerization techniques
Keywords:
Triad Resiline) to three denture base polymers (Paladon 65, Palapress Vario, Ivocap Plus) were
Adhesion
assessed with a modied method. Paladon 65 specimens immersed in water for 3 months
Chairside
were also used to test the effect of water content of denture base polymer on bond strength
Dental materials
results. After testing, a visual examination of the fracture surfaces and a SEM investigation
Relining
of the interface structure were performed. Tensile strength of each soft liner material was
Silicone
also tested. Data were analyzed statistically by two-way ANOVA (alpha = 0.05).
Tensile failure
Results. Signicant differences were found among tensile bond strength results (P < 0.05).
Vinyl poly(organosiloxane) soft liners (Mollosil Plus, Dentusil, U gel Soft, GC Reline Soft,
Silagum Comfort) and a plasticized PMMA soft liner (Vertex Soft) gave statistically similar
bond strength results for different denture base polymers (P > 0.05). For the other materials
used (Astron Soft, Molloplast B, Flexacryl Soft, Triad Resiline), different denture base polymers caused signicantly different results (P < 0.05). Poly(organosiloxane) based materials
gave slightly higher bond strength results with water immersed specimens than with the
dry specimens.
Signicance. A wide variety of newly formulated soft liners used in this study gave comparable
or better bond strength results compared to Molloplast B.
2006 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.
1.
Introduction
Correspondence author at: NIOM, Nordic Institute of Dental Materials, Kirkeveien 71B, P.O. Box 70, NO-1305 Haslum, Norway.
Tel.: +47 67 51 22 00; fax: +47 67 59 15 30.
E-mail address: eystein.ruyter@niom.no (I.E. Ruyter).
0109-5641/$ see front matter 2006 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.
doi:10.1016/j.dental.2006.11.014
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d e n t a l m a t e r i a l s 2 3 ( 2 0 0 7 ) 13731381
types of soft liners used today include addition and condensation poly(siloxanes) and plasticized acrylic soft liners [13].
To obtain adequate bond strengths, soft liners usually need
special bonding agents that interact with the surface layer
of the denture base polymer and the soft liner. Several different types of bonding agents were used for silicone soft
relining materials. A popular formula used for recent materials contains a polymeric substance dissolved in a solvent.
This substance can either be a reactive molecule, i.e. an
organo-silane which usually enhances bonding with its reactive groups, or molecules like PMMA dissolved in solvents
which work by increasing the wettability of the substrate and
by impregnating the surface layer with the polymeric ingredients [20].
Another frequently used type of bonding agent consists of
a single solvent or multiple solvents. A solvent-based bonding agent enhances bond strength by swelling the surface
and improving wettability of the substrate. Solvents also have
the advantage of cleaning the surface from environmental
pollutants and dissolving and dispersing loose particles covering the surface of PMMA. Some of the solvents are also
capable of displacing water and reaching deeper into the
polymer and thus facilitating the penetration of monomers
[12,20].
The mechanical properties of soft relining materials and
their bonding characteristics have been evaluated by various test methods [24,69,11,12,19,21]. There are three widely
accepted methods for testing adhesion of denture soft liners
to denture base polymers: peel, lap-shear and tensile testing [2]. The usefulness of these methods have been discussed
[24,69,11,12,19]. Testing the soft liners using peel testing is
believed to be the best simulation of the clinical setting for the
failure of soft lining materials. However, the results obtained
from peel tests were reported to be unsatisfactory due to the
higher probability of cohesive failures in the soft materials
[9,12,16,22]. Another point is that the results obtained in a peel
test are inuenced by the compliance of the materials as well
as the thickness [2].
In lap-shear testing, the stresses applied to the specimen
are believed to be concentrated at the edges of the lining material [2]. This may make the interpretation of bond strength
results and failure mechanisms difcult. The shear strength
of the bond is also affected by the deformation rates of the
component materials which make the situation even more
complicated given the differing viscoelastic properties of different relining materials [2].
For testing the adhesion between the soft lining materials
and PMMA denture base polymer, the tensile test method was
preferred. This method was described by American Society
for Testing and Materials (ASTM) and data obtained from such
samples were found signicant for testing the effectiveness of
different processing techniques and various adhesive systems
[23].
Testing the adhesion of soft liners to a hard substrate has
some practical difculties which originate mainly from low
tear strengths of the soft materials. Debonding the soft liner
from the hard surface during bond strength testing usually
initiates rupture. Many authors have investigated the fracture
surfaces after testing and reported cohesive failures. In case of
tearing of the soft lining material, the strength of the adhesion
2.
The manufacturers information, identication codes and recommended processing methods of the materials used in this
study are presented in Table 1.
A standard test method for evaluating tensile strength
of adhesion [23] was used with some modications with
regard to specimen production. The denture base polymer
was cured around stainless steel screws (Fig. 1A) for easy
manipulation during surface standardization, soft liner application and testing [25]. An acrylic block with 16 cylindrical
recesses was used (Fig. 1A, simplied by using one recess for
demonstration purposes) and a stainless steel screws head
was inserted into every recess leaving the rest of the screw
outside and xed using modelling wax (Fig. 1A). After moulding the pattern, wax was boiled out and the acrylic block
was removed from the mold. The denture base polymer was
cured in the space obtained around the steel screw heads
(Fig. 1A). After polymerization of the denture base polymer,
the surface of the specimen to which soft liner was to be
applied was ground wet with 220, 500, 1200 grit (FEPA) (particle size 68, 30, and 14 m, respectively) SiC abrasive papers
(Struers A/S, Copenhagen, Denmark), using a Planapol (Struers
A/S) grinding machine. This procedure was carried out in
order to obtain surfaces perpendicular to the long axis of the
specimen.
The PMMA specimens and the axial alignment jig are
shown diagrammatically in Fig. 1AD. A cylindrical, translucent poly(ethylene) tube of 3 mm height and 11 mm diameter
was used as a mould for the soft relining material (Fig. 1A).
The polyethylene collar used in this study has previously been
used to control the volume and bonding area of the soft liner
and was reported to cause no interference with bond testing
[12].
The soft relining materials were cured between the two
denture polymer specimens (Fig. 1C). Two tapped brass bars
held the specimens in the correct position. A constant
downward pressure was applied to the specimens during
polymerization for a better simulation of a chairside reline
procedure in which the patient bites on the material (Fig. 1C).
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d e n t a l m a t e r i a l s 2 3 ( 2 0 0 7 ) 13731381
Material type
Manufacturer
Processing method
Denture base
polymer Colour:
pink 1
Denture base
polymer Colour:
clear 7
Denture base
polymer Colour: S
Soft liner
Soft liner
Primer
Dentusil (DNT)
Dentusil Adhesive (DNTB)
Soft liner
Adhesive
Molloplast B (MLP)
Primo adhesive (MLPB)
Soft liner
Adhesive
Soft liner
Primer
Soft liner
Bonding agent
Soft liner
Adhesive
Soft liner
Primer
Soft liner
Primer
Soft liner
Paladon 65 (P65)
Light activation
Autopolymerizing
Recommended for Mollosil plus. Apply
and let solvent dry for 1 min
Autopolymerizing
Recommended for Dentusil. Apply and
air-dry for 3060 s
Heat-cure
Recommended for Molloplast B. Apply
and let dry for 6090 min
Autopolymerizing + air pressure unit
Recommended for Flexacryl soft. Apply
and allow to dry
Light-cured
Recommended for TRS. Bench set for
2 min, cure in Triad curing unit for 2 min
Autopolymerizing
Recommended for Ugel soft. Apply to
the surface and let aerate for 1 min
Autopolymerizing
Recommended for GC Reline soft. Apply
to the surface and gently dry with air
Autopolymerizing
Recommended for Silagum AM Comfort.
Apply and let solvent dry for 1 min
Heat-cure
Fig. 1 Illustration showing (A) A stainless steel screws head inserted into the recess of the acrylic block leaving the rest of
the screw outside and xed using modelling wax. After moulding the pattern, wax was boiled out and the acrylic block was
removed from the mold. The denture base polymer was cured in the space obtained around the steel screw heads. (B) The
alignment jig and testing assembly before the application of soft liner. (C) Force applied to the specimen during
polymerization. (D) Testing of specimen under tension.
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3.
Results
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Components
Primer
UFS
SLC
MLS
FLS
DNT
TRS
VRS
ASL
PMMA: poly(methyl methacrylate); PEMA: poly(ethyl methacrylate); MMA: methyl methacrylate; THFMA: tetrahydrofurfuryl methacrylate;
HDDMA: hexanediol dimethacrylate; EGDMA: ethylene glycol dimethacrylate; bis-EMA: bisphenol-A-diethyl methacrylate.
Table 3 The results of tensile strength and tensile bond strength values (in MPa)
Tensile strength
Mean
ASL
MLS
DNT
MLP
FLS
TRS
UFS
GCS
SLC
VRS
1.12a,z
1.64a,zy
1.66a,zy
2.42a,wx
1.62a,zy
2.85a,x
1.86a,y
3.96a,w
3.24a,xw
4.46a,v
S.D.
0.27
0.35
0.48
0.75
0.63
0.42
0.25
0.66
0.22
0.68
PPVa
IVPa
Mean
S.D.
Mean
S.D.
Mean
S.D.
0.71c,z
0.99b,zx
1.36a,zx
0.74b,zyx
2.05a,zyx
2.44a,zyx
1.59a,yx
2.08a,y
2.43a,y
4.18a,w
0.13
0.28
0.19
0.44
0.43
0.57
0.49
0.77
0.65
1.44
0.53d,z
1.05b,zy
1.34a,zyx
2.02a,zyx
1.59ab,zyx
1.47ab,yx
1.46a,yx
2.09a,yx
1.85a,x
4.59a,w
0.03
0.05
0.25
0.36
0.44
0.33
0.22
0.57
0.35
1.14
0.88b,z
0.84b,z
1.38a,zy
1.49a,zy
1.22b,zy
1.44b,zy
1.71a,y
2.74a,x
2.45a,x
3.35a,w
0.11
0.27
0.16
0.32
0.18
0.49
0.43
0.42
0.47
0.31
Groups with same letters ad horizontally, vz vertically are not signicantly different (P > 0.05).
a
statistically similar (P > 0.05) except for ASL and MLS where
the tensile strength of the liners were higher than the bond
strength (P < 0.05).
Fig. 2 shows how the failure types were distributed for every
soft liner-denture base polymer combination. The majority of
bond failures were a mixture of failure in the bulk of the reline
material and at the interface. The locus of failure was observed
to be 12.6% A, 32.2% B, 36.6% C, and 18.6% D.
Test results for bond strength to dry P65 and P65 which
had been immersed in water are graphically presented in
Fig. 3. The bond strength results for poly(organosiloxane)
based soft liner materials were slightly higher compared to the
specimens made using wet substrate than the corresponding
untreated substrate.
Precipitates could be collected after centrifugation of the
bonding agents FLSB and SLCB. The analysis showed that both
Fig. 2 Chart showing the locus of failure for each specimen group. Visually pure interfacial failure (adhesive) (A, open),
interfacial failure with thin residue (B, pointed), interfacial failure with bulk failure (C, dashed), complete bulk failure of
relining material (D, closed).
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FLSB and SLCB contained PMMA. For the other bonding liquids,
centrifugation with ethanol resulted in no precipitate showing
that they do not contain poly(methacrylates).
The SEM images obtained from the interface of SLC, VRS
and FLS when used versus P65 are presented (Figs. 46). The
interface layers formed by soft liners and bonding agents were
observed to vary revealing different effects. The system with
SLC (Fig. 4) material shows a discernible but intimate contact whereas for VRS (Fig. 5) a much closer state indicating
interpenetration was observed making it difcult to distinguish the substrate and the soft liner. FLS (Fig. 6) had a very
obvious interface layer where the two materials meet and this
interface layer also shows gaps and cracks.
Fig. 4 (A) SLC and (B) P65. The arrows showing the intimate and continuous contact at the interphase.
Fig. 5 (A) VRS and (B) P65. Arrows indicate continuous interpenetration in the interphase.
d e n t a l m a t e r i a l s 2 3 ( 2 0 0 7 ) 13731381
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Fig. 6 (A) FLS and (B) P65. Arrows indicate the appearance of Acrylic Primer layer.
4.
Discussion
The 10 soft liners that were chosen for this study cover the
spectrum of main material types available today. With a large
sample size the bond strength results for different soft materials and the success of different bonding mechanisms can be
compared.
One material (MLP) is a well-known and extensively studied
liner, claimed to be a hydroxyl-terminated polydimethyl siloxane [21]. Studies [17,18,28] show it to have acceptable bonding
properties, suitable softness and relatively long service life.
In the present study, MLP was among the materials found to
have low bond strength, but failure was recorded as type C or
D (Fig. 2). These failure types include bulk failure in the liner
and show that the cohesive strength of this material played
an important role in failure during either initiation or propagation of the cracks.
Three different denture base polymers were used in the
present study. Although they had minor chemical differences,
they were chosen because of their different processing methods. Processing methods may inuence the surface properties
of the materials and hence bonding to the soft liners. The
MLP material has 3-methacryloyloxypropyltrimethoxysilane
in both the primer and the paste itself, which aids bonding
to PMMA via the methacrylate groups of the organo-silane in
addition to its function as a cross-linker [21]. The methacrylate group may bond to the pendant methacrylate groups on
the surface of the denture base [29]. The results show that the
MLP material had signicantly better tensile bond strength
to IVP and PPV than to P65. Different quantities of pendant
methacrylate groups present in the denture materials can be
one explanation [29].
Vinyl-containing poly(organosiloxane) (A-silicone) materials were proposed as replacement for MLP because of their
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5.
Conclusion
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