Dental Materials Journal 24 (3) : 433-439, 2005

Mechanical Properties of An Experimental Soft Lining Material Based on

Urethane Oligomer

Takahito KANIE1, Akihiko KADOKAWA2, Hiroyuki ARIKAWA1, Koichi FUJII1 and Seiji BAN1
Department of Biomaterials Science, Graduate School of Medical and Dental Sciences, Kagoshima 1 University, 8-35-1
Sakuragaoka, Kagoshima 890-8544,Japan
Department of Fixed Prosthetic Dentistry,
2 Graduate School of Medicaland Dental Sciences,Kagoshima University, 8-35-1
Sakuragaoka, Kagoshima 890-8544,Japan
Correspondingauthor, E-mail:[email protected]

Received June 6, 2005/Accepted July 29, 2005

The purpose of this study was to investigate the apparent viscosities and mechanical properties of two experimental light-
curing soft lining materials (SLM-1 and SLM-2) based on soft-type urethane oligomers, as well as the shear bond strength
and dye penetration between the denture base resin and the polymerized SLMs after storage in water. The apparent
viscosities of SLM-1 and SLM-2 were 144.0-146.9 and 1.9 Pa •s respectively. After storage in water for two prescribed periods
(one day and three months) , the mechanical properties of the SLMs on the overall were 10.6-20.6 MPa for elastic modulus,
69.3-72.1 for hardness, and 3.8-4.0 MPa for adhesive strength. Tensile strength was observed to decrease after three months'
storage in water, when compared to that after one-day storage (p< 0.01) . Water sorption rates also differed significantly
(p<0.05) — namely 3.0 and 2.8 mg/cm2 for SLM-1 after one day and three months respectively, and 2.0 and 2.2 mg/cm2 for
SLM-2. As for dye penetration, no infiltration was observed at the denture base resin-SLM interface after three months'
storage. Based on the results of this study, it seemed like the SLMs possess many suitable properties for use with a new
technique that we recently developed for preparing denture base resin and soft lining material.

Key words : Soft lining material, Mechanical property, Light-curing

patients as a means to enhance denture retention,

INTRODUCTION
stability, and adaptability between the denture and
Some patients with maxillary complete dentures use the oral soft tissue. Their usage is most effective
an elastic (or viscoelastic) material between the den- when used on the denture at all times. The flip side
ture and the oral soft tissue. Jepson et al.1) and is that using such products without proper medical
Thomas and Mori2) analyzed the viscoelastic proper- instruction can lead to stomatitis, bacterial infection,
ties of denture soft lining materials based on creep and resorption of the alveolar ridge9) . Hence, if pro-
and recovery tests. Grasso3) discussed the efficacy fessionals are equipped with a thorough knowledge of
and effect of denture adhesives on the health of the the attributes and limitations of denture adhesives,
underlying oral tissue. Aloul and Shen4) studied the they can better guide and educate patients in the
roles of alcohol and plasticizer in the mechanical management of their prostheses10,11) Although the
properties of soft liners. misuse of soft lining materials for denture wearers
Tissue conditioners, soft lining materials, denture often causes medical problems, many dental profes-
adhesives, and home reliners are available to denture- sionals and patients support using the materials as a
wearing consumers for use between the denture and means to enhance denture stability and retention12-14) .
the oral soft tissue. Professionals use tissue condi- The common technique for preparing denture
tioners and soft lining materials to correct anatomi- base resin and soft lining material involves adhering
cal or physiological defects. Existing soft lining ma- the elastic material to the denture after the prosthe-
terials are classified into two main types — acrylic sis has been made. Although some new lining mate-
and silicone rubber lining materials. Most silicone rials have been investigated15 -17), their application fol-
rubber materials do not adhere well to acrylic den- lows the traditional technique. If there exists a tech-
ture base resins, although there have been some suc- nique that produces denture with an accurate elastic-
cesses5,6). Acrylic materials tend to harden owing to ity on the mucosa side right from the beginning,
the loss of plasticizer in the mouth and roughing of then not only can the patient cut down on the num-
the surface by denture cleansers7,8) . Denture adhe- ber of hospital visits, but is also able to obtain a
sives and home reliners are sold over-the-counter for denture that fits closely against the alveolar ride and
self-use by patients with maxillary complete den- one that properly disperses the bite pressure. To
tures. All of the elastic (or viscoelastic) materials this end, the authors developed a new technique
mentioned above are accepted by professionals and wherein the denture was created with a cushion of
434 MECHANICAL PROPERTIES OF A SOFT LINING MATERIAL

elastic material built into the prosthesis18) . In this and three months. A compression test was con-
new technique, a soft lining material was placed at a ducted with a universal testing machine (TG-50kN,
designated position on the tissue side of the denture, Minebea, Nagano, Japan) at a cross-head speed of 2
followed by adding a dough of the denture base resin mm/min and within the proportion limit in air at 37
before polymerization. To ensure success with this . The same irradiation and storage conditions
new technique, the polymerized or hardened elastic were used for the following tests.
material must bond tightly to the acrylic denture
base resin because the elastic material was placed on 2. Hardness
the model plaster first. Existing materials, however, Test specimens (30 X 30 X 6 mm) were made using a
could not bond with denture base resins, and there- PTFE mold. The mold was sandwiched between two
fore could not be used in our new technique. glass plates, and SLM in the mold was irradiated
Our previous investigations suggested that two times through the glass plate — once from the
acrylic denture base resin and polymerized urethane top and the other time from the bottom. After stor-
oligomer bond tightly when an acrylic denture base age, Shore A hardness was measured with a
resin was reinforced with various pre-polymerized durometer (GS-710, Teclock, Nagano, Japan) in air
urethane oligomers19) . The purpose of this investiga- at 37°C.
tion was to evaluate the mechanical properties of po-
lymerized experimental soft lining materials made 3 . Tensile strength
from two soft-type urethane oligomers. The SLM was put into a PTFE mold with a dumb-
bell-type hollow (No.6, JIS K6251-1993, Japan) , and
the surface was covered with polyethylene film.
MATERIALS AND METHODS
After polymerization with light and storage for the
Materials prescribed period, a tensile strength test was con-
The self-curing denture base resin, a PMMA-based, ducted with the universal testing machine using a
slightly cross-linked, multiphasic polymer (Pour cross-head speed of 254 mm/min at 23°C in air.
Resin, Shofu, Kyoto, Japan) , was used at a powder-
liquid ratio of 1.8 g/ml. 4 . Water sorption
Two soft-type urethane acrylate oligomers (UA- Test specimens (20 mm in diameter X 6 mm in
160TM, Shin-Nakamura Chem., Wakayama, Japan; height) were made using a PTFE mold, which was
and SH-9832, Negami Chem., Ishikawa, Japan) — sandwiched between two glass plates. The specimens
consisting of acryl residue, isocyanate residue, diol were irradiated two times — once from the top and
residue, and with two functional groups — were used the other time from the bottom. After polymeriza-
as a main component of two experimental soft lining tion and arranging the shape, the test specimens
materials in this study (SLM-1 and SLM-2) . They were weighed immediately (Wa) on an analytical bal-
were added 1 wt % camphorquinone (Wako Pure ance (FR-200MKII, A&D, Tokyo, Japan) and stored
Chem., Osaka, Japan) as a photosensitizer and 1 in water at 37°C. After each storage interval at one
wt% 2- (dimethylamino) ethyl methacrylate (Wako day or three months, test specimens were removed
Pure Chem.) as a reducing agent. For mixing, a ho- and wiped with soft papers to remove excess mois-
mogenizing machine (AR-100, Thinky, Tokyo, Japan) ture on the surfaces. The test specimens were then
with high-speed rotation and orbit motion was used weighed on the balance until a stable weight (within
in a dark room. After mixing, the mixtures were 1 mg) was obtained (Ws) . Water sorption was de-
put into a black bottle. termined with the following formula:
The apparent viscosity of the experimental soft
lining materials (SLMs) was measured with an E-
type viscometer (Visconic EHD, Tokyo Seimitsu,
Tokyo, Japan) at shear rates of 1.75, 3.5, 7.0, and where S is the surface area of the test specimen.
17.5 sec-1 at 23±0.5°C.
5 . Adhesive strength
Specimens preparation and measurements Fig. 1 shows a schematic representation of a test
1 . Elastic modulus in compression specimen used for the adhesive strength test. First,
The SLM was put into a *polyethylene tube (10 mm the SLM was put into a PTFE mold (30 X 20 X 0.5
in diameter X 10 mm in height) on a glass plate, and mm) and polymerized. Second, the self-curing den-
the top of the tube was covered with another glass ture base resin was mixed, poured into the PTFE
plate. It was then polymerized for five minutes mold five minutes later, and heated in an oven at
using a light irradiation unit (a -Light, Morita, 50 °C for 30 minutes (SDR-1) according to
Tokyo, Japan) . After removal from the polyethylene manufacturer's recommendation. Finally, a SDR-2
tube, the polymerized test specimens were soaked in was arranged in the same manner as SDR-1. After
water at 37°C for two different time periods: one day storage for the prescribed period, a tensile test was
 KANIE et al. 435

strength, and adhesive strength tests respectively.

Three test specimens were tested for water sorption
and dye penetration. Student's t-test was used to
identify significant differences between the values
measured at one day and at three months.

RESULTS
Fig. 2 shows the variations of the apparent viscosity
of the experimental soft lining materials (SLMs)
Fig. 1 Schematic representation of a test specimen for
with shear rate. The apparent viscosity of SLM-1
the adhesive strength test, where SDR (1) and
ranged from 144.0 to 146.9 Pa.s and significantly de-
SDR (2) : self-curing denture base resin, and SLM:
creased with increasing shear rate (p<0.01). The ap-
experimental soft lining material.
parent viscosity of SLM-2 was at a constant value of
1.9 Pa.s.
Table 1 shows the results of elastic modulus in
conducted with the universal testing machine using a compression, hardness, tensile strength, and water
cross-head speed of 0.5 mm/min in air at 23°C. Ad- sorption of SLMs soaked in water at 37 °C for one
hesive strength was calculated using the tensile force day and three months. Highly significant differences
based on an adhesion area of 20 X 10 mm.

6 . Dye penetration
First, the SLM was put into a PTFE mold (40 X 10
x 0.5 mm) and polymerized. Second, the polymerized
SLM was put on the center of another PTFE mold
(40 X 30 X 1.0 mm) . The self-curing denture base resin
was mixed, filled into the PTFE mold five minutes
later, and heated in an oven at 50 °C for 30 minutes.
After polymerization, nail enamel was painted near
the border between the SLM and the self-curing den-
ture base resin to prevent penetration of the basic
fuchsin solution. The top and bottom surfaces of the
test specimen were polished using a # 1200 water-
proof polishing paper, and the test specimen was
soaked in 0.2% basic fuchsin solution at 37°C for one
day and three months. After washing in running
water, the test specimen was observed with an optical
microscope ( x 10 magnification, Nikon, Tokyo,
Japan) .

Statistical analysis Fig. 2 Viscosities of the experimental soft lining materi-

One-way analysis of variance (ANOVA) and Tukey's als before polymerization measured at shear rates
test were used to compare the differences in apparent of 1.75, 3.5, 7.0, and 17.5 sec-1 (a: SLM-1; b:
viscosity. Five test specimens were used for the SLM-2) .
elastic modulus in compression, hardness, tensile

Table 1 Mean value (standard deviation) of SLM-1 and SLM-2 measured at one day and three months of storage
436 MECHANICAL PROPERTIES OF A SOFT LINING MATERIAL

soft tissue (0.7-4.4 MPa) 23). • Future investigations

are needed to address whether the elasticity of SLM
should become lower or higher than that of oral soft
tissue. As for the elasticity of denture adhesives, it
is a rarely researched topic. Nonetheless, Murata et
a1.24) have reported that the storage modulus of
cream-type denture adhesives was 16-236 Pa at 1 Hz
- which is extremely low relative to those of other
soft lining materialsm.
Fig. 3 Photographs on dye penetration after three
Surface hardness also affects oral sensitivity.
months (left: SLM-1; right: SLM-2).
The hardnesses of polymerized SLMs were 69.9 and
69.3, and there were no statistical differences between
the values at one day and at three months (p>0.05).
were seen in the tensile strength values of test speci- According to Inoue et al.22), the hardness values of
mens soaked for one day versus three months acrylic, silicone, olefin, and fluoro soft lining materi-
(p<0.01). Likewise, water sorption of specimens als ranged from 2.0 to 66.2 reflecting the same
soaked for one day was significantly different from range as the elastic modulus values. Another study
that soaked for three months (p<0.05). measured the hardness of oral soft tissue using a
Table 1 also shows the shear bond strength after trial hardness tester, and reported the value to be
one day and three months of storage. No significant 0.5-40.023). These findings revealed that the individ-
differences in shear bond strength between the soak- ual variability and thickness of oral soft tissue must
ing periods were observed (p>0.05). Further, no dye be taken into consideration. Fine tuning between
penetration was observed by optical microscopy (x 10 strength and oral sensitivity is difficult for long-
magnification) between the denture base resin and term usage. On this note, the elasticity and hard-
SLMs after three months (Fig. 3) . ness required by our new technique would be more
thoroughly investigated and determined through
clinical trials.
DISCUSSION
Waters and Jagger25) measured the tensile
Viscosity is an important property of soft lining ma- strength of both commercially available and experi-
terials. In particular for our new technique, the mental silicone soft lining materials, and reported
SLM is to be painted on the model plaster with a values of 2.12 and 5.20 MPa respectively. The tensile
brush or spatula before polymerization. Our results strengths of SLMs were similar to those of silicone
showed that the apparent viscosity of SLM-1 was be- soft lining materials. Apart from tensile strength,
tween 144.0 and 146.9 Pa • s, which was higher than Al-Athel and Jagger also measured the shear bond
the viscosity of UDMA measured by Silikas and strength of silicone soft lining materials26,27) . The
Watts (7.1 Pa •s)20), but similar to that of the base initial tensile and shear bond strengths were reported
paste of a polyether rubber impression material by to be 1.96 MPa and 1.48 MPa respectively26), but de-
McCabe and Arikawa (120.0 Pa •s)21). Although the creased to 1.46 and 0.78 MPa after 3 months27)
required viscosity has not been determined, the meas- Thus, it has been shown by Al-Athel and Jagger
ured viscosity was adequate for our new technique to that tensile bond strength is greater than shear bond
accomplish its goal of preparing the denture base strength26). In general, the tensile bond strength of
resin and the SLM. Meanwhile, the SLM must also silicone soft lining materials is 0.79-3.11 MPa28), and
keep its shape until irradiated with light. Fig. 2 (a) that of acrylic soft lining materials is 0.61-1.44
shows the thixotropic property of SLM-1. Prefera- MPa29). However, the shear bond strengths of SLMs
bly, SLM-1 should be soft for painting and be hard (3.8-4.0 MPa) were greater than the tensile bond
after painting, and that SLM-2 has sufficient fluidity strength of acrylic or silicone soft lining materials.
to be painted with a brush. The result implied that the non-polymerized surface
Elasticity is an important property for the po- layer of SLM played an important role in bonding.
lymerized SLM. In the present study, the elasticity Small molecular chains, such as the MMA monomer
modulus did not decrease after three months of stor- of denture base resin, are advantageous when the
age (p>0.05), indicating stable oral sensitivity. monomers permeate into a resin matrix, providing
Elastic moduli of 0.4-0.5 MPa for acrylic soft lining better adherence30).
materials, 0.5-2.0 MPa for silicone rubber, and 8.9 In this investigation, the water sorption of SLM-
MPa for olefin have been reported22) - which are 1 after one day was 3.0 mg/cm2 but decreased sig-
lower than the elastic moduli obtained in the present nificantly after three months (p<0.05). The water
investigation (10.6 and 20.6 MPa). The elasticities of sorption of SLM-2 after one day was 2.0 mg/cm2,
commercially available soft lining materials are ei- but increased significantly after thee months
ther too low or too high compared with that of oral (p<0.05). This result of SLM-1 indicated that the
 KANIE et al. 437

weight of the absorbed water was less than that of model plaster by using a spatula or brush and then
the eluted monomer, although both the elution of polymerized. Following which, the denture base resin
monomers and water sorption progress simultane- mixture was added. This new technique may be used
ously in the matrix resin in water. Different speci- to laminate SLMs with different elastic moduli by re-
men shapes have been tested for water sorption, and peating the second and third steps of the flowchart
data have been expressed in various units31-33) . Even in Fig. 4. Moreover, it is possible to change the elas-
though the apparent diffusion rate of water into a ticity both inside and outside, such as in a functional
resin matrix may be the same for different shapes, gradient material (Fig. 5) . Other advantages of this
water sorption for each shape may differ because the new technique include having partially hardened or
surface area has been changed by the shape — but partially softened SLM by using materials of differ-
the different shapes still yield the same weight. ent elastic moduli, and applying the SLM to both full
Therefore, water sorption is expressed as weight per and partial dentures.
area unit. Many concerns — such as the extent of elasticity
Leon et al.31) reported 0.2-3.0% water sorption for SLM, the reduction of oligomers' water sorption
for acrylic soft lining materials. The water sorption capacity, and the thickness of SLM to be applied —
values determined in the present study were 2.0 and remain regarding the use of SLM both in vivo and in
1.3% after converting our measured values, although vitro. Nevertheless, no dye penetration was observed
the shapes of the test specimens differed. Muraoka between the experimental soft lining materials and
et a1.32)reported the maximum water sorption of sili- the denture base resin after three months. In conclu-
cone soft lining materials to be 6.4 mg/cm3. Our sion, the SLMs possess many suitable properties for
study showed 23.1 and 15.5 mg/cm3 water sorption
after converting our measured values, although again
the shapes of the test specimens differed. The results
indicated that the water sorption of SLMs was
within the range of acrylic soft lining materials but
greater than that of silicone. Labella et al.33) re-
ported 2.0-6.3% water sorption using polyfunctional
co-monomers and indicated an effect of hydrophilic
groups. Although water sorption occurs with all
materials, the water sorption of SLM was greater
than that of acrylic denture base resin (0.69 mg/
cm') . To circumvent this problem, it may be effective
to add a hydrophobic group, such as an alkyl or
phenyl group, to the urethane oligomers used here.
According to some reports on denture adhesives,
using denture adhesives contributed to reduced den-
ture movement, that almost all denture adhesives
tested exhibited greater retentive ability than saliva,
water, and alcohol (1.6-22.1 N) , and that the reten-
tive force between denture adhesives and various
Fig. 4 Flowchart comparing the newly designed and tra-
adherends were 0.9-21.8 N34-36). These measured val-
ditional techniques for the preparation of a den-
ues span a wide range, and it is not clear whether a
ture base resin and soft lining material.
higher value reflects the greater effectiveness of an
adhesive or the better viscoelastic properties of a
well-fitting prosthesis.
A tight adhesion between the pre-polymerized
(or hardened) soft lining material and the acrylic
denture base resin is one of the critical factors that
determines the success of a denture liner, and like-
wise the success of our new technique. In previous
studies on denture base resin reinforcements, the
authors have reported that acrylic denture base resin
could firmly adhere to pre-polymerized urethane
oligomers1s18,19). Leveraging on this finding, soft-type
urethane oligomers that would provide sufficient ad- Fig. 5 Schematic representation of some examples of
hesion were therefore selected for the experimental hard and soft experimental soft lining materials
soft lining materials. These experimental soft lining applied to a denture.
materials (SLMs) were first placed directly on the
438 MECHANICAL PROPERTIES OF A SOFT LINING MATERIAL

use with our newly developed technique to prepare 17) Zhao K, Cheng XR, Chao YL, Li ZA, Han GL. Labora-
denture base resin and soft lining material. tory evaluation of a new denture adhesive. Dent Mater
2004; 20: 419-424.
18) Kanie T, Arikawa H, Fujii K, Ban S. Mechanical prop-
ACKNOWLEDGEMENTS erties of soft lining materials based on urethane
oligomer. J J Dent Mater 2005; 24: 121, Abstr. P-34.
This work was partially supported by a Grant-in-aid
19) Kanie T, Arikawa H, Fujii K, Ban S. Light-curing re-
for Scientific Research (No.17592031) from the Japan
inforcement for denture base resin using a glass fiber
Society for the Promotion of Science.
cloth pre-impregnated with various urethane
oligomers. Dent Mater J 2004; 23: 291-296.
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