Andres Guzman, DDS

Influence of Surface
Treatment on Bond
Strength Between a HeatActivated and a LightActivated Resin Composite

Graduate Student of Dental Materials

B. Keith Moore, PhD
Director of Dental Materials

lahoratory

School of Dentistry

Indiana Uni-er/y
Indianapolis, Indiana

The shear bond strength of two light-aclivated resin composite materials to a

preformed heat-poiymerized resin material was measured. The substrate was
a ureihane dimethacrylate material designed for use as a direct bonded
pontic. In the first phase of the study, the shear bond strength between the
substrate and a urethane-based resin composite and seven surface treatments
was evaluated. In the second phase, a Bis-GMA re;in composite and three
surface treatments were studied. The study showed that a bonding agent was
essential tor the achievement ot an adequate bond strength between tbe
light-activated and heat-polymerized resin. However, there was a significant
difference in bond strength depending on the type of light-activated resin
composite and bond agent used. A Bis-CMA-based light-activated
composite, togetber witb its bond system (22.82 MPa), provided higher bond
strength than a urethane-based resin composite and its bonding system
(14.4.S MPa), There was a direct relationship between cohesive failure and
bond strength; as bond strength increased, tbe number of cohesive failures
increased as well, intj Prosti^odont 1995,-8:179^186.

esin bonded fixed partial dentures have been in

use for approximately 20 years. Rochette' first
described the use of a perforated framework for
splinting mobile, periodontally involved mandibular incisors. Howe and Denehy' adapted Rochette's
technique for the fabrication of an anterior fixed
partial prosthesis. A resin bonded direct pontic is an
alternative to the conventional resin bonded prostheses. Three different direct pontics have been
described-*: the acrylic resin tooth pontic, the ail
resin composite pontic, and the natural pontic.
One potential disadvantage of the direct pontic
technique is the lack of adequate strength to resist
torquing forces, resulting in cohesive fracture of
the resin composite.
The use of heat and pressure polymerized composite resins instead of unfilled acrylic resins has
substantially improved the properties of the resin
pontic. Currently, light- or dual-activated resin

composites are used to bond the pretormed resin

composite pontic to the abutment teeth.
Obviously, an "adequate" bond between the two
resin materials is essential. If one considers the
complete restoration, the bond strength between
the resin cement and natural tooth structure can be
used to define "adequate." According to the literature, bond strengths of resin composite to enamel
vary from 10 MPa to 21 MPa.-^'

Reprint requests: Dr B. Keith Moore, Director of Dental

Materials Laboratory. School of Dentistry, Indiana University,
I 21 West Michigan Stieet, tndianapoiii, Indiana 46202.

179

Several studies of the bond strength between

resin composites have been published. Chemical
bonding has been reported by Vankerckhoven et
al,' although Pounder and Forsten"'" concluded
that repaired resin composite did not provide adequate flexural strength after surface preparation.
Other studies have shown surface treatments
improving bond strength between resins. It has
been found that the application of an unfilled resin
(bonding agent) between layers of composite is
essential to attaining adequate bond strength."-'^
Roughening the surface ot the mature composite
has beert shown to improve the bond strength of
the new layer of resin placed using a bonding

The fnternationaf Journal of Prosthodonlics

Bond Strertii o Treated He.- and

it-Activated Resins

Table 1 Materials
Description

Bonding Agent
Dene Bridge pontic material Dirotian, Chicago, iL

TPH composite resin

CaulWDentsply, Miiford, DE

Pro Bond
XRV Herculite composite

Cauik/Dentsply, Miiford, DE
Kerr Manufacturing, Romulus, Mi

Optibond

Kerr Manufacturing, Romulus, Mi

Materials and Methods

agent."" Some of the resin composite manufacturers recommend the use of airborne particle abrading followed by acid-etching and silane coupler
application to improve bond strength. However,
Aida et al'' compared a resin bond agent with a
silane coupling agent and found that siiane coupling agents were not effective in improving the
bond strength. They also reported that the bond
agent 4-META produced good adhesion between
the resin composites. Ibsen and Neville" recommended placing resin composite in several layers
to minimize the effect of shrinkage.
Although studies"*-' have shown that the acid
etch technique for bonding resin composite to
enamel is effective, other investigators'' have found
that the acid etch of a composite surface being
bonded to another resin composite does not
increase retention significantly.
The effect of solvents on a composite surface has
been studied by Pestaner and Bowen,'' who concluded that a solvent such as chloroform or acetone produces surface softening of the resin composite, allowing the resin monomer to penetrate
the surface. The result would be both chemical
and mechanical bonding, since the resin
molecules would gain contact with unsaturated
bonds in the original composite material.
The purpose of this study was to measure the
shear bond strength between a preformed, heatactivated resin composite and a light-activated
resin composite to identify optimal surface treatments to promote bonding.
A second objective was to compare the maximum bond strengths measured with reported values for resin composite bonded to human enamel.
If the maximum bond strengths found exceed the
values reported for the resin-enamel bond (10 MPa
to 21 MPa), it could be concluded that the bond to
the resin composite pontic materials was adequate
for the clinical application.

i of Prosthodontics

heat, pressure poiymerized, urethane dimetfiacrylate resin with 60% filler

comprised ot a blend ot
microfine and smail
partie i es and short
cerarnic fibers
u ret han e based, iightactivated composite resin
universal bonding agent
BIS-GMA based, iightactivated composite resiri
universai bonding agent

Specimen Design
Preformed, resin p o n t i c blanks of Dene
Bridge material (Table 1), as shown in Fig 1,
were sectioned using a water-cooled diamond
blade in a buccolingual plane, and mounted in
a c r y l i c resin t u b i n g w i t h the cut surface
exposed. Either a c h e m i c a l l y p o l y m e r i z e d
acrylic resin (Sampl-Kwick, Buehler, Lake Bluff,
IL) or an epoxy resin (Epoxide, Buehler) was
used to mount the the resin blanks in the tubing
Fig 2). The embedded specimens were left for
24 hours to ensure complete hardening of the
embedding material.
The end of the cylinder with the specimen
exposed was then finished flat by wet grinding
with no. 180 silicone-carbide (SiC) paper.
All specimens were examined using a stereomicroscope to ensure that the heat-polymerized resin
surface was exposed for an area in excess of that
required for bonding. The specimens were then
cleaned ultrasonically in detergent (Ultramet
Sonic, Buehler) two times for 5 minutes, followed
by a 20-minute ultrasonic cleaning in distilled
water.
The mounted specimens were assigned to different surface treatment groups with 20 specimens
per group. The experiment was conducted in two
phases. In the first phase, the resin composite and
bonding agent used were urethane-based resins
(Table 1) similar to the chemistry of the pontic
resin. In the second phase, a Bis-GMA-based resin
and bonding agent were used.
Surface Treatment
Phase 1. Croup 1: No Treatment (Control). The
light-activated resin composite was applied to the

180

Gu2man/Moorc

Bojid Strenstli of Trearetl He.it- and Li^ht-Actvaled Re

Fig 1 The Dene Bridge (heat-activated resin).

Fig 2 Heat-activated resin mounted in the plexigias acrylic cylinder betre light-aclivated resin
compositeapplication.

flat ground surface of the specimens without further surface treatment.

were then washed thoroughly with distilled water

and dried using oil-free air for 30 seconds. A silane
coupling agent (Silane Coupling Agent, CaulkDentsply, Milford, DE) was applied following manufacturer's instructions. The bonding agent and
light-activated resin were applied in the same manner as in group 4.
Croup 7: Bonding Agent Appiication Only. In
this group the bonding agent was applied to the
specimen sitrface without surface preparation prior
to application ofthe light-activated resin composite.
Phase 2. To generalize the study, a second phase
was conducted using a Bis-GMA light-activated
resin and bonding agent. Three groups, each having 20 specimens, were prepared and given one of
three surface treatments:
Croup 8: Control With No Treatment.
Croup 9: Acid Etching and Bonding Agent
Croup 10: Bonding Agent Only.
These treatments were selected based on the
results of Phase 1 with the following considerations. Use of silane pretreatment requires an extra
step with a moderately expensive material having a
short shelf life. It did not significantiy improve the
bond strength in Phase 1 and was omitted. HF is a
potentially hazardous material that is not routinely
used in dentistry. Universal bonding agents, on the
other hand, are standard materials used with direct
filling composite restorations and recommended
for use when bonding to enamel. Air abrasion did
not result in improved bonding compared to bonding agent only and was omitted since it requires
special equipment. All other treatments from Phase
1 gave significantly lower bond strengths.

Croup 2: Monomer Application (MMA). The

specimens in this group were embedded in epoxy
resin instead of acrylic resin to avoid solvent attack
on the acrylic resin. The flat ground surface of
these specimens was treated with methyl
methacrylate monomer (Formatray i.iquid, Kerr,
Romulus. Ml) for 3 minutes.

Croup 3: Acetone Solvent Application. The

specimens in this group were also embedded in
epoxy resin. The specimen surface was treated
with acetone for 3 minutes followed by drying
using oil-free air for 20 seconds.
Croup 4: Surface Abrasion and Bonding Agenl
Application. The surface of these specimens was
airborne particle abraded using unrecycled 50 |jm
aluminum oxide powder for 10 seconds at 50 psi
from a distance of 2 inches- Treated specimen surfaces were washed twice with distilled water followed by ultrasonic cleaning for 15 minutes and
dried using oil-free air. Probond bonding agent was
applied according to manufacturer's instructions.
Croup 5: Acid Etching and Bonding Agent Application. The surface of specimens in this group was
acid etched using hydrofluoric acid gel (Porcelain
Etch Ultradent Products, South |ordan, UT, Lot
no. 10100) with 9.5% concentration for 1 minute.
The application ofthe bonding agent and light-activated resin was the same as in group 4,
Croup 6: Acid-Etching + Silane Coupling Agent
+ Bond Agent Application. The surface of these
specimens was acid etched using hydrofluoric acid
gel in the same manner as Croup 5. Specimens

nber 2, 1995

181

Tiie International joLrnai of Prosthodontk

Bord Strength of Treated Heal- and Liglil-Actvaled Re^ii

Application of Light-Activated Resin

40 seconds for the second. After placement of

the resin, specimens were stored in distilled
water for 2 weeks at room temperature before
testing.

To form the shear test Specimen, the specimen in

its plexiglas tube was placed into an aligning
device and positioned against a split Teflon mold.
Then, the plexiglas cylinder and the split Teflon
mold were tightened in position with the aligning
device screws. To obtain a good seal between the
heat-polymerized resin surface and the split Teflon
mold, a silicone impression material gasket was
used (Fig 3),
The light-activated resin was applied in 1-mm
layers using a plastic condenser. The polymerization time was iO seconds for the first layer and

Bond Strength
The shear bond strength between the two
resins was measured using a knife-edge shear test
in a universal testing machine (Instron Model
1123, Instron, Canton, MA) at a crosshead speed
of 1,0 mm per minute (Fig 4), The knife edge of
the testing apparatus was oriented at fhe interface of the heat-activated/Iight-activated resins.
The bond strength was calculated in MPa based
on maximum force applied and specimen bond
area (19.6 mm^).
Fracture Mode

Light-activated.
resin oomposite

After testing, the specimens were examined

under oblique illumination in a light microscope at
X40 to determine the fracture site. The type of failure, adhesive or cohesive, was reported. Adhesive
failure was recorded as fracture at the heat-activated resin/light-activated resin interface. Cohesive
failure was recorded as fracture in either the lightactivated or heat-activated resin alone.

Split Teflon moid -

Heat-aotivated
resin composite
Alignment sleeveFMMA cylinder-

Statistical Analysis
The mean and the standard deviation of the bond
strengths for each group were calculated. Bond
Strength data for all surface treatments were tested for
homogeneity of variance using Bartlett's test.
Because of the heterogeneity of variances, the Welch
test at a significance ievel of ,05 was used, and the
Newman-Keuls multiple comparison test was used to
test for differences between specific groups.

Embedding resin

Fig 3

Specimen preparation.

Results
Bond Strength
Phase 1. Urethane-Based Light-Activated Resin
Composite. The mean bond strengths and standard
deviations for the seven groups in Phase 1 are
given in Table 2 and Fig 5, Failure mode data are
also given in Table 2. The Welch test showed a
significant effect (F = 73.0; df= 6, 58; P < ,05) for
surface treatments on bond strength. The NewmanKeuls multiple comparison test showed that the
seven treatments formed three groups witb significant differences. The strongest bonds were formed

Fig 4 Speoimen testing in the Instron

machine (knife-edge shear test).

The Inlernational lournal of Pro5thodontic

182

Hund Strength of Treated Heat- and Ligh(-Activated Resins

Table 2 Shear Bond Strength Versus Surface Treatment Using Urethane-Based

Resin Composite
Group

Standard
Number o[
PJumer of
deTOtton aahesn'e failures cohesive failures

Mean(MPa)'

1, Control
2, MMA monomer
3, Acetone
4, Airborne particle
abraded+bonding agent
5, HF + bonding agent
6, HF + silane+bonding agent
7, Bonding agent only

8,81'
7,798,47"

3.18
1.49
2-17

19
20
20

0
0
0

12,76
17,50'
17,44=
14.45

2.64
1,96
3 22
2.53

17
15
11

3
5
9
2

ia

'Means (ollowed by the same letter were nol significantly diffrent P< 05)

Fig 5 Bond strength mean

vaiues ot aii the groups,
UrethaneGroup 1: Control;
Group 3: MMA; Group 3:
Acetone: Group 4: Airborne
particle abrading + bonding
agent; Group 5; HF + bonding
agent; Group 6: HF + silane +
bonding agent Group 7;
Bonding agent oniy.
BIS-GMAGroup 8: Controi;
Group 9: HF + bonding agent
group; Group 10: Bonding
agent only.

I Urethane resin composite

^^M

Bis-GMA resin composite

1
I. X
1

5
6
7
Surface treatments

the ground pontic composite and the light-activated

resin composite is somewhat unreliable.
The airborne particle abraded surface showed a
higher bond strength than the control but was not
significantly different from the group surface
treated only with bonding agent. There would
appear to be no advantage to using this particular
airborne particle abrasion technique as compared
to the simpler treatment with bonding agent.
The data from the treatment with and without
silane are somewhat mixed. The mean bond
strengths are not different, although the use of
silane did result in more cohesive failures.
However, the standard deviation for the silane
group is 50% higher than for the group without
silane, indicating that the silane process introduces
more variation in the results.

using HF + bonding agent and HF -F silane + bonding agent. The intermediate group was bonding
agent only and airborne particle abraded -i- bonding agent. The weakest bond strength groups were
the control, the monomer-, and the acetone-treated
groups.
Treatment of the surface with solvents, monomer,
or acetone, did not result in an increase in bond
strength compared to the control. When the
monomer-treated surface was examined microscopically, it did not appear to be significantly attacked
by the monomer. The surface treated with acetone,
however, showed signs of surface attack. The control group had a higher standard deviation than
either of the solvent-treated groups, and one control
specimen actually failed during handling prior to
testing. This would suggest that the bond between

Number 2, 1995

183

The Intematiorial ournal of Prosthodontics

Bond Strenuth of '1 re.ited Hedt- ind Liglit-Activaied Resins

Table 3 Shear Bond Strength Versus Surface Treatment Using Bis-GMA Based
Resin Composite
Group
8. Control
9. HF + bonding agent
10. Bonding agent only

Mean(tvlPa)'

Standard
deviation

8.64
21.68''
22.82-'

2.29
3.74
4.98

Number ot
adhesive tailures

Number ot
cohesive iailLires

"tulean followe by the same ietter were rot significantly ditlerent (Pe 05).

Fig 6 (Left Cohesive laiiure of the

iight-activated resin composite.
Fig 7 (Right) Cohesive failure of the
heat-activated resin.

Discussion

Phase 2. Bis-GMA-Based Light-Activated Resin

Composite. The bond strength and failure mode
data for the Bis-GMA resin composite are shown in
Table 3 and Fig 5. The Welch test indicated a significant effect of surface treatment (F = 120.5; df =
2, 34; P < .05). The Newman-Keuls tesl showed
that there was no significant difference between the
two groups with highest bond strengths, the HF +
bonding agent and bonding agent only. The
untreated control group was significantly weaker.
There was also no difference in bond strength
between the control groups in Phase "I and Phase 2.
The failure mode for the HF + bonding agent and
bonding agent only groups was very different from
those seen for the urethane resin composite. The
Bis-GMA specimens in these groups showed mostly
cohesive failures (Figs 6 and 7). There was no difference, however, in failure modes for the fwo control
groups that exhibited only adhesive failure.
There appeared to be a direct relationship
between the bond strength and the incidence of
cohesive failure. A linear correlation test gave a
value of the Pearson Correlation Coefficient, P =
0,935, indicating a high correlation between the 2
measurements.

Tlie Intemarioral lournal of Prosthodontii

Surface treatment using a bonding agent proved

to be an excellent bond promoter when the heatactivated resin was bonded to the Bis-GMA-based,
light-activated resin. This finding agrees with other
investigators' results." ''' The bond strength reached
with the application of bonding agent appears to
be adequate for clinical use because it is in the
same value range as the bond strengths reported
for resin composites to etched enamel.^-'
The use of acetone to improve bonding between
two resins did not appear to be effective. This does
not agree with other findings.'The effect of hydrofluoric acid etching before
bonding agent application was mixed. It improved
the bond between the heat-activated resin and the
light-activated resin when a urethane-based resin
composite was used, but it did not improve the
bond when a Bis-GMA-based, light-activated resin
was used. Furthermore, the use of FHF requires special precautions to avoid potential injury to the
patient or dental staff.
When the three similar groups (controls, HF +
bonding agent, and bonding agent only) from

184

Bond Strength of Treated Heal- and Light-Activated Re

Phase 1 and Phase 2 are compared, the following

are noted. There is no significant difference in the
bond strengths of the controls for the two different
light-activated resin composites. However, when
the bonding agent is used, with or without HF
treatment, the Bis-GMA material yields significantly higher bond strengths. This suggests thai the
difference seen results from use of Ihe bonding
agent. Since the control groups are not different,
the chemistry of the base resin would not appear to
explain the differences seen with the use of bonding agents. The Bis-GMA bonding agent contains
some filler that might improve its properties and
result in higher bond strengths. Additional research
in this area is indicated.
The application of a silane coupling agent did
not appear to improve the bond when the surface
was etched and bond agent used. This agrees with
Aida et al.'"
Airborne particle abrading the surface of the
heat-activated resin improved the bond strength
compared to the control, but the bond strength was
not significantly different from that obtained with
only bonding agent treatment.

ment + bonding agent.

5. When bonding agents were used, the Bis-GMA
system gave significantly higher bond strengths
to the pontic substrate compared to the tjrethane
based, light-activated resin and bonding agent.
6. For all of the groups included in this study there
was a significant correlation between the bond
strengths and the incidence of cohesive failures
observed.
7. The highest bond strengths found with either
resin composite were in the range of those
reported for resin composite bonded to tooth
structure, suggesting that an adequate bond
between the heat-activated pontic material and
the light-activated resin was attained.
Ackrtowledgments
The authors acknowledge Ihe support of Dirotian inc for
funding for ttiis study and providing the tieat polymerized resin
[Dene Bridge), The Kerr Co is aci<nowledged for supplying
Herculite XRV resin composite and Optibond bond agent.

References

Conclusion
In the first of a two-phase project, a preformed
urethane resin material was bonded to a urethanebased resin composite under seven conditions, in
the second phase, the preformed material was
bonded to a Bis-GMA-based resin composite
under three conditions. The shear bond strength of
the light-activated resin to the substrate material
was measured. Within the parameters of this study
and the particular materials used, the following
conclusions may be made:

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light-activated resin composite used, treatment
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compared to the control ground surface.
2. If the bonding agent recommended with the lightactivated resin composite was used, additional
treatment of the pontic surface with airborne particle abrasion did not improve bond strength.
3. Acid treatment with hydrofluoric acid did significantly increase bond strength, but additional
treatment of the acid etched surface with a
silane was not effective.
4. Bonding to the Bis-GMA-based, light-activated
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comparable to those achieved with HF treat-

Number 2, 1995

1.
2.

185

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Carpersen I. Residual acrylic adhesive after removal of

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The imernational lournal of Proslhodontics

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Literature Abitraci -

Study of Corrosion Between a Titanium Ituplant and Dental Alloys

While it is commonly agreed that titanium has proved its qualities as a material for
endosseous implantation, the choice of a suitable alloy for the superstructure remains controversial. Since the infiltration of saliva into the multimetallic structures on titanium rmptants
bnngs different types of alloys into temporary or permanent contact, a galvanic cell is established as a result ot their potential differences. The galvanic cell phenomenon is compounded
by another type of corrosion resulting trom fhe geometry ot the assembly: localized crevice
corrosion. This study examined the corrosion behavior of alloys vuhich may potentially be used
for superstructures in a galvanic coupling vjith titanium implants. Fitteen galvanic couples
(Ti-gold-based alloys, Ti-palladium-based alloys, and Ti-nonprecious alloys) were studied in
a test milieu of artificial saliva at a temperature of 37'C and pH 5. Various electrochemical
parameters {E^^,,. fcommon. E'couple corr. ^crevice, 'com 'couple corn ^'^'i Tafel slopes] were
analyzed. The galvanic currents measured, except Ti-stain!ess steel, were ot the same low
order ot magnitude. Examination of the surface state before and after the galvanic corrosion
tests showed that a number of alloys underwent a surface degradation, despite the low quantities of current generated by the couples. However, there was no change of surface state In the
gold- and palladium-based allows. On fhe basis ot the results obtained, the authors believe
that when choosing superstructure alloys, if is essential to fake inlo consideration fhe alloys'
behavior in localized corrosion phenomena. The authors concluded that there is no risk of
triggering the crevice corrosion pfienomenon with Ti-gold-based alloy or Ti-palladiumbased alloy couplings.
Reclaru L, Meyer JM. J Dent 1994:22(3): 159-16a. References: 23 Reprints: Protessor Jean-Marc
Meyer, Division ot Dental iuiaterials. School ot Dentistry, 19, Rue Barthelemy-Menn, 1211 Geneva 4,
Swtzerlan.Richard R Seals. Jr, DDS. MEd. MS. Department of Prosthodontics, University of Texas
i-taith Center at San Antonio, San Antonio. Texas

The trternalioral lournjl of Frostliodonlie

186