Durability of Resin-Dentin Bonds

Yasuo ShonoV Masamichi TerashitaV Jun ShimadaV Yoshio Kozono^ /

Ricardo M. CarvalhoV Carl M. Russell^/ David H. Pashiey
Purpose: The purpose of this study was to determine if the durabiiity of resin-dentin bonds couid be evaluated more quickly if the bond specimen was divided into 1 x 1 x S mm beams incubated at 37C for a 90day period.
Materials and Methods: Extracted human third molars were prepared for bonding by removing the occiusal surface near the dento-enamel junction (superficial dentin group) or near the pulp (deep dentin
group). The teeth were bonded either with MaoBond, One Step or Ciearfil Liner Bond 2, and then builtup to
form a flat resin composite crown. After 24 hours in water, eaoh buildup was verticaiiy divided into slabs 1
mm thick, the top half of whioh was resin, with the bottom haif as dentin. Each siab was then vertically
sectioned at 1-mm increments to create 1 X 1 X 8-mm beams of resin-bonded dentin. They were incubated
for 1 day or 90 days at 37"C, foliowed by measurement of the tensiie bond strengths. The results were analyzed by the Least-Squares Means method at the 95% confidence level.
Results: iVlacBond gave the highest p < 0,05] 1-day bond strengths to superficial dentin, but signifioantly
lower bond strengths were measured in deep dentin. There were no significant differences in the bond
strengths of either One Step or Ciearfii Liner Bond 2 to superficial vs deep dentin at 1 day, but at 90 days
their bond strengths to deep dentin had fallen significantiy (p < 0,05), Prepoiymerized cylinders of resin
composite bonded together with One Step showed littie variation in bond strength over the 90-day experiment. SEM examination of the failed bonds showed increased porosrty in intertubuiar dentin overtime.
Conclusion: The results indicate that division of large specimens into many smaii beams acceierated the
deterioration of bond strength in deep dentin in aii three bonding systems and in both superficial and
deep dentin in the iVlacBond treated specimens. This method seems promising for studying the durabiiity
of resin-dentin bonds.
J Adhesive Dent 1999:1:211-218.

Submitted for pijblic3tion:12.03.99: accepted for publication:25.05.99.

hear and tensile tests have been widely used to

measure resin-dentin strength in dentai research for many years. Bonding is usualiy done in
the center of flattened coronai dentin, using cylinders of resin composite 3 to 5 mm in diameter.S'i2
This approach worked very well with the eariy commercially availabie adhesive resins, whioh yielded

bond Strengths of 10 MPa or less, and exhibited a^dhesive failures. However, newer, improved products
have been deveioped which routineiy provide adhesive strength of 15 MPa or more, and almost aiways
produce cohesive faiiure in the dentin or the resin
during testing,!^ In the case of large surface areas,
non-uniform stress i ng^^.ig seems to initiate crack
formation in the resin-bonded substrate, resulting
in catastrophic failure. Cohesive faiiures of dentin
preclude evaluation of the true interfaciai bond
= Department of Operative Dentistry, Kyushu Dentai College, Kistrength when using large surface areas. In 1994,
takyushu, Japan.
Sano developed the so-cailed microtensile bond
" Department of Dental Materials Sciences, Kyushu Dentai College,
strength test,^2,i3 using bonded areas as small as
Kitaifyushu, Japan.
0,5 mm2. One of the advantages of this microten^ Oepa'lriient of Restorative Dentistry, University of Sao Pauio,
siie bond strength test is that when cross-sectionai
Bauru, SP, Brazil.
" Department of Oral Biology and Maniliofacial Pathoiogy, Schooi of bond areas were iess than 1 mm^, aimost all of the
Dentistry, Medicai Coiiege of Georgia, Augusta, Georgia, USA.
faiiures were adhesive in nature, even though the
Reprint requests: Dr. David H. Pasbtey, Department of Oral Biology &
bond strengths v^fere 25 MPa or more. There are
Msxitiofaciai Pathology, Schooi of Dentistry, Medica/ College of Georgia, Augusta, Georgia 30912-1129

211

Shono tal

many advantages to that technique, but a great

deal of tooth structure is sacrificed to create an
hour-glass configuration.i'' This limits the number
of specimens that can be prepared from a singie
tooth. We recently deveioped a new version of the
microtensiie test technique to evaluate regional
variations in resin-dentin bond strength.^^ In essence, a resin composite buildup of a tooth specimen is vertically, seriaiiy sectioned into slabs. Each
slab is sectioned into 1-mm-wide beams, each with
a cross-sectional area of 1 mm^. The resulting 20
to 25 individuai values can be compared individually as a function of position within the same
tooth,16 or an overall mean and standard deviation
can be calculated, as weii as the frequency distribution or spatial distribution of the bond strengths.
The durability of resin-dentin bonds is of vitai importance if resin composites are to be successfully
used as esthetic restorations over long time periods. During prolonged storage, it is assumed that
water siowly diffuses from the externai surface into
the bonded interface. In a 3 to 4-mm-diameter
cylindricai resin bond, water must diffuse 1.5 to 2
mm to reach the center of the specimen from the
periphery. Some investi gato rs^ reported that it may
take as iong as 3 to 5-years for the adhesive to
slowly hydrolyze. However, within that 3 to 5-year
period, the tested adhesive products are usually superceded by a new generation of products. Thus,
when long-term observations on the durabiiity of
products are pubiished, the products have usually
been replaced with an improved version. It would
be desirable to develop an accelerated aging model
that could chalienge the durability of resin-dentin
bonds in a relatively short period of time. One approach to this is to divide bonded specimens into 1
X 1 X 8-mm beams as described above,
Uniike conventionai bonding methods, the center
of the 1 x 1 mm2 resin-bonded dentin beams used
in the microtensiie test is only 0.5 mm from any externai surface. We speculated that such a specimen might provide a useful method of accelerating
whatever hydrolysis of resin-dentin bonds might
occur over time.i^ This has recently been confirmed by Dickens et al.'' They compared the bond
strengths of Scotchbond Multi-Purpose Plus and an
experimental bonding system tested 1 day (23C)
after bonding, compared to after storage at 60C
for 7 days. The specimens had cross-sectional
bonded areas of either 0.7 mm2 or 12 mm^. There
was a much iarger faii in bond strengths in the 0.7
mm2 vs the 12 mm^ groups over the 7-day storage

212

period indicating an acceierated aging effect. There

IS some concern, however, that O-C temperatures
may be too high for such studies.i
The purpose of this study was to test the hypothesis that small (ca, 1 x 1 x 8 mm) beams of resinbonded dentin specimens will exhibit iower bond
strengths after incubation for 90 days, compared
to 1 day, by measuring their microtensiie bond
strengths.

MATERiALS AND iVIETHODS

reeth; Human third molars were used within 1
month of extraction. They were stored in 4^0 water
until used. There were two preparation variables: In
the superficial dentin group (SD), the bonded occlusal superficial dentin was prepared just beneath
the dentin-enamel junction. In the deep dentin
group (DD), the dentin surface was prepared within
0.5 mm of the highest puip horn. These flat surfaces were created with an Isomet saw (Buehier
Ltd., Lake Bluff, IL, USA) with water as a iubricant.
Three bonding systems were compared: iVlacBond
(MB) (Tokuso Corporation, Tokyo, Japan); OneStep
(OS) (Bisco, inc., Schaumburg, IL, USA); and Clearfii
Liner Bond 2 (LB 2) (Kuraray Co., Ltd,, Osaka,
Japan) were used according to the manufacturer's
instructions (Table 1). Specimens bonded with One
Step were built up with ZIOO resin composite (3iVl
Dental Products, St, Paul, MN, USA). Those specimens bonded with iVIacBond were built up in Paifique Estelite resin composite (Tokuso Corp., Tokyo,
Japan), and the specimens bonded with Clearfii
Liner Bond Ii were buiit up in AP-X resin composite
(Kuraray Co., Ltd., Osaka, Japan). After 24 h of storage in water at 37C, the specimens were verticaiiy
seriaiiy sectioned at 1-mm thickness intervais,
using the Isomet iow speed diamond saw (Fig 1).
Then a second section was made perpendicular tc
the bonded interface to make 1 x 1-mm beams. The
procedure created a total of about 20 beams with a
cross-sectional area of 1 mm^ (ie, 1 x 1 mm). The
top half of each beam was resin composite and the
bottom half was dentin. Controls consisted of pairs
of prepoiymerized resin composite cylinders 6 mm
in diameter that were bonded together with One
Step adhesive resin. These were sectioned into
slabs and then into 1 x 1 x 8-mm stioks as described above. In each bonding group, three teeth
were used and each bonded tooth was prepared
into an array of about 20 individual beams 1 x 1 x 8

Journal tff Abgsive Dentistry

Shono et al

Table 1

Adhesive Systems

Adhesive Systems

Etchant

Adhesives

MacBond (MB)

Self-etching

Mac-10

a(20s)b,e,g, (lOsl

(Tokuso Corp,

maleic acid,

HEMA

f(lOs)

Tokyo, Japan)

Mac 1 0

Procedures^

bis-GMA

alcohol
One Step (OS)

3 2 % phosphoric

BPDM, bis-GMA

a(15 s)b,c,d,g

(Biscc, Schaumburg,

acid (Uni-Etch)

HEMA, acetone,

f(10s

IL, USA

photoinitiator

Clearfii Liner

Self-etching

MDP

Bond 2 (LB 2)

Phenyi-P

HEMA

(Kuraray, Osaka,

HEMA, water

bis-CMA

a(30 s),g,e
f(20 s)

Japan)
Abbreviations: MAC-10= ii-methaceyloiy.H-undecanB-dicarbaiiylic acid; MDP = lO-methacryloxydecamethylere phosphoric acid: HEMA = hydronyetliyl-methacrylale, Pheryl.p ^ 2.methacryloxyaihyl phenyl phosphoric aciO; bis-GMA = 2,2.Bis [4.2-hydroxy.3.methacryloyoxypropDxyphenyl
propane.
sProcedjresi (a) acid-etching; (b) rinse: (c) blol-dry: (d] apply 2 coats of adhesive; |e) applied one
layer of adhesive; (f) light-cjre; g) blow dry.

NEW VERSION OF MICROTENSILE BOND TEST METHOD

Fig 1 Schematic illustration of how resin

composite buildup was verticaily sectioned into slabs that were, in turn, divided into beams that were individually
tested.

mm. Of the 60 individual beams in each group, 10

were used for SEM studies and the remaining individual beams were mixed together in each group.
Incubation: The 60 beams from the three
bonded teeth or composite cylinders were incuVcl 1,

bated in separate vials containing steriie 0,85%

NaCi solution containing penicillin (10,000 units/
ml), streptomycin (10 pg/mi), and a few drops of
ION NaOiH and phenol red as a pH indicator to
achieve a pH of 7.0. Although ail glassware and
213

Shono et al

Specimens were clean, they were not sterile. Once

sealed, the vials were placed in an inoubator-shaker
for the specified time interval at 37C,
Measuring bond s t r e n g t : At the appropriate
time, a vial was opened and each individual beam
was removed and bonded to steel "grips" of a Bencor Multi-T device (Danville Engineering, Danville,
CA. USA) using Zapit-brand cyanoacryiate {Dental
Ventures of America, Ventura, CA, USA) (Fig 1) to
permit measurement of the tensile bond strength of
each specimen in an Instron machine operated at
1 mm/min with a 49-N load cell. Ten specimens
were used for SEM observations (5 at day 1 and 5
at 90 days). Selected specimens of the failed bonds
were also examined by SEM to look for microcrack
or other defects aiong the edges of the beams and
to examine the quaiity ofthe dentin interface.
Ca/C(j/ations: Load at failure was divided by the
cross-sectionai area to yield the stress at failure in
MPa. The data were entered into an Excel spreadsheet to permit calculation of descriptive statistics
(mean SD), The mode of failure was evaluated
using a stereomicroscope at 18X magnification.
Statistics: The data were collected in a three-way
analysis of variance (ANOVA) design, with bonding
materiai, dentin depth, and time of incubation the
three factors. In addition, the interaction of the factors was tested. The response variable was tensiie
bond strength. Group comparisons were done by
the Least-Squares Means method. Least-squares
means are the expected vaiue of a group or subgroup means that one expects for a balanced design involving the group variable with all covariates
at their mean vaiue. Statistical significance was set
in advance at the 0.05 level. Aii anaiyses were conducted with SAS software for the personal computer (SAS Institute, Cary, NC).
Scanning electron microscopy: Scanning electron microscopy was done on the dentin sides of selected failed bonds to obtain information about the
types of faiiures and the appearance of the bonded
interface after prolonged storage. The specimens
were rinsed with distilled water, allowed to air dry
overnight, gold coated, and examined in a JEOL
SEM.
image analysis: The SEM prints of the failed
bonds were scanned to convert them from analog
to digital form. They were then subjected to image
analysis using NIH Image PC (Scion, Eredrick, MD,
USA). Four areas were selected in each micrograph
that avoided resin tags in dentinai tubules or areas
of pure adhesive resin. Each of these regions of in214

tertubular dentin had the same surface area

(24 nm^). The porosity of the intertubular dentir
was integrated to yield a total surface area vaiue.
The same gray scale window was used to evaluate
all SEM prints. Then means and standard deviations were calculated for the intertubuiar porosity
observed at each time period (1 day vs 90 days).
One-way ANOVA was performed to determine if
there were any statistically significant differences
among the surface porosities as a function of time.
Statistical significance was considered as a a 0,05,

RESULTS
Table 2 shows the mean microtensile bond
strengths (MPa) of the three bonding systems to superficial (SD) and deep dentin (DD) at 1 day vs 90
days. The highest 24 h tensile bond strengths were
obtained with MacBond on superficial dentin. After
9 0 days of i n c u b a t i o n , the resin-dentin bond
strength of MacBond in superficiai dentin had
fallen to iess than half the initial value (p < 0.001),
Bonds made to deep dentin were only haif as large
(28 MPa) as those obtained on superficial dentin at
1 day (p < 0.001) and they fell to iow values (8.3
MPa] after 90 days. One Step gave iower 24 h bond
strengths to superficial dentin (ca 20 MPa), but
they did not change over 90 days (Table 2), OneStep bonds to deep dentin were similar to those of
MacBond in that the 24 h bond strengths were 26
Mpa, which feli to low values (5.9) after 90 days.
Liner Bond 2 gave moderate 24 h bond strengths to
superficial dentin (ca 26 MPa) that did not change
over 90 days, while bonds made to deep dentin fell
from 23 MPa at 1 day to 6 MPa at 90 days (Table
2).
In contrast to the variable resuits obtained with
resin-dentin bonds, the oontrol group of prepolymer\ze cylinders of resin composite bonded to composite specimens gave similar bond strengths at 1
day vs, 90 days, with little variation (note the small
standard deviations).
Most bond failures of all of the bonding materials were adhesive in nature (Table 3), Only a few
beams failed in dentin or in resin. There was no correlation between failure mode and bond strength.
Figure 2a shows the fractographs of the One Step
system bonded to superficial dentin after 90 days.
Figure 2b shows the dentin side of a failed bond to
deep dentin after 1 day, and Fig 3 shows deep
dentin after 90 days. After 90 days of immersion in

_Thfi lniirnal-QlAdt)gsive Dentistry

Shono et al

Table 2 Tensile bond strengths (MPa) of superficial dentin and deep

dentin at 1 vs 90 days.
Materiai/Location

lday

MacBond/Superficial dentin
MacBond/Deep dentin
OneStep/Superficiai dentin
One Step/Deep dentin
Liner Bond 2/Superficiai dentin
Liner Bond 2/Deep dentin
Composite/One Step/Composite

M0.613.1 (51)
'i27.711.6 (53]
i'19.920.1 (52)
026.3114,6(501
i'25.418,9 (51)
"22.5*17,2 (53)
36.11.9 (52)

90 days

NS
.
NS
*
NS

19.811.2(53)'^
8.36-0{52)='
20.2tl3.1(51)=
5.96.4{53)='
23.1tl2.4(53)<^
6.37.5(52}='
37.14.4(52)

'P-: 0.001; groups identified by diffre t supe'scripls are significan Ilydiffe ent(p<0.05) NS = not5\atisticallysignficantiy different. Numbers n psrenthese; indicate the numbe of specimens tested in eacb
group.

Table 3 Failure modes for the materials at the two dentin depths at 1
vs 90 days.
ncubation time
90 days

lday

MacBond/SD
MscBond/DD
One Step/SD
One Step/DD
Ciearfii Liner Bond ll/SD
Clearfil Liner Bond li/DD
Resin to resin

38/51
47/53
44/52
42/50
41/51
45/53
52/52

8/51
2/53
4/52
3/50
1/51
3/53
0/52

5/51
1/53
3/52
5/50
7/51
4/53
0/52

0/51
1/53
1/52
0/50
2/51
1/53
0/52

53/53
52/52
51/51
53/53
53/53
52/52
52/52

0/53
0/52
0/51
0/53
0/51
0/51
0/51

0/53
0/52
0/51
0/53
0/53
0/52
0/52

0/53
0/52
0/51
0/53
0/53
0/52
0/52

ure, M = med codesive failL res in Ooth resin a d dentin; R = resi cohesive failure; D ' cohesive failure ir dentina SD = sijpeificial dentin; DD = deep a =ntin. Val es are the numBer of sepcirrens eihibiting that type of failure/tota n u . . e of spec "nens m each subgroup.

water, a significant increase (p < 0.001) in interfacial porosity was noted in dentin bonded with One
Step compared to superficial dentin and to 1-day
deep dentin specimens. Simiiar changes were
noted with tiie other adhesive systems.

DISCUSSION
in bonding systems that demineraiize the dentin
surface, the minerai is removed from around the
coiiagen fibriis of the dentin,i>ii foiiowed by appiication of adhesive resin monomers to infiitrate to
Voll.

the depth ofthe demineraiization. However, several

reports suggest that this infiltration is incompiete.^'
This may cause the slow hydroiysis of the non-infiltrated coiiagen or associated noncoiiagenous proteins, thereby weakening the resin-collagen network
over time. The conversion of monomers to well
cross-linked, long-chain polymers in moist dentin
may be incomplete,^ thereby aliowing extraction of
unreacted monomers and oiigomers from between
coiiagen fibriis over time.
Most investigators simpiy store bonded specimens in water at 250 or 37=^0 for varying iengths
of time. One day is the usuai storage time for most
215

Shoho et al

Fig 2a Secondary electron image of the dentin side of a

specimen of superficial dentin that was bonded with One
Step and then tested for bond strength 90 days later, it appears that the resin tags puiied outof the tubules but that the
intertubuiar dentin remained infiitrated with resin.

Fig 2b Secondary eiectron image of the dentin side of a

specimen of deep dentin that was bonded with One Step and
then tested to faiiure after 1 day. Most ofthe resin tags broke
cohesively at the top of the hybrid layer, although a few came
loose or puiied out. The intertubuiar dentin remained sealed
with resin.

Fig 3 Secondary electron image of the dentin side of a specimen of deep dentin that was bonded with One Step, then incubated for 90 days prior to bond testing, iVlost of the resin
tags broke cohesively but they appeared to be surrounded by
voids. The intertubuiar regions were very porous and consisted of a ioose reticuiar network.

studies, although some investigators have gone as

iong as 5 years.^
Burrows et ai^ bonded bovine dentin with 12 different bonding systems and then measured tensile
bond strength after 1 day, 1, 3, 6 months and 1
year, Ciearfil Liner Bond 2 and Superbond D Liner
were unaffected by storage for 1 year, but most of
the other bond strengths fell with time, Gwinnett
and YuS found a significant ioss of initial resindentin bond strength foiiowing immersion in water
for 6 months. Burrow et ai^ reported the effects of
216

3 years of water storage on the bond strength of

bonds made with or without primer (3% N-methacryloyl-5-aminosaiicyiic acid) using Clearfii Photobond
as the bonding agent. Bovine dentin bonded with
the primer gave stabie bonds (ca 10 MPa) for 1
year but they feli to 5,5 MPa by 3 years.
In the current study, the bond strengths of
MacBond to superficial dentin were significantly
higher (p < 0.001) than those made to deep dentin
when tested at 1 day, but there were no significant
differences between superficial or deep dentin
ve Dentistry

Shono tal
bond strengths with the other 2 bonding systems at
1 day (Table 2). Apparently, One Step and Liner
Bond 2 could form bonds equally well to either substrate. However, the bonds made to deep dentin by
all of the test materiais deteriorated over the next
90 days, resulting in significantly (p < 0.001) iower
bond strengths in all cases. Scanning eiectron microscopy of the failed bonds reveaied extensive
porosity in the intertubular regions of deep dentin
that was not as evident in superficial dentin at 90
days. The loss of intertubuiar mass appears to be
due to both a ioss of resin and coiiagen fibrils. We
speculate that the higher water content of deep
dentin is a result of the higher tubule density and
diameter,^ causing more rapid hydrolysis of these
two phases of the hybrid layer. The susceptibility of
the resin to hydrolysis^ is probabiy due to its low degree of polymerization.^ The 'nearest neighbor"
tubuie in deep dentin is only about 3 pm away (Fig
2b), whiie in superficial dentin it is over 10 pm distant (Fig 2a). It is clear that more information is
needed about the degree of conversion of monomers to polymers, their amount of cross iinking,
their concentration, and how well they envelop collagen fibrils before improvements can be made in
the durabiiity of bonding to deep dentin. Resin
bends made to superficial dentin may or may not
deteriorate over time (Table 2) depending on the
materiai.
Although the storage solution consisted of unbuffered isotonic sodium chloride containing penicillin and streptomycin, the presence of these antibiotics provided significant buffer capacity. When
the solution was adjusted to pH 7.0, it maintained
that pH for the duration of the 90-day experiment
{data not shown). Thus, the fall in bond strength n
deep dentin specimens cannot be expiained by low
pH. An alternative explanation is that calcium may
have siowiy dissolved from the dentin into the caicium-free storage soiution. Since changes in medium calcium were not measured, the potentiai of
calcium-free media to cause deterioration of resindentin bonds remains specuiative. The ioss of mass
from the bonded interface shown in Fig. 3 cannot
be due to a loss of calcium since that region had
been acid-etched prior to bonding.
The use of smail (ca, 1 mm^) cross-sectional
areas apparently accelerates the degradation of
dentin bonds," When incubated at 37''C for 90
days, the method easily detected s i g n i f i c a n t
decreases in resin bond strength to deep dentin
(Table 2). One of the three adhesive systems
Vol 1,

(iViacBond) tested on superficial dentin also detected a significant decrease in resin-dentin bond
strength over the 90-day test period. Whether the
other two adhesives (One Step and Liner Bond 2)
bonded to superficial dentin would have exhibited
lower bond strengths had we incubated them
longer, remains to be determined in future experiments.
The fact that specimens of the same size made
from resin composite cylinders bonded to each
other with One Step showed stabie bond strength
over the 90 day experiment (Table 2) implicates
dentin as being the weakest link in resin bonds to
teeth. However, the One Step bonds to prepoiymerized cylinders of resin composite were made in the
absence of water. That is, wet bonding had not
been done. In the future, we will inciude another
group of bonded composite cyiinders that are
bonded dry vs wet.
From this study, we can conclude that the new
version of the microtensiie test method may serve
as a good model to test the durabiiity of resindentin bonds.

ACKNOWLEDGMENTS
The authors wish io thank Shirley Johnslon for secretarial support.
Tiiis work was supported, in part, bji grants DE06427 from the
NIDCRandby granl-in-aid C1O67I7% from the Ministry of Education of FAPESP 95/3S95-9. Japan.

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3. Calais JG, Sderholm K-J. Influence of filler type and water
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217

Shono et ai

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Contents
Tbe InternetHistory and Evolution Accessing the
Internet Basic Services of the Internet Overview of
Dental Internet Resources tJniversity-Based Research
Projects on the Internet Online Services for Medicine
and Dentistry Quality Assurance in Digital Publishing
Intranets Tips and Tricks Outlook
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