MILITARY MEDICINE, 165, 10:742,2000
Effect of Universal Testing Machine Crosshead Speed on the Shear
Bond Strength and Bonding Failure Mode of Composite Resin to
Enamel and Dentin
Guarantor: Lt Col James S. Lindemuth, USAF DC
Contributors: Lt Col James S. Lindemuth, USAF DC*; Col Mark S. Hagge, USAF DC (Ret.It
An investigation was conducted to determine if testing ma-
chine crosshead speed influenced shear bond strength (SBS)
or the failure mode of composite bonded to enamel and dentin.
Composite cylinders were bonded to 50 enamel and 50 dentin
surfaces and thermocycled. Groups of 10 samples were
debonded at speeds of 0.1, 0.5,1.0,5.0, and 10.0 mmlmin. Data
were examined with analysis of variance and post-hoc testing.
Failure modes were determined using lOX magnification. With
enamel, no significant differences in SBS existed, and cohe-
sive vs. adhesive failure modes were similar for all groups.
With dentin, the 0.5, 1.0, and 5.0 mmlmin samples had signif-
icantly higher SBS than the 0.1 and 10.0 mmlmin samples (p <
0.05). No other differences in SBS were found. Samples tested
at 0.5 mmlmin demonstrated strikingly better cohesive vs.
adhesive results than all other groups. SBS and cohesive vs.
adhesive failures achieved with dentin bonding were signifi-
cantly affected by crosshead speed.
Introduction
L
ongitudinal clinical trials are the final arbiter of any dental
restorative material'sefficacy; however, they are costly, time
consuming, and difficult to standardize. In addition, the rapid
introductionof new adhesive bondingsystems has forced den-
tists to rely increasingly on laboratory tests for evaluation of
these products.r" Unfortunately, predicting the clinical perfor-
mance of dental restorative materials by extrapolating in vitro
results has inherent limitations. Laboratory designsare unable
to accurately replicate intraoral conditions, in which cyclic
stresses are applied to restorative materialsin a wet and chem-
ical environment, and as a result, in vitroresearch results have
not correlated consistently withsubsequent clinical ftndtngs.""
Despite the recognized shortcomings of in vitro methodology,
laboratory testing of enamel and dentin bonding systems is
nevertheless regarded as necessary in the evaluation of new
products and continues at a rapid pace.
One of the most widely used laboratory tests, shear bond
strength (SBS), measures the ability ofadhesive resins to bond
to tooth structure or to a second restorative material. This rel-
atively simple procedure typically uses a chisel-shaped tool
mounted in a universaltesting machine to forcefully fracture a
disc of bonded material from the bonding substrate (Fig. 1).
Higher SBSis equated with enhanced performance, and cohe-
*60th Dental Squadron/SGDE, 101 Bodin Circle, Building 777, Travis Air Force
Base, CA 94535.
tDepartment ofOperative Dentistry, University ofthe Pacific School ofDentistry,
2155 Webster Street, SanFrancisco, CA 94115.
Presented previously in abstract form at the International Association for Dental
Research 78thGeneral Session, Washington, DC, April 5-8, 2000.
This manuscript wasreceived for review in November 1999 andwasaccepted for
publication in December 1999.
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sivefailures within tooth structure or composite resin are con-
sidered superior to failures within the adhesive layer. A mixed
failure mode, with regions of cohesive and adhesive failures,
may also occur. When SBSvalues ofadhesive bondingsystems
exceed the reported SBSoftooth structure, the adhesive resin is
assumed to no longer be the limiting factorin bonding success."
The specific physical mechanics of the SBS test,2,13-19 its
clinical relevance,20-22 and the myriad testing variables
involved1. 23-27 have all been criticized in depth. Van Noort18,19
has extensively analyzed the stress patterns produced in the
SBS test and found them to be complex and nonuniform in
nature, highly concentrating stress at the edge of the bonding
interface. Variables in testing include the modulus of elasticity
and the diameterofthe bondedrestorative composite resin, the
thickness of the adhesive resin, the presence of bondingresin
flash, the location (superficial vs. deep) ofthe dentin substrate,
the contact area and shape of the chisel, and the crosshead
speed of the testing machine. Numerous appeals have been
made to standardize bond strength testing, and in 1991 the
InternationalOrganization for Standardization (ISO) published
guidehnes for testing adhesion to tooth structure, describing
both tensile and shear tests." Despite this attempt, the ISO's
proposed standard has been little used and heavily criti-
cized. 15,27,29 In fact, one investigation reporteda 500/0 coefficient
of variation in one series of test specimens using the ISO's
testing methododology." Alternative methods of testing bond
strength have also been developed, including the microtensile
test,30 quantitative margin analysis." the extrusion test," and
the fracture toughness test.32-34 Regrettably, each ofthese tests
is significantly more time consuming and technically demand-
ing than the SBS test, and none has yet demonstrated an im-
proved association with clinical fmdings.
Despite all its prospective liabilities, SBStests continueto be
used routinely byleading researchers.":" and recently, another
study reportedan excellent correlation between in vivo fmdings
and in vitro results obtainedwith dentin bonding." Consider-
able latitude has persisted with regard to most test variables,
however. Of these, the widest disparity has almost certainly
been the universaltestingmachinecrossheadspeed selected to
fracture bonded samples. Studies presented during the 1996
and 1997 International Association forDentalResearch general
sessionsused crossheadspeedsrangingfrom 0.05 mm/mm" to
50 mm/mtn." a variation ofthree orders ofmagnitude.
Theviscoelastic nature ofdental adhesives suggeststhat SBS
and failure mode couldbe affected by the rate ofstress applica-
tion. Slower crossheadspeedscouldallow an extended recovery
period during which stress and strain are compensated for by
the elasticity of the bonding agents; at lower speeds, the resin
behaves like a viscous material, deforming more as increased
742
 Bond Strength and Bonding Failure ofComposite Resin to Enamel and Dentin 743

mond wheel using water irrigation under 2.5x magnification.

Teeth were stored in tap water at room temperature. then ran-
domly sorted into five groups of 10 teeth before bonding. In a
recent study. one dentin bonding system (Prime & Bond,
Dentsply/Caulk, Milford. Delaware) produced nearly equal
numbersofadhesive and cohesive failures whenapplied at room
temperature." Based on these results. this recently updated
system (Prime & Bond 2.1. lot 970808) was selected for the
study because of its projected sensitivity in revealing failure
mode differences.
Teeth were etched with 37% phosphoric acid (Dentsply/
Caulk. lot 971001) for 20 seconds. rinsed for 20 seconds. and
then thoroughly dried (enamel) or gently dried leaving the sur-
face moist(dentin). The bonding system was applied according
to the manufacturer's instructions at room temperature and
cured for 10 seconds using a visible light unit (Optilux 500.
Demetron/Kerr, Danbury. Connecticut). Composite cylinders
from 2 to 5 mm in diameter have been reported withequivalent
SBS.20so Teflon tubingwithan internal diameter of2 mmwas
selected as a matrixto place the composite [Prisma TPH (shade
AI), Dentsply/Caulk, lot9712311. Thecomposite cylinders were
cured using the same light curing unit at 730 mW/cm2 for 80
seconds. and the unit was monitored frequently with a curing
radiometer to ensure consistent output. Specimens were stored
in 100%humidity at 37°C for 1week. thermocycled 1,000 times
from 5 to 55°C using l-mlnute dwell intervals. then returned to
storage for 1week. Toeliminate the effect ofbonding resinflash.
the areas bordering the Teflon cylinders were scored withsharp
dental explorers and disposable scalpel blades. After mounting
in 1-inch-diameter polyvinyl chloride pipe with tray acrylic.
Fig. 1. Bonded composite cylinder mounted in a universal testing machine. samples were loaded perpendicularly under compression in a
universal testingmachine (model 5566. Instron, Canton. Mas-
pressure is applied. with a resultant increase in SBS. Con- sachusetts) using crosshead speeds of 0.1. 0.5. 1.0. 5.0. and
versely. the potential for higher SBS also exists with faster 10.0 mm/min until bonding failure occurred. SBS values in
crosshead speeds. At more rapid crosshead speeds, the resin megapascals were calculated from the peak load of failure di-
may perform as a brittle solid. with increased energy directed vided by the specimen surface area. Data were then examined
toward fracture ofthe specimen rather than molecular deforma- usingone-way analysis ofvariance (ANOVA) or Kruskal-Wallace
tion and flexure. 16,27 If either of these premises were valid. sig- ANOVA, with differences between individual treatment groups
nificant differences in SBS between tested materials could re- determined by post-hoc Student-Newman-Keuls comparisons.
sult just from varying the crosshead speed. Perhaps more In addition. fracture sites were examined under a stereomicro-
importantly. the mode of failure (cohesive vs. adhesive), re- scope at lO Xmagnification to determine the mode offailure.
garded as a more essential characteristic of bond strength.s "
maynot be immune to variations in crosshead speed. Results
Several otherstudieshave briefly examined the effect ofcross-
head speed on SBS. but these have been limited to abstract TheKolmogorov-Smirnov test for normality and a Levene me-
presentations with incomplete statistical information. have dian test indicated that the enamel SBS data were normally
used a narrower range of test speeds. or have not investigated
distributed with equal variances across the treatmentgroups.
the mode of failure.23.25.27Therefore. the purpose of this study
For this reason. differences in the crosshead speed at which
bonding failure occurred in the enamel samples were examined
wasto determine if variation in universal testingmachine cross-
usingone-wayANOVA. No significant differences in SBS existed
head speed resulted in significant differences in SBS or failure
mode ofcomposite resin bonded to enamel and dentin. between any ofthe enamel bonded groups IF (4.45) = 2.01. P >
0.10]. In contrast. the dentin data were not normally distrib-
Materials and Methods uted; therefore. differences in the dentin treatmentgroups were
analyzed using Kruskal-Wallace ANOVA, a nonparametric test.
Thestudy was divided into two parts. first usingenamel and and significant differences were found [H (4. N = 50) = 14.8. P <
then dentin as the bonding substrate. For each part of the 0.01]. Dentin bonded groups testedatO.5. 1.0. and 5.0mm/rnin
study. the mesiofacial surfaces of 50 extracted human molars speeds exhibited higher SBS values than samples fractured at
were coarsely ground and then smoothed with a 600-grit dia- 0.1 and 10.0 mm/min (p < 0.05) . No other significant differ-

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 744 Bond Strength and Bonding Failure of Composite Resin to Enamel and Dentin

20 - - - - - _._ --_._--- - - - - - - - - - - _._ - - --,

18

16

14

12
ns
c.. 10
:2
8

o ----
ID 0.1 mm/min ~ 0.5 mm/min m1 mm/min rlI5 mm/min E11 0 mm/min I
Fig. 2. Mean shear bond strength (SD)for enamel bonded samples with group ranking" (p < 0.05): 0.1 mm/min, 16.77 (2.28)' : 0.5 mm/min, 15.83 (2.00)'; 1.0 mm/min,
16.48 (2.45)'; 5.0 mm/min, 15.39 (3.05)'; 10.0 mm/min, 13.80 (3.09)' . *Values marked by the same letter were not significantly different.

ences were found between dentin bonded groups. SBS values
are shown forenamel bonded samples in Figure 2 and for dentin
in Figure 3.
Themode offailure for all enamel bonded groups was almost
exclusively cohesive within enamel, and no mixed failures were
observed. In contrast, only the dentin bonded group tested at
0.5 mm/min had predominantly cohesive failures, located
mostly within the composite rather than within dentin. Ateach
of the other four test speeds, 7 to 10 adhesive failures were
observed. In this investigation, mixed failures in the dentin
bonded samples were found to be primarily cohesive in nature
and were classified as cohesive failures. Failure modes for
enamel and dentin are shown in Tables I and II.
Discussion
Enamel bonded samples proved largely immune to the varia-
tionin crosshead speedsused in this studywithrespectto both
SBS and mode offailure. Although no significant differences in
SBS were found between the enamel bonded groups, a tendency
was noted toward decreased strength at the most rapid speed,
accompanied by a corresponding increase in adhesive failures.
Dentin displayed wider ranges of test values at all crosshead
speeds than enamel, which was expected, given the well-docu-
mented Variability of clinical dentin substrates." Within the
dentin groups themselves, SBS decreased significantly at both
test extremes compared withthe three middle test rates, essen-
tially disproving both experimental premises.
Comparable studies have also described equivocal results.
Two recent reports on dentin SBS vs. crosshead speed using
bovine teethwere published in abstract format only withincom-
pletedata and statistical information, so they must be consid-
ered from that perspective. One ofthese studies used speedsof
0.25, 0.5, and 5.0 mm/rntn and found that 0.25 rum/min re-
sulted in higher SBS than 0.5 mm/mtn but was not different
from 5.0 mm/min." The second study used the same range of
crosshead speedsas our investigation but reported results only
from the two extremes." These authors reported higher SBS at
10.0 mm/rnln than at 0.1 mm/min for both bonding systems
tested. Athird study, also usingbovine dentin, reported equiv-
alent SBS at 0.5 and 1.2mm/min, but it found that the higher
speedresultedin increasing cohesive failure in composite, with
a corresponding decreased pulloutofdentin. The authors con-

20
18
16
14
12
III
Q. 10
:E
8
6
4
2
0

D .1 mm/min ElI .5 mm/min III 1 mm/min 11iI 5 mm/min §1 0mm/min

Fig. 3. Median shear bond strength (SD)for dentin bonded samples with group ranking" (p < 0.05): 0.1 mm/mtn, 8.47'; 0.5 mm/min, 12.17'; 1.0 mm/min. 15.n'; 5.0
mm/min. 11.28'; 10.0 mm/min. 8.00'. *Values marked by the same letter were not significantly different.

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 Bond Strength and Bonding Failure of Composite Resin to Enamel and Dentin 745

TABLE I 2. Sudsangiam S, van Noort R: Do dentin bond tests serve a useful purpose? J
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ENAMEL FAILURE MODES
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0.1 mm/ 0.5mml 1.0 mm/ 5.0mml 10.0 mm/ 5. Duke ES: Clinical studies of adhesive systems. Oper Dent 1992; (suppI5): 103-
min min min min min 10.
6. Albers H: Tooth Colored Restoratives, pp 1-11-1-12. Santa Rosa, CA,Alto Books,
Cohesive 9 9 9 9 7
1996.
Adhesive 1 1 1 1 3
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DENTIN FAILURE MODES 8. Tyas MJ, Chandler JE: One-year clinical evaluation of three dentine bonding
agents. Aust Dent J 1993; 38: 294-8.
9. Platt JA, Winkler MM,Matis BA, Moore BK: Correlation of dentin adhesive labo-
Crosshead Speed
ratory and clinical performance at three years [abstract 1044]. J Dent Res 1998;
0.1 mm/ 0.5mml 1.0 mm/ 5.0 mm/ 10.0 mm/ 77: 236.
min min min min min 10. van DijkenJWV: Clinical performance of nine dentin adhesives in class 5 cervical
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Cohesive a 10 a 3 2
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Adhesive 10 a 10 7 8
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12. Burgess JO, Summitt JB, Robbins JW, Haveman C, Nummikoski PV, lazetti G:
Clinical evaluation of base, sandwich, and bonded class II composite restorations
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Our unusual and unexpected pattern offailure modes within bonded to ceramic. J Dent Res 1996; 74: 1591-6.
14. Pashley DH, Sano H, Ciucchi B, Yoshiyama M, Carvalho RM:Adhesion testing of
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a reasonable conclusion could have been developed. However, 17. Van Noort R, Noroozi S, Howard IC, Cardew G: A critique of bond strength
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cohesive failures than all other groups, despite a statistically 18. Van Noort R: Dental materials 1994 literature review: dentine bonding. J Dent
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19. Van Noort R: Dental materials 1995 literature review: dentine bonding. J Dent
"sweet spot" implies that a unique relationship exists between 1996; 25: 178-80.
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in this manner, our results tend to partially corroborate the 1988; 1: 184-8.
fmdings ofVersluis et al.27 However, with the exception of in- 21. Eliades G: Clinical relevance of the formulation and testing of dentine bonding
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22. Swift EJ Jr, Perdlgao J, Heymann HO: Bonding to enamel and dentin: a brief
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Delaware), who donated the adhesive and restorative resin systems used. 31. Dietrich T, Losche AC, Losche GM, Roulet J-F: Marginal adaptation of direct
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dentine. J Dent 1999; 27: 119-28.
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131-3 .

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