Adhesion To Tooth Structure, A Critical Review of Macro Test Methods
Adhesion To Tooth Structure, A Critical Review of Macro Test Methods
available at www.sciencedirect.com
Roberto R. Braga ∗ , Josete B.C. Meira, Leticia C.C. Boaro, Tathy A. Xavier
University of São Paulo School of Dentistry, Dept. of Dental Materials, Av. Prof. Lineu Prestes, 2227, São Paulo, SP 05508-000, Brazil
a r t i c l e i n f o a b s t r a c t
Article history: Objectives. Bond strength between adhesive systems and the tooth structure is influenced by
Received 19 November 2009 a large number of variables, which makes the comparison among studies virtually impossi-
Accepted 19 November 2009 ble. Also, failure often times propagates into the dental substrate or the composite, deeming
the results questionable at best. In spite of the increased popularity gained by micro-tensile
and micro-shear tests, in vitro evaluations using specimens with relatively large bonding
Keywords: areas remain frequent. This review focuses on aspects related to specimen geometry and
Bond strength test mechanics of “macro” shear and tensile bond strength tests.
Shear Methods. Besides information drawn from the literature, the effect of some parameters on
Tensile stress distribution at the bonded interface was assessed using finite element analysis (FEA).
Dental adhesives Results. Bond strength tends to increase with smaller bonding areas and with the use of high
Finite element analysis elastic modulus composites. Stress concentration at the bonded interface is much more
severe in shear compared to tension. Among shear methods, the use of the chisel shows the
highest stress concentration. Within the limits suggested by the ISO/TS 11405, crosshead
speed does not seem to influence bond strength values. Pooled data from currently avail-
able adhesives tested in either shear or tension showed 44% of adhesive failures, 31% mixed
and 25% cohesive in the substrate (tooth or composite). A comparative bond strength study
involving three adhesive systems revealed similarities between “macro” and “micro” coun-
terparts regarding material ranking, whereas “macro” tests presented a higher incidence of
cohesive failures.
Significance. Simplicity warrants “macro” bond strength tests an enduring popularity, in spite
of their evident limitations. From a mechanical standpoint, knowing the stress distribution
at the bonded interface and how it is affected by the materials and loading method used is
key to explain the results.
© 2009 Published by Elsevier Ltd on behalf of Academy of Dental Materials. All rights
reserved.
Contents
1. Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . e39
2. A survey of recent bond strength studies . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . e40
3. Variables of influence related to specimen design . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . e40
3.1. Bonding area . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . e40
3.2. Elastic modulus of the resin composite . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . e41
∗
Corresponding author. Tel.: +55 11 30917840.
E-mail address: [email protected] (R.R. Braga).
0109-5641/$ – see front matter © 2009 Published by Elsevier Ltd on behalf of Academy of Dental Materials. All rights reserved.
doi:10.1016/j.dental.2009.11.150
d e n t a l m a t e r i a l s 2 6 ( 2 0 1 0 ) e38–e49 e39
Fig. 1 – Number of articles/year published on dentin and enamel bond strength between 1982 and 2008, according to
www.scopus.com. Left: articles grouped by testing method, right: articles grouped by specimen dimensions, i.e., “macro” or
“micro” (publications on bond strength of orthodontic brackets to enamel were not included).
e40 d e n t a l m a t e r i a l s 2 6 ( 2 0 1 0 ) e38–e49
Fig. 2 – Three-dimensional models used for finite element analysis (left: shear; right: tension). Points A and B define the
diameter of the bonding area.
Fig. 3 – Stress distributions (maximum principal stress, max , and maximum shear stress, max ) at the dentin side of the
dentin/composite interface according to the type of shear loading. Left: 0.2-mm knife-edge chisel; center: 2-mm flat rod;
right: wire loop. Load was applied at 0.2 mm from the bonded interface. Line A–B indicates the diameter of the bonding area.
e42 d e n t a l m a t e r i a l s 2 6 ( 2 0 1 0 ) e38–e49
Fig. 4 – max / max across half of the diameter of the bonded interface according to the type of shear loading, applied 0.2 mm
distant from the dentin/adhesive interface (left) or according to the point of load application using a 0.2-mm thick
knife-edge chisel (right).
areas of composite cohesive failure close to the loading point bution. When load is applied up to 1 mm from the interface,
observed experimentally [134]. Also, it may explain the sta- tensile and shear stresses increase towards the bonded inter-
tistically lower bond strengths when the chisel is compared face, explained by the Saint Venant principle (i.e., a generalized
against testing assemblies using larger contact areas between stress concentration in areas close to the load application
the composite and the loading device, such as the Single-Plane point) [136]. This trend for higher stress concentration with
Shear Test Assembly (SPSTA) [131], the Ultradent notched rod smaller distances is supported by experimental evidence
and the wire loop [27–29]. showing lower bond strength when the load was applied
Another important aspect of shear tests is that closer to the at the interface as opposed to a 0.5 mm distance from the
interface tensile stresses are actually higher than shear, sug- dentin substrate [134]. The ratio between maximum shear
gesting that the former is responsible for failure initiation, as and maximum principal stress decreases as load applica-
previously stated [9,135,136]. For the knife-edge chisel and the tion moves away from the interface, indicative of an increase
wire loop methods, shear stresses start to prevail over ten- in bending moment (Fig. 4, right). When load is applied
sion at 0.3 mm from the load application area, while for the at distances beyond 1 mm from the interface (not shown),
flat rod tensile stresses predominate up to 1.2 mm (Fig. 4, left). the increase in tensile stress as load application moves
Therefore, the term “shear bond strength” would more appro- away from the bonded interface becomes even more evident
priately refer to the loading mode, rather than the nature of [9,136].
the stress responsible for bonding failure. In the tensile test, stresses are far more homogeneous
The distance between the point of load application and across the interface than in shear and, therefore, maxi-
the bonded interface in shear tests also affects stress distri- mum principal stress values are much closer to the nominal
Fig. 5 – Stress distributions (maximum principal stress, max , and maximum shear stress, max ) at the dentin side of
dentin/composite interfaces loaded in tension (left) or shear, using a 0.2 mm chisel applied at 0.2 mm from the interface
(right). Line A–B indicates the diameter of the bonding area.
d e n t a l m a t e r i a l s 2 6 ( 2 0 1 0 ) e38–e49 e43
ter) and while one did not report differences among crosshead
speeds ranging from 0.5 to 5.0 mm/min [140], the other found
strength. However, the area subjected stress levels close to the
statistically higher bond strengths for crosshead speeds of 5.0
maximum is much larger than in the shear test (Fig. 5). The
and 10.0 mm/min compared to 0.1, 0.5 and 1.0 mm/min [141].
height of the composite cylinder in the tensile test does not
Such inconsistencies found for both shear and tensile tests
influence stress distribution or magnitude if kept above 2 mm
may be explained by differences among testing assemblies
[9].
and/or the brittle nature of dental adhesives and composites.
The comparison of crosshead speeds among testing assem-
4.2. Crosshead speed
blies with different compliance levels is problematic and less
meaningful than comparing load rates. Also, it has been ver-
Due to the viscoelastic nature of polymers and compos-
ified that at small strains, the strain rate variation had a
ites, it could be expected that bond strength tests would
negligible effect on the measured stress values of amorphous
present some strain rate sensitivity. Experimental obser-
polymers [142]. Nevertheless, it is important to emphasize that
vations revealed that composite yield strength and elastic
among the studies described, only one reported differences in
modulus increase at higher strain rates [137], possibly due to
bond strength within the crosshead speed range proposed in
secondary molecular processes. At high strain rates, the poly-
the ISO/TS 11405 (0.75 ± 0.30 mm/min).
mer chains become stiffer and molecular mobility is reduced
[138]. Determining the actual strain rate (unit: mm/mm s or
s−1 ) requires an extensometer and depending upon the spec- 5. Incidence of cohesive failures
imen geometry it may not be feasible. Therefore, specimen
loading is usually expressed in terms of crosshead speed, in As mentioned above, reporting bond strength in terms of
mm/min. nominal stress values is questionable due to the heteroge-
Studies evaluating the influence of crosshead speed on neous stress distribution and also due to the occurrence of
“macro” shear and tensile bond strength are few and show cohesive failures both in the dental substrate and the resin
contradictory results. Coincidentally, two of them used the composite. Defining categories for classification of failure
same adhesive system and composite (Single Bond and Z100, modes of debonded specimens is a complicated task and,
3M ESPE). However, bonding areas, specimen storage times in some instances, the limit between mixed and cohesive
and test assemblies were different. One study used the failure becomes merely subjective. Fig. 6 shows the failure
Single-Plane Shear Test Assembly (SPSTA) on specimens with mode distribution observed in 37 studies recently published
5-mm diameter bonding areas, finding no statistically signif- according to the bonding substrate and the loading mode
icant differences among crosshead speeds between 0.5 and [31–34,37,39–41,43,45,64,73,76–80,84,86–88,95–99,101,102,108,
10 mm/min [131]. The other study used a knife-edge steel 109,117,118,120,121,123–125]. Overall, 44% of the specimens
rod to test specimens with 3-mm diameter bonding area and failed exclusively along the bonded interface, while 31%
found statistically higher bond strengths for those loaded at presented mixed failures and 25% presented predominantly
1.0 and 5.0 mm/min compared to 0.5 and 0.75 mm/min [139]. (i.e., more than 75% of the bonding area) cohesive failure
A similar scenario is observed with two studies that eval- either at the composite or the dental substrate.
uated the effect of crosshead speed on tensile bond strength. Rather than an indication of strong bonding, cohesive
Both used similar bonding areas (3.6 and 4.0 mm in diame- failure is explained by the mechanics of the test and the brit-
e44 d e n t a l m a t e r i a l s 2 6 ( 2 0 1 0 ) e38–e49
Fig. 8 – Failure mode distributions (in %) observed under 10–30× magnification for each adhesive system, according to the
testing method. Top, left: Adper SE Plus; top, right: Adper Single Bond 2; bottom, left: Adper Scotchbond Multi-Purpose;
bottom, right: pooled data.
tleness of the materials involved. In the shear test, tensile (Adper Single Bond 2) and a self-etch system (Adper SE Plus),
stress concentration in dentin near the crack tip causes the all from the same manufacturer (3M ESPE, St. Paul, MN, USA),
failure to propagate into the substrate. Versluis et al. [134] ver- were tested for bond strength to superficial bovine dentin.
ified both experimentally and using a failure accumulation Except for the micro-tensile specimens, teeth were embed-
computer model a tendency for dentin failure to increase at ded in PVC cylinders using self-cure acrylic, with the dentin
lower crosshead speeds, thicker adhesive layers and moving surface kept 2 mm above the embedding material. Dentin
the point of load application away from the bonded interface. roughness was standardized using a 600-grit SiC paper. For
Dentin pull-out was also associated with high bond strength macro shear and tensile tests (n = 10), a 3-mm diameter area
values, although the correlation for individual specimens was was delimited with adhesive tape. After adhesive application
weak. following manufacturers’ directions, a 3-mm height truncated
A recent study evaluating the tensile bond strength of five cone was built using a microhybrid composite (LLis, FGM Pro-
resin cements to dentin reported a strong positive correlation dutos Odontológicos, Joinville, Brazil) with the smaller base
between strength values and the area of cohesive failure in (3-mm diameter) contacting the adhesive layer. Micro-shear
resin observed in mixed mode failures, evaluated using scan- specimens (n = 5) were built by inserting the composite into
ning electron microscopy [31]. Bonding area has also been segments of Tygon tubing (Saint-Gobain Performance Plas-
associated with the incidence of cohesive failures. Specimens tics, Akron, OH, USA), four per tooth, with internal diameter
with rectangular cross-sectional areas larger than 7.17 mm2 of 0.76 and 0.4 mm in height, and photo-activating it in con-
built using a self-etching primer system (Clearfil Liner Bond 2, tact with the adhesive-coated dentin. For the micro-tensile
Kuraray) and loaded in tension showed exclusively cohesive specimens (n = 5), teeth crowns were sectioned perpendicu-
failures in dentin. Between 2.31 and 7.17 mm2 , both cohesive larly to the exposed dentin surface and the resulting dentin
and adhesive failures were observed [13]. area received the adhesive application. Such modification in
dentin tubule orientation was necessary to increase the dentin
thickness available for specimen sectioning. A 4-mm high
6. A comparison between macro and micro composite block was built onto the dentin surface. All spec-
bond strength tests imens were stored in distilled water at 37 ◦ C for 24 h prior
to testing. For the micro-tensile test, stick-shaped specimens
In order to verify how “macro” bond strength tests compare to 0.8–1.0 mm2 (five per tooth) were cut using a diamond wafering
their “micro” counterparts in terms of material ranking, inci- blade immediately prior to testing. For macro- and micro-
dence of cohesive failures and data scattering, a three-step shear testing, a 200-m knife-edge chisel placed in contact
(Adper Scothbond Multi-Purpose), a two-step etch-and-rinse with the dentin surface was used to debond the composite
d e n t a l m a t e r i a l s 2 6 ( 2 0 1 0 ) e38–e49 e45
truncated cones/cylinders. Tensile test used a clamp that con- mens loaded in shear, compared to tension. Among the shear
tacted three-quarters of the truncated cone circumference. methods, the use of the chisel as a loading device causes
Articulated joints were used to assure that the bonded inter- the most severe stress concentration, which is also supported
face was perpendicular to the loading axis. For micro-tensile by experimental findings showing lower bond strengths com-
testing, Geraldeli’s jigs were used [143]. All tests were carried pared to other shear loading methods, such as the wire loop
out at a crosshead speed of 0.5 mm/min. Specimen failure or the flat rod. Within the limits suggested in the ISO/TR
mode was assessed under a stereomicroscope at 10–30× mag- 11405, crosshead speed seems to have little influence on bond
nification. Results were submitted to one-way ANOVA/Tukey strength results. Finally, in view of the many aspects affecting
test at a pre-set global significance level of 5%. the results of “macro” bond strength tests, in order to allow
Bond strength results are displayed in Fig. 7. As discussed for a more judicious comparison among studies researchers
above, the reduction in bonding area corresponded to an must provide a thorough description of the specimen design
increase in bond strength values. “Macro” tests displayed a and test configuration.
similar range of values, between 5.6 and 11.5 MPa. Both shear
tests ranked the adhesive systems similarly, while for the ten-
sile tests there was an inversion between the two systems with Acknowledgements
the highest bond strengths. Coefficients of variation ranged
between 28 and 36% for shear, 21 and 40% for micro-shear, Authors would like to express their gratitude to FGM Produtos
32 and 38% for tension and 25 and 64% for the micro-tensile Odontológicos and 3M ESPE for kindly donating the materials
test. The higher scattering displayed by the self-etch system used in the experimental section of this review.
in both “micro” tests may be explained by the association of
lower bond strength with a more technique-sensitive speci-
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