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Testing Adhesion of Direct Restoratives to Dental Hard Tissue - A Review

Article  in  The journal of adhesive dentistry · October 2010

DOI: 10.3290/j.jad.a19741 · Source: PubMed

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Testing Adhesion of Direct Restoratives to Dental Hard

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Ulrich Salza/Thorsten Bockb

Abstract

This articles concerns itself with the testing of adhesion between direct restoratives and dental hard tissue,
ie, enamel and dentin. The aim is to survey available methods for adhesion testing and influential parameters
affecting experimental outcome. The testing of adhesion to indirect restorative materials, eg, ceramics and met-
als, is beyond the scope of this article and shall be discussed elsewhere. The longevity and success of modern
dental restorations very often relies on potent dental adhesives to provide durable bonds between the dental
hard substance and the restorative composite. To predict the clinical outcome of such restorative treatment, a
large variety of in vitro laboratory tests and clinical in vivo experiments have been devised, analyzed, and pub-
lished. The purpose of this review is to provide a current overview of bond strength testing methods and their
applicability to the characterization of dental adhesives. Regardless of the method employed, subtle variations
in sample preparation may already severely impact test results, usually necessitating at least co-testing of a
well-known internal reference to allow conclusive interpretation. This article attempts to list and discuss the
most influential parameters, such as substrate nature, age, health status, storage, clinically relevant pre-treat-
ment, and sample preparation. Special attention is devoted to the last aspect, as numerous publications have
stressed the tremendous influence of preparatory parameters on the validity and scope of obtained data. Added
to the large variety of such factors, an equally large diversity of load-applying procedures exists to actually quan-
tify adhesion between composites and dental hard substance. This article summarizes the basics of macro and
micro approaches to shear and tensile bond strength testing, as well as push- and pull-out tests. The strengths
and weaknesses inherent to each method and influential test parameters are reviewed and methods for acceler-
ated sample aging and simulation of clinical conditions presented. Alternatively to shear or tensile bond strength
tests, fracture toughness is introduced together with its application to dental adhesives and an overview of its
physical background.
Keywords: dentin, enamel, adhesion, in vitro test, shear bond strength, tensile bond strength, marginal ad-
aptation, fracture toughness.

J Adhes Dent 2010; 12: 343-371. Submitted for publication: 09.06.10; accepted for publication: 01.08.10.

T he demand for esthetic restorations, such as tooth-

colored fillings with invisible margins or highly es-
thetic crowns, inlays, onlays, and veneers has increased
significantly with the shift towards more image-focussed
societies. Teeth impaired by fracture or caries are to be
reconstructed indiscernibly, and ideally by a minimally
invasive approach. In preventive dentistry, pit and fis-
a Chemist, DSc, Head of Department of Adhesive and Temporary Materials,
Ivoclar Vivadent, Schaan, Liechtenstein.
b Chemist, DSc, Team Leader of Department of Adhesive and Temporary Mate-
rials, Ivoclar Vivadent, Schaan, Liechtenstein.
Correspondence: Dr. Ulrich Salz, Research and Development, Ivoclar Vivadent,
Bendererstr. 2, Schaan FL 9494 Liechtenstein. Tel: +423-235-3421, Fax:
+423-233-1279. e-mail: ulrich.salz@ivoclarvivadent.com
sure sealants have become a common and effective
approach to caries prevention. In orthodontic treatment,
brackets may be bonded to acid-etched enamel using
composite based cements. All these treatments have
only become possible through the realization of effec-
tive enamel/dentin adhesives in the 1980s and 1990s.
Meanwhile, there have been various improvements to
adhesive systems, both in terms of efficacy and user
friendliness.
Despite these advances, the adhesive technique re-
mains encumbered by its need for a clean, dry operation
field, often difficult to provide in subgingival regions. For
the sake of convenience and to reduce technique sensitiv-
ity, increasingly simplified adhesives are being introduced,
despite some apparently inherent technique limitations.
A concomitant improvement of long-term adhesion per-
formance seems, at least in some cases, to have lower

Vol 12, No 5, 2010 343

Salz and Bock
Fig 1a Schematic drawing of the composite/adhesive/dentin
interface.
priority. The reduced clinical longevity and long-term es-
thetic appeal of composite restorations prepared using
simplified self-etching adhesives are a constant source
of complaints.183,351 In spite of enormous advances in
adhesive technology since the introduction of enamel
etching by Buonocore five decades ago, the interface of
dental hard substance and composite, luting material, or
adhesive (Figs 1a and 1b) remains the Achilles heel of
adhesive restorations.43,78
Consequently, adhesive technology still faces the chal-
lenge of combining the improvements made in adhesion
performance, adhesive reliability and simplified applica-
tion protocols. These demands can now be extended to
the recently introduced self-adhering direct restorative
and luting materials. To verify the improvements claimed
for such materials, reliable, reproducible, and conclusive
analytical and in vitro methods are indispensable. The
analysis of material properties demands reproducible
quantification of both short- and long-term adhesive per-
formance, the simulation of long-term loading effects,
and methods to investigate the underlying adhesion
mechanisms. Microscopic imaging methods, such as
scanning electron microscopy (SEM),42,95,99,277,348,377
transmission electron microscopy (TEM),37,43,189,350
confocal laser scanning microscopy (CLSM),248,365 or
atomic force microscopy (AFM)93,277,350,379 can be used
to identify micromorphological alterations at the inter-
face. Spectroscopic methods such as nuclear magnetic
resonance spectroscopy (NMR),27,118,210,209 x-ray pho-
toelectron spectroscopy (XPS), electron spectroscopy
for chemical analysis (ESCA),191,380 FT infrared,309 Ra-
man,154,292,362,368 or Auger91 spectroscopy are helpful
for identifying and analyzing interfacial chemical interac-
tions or reactions and provide better understanding of
adhesion mechanisms.
The discovery of the elementary mechanisms of enamel
and dentin adhesion date back to the investigations of
Buonocore47,46 and Nakabayashi.200 Adhesion to both
substrates is attributed to a mixture of micromechanical
interlocking and the chemical interaction of functional-
ized monomers with apatite.380 Commonly, preparation
for adhesive treatment involves the superficial dissolution
344
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Fig 1b Schematic drawing of the composite/adhesive/enamel
interface.
of dental hard substance by phosphoric acid (“etch-and-
rinse technique”) or by acidic monomers (“self-etching
technique”). In the etch-and-rinse technique, the adhe-
sive is applied after the rinse step to impregnate the
morphological features exposed by phosphoric acid with
polymerizable monomers. In the self-etching technique,
features exposed by the action of acidic monomers are
simultaneously infiltrated with adhesive.
Generally, acids selectively demineralize enamel to ex-
pose patterns of prismatic and interprismatic enamel.
On dentin, the smear layer caused by mechanical cavity
preparation is dissolved to varying degrees, exposing col-
lagen fibers and opening dentin tubules. The morpho-
logical features are impregnated by appropriate (meth)
acrylate or (meth)acrylamide monomers, the in situ radi-
cal polymerization of which results in various forms of
interpenetrating networks (“hybrid layer”, Fig 2). Com-
pared to the etch-and-rinse approach, self-etching dentin
adhesives form thinner hybrid layers, or with mild acidic
formulations, even only nano-interaction zones.164
In addition to the micromechanical aspects mentioned
above, adhesives chemically interact with dental hard sub-
stance,380 although this contribution to overall enamel/
dentin adhesion or long-term performance is difficult to
quantify. While spectroscopic methods allow analysis of
chemical or physicochemical interactions of monomers,
polymers, and dental hard tissues, the comprehensible
correlation of such data with mechanical analysis remains
an unsolved problem.
The long-term durability of dentin adhesion appears to
be influenced by substrate stability, metal matrix proteins
(MMPs),37,136,174,206,334 and the ongoing decalcification
by bacterially generated acids.168,225
A number of procedures have been proposed and stand-
ardized to evaluate performance of industrial adhesives82
based on polyurethanes or cyanoacrylates, for instance.
With some exceptions, the majority of these long-standing
adhesive joint strength tests fall into three categories:
tensile, shear, and peel. The performance of enamel and
dentin adhesives is predominantly investigated via shear
or tensile bond strength. Due to the complexity of the
adhesive/substrate interaction, it is however paramount
The Journal of Adhesive Dentistry

not only to design or select an appropriate test procedure,
but also to carefully interpret the obtained results. As the
literature corroborates, the latter aspect often requires
considerable background and detailed insight into the
physical background of the method.82
IN VITRO/IN VIVO INVESTIGATIONS
Adhesive development and product quality assurance
require reliable and conclusive laboratory methods to
assess material properties. However, validation and re-
producibility of hitherto available analytical approaches
to adhesion testing on dentin or enamel suffer from
the nonstandardizable nature of the substrates. Further
aggravation results from the influence of the test envi-
ronment on adhesive performance. These influences
greatly complicate the prediction of adhesives’ clinical
behavior from in vitro laboratory data, such as prob-
ability of postoperative sensitivity, marginal integrity and
discolorations, long-term performance, and life-span of
restorations.228 Since routine clinical investigation of
new adhesive formulations or monomers is technically
and ethically not feasible, some notes for guidance re-
garding in vitro investigations have been published.301
Still, cynics consider dentin adhesives to be among the
few medical devices to reach market introduction without
adequate clinical data.237 This opinion disregards the
potency of lawsuits, which in itself urges manufacturers
to invest resources in clinical investigations. However, the
results of time- and labor intensive clinical investigation
of an adhesive’s long-term performance often become
available only after the adhesive has been superceded by
follow-up products. This observation is substantiated by
the fact, that only a few long-term clinical adhesive stud-
ies have been published in the recent past.23,259
Ideally, a sound correlation between in vitro and in vivo
data is established, which allows prediction of clinical
performance from laboratory data. Different procedures
have been proposed to simulate clinical situations, chiefly
involving the treatment of vital teeth scheduled for later
extraction for periodontal or orthodontic reasons. These
methods, although laborious and time consuming, allow
near-perfect simulation of the oral environment and its
effects on adhesives and adhesively prepared cavities.
A comparison of in vitro and in vivo data obtained for
orthodontic bracket cements, for example, showed devia-
tions regarding prediction of clinical outcome from bond
strength.315 While resin-modified glass ionomers gave
significantly lower in vitro bond strength than resin-based
bracket cements, the two materials were comparable re-
garding clinical survival rate after 1.3 years. Murray et
al196 also found in vivo placement of bracket cement to
yield lower bond strength than in vitro application. How-
ever, this observation could not be confirmed by Chatzista-
vrou et al,60 who obtained comparable results by in vivo
and in vitro tests.
In vivo placement of adhesives was repeatedly found to
reduce bond strength on dentin compared to in vitro appli-
cation, although the effects showed a certain dependency
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Fig 2 SEM image of a hybrid layer.
on the employed adhesive.186,201,253,320 Purk et al254,253
explained lower in vivo bond strength by the technically
more challenging placement of adhesive and composite
in the oral cavity. Although in vitro and in vivo placement
led to comparable interface micromorphologies,63,87,106
in vivo placement was accompanied by a higher occur-
rence of voids under the composite.
Several investigations on marginal adaptation and
quality of restorations placed in vitro were carried out to
predict in vivo performance of the corresponding adhe-
sive/composite system. Unfortunately, different teams
obtained differing results, and/or drew different conclu-
sions from their data. For instance, Frankenberger et al115
concluded that “clinical behavior of restoration margins is
predictable with the restriction that marginal adaptation is
only one among several important aspects in restorative
dentistry, ie, clinical outcome is not predictable from mar-
ginal integrity alone”. Conversely, Heintze137,138 asserts
that “the surrogate parameter ‘marginal adaptation’ of
restorations placed in extracted teeth has a mediocre
value to predict the clinical performance of an adhesive
system in cervical cavities. The composite is an important
factor for successful prediction. The comparison between
in vitro and in vivo investigations is occasionally hampered
by the great variability of clinical results obtained with the
same adhesive.” In addition to environmental influences,
the outcome of in vitro and in vivo adhesive investigations
are highly sensitive to the experience, motivation, and
skill of the operator.4,107,117,125,149,193,303,302
Given optimal conditions, a very good correlation was
established between in vitro tests of microtensile bond
strength and long-term clinical success of Class V cavities
using a variety of adhesives.241-243,347,352,353 Neverthe-
less, the ability of bond strength data to predict the clinical
performance of an adhesive/composite system or even
single aspects of performance, such as marginal integrity,
is questionable. The shear and tensile bond strength tests
345
Salz and Bock
Table 1 Bonding variables according to Pashley et al230 influencing the test results of adhesive bond or
measurements
A. Substrate
1. Human or bovine dentin?
2. Superficial, middle or deep dentin?
3. Occlusal, proximal, buccal?
4. Third molars or incisors?
5. Sanded surfaces? Grit? Method?
Al2O3? SiC, 320, 600, 800 or 1000 grit?
6. Dental burs? Diamond, carbide?
7. Reuse of teeth?
8. Mount in plastic, stone, etc.?
C. Priming
1. Cover entire surface or apply within matrix
2. How much primer?
3. Passive or active? How long?
4. Wash or evaporate? How long?
5. Light cure or not?
6. Wet vs dry? How wet, how dry?
E. Storage
1. Water, isotonic, saline, etc.?
2. Room temperature or 37°C?
3. 100% RH or water?
4. Preservatives? Sodium azide, thymol, chloramine?
5. Pulpal pressure or not, magnitude? Composition of fluid?
6. Time: 24 h? months? years?
7. Thermal stress? Temperatures, dwell time, number of cycles?
8. Tooth flexure (load) tests. Magnitude, number of cycles?
have been criticized for their uneven interfacial stress distri-
bution upon loading,18,40 which induces crack propagation
into tooth substrate or composite (“cohesive” or “mixed”
failure). Such a failure mode implies that the dentin/ad-
hesive/composite interface evaded stress and the data,
rather than elucidating bond durability, reflect a convoluted
mixture of material properties. Cohesive or mixed failures
also distort nominal bond strength values, as the fractured
area is usually greater than the interfacial area used to
calculate bond strength.329
In spite of considerable advances regarding bond
strength analysis, shortcomings of present methods and
the lack of an accepted standard protocol necessitate
new bond strength testing procedures. This unsatisfac-
tory situation was a topic at the Academy of Dental Materi-
als annual meeting in 2009. The generally observed wide
variation of bond strength of given adhesives as obtained
by different research groups was attributed to the chal-
346
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B. Etching
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1. Etch or no etch?
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2. What type of etchant?
3. How much etchant? Renewed?
4. How long?
5. Passive or active?
6. Rinse? How long?
7. Dry? How long?
8. Rewet? How much?
D. Bonding
1. How much adhesive for how long?
2. Spread with air? How thin, how dry?
3. What diameter bonding area?
4. Pack with pressure or no pressure?
5. Pulpal fluid/pressure or no pressure?
6. Light curing. How much light? How long?
F. Testing
1. Shear vs tensile
2. Stress rate
3. Immediate vs 24 h, vs months
4. Express dentin bonds in MPa or as % of enamel bond strength?
5. Microleakage vs bond strength
6. Gap size vs bond strength
7. Regional bond strength vs center of tooth
8. Gingival floor of Class V vs occlusal floor of Class I cavities
9. Configuration factors: flat surfaces vs 3D cavities
lenging number of influencing factors in specimen prepa-
ration and testing. It was concluded that reliable results
demand the strict limitation of experimental variations to
those actually focussed on in the investigation, that ma-
terials and methods must be described in as much detail
as possible, and incidents such as pre-test failures be
noted and integrated into the results. These requests are
substantiated by a systematic review and a meta-analysis
on in vitro orthodontic bond strength testing conducted
by Finnema et al.108 Experimental conditions significantly
influencing in vitro bond strength of orthodontic brackets
on enamel are water storage of the test specimen, pho-
topolymerization time, and crosshead speed. Based on
the results of the systematic review, it was concluded that
many studies did not properly report test conditions which
could have significantly affected the outcomes.
An often disregarded factor when comparing in vitro data
to everyday clinical performance is the age of dental adhe-
The Journal of Adhesive Dentistry

sives employed. Most materials on the market are based
on aqueous methacrylate solutions and are thus subject
to degradation by ester hydrolysis.185 Whereas company-
sponsored tests tend to employ freshly produced mate-
rial, methacrylate-based single-component self-etching
adhesives in the practioner’s office may have undergone
acid-catalyzed hydrolysis during storage that detrimentally
affects adhesive performance.7,211,212,268,269 Addition-
ally, the evaporation of solvent from acetone-based adhe-
sives during storage can cause phase separation of hy-
drophobic and hydrophilic components in the bottle, thus
influencing the composition of adhesive taken from the
package. If acetone-based adhesives are dispensed into
a dappen dish prior to use, rapid phase separation prior
to application can be observed. The degree of manual
mixing of phase-separated liquids introduces yet another
variable to the process.119,349
It goes without saying that any investigation of adhe-
sive performance is strongly influenced by changes in
adhesive formulation. Unfortunately, little regard is paid
to these factors, as the investigators are often unaware of
the implications of material age, storage conditions, and
phase compatibility during storage or application.
For reasons of availability, most investigations are car-
ried out using dentin as the tooth substrate. For etch-and-
rinse adhesives, this is a reasonable approach, as these
materials’ enamel bond strength generally surpasses
their dentin adhesion.230 It is, however, a well-known
experimental fact that most one-component self-etching
adhesives show lower bond strength on enamel than on
dentin.269,302 As most cavities are enamel bordered, a
self-etching system’s enamel margins pose a weak link
in this form of restorative therapy.
INFLUENCING FACTORS
Pashley et al230 summarized the bonding variables for
etch-and-rinse adhesives as shown in Table 1, subdi-
viding them into substrate, etching, priming, bonding,
storage, and testing. Obviously, the recent introduction
of self-etching adhesives with their specific application
and bonding mechanism introduced further variables.
In a meta-analysis of factors involved in bond strength
testing, Leloup et al175 found the elastic modulus of the
composite, bonded area, storage conditions of the test
samples, and test design (ie, shear, tensile, crosshead
speed) to have a significant influence on bonding to
dentin. Furthermore, mean bond strength and failure
mode significantly correlate: higher bond strength in-
creases the rate of cohesive failures. Yet, cohesive fail-
ure does not imply perfect adhesion and therefore does
not permit the conclusion that the adhesive’s perform-
ance is beyond improvement.72 The factors influencing
the in vitro and in vivo performance of dental adhesives
can be roughly divided in two main groups:
A: the substrate itself, storage of substrate, and pre-
treatment of the substrate
Vol 12, No 5, 2010
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B: methods of adhesive application, measurement pro-
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Substrate Enamel/Dentin e ss e n c e
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Storage conditions of extracted teeth
Extracted teeth are normally stored over a period of sev-
eral weeks in disinfecting solutions, eg, 10% formalin,
70% ethanol, 0.1-1% chloramine-T, or 0.05-0.1% thymol
prior to use. In the USA, for instance, the Centers for
Disease Control and Prevention (CDC) has adopted
guidelines for disinfection of extracted teeth used in
research and teaching.162 Prior to use, teeth devoid of
amalgam are to be heat sterilized by an autoclave cycle
for 40 min. Teeth containing amalgam are to be stored
in 10% formalin for 2 weeks. While heat treatment may
plausibly affect the collagen structure and thereby influ-
ence the formation of smear and hybrid layer, aldehydes
such as formalin or glutaraldehyde are known to react
with collagen.34 Phenolic compounds, eg, thymol, are
known to inhibit radical polymerization and may thus
reduce the degree of conversion and influence adhesive
performance.
Depending on the adhesive employed, no11 or a neg-
ative effect258 on bond strength was observed when
the teeth were stored for 3 or 6 months, respectively,
in 0.05% saturated solution of thymol. Recently, Lee et
al172 compared bond strength to bovine incisor crowns
stored at 37°C for 60 days in distilled water, 0.9% NaCl,
0.5% chloramine-T, 5.25% NaOCl, 2% glutaraldehyde, or
10% formalin. A subset of 10 specimens from all groups
was autoclaved, while a subset of 10 specimens from all
groups (except formalin) was kept in 10% formalin for 2
weeks. Storage in NaOCl resulted in lower bond strengths,
while sterilization with the autoclave negatively affected
the bond strength of specimens stored initially in distilled
water or 10% formalin. Sterilization with formalin alone
had no significant effect on bond strengths; therefore, the
recommendation was given to use extracted teeth stored
in 10% aqueous formalin solution.
No difference in dentin bond strength was found be-
tween samples prepared from teeth 30 min and 2 years
after extraction.190 However, it may be expected that ex-
tracted teeth stored for more than six months are subject
to degenerative changes in dentinal proteins.
Mechanical function of the substrate enamel/dentin
For a better understanding of the mechanical resilience
of restored teeth, it is important to comprehend (and
possibly simulate) the behavior of restored dentin and
enamel under external loads. During a lifetime, perma-
nent teeth undergo a vast number of cyclical loads that
inevitably lead to abrasion, mechanical fatigue, or crack
propagation from stress overload. To withstand everyday
circumstances, teeth must therefore simultaneously be
tough and resistant to abrasive wear. These two proper-
ties are usually considered antagonists, because hard
structures, while resistant to wear, tend to be brittle and
prone to crack formation, whereas tough materials lack
347
Salz and Bock
wear resistance. By evolutionary processes, tooth anat-
omy has incorporated both properties: enamel acts as
a hard, highly stiff, wear-resistant shell, approximately
five times harder than dentin66,308 which, in contrast,
has considerably lower stiffness and is about four times
tougher than enamel.255 Together, the two materials
offer a unique combination of properties that allows the
dentition to perform in a mechanically extremely chal-
lenging environment.
Substrate changes depending on the age of the donor
Due to ongoing mineralization processes, tooth mor-
phology is subject to constant change. The overall thick-
ness of coronal dentin, for example, increases around
6.5 μm per year, root dentin also increases, whereas
the density of odontoblasts, sub-odontoblasts, and pulp
fibroblasts decreases. 198 The degree of age-related
morphological changes in teeth appears to be asymmet-
rical, with decreases in root dimensions being greater
than in the crown. At all ages, pulp cell densities, in-
cluding odontoblasts, in the crown were greater than
in the root. Decreases in pulp cell density may reduce
pulp repair activity after restorative treatment, although
increases in dentinal thickness may augment pulpal
protection. Understanding of these age-related changes
may improve restorative and endodontic care, especially
in older patients. About 10 vol.% of coronal dentin
consists of tubules, which seems to be independent of
age,121 although over time, tubule diameter decreases,
resulting in lower dentin permeability. Consequently,
human teeth older than 50 years contain less water
than younger teeth, which (among other effects) embrit-
tles the dental hard substance.237,238
The influence of subject age on bond strength to human
teeth was investigated by several groups.36,223,318 Brack-
ett et al36,24 examined the microtensile bond strengths
of an etch-and-rinse adhesive to dentin and enamel and
a resin-modified glass-ionomer adhesive to dentin. No
difference in bond strength was detected between teeth
originating from subjects over 60 years and those coming
from younger subjects. Although SEM evaluation of the
etched surfaces of aged dentin exhibited decreased depth
of decalcification in the intertubular areas, there was no
observable difference between the tubules of young and
aged dentin. Other authors223 evaluated the effect of age
on dentin and enamel microtensile bond strength of a
glass ionomer, a one-step self-etching adhesive (React-
mer Bond), and a two-step self-etching adhesive with an-
tibacterial properties (ABF Bond). Extracted molars from 3
age groups (20 to 25, 35 to 40, and 50 to 55 years) were
used. Enamel bond strength values were not affected
by the age of teeth for any bonding system. Dentin bond
strength using the two-step self-etching adhesive was
affected by tooth age, while the one-step self-etching ad-
hesive was not influenced. Tagami et al318 evaluated the
effect of age on the dentin tensile bond strengths of four
adhesives using proximal dentin of premolars extracted
from young (age: 9 to 21 years) and older (age: 42 to 64
years) subjects. The investigation concluded similar bond
strength for each adhesive, regardless of substrate age.
348
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Tubule and prism orientation t fo
Due to its prismatic morphology, enamel rexhibits
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sotropic mechanical properties. Consequently, cat
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ness will be greater for loads applied parallel to prism
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orientation than for loads perpendicular ss e n c e
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the prisms are orientated roughly orthogonally to the
enamel-dentin junction,308 the preparation of teeth prior
to bond strength testing is an influential factor.
Dentin also possesses anisotropic properties: tubules
pose some 10% of the total dentin volume in the form
of cylindrical voids, with tubule density and diameter de-
creasing from pulp to outer dentin. Since tubules are
involved in stress transfer upon mechanical loading, the
depth of an adhesive’s dentin infiltration plays an impor-
tant role in bond strength assessment.161
The effects of regional variations in tooth structure,
such as the orientation of enamel prisms and dentinal
tubules and the influence of cavity geometry on bond
strength, are variously discussed. In one study,213 tubule
orientation parallel to the bond interface gave higher ten-
sile bond strength than a perpendicular tubule orienta-
tion, independent of the type of adhesive system used
(self-etching vs etch-and-rinse). In contrast, other authors,
such as Adebayo et al,5 Phrukkanon et al,246 and Watan-
abe et al363 found no influence of tubule orientation on
microtensile bond strength.
In enamel bond strength assessment, the generally
accepted mode of substrate preparation is to expose per-
pendicularly cut enamel prisms in order to obtain higher
bond strength.143,196 However, this observation is contra-
dicted by Shimada et al,192,291 with their recent discovery
of a weak influence of enamel prism orientation for a self-
etching adhesive system.
Sclerotic dentin in noncarious cervical lesions (NCCL)
Noncarious cervical lesions are defined as loss of tooth
substance at the cementoenamel junction. The cause of
lesions on the cervical margins of teeth is attributed to
erosion, abrasion, and attrition. Erosion may be due to
chemical or idiopathic factors;26,177,235 abrasion results
from mechanical forces; attrition is caused by functional
or parafunctional contact, including normal chewing and
bruxism. However, the occurrence of a lesion on a sin-
gle tooth flanked by nonaffected teeth raises doubt as
to whether all NCCL originate due to erosion, abrasion,
or attrition.188,215
A Raman spectroscopic investigation of noncarious
sclerotic cervical lesions155 revealed hypermineralized
dentin with a mineral to matrix ratio 2 to 3 times higher
than that of normal dentin. This may result from increased
mineral contents, decreased organic matrix (collagen)
contents, or both. In addition, the phosphate and carbon-
ate content in NCCL sclerotic dentin is lower than that
of normal dentin. Compared to the changes in inorganic
composition, alterations in the organic phase are not
dramatic. Still, there is a notable decrease in the ratio of
nonreducible to reducible cross links in NCCL sclerotic
dentin, indicating constitutional changes in the collagen
matrix during NCCL formation.
The Journal of Adhesive Dentistry

Loss of tooth substance in the cervical area may pose
esthetic problems, cause dentinal hypersensitivity, and
therefore require restorative treatment. Irrespective of the
use of etch-and-rinse or self-etching adhesives, bonding
to sclerotic dentin in NCCL has resulted in compromised
results.169,381 Removal of the surface layers of sclerotic
dentin and/or conditioning with stronger acids may facili-
tate stronger bonding to sclerotic dentin.169 The benefit
of this procedure was confirmed by a clinical study car-
ried out by Kim et al,159 who found that surface prepa-
ration (removing sclerotic dentin and bevelling margins)
improved the retention rate of composite restoration of
noncarious cervical lesions. Additionally, significantly less
marginal discoloration was observed in comparison to
those lesions restored without surface preparation.159
Caries-affected dentin
Dentin consists of about 70% hydroxyapatite, 18%
to 20% organic matter and 10% to 12% water.61 The
hydroxyapatite crystals are randomly oriented in an
organic matrix, which is mainly composed of type I col-
lagen and collagen-like compounds. Morphologically,
dentin can be differentiated into odontoblasts, dentinal
tubules with the periodontoblastic area, and peritubular
and intertubular dentin. The caries process involves dis-
solution of hydroxyapatite (demineralization) invoked by
acidic by-products of oral bacteria.346 The acid-induced
demineralization of dentin is followed by the decompo-
sition of the collagenous organic matrix in which den-
tin-endogenous metallomatrix proteinases apparently
participate.61,339
The pulp-dentin complex responds to the carious proc-
ess either by completely blocking the dentinal tubules,
or by a decrease of the tubule diameter to counter pul-
pal contamination by bacteria and toxins. The deposits
in the dentinal tubules are composed of B-tricalcium
phosphate (also called whitlockite).70,89 The effects of
the caries process on the composition, structure, and
mechanical properties of dentin are given in detail by
Perdigão.237,238
The restoration of carious dentin using adhesive
technology and the adhesion to caries-affected dentin
have been the subject of many studies. Typically, bond
strength to caries-affected dentin is lower than to nor-
mal unaffected dentin, independent of the type of adhe-
sive used.58,239,281,367,382,383 Additional and extended
acid etching of caries-affected dentin can improve bond
strength, but without reaching the performance on unaf-
fected substrate.20 The lower bond strengths on caries-
affected dentin may be the result of the lower tensile
strength and hardness of the altered substrate.367,382
The hybrid layer of adhesives on caries-affected dentin
is usually 5 to 7 μm thicker and less homogeneous than
those produced on sound dentin.383
Human or bovine teeth?
Due to the often inadequate availability of human
teeth and the increased awareness of infection haz-
ards, 162,261 bovine teeth are used in many in vitro
studies. Bovine teeth may be considered a suitable
Vol 12, No 5, 2010
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t fo tests for
alternative to human teeth in bond strength
r P pos-
by N
primary dentition.166 While bovine coronal dentinub
Q ui
sesses wider dentinal tubules 90,202 lica
and thicker peritu-
bular dentin,90 it gives bond strength values similar totion
human permanent dentin.284 Bovine roott edentin
ot
n
ss e n cand
fo re
dentin near the pulp produce bonding results different
from human substrate.284 To compare in vitro adhesion
and cytotoxicity test data, the permeability character-
istics of human and bovine dentin must be similar. An
experiment using tritiated physiological saline solution
to test hydraulic conductance and diffusional water flux
in human and bovine dentin slices showed bovine den-
tin near the cementoenamel junction to be a suitable
alternative to coronal human dentin.285
Despite the applicability of bovine teeth in certain ex-
periments, their larger mean tubule diameter (4.0 μm),
lower tubule density (approximately 17,100 tubules/
mm2) and smaller average apatite crystallite radius (22
to 23 nm),270 bovine teeth cannot be recommended for
micromorphological investigations.
Recently, SEM observations showed that porcine teeth,
too, could be a potential substitute for in vitro tooth adhe-
sion investigations.181
Cavity Preparation
The most common instrument for clinical cavity prepa-
ration is the rotary bur. Although less often employed,
alternative methods are available to the dentist, such
as chemomechanical caries removal,130,184 laser abla-
tion,45,53 or air abrasion.290,374
Each of these methods has a distinctive influence on
the dentin/enamel surface conditions,374 which must be
considered for the selection of the corresponding adhe-
sion technology and the adhesive system. Mechanical
tooth preparation with a rotary bur affects surface rough-
ness, as well the thickness and the density of the smear
layer. The variables in this case are type of bur (steel, dia-
mond, tungsten carbide), roughness or grit size of the bur,
as well instrument rotation speed. Several investigations
of different adhesive systems have shown these vari-
ables to influence bond strength to dentin and enamel.
Self-etching adhesives gave higher bond strengths when
dentin surfaces were prepared with tungsten carbide
burs,83,377 and adhesives performed significantly better
when a smaller grit size was used to prepare the dentin
surface.101,214,288
The result of air abrasion depends on the type of abra-
sive and on the applied air pressure. Air abrasion with
glass beads significantly decreased the bond strengths
to enamel and dentin, whereas use of alumina lowered
adhesion to enamel but not to dentin.204 Other investiga-
tors found no negative influence on enamel adhesion by
air abrasion.289
Cavity preparation with the commonly employed Er:YAG
laser does not create a smear layer, yet no discernible differ-
ence in adhesion compared to bur prepared or air-abraded
substrate was found.45,307 In contrast, Er,Cr:YSGG laser
irradiation adversely influenced the bonding efficacy of
adhesives to dentin.53,317
349
Salz and Bock
Caries may be removed by a chemomechanical ap-
proach using the sodium hypochlorite-based Carisolv
(Mediteam; Göteborg, Sweden). This sodium hypochlorite
formulation partially decomposes the denatured collagen
found in carious dentin. As the presence of collagen fibrils
is essential for hybrid layer formation, excessive collagen
dissolution may jeopardize adhesive performance. Stud-
ies using Carisolv for caries removal showed conflicting
effects on dentin adhesion: while some studies obtained
positive results,130 others observed no effect49 and even
a significant decrease of shear bond strength to primary
dentin using a self-etching adhesive.141 In contrast, the
application of Carisolv to permanent dentin did not influ-
ence the shear bond strength.141
For laboratory in vitro studies, tooth surfaces are usu-
ally prepared by (water) wet grinding with abrasive papers
of different grit size. Dentin shear bond strength values
are not notably affected by the type of abrasive paper, for
example, silicon carbide or aluminum oxide.187 Grit size,
however, does influence the thickness and density of the
smear layer, which is relevant for the bond strength of self-
etching adhesives, as some systems do not fully dissolve
and hybridize thick smear layers, which may result in low
bond strength values.163
Tooth Bleaching
In the past few years, esthetic tooth whitening using
hydrogen peroxide or carbamide peroxide (10% to 35%)
has become increasingly popular. Recent studies have
shown that peroxide bleaching agents adversely af-
fect the bond strength of composites to acid-etched
enamel, the effects becoming more pronounced with
longer contact times and rising peroxide concentra-
tions.85,316,338,341 This reduction in bond strength may
be due to peroxide-induced structural changes in the
surface morphology, but the main reason seems to be
polymerization inhibition by oxygen liberated from ad-
350
pyrig
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t fo
rP
by N
ub
Q ui
lica
tio
te ot n
n
ss e n c e
fo r
Fig 3 Test setup for the application
of pulpal pressure.279,280
sorbed peroxide.50 An interval of at least one week be-
tween whitening treatment and adhesive application is
required before enamel bond strength returns to values
obtained for unbleached enamel.24,57 This interval may
be avoided by removal of the surface enamel layer prior
to bonding,68 or application of antioxidants, eg, ascorbic
acid197 or sodium ascorbate,171 after bleaching.
Simulation of Pulpal Fluid Flow
The simulation of in vivo conditions may be refined by
applying hydrostatic intrapulpal pressure to the pulp
chamber of extracted teeth during adhesive application
(Fig 3).2,140,194,203,224,247,251,279,280 The dentin surface
for adhesive treatment is provided by occlusally remov-
ing the crown, after which the pulp chamber is opened
by removal of the roots. The obtained tooth disk is
mounted with the occlusal surface up onto a Plexiglas
support. The pulp chamber is connected to a liquid res-
ervoir by a tube spliced with a glass tube. An air bubble
is injected into the tube just in front of the glass tube
and the liquid reservoir is raised above the tooth disk
to generate the desired hydrostatic pressure. Fluid flow
through the tooth disk may be measured via movement
of the air bubble in the glass tube. Generally, the pres-
ence of a smear layer reduces fluid flow, whereas phos-
phoric acid etching increases it.260 After appropriate
dentin surface preparation of the mounted specimen,
the adhesive and composite are applied against the de-
sired fluid pressure. To simulate dentinal liquor, distilled
water or saline have often been used,194,247,251 which
resulted in decreased bond strength due to dilution of
the adhesive and/or formation of a water layer on the
adhesive layer. The degree of bond strength reduction
was found to depend on the adhesive.2,140 Among those
tested, HEMA-based adhesives showed the largest
reduction in bond strength from pulpal pressure appli-
cation.182,279,280 When dentinal liquor was replaced by
The Journal of Adhesive Dentistry

bovine serum, Nikaido et al203 showed that no decrease
in bond strength occurred. Apparently, the adhesives’
acidic monomers led to intertubular protein precipita-
tion and reduced dentin permeability. Pameijer et al224
confirmed these results by comparing the adhesion of
vital and nonvital teeth, where no statistically significant
difference between the two substrates was observed.
When interpreting data from in vitro studies simulating
pulpal liquid flow, one must consider that dental restora-
tions are commonly placed under local anesthesia. Sev-
eral investigations158,219 showed that local anesthetics
containing vasoconstrictors, such as epinephrine or fely-
pressin, lower pulpal blood flow and thus pulpal fluid flow.
However, Harnirattisai et al132 recently published a study
in which non-anesthetized patients or patients receiving lo-
cal anesthetics with vasoconstrictors received restorative
treatment. In the study, occlusal cavities were prepared
on maxillary premolars scheduled for extraction, treated
with an etch-and-rinse adhesive (Adper Single Bond, 3M
ESPE) or a two-component self-etching adhesive (Clearfil
SE, Kuraray) and filled using a composite filling material
(Z250, 3M ESPE). Once extracted, the teeth were investi-
gated for microtensile bond strength and compared to a
third group prepared in an in vitro experiment. Although
the bond strength of both adhesives applied in situ were
significantly lower than those in vitro, no significant differ-
ences between the anesthetized and the nonanesthetized
groups for either type of adhesive were detected.
Previous Provisional Cementation
Prior to the final indirect restoration, provisional restora-
tive materials are often used to protect the dentinal
wound and the pulp, as well as to fulfill patients’ es-
thetic and functional needs. However, temporary resto-
rations may negatively affect the subsequent permanent
restoration by depositing residues of provisional filling
material or luting cement.
Zinc oxide provisional cements are considered critical
to subsequent adhesive restorations due to their content
of eugenol. Eugenol, like other phenolic derivatives, is
known to inhibit radical polymerization and can thereby
reduce bond strength of the final adhesive cementation.
The effects of eugenol-containing provisional cements on
subsequent adhesive restoration have prompted much
debate. Some investigators found such provisional ce-
ments to adversely affect bond strength56,372 and pro-
mote microleakage.373 In other investigations, however,
no such effects on bond strength100,244 or marginal ad-
aptation of the final restoration were observed.240 A third
set of authors concluded that provisional restorations
reduced bond strength compared to an untreated control,
but failed to distinguish between eugenol-containing and
a eugenol-free provisional cement.56,109,116
Remnants of provisional restoratives may be removed
from dentin and enamel by several products with different
composition. Saraç et al276 even found a positive effect
of dentin-cleaning agents on resin cement bond strength
to dentin. Two of the investigated products (Sikko Tim
[Voco], mixture of ethyl acetate, acetone, and 2-propanol;
Consepsis Scrub [Ultradent], polishing paste containing
Vol 12, No 5, 2010
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2% chlorhexidine) led to slightly increasedt bond
for strength
by N
of the subsequently placed etch-and-rinse adhesivePu sys-
bli
Q ui
tem and an adhesive resin cement. cat
ion
te ot
n
Cavity Cleaning and Disinfection ss e n c e
fo r
The use of antibacterial agents during any stage of cav-
ity preparation has been recommended to reduce the
risk of recurring bacterial infections. However, there is
serious concern about the influence of cavity disinfect-
ants on the efficacy of dentin bonding agents. The most
commonly used cavity disinfectants are chlorhexidine,
benzalkonium chloride, hydrogen peroxide, and sodium
hypochlorite (NaOCl). Further contributions to the overall
level of biocide concentration may arise from the biofilm
suppressors in dental-unit water systems.30,335,358
The disinfection of enamel and dentin prior to adhesive
application with chlorhexidine and benzalkonium chloride
showed no negative influence on marginal seal,342 un-
less the antimicrobial agent was applied with a scrub-
bing motion.222 Application of chlorhexidine in concentra-
tions up to 2% did not interfere with microtensile bond
strength.102,300 Generally, etch-and-rinse adhesives seem
less sensitive to disinfection of enamel and dentin than
self-etching systems.94
The ability of NaOCl to dissolve collagen has been rec-
ognized for some time.67 As dentin adhesion relies on the
formation of a hybrid layer, ie, a network of collagen fibrils
and polymerized adhesive,200 it follows that exposure to
NaOCl can affect dentin bond strength.170,264,275 The ef-
fect of 6% NaOCl on dentin bond strength correlated with
application time and type of dentin. While a 15-s NaOCl
treatment of caries-affected dentin significantly improved
the microtensile bond strength of two self-etching adhe-
sives, a 30-s exposure had no positive effect. On sound
dentin however, 15-s exposure to NaOCl had no discern-
ible effect on the microtensile bond strength of either self-
etching adhesive, whereas 30-s treatment significantly
lowered bond strength.328
Cavity disinfection by ozone28 prior to restoration
placement showed no adverse influence on microten-
sile bond strength to enamel or shear bond strength
dentin.51,286
Pre-cementation Use of Desensitizer
Prior to the cementation of provisional restorations,
dentists often use desensitizers to avoid postoperative
sensitivity until adhesive placement of the final restora-
tion. Hypersensitivity is usually attributed to the pulpal
nerve response to pressure alterations from fluid flow in
dentinal tubules (hydrodynamic theory).39,229 Fluid flow
may be induced by osmotic pressure, or thermal and
mechanical factors. Proper sealing of the tubules is the
key factor to preventing fluid movements and thus post
operative sensitivity.65,227
The most common approaches to reduce permeability
and sensitivity of exposed dentin are precipitate-forming
agents, eg, potassium oxalate, and protein coagulants,
eg, glutaraldehyde.227,287
Several investigations on glutaraldehyde-containing
desensitizers, eg, Gluma Desensitizer (Hereaus Kulzer,
351
Salz and Bock
Fig 4 Guillotine jig for evaluation shear bond strength.
Germany) or Systemp.desensitizer (Ivoclar Vivadent,
Liechtenstein) found no negative influence on dentin bond
strength.12,142,289,306
Pre-bonding

TUBUF

TUPSBHF
DPOEJ-
As an alternative to desensitizer application, dentin
may be sealed immediately upon tooth preparation by
application of an adhesive, occasionally combined with
flowable resin composites. This so-called pre-bonding
technique claims to offer effective bonding between the
resin-coated dentin and the final adhesively luted indi-
rect restoration for up to several months of placement
of the provisional restoration.
The application of a self-etching dentin bonding sys-
tem and a flowable resin composite to dentin significantly
improved the microtensile bond strength of luted indirect

DPNQPTJUJPO

MPU
OVNCFS

FY-
restorations.152,205,206,218 Sealing dentin with a three-step
etch-and-rinse or a two-step self-etching adhesive prior to
impression making resulted in microtensile bond strength
similar to that obtained with a freshly placed adhesive.
Bond strength was not affected by intervals of up to 12
weeks until placement of the definitive restoration.182
General Recommendations Regarding Substrate and
Sample Preparation
To provide data which are as dependable as possible in
a highly technique-sensitive environment, investigators
are strongly encouraged to respect the following points:
r

6TF
GSFTI
NBUFSJBMT
XIFSF
QPTTJCMF
r

5P
NJOJNJ[F
PQFSBUPS
JOGMVFODF

POMZ
POF
QFSTPO

Adhesive performance on enamel and dentin may be
should prepare the specimen for each sample group
and describe any noteworthy manual skills or appli-
ances employed.
r

5IF
JOWFTUJHBUJPO
TIPVME
JODMVEF
BO
BQQSPQSJBUF
iHPME


standard” product as internal reference.
352
pyrig
No Co
ht
t fo
rP
by N
ub
Q ui
lica
tio
te ot n
n
ss e n c e
fo r
Fig 5 Different configurations to apply shear forces, top the
notched rod, bottom the knife edge.
The following factors can have a significant impact on
experimental data and should be described as accu-
rately as possible:
r

4VCTUSBUF
QSPDFTTJOH
PSJHJO
tions of substrate; storage medium, preservatives
used and their concentration; age group of donors;
any known and noteworthy pre-treatment; embedding
resin and embedding technique (eg, use of vacuum,
pressure pots, curing at elevated temperatures).
r

4VSGBDF
QSFQBSBUJPO
DBWJUZ
PS
TVSGBDF
QSFQBSBUJPO

techniques, apparatus and materials employed (eg,
size, material and speed of burs; cavity geometry,
bevelling of enamel; grinding technique, type and grit
size of abrasive paper; use of water irrigation).
r

.BUFSJBMT
CSBOE
OBNF
piration date, storage duration and conditions before
use; appearance and pre-use treatment where note-
worthy or deviant from routine (eg, agitation, mixing
steps and ratios).
TEST METHODS
Bond Strength Measurement
Bond strength testing remains one of the key aspects
used to screen new products and study the influence of
experimental variables.
Macro and micro bond strength methods
quantified using several methodologically distinct ap-
proaches,48 roughly divided into macro or a micro setups,
depending upon the size of the bonded area. The macro-
bond strength, ie, with a bonded area larger than 3 mm2,
can be measured in shear or tensile mode, or using a
push- or pull-out protocol.
The Journal of Adhesive Dentistry

Composite
Interface
Over the last two decades, most peer-reviewed scien-
tific articles published made use of macro test methods,
so that much of the available data on dental adhesion is
derived from mechanical tests of large bonded areas.40
However, since 1995, the use of macro test methods in
scientific publications has been somewhat eclipsed by
the micro test methods, especially the microtensile bond
strength test.40
Macroshear bond test
For its unrivalled ease and speed of use, the shear bond
strength technique remains the most commonly used
macro bonding test method.48 A composite cylinder with
a diameter of about 3 or 4 mm is polymerized onto a flat,
ground enamel or dentin surface after application of the
adhesive system. Following specimen preparation, testing
is usually carried out immediately, after 24 h, or after up
to several months of water storage at 37°C. For testing,
the composite cylinder is sheared off by application of a
force parallel to the tooth surface.
To standardize the test protocol, special jigs have been
prepared; the device recommended by ISO/TS 11405 (Fig
4) is referred to as a “guillotine”.147 An alternative setup
for shear bond strength evaluation, widely used in North
America, is the “Ultradent jig”, employing a composite
cylinder 2.37 mm wide.153
Several different configurations are used to exert shear
force, including wire loops, notched chisels, and knife
edges (Fig 5). The test assembly has great influence on
stress distribution and is an important source of vari-
ability in shear bond measurement. A knife-edge chisel
causes severe stress concentration at the load applica-
tion area, whereas the wire loop and the notched chisel
render a more even stress distribution at the edge of the
bonding area.73
Peak stress during application of force by blunt knife
edges (Fig 5, below) may explain the frequently observed
Vol 12, No 5, 2010
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t fo
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by N
ub
Q ui
lica
tio
te ot n
n
ss e n c e
fo r
Fig 6 (left) Schematic drawing of the push-out test.
Fig 7 (right) Schematic drawing of the tensile bond strength
test with a conical composite plug.
cohesive composite failure close to the loading point.357
For the same reason, blunt knife-edges may induce the
statistically lower bond strength compared to the Ultradent
notched chisel (Fig 5, above) and the wire loop.84,234,297
Overall, the improvement of adhesive performance over
the last couple of years has led to an increased incidence of
cohesive failure in dentin during shear bond tests.22,64,173
Such cohesive failures led to the misconception that the
interface can withstand the shear forces and adhesive
performance is beyond improvement. However, it was dem-
onstrated that cohesive failure of the tooth, composite, or
mixed failure of both is an intrinsic side effect of shear
bond testing. Upon application of a shear load, stress
distribution in the tooth/adhesive/composite interface is
highly inhomogeneous, resulting in stress peaks that initi-
ate monolithic fracture in enamel, dentin or the compos-
ite.73,355 Additionally, recent studies revealed a positive
correlation between dentin shear bond strength and flexu-
ral modulus of the composite used.337,353 Surprisingly, ad-
hesives’ bond strength are often tested using a composite
by the same dental company, assuming that the composite
was fine-tuned to the adhesive (or vice versa). While this
may be true to a certain extent, comparative bond strength
tests are possible only at the level of identical adhesive/
composite combinations, and certainly not at the level of
the adhesive alone.
Push-/pull-out test
A test in which shear forces also are applied to the sub-
strate is the push-out test, shown in Fig 6.360 An advan-
tage of the push-out test is that marginal adaptation via
SEM analysis and bond strength can be evaluated with
the same test specimen. The test’s drawback is that
minor degrees of composite swelling upon water storage
can induce a significant amount of friction, independent
of adhesive performance.
353
Salz and Bock
80
70
60
50
Adper S E P lus
MP a 40
Adper S E 2
30
S B MP
20
10
0
s hear tens ile micro s hear micro tens ile
Fig 8 Bond strength of three adhesives measured with the
four different methods, shear, tensile, microshear, and micro-
tensile.
The push-out approach has also been employed to dy-
namically test the fatigue resistance of adhesive/dentin
interfaces.88 However, it was never adopted as a universal
bond strength test method. This method, supplemented
by a pull-out approach, appears to be useful to test the
retention of posts luted in root canals.55,127,220,385
Macrotensile bond test
In contrast to the shear bond strength test, a more
even stress distribution is associated with tensile bond
strength methods. Tensile force may be exerted on com-
posite cylinders polymerized onto the tooth surface using
chucks, or conical composite plugs employed instead of
cylinders (Fig 7).195
From 1991 to 2001, the macrotensile bond strength
test was used almost as frequently as the macroshear
bond strength test.40 Nowadays, the macrotensile bond
strength approach is less common, although it is still an im-
portant means to measure bond strength to hard restora-
tive materials such as ceramics and metal alloys.3,156
Micro bond strength methods
One of the incentives for micro bond strength tests was
their ability to evaluate the effect of local tooth structure
on bond strength,213,246,252,291,295 and to allow depth
profiling of different substrates. Both tensile246,271,295
and shear143,246 bond methods have been used for this
purpose.
While microshear and macroshear tests usually yield
similar bond strength values, microtensile bond strength
tends to be up to four times greater than corresponding
macrotensile data. Braga et al40,41 compared three dif-
ferent adhesives (Adper SE Plus, Adper Single Bond 2,
Scotchbond Multipurpose, all 3M ESPE) using all four
bond strength test methods (Fig 8). Among the methods
assessed, microtensile bond strength was most apt to
differentiate between the adhesive.
354
pyrig
No Co
ht
t fbond
A theoretical explanation for the higher or strengths
by N
derived from micro methods is given by the Griffith
Puequation.
bli
Q ui
 
åååå

cat
Cf = 2 E G
ion
te ot
n
PCo ss e n c e
fo r
where Cf = fracture strength, E = plane-strain elastic mod-
ulus, G = surface energy per unit, and C0 = starter crack
size.
The Griffith equation relates applied nominal stress
and crack length at fracture, thus describing the onset of
energetic preference for crack growth. As the probability
of critically sized and correctly aligned defects correlates
to the bonded area, the equation predicts higher energy
per unit to fracture micro samples than macro samples.
Microshear bond strength
Finite element analysis (FEA) of shear force application
revealed the tensile component at the load application
site to be the main cause for fracture initiation. Accord-
ing to FEA, results are also influenced by the highly non-
uniform stress distribution, which consequentially leads
to severe underestimation of the true local stress the
specimen was subjected to at fracture.355,357
Nonetheless, microshear bond strength testing re-
mains a useful method for brittle substrates, eg, glass
ionomers or enamel, that are particularly susceptible to
preparation artefacts such as those that accompany the
microtensile bond strength method, for instance.
Microtensile bond strength
The microtensile bond strength method (μTBS) has
become the scientifically most widely accepted and
therefore the most frequently employed test setup for
measuring bond strength to dentin.18,145,231
The microtensile bond strength method was introduced
by Sano et al in 1994.271 It was observed that tensile
bond strength is inversely related to bonded surface areas
of 0.25 to 12 mm2 and that the cross-sectional bonded
area and the failure mode correlate. Below 2 mm2, all
the test specimens failed adhesively at the interface. In
a follow-up publication, Pashley et al231 summarized the
versatility of microtensile methods over conventional ap-
proaches, as shown in Table 2. The method’s advantages
are somewhat diminished by its labor intensity, demand
of technical aptitude, and the fast dehydration of small
samples during handling.
For sample preparation, as shown in Fig 9, the adhe-
sive is applied to prepared dentin and a large composite
plug incrementally polymerized onto the adhesive. After
the desired storage duration, this assembly is sectioned
using precision circular saws into 1-mm-thick slices, which
are then cut into sticks of about 1 mm by 1 mm. To further
improve stress distribution, some approaches trim such
sticks to dumbbell or hourglass shapes (Fig 10). It was
observed that stick- and dumbbell-shaped specimen with
rectangular bonded areas show similar bond strength and
failure modes.29,250,283
Sawing and trimming of the test samples appears to
be the most technique-sensitive part of the microtensile
The Journal of Adhesive Dentistry
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Table 2 Advantages and disadvantages of the μTBS test according to Pashley et al230 t fo
rP

by N
ub

Q ui
Advantages Disadvantages lica
tio
te n ot

n
1. More adhesive failures, fewer cohesive failures 1. Labor intensive, technically demanding ss e n c e fo r
2. Higher initial bond strengths 2. Difficult to measure bond strength < 5 MPa
3. Permits measurements of regional bond strengths 3. Requires special equipment
4. Means and variances can be calculated for single teeth 4. Samples are so small that they dehydrate rapidly
5. Permits testing of bonds to irregular surfaces
6. Permits testing of very small areas
7. Facilitates SEM examination of the failed bonds since the
surface area is approximately 1 mm2

1 mm
1 mm

C ompos ite
C ompos ite C ompos ite
10 – 24 mm

Dentin
Dentin Dentin

S tick Dumbbell Hourglas s

Fig 9 Schematic drawing of the sample preparation for micro- Fig 10 Different test specimen shape for microtensile bond
tensile bond strength testing. strength investigation.

bond strength test.18 Interfacial stress during sample
preparation is reflected by the number of pre-test fail-
ures, as often occurs with lower-performance adhesives
or on brittle substrates. SEM analysis of enamel samples
revealed a more frequent occurrence of microcracks com-
pared to dentin samples, with microcracks most often lo-
cated at the sample periphery, as would be expected from
preparation artefacts (see Fig 11).105 The use of a dia-
mond wafering blade resulted in a higher rate of pre-test
failures than sectioning with a diamond wire (35.4% for
enamel and 18.2% for dentin).266 For these reasons, mi-
crotensile bond strength testing has been questioned as
an appropriate method to test adhesion to enamel.105
Since specimen geometry significantly influences
stress distribution, samples trimmed to an hourglass
shape differ greatly from dumbbell and stick samples
regarding bond strength, stress concentration, and failure
locations.299 Compared to the stick or dumbbell, hour-
glass samples fail at lower stress, due to the high stress
concentration in the adhesive layer.124,126 The hourglass
geometry appears even more sensitive to microcracks
introduced during specimen preparation (Fig 11).29,124
Reproducible preparation of specimens is difficult, es-
pecially as hourglass trimming places additional pre-test
strain on samples, and deviations in bonded area signifi-
cantly affect stress distribution.299,344
For more uniform stress distribution and reduced sec-
ondary crack formation, microtensile specimens are occa-
sionally lathed to give rounded samples (Fig 12),79,129,145
for instance, using the “MicroSpecimen Former” devel-
oped by the University of Iowa, Iowa City, IA, USA.18 None-
theless, due to lack of consensus regarding specimen
design and the relatively high incidence of pre-test failures
during trimming, some laboratories have recommended
using only the unnotched sticks231 or a “non-trimming”
preparation technique.33
Following sample preparation, test specimens are
mounted on a variety of jig designs using fast-setting ad-
hesives (Fig 13) to standardize sample fixation to the uni-
versal testing machine’s load cell.236,249,271,294,312,381
Regardless of design, jigs must ensure that test speci-
mens are subjected to tensile strain only. Bending forces
during load application can arise from non-parallel align-
ment of the specimen with direction of force and/or un-
even gripping forces, ia.296,355,384 Often, the specimen is
glued to a flat jig surface, even though such devices obvi-
ously complicate proper test specimen alignment.249,384
Specimen alignment may be improved by the V-shaped

Vol 12, No 5, 2010 355

Salz and Bock
C ompos ite
Dentin
Hourglas s
Fig 11 Microcrack formation due to test specimen trimming.
Fig 13 Schematic drawing of the gripping device for measur-
ing microtensile bond strength.
groove parallel to direction of load, as integrated in Geral-
deli’s jig. Later, Ciucchi’s jig was modified similarly for the
same reasons.249 In addition to promoting proper sample
alignment, notched gripping devices reduce the possibility
of glue contamination of the samples.
It is obvious from the description above that micro-
tensile bond strength measurement incorporates an im-
pressive number of methodological variables. The evalu-
ation of microtensile bond strength data for a fixed set
of restorative materials on a specified substrate in dif-
ferent laboratories gave greatly divergent results, and
indicates the challenge of keeping all relevant variables
constant.124,299
Recently, Scherrer et al282,283 carried out a meta study
on publications dating from 1998 to 2009 investigating the
bond strength of resin composite to dentin using four pro-
tocols: shear, tensile, microshear and microtensile bond
strength. Six adhesives were selected covering three-step
systems (OptiBond FL, Kerr-Sybron; Scotch Bond MP Plus,
356
pyrig
No Co
ht
t fo
rP
by N
ub
Q ui
lica
C ompos ite
tio
te ot n
n
ss e n c e
fo r
Dentin
S tick
Fig 12 Chamfered stick test specimen.
3M ESPE), two-step systems (Prime & Bond NT, Dentsply;
Single Bond, 3M ESPE; Clearfil SE Bond, Kuraray) and a
one-step adhesive (Adper Prompt L Pop, 3M ESPE). The
pooled results of 147 references showed high scattering
in the bond strength data regardless of adhesive and test
method. Regardless of protocol, variance was high (20%
to 50%), and even the microtensile bond assessments
included a high percentage of cohesive failures.
Table 3 summarizes the lowest and the highest micro-
tensile bond strength values published for the six adhe-
sives mentioned above. However, it must be considered
that most of the cited publications investigated factors
affecting bond strength, eg, carious substrate or applica-
tion of self-etching adhesives without agitation.
The well-established adhesive Clearfil SE Bond was
used in 77 of the published bond strength investigations
as a benchmark, with bond strengths ranging from 18
to 81.6 MPa. This remarkable spread might lead to the
conclusion that either Clearfil SE Bond is very technique
sensitive, or that bond strength investigation itself is sen-
sitive to a number of preparatory artefacts. In order to
publish data which are as transparent as possible, all
conceivable influential factors must be kept constant and
all observations (eg, pre-test failures) should be reported
in detail.
INFLUENCE OF TEST CONDITIONS
Crosshead Speed
Since composites possess viscoelastic properties, the
speed by which a load is applied to a sample (crosshead
speed) influences results of bond strength tests. The few
studies that evaluated the influence of crosshead speed
on “macro” bond strength unfortunately yielded contra-
dictory results. Watanabe et al364 found no statistically
significant differences between crosshead speeds of 0.5
to 10 mm/min, using a single-plane shear test assembly
(SPSTA) with composite plugs having bonded areas 5 mm
The Journal of Adhesive Dentistry

Table 3 Lowest and highest microtensile bond strength values found in the literature for 6 different
systems (from Scherrer282, 283)
Adhesive Lowest value (MPa)
Adper Prompt L-Pop 5.2 ± 6.1113
Clearfil SE Bond 18.0 ± 4.78
OptiBond FL 20.2 ± 5.0245
Prime & Bond NT 19.0 ± 3.9113
Scotchbond MP Plus 12.7 ± 2.959
Single Bond 12.5 (?)282,283
?: There may be a mistake in References 282 and 283. The cited reference for the lowest microtensile bond strength of Single Bond is a
shear bond strength investigation.
in diameter. On the other hand, Hara et al131 observed
statistically higher bond strengths for crosshead speeds
of 1.0 and 5.0 mm/min than of 0.5 and 0.75 mm/min
when applying a knife-edge steel rod on 3-mm-diameter
bonded areas. Equally inconsistent results were obtained
for the influence of crosshead speed on tensile bond
strength: whereas some researchers reported data un-
influenced by crosshead speeds from 0.5 mm/min to
5.0 mm/min,321 other authors found statistically higher
bond strength for 5.0 mm/min and 10.0 mm/min com-
pared to 0.1, 0.5 and 1.0 mm/min.221
Only a few investigations have addressed the influence of
crosshead speed on microtensile bond strength.250,256,370
These studies unanimously reported the indifference of mi-
crotensile bond strength to crosshead speeds ranging 0.01
to 10.0 mm/min. According to Yamaguchi et al,370 smaller
microtensile bond strength specimens contain fewer and
more homogeneously distributed internal defects than do
macro test samples. Small samples are accordingly less
affected by the strain rate, which reduces the impact of
speed on bond strength values.
Application Temperature
It is common knowledge that temperature greatly af-
fects many chemical, physicochemical, and physical
properties and processes such as reaction, polymeriza-
tion and transport kinetics, vapor pressure, viscosity,
diffusion, etc. Therefore, several adhesive bond strength
studies9,52,123 have focussed on the temperature influ-
ence, concluding that raised substrate temperature
of up to 40°C during adhesive and composite applica-
tion was beneficial to the outcome of the test. While
intraoral temperatures are ≥ 30°C, for the sake of con-
venience, in vitro investigations are usually carried out
at room temperature or even on refrigerated teeth. In
addition, adhesives may be applied straight out of the
refrigerator, or samples may be stored in cold tap water,
which in winter can be as cold as 10°C. To provide clini-
cally relevant data, investigations where temperature
Vol 12, No 5, 2010
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ub
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lica
Highest value (MPa) tio
t n ot
n
52.0 ± 17.5239 e ss e n c e fo r
81.6 ± 3.535
63.2 ± 15.8278
56.3 ± 11.158
42.6 ± 5.5257
58.5 ± 20.8150
has a dominant effect (eg, initial bond strength, time of
air blowing), substrate temperature should be approxi-
mately 30°C.
Application Protocol
Bond strength and resilience rely on a variety of at-
tributes connected to the hybrid layer, such as hybrid
layer thickness or resin tag formation and length. 180
Hybrid layer formation requires the smear layer to be at
least partially removed or dissolved, followed by mono-
mer infiltration of intertubular and peritubular dentin,
evaporation of solvents, and, subsequently, adequate
monomer polymerization.
Active agitation of self-etching adhesives may improve
adhesion performance by assisting smear layer removal
and contacting the acidic monomers with the tooth sur-
face. Agitation is especially beneficial to two-step and
one-step self-etching adhesives, significantly raising the
shear bond or microtensile bond strength to dentin.86,336
Agitation’s expedient effects are corroborated by de-
creased interfacial silver nitrate deposition for adhesives
applied under agitation.86
Most enamel/dentin adhesives are based on water-
miscible organic solvents to decrease viscosity of the
formulation, compatibilize hydrophobic monomers such
as bis-GMA, and enhance infiltration of tubuli and colla-
gen fibrils. Aqueous alcohol evaporates under azeotrope
formation, thereby helping to reduce the residual water
content of the adhesive layer. Numerous studies con-
firm excessive air drying to be detrimental for high bond
strength112,120,144,336 and good marginal adaptation,112
regardless of the adhesive employed.
Low viscosity adhesives may require the applica-
tion of several layers to maximize microtensile bond
strength.69,298 Despite the fact that a minimum adhesive
layer thickness is required for proper performance, exces-
sive adhesive coating can aggravate bond strength and
the quality of adhesion.69
357
Salz and Bock
C-value --0.2------0.5-----1.0-----2.0------5.0---
Fig 14 Relation between different schematic, rectangular rest-
orations and corresponding C-values.
Cavity Geometry (C-factor)
Years ago, Feilzer et al104 showed that polymerization
stress in composite fillings is related to restoration
configuration. To describe this influential element, the
configuration factor C was defined as the ratio of the
restoration’s bonded to unbonded (free) surfaces (Fig
14). The lower the C-factor of a restoration, the more
likely it is to endure polymerization stress and remain
tightly bonded to the cavity walls. Larger cavities usually
have C-factors greater than one and pose considerable
problems in the preparation of cavities with perfect mar-
gins. Class I and II preparations have mean C-factors
of 4.03 and 1.85, respectively,74 which in part explains
why in vitro bonding to flat surfaces (C < 0.2) usually
surpasses in vivo bond strengths. With the introduction
of the microtensile bond strength method, it became
possible to investigate the influence of cavity size and
composite layering technique on bond strength, confirm-
ing the negative impact of high C-factors. Bulk filling
of cavities with a high C-factor reportedly produced the
lowest microtensile bond strength134,135 and an inferior
marginal seal.366 However, appropriate layering makes
high bond strengths achievable even on deep cavity
floors.134,207
The effect of shrinkage stress is further exacerbated
by hydrolysis during long-term sample storage in water.15
For example, Shirai et al293 found a conventional three-
step etch-and-rinse adhesive to bond most effectively to
dentin, and resist both polymerization shrinkage stress
and water degradation. A two-step self-etching adhesive
was only marginally less effective in adhesive perform-
ance, with bond strength decreasing only slightly within
1 year of water exposure. However, another two-step
etch-and-rinse adhesive and a one-step self-etching ad-
hesive were greatly affected by cavity configuration and
water aging. Surprisingly, bulk-filling Class I cavities with
the low-shrinking silorane-based composite Filtek Silo-
rane, also resulted in significantly decreased microtensile
bond strength compared to layering of the same mate-
rial.345
Long-term Water Storage
Water uptake appears to be one of the main reasons
for long-term in vivo tooth/composite bond degradation.
358
pyrig
No Co
ht
t fo components
Biodegradation of collagen and/or polymer
r P mono-
by N
of the hybrid layer may be related to incomplete ub
Q ui
mer infiltration into the dentin substrate,378 lica
inhomoge-
neous monomer distribution through the interdiffusion tio
t ot n
n
e
zone, insufficient polymerization, alterationss eofnthe
fo r c e or-
ganic matrix by surface preparation, enzymatic collagen
degradation,232 enzymatic polymer degradation,165,226
nanophase separation,310,375 and hydrolysis. The im-
portance of water absorption to bond strength reduction
was demonstrated by comparative sample storage in
water or oil. While storage in oil was associated with
either preserved or increased bond strength,54 water
storage had negative effects on bond strength of dif-
ferent adhesives.16,17,75,110,267,376 Studies using SEM
and TEM to investigate deterioration of the adhesive/
composite interface78,133,311 found unprotected and
partly disrupted collagen fibrils. Tay et al332 observed
water channels and water tree formation at the inter-
face of long-term water stored samples. Micro-Raman
spectroscopy substantiated the elution of unreacted
monomer, which may influence mechanical properties of
the adhesive layer.311
Thermocycling
To evaluate the influence of aqueous conditions on long-
term marginal adaptation or bond strength stability, a
stress test comprising cyclic thermal fluctuations (ther-
mocycling) is often carried out.122 The test specimens
are shuttled between water baths set to 5°C and 55°C
or 60°C for 5000 to 10,000 cycles, with dwell times of
0.5 to 3 min. Due to differences in the thermal expan-
sion coefficients of composite (80 to 120 ppm–K-1) and
tooth substrate (8 to 12 ppm–K-1), thermal stress is
highest at the adhesive interface. Some studies on sin-
gle-step self-etching adhesives found no effect of ther-
mocycling, whereas others observed decreasing bond
strength after thermocycling.1,21,22,76,92 Depending on
the chemical composition of the investigated adhesive,
the interfacial ultrastructure was either unchanged after
up to 100,000 thermocycles, or voids as well as col-
lagen depletion were detected.146 The combination of
long-term water storage and thermocycling was found to
particularly affect Class V enamel margins of single-step
self-etching adhesives.31
Fatigue Tests
Besides water uptake and matrix degradation, the me-
chanical stress of mastication is probably the clinically
most important factor afflicting the tooth/adhesive/
composite interface. Since conventional bond strength
tests do not reflect cyclic subcritical loading,78 fatigue
tests have been developed. 353 Such investigations
may be executed as macro push-out,88,111,262 macro-
shear, 25,88,96,97,98,114,262 microrotary, 77,79,80 micro-
shear,38 micro 4-point bend,313,314 and microtensile
fatigue tests.354 However, despite the comparatively
labour-intensive and time-consuming nature of fatigue
test protocols, they provided little new information on
bonding effectiveness and the long-term in vivo behavior
of dental bonding systems. For example, both microro-
The Journal of Adhesive Dentistry

tary77 and microtensile fatigue testing353,354 revealed
superior bonding effectiveness of a 3-step etch-and-
rinse adhesive over a 2-step self-etching adhesive,
that in turn performed significantly better than a 1-step
adhesive. Additionally, these fatigue tests have largely
been applied to dentin, since enamel’s brittleness im-
pairs assessment of fatigue effects.
Microleakage
Microleakage can be defined as the clinically undetect-
able passage of bacteria, fluids, molecules, or ions
between cavity walls and a restorative material. Polymeri-
zation shrinkage of resin-based restorative materials
induces interfacial stress, which may lead to gap forma-
tion, so that adhesives usually provide only incomplete
marginal sealing and do not fully prevent microleakage.
The detection of microleakage has been attempted
by a variety of methods with considerable variation
of results.139 The most widespread, albeit qualitative
method for leakage detection is dye penetration: the
samples are immersed in dye solution and, after a
certain interval, sectioned to evaluate the extent of dye
infiltration around the restoration. 139 Cyclic thermal
stress may be applied to accelerate aging of the inter-
face as mentioned above. Compared to bond strength
tests, the impact of artificial aging, such as water stor-
age and thermocycling, on microleakage is low.122,359
However, microleakage appears more sensitive to cyclic
mechanical loading,151,167,192 further exacerbated by
additional thermocycling.139
Microleakage can be quantitatively evaluated by meas-
uring the flow of a fluid across the interface.32,81 With
this nondestructive method, specimens may be followed

POMZ
POF

longitudinally, thus increasing the informative value of the
study. However, interfacial leakage values may be falsified
by the often undefined leakage paths and leakage occur-
rence through the dental substrate itself.
Nanoleakage
Using perfusion with silver ions, Sano et al revealed


a new type of leakage between the hybrid layer and
intact dentin in the absence of marginal gaps (na-
noleakage).273 This silver infiltration indicates voids
in the hybrid layer or the demineralized submicron
region that have not been adequately impregnated
by adhesive resin.274 Such voids make the adhesive
layer more susceptible to hydrolytic degradation and


bacterial acids and enzymes. 233 In spite of their
descriptive appearance, leakage studies often lack
appropriate controls,6 and the results often do not
correlate with other data (eg, bond strength). For
these reasons, nanoleakage experiments should be
interpreted with caution.319
Tay et al331 found silver ion uptake to rise in areas
of the adhesive layer with increased permeability. It is
presumed that spots stem from incomplete evaporation
of water, which leads to incomplete polymerization and/
or formation of hydrophilic domains (eg, HEMA-rich hydro-
gels). Due to their polar composition, one-step self-etching
adhesives are especially prone to formation of hydrophilic
Vol 12, No 5, 2010
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and
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ig
No Co
ht
t fo
zones,330,333 forming semi-permeable membranes with
rP
by N
high water permeability. ub
Q ui
lica
Nanoleakage seems to be little affected by thermocy-
cling176 or by cyclic mechanical loading.177 Water storagetion
te ot
n
of the specimens, in contrast, increased nanoleakage,
ss e n c e
fo r
which even correlated well with a decrease in microtensile
bond strength for some adhesives.216,217 Mechanic load-
ing or combined loading and thermocycling also increased
nanoleakage and decreased microtensile bond strength
of current self-etching adhesives.343 Additionally, Saboia
et al265 showed that chemical aging with 10% sodium
hypochlorite (NaOCl) had similar effects in the case of
two-step etch-and-rinse adhesives.
General Recommendations Regarding Specimen
Preparation and Test Methods
Application of materials to the substrate and test pro-
cedure are highly technique sensitive, and experience
shows even minor variations to significantly affect ex-
perimental outcome. Conclusive discussion of results
therefore requires a detailed description of the em-
ployed test method and possible impacts of conceivable
alterations where applicable.
There are several key issues regarding specimen prep-
aration and test methods that investigators are encour-
aged to keep in mind:
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foreseeable interplay of such alterations (eg, use one
composite only, as flexural strength may influence
bond strength).
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solvent evaporation and light curing; age of jig molds;
composite layering technique; environmental factors
conceivably affecting experimental outcome (eg, tem-
perature of samples, use of tap or distilled water or
other liquids; sample storage temperature and dura-
tion).
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ized sample orientation where possible (eg, “crown
down” or grooved microtensile jigs).
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speed of circular saw, wafering blade, automated sec-
tioning protocols and infeed employed. State when
using alternative sectioning methods (eg, wire). De-
scribe accurately any trimming of sticks, apparatus,
and methods employed as well as pre-test failures
during trimming.
359
Salz and Bock
Mode II
Mode I
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where
modes, and their inclusion in the evaluation.
FRACTURE TOUGHNESS
Shear or tensile bond strength tests have been criti-
cized for their uneven interfacial stress distribution,
which is incompatible with determination of nominal
bond strength. For unambiguous adhesion data, a test
method should be employed which tolerates flaws
within the material and the interface, leads to interfacial
failure, and is independent of the test geometry.160
Interfacial material properties, such as crack growth
resistance, are appropriately described by linear elastic
fracture mechanics. Fracture mechanics is well estab-
lished in the engineering community to describe the prop-
erties of monolithic materials and is becoming increas-
ingly common to investigate the interface of dissimilar
materials.71,371
Basics of Fracture Toughness
Fracture toughness relates a loaded sample’s ability
to resist flaw propagation to its mechanical durability.
Flaws appear as cracks, voids, metallic inclusions, weld
defects, design discontinuities, or a superimposition of
the above, and are considered an unavoidable conse-
quence of specimen processing, fabrication, or service
of a material/component. For this reason, flaws must
be expected in at least some components of an assem-
bly and critical components designed by a linear elastic
fracture mechanics (LEFM) approach. This approach em-
ploys flaw size and features, component geometry, load-
ing conditions and fracture toughness to predict fracture
resistance at a flawed site.
Fracture toughness of materials is described by the
stress-intensity factor (K) that combines load, crack size,
and structural geometry. A Roman numeral subscript is used
to indicate fracture mode, as illustrated in Fig 15. Mode I
fracture is the most common mode and attributed to a crack
360
pyrig
No Co
ht
t fo
rP
by N
ub
Q ui
lica
tio
te ot n
n
ss e n c e
fo r
Mode III
Fig 15 The three different modes of
fracture (tensile force, shear force,
torsional force).
plane orthogonal to the highest tensile load. The stress in-
tensity factor is represented by the following equation:
+IS•PAB
S = applied stress [MPa], A = crack length [m], and B =
individual geometry factor.
Differently sized specimens, even when of identical
proportions, give different values for KI, since stress act-
ing adjacent to a flaw of a given size is influenced by speci-
men dimensions (B, Fig 16) up to a critical dimension.
Beyond this critical dimension, the value of KI becomes
a true material property called the “plane-strain fracture
toughness” KIC. The stress intensity KI represents the
level of “stress” at the tip of the crack, and the fracture
toughness KIC denominates the highest stress intensity
a material under plane-strain conditions can withstand
without fracture.10
Fracture Toughness Assessment
The most widely used fracture toughness test configura-
tions are the single edge notch bend (SENB or three-
point bend) and the compact tension test (CT) (Fig 16).
Other specimen configurations include center-cracked
tension (CCT) panels, single edge notch tension (SENT)
specimens, and shallow-crack tests.
Compared with the SENB, compact tension specimens
require less material, but involve more labor to machine
and are more complex to test. Also, special requirements
are needed for temperature control (eg, use of an envi-
ronmental chamber). SENB specimens are typically im-
mersed in a bath for low temperature tests. After intro-
duction of a sharp fatigue notch, the specimen is loaded
to failure and the force required for crack propagation
determined to render fracture toughness.10
Employment of Fracture Toughness Tests to Enamel/
Dentin Adhesives
Criticism regarding bond strength testing and the
demand for a linear elastic fracture mechanics ap-
proach73,355,356 were addressed at the annual ADM
meeting in 2009. 282,283 At this meeting, Söder-
holm304,305 gave an extensive review of fracture me-
chanics and the relation of fracture toughness to
The Journal of Adhesive Dentistry

S E NB S pec imen C T S pecimen
F /2 F /2 F
S pan = 4W
a a
B
W = B or 2B
W
B
F F
Fig 16 Common fracture toughness test specimen types.
specimen geometry, load application, and other param-
eters (eg, speed, temperature).
A loaded adhesive joint is usually composed of differ-
ent materials, each exhibiting different mechanical prop-
erties, such as Young’s modulus (E), shear modulus (G),
Poisson’s ratio (N), yield strength, fracture strength, strain
in uniaxial tension, and pure shear. Due to the differences
in mechanical properties, the stress distribution between
the joint components follows complex patterns. In vitro
analysis of dental adhesives is further complicated by
residual polymerization stress, inhomogenity of the tooth
substrate and interface (adhesive layer, hybrid layer, prism,
tubule orientation etc). Even tensile stress distribution
occurs only if none of the involved components deforms
laterally under tension, or if the same deformation results
from tensile stress applied orthogonally to the adhesive.
Equal lateral deformation requires an identical relation-
ship of Poisson ratio N to Young’s modulus E (“N:E”) for
all components of the adhesive joint. If this condition is
not met, the dissimilar lateral deformation of the adhe-
sive joint components gives rise to crack formation and
propagation.
Of the components involved in tooth/adhesive/com-
posite specimen, the adhesive usually shows the highest
N:E. Therefore, assuming the interfaces remain intact, the
adhesive adjacent to the more rigid adherents is put un-
der a greater lateral strain than if it were allowed to strain
freely. That behavior leads to complex stress distribution
patterns within the adhesive layer, and sets the stress dis-
tribution in multicomponent specimens completely apart
from that of homogeneous monolith.
Based on extensive theoretical considerations re-

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holm304,305 came to the following conclusions:
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to induce fracture by crack growth. In other words,
an adhesive joint does not fail instantaneously, but
rather because a crack propagates from a locally
overstressed area.
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material properties, such as GC (fracture energy or
critical strain energy release rate, J/m2) and KIC (frac-
ture toughness) and can be used to compare differ-
Vol 12, No 5, 2010
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and
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ht
t fo
rP
by N
ub
Q ui
lica
tio
te ot n
n
ss e n c e
fo r
Fig 17 Single edge notch bend test specimen used by Toparli
and Aksoy.340
ent materials. Of these two parameters, GC relies on
thermodynamic deductions, while KIC is derived from
a purely mechanical approach. While the thermody-
namic approach to GC relies on the description of en-
ergy exchange, the mechanical approach is defined
by stress conditions, often under the assumption
that the material is truly elastic.
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mechanism of adhesives. If the crack is adjacent or
very close to an interface, the different failure modes
will contribute to crack propagation.
r

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BO
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on stress distribution complicates the determination
of K.
r

5IF
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GBDUPS B, used to determine the KIC
value, is a function of the ratio of the moduli Ea:Es (Ea
= Young’s modulus adhesive, Es = Young’s modulus
substrate) and the thickness of the adhesive layer,
ha. It is also dependent on the overall geometry of
the joint.
r

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,
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(C,
and vice versa, by using the appropriate modulus
value. For an adhesive joint, however, this conversion
requires the knowledge of the modulus of that adhe-
sive joint, which may be unknown.
r

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ture experiment. The more brittle an adhesive is, the
more important a sharp crack initiation becomes for
determining GC or KC.
r

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(C or KC values of tough adhe-
sives more than brittle adhesives.
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may affect plastic deformation at the crack tip, which
in turn influences GC or KC values. In other words, a
plastic-elastic fracture mechanics approach may be
more appropriate than a linear elastic approach.
Fracture Toughness Testing of Enamel/Dentin Adhesives
A MedLine literature search of publications prior to May
2009 querying “dental adhesion testing AND enamel
OR dentin AND fracture toughness” yielded a total of 61
articles.282,283 A remarkable number of different test
setups (listed below) have been used:
361
Salz and Bock
1. Single edge notch bend test: Toparli and Aksoy340
investigated the single edge notch bend test (SENB,
Fig 17) to determine fracture toughness of composite
resin and dentin/composite resin adhesive inter-
faces. Single edge notch bars have also been used
by Khajotia et al.157
2. Short Rod Chevron Notch: Fracture toughness of
dental adhesives is most commonly tested with the
short rod chevron notch approach. Tam and Pilliar
conducted the first fracture toughness investigation
of dentin/composite interfaces in 1993. 322 Later,
Tam et al323-327,361 used a test setup where a 7 x 4 x
0.75 mm dentin disk was covered with composite. To
prepare samples, a chevron-shaped area is blocked
out by placing an appropriate mask on the exposed
dentin. The adhesive is then applied to the exposed
dentin and light cured; subsequently, a composite
cylinder is polymerized onto the adhesive via a mold
placed on top of the blade. After removal of the mold
and blade, a cylindrical chevron notch specimen is

JODMVEJOH
UIPTF
CZ
UIF
TBNF
SF-
obtained. Armstrong et al13,14 Lin and Douglas,178
and Ruse et al103,148,263 also used short rod chevron
notch tests, but employed rectangular specimens (Fig
18). The rectangular specimen of Armstrong et al13,14
consists of a dentin monolith bonded to a composite
monolith. The chevron notch can be introduced prior
to polymerization using adhesive tape to appropri-
ately block the dentin surface,178 or after polymeri-
zation by sawing on the dentin/composite boundary
(Fig 18). Ruse et al103,148,263 used prismatic dentin/
composite specimens affixed to a split metal cylinder,
which was attached to the universal testing machine.
3. Critical plane-strain energy release rate: Versluis et
al357 postulated fracture toughness of adhesives to
be superior to conventional strength measurements
in evaluation of adhesive properties. To validate
that claim, Tantbirojn et al329 compared six dentin
bonding agents subjected to the nominal shear bond
strength test or to the interfacial fracture toughness
test (critical plane-strain energy release rate) (Fig
19). The critical plane-strain energy release rate, GIc,
was calculated according to the following formula as
a function of specimen shape and elastic material
behavior.62
4. Critical plane-strain energy release rate
104.5 (F max)2 L3
GIc(J/m2)= ED6
where Fmax = load at failure, L = distance to loading
point, E = elastic modulus of composite cylinder, and
D = diameter of the composite cylinder (4 mm).
The composite cylinder bonded to the dentin surface
was 11.0 mm long and 4.0 mm in diameter. The notch
was stencilled by placing adhesive tape with a chevron de-
sign on the dentin surface before composite placement.
The notch distance a0 was 0.6 mm, and the angle GTH 90
degrees (Fig 19). The load was placed 9.5 mm from the
dentin surface with a load rate of 0.5 mm/min.
362
pyrig
No Co
ht
t fo
Fracture Toughness Studies of Dental Adhesives
r Padhesives
by N
Studies of the fracture mechanics of dental u
as follows: blic
Q ui
were reviewed by Söderholm 282,283
ati
te BEIFTJWFT

ot on
n
r
5IF
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ss e n c e
fo r
is limited, and were mostly performed using different
test setups, sample geometries, and loading rates.
r
4PNF
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PO
EFOUJO
BEIFTJWFT
QSFTFOU

results in fracture energy G, whereas others use frac-
ture toughness K.
r
4&.
TIPXT
GSBDUVSF
NFDIBOJDT
TQFDJNFOT
UP
NPSF

dominantly exhibit adhesive failure than do shear
bond specimens.
r
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NFDIBOJDT
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NPTU
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GBJM
BU

the interface of the hybrid layer and adhesive resin.
Fracture tendentially converges on the dentin surface
with increased aging in aqueous conditions.
r
5IF
GSBDUVSF
UPVHIOFTT
WBMVF
SFNBJOT
SFMBUJWFMZ
DPO-
stant during aging.
r
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search group, render fracture toughness values of
1 to 2 MPa–m½, with high standard deviations often
exceeding 25%.
r
0OMZ
POF
TUVEZ
IBT
DPOTJEFSFE
UIF
DPNQMFYJUZ
PG
BO

adhesive joint, such as polymerization shrinkage
stress. All the other studies assumed a linear-elastic
approach valid only for a material lacking interfaces.
r
5IF
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OBUVSF
PG
TBNQMF
QSFQBSBUJPO
NJHIU

explain the limited number of available fracture me-
chanics studies.
Recommendations for Fracture Toughness
To meaningfully estimate an adhesive’s performance by
fracture toughness or the fracture energy, the following
requirements must be met.
r
$MJOJDBM
SFMFWBODF
PG
GSBDUVSF
EBUB
NVTU
CF
QSPWFO
TV-
perior to shear bond strength measurements.
r
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BOE
UIF
UFTU
TFUVQ
OFFE
UP
CF

less complex, labor intensive, and error prone than is
currently the case.
r
0OF
VOJGPSN
HVJEFMJOF
GPS
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PG
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FYQFS-
imental conditions should be agreed upon. Ideally, a
standardized version of sample holder, jig, and mold
should be made commercially available.
r

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with low standard deviation.
r

$MJOJDBMMZ
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distin-
guishable.
CONCLUSION
To conclusively test material properties in the devel-
opment and product quality assurance of dental ad-
hesives, reliable laboratory methods are required.
However, the validation and reproducibility of hitherto
available approaches to testing dentin or enamel adhe-
sion suffer from the unstandardizable nature of the sub-
strates. Dental hard tissue is structurally anisotropic
The Journal of Adhesive Dentistry

Fig 18 Short rod chevron notch bend test specimen used by
Armstrong et al.13,14
and, in terms of micromorphology and composition, re-
flects a number of factors, such as location and patient
age and health status. To simulate clinical situations,
restorations can be placed in teeth destined for extrac-
tion and subsequently investigated in the laboratory. In
vivo placement of adhesives reproducibly lowered bond
strength on dentin compared to in vitro investigation,
although the effects showed a certain dependency on
the employed adhesive. In vivo conditions in extracted
teeth may be simulated by application of hydrostatic in-
trapulpal pressure to the pulp chamber during adhesive
placement.
In vitro and in vivo performance of dental adhesives may
be affected by two groups of factors. The “substrate group”
includes the substrate itself, its storage and pre-treatment
(eg, cavity preparation, tooth bleaching, previous provisional
cementation, cavity cleaning, disinfection, desensitizing
treatment) and the “method group”, including methods
and conditions of adhesive application, sample storage,
and pre-treatment (storage medium, long-term loading,
thermocycling) and measurement protocol (eg, knife/sam-
ple holder geometry, cross-head speed). For its unrivalled
ease and speed of use, shear bond strength measurement
remains the most common method, whereas the more
laborious tensile bond strength measurement offers more
evenly distributed stress.
Both methods may be carried out on “macro” and “mi-
cro” samples, where bonded areas > 3 mm in diameter
define macro methods. While more difficult to prepare,
micro methods allow evaluation of local tooth structure
effects on bond strength and depth profiling of different
substrates. While microshear and macroshear tests usu-
ally give similar bond strength values, microtensile values
tends to be two to four times higher than corresponding
macrotensile data. A general point of criticism of shear or
tensile tests is the uneven interfacial stress distribution
during loading, as such processes are regarded as in-
compatible with determination of nominal bond strength.
A conclusive test method should anticipate and tolerate
flaws in the material or the interface, lead to interfacial
failure, and be independent of test geometry. To deter-
Vol 12, No 5, 2010
Salz p
and
yrBock
ig
No Co
ht
t fo
rP
by N
ub
Q ui
Notc h lica
tio
te n
ot
n
ss e n c e
fo r
T a o
G D H
Dentin
Fig 19 Critical plane-strain energy release rate test setup
according to Tantbirojn et al.329 D = diameter (4.0 mm), ao =
0.15 D, ∢ GTH = 90°.
mine interfacial material properties, such as crack growth
resistance, linear elastic fracture mechanics appears ap-
propriate. Fracture mechanics is well established to de-
scribe monolithic materials and is becoming increasingly
common to investigate interfaces of dissimilar materi-
als. Up to now, the limited number of fracture mechanics
studies on dental adhesives published have been carried
out with different test setups, sample geometries, and
loading rates. In spite of several intrinsic methodological
advantages, the use of fracture mechanics as a more con-
clusive method to predict clinical performance of dental
adhesives therefore remains to be proven.
Concluding Recommendations
Any adhesion testing is a highly technique-sensitive pro-
cedure. In dental research, this is further aggravated by
the nonstandardizable biological substrates employed,
the often barely traceable age and state of materials,
the significant influence of operator skill and motivation,
and the astonishing impact of even minor variations in
any of the numerous experimental steps.
To master this array of important variables, investiga-
tions should account in detail for substrate collection and
processing, age and storage conditions of restorative ma-
terials, and the protocol used for sample preparation and
storage. Admittedly, this is easier said than done; never-
theless, this will eventually provide the insight required to
further improve materials and methods. Some key points
that may help minimize experimental variations:
r

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UP
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unintended or unforeseeable interplay of such altera-
tions.
r

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PS
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Name storage conditions, age of material, and expira-
tion dates.
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UP
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Describe noteworthy manual skills or appliance em-
ployed for consistent results.
r

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MFBTU
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PG
SFTVMUT
r

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BMM
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363
Salz and Bock pyrig
No Co

ht
priate “gold standard” product as internal reference. 12. Aranha AC, Siqueira Junior Ade S, Cavalcante t
LM, Pimenta LA, Marchi
GM. Microtensile bond strengths of composite to fodentin
r treated with

by N
Where appropriate, reference other investigators’ desensitizer products. J Adhes Dent 2006;8:85-90. Pu
b

Q ui
data to own results. 13. Armstrong SR, Boyer DB, Keller JC, Park JB. Effect of hybridlilayer
caton
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TUPSBHF
BOE
TVC- ion
fracture toughness of adhesively bonded dentin-resin composite joint.
Dent Mater 1998;14:91-98. te ot

sequent processing are vital for conclusive interpreta-
tion of data.
r

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PS
TVSGBDF
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FY-
perimental outcome and must be described in detail.
r

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QSPWJEF
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and C-factor on the dentin-resin composite microtensile bond strength
name and lot number, but also pre-use duration and
conditions as well as pre-use treatment.
r

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BOE
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strength of a total-etch 3-step, total-etch 2-step, self-etch 2-step, and
those not commercially available. Where possible,
employ equipment available to other investigators.
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the stereotypical “applied as described in instruc-
tions for use”.
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reproducibility and especially vital for microtensile
procedures. Therefore, unambigiously describe re-
lated points with requisite clarity.
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GPS
JO- Adhesion to tooth structure: a critical review of “micro” bond strength
stance, type of testing machine, geometry of sample
jig and force-exerting apparatus, as well as specimen
alignment with respect to direction of force.
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modes, and state how these were included in the
evaluation.
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Vol 12, No 5, 2010
Salz p and
yrBock
ig
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ht
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