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Review Article

Validity of bond strength tests: A critical review-Part II


Kantheti Sirisha, Tankonda Rambabu1, Yalavarthi Ravishankar2, Pabbati Ravikumar3
Departments of Conservative Dentistry and Endodontics and 2Prosthodontics, GITAM Dental College and Hospital, Visakhapatnam,
1
Departments of Conservative Dentistry and Endodontics, Vishnu Dental College and Hospital, Bhimavaram, 3Conservative Dentistry and
Endodontics, SIBAR Institute of Dental Sciences, Guntur, Andhra Pradesh, India

Abstract
Background: Macro-bond strength tests resulted in cohesive failures and overestimation of bond strengths. To reduce the flaws,
micro-bond strength tests were introduced. They are the most commonly used bond-strength tests.
Objective: Thus the objective of this review is to critically review the reliability of micro-bond strength tests used to evaluate
resin-tooth interface.
Data Collection: Relevant articles published between January 1994 and July 2013 were collected from Pubmed database,
Google scholar and hand searched journals of Conservative Dentistry, Endodontics and Dental materials.
Data Synthesis: Variables that influence the test outcome are categorized into substrate related factors, factors related to specimen
properties, specimen preparation and test methodology. Impact of these variables on the test outcome is critically analyzed.
Conclusion: Micro-bond tests are more reliable than macro-bond tests. However, no standard format exists for reporting the
bond strength tests which could lead to misinterpretation of the data and bonding abilities of adhesives.
Keywords: Bond strength test; micro-tensile; micro-shear; micro-push out

INTRODUCTION Micro-shear (μSBS) test


Shear bond strength (SBS) testing with bonded cross-
The rapid progress in dental adhesive technology has sectional areas of 3 mm2 or less is referred to as ‘micro’
extensively influenced modern restorative dentistry. SBS.[5,6] It permits efficient screening of adhesive
Despite the vast advances made in adhesive technology systems, regional and depth profiling of a variety of
during the last 50 years, the bonded interface itself substrates, and conservation of teeth. A significant
remains as a weakest point of an adhesive restoration.[1] advantage over micro-tensile strength (μTBS) methods
Smaller test specimens are ‘stronger’ than larger ones is that the μSBS specimen is pre-stressed prior to testing
due to the lower probability of presence of critical only by mold removal. However, the use of the mold for
sized defects.[2] Thus micro-bond strength tests (bond composite placement can lead to the introduction of
area less than 3 mm2) were developed [3] and higher flaws and different stress concentrations upon shear
apparent ‘strength’ can be measured with more failures loading. [7]
at the interface. Unlike the macro tests, which were
discussed in previous article (Validity of bond Strength The findings of Finite Element Analysis (FEA) reported
tests-part I: A critical review on macro-bond strength uneven stress distribution by creating tensile stresses
test methods) failures are adhesive rather than too.[8,9] A three-dimensional FEA[10] demonstrated minimized
cohesive.[4] tensile forces during loading by optimizing specimen
dimensions and load application location. Micro-shear test
MICRO-BOND STRENGTH TESTS results may actually worse represent shear bond strength
than the conventional macro-SBS test.[9] Area delimitation
Micro-bond strength tests are categorized into three types: technique renders μSBS testing less questionable and
Micro-shear, micro-tensile and micro-push out tests based should be considered as an important step during the
on the stresses exerted on the test specimens. application of the method.[11]

Address for correspondence: Access this article online


Dr. Kantheti Sirisha, Department of Conservative Dentistry and Quick Response Code:
Endodontics, GITAM Dental College and Hospital, Website:
www.jcd.org.in
Visakhapatnam - 530 045, Andhra Pradesh, India.
E-mail: sirishaky@gmail.com
Date of submission : 02.03.2014 DOI:
Review completed : 20.05.2014 10.4103/0972-0707.139823
Date of acceptance : 04.06.2014

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Sirisha, et al.: Critical review on micro-bond strength tests

Micro-shear tests remain an extremely useful test for


those substrates with properties such as glass ionomers
or enamel that make them particularly susceptible to the
specimen preparation effects and testing conditions of
μTBS testing.[4]

Micro-tensile (μTBS) test


In micro-tensile test, further specimen processing or the
actual preparation of the micro-specimens is required Figure 1: Variables influencing micro-tests
after the bonding procedure.[12] Advantages are that it
involves better economic use of teeth (with multiple micro
Lopes[19] found many structural similarities between human
specimens originating from one tooth), the better control
and swine teeth and suggested use of porcine teeth.
of regional differences (e.g. peripheral versus central
Morphological, chemical composition and physical property
dentin), the better stress distribution at the true interface,[3]
differences between human and bovine teeth must be
ability to test irregular surfaces and very small areas and
considered when interpreting results obtained from any
facilitates microscopic examinations of the failed bonds
experiment with bovine teeth substrate.[20] For more
due to smaller areas. Drawbacks are the labor intensity,
predictable results, use of human teeth is recommended.
technical demand, dehydration potential of these smaller
samples, difficulty in measuring bond strengths lower than
Substrate condition
5MPa, difficulty in fabricating specimens with consistent
Micro-tests have the added advantage of ability to test
geometry, easily damaged specimens and loss or fracture
the bond strengths to various substrates like sclerotic,
of post-fracture specimens.[12,13] Micro-tensile bond test
infected or affected carious dentin, hypoplastic enamel
(μTBS) allowed additional research designs that the ‘macro’
etc. Micro-tensile bond strength to caries-affected
tests did not, such as, the elimination of tooth dependency
dentin[21,22] and sclerotic dentin[23,24] was lower when
through balanced designs.[14]
compared with that of normal dentin. This was due to
decreased resin infiltration into dentinal tubules of caries-
Micro-push out (μPO) test affected dentin by the mineral deposits.[25] Mechanical
Micro-push-out test is a modification of push out test
treatment with diamond bur or diamond paste[24] or
where the specimen thickness is less than or equal to
conditioning with stronger acids may facilitate stronger
1 mm2. Micro-tensile bond strength test method is not
bonding to sclerotic dentin.[23]
appropriate for use with intracanal filling materials
because of the high percentage of premature bond failures
Dentin depth and permeability
and the large variation in test results.[15] Micro-push out is
Majority of studies showed decreased micro-tensile[26,27]
more dependable than the micro tensile technique while
and micro-shear bond strengths[28] with increased dentin
measuring the bond strength of luted fiber posts.[16] A
depths unlike the varied results of macro-tests. This may be
study[17] reported that a modified push-out approach and
due to increased permeability[29] and reduced percentage of
micro-tensile test revealed higher values than traditional
solid dentin available for bonding. It is advisable to consider
pull-out and push-out methods. But this modified push-
the type of adhesives while interpreting the results of bond
out approach needs more studies before making any
strength tests.
conclusions.
Smear layer
VARIABLES INFLUENCING MICRO-BOND Smear layer denseness, more so than thickness, may
STRENGTH TEST RESULTS compromise bonding efficacy of adhesives, especially of
self-etch systems.[30] Smear layer thickness did not affect
Variables related to the clinical situation and the bond strengths in majority of the studies but the
the substrate treatment type of adhesive affected the bond strengths.[31,32] Higher
Many variables related to clinical situation and substrate bond strengths were noted with etch and rinse systems
affect the micro-bond strengths [Figure 1]. where smear layer was removed[31] and with agitated self
etching systems where smear layer was dispersed or
Substrate related factors dissolved.[33]
Source of teeth
Unlike the contradictory results of macro-tests, bovine teeth Enamel prism and dentinal tubule orientation
were found to be better substitutes for human teeth than The effects of regional variations in tooth structure,
porcine teeth for micro-tests. In porcine teeth, the enamel such as the orientation of enamel prisms, orientation of
prism orientation is different from that of human enamel.[18] dentinal tubules and the influence of cavity geometry on

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Sirisha, et al.: Critical review on micro-bond strength tests

bond strength, are variously studied, in which the results application distance resulted in non-uniform stress
were contradictory like macro-tests. This may be because distribution along bonded interfaces.[9] Mechanical properties
of structural anisotropy; variation in enamel bonding sites of the composite affected the μTBS values due to uneven
and the type of adhesive.[28,34,35] stress distribution.[52]

Substrate location Variables related to specimen preparation for


Substrate location can be occlusal, cervical, buccal or bond strength testing
gingival and root or crown. Micro-tensile bond strength Aging media
to enamel[36] and dentin[35,37,38] and micro-shear[28] bond Various solutions like distilled water, artificial saliva and
strengths to dentin varied depending on the location of sodium hypochlorite (NaOCl) were used for aging.[47] No
substrate similar to that of macro-tests. Majority of the change in micro-tensile bond strength was observed
authors concluded that results depended on the type of after six months of water storage[53] whereas another
adhesive system.[35,38] study[54] observed sensitivity of resin-dentin bond to water
degradation for four years. It was concluded that resin
Pulpal pressure bonded to enamel protected the resin-dentin bond against
The presence of pulpal pressure resulted in a decrease of degradation, while direct exposure to water for four years
μTBS of various bonding systems while simulating in vivo affected bonds.
conditions.[39,40] Few studies reported reduction of μTBS
was adhesive-dependent,[41,42] which is similar to macro- Failure analysis of immersed test specimens in sodium
bond strengths. One study,[43] reported no bond strength hypochlorite (NaOCl) revealed a drop in μTBS correlated
reduction when adhesives were applied to dentin supplied with specific dissolution of the hybrid layer, similar to
with water pressure. in vivo failure patterns.[55,56] Thus aging specimens in 10%
NaOCl for 1 or 3 hours can be an alternative method for
Tooth donor age long-term water storage (6 or 12 months) micro-tensile
Physical properties and morphological features of enamel bond strength studies.[57] Main drawback of this method
and dentin vary with age progression. Age did not affect is due to the non-specific properties; NaOCl also causes
bond strength values of glass-ionomer based, all-in-one, the mechanical properties of the dentin substrate itself to
single-step, self-etching adhesive system to dental hard deteriorate.[58]
tissues.[44-46]
Aging time
Storage conditions and time Aging in artificial saliva for more than six months reduced
Distilled water, saline, 0.05% saturated solution of thymol, bond strength.[56] One year water storage did not have any
0.5% chloramines-T, 2% gluteraldehyde, 10% formalin effect on micro-tensile bond strength[59] whereas three year
solutions were studied as storage media for bond-strength storage reduced the bond strength.[60] Effect of aging time
tests.[47,48] Zheng et al.[49] recommended use of frozen on micro-tensile bond strength varied with the medium
teeth at −20oC or storage of teeth in 1% chloramine at used for aging and type of adhesive.[61]
4oC. Before using any teeth that were preserved in dry
state, rehydration with distilled water for two weeks is Thermal cycling
recommended.[50] Researchers reported diverse results though majority
of them concluded that thermocycling reduced the
Teeth that have been extracted for longer than six months bond strength to enamel and dentin.[56,62-69] The effect of
could undergo degenerative changes in dentinal protein.[47] thermocycling depends on the chemical bonding potential
According to the ISO/TS 11405, teeth those were stored for of functional monomer, i.e. type of adhesive system.[64] Very
one month, but not more than six months, after extraction few studies employed the thermocycling at a frequency
should be used.[51] of 500 cycles as recommended by ISO/TS specification. If
it exceeds this frequency, bond strength was reduced in
Variables related to test specimen properties majority of these studies. Hence, for reliable results ISO/TS
Bonding area recommendations must be followed.
Bond area depends on the specimen size; hence it is
discussed in detail under the section of ‘specimen size’. Mechanical cycling
Amount of load exerted while chewing and swallowing varies
Elastic modulus of the resin composite between 70N and 150N.[70] Load application of 500,000
Mechanical properties of composite can affect the bond- cycles is equivalent to six months and 1,000,000 cycles is
strength test results. High elastic modulus of bonded equivalent to one year of in vivo mastication.[71] Researchers
composite, relative adhesive layer thickness and load used loads ranging from 50N to 125N at frequencies

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Sirisha, et al.: Critical review on micro-bond strength tests

ranging from 0.5 Hz to 4 Hz.[62,63,68,72-75] Number of cycles preferred for enamel specimens as they can be prepared in
ranged from 10,000 cycles to 500,000 cycles. Mechanical a less destructive, easier, and more precise way.[83]
cycling resulted in mixed type of failures and bond strength
was reduced in specimens when they were subjected to Other factors such as specimen–jig attachment, specimen-
thermal and mechanical cycling.[68,72,73] loading speed and specimen alignment also influence
the final outcome; and therefore, should be standardized
Operator skill and technique sensitivity within the test set-up.[84]
Operator’s skill in handling a material and/or using the
test apparatus may affect the measured micro-shear bond One major concern is the required number of individual
strength. Operator skills may improve with repeated teeth from which many micro-specimens can be prepared
testing and material use.[76] In contrast to this, no to be statistically sound.[85] An elegant way to handle this
statistically significant difference was observed in micro- problem is to use every tooth as its own control.[82] As also
push out bond strength values between the operators of recommended by ISO/TS No. 11405[51], another way would
different clinical experience.[77] Though adequate literature be to apply survival analysis like the Weibull model or Cox
is not available regarding its effect on micro-tensile bond proportional hazard using the force that is required for
strength, operator skill can increase the reliability of bond failure.[86]
test results.
Gripping devices
Variables of influence related to test mechanics Test specimens are attached to the load train couplers of
Specimen size mechanical testing machines by either active or passive
The micro-specimen preparation protocols are more gripping devices. A non-normal load application, either
technique-sensitive. For the micro test methods ‘trimmed’ the specimen or gripping mechanism significantly alters
and ‘non-trimmed’ micro-specimens are prepared and both the stress distribution at the bonded interface.[87] Several
have their advantages and disadvantages.[52,78] A reduction specimen gripping devices, both active and passive, have
of bond strength was observed in enamel[36], when the been developed in an attempt to apply a tensile load normal
bonding area was increased from 0.5 to 3.0 mm2. Similar to the bond line by aligning specimen’s bond line with
phenomenon was observed in specimen sizes with 1.2 and its gripping surfaces.[84,88,89] Active gripping can be either
2.0 mm in diameter where an inverse linear relationship mechanical or through a fast-setting glue. Bending forces can
between specimen size and bond strength when tested occur during load application due to: Non-parallel specimen
either in tension or shear[5] and that cross-sectional shape alignment, bond line not perpendicular to the specimen
(cylindrical or rectangular) has little effect on micro-tensile gripping surfaces, and/or, uneven gripping forces.[87,90]
bond strength.[79]
These specimen-fixation procedures require careful
Specimen geometry manipulation and special test jigs like Bencor multi-T
Stick shaped, hour glass and dumbbell-shaped specimens gripping device and Ciucchi’s jig. None of these gripping
are used for micro-tensile testing. Trimming the specimens devices guarantees proper alignment because the specimen
at the interface to hourglass-shaped specimens better is glued to a flat surface.[84] In Geraldeli’s jig and modified
concentrates stress at the interface and may result in Ciucchi’s jig, a groove parallel to the applied load was
premature failures due to interfacial defects.[80] added in to improve specimen alignment.[88]

Interfaces can be trimmed by free hand using a dental Dirck’s device was introduced as self aligning, glue-less,
handpiece[3,81] or a plexiglass table on an Isomet saw passive gripping device.[30] It is less sensitive to human
(Buehler, Lake Forest, IL, USA) and trim the specimen under error than Geraldeli’s, and produced a more uniform stress
microscopic observation, using a device like table saw.[12] distribution at the dumbbell specimen adhesive layer than
Use of a semi-automatic trimming of micro-specimens using did the Geraldeli’s device at the stick layer.[91] Poitevin
a Micro Specimen Former (University of Iowa, Iowa City, IA, et al.[27,84], developed a μTBS testing device with top bottom
USA) is highly advisable to trim rectangular specimens into fixation to minimize stress concentrations.
specimens with a circular cross-section.[82]
Cross-head speed
Dumbbell-shaped specimens distribute the stress Cross-head speeds ranging from 0.01 mm/min to 10.00 mm/
more uniformly due to their cylindrical geometry and min were tested for their influence on micro-tensile bond
boundary conditions only if manufacturing process strength test. Unlike controversial results of macro-tests,
would be improved (like CAD-CAM® process) to reduce all the studies concluded that the influence of the cross-
imperfections into the interface. Otherwise, stick-shaped, head speed might be negligible while measuring micro-
non-trimmed specimens sectioned with diamond wire are tensile bond strengths.[27,92] Poitevin et al. recommended

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Sirisha, et al.: Critical review on micro-bond strength tests

a cross-head speed of 1 mm/min for more uniform stress- between micro-tensile bond strength data and the clinical
time pattern.[27] index, there existed a correlation between micro-tensile
bond strength and 6-month water storage and marginal
FRACTOGRAPHIC ANALYSIS discoloration of Class V restorations. A significant, quite
reasonable correlation was nevertheless found between
Fractographic analysis includes classification of the the aged bond-strength data and the 5-year clinical data.
interfacial phases, crack initiation, direction and pattern of Hence, besides measuring the ‘immediate’ bond strength
crack propagation, energetics of the fracture (single event of adhesives to enamel and dentin, measuring the ‘aged’
or fatigue; brittle or ductile), and the phases included along bond strength should be encouraged in order to predict
the fracture plane.[93] the clinical effectiveness of adhesives.[82]

Possible failure modes [Figure 2] of fractographic analysis Bond-strength test results of specimens after 24 hours and
are: 3 months of storage in water should be comparable with
a. Cohesive in dentin, those of comparable adhesive systems with an acceptable,
b. Cohesive in resin, proven clinical record.[96] Non-invasive methods of bond
c. Adhesive (dentin–adhesive interface), evaluation like X-ray micro computed tomography (CT)
d. Adhesive (resin–adhesive interface), and acoustic emission can be considered while testing
e. Mixed (dentin–adhesive–resin with small portions of adhesives.[97]
dentin),
f. Mixed (dentin–adhesive–resin with large portions of RECOMMENDATIONS FOR IMPROVING
dentin). VALIDITY OF MICRO-TESTS
Depending on the fracture path, cohesive failures and Specific recommendations are put forth for consideration
mixed failures with large portions of dentin and resin while testing the adhesive strengths.
should be excluded in results.[94] To characterize the
1. If traditional bond strength tests (shear, micro-shear,
adhesive joints several surface analysis methods are
tensile, micro-tensile) are to be used, only adhesive
available, including electron spectroscopy for chemical
failures or mixed failures with small (<10%) resin or
analysis (ESCA), secondary ion mass spectroscopy (SIMS),
dentin involvement should be considered for the
Fourier transform infrared spectroscopy (FTIR), Raman
bond strength calculation. This requires thorough
spectroscopy, scanning electron microscopy (SEM), energy
microscopic evaluation (stereo and SEM) of the
dispersive X-ray spectroscopy (EDS) and atomic force
fractured surface.
microscopy (AFM).[95]
2. Use of Weilbul statistics should be systematically
applied to evaluate bond strength data to provide more
CLINICAL RELEVANCE information that is relevant. Studies should utilize a
minimum of 30 non-cohesive failed specimens.
In a systematic review[96], the results of bond strength tests 3. Fracture mechanics approach that includes estimation
did not correlate with laboratory tests that evaluated the of fracture toughness or the strain energy release rate
marginal seal of restorations such as micro leakage or
is encouraged.[94]
gap analysis. Though there was no significant correlation
CONCLUSION

Bond strength testing can be used in the laboratory while


developing newer adhesives but cannot be used solely
as a means of predicting clinical performance.[98] Bonding
effectiveness in the laboratory should be assessed by
1. Micro-tensile bond strength testing,
2. Sealing effectiveness testing using semi-quantitative
marginal analysis or fully quantitative margin permeability
measurement and possibly
3. Dynamic fatigue testing.[82]

Though a great diversity in laboratory testing of adhesives


exists, validity of these tests can be improved by
application of standardized protocols in test methodology
Figure 2: Fractographic analysis and supplementing with the dynamic fatigue test results.

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Sirisha, et al.: Critical review on micro-bond strength tests

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Influence of thermal and mechanical load cycling on microtensile Ravikumar P. Validity of bond strength tests: A critical review-
bond strengths of total and self-etching adhesive systems. Oper Dent
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Effect of cyclic loading on the microtensile bond strengths of total-etch Source of Support: Nil, Conflict of Interest: None declared.
and self-etch adhesives. Oper Dent 2006;31:25-32.

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