Effect of Air Abrasion and Thermocycling
Effect of Air Abrasion and Thermocycling
Effect of air abrasion and thermocycling on resin adaptation and shear bond
strength to dentin for an etch-and-rinse and self-etch resin adhesive
Rebecca FREEMAN, Srinivas VARANASI, Ian A. MEYERS and Anne L. SYMONS
The University of Queensland, School of Dentistry, 200 Turbot Street, Brisbane, Queensland 4000, Australia
Corresponding author, Anne L. SYMONS; E-mail: [email protected]
This study examined the effect of air abrasion and thermocycling on the adaptation and shear bond strength, of composite resin
bonded to dentin using etch-and-rinse and self-etch resin adhesives. Confocal microscopy showed both adhesives closely adapted to
dentin and a signiicantly (p<0.001) greater number of resin tags were observed for the etch-and-rinse adhesive. Air abrasion
signiicantly increased resin tag length (p<0.05) for the etch-and-rinse adhesive and signiicantly increased the number (p<0.001),
length (p<0.001) and thickness (p<0.01) of tags for the self-etch adhesive. However, air abrasion resulted in defect formation within
the hybrid layer and thermocycling caused separation of the hybrid layer from adjacent dentin containing resin tags. A signiicant
(p<0.05) reduction in shear bond strength was observed for the etch-and-rinse adhesive following thermocycling. Both adhesive
systems adapted well to dentin in vitro and shear bond strengths were similar. The area of tag penetration into dentin was signiicantly
(p<0.0001) enhanced following air abrasion.
Adper Prompt L Pop Self-Etch 2-propenoic acid, 2-methyl-phosphinicobis (oxy-2,1-ethandiyl) ester, mono HEMA
Adhesive* phosphate, methacrylated pyrophosphates, Tris[2-(methacryloyloxy) ethyl]
phosphate ethylene dimethacrylate, phosphoric acid, Bis (2,6-dichlorobenzoyl)
butylphenyl phosphine oxide, 2-hydroxyethyl methacrylate, 4-methoxyphenol,
hydroquinone, Bis-GMA, DL-camphorquinone, ethyl 4-dimethyl aminobenzoate
Z100 Restorative Composite* Silanetreated ceramic, Bis-GMA, triethylene glycol dimethacrylate (TEGDMA),2-
benzotriazolyl-4-methylphenol
*3M ESPE, St. Paul, MN, USA.
Adper Single Bond Adhesive* Dentin and enamel etched for 15 s (37% phosphoric acid), rinsed for 10 s and gently
air dried. Two coats of adhesive applied with a microbrush, gently air dried 2–5 s
and light cured for 10 s.
Adper Prompt-L-Pop Self-Etch Components were activated and applied to cavity preparation on a microbrush and
Adhesive* the adhesive massaged for 15 s, air dried and light cured for 10 s.
3M Z100 Restorative Dental A single increment of composite resin was condensed into the cavity preparation
Composite* and light cured for 40 s.
Thermocycling 1,000 cycles between water baths at 5°C and 55°C, with a dwell time of 30 s in each
bath.
*3M ESPE, St. Paul, MN, USA.
Confocal microscopy
Tooth-restoration sections of control and thermocycled
Fig. 2 Confocal micrograph showing the hybrid layer (H)
teeth were examined using CLSM (LSM510, Carl Zeiss,
and adhesive resin penetrating dentin (D). The
Tessovar, West Germany) with a 10× objective and oil width of the resin hybrid layer, thickness and
immersion 40× and 60× objectives. The luorescence length of resin tags and the area of the adhesive
emission of the resin layer along the axial wall of the resin within the dentin were measured over a 100
cavity preparation and within the dentin tubules was µm length of the axial wall. Bar represents 10
detected using a 488 nm excitation line. Sections were µm.
immersed in water and covered with a transparent cover
slip. A length of 100 µm in the central region of the axial
wall was examined for the presence of defects, adhesive dentin tubules were counted along a 100 µm length of
resin adaptation and penetration into dentinal tubules. the axial wall (Fig. 2). The length of the resin tags was
Using CLSM, the number, length, thickness and measured from the axial wall of the tooth (below the
area of the adhesive resin tags within the dentin tubules hybrid layer) to the end of the tag penetrating the tubule.
were determined using interpolated image stacks (400× For each specimen the mean adhesive tag length was
magniication) of tooth sections containing the luorescent determined. The thickness of the tag was measured
adhesive resin. These images were reconstructed into a approximately 5 µm beneath the hybrid layer, within the
2-D data set, using surface rendering techniques. dentin tubule. The area occupied by adhesive resin tag
Following surface rendering, the 2-D images were penetration into dentin was measured using
intensity thresholded, for isosurfacing and isocountering, densitometry (Fig. 2). Data obtained for each group was
using the Axiovision Automeasure 4.3 Image Analysis compared using the Axiovision Automeasure 4.3 Image
Software (Carl Zeiss). Analysis Software Program (Carl Zeiss).
The number of adhesive resin tags penetrating
Dent Mater J 2012; 31(2): 180–188 183
Shear bond strength force at failure was used to calculate shear bond strength.
A 1.00 mm thick sagittal slice of coronal dentin, from a Data was analysed using Graph Pad Instat 3 (San
region 0.5–1.5 mm below the dento-enamel junction on Diego, California, USA). For resin tag measurements,
the buccal or lingual aspect of the crown, was cut using a data was tested for normality using the Kolmogorov-
slowly rotating diamond blade. Dentin tubules in the Smirnov test and analysed using t-tests. Statistical
center of the slice were estimated to be perpendicular to differences in resin tag number, length, thickness and
the cut surface. The dentin slice was covered with a area were determined between the two adhesive systems
waterproof, 1 mm thick, double-sided, adhesive polyvinyl- (Groups A and C) and within each adhesive system
chloride tape, pre-punched to expose a circular area of following air abrasion (Groups A and B; Groups C and
dentin, 2.00 mm in diameter in the center of the tooth D). Differences were considered signiicant with p<0.05.
section. The exposed dentin was treated as described for Normality and equality of variances were conirmed for
A, B, C or D above and a 1.5 mm high disk of composite shear bond strength data which was analysed using
with a diameter of 2.00 mm bonded to the dentin surface. t-tests comparing adhesive systems (Groups A and C)
Sections were stored in PBS at 25°C for 2 weeks prior to and the effect of air abrasion (Groups A and B; Groups C
testing. Sections were divided into control or thermocycled and D). In addition, the effect of thermocycling on shear
(N=8). Shear bond strength was measured at 25°C using bond strength, in each restorative group, was analysed
a custom-made, single-plane jig attached to a tensometer using t-tests and signiicance determined where p<0.05.
(Monsanto Houndsield Tensometer, Test Equipment,
Croydon, England) itted with an electric load cell. The
RESULTS
force was registered using a strain gauge (400×, 0.02 N).
Specimens were tested to failure using a cross-head Macroscopic examination of the axial wall using a
speed of 5.00 mm/min. Testing was performed without dissecting microscope revealed Rhodamine B colouration
knowledge of the treatment procedures undertaken. The along the interface between the restoration and dentin.
Fig. 3 Confocal micrographs showing resin tag formation and adaptation to dentin for control specimens from each
restorative group: (a) Group A, (b) Group B, (c) Group C and (d) Group D. Bar represents 10 µm.
184 Dent Mater J 2012; 31(2): 180–188
For all groups, the dye penetrated the dentin and the portion of the axial wall and penetrated the dentin
restorative material appeared well adapted. tubules (Fig. 3). Following air abrasion and thermocycling,
CLSM examination showed that for groups A and C, specimens exhibited adhesive defects along the axial
the adhesive resin was well adapted to dentin in the mid dentin (Fig. 4). Defects were located at the adhesive
Fig. 4 Confocal micrographs showing separation of the hybrid layer from dentin containing resin tags following
thermocycling for each restorative group (a) Group A, (b) Group B, (c) Group C, (d) Group D. In addition to
separation, disturbances in the hybrid layer were also observed in some thermocycled specimens as shown in (e)
section from a Group B specimen. Bar represents 10 µm.
Dent Mater J 2012; 31(2): 180–188 185
Table 4 Distribution of defects in the adhesive layer for control (C) and thermocycled (T) specimens in each restorative
group (n=8)
Restorative group
A B C D
C T C T C T C T
Adaptation defects present 0 7 4 8 0 7 4 7
Well adapted (no defects) 8 1 4 0 8 1 4 1
Table 5 Resin tag measurements, mean (SD), comparing adhesives (A vs C) and the effect of air abrasion on tag
number, length, thickness and area for each adhesive system (Groups A vs B, C vs D)
Resin tag measurements
Group A B C D
AC
Number/100 µm 17.5 (7.26) 20.47 (8.4) 5.06 (4.8) *** 18.56 (8.15)CD***
Length (µm) 9.6 (9.0) 23.09 (13.7)AB* 3.63 (3.21)AC** 31.79 (16.84)CD***
Thickness (µm) 0.77 (0.58) 1.28 (0.26) 0.41 (0.42) 1.26 (0.21)CD**
Area (µm2) 104.7 (41.09) 405.76 (183.16)AB**** 65.6 (32.58)AC** 412.24 (177.21)CD****
**p<0.01; ***p<0.001; ****p<0.0001. n=16
Table 6 Mean (SD) shear bond strength (MPa) for each restorative procedure comparing resin adhesives (Group A vs
Group C), effect of air abrasion (Groups A vs B, Group C vs D) and thermocycling (within the restorative group)
on bond strength (n=8)
Shear bond strength MPa Mean (SD)
Group A B C D
Control 16.15 (4.64) 17.96 (5.99) 17.50 (5.36) 15.05 (3.93)
Thermocycled 9.57 (2.86)C-T* 14.96 (3.94) 11.52 (2.94) 14.59 (1.37)
C-T compares bond strength for Group A controls (C) with Group A thermocycled (T) specimens. *p<0.05.
resin-dentin interface and included separation of the strength (Table 6) between the two adhesives tested
hybrid layer from resin penetrating tubules, presence of (Group A and C) and air abrasion did not signiicantly
clefts and/or voids within the hybrid layer (Fig. 4) or a increase shear bond strength (Group A and B; C and D).
combination of both (Fig. 4e). Clefts or voids in the hybrid Thermocycling signiicantly (p<0.05) reduced the shear
layer were observed in air abraded specimens and bond strength of the Group A etch-and-rinse adhesive,
separation of the hybrid layer from the dentin surface but within other restorative groups, no reduction in
containing resin tags was characteristic of thermocycling. shear bond strength was observed following
Thermocycling did not appear to disrupt penetration of thermocycling. In general, thermocycling tended to
resin into the tubules. Air abraded, thermocycled reduce and air abrasion tended to increase the mean
specimens contained the greatest distribution of adhesive shear bond strength to dentin (Table 6). The mode of
defects with a combination of clefts or voids in the hybrid bond failure was adhesive for each material tested.
layer and separation from the dentin (Table 4). The Dentin surfaces were smooth and clean indicating that
distribution of defects was similar for both adhesive fracture occurred at the interface between dentin and
systems (Table 4). resin.
The number (p<0.001), length (p<0.01) and area
(p<0.01) of the resin tags penetrating dentin tubules was
DISCUSSION
signiicantly higher for Group A compared with Group C
(Table 5). Air abrasion signiicantly increased the length The current in vitro study observed close adaptation of
(p<0.05) and overall area of resin tags (p<0.0001) adhesive resin to the dentin surface for the etch-and-
observed for the etch-and-rinse adhesive and signiicantly rinse and self-etch systems. Adaptation to dentin was
increased the number (p<0.001), length (p<0.001), compromised by air abrasion and thermocycling, with
thickness (p<0.01) and overall area (p<0.0001) of specimens showing separation of the hybrid layer from
adhesive resin tags observed for the self-etch adhesive the underlying dentin. Thermocycling signiicantly
(Table 5). (p<0.05) reduced the shear bond strength for the etch-
There was no signiicant difference in shear bond and-rinse adhesive to dentin. Pre-treatment with air
186 Dent Mater J 2012; 31(2): 180–188
abrasion increased the number of resin tags penetrating adhesive, tag number and thickness signiicantly
the dentin tubules for both adhesives. Air abrasion had a increased. Reducing the thickness of the smear layer and
more profound effect on resin tag formation for the altering the dentin surface structure following air
self-etch adhesive where tag number (p<0.001) and abrasion may potentiate the penetration and eficacy of
thickness (p<0.01) were signiicantly increased. Both the etch component in an adhesive system. Thus, a thin
adhesive systems demonstrated similar shear bond smear layer occluding the dentin tubule may be easily
strengths to dentin which was not signiicantly enhanced removed when etched. This could enhance resin tag
following air abrasion. However, shear bond strength formation for all adhesive systems, having a greater
values tended to remain higher, following thermocycling, impact for self-etch adhesives.
for air abraded specimens. The self-etch adhesive system used in this study,
While the aim of dental adhesion is to obtain Prompt-L-Pop, has an initial pH of approximately 0.9
intimate adaptation of the restorative material to tooth compared with the standard 37% phosphoric acid gel
structure6), bonding is challenged by the high water and which has a pH of approximately 0.6. The slightly lower
organic content of dentin7). The smear layer created pH of the phosphoric acid may be more effective in
during cavity preparation forms a physical barrier which removing the smear layer and opening dentin tubules to
must be dissolved or made permeable so adhesive allow resin penetration and tag formation. The process
monomers can contact the dentin surface6). The basic of washing off the acid and gently air drying is not
composition of the smear layer is hydroxyapatite and reliable in producing the ideal surface moisture to enable
altered collagen27), and the morphology of the smear resin interpenetration and tag formation. The
layer varies with the type of instrument that creates it Prompt-L-Pop system avoids this step, as it dissolves the
and the site where it is formed6,28,29). Although the dentin smear layer and incorporates remnants of the smear
surface prepared with airborne-particle abrasion is layer within the hybrid layer and resin tags and which
covered by a thin smear layer, use of an acidic conditioner may in turn affect resin interpenetration and tag
prior to resin application is necessary to obtain good formation. Failure to remove the smear layer which
bonding30,31). A thinner smear layer covering a macerated forms a plug at the tubule opening may inhibit tag
dentin surface may potentiate the activity of the formation. It is clear from the air abraded specimens
conditioning agent and result in an over etching of the that the resin components in both adhesive systems have
fragile dentin surface32,33). the potential to penetrate dentin tubules and form a
Development of the self-etch adhesive systems hybrid layer.
aimed to simplify and improve the eficacy of resin A more intimate contact with dentin may improve
adhesion to dentin4). However, resin restorations placed the reliability of the dentin-adhesive interface and
using self-etch adhesives are reported to demonstrate enhance clinical durability of the resin bond. The
lower bonding effectiveness in vitro34) and clinical trials importance given to the iniltration and low of the
report a less favourable clinical effectiveness for adhesive resin inside the acid-treated dentinal tubules
composite restorations using this adhesive system1). In remains to be determined. For optimal dentin bonding,
the current study, confocal microscopy showed that both the adhesive must penetrate the demineralised dentin
adhesive systems demonstrated an ability to closely tubule prior to polymerization36). Resin tags are believed
adapt to dentin, via the formation of a hybrid layer and to have the capacity to adhere to the tubular surface only
resin tags. This intimate contact with dentin is considered where they iniltrate the interibrillar spaces in the
essential for clinical success of the restoration, prevention surrounding demineralised intertubular dentin37).
of postoperative sensitivity and to counteract forces However, polymerization shrinkage may cause
resulting from the polymerization shrinkage of composite separation of the adhesive from the tubule wall38). It has
resins6). However, the diminished ability of the self-etch also been shown that the length of the resin tag may
adhesive to form resin tags may reduce their clinical exceed the area where dentin has been demineralised4).
effectiveness. The relative importance of resin tag formation with
Hybrid layer and resin tag formation are dependent respect to sealing the pulp-dentin complex and bond
on the adhesive system used, dentin surface strength may vary according to location. Resin tags
characteristics, tubule orientation, mineral content of approximating the hybrid layer may play a greater role
intertubular dentin and the density, morphology and with respect to bond strength and permeability of the
approximation of the dentin tubules to the pulp35). This pulp-dentin complex36). Deeper resin tags may occupy
study attempted to minimize these variations by the tubule without adhering to the walls and where the
selecting third molars extracted from young adults, bonding agent adheres to dentin, polymerization
conining the surface examined to the axial dentin wall shrinkage may produce hollow resin tags37). In addition,
and placing dimensionally similar restorations in the polymerization shrinkage may result in tearing of the
same tooth. Hybrid layer and resin tag formation were dentin surface damaged by air abrasion, compromising
observed for all groups studied. Resin tag formation for adhesion. However, resin tag formation may not
the etch-and-rinse adhesive was longer and more contribute to shear bond strength where the hybrid layer
numerous than that observed for the self-etch adhesive. becomes separated from the adjacent dentin following
Following air abrasion, resin tag length signiicantly polymerisation shrinkage and aging of the restoration.
increased for both adhesive systems and for the self-etch Where separation occurs, resin tags penetrating the
Dent Mater J 2012; 31(2): 180–188 187
dentin may only contribute to the protection of the pulp For both adhesive systems examined, an increase in the
by sealing the tubules. number of defects located at the dentin-adhesive surface
Confocal micrographs revealed defects in the was observed following thermocycling. Where
adhesive layer of thermocycled and air-abraded air-abrasion has severely damaged the dentin surface,
specimens. These defects include separation of the the permeation of biological luids that cause hydration
hybrid layer from underlying dentin and disturbances of the resin matrix and breakdown adhesion to the
within the hybrid layer and were observed for both collagen ibers50) may be enhanced and result in reduce
adhesive systems. Thermocycled specimens tended to long term clinical durability.
show separation of the hybrid layer from dentin in which
resin tags were located. This separation may account for
CONCLUSION
the reduction in shear bond strength observed for the
etch-and-rinse adhesive. Air abrasion has been suggested Using conventional preparation techniques, good
to cause supericial maceration of the collagen ibers on adaptation of both resin adhesives to dentin was
the dentin surface39) and increase the incidence of observed but resin tag formation was markedly reduced
adhesive fractures40). This effect may weaken the for the self-etch adhesive. Resin adhesives initially
supericial structure of the dentin and affect the quality showed close adaptation to dentin and this adaptation
of the hybrid layer39) resulting in the formation of defects was compromised following thermocycling. Air abrasion
such as voids and clefts. signiicantly increased the area of resin tag formation
Thermocycling protocols to evaluate bond durability into dentin. This effect was more apparent for the
range from 100 cycles41) to more than 50,000 cycles42). self-etch adhesive. Although air abrasion tended to
The current study used 1,000 thermal cycles, which is increase the number, length and diameter of resin tags,
more than the regimen proposed by the ISO standard43). it increased the number of defects observed in the hybrid
A signiicant reduction in shear bond strength was layer on the dentin surface and minimally enhanced
observed for the etch-and-rinse adhesive controls shear bond strength of resin to dentin. The clinical
following 1,000 cycles but not for the other restorative signiicance of enhanced resin tag formation in air
protocols. Similar bond strengths and the failure of 1,000 abraded dentin for self-etch adhesive restorations
cycles to signiicantly reduce shear bond strength have remains to be determined.
been reported previously44) and may indicate bond failure
had not occurred across the entire dentin surface.
ACKNOWLEDGMENTS
Increasing the number of cycles may result in a more
signiicant reduction in shear bond strength. The This research was supported by an ADRF undergraduate
addition of 10% Rhodamine B dye to the bonding system vacation research scholarship.
had the potential to disturb adhesion but CLSM images
demonstrated good adaptation and shear bond strengths
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