NIH Public Access: Author Manuscript

Effect of solvent content on resin hybridization in wet dentin
bonding
Yong Wang
1
, Paulette Spencer
1,2
, Xiaomei Yao
1
, and Bohaty Brenda
2
1Department of Oral Biology, University of Missouri-Kansas City School of Dentistry, Kansas City, Missouri
64108
2Department of Pediatric Dentistry, University of Missouri-Kansas City School of Dentistry, Kansas City,
Missouri 64108
Abstract
With wet bonding techniques, the channels between the demineralized dentin collagen fibrils are
filled with debris, solvent, and water. Commercial adhesives include solvents such as ethanol or
acetone to facilitate resin-infiltration into this wet substrate. Under in vivo conditions, the solvent
may be diluted because of repeated exposure of the material to the atmosphere, or concentrated
because of separation of the bonding liquids into layers within the bottle. The purpose of this study
was to investigate the effect of different concentrations of ethanol (1050%) on infiltration of the
adhesive resin and collagen fibril encapsulation in the adhesive/dentin interface using light
microscopy, micro-Raman spectroscopy, and scanning electron microscopy. The results indicated
that under wet bonding conditions the hybridization process was highly sensitive to the initial solvent
concentration in the adhesive system. The staining and scanning electron microscopy results showed
that the quality of the interfacial hybrid layer was poor at the lower (10%) or higher (50%) ethanol
content. Micro-Raman analysis indicated that there was a distinct difference in the degree of adhesive
penetration among adhesives containing different concentrations of ethanol. Adhesives containing
10 or 50% ethanol did not realize effective penetration; the penetration of the adhesive monomers
increased dramatically when the initial ethanol content was 30%. The amount of solvents are essential
for achieving effective bonding to dentin.
Keywords
dentin; adhesive; Raman; solvent; interface; hybridization
INTRODUCTION
Bonding of current one-bottle adhesive systems that acid-etch the dentin relies on resin-
infiltration and encapsulation of collagen fibrils in the wet demineralized dentin to form the
hybrid layer or resindentin interdiffusion zone. Ideally, this layer/zone is a structurally
integrated resincollagen biopolymer hybrid that provides a continuous and durable link
between the bulk adhesive and dentin substrate. However, upon removal of the dentin mineral
by acid, the demineralized collagen matrix is suspended in water. Under these conditions, the
quality of the resincollagen layer is highly sensitive to the specific wetting characteristics and/
or composition of the adhesive system.
Correspondence to: Y. Wang; e-mail: Wangyo@umkc.edu.
NIH Public Access
Author Manuscript
J Biomed Mater Res A. Author manuscript; available in PMC 2008 November 4.
Published in final edited form as:
J Biomed Mater Res A. 2007 September 15; 82(4): 975983. doi:10.1002/jbm.a.31232.
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The basic ingredients of mostly one-bottle bonding agents are hydrophilic and hydrophobic
monomer mixtures and solvents. The most popular solvents in use today are acetone, ethanol,
and water. Acetone and ethanol are frequently used as the high vapor pressure solvents. The
presence of these solvents is essential for achieving effective bonding to demineralized dentin
substrates, since they can promote wetting of the dentin substrate and displace water that is
within the wet demineralized dentin matrix. Under wet bonding conditions, the type and
concentration of solvent are expected to have a big impact on the ability of the adhesive
components to tolerate water.
Previous studies suggest that solvents have important effects on the bond strength of one-bottle
dentin bonding systems that require separate acid etching.
1-4
These studies indicate that
varying the solvent content affects the resulting bond strength. In one study, it was suggested
that loss of solvent because of repeated opening of bottles might cause lower bond strength of
acetone-based one-bottle bonding agents.
5
However, in another study, when the acetone
content of the adhesive was increased, the microtensile bond strength decreased from the
highest value of 64 MPa (37% acetone) to 38 MPa (67% acetone).
6
The reasons for the
differences in bond strength as a function of solvent content of dentin bonding agents remain
unclear. The authors assigned a reduction in bond strength to interfacial cracks in specimens
with acetonerich bonding agents.
6
It can be speculated that differences in composition and concentration of solvents could affect
the penetration of adhesive bonding agents and introduce differences in the structure of the
bond formed at the adhesive/dentin interface. In addition, it is agreed that the presence of
solvents with other ingredients of one-bottle bonding agents must have an optimum
concentration. To date, questions regarding adhesive dentin bonding have mainly been
investigated using bond strength studies in combination with morphological analyses. Very
few techniques are available that can evaluate the effects of solvent content on the penetration
of resin monomers, and interfacial structure of the resin-infiltrated layer. Raman microscopy
has been shown to be a promising analytical technique for studying the composition and
structure of bonding of resin to dentin.
7-14
To understand better the relationship between the
solvent concentration and bonding, the morphology, quality, and chemistry of the interfaces
between dentin and Single Bond (SB) adhesives containing different ethanol concentrations
were studied using staining/light microscopy, scanning electron microscopy (SEM), and
micro-Raman spectroscopy. This study tested the hypothesis that varying the solvent content
of a one-bottle adhesive system would affect the penetration of resin and integrity of the
interface using wet bonding techniques.
MATERIALS AND METHODS
Adhesive/dentin specimen preparation
Extracted unerupted human third molars stored in 0.96% w/v phosphate buffered saline (PBS)
containing 0.002% sodium azide at 4C were used. The teeth were collected after the patients'
informed consent was obtained under a protocol approved by the University Adult Health
Sciences IRB. The occlusal one-third of the crown was removed by means of a water-cooled
low-speed diamond saw (Buehler, Lake Bluff, IL). A smear layer was created by abrading the
dentin with 600 grit SiC under water for 30 s. The prepared dentin specimens were selected
for treatment with Single Bond (SB) adhesive (3M ESPE, St Paul, MN) containing different
concentrations of solvents. The procedure to make SB adhesive system with different ethanol
contents is as follows: the adhesive resin was taken from SB adhesive bottle and allowed to
evaporate in a dark box. The weight loss was monitored until no loss was recorded. At the same
time, FTIR spectra of the above resins were detected by PerkinElmer Spectrum One
spectrometer in the ATR sampling mode, so that OH band of ethanol at 1040 cm
1
was
tracked until the peak intensity no longer decreased. After the solvent in SB adhesive was
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completely evaporated, the ethanol content of the original bottle was calculated to be 32.5%
(wt) based on weight loss method. Then 10, 30, and 50% (wt) solutions were prepared after
the appropriate amount of ethanol added and the mixtures were shaken overnight. These
adhesive mixtures were applied to the above prepared dentin specimens using wet bonding
technique according to manufacturer's instructions. The dentin was etched with 35%
phosphoric acid gel and rinsed with water; then blotted with absorbent paper to leave a visibly
moist surface. Two consecutive coats of a bonding agent were applied with a fully saturated
brush. The surface was gently dried for 5 s with an oil-free, moisture-free air spray (18 psi).
After air-drying, the adhesive coated dentin surfaces were light cured for 20 s using a
conventional halogen light unit (Spectrum light, Dentsply, Milford, DE). These specimens
were stored for 24 h in PBS at 25C before sectioning. The treated dentin surfaces were
sectioned perpendicular and parallel to the bonded surface.
Differential staining technique
The rectangular, 10 2 1.5 mm
3
, slabs of the three adhesives dentin interface specimens
were mounted on a methacrylate support and 5-m thick sections were cut from the face of the
slab using a tungsten carbide knife mounted on a Polycut S sledge microtome (Leica,
Germany). Following recovery of the microtomed sections, the remaining fraction of the
adhesive/dentin interface slabs was used for micro-Raman spectroscopic analysis and field
emission scanning electron microscopy. Thus, the same slab was used for light microscopic,
micro-Raman, and SEM analyses. Differential staining was accomplished with Goldner's
trichrome
15,16
and the sections were examined and photographed at 100magnification with
a Nikon E800 light microscope. The width of dentine demineralization and the exposed
collagen layer were determined by measuring directly from photomicrographs whose exact
magnification was established with a stage micrometer.
Micro-Raman spectroscopy
The remaining fraction of above interface slabs was prepared for investigation using micro-
Raman spectroscopy. The micro-Raman spectrometer consisted of an argon ion laser beam
(514.5 nm) focused through a 60Olympus water immersion objective (NA 1.2) to a 1.5
m beam diameter. Raman spectra were acquired at positions corresponding to 1 m intervals
across the adhesive/dentin interface using the computer controlled xyz stage with a minimum
step width of 50 nm. Two consecutive scans of spectra (with 90 s accumulation time each)
were obtained from each site. Multiple sites across the interface of each specimen were
examined spectroscopically. The laser power was 7 mW. Since the micro-Raman technique
is nondestructive, these same specimens were available for analysis using SEM.
Scanning electron microscopy
Following micro-Raman analysis, the specimens described earlier were prepared for SEM
examination. To evaluate the presence of interface and resin tags, the specimens were subjected
to 30 s of 5N HCl, washed with water, followed by soaking in 5% NaOCl for 30 min. After
drying, the prepared specimens were mounted on aluminum stubs and sputter coated with
20 nm of gold-palladium. Specimens were examined at a variety of magnifications and tilt
angles in a Philips XL30 ESEM-FEG (Philips, Eindhoven, Netherlands) at 10 kV.
RESULTS
Staining microscopic technique
Representative light micrographs of Goldner's trichrome stained sections of the adhesive/
dentin interface are shown in Figures 1-3. Using these trichrome differential stains, mineralized
dentin collagen usually is stained green, unprotected demineralized collagen/protein stains red
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and pure adhesive is either stained pale beige or remains unstained. If the adhesive does not
penetrate the full depth of the demineralized layer or does not envelop the collagen/protein,
the Goldner's stains interact with the exposed collagen causing it to appear red. Representative
micrographs of stained adhesive/dentin specimens that were treated with the SB adhesive
containing 10% ethanol are shown in Figure 1. A spotted, discontinuous red layer is clearly
seen between the unstained adhesive and the green stained mineralized dentin. The width of
this red layer was about 3.1 m. It was also noticed that a thin green line was seen on the top
of the dentin surface [arrows, Fig. 1(B)]. The overall interface lacks structural integrity;
separation was noted between the adhesive and dentin layer. Representative micrographs of
stained dentin sections treated with the SB adhesive containing 30 and 50% ethanol are shown
in Figures 2 and 3, respectively. For both cases, a uniform, continuous, red layer distinct from
either the adhesive or dentin is visible along the length of the adhesive/dentin interfaces. The
width of both the red layers was similar, about 6.5 m. The interfacial zone shows orange-red
color when it is treated with SB containing 30% ethanol. The color of the interfacial zone is
dark red when treated with SB containing 50% ethanol. The difference in color represents the
extent of exposed collagen at the interface. The dark red color indicates that the exposed
collagen remains unprotected and thus, is totally available for reaction with the stains. The
orange color indicates the resin-infiltrated layer where exposed collagen was slightly more
encapsulated with adhesive.
15-17
Scanning electron microscopy
Representative SEM micrographs of the dentin interfaces with SB adhesive systems containing
10, 30, and 50% ethanol are shown in Figures 4-6. The common exposure technique, in which
the sectioned adhesive/dentin interface specimen was treated with 5N HCl (30 s) followed by
5% NaOCl (30 min), was used to reveal the adhesive penetration into the dentin. Representative
SEM micrographs of cross sections of adhesive/dentin specimens that were treated with SB
adhesive containing 10% ethanol after the acid/bleach treatments are shown in Figure 4. Short,
funnel-shaped resin tags were clearly observed in the 10% ethanol specimens by this SEM
evaluation. However, it was difficult to reveal the microscopic presence of an acid/bleach
resistant hybrid layer in the specimens. In addition, a separation between the adhesive layer
and the top of dentin was noted [Fig. 4(A)]. For the specimens treated with SB adhesive
containing 30% ethanol, the adhesive penetrated into the dentin and formed a well-defined
acid/bleach resistant hybrid layer (Fig. 5). Resin tags were longer, and also show small lateral
branches. For the specimens treated with SB adhesive containing 50% ethanol, a thick layer
was observed (Fig. 6). However, the surface of the hybrid layer was irregular, with a very
rough, porous appearance, with sites of incomplete adhesive penetration readily identified in
the micrographs. Adhesive tags were short and irregular (Fig. 6).
Micro-Raman spectroscopy
Representative micro-Raman mapping spectra of the dentin interfaces with SB adhesives
containing 10, 30, 50% ethanol are shown in Figure 7(AC), respectively. All spectra were
recorded from 8751785 cm
1
, which spans the fingerprint region associated with adhesive,
collagen, and mineral. The peaks associated with the adhesive occur at 1720 cm
1
(carbonyl),
1609 cm
1
(phenyl C=C), 1113 cm
1
(COC); the major peaks associated with the collagen
appear at 1242 cm
1
(amide III), 1273 cm
1
(amide III), 1453 cm
1
(CH
2
), and 1667 cm
1
(amide I). Those spectral features associated with the mineral occur at 961 (PO symmetric
stretch) and 1072 cm
1
(carbonate).
As shown in Figure 7, the first three spectra were acquired from pure adhesive. Peaks associated
with the adhesive and collagen components of dentin were noted in the fourth spectrum. The
Raman peak of the PO group in the 11th or 12th spectrum suggested that this represented
the bottom of the demineralized dentin layer. Dentin was demineralized to a similar depth for
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the dentin specimens treated with adhesives containing 10, 30, 50% ethanol. Overall, the
intensity of the Raman bands associated with the adhesive (1113, 1609, 1720 cm
1
) decreased
as a function of depth, indicating the gradual decrease of adhesive penetration into the
demineralized dentin. In situ spectra recorded at the second micrometer positions of the dentin
interfaces with SB adhesives containing 10, 30, 50% ethanol are shown in Figure 8. Major
spectral changes have been marked with arrows. In comparison of these spectra, we note that
the bands associated with collagen (1667 cm
1
) were dominant in the 10% ethanol specimens,
while the features associated with adhesive (1720 and 1609 cm
1
) were dominant in the 30%
ethanol specimens. The contribution from spectral features associated with the adhesive in the
50% ethanol specimens were decreased when compared with that in the 30% ethanol
specimens.
The ratios of the relative integrated intensities of the spectral features associated with the
adhesive and collagen were calculated, to determine differences in adhesive penetration as a
function of spatial position across the interfaces. The COC in BisGMA monomer (1113
cm
1
) and the CH
2
in HEMA/BisGMA (1453 cm
1
) were used to monitor the concentration
of the adhesive monomers and the amide I peak (1667 cm
1
) was selected for collagen. Because
of the overlapping of the collagen amide I peak with adhesive peaks, difference spectral method
was used for peak area measurement.
12,18
Figure 9 shows the ratios of 1113/1667 as a function
of spatial position across the dentin interfaces with adhesives containing 10, 30, 50% ethanol.
All showed a gradual decrease, while there were differences in the ratios of 1113/1667 as a
function of position. The ratios of 1113/1667 were the highest at each position for SB adhesive
containing 30% ethanol, and were the lowest for SB adhesive containing 10% ethanol.
Figure 10(AC) represent the adhesive penetration and degree of dentin demineralization as a
function of depth for SB adhesive containing different contents of ethanol. The ratios of the
relative integrated intensities of the spectral features from the mineral (961 cm
1
, PO) and
collagen (1453, CH
2
) (mineral/matrix ratios) were used to measure the extent of dentin
demineralization. Using this technique, the interfacial profile of adhesive penetration and
depth/degree of demineralization were observed clearly. As shown in Figure 10, dentin was
demineralized to a similar depth of 78 m, indicating well-controlled etching process. The
profiles of adhesive infiltration were totally different for these adhesives containing different
ethanol content. When adhesive contains only 10% ethanol, there was a very limited infiltration
of adhesive monomers (little BisGMA monomer) into the demineralized dentin. There was a
demineralized zone with little contribution of both the adhesive monomers and mineral [Fig.
10(A)]; this zone of exposed collagen measures 4 m (from the 4th to 8th m). When adhesive
contains 30% ethanol, the penetration of HEMA/BisGMA resin and BisGMA monomer
increased dramatically when compared with adhesive containing 10% ethanol. The zone with
little contribution of the adhesive and mineral was narrowed to 12 m [Fig. 10(B)]. The
penetration of adhesive monomers decreased when the ethanol content in the adhesive
increased to 50% [Fig. 10(C)].
DISCUSSION
The hybridization process is very complex and affected by many factors during dentin bonding.
19,20
Thus, it is desirable that multiple structural and chemical characterizations of an interface
can be done on the same specimen. In this study, direct and comprehensive information
regarding morphology, quality, and chemistry of the interfaces between dentin and adhesives
containing different ethanol concentrations was obtained using staining/light microscopy,
SEM and micro-Raman spectroscopy. This characterization protocol allows us to complete
complementary, physicochemical analyses on the same interface specimens. The results of this
investigation indicated that under wet bonding conditions the hybridization process was highly
sensitive to the solvent concentration in the adhesive system.
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The morphology and properties of the adhesive/dentin interfacial layer are highly affected by
the solvent content in the adhesive. At the lower initial ethanol content (10%), the quality of
the hybrid layer was very poor (Fig. 1), and the hybrid layer formed with this adhesive system
was not resistant to the acid/bleach treatments (Fig. 4). Some areas of de-bonding occurred at
the interface between the hybrid layer and the adhesive. The gaps or separations were possibly
related to water that had penetrated from the underlying dentin. Previous authors have similarly
reported reduced bond strength values with reduced solvent content, that is, Reis et al. reported
that the micro-tensile bond strength values of resindentin specimens were significantly
reduced when adhesives were applied to moist dentin without their solvents.
3
The quality of the hybrid layer was improved at the higher initial ethanol content (30 and 50%).
A uniform, acid-resistant layer was observed for these specimens (Figs. 2,3,5,6). However, the
quality of the hybrid layer in 30% ethanol specimens was better than that of 50% ethanol
specimens. This difference may be related to a variety of factors including evaporation of the
high initial content of solvent that leads to porous hybrid layers. Results from previous studies
have indicated that increasing the initial content of acetone in one-bottle bonding agents
decreased their micro-tensile bond strength.
6
The higher initial solvent content (67%) resulted
in thinner adhesive layers and might leave residual solvent in the adhesive resin, which in turn
lead to pores in the cured adhesive and interfacial layers.
6,21
Our morphologic results were
consistent with these previous bond strength studies.
Micro-Raman results indicated that there was a distinct difference in the degree of adhesive
penetration among Single Bond (SB) adhesives containing three different concentrations of
ethanol. Adhesive monomers containing 10% ethanol resisted penetration into the wet
demineralized dentin matrices. The penetration of these adhesives monomers increased
dramatically when the initial ethanol content was increased to 30%. It is postulated that the
inclusion of ethanol decreased the viscosity of the adhesive solution, allowing better
penetration. In addition, because ethanol has a water-displacing effect, the impact of water on
the penetration of relatively hydrophobic adhesive components into the wet demineralized
dentin matrix is likely reduced. When the adhesive only contains 10% ethanol, the relatively
high viscosity of the adhesive solution resulted in poor penetration of adhesive monomers into
the wet demineralized dentin layer. Lower ethanol content will also cause thicker adhesive
layers. Apparently the ethanol content is not adequate to displace the residual water within the
demineralized dentin matrix and thus, the penetration of the hydrophobic components is
impeded. With increasing ethanol content, the viscosity of the adhesive solution decreases and
the penetration of the adhesive monomers into the wet demineralized dentin layer is enhanced.
However, when the ethanol content was higher (50%), the penetration of adhesive monomers
decreased again; which may be due to component dilution, or also due to greater chemical
dehydration with higher concentrations of ethanol that could have partially collapsed the
nanochannels between fibrils.
22
The differences in solvent concentrations of bonding systems determine their wetting
capability. There must be an optimum concentration of solvents with other ingredients of the
bonding agent. Based on the above morphologic and Raman spectroscopic results, 30% ethanol
appears to be the optimum concentration for the adhesive formulation used in this study. Our
morphological analyses in combination micro-Raman studies provide promising
characterization techniques for evaluating the dentin bonding performance of adhesive
systems. Most current bonding agents are mixtures of hydrophilic/hydrophobic monomers and
solvents. The selection and composition of these ingredients have dramatic effects on the
structure and durability of the bond formed at the adhesive/dentin interface. The formulation
of adhesive systems has mainly been determined based on the results of bond strength studies
in combination with SEM morphologic analyses. This protocol only provides a single measure
at one point; it provides a gross overview as opposed to specific identification of the site that
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experiences breakdown. In addition, many factors from dentin substrates and adhesives could
affect the final bond strength values. The research protocol used in this study could provide a
remarkable tool for the development of dentin bonding agents. The differences in quality and
adhesive penetration of the interfacial zone were clearly observed for adhesives with difference
concentrations of solvent. Direct measurements of the complete chemical profile and
monomer/mineral distribution across the adhesive/dentin interfaces will offer critical data that
is integral to the appropriate selection and determination of adhesive composition.
The results shown in this study also have important clinical relevance. Solvents such as acetone
and/or ethanol are volatile solvents that could easily evaporate from bottles during use of
adhesive systems in the clinical environment. The concentration of solvents may change as a
function of time. Several authors have raised concerns as to the effects of solvent evaporation
in one-bottle adhesives.
5,23
In an in vitro study, the effects of repeatedly opening of bottles
on dentin shear bond strength were evaluated. The acetone-based adhesive had significantly
lower mean bond strength because of the evaporation of the acetone after 3 weeks of simulated
use.
5
In another study, the four one-bottle bonding agents were tested for phase separation of
the liquids into layers within the bottle.
24
Since the liquids (resin monomers and solvents) in
the bottles have different densities, phase separation can easily occurs within 12 h, which can
even be visualized by the naked eye. In the clinic, if dentists do not shake the bottles before
each use, agents containing mostly solvent will be applied to the dentin surface; after such
several applications, then primarily resin with less solvent will be applied to the dental cavity.
Our results indicated that the amounts of solvent were essential for achieving effective bonding
to dentin. Solvent content has a substantial effect on resin infiltration and the interfacial
structure of the hybrid layer. Adhesives containing higher or lower initial solvent content did
not realize effective penetration and the integrity of the bond formed at the adhesive/dentin
interface was severely compromised. Dentists must pay careful attention to the volatile
characteristics and the differences in density of the ingredients of bonding agents. All bottles
must be shaken thoroughly to obtain a uniform mix before applying to the tooth structure. In
addition, attention should be paid to minimize solvent loss during clinical use by immediately
replacing caps on solvent-based dentin bonding agents.
Acknowledgements
This work is a contribution fromthe UMKC Center for Research on Interfacial Structure and Properties (UMKC-
CRISP).
Contract grant sponsor: National Institute of Dental and Craniofacial Research, National Institutes of Health; contract
grant number: R01DE14392, K25DE015281, K23DE/HD00468
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Wang et al. Page 8
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Figure 1.
Representative light micrographs of the dentin interfaces with SB adhesive containing 10%
ethanol. The overall interface lacks structural integrity; a spotted, discontinuous red layer is
clearly seen between the adhesive and dentin (A), separation is also noted between the adhesive
and dentin layer (B). [Color figure can be viewed in the online issue, which is available at
www.interscience.wiley.com.]
Wang et al. Page 9
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Figure 2.
Representative light micrograph of the dentin interfaces with SB adhesive containing 30%
ethanol. [Color figure can be viewed in the online issue, which is available at
Wang et al. Page 10
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Figure 3.
Representative light micrograph of the dentin interfaces with SB adhesive containing 50%
ethanol. [Color figure can be viewed in the online issue, which is available at
Wang et al. Page 11
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Figure 4.
Representative SEM micrographs of acid-bleach treated dentin interfaces with SB adhesive
containing 10% ethanol. (A) 2000; (B) 4000.
Wang et al. Page 12
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Figure 5.
Wang et al. Page 13
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Figure 6.
Wang et al. Page 14
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Figure 7.
Representative micro-Raman mapping spectra of the dentin interfaces with SB adhesives
containing 10% (A), 30% (B), 50% (C) ethanol. [Color figure can be viewed in the online issue,
which is available at www.interscience.wiley.com.]
Wang et al. Page 15
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Figure 8.
Raman spectra recorded at the second micrometer positions of the dentin interfaces with SB
adhesives containing 10% (A), 30% (B), 50% (C) ethanol. [Color figure can be viewed in the
online issue, which is available at www.interscience.wiley.com.]
Wang et al. Page 16
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Figure 9.
Adhesive penetration as a function of depth across the dentin interfaces with adhesives
containing 10, 30, 50% ethanol. [Color figure can be viewed in the online issue, which is
available at www.interscience.wiley.com.]
Wang et al. Page 17
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Figure 10.
Adhesive penetration and degree of dentin demineralization as a function of depth for SB
adhesive containing different contents of ethanol. [Color figure can be viewed in the online
issue, which is available at www. interscience.wiley.com.]
Wang et al. Page 18
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Effect of solvent content on resin hybridization in wet dentin

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