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How wet should dentin be? Comparison of methods to remove excess water
during moist bonding

Article  in  The journal of adhesive dentistry · October 2001

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Gisele Damiana da Silveira Pereira Luis Alexandre Maffei Sartini Paulillo

Universidade Gama Filho University of Campinas
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 How Wet Should Dentin Be?
Comparison of Methods to Remove
Excess Water During Moist Bonding
Gisele Damiana da Silveira Pereiraa/Luis Alexandre Maffei Sartini Paulillob/
Mario Fernando De Goesc/Carlos Tadeu dos Santos Diasd

Purpose: The aim of this study was to evaluate the shear bond strength of two adhesive systems when ap-
plied on dentin surfaces with different degree's of wetnesS.

Materials and Methods: Two-hundredten dentin specimens were used. After conditioning with 35% phos-
phoric acid gel and washing, seven,.rnethods'ofClryirig«en,tHi were used: 30 s air spray (groups 1 and 2), 5
" -" !",·/r)"i', t oJt I,";,

S air spray (groups 3 and if), dry cotton pellets' (groups '7 and 8), wet cotton pellets (groups 9 and 10), mi-

crobrush (groups 11 and 12), absorbent paper (groups 13'and 14). The last group was not dried; the
dentin surfaces were left overwet (grQUPS5 and'6): P.rim~ & Bond 2.1 adhesive was applied on the odd-
numbered groups and,Scotchbond Multi ..purpQseon tH,eev~n-numbered groups. Z100 composite cylin-
ders were bonded to tM ',;Idhesive ~l!ld tli~,spedmei:lsw~resubjected toa shear bond test.
;,: "~~,io". \oJ: ;-!~.>;,:i;" rl
-. • -. __:~" _ "
Results: The Least-sqQa're~'Means testwasuseB't9 compare the following results, where different letters
indicate;significantly diff,€rent mElar 'va'lo~;'Group 9 ~(~~)~;':}23:2- MP~ (a); G3 = 21.3 MPa (ab), G2 = 19.5
MPa (be), G10 = 18.6 MRa (-be),G14 = 16(:{NPa (Cd),:G8'''; ~6.1.'MPa (cd), G4 = 14.6 MPa (de), G13 = 14.0
MPa (de), G11 = 13.9 'MPa ~de);
(;.<7' = '13;5 ~p~ (de)i GI1~l,~~±2:f MPa (~), G1 = 8.2 MPa (f), G.5 = 2.7 MPa
(g), G6 = 2.4 MPa (g). ' .' ", ,"-

Conclusion: The adhesidri values were affeciE;Gi,both by the degree of dentin wetness and by the adhesive
systems. .i

ne of the principal aims of restorative dentistry
O is to obtain dental materials capable of bonding
a Professor of Restorative Dentistry, Gama Filho University, School of
Dentistry, Rio de Janeiro, Brazil, and Postgraduate student, UNI-
CAMp, Piracicaba School of Dentistry, Gampinas State University,
Sao Paulo, Brazil.
b Professor of Restorative Dentistry at UNICAMp, Piracicaba School
of Dentistry, Campinas State University, Sao Paulo, Brazil.
e Professor of Dental Materials at UNICAMP, Piracicaba School of
Dentistry, Campinas State University, sao Paulo, Brazil.
d Professor, Mathematics Department, Luiz de Queiroz Agronomy
School, Sao Paulo State University, USP, Piracicaba, Sao Paulo,
Brazil.
Reprint requests: Gise/e Damiana da Silveira Pereira, Moraes Bar-
ros, 1336\101, Bairro Alto, Piracicaba, Sao Paulo, Brazil, CEP-13416-
740. Tel: +55-19422-7902, Fax: +55-19430-5218, e-mail:
gise/edamiana@yahoo.com
effectively to dental tissues in order to minimize mi-
croleakage and subsequent secondary caries,17
In 1955, Buonocore2 proposed that acid etch-
ants could be used to alter the enamel surface and
make it more receptive to adhesion. Acid etching
enamel creates a microporous layer ranging from 5
to 50 IJm deep. When a lOW-Viscosity resin is ap-
plied, it flows into the microporosities and polymer-
izes, forming a micromechanical bond with the
enamel. Adhesion of restorative materials to ena-
mel has been very successful, and its reliability is
verified by the absence of marginal leakage and by
high adhesive bond strengths that make several
conservative and esthetic restorative procedures
possible,17
On the other hand, dentinal adhesion has proved
to be more difficult and less predictable.10 Much of
the difficulty in bonding to dentin results from its
structure, which is morphologically heterogeneous
and physiologically dynamic.10 Its composition by
weight is 20% water, 30% organic matrix, and 50%
inorganic hydroxyapatite,10.17 arranged in intertubu-
lar and peritubular matrices, which form the tubule
walls from which pulp fluids emerge and keep
dentin constantly moist.10 Dentinal adhesion is fur-
ther complicated by the formation of the smear
layer which appears on the dentinal surface when
the dentin is cut or ground.10
Adhesive systems have undergone a great evolu-
tion,10.11 with major improvements in dentinal
bonding occurring when hydrophilic monomers and
organic solvents were added to primers and adhe-
sives, enabling their use on a moist dentin sub-
strate.6,7 When these adhesive systems are applied
on conditioned dentin,7.16 a hybrid layer composed
of collagen fibrils and residual hydroxyapatite crys-
tallites encased in resin13 is formed. The hybrid
layer recovers much of the resistance and rigidity19
of the original mineralized dentin, and it is the main
bonding mechanism of most current dentin adhe-
sive systems.16,19
The bond strength of a dentin adhesive may rely
on its ability to completely replace the dissolved hy-
droxyapatite with polymerized resin.15.17 If this does
not happen, an exposed layer of collagen fibrils not
impregnated by resin14.15.17and containing
nanometer-sized porosities19 within the hybrid layer
may be formed. These may serve as critically-sized
defects that promote fracture propagation and de-
crease the resistance and durability of the adhe-
sion.14.15
The maintenance of a moist dentin surface after
acid conditioning is of major importance for optimal
development of a uniform hybrid layer,6-8.14,15,18.22
as the organic solvents contained in the primers act
as water chasers, displacing water and carrying the
resin monomers into the demineralized dentin,17 fa-
voring hybridization.6 On the other hand, if the
etched dentinal surface is desiccated, the interac-
tion of the above elements does not occur.7 The
primer is deposited on the dentinal surface without
diffusing into the underlying collagen network.7
The removal of hydroxyapatite crystals by dentin
conditioning exposes the collagen fibrils of the ma-
trix. The separation of the fibrils into a meshwork
only occurs when water is present.20-22 Dehydration
of the conditioned dentin surface with air jets can
collapse the collagen fibril meshwork,5,9 causing
the interfibrillar spaces to disappear and thereby in-
hibiting penetration of the primer. Thus, the me-
chanical retention is reduced.5.9.20-22 Nevertheless,
the integrity of the fibril network is partially recov-
ered by rewetting the substrate.5.9
However, the dentinal surface should not be
overwet, as excess water can dilute the primer and
render it less effective. Excess water can promote
phase separations in the primer and the formation
of resin globules, which prevent adequate adhesive
wetting, infiltration, and polymerization.15.20.22 As a
result, the quality of the adhesive interface is re-
duced.15.22
The importance of the composition of adhesive
systems and the drying method used in the bonding
procedures are evident, as they favor the formation
of a homogeneous and uniform hybrid layer, en-
abling an effective bond between dentin and
restorative materials,12 The aim of this study was to
evaluate the influence of seven drying methods on
the shear bond strength of two adhesive systems to
acid-conditioned dentin.
One hundred-five caries-free third molars were se-
lected. The teeth were cleaned and stored in 0.9%
saline solution at 4°C and used within one month
of extraction.
An initial cut was made perpendicular to the
long axis of the molars, 1 mm below the cemento-
enamel junction, using diamond disks with double
sharp-edged facettes in a low-speed handpiece
under air-water spray to remove the roots. A second
cut was made in the mesiodistal direction, dividing
each crown into two halves, thereby creating 210
coronal fragments that were embedded in poly-
styrene resin. When the resin was fully polymerized,
the resulting cylindrical blocks were removed from
the molds. Subsequently, the buccal, palatinal, or
lingual enamel surfaces were ground off using 200-
and 320-grit wet silicon carbide (SiC) abrasive
paper until a flat superficial dentin area was ex-
posed. Final polishing was carried out using 600-
and 1000-grit wet SiC abrasive paper.
After being coded, the samples were randomly
assigned to 14 experimental groups of 15 speci-
mens each. Due the large number of specimens,
adhesive procedures were done in blocks, with
each block containing one sample of each experi-
mental group (total = 15 blocks). Adhesive tape with
a 3-mm-diameter hole was used to demarcate the
adhesion area, and was placed on the dentin prior
 Table 1 One-way ANOVA for shear bond strength means
Source OF
Model 27
Error 160
Total 187
CV 28.4%
DF: degrees of freedom; SQ: sum of squares; MQ: mean square; F: F value; CV: coefficient
to the application of the subsequent treatments. All
the specimens were conditioned with 35% phos-
phoric acid gel (3M Dental Products Division, St
Paul, MN, USA) for 15 s and rinsed with distilled
water for 20 s. Once this was done, one of the dry-
ing methods was applied according to the following
experimental groups. Groups 1 and 2: The dentin
was dried with an oil- and dust-free air blast for 30
s parallel to the surface at a distance of 1 cm.8
Groups 3 and 4: The dentin was dried with oil- and
dust-free air for 5 s parallel to the surface at a dis-
tance of 10 cm.8 Groups 5 and 6: The dentin sur-
face remained overwet and no drying method was
applied. Groups 7 and 8: The dentin was dried with
a dry hydrophilic cotton pellet gently applied to the
surface for 10 s. Groups 9 and 10: The dentin was
dried with a moist hydrophilic cotton pellet gently
applied to the surface for 10 s. Groups 11 and 12:
The dentin was dried using a microbrush (Dentsplyj
Caulk, Milford, DE, USA) gently applied to the sur-
face for 10 s. Groups 13 and 14: The dentin sur-
face was dried by using small pieces of absorbent
filter paper gently applied to the surface for 10 s.
Immediately after drying, the adhesive Prime &
Bond 2.1 (DentsplyjCaulk) was applied in the odd
groups and the adhesive Scotchbond Multi Purpose
(3M Dental) was applied in the even groups, accord-
ing to the respective manufacturer's instructions.
A split teflon matrix having a 3-mm-diameter cen-
tral perforation was positioned over the adhesive
area of the samples, and the composite resin Z100
(3M Dental, shade A-2) was applied in incremental
layers 2 mm thick. Each layer was photopolymer-
ized for 20 s. The teflon matrix was then carefully
separated and a final polymerization was carried
SO MO F PR>F
6100.94146 225.96070 13.04 0.0001
2771.81846 17.32387
8872.75992
of variation.
cylinder. All the specimens were created under sta-
ble temperature conditions (23°C) and 55% humid-
ity. After bonding, the specimens were immersed in
distilled water and stored for 7 days at 3rC ± 1°C
prior to the shear bond strength test.
The tests were performed on a universal testing
machine (Emic-DL 500, Ind Bras, Sao Paulo, Brazil),
at a crosshead speed of 0.5 mmjmin.3 The shear
load was applied by means of a chisel with a 0.5-
mm-wide blade, positioned near the base of the
composite cylinder, as close as possible to the ad-
hesive interface. The load (in MPa) necessary to
fracture each specimen was recorded.
The means of shear bond strengths were calcu-
lated for each group (group = dentin wetness and
adhesive system). The shear bond strengths for var-
ious dentin wetnesses for each bonding system
were compared using one-way ANOVA (Table 1 and
2) and the Least-Squares Means multiple compari-
son test (Table 3) at a = 0.05.
A contrast analysis test was done to compare the
bond strengths results of the two adhesive systems
(Table 4) at a = 0.05.
Statistical analysis of the data by one-way ANOVA
showed a statistically significant F value at p =
0.0001. ANOVA decomposition showed a statis-
tically significant difference for the group bond
strengths values, but no effect of blocks (p = 0.217,
Table 2). The Least-Squares Means test at a = 0.05
was used to compare the statistical difference
among the experimental groups (Table 3 and Fig 1).
 Table 2 One-way ANOVA analysis decomposition to evaluate the block
and group effects

Source OF Type III SS MQ F Value PR>F

Block 14 313.48226 22.39159 1.29 0.2172

Group 13 5573.82919 428.75609 24.75 0.0001*

* Mean values were significantly different (p < 0.0001).

DF:degreesof freedom; MQ: mean square.

Table 3 Least-Squares Means test for shear bond stregths (MPa) of the
groups

Group Mean Shear Bond (MPa) LS Means

G9 23.2 a* Prime & Bond 2.1, moist cotton pellet

G3 21.3 ab Prime & Bond 2.1, air dried 5 s
G2 19.5 bc SBMP, air dried 30 s
G10 18.6 bc SBMP, moist cotton pellet
G14 16.3 cd SBMP, absorbent paper
G8 16.1 cd SBMP, dry cotton pellet
G4 14.6 de SBMP, air dried 5 s
G13 14.0 de Prime & Bond 2.1, absorbent paper
G11 13.9 de Prime & Bond 2.1, microbrush
G7 13.5 de Prime & Bond 2.1, dry cotton pellet
G12 12.1 e SBMP, microbrush
G1 8.2 f Prime & Bond 2.1, air dried 30 s
G5 2.7 g Prime & Bond 2.1, overwet
G6 2.4 g SBMU, overwet
a= 0.05
*Different letters indicate significantly different mean values (p < 0.05).

Table 4 Contrast analysis test for adhesive systems shear bond

strengths

OF Contrast MQ F Value PR>F

SBMP vs P&B 2.1 1 6.97487 6.97487 0.40 0.5266*

* Mean values were not statistically different (p > 0.05).

tistical difference between mean values of Prime &
Bond 2.1 and Scotchbond Multi Purpose.
The box-plot diagram (Fig 1) is a schematic repre-
sentation of the distribution of bond strength val-
ues. The vertical lines in the box mark the 25th,
50th, and 75th percentiles of the data. The 50th
percentile is called the median, which is repre-
sented in the box by a horizontal line, and the 25th
and 75th are called quartiles. The '+' sign repre-
sents means, and asterisks represent outliers.1,25
For Prime & Bond 2.1, the highest bond strengths
were obtained when dentin was dried with moist
cotton pellet (23.2 MPa). Interestingly, similar bond
strengths were obtained when dentin was dried
Fig 1 Box-plot diagram for mean shear bond strengths (MPa) of the groups. G = groups, P&B = Prime & Bond 2.1, SBMP =
Scotchbond Multi Purpose. 30 s = 30-s air blast, 05 s = 5-s air blast, MC = moist cotton, mB = microbrush, AP = absorbent paper,
DC = dry cotton, OW = overwet. Vertical lines in the box = 25th, 50th and 75th percentiles. Horizontal line in box = median. Hori-
lontallines outside of the box = quartiles. + = means, * = outliers.

with a 5-s air blast (21.3 MPa). For Scotchbond
Multi-Purpose, the highest mean bond strength was
obtained when dentin was dried with a 30-s air
blast (19.5 MPa). For both adhesive systems, the
lowest means were obtained when the dentin sur-
faces remained overwet (G5: 2.7 MPa; and G6: 2.4
MPa).
In spite of the fact that resin adhesion to dentin is
more difficult and less predictable due to its mor-
phology and heterogeneous composition,10 signifi-
cant progress has been achieved after increasing
understanding of the properties the substrate. In
order to obtain a strong and long-lasting adhesion
of resin to dentin, it is important that a dense, ho-
mogeneous, and uniform hybrid layer be formed, re-
gardless of its thickness.3,15 To accomplish this, it
is necessary for the demineralized dentin to be
completely infiltrated by the adhesive, encasing all
the exposed collagen and the hydroxyapatite.14,15,17
However, several factors can jeopardize monomer
diffusion.14 The amount of surface moisture is ex-
tremely important for hybridization of dentin. Higher
bond strength can be achieved under moist condi-
tions than dry.5-7,21,23The results obtained in the
present study support the findings of other studies,
in which the drying methods that kept the dentin
surface moist and the adhesive systems that rewet
the dehydrated substrate were the ones that ob-
tained the highest shear bond strength values.3,4,6
This is substantiated by the bond strength va-
lues obtained in Group 9 (23.2 MPa), in which acid-
etched dentin was dried with moist cotton pellets
prior to the application of Prime & Bond 2.1. This
drying method left the dentin visibly moist. We
speculate that the water occupying the interfibrillar
spaces of intertubular dentin was responsible for
maintaining the collagen network in an expanded
state, thereby preserving the porosity necessary for
resin infiltration into intertubular and tubular
dentin. The acetone present in the primer interact-
ed with this water.3-5,7,22 This interaction presum-
ably promoted water evaporation and made the
primer and the adhesive spread, penetrate, and
adapt into the open interfibrillar spaces.16
Despite the fact that the results for this group
were the highest values obtained, they did not dif-
fer significantly from the values of group 3 (21.3
MPa). In group 3, the dentin was airdried for 5 s at
a distance of 10 em from the surface prior to the
application of Prime & Bond 2.1. The average bond
strength for this group was lower, probably due to
slight overdrying, which can cause a collapse of the
collagen fibril network,4,5,7 although the degree of
wetness in the two groups seemed to be similar to
the naked eye.
A satisfactory value for adhesive strength was
also obtained in group 2 (19.5 MPa), where the
conditioned dentin surface was dried by an air blast
for 30 s from a distance of 1 em. However, the
Scotch bond Multi Purpose system was applied in
this group; it contains sufficient water to rewet the
dentin, recovering the integrity of the collagen net-
work and its spaces.24 Once dried, collapsed colla-
gen needs water to lower the modulus of elasticity
enough to let it re-expand and enable the diffusion
of monomers into the collagen fibril network, form-
ing the hybrid layer.5,9,20,21,23,24 The same result
was not observed when the Prime & Bond 2.1 was
applied to similarly treated dentin (Group 1). Appar-
ently, the acetone present in this system was not
capable of expanding the collapsed matrix. Presum-
ably, the monomers could not diffuse into the dried
sUbstrate,4,9,20,21,24 resulting in the lower values for
adhesion4.9,20,21,24 found in group 1 (8.2 MPa).
These were statistically significantly lower than
those of the other groups (Table 3, Fig 1).
Scotch bond Multi Purpose produced satisfactory
results regardless of how dentin was dried7.24 (air
dried for 30 s, absorbent paper, or dry cotton pel-
lets, G2 = 19.4 MPa, G14 = 16.3 MPa, and G8 =
16.1 MPa, respectively). We believe that the water
content of the primer allowed the collagen fibril net-
work to re-expand to the same degree. These val-
ues were not significantly different from those
obtained in group 10 (18.6 MPa), where the same
adhesive system was applied to a substrate left vis-
ibly moist3 after being dried with moist cotton pel-
lets. Apparently, the hydrophilic monomers in the
Scotch bond Multi Purpose system can tolerate wide
variations in surface moisture.3,6,24 Thus, reliable
adhesion can be obtained when this system is em-
ployed either in moist or dry conditions.6.9.24
When Prime & Bond 2.1 was applied, the bond
strengths obtained with moist substrates (G9 =
23.2 MPa and G3 = 21.3 MPa) were higher (p <
0.05) than with dry substrates (G1 = 8.2 MPa). The
application of Prime & Bond 2.1 to relatively dry
dentin, as in the groups where the absorbent paper
(G13 = 13.9 MPa) or dry cotton pellet was used (G7
= 13.5 MPa), produced significantly (p < 0.05) lower
bond strengths (Table 3). This was probably be-
cause the composition of this system does not in-
clude water, and the drying techniques decreased
the surface water concentration of the dentin to a
point which allowed the primer's organic solvent to
stiffen the collagen network faster than the water
could plasticize ip,9
When the microbrush was used as a drying me-
thod, a moister surface was observed compared to
the previously described conditions. Even though
this situation should have favored the Prime &
Bond 2.1 system,? it resulted in low values of adhe-
sion for both systems (G11 = 13.9, G12 = 12.1
MPa). This might have occurred because there was
excess water on the substrate. Acetone, the volatile
polar solvent found in Prime & Bond 2.1, has the
ability to displace water, although in this case, it
was not capable of evaporating all the excess
water. Consequently, much water remained on the
surface, which may have caused phase changes
and reduced polymerization,21,23 thus reducing the
bond strength values, as exemplified by group 11
(13.9 MPa). This group did not differ statistically
from the average obtained when this adhesive was
applied to the drier substrate of groups 13 (14.0
MPa, absorbent paper) and 7 (13.5 MPa, dry cot-
ton) even though it was visibly wetter. This situation
worsened when the water-containing Scotchbond
Multi Purpose system was applied to wet dentin
that was left "dried" by a microbrush in group 12
(12.1 MPa). The resulting bond strength was proba-
bly due to the large amount of residual water that
was not evaporated prior to polymerization.21,23,24
The worst results in this study were obtained
when no drying method was used and the dentin
was left with excess water on its surface (G5 = 2.7,
G6 = 2.4, Table 3). According to Tay and others,21-23
the presence of excessive water dilutes the primer
of some adhesive systems, and its components
separate into different phases. This leads to the for-
mation of water blisters and micelles of resin which
are located on the adhesive interface, preventing
the penetration of the resinous agent into the
dentin and making hybridization of the demineral-
ized matrix difficult. The presence of water-filled
blisters may promote the degradation of the bond
by hydrolysis of the exposed collagen.21,22
Although both systems had different composi-
tions that resulted in affinity to substrates with dif-
ferent degrees of wetness, the results obtained in
the Contrast Analysis Test (Table 4) of these sys-
tems did not show significant statistical differ-
ences, no matter which drying method was used.
Adhesion is highly influenced by the operator,
who can commit errors during the different stages
of the adhesive procedure, including drying of the
dentin. Thus, adhesive systems that are less mois-
ture-sensitive should be employed, because they
are less technique sensitive.
The highest shear bond strength was achieved with
Prime & Bond 2.1 applied to wet dentin dried with a
moist cotton pellet. However, this value was not sig-
nificantly different from bond strengths obtained
when the same adhesive was applied to the dentin
dried by a 5-s air blast.
The lowest shear bond strengths were obtained
when either adhesive system was applied to over-
wet dentin, and there was no significant difference
between their bond strengths to overwet dentin (ca
2 to 3 MPa).
Prime & Bond 2.1 showed higher (p < 0.05)
shear bond strength values when applied to dentin
kept moist after the drying process than when it
was applied to the drier dentin.
Scotch bond Multi Purpose achieved satisfactory
bond strengths (ca 15 to 20 MPa) not only with
moist dentin but also with drier dentin surfaces,
showing no significant statistical difference be-
tween substrates.
There was no significant statistical difference be-
tween the averages of shear bond strength pro-
duced by Prime & Bond 2.1 and Scotch bond Multi
Purpose adhesive systems when they were com-
pared with each other, independent of the dentinal
drying methods.
This study was supported by the FAPESP Foundation,
97/04569.
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916-921.

HYBRIDIZATION OF DENTAL HARD TISSUES

Nobuo Nakabayashi and David H. Pashley

The hybridization of dentin-a process that cre-

ates a molecular-level mixture of adhesive poly-
mers and dental hard tissues-gives clinicians a
versatile new material, useful in a wide array of
advanced dental treatments. As the first in-depth
exploration of the subject, this book covers the
development, present understanding, and future
research areas of this multifunctional dental mate-
rial. A thorough review of the current literature
rounds out the text.
Valuable for students, researchers, and clini-
cians seeking a greater understanding of resin
hybridization of tooth structure.

Evolution of Dentin-Resin Bonding

Properties of Dentin
Acid Conditioning and Hybridization of
Substrates
4 Characterization of the Hybrid Layer
5 The Quality of the Hybridized Dentin
6 Clinical Applications of Hybrid Layer
Formation

129 pp; 80 iI/us (some in color);

ISBN 0-87417-575-9 C3047; US $401£26

Call +44 (0)2089496087 quintc/lCncc

or Fax +44 (0)2083361484 boolu
Visit our web site http;//www.quintpub.com
Quintessence Publishing Co, Inc

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