Surface Topography: Its Influence on Wetting and Adhesion
in a Dental Adhesive System
J. D. EICK, L. N. JOHNSON, J. R. FROMER, R. J. GOOD, and A. W. NEUMANN
Departments of Dental Materials and Chemical Engineering, State University of New York
at Buffalo, Buffalo, New York 14214, USA and Division of Dental Materials Science,
Faculty of Dentistry, University of Western Ontario, London, Ontario, Canada
The fracture surface between bovine dentin
and enamel and a dental cement was ob-
served at magnifications up to 10,OOOX by
use of the scanning electron microscope.
The topography of the tooth structure
played an important role in the formation of
an adhesive bond and in the fracture pattern
of an adhesive joint, even when cohesive
failure was involved.
Considerable time, money, and effort has
been devoted to the development of an ad-
hesive dental material in recent years. Sev-
eral investigators have pointed out that the
development of an adhesive dental material
would enhance substantially the effective-
ness of dental health care. For example,
such a material would increase the perma-
nency of restorative materials,1 13 and when
used as a protective coating on the occlusal
surfaces of teeth, it could be effective in re-
ducing pit and fissure caries.'4-23 Most
previous investigators have approached this
subject by studying various resin systems to
obtain a permanent adhesive. To date, how-
ever, a completely satisfactory material has
not been developed.
Often it is difficult to explain the behavior
of an adhesive joint by theoretical considera-
tions. Generally, the three major require-
ments for the formation and permanency of
an adhesive bond are (1) intimate contact
must be established between the liquid ad-
hesive and the solid adherend; ie, good wet-
ting must take place; (2) the stress concen-
tration at the interface must be minimum;
Presented in part at the 49th general session of the
IADR, Chicago, III, March 1971.
Received for publication April 15, 1971.
780
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and (3) the attack on the interface by en-
vironmental factors must be minimum.
Parameters such as shrinkage during hard-
ening of the adhesive, the mechanical prop-
erties of the adhesive and adherend, and the
coefficient of thermal expansion of the ad-
hesive and adherend influence the stress
concentration at the interface. In vivo pa-
rameters such as moisture and acid pro-
duced by bacteria attack the adhesive bond.
Most investigators in the field of adhesion
and adhesives agree, at least in principle,
that the process of wetting a solid by a
liquid adhesive to obtain intimate contact is
of primary importance in the development
of an adhesive bond.24 29 In other words, if
good wetting is not achieved, the success of
the adhesive bond will be decreased greatly.
This leads to the question of what param-
eters influence the wetting of a solid by a
liquid. Three major factors are involved.
The first factor is the surface free energy of
the solid and the liquid. This factor is
mainly a function of the chemical composi-
tion and chemical heterogeneity of the
liquid adhesive and the outer surface layer
(~ 10 A) of the solid adherend. For exam-
ple, an organic film adsorbed on the tooth
surface, or debris remaining after cutting
the tooth,8 would influence the wetting pro-
cess and subsequently influence the ad-
hesive bond.28-30 The second factor is the
surface topography of the adherend. The
rugosity of the adherend may promote wet-
ting as a result of capillary pressure effects.
Conversely, the surface may be too rough
and act as a barrier to the flow of the liquid
adhesive, and thus produce air pockets at
the interface, or what is commonly termed a
Vol 5 I No. 3 SURFACE TOPOGRAPHY & WETTING & ADHESlON
20 x
composite surface.)'1-33 The viscosity of the
liquid34 is the third factor.
Of the three major factors that affect wet-
ting, the influence of surface topography
probably is the least understood. It is easy
to see that if a surface is roughened, pro-
ducing more surface area, and if intimate
contact between the adhesive and adherend
is established, the actual adhesive bond will
be stronger because of the increase in sur-
face area. However, there should be some
"ideal roughness" that produces optimum
wetting because of capillary pressure and
yet is not so rough that a composite surface
or a surface with air entrapped at the inter-
face is produced.31 82 The exact topographic
nature of this ideal roughness has not been
established.
The purpose of this investigation was to
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781
FIc 1.-Adhesive interface be-
tween bovine dentin and cement.
contribute to the clarification of the argu-
ments discussed by investigating directly the
surfaces exposed after fracture of a dental
adhesive joint by means of scanning electron
microscopy.?9536"I Furthermore, we intended
to help answer the question of whether the
topography of the adherend plays a role
only in the formation of an adhesive bond,
or whether it also influences the strength of
the adhesive joint.
Materials and Methods
A dental cement* placed on bovine dentin
and enamel under controlled conditions was
used. This cement reportedly37 chelates with
the inorganic phase of tooth structure in the
* Durelon. manufactured by ESPE GmbH,
Seefeld/
Oberbay, W Ger, Liquid Lot No. 105 and Powder Lot
No. 437.
782 LIsCK GET A l J Dent Res Mciv-lone .1972

I
500 x 1000 x

2000 X 5O x
FIG 2. Adhesive interface between bovine dentin and cement.

presence of water and an adhesive bond is
formed.
Samples of bovine enamel and dentin
were surfaced flat through 400 grit with
SiC paper under wet conditions. The pre-
pared tooth surface was placed in a specially
designed jig18 used to minimize stress con-
centrations during sample preparation. A
Teflon disk, one inch in diameter and three-
tenths inch thick with a 5 mm diameter hole
centrally drilled, was used as a die to limit
the spread of the cement on the substrate
surface. The cement was mixed according
to the manufacturer's directions and packed
into the Teflon mold on the tooth surface.
A machine screw was placed 1 mm above
the substrate surface in the cement to act
as an attachment for tensile testing, and the
specimen was stored under wet conditions at
37 C for 24 hours. The adhesive bond was
then tested in tension by use of an Instron
testing machine operated at a crosshead
speed of 0.05 cm/ minute. The procedure
described by the Subcommittee on Standard
Test Methods for Direct Filling Resins,
IADR8' for preparation and testing of the
specimens was followed.
Five samples using bovine enamel and five
samples using bovine dentin were tested. The
specimens were maintained in water at 23 C
after tensile testing to minimize dimensional
changes of the cement during storage and
then vacuum-coated with a 200 to 400 A
layer of gold (Au)-palladium (Pd) immedi-
ately before being placed in the scanning
* Instron Corp., Canton, Mass.

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VoI 51 NO. 3 SURFACE TOPOGRAPHY & WETT IN\G & ADHESION 783

iII

iA!

500 x 1000 x

2000 x 5000 x
FIG 3. Adhesive interface between bovine dentin and cement.

electron microscope. A scanning electron generally more cement remaining on the

microscope1 operated at 10 kv and with a
specimen stage tilt of 450 was used to ob-
serve the fractured surfaces up to magnifica-
tion l0,OOOX.
Results and Discussion
A fractured interface is shown in Figure
I at 20X, 1OX and 500X; the adherend
in this instance was bovine dentin. Approxi-
mately half of the cement had been removed
completely from the dentin and a rather
thick outer ring of cement remained; this
suggests that a ductile fracture pattern pre-
dominated.?9!) This fracture pattern was typi-
cal of most of the specimens tested, with
* Cambridge Stereoscan, Cambridge Instrument Co.,
L ondon. Eng.
enamel samples than on the dentin samples.
This may be related to the larger amount of
inorganic material in enamel than in dentin
which could have caused the chelation re-
action to be more extensive, thus producing
more complete bonding. An interpretation
of the fracture pattern (Fig 1, 20X) is that
failure started somewhere inside of the speci-
men, probably ait the adhesivc-dentin inter-
face, and propagated outward. Near the
edge of the sample, the failure locus moved
away from the interface and into the ad-
hesive. This interpretation seems reasonable,
especially since the fraicture Joint appeared
to have a Cup and cone configuration, which
indicates that ductile fracture predominated.
In such instances, the crack nucleates near

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784 F1ICK E-T A L J De at Rehs May-Jane 1972

Adhesive interface between bovine dentin and cement.

FIG 4.
the center of the specimen and proceeds the upper right corner. The mass of adhesive
outward.:9'9 was porous or spongy throughout with void
The scratches produced during prepara- spaces in the range of 0.2 to 15 micrometers
tion are shown clearly at bOOX, and the (Qim) across. The void spaces are of two
dentinal tubules appearing as small holes are kinds, those that extended down to the den-
visible at S0OX. Of particular interest is the tin surface (see Fig 4) and those that did
region shown at 100 X. In three separate not. The bubbles that were entirely in the
areas, the fracture pattern appeared to fol- cement probably were formed by entrap-
low closely the scratches in the substrate left ment of air during the mixing of the ce-
during preparation. This point is illustrated ment, or from the chemical reaction during
more clearly at 50OX, where the center area setting. Those that extended down to the
has been magnified. dentin probably were formed by entrapment
In Figure 2, scanning electron micro- of air during the application of the cement
graphs of the center area that was shown in onto the tooth surface; they generally were
Figure 1 are shown up to 5,OOOX. Filler larger than those entrapped during mixing.
particles of zinc oxide37 remained on the Two large voids that appear to be a cluster
surface of the cement, and a large particle of two or three bubbles are shown at 2,0O0x
is visible clearly at l,OOOX and 2,OOOX in and 5,OOOX in Figure 2. They may be air

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Vol S 1 No. 3 SURFACE TOPOGRAPHY & WElTING & ADESIVOJ7N785
8

500 x area I 100 x

IS
__

SO0§x::.:
FIG 5. Adhesive interface between bovine enamel and cement. Note concentration of air
pockets along grooves.
pockets; however, because of their irregular
shape, they probably are depressions left
after filler particles had been removed dur-
ing testing. The topographic appearance of
the dentin after surface preparation and ad-
hesion testing also is shown clearly in this
series of micrographs.
A different region of this same area is
shown in Figure 3. Again, filler particles, air
bubbles, and the topography of the dentin
are shown clearly. Of special interest is the
fracture pattern of the adhesive bond be-
tween the cement and the dentin. The gap
between the cement and the dentin, a space
about 0.5 [cm wide (running diagonally in
the photographs and parallel to ridges in the
I
area .2 G:
lOOx
dentin), probably was formed long after the
fracture occurred. It probably developed
during the drying and subsequent shrinkage
of the cement during metal coating. The
fracture surface itself appears to have prop-
agated from lower left to upper right, fol-
lowing the dentin surface. At the top of one
of the ridges it started into the cement, and
thereafter continued as a cohesive failure. It
is well-known from stress analysis that a
sharp edge, such as the tip of this ridge,
will be a region of stress concentration, and
consequently will influence the fracture pat-
tern. In this instance, the topography of the
dentin substrate obviously influenced the
fracture pattern to a considerable extent.

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786 1,1'1lC'K 111-T A L
500 x
:w0Xt
f S
FIG 6. Adhesive interface between bovine enamel and cement. Note crack propagating
along line of air pockets.
Also of interest is the fact that the dentinal
tubules acted as capillaries during the wet-
ting process; this is illustrated by the fact
that the cement had penetrated into the
tubules, as shown at 2,OOOX and 5,OOOX.
Therefore, the tubules also influenced the
wetting and subsequent fracture pattern con-
siderably.
Another specimen of a fractured surface
of bovine dentin and cement is shown in
Figure 4. This specimen was cleaved
through the tooth structure perpendicular to
the plane of the adhesive bond. The cleavage
is shown in the lower left corners at 500x
and 1,000X. In this area dentinal tubules
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J Dent Re.s Mav-Jxtne 1972
1000 x
I lmr :.i
:1
II
X SaV:X D:lO100Adx
and the structure of the dentin can be ob-
served clearly.
A few rather large air pockets were pres-
ent in the cement and one of them is visible
at the region between the dentin and cement.
This bubble was entrapped at a large groove
in the substrate and it can be seen that the
cement did not wet the dentin completely in
this area. This is shown at 2,OOOX and
5,000X. These photomicrographs illustrate
that the topography of the dentin also af-
fected the wetting process itself, as well as
the subsequent adhesive bond.
Two different areas of fracture of speci-
mens of cement on enamel are shown in Fig-
Vol 51 No. 3 SURFACE TOPOGRAPHY & WETTING & ADHESION
ure 5. The enamel surface outside of the test
area is shown in the upper right corner of the
micrographs. There were no tubules present
in this structure; however, the grooves pro-
duced during surface preparation were pres-
ent. In the area shown, the cement fractured
cohesively near the enamel surface, unlike
the fracture surfaces with dentin where the
cement failed cohesively farther from the
dentin substrate. A thick ridge of cement
remained around the outer circumference
(this ridge runs diagonally through the mi-
crographs). It is clear that small air pockets
in the cement tended to line-up along the
grooves produced during surfacing. Thus,
the topography of the solid substrate affected
the manner in which the cement came in
contact with the tooth surface and the sub-
sequent microstructure of the hardened ce-
ment near the interface. The actual source
of the entrapped air may be open to ques-
tion; however, the inference remains that
the grooves in the solid substrate caused the
air pockets to concentrate along them.
A concentration of air bubbles also may
act as weak areas or areas of stress concen-
tration, similar to a sharp edge as discussed
previously. In Figure 6, one of the grooves
in area 2 is shown at magnifications up to
10,OOOX. At 5,OOOX and 10,OOOX a crack
may be observed along the line of bubbles
in this groove. The crack down the line of
bubbles may have developed during fracture
or during drying and metal-coating of the
sample. In either instance, it is a result of
weakness associated with a concentration of
air bubbles along the groove. Thus, the
topography of the substrate affected the
fracture pattern, even when the cement
failed cohesively.
Conclusions
It has been shown in this investigation
that fracture most likely began as an ad-
hesive failure at the interface, and that both
adhesive and cohesive failure were involved.
The topography of the adherend affected the
direction and mode of propagation of the
fracture, and the topography affected the
wetting process by causing entrapment of
air at the interface between the cement and
tooth structure. In addition, the topography
influenced the microstructure of the cement
near the interface, since air bubbles in the
cement were lined up along grooves in the
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787
substrate. It has been shown, therefore, that
the topography of the adherend (tooth struc-
ture) does play an important role in the
formation of an adhesive bond and in the
fracture pattern of an adhesive joint, even
when cohesive failure is involved.
The authors express their appreciation to W. Kam-
merath, Division of Dental Materials Science, Faculty
of Dentistry, University of Western Ontario, for his
assistance during this investigation.
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