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dental

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Dental Materials 15 (1999) 250–256
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Surface roughness and bond strength of enamel to composite


M. Jung*, L.O. Wehlen, J. Klimek
Department for Operative and Preventive Dentistry, Justus-Liebig-University, Schlangenzahl 14, D-3592 Giessen, Germany
Received 19 November 1998; accepted 18 March 1999

Abstract
Objectives: The aim of the study was to assess the influence of pretreating enamel by different rotary instruments on shear-bond strength of
composite to enamel after the acid etch technique.
Methods: Ninety human enamel specimens with transversely and longitudinally sectioned prisms were ground flat, and half of the enamel
area of each specimen was prepared with one of the eight different rotary instruments: a 120 mm diamond bur, three finishing diamonds (30,
15 and 8 mm), two tungsten carbide finishing instruments (8- and 30-fluted) and two stones (Dura green and Dura white). The other half of the
enamel area was left untreated. Enamel roughness was measured by laser-stylus profilometry. Two cylinders filled with the hybrid composite
Pertacw were adhesively fixed on each enamel surface, one on the prepared side and the other on the untreated side. After seven days of water
storage, shear-bond strength was measured with a Universal testing machine.
Results: Rz values of the treated enamel surfaces were between 4.14 and 17.75mm. The shear-bond strength data varied between 16.8 and
29.4 MPa and were similar for transversely and longitudinally orientated prisms. The different roughness data had no significant influence on
shear-bond strength of composite to enamel. Additional SEM investigation showed that the surface geometry caused by the rotary instru-
ments largely persisted after acid etching.
Significance: With regard to shear-bond strength, there was no advantage in using a special bur for finishing enamel surfaces prior to the
acid etch technique. Burs causing extreme roughness should not be used for this purpose. q 1999 Academy of Dental Materials. Published by
Elsevier Science Ltd. All rights reserved.
Keywords: Acid etch technique; Enamel; Adhesion; Surface roughness; Composite resin; Finishing

1. Introduction known about the influence of different enamel surface


textures resulting from cutting with rotary instruments on
The bonding of composite to enamel after acid etching is bond strength after acid etching.
one of the most common techniques in current operative Our study aimed to assess the effect of varying surface
dentistry. This includes the placement of direct restorations roughness caused by rotary instrumentation on the shear-
and the application of fissure sealants, as well as the bond strength of enamel to composite. The influence of
adhesive cementation of tooth-coloured inlays made of acid etching on machined enamel surfaces was also consid-
composites or ceramics. In contrast to conventionally placed ered in the investigation.
or cemented restorations, adhesive bonding permits a mini-
mum reduction of dental hard tissue and increases the
fracture resistance of restored teeth, by reducing the cusp 2. Materials and methods
deformation under load [1].
Since its introduction by Buonocore in 1955 [2], the acid Ninety previously impacted third human molars were
etch technique has been the subject of many investigations. used for the study. Tissue remnants were removed with a
The major topics of concern among these studies have been scaler and the teeth were cleaned with a rotating brush and
the type and concentration of acids [3–5], the time and pumice. Each tooth was then embedded in a chemically
practice of rinsing [6], the influence of air drying [7] and curing acrylic resin (Technovitw 4071, Kulzer, Wehrheim,
the effect of enamel contamination [8,9]. Presently little is Germany), with the buccal surface left uncovered. With the
help of a water-cooled tape-saw (Exakt-Trennschleifsystem,
* Corresponding author. Tel.: 1 49-641-99-46173; fax: 1 49-641-99-
Exakt Apparatebau, Norderstedt, Germany) each embedded
46169. tooth was cut mesio-distally from cusp-tip to cusp-tip. The
E-mail address: martin.jung@dentist.med.uni-giessen.de (M. Jung) buccal surfaces and the sectioned surfaces were ground flat
0109-5641/99/$20.00 + 0.00 q 1999 Academy of Dental Materials. Published by Elsevier Science Ltd. All rights reserved.
PII: S01 09-5641(99)0004 2-1
M. Jung et al. / Dental Materials 15 (1999) 250–256 251

Table 1
The nine different test groups with the corresponding rotary instruments

Test group Type of rotary instrument Grain size/blades Code number Producer

0 Abrasive paper disc 600 grit Leco Corp., USA


1 Diamond instrument 120 mm 6852314023 Brasseler, Germany
2 Finishing diamond 30 mm 8852314014 Brasseler, Germany
3 Finishing diamond 15 mm 852EF314014 Brasseler, Germany
4 Finishing diamond 8 mm 852UF314014 Brasseler, Germany
5 Tungsten carbide finishing instrument 8-Fluted 134314014 Brasseler, Germany
6 Tungsten carbide finishing instrument 30-Fluted 134UF314014 Brasseler, Germany
7 Dura-green stone 105 mm CA/CN1/0052 Shofu, Japan
8 Dura-white stone 28 mm CA/CN1/0221 Shofu, Japan

with 600 grit SiC abrasive paper discs (Leco Corpration, St. 2.1. The rotary instruments
Joseph, MI, USA) at 120 rpm under water cooling by use of
an automatic polisher A-250 (Jean Wirtz, Düsseldorf, The test halves of the specimens were prepared manually
Germany). This resulted in two specimens from each using eight different rotating instruments: a coarse diamond
tooth: the flattened buccal surface with mainly transversely with a grain size of 120 mm, three finishing diamonds, two
cut enamel prisms (n ˆ 90; referred to as “transverse speci- tungsten carbide burs and a Dura-green and a Dura-white
mens”) and the sectioned surface with mainly longitudinally stone (Table 1). The diamonds and tungsten carbide burs
orientated enamel prisms (n ˆ 90; referred to as “longitu- were used in a red-ring handpiece with friction-grip
dinal specimens”). One half of each surface was used as the mechanism (Intramatic Lux 2 25 LS, KaVo, Biberach,
test surface, the other half was left untreated and served as a Germany) at 120 000 rpm under three-way water-cooling.
control. A blue-ring handpiece Intramatic Lux 20L with the head 68
LDN (KaVo) at 20 000 rpm and two-way water-cooling
was used for the stones. Each surface was cut for 20 s;
after two preparations a new bur was selected.
The treatment with the abrasive discs and the eight differ-
ent rotating instruments resulted in nine test groups. Ten of
the transverse specimens and ten of the longitudinal speci-
mens were randomly assigned to each group.

2.2. Quantitative surface analysis

Quantitative surface analysis values were determined by


profilometry for two specimens of each group. The laser
stylus pick-up Focodyn with a focus diameter of 1 mm
(Rodenstock, Munich, Germany) was used in combination
with the processing unit S8P (Mahr, Göttingen, Germany).
Because of the limited enamel thickness of the sectioned
surfaces, profilometry had to be performed under different
conditions for the longitudinal and transverse specimens.
The transverse length (LT) was 1.75 mm for transverse and
1.39 mm for longitudinal specimens; the cut-off (RC-filter)
was set at 0.25 and 0.08 mm for transverse and longitudinal
specimens respectively.
Nine automatically generated parallel tracings were
carried out on each transverse surface, six tracings on
each longitudinal surface, resulting in a scanned surface of
1.75 × 1.75 mm 2 for transverse and 1.39 × 0.56 mm 2 for
longitudinal specimens. The mean depth of roughness
among five adjacent spaces (Rz) was recorded.

Fig. 1. Schematic drawing of the specimen preparation and the positioning 2.3. Shear-bond strength tests
of the composite cylinders on the enamel surfaces with transverse and
longitudinal prism orientation. The test and control areas on each surface were etched
252 M. Jung et al. / Dental Materials 15 (1999) 250–256

in a Zwick Universal Testing machine (Zwick of America


Inc, East Windsor, USA) using a wedge-shaped rod at a
crosshead speed of 1 mm/min (Fig. 2). The maximum
load at failure was recorded in N and then converted
to MPa.
Statistical analysis to determine the effect of rotary treat-
ment of the nine test groups and of the prism orientation on
shear-bond strength data was carried out with 3-way
ANOVA.

2.4. SEM evaluation

In order to assess the influence of etching on the surface


geometry of the enamel after cutting, 18 additional teeth
were prepared as described above, resulting in 18 transverse
and 18 longitudinal specimens. Following instrumentation,
half of the treated surfaces were coated with nail varnish
while the other half were etched with 37% phosphoric acid
for 40 s (Etchant Gel, Espe). After water rinsing and drying
Fig. 2. The positioning of the enamel specimen with the composite cylinder
of the etched area, the nail varnish was removed with acet-
and the wedge-shaped crosshead before shearing. one.
The specimens were sputtered with gold (SCD 040,
with 37% phosphoric acid (Etchant Gel, Espe, Seefeld, Balzers Union, Liechtenstein) and examined under SEM
Germany) for 40 s, rinsed with tap-water for 20 s and (PSEM 500, Philips, Eindhoven, Netherlands) at a tension
dried for 10 s. Pertacw Universal Bond (Batch No. of 25 kV.
743410/05, Espe) was applied and air-thinned. Plastic
cylinders with an inner diameter of 1.004 mm and a 3. Results
height of 3 mm were filled with Pertacw Hybrid Unifil
(Batch No. 004/0010, Espe). Two cylinders were placed 3.1. Quantitative surface analysis
on each specimen, one on the test-side, and one on the
control-side (Fig. 1). Light curing was done for 40 s The cutting of the specimens with eight different rotating
with the polymerization unit Optilux 400 (Demetron instruments yielded roughness values ranging from an Rz of
Research Corporation, Danbury, USA). Finally, the plastic 4.14 mm for the smoothest to 17.75 mm for the roughest
coverings of the cured composite cylinders were removed enamel surface (Fig. 3). By the application of the 600 grit
with a scalpel. abrasive paper discs, the specimens were polished to an Rz
After seven days of water storage at 378C, shear-bond of 4.05 mm for transversely and 6.08 mm for longitudinally
strength tests were performed by mounting the specimens sectioned prisms. Only the use of the 30-fluted tungsten

Fig. 3. Roughness (Rz) of enamel surfaces with transversely and longitudinally orientated prisms after use of different rotary instruments (each bar represents
the mean and standard deviation of 18 parallel tracings on two enamel surfaces for transverse and 12 tracings on two enamel surfaces for longitudinal
specimens: FD—finishing diamond; TCFI—tungsten carbide finishing instrument).
M. Jung et al. / Dental Materials 15 (1999) 250–256 253

Fig. 4. Shear-bond strength …x ^ SD† of enamel surfaces with transversely sectioned prisms after the use of different rotary instruments (n ˆ 10 for each group:
FD—finishing diamond; TCFI—tungsten carbide finishing instrument).

carbide finishing instrument achieved a further reduction of 3.2. Shear-bond strength tests
roughness to 5.59 mm on longitudinally sectioned prism
surfaces. All the other rotating instruments caused a rough- Both transversely and longitudinally sectioned prisms
ening of the enamel surfaces to various degrees. The rough- exhibited no statistically significant difference between
est surface was produced by the coarse diamond (Rz ˆ groups regarding their shear-bond strength values (p ˆ
17.75 mm for transverse and 11.77 mm for longitudinal 0.644). A comparison between the four diamond instrument
sections). The three different diamond finishing burs led to groups revealed only a slight tendency towards higher
successively smaller roughness values. The Dura-green and shear-bond strength data with increasing roughness (Figs.
Dura-white stones as well as the 8-fluted tungsten carbide 4 and 5). The use of the tungsten carbide instruments
bur yielded Rz data, which were similar to those of the 8 and produced similar shear-bond strength values for the long-
15 mm finishing diamonds. itudinally sectioned prisms; for transversely sectioned
When comparing the two types of sectioned surfaces, it prisms, shear-bond strenth reached 25.39 MPa after the
became evident that the Rz values of the transversely use of the 30-fluted instrument and 15.05 MPa after use of
sectioned prisms were of a much wider range (from 4.14 the 8-fluted carbide finishing bur. For both types of prism
to 17.75 mm) than those of the longitudinally sectioned orientation, the shear-bond strength data obtained after the
prisms (from 5.59 to 11.77 mm). use of Dura-white stones were similar. The Dura-green
The surfaces with transversely sectioned enamel stones yielded 27.83 MPa on longitudinally and
prisms could be finished to lower Rz values than the 16.81 MPa on transversely sectioned prisms. As mentioned
corresponding specimens with a longitudinal prism above, these differences were not statistically significant.
orientation. The only main effect observed was in the overall

Fig. 5. Shear-bond strength …x ^ SD† of enamel surfaces with longitudinally orientated prisms after the use of different rotary instruments (n ˆ 10 for each
group: FD—finishing diamond; TCFI—tungsten carbide finishing instrument).
254 M. Jung et al. / Dental Materials 15 (1999) 250–256

the etched surface. The same effect could be seen after the
application of a 30 mm diamond finishing instrument on
transversely cut enamel prisms (Fig. 7). In some cases
however, only a few of the surface irregularities could be
recognized on the etched surface. This is depicted in Fig. 8,
at the borderline between the etched and unetched areas
after the use of a Dura-white stone.

4. Discussion

The aim of the sample preparations was to simulate the


two most common types of enamel margin quality prior to
the acid etch technique. A primarily transverse prism orien-
tation is created clinically when the margins of a class III
Fig. 6. Application of a 120 mm diamond instrument on enamel surface
cavity preparation are bevelled. By flattening the buccal
with longitudinal prism orientation (left side) and after etching with phos-
phoric acid (right side). surface with the abrasive paper an enamel surface was
created with a prism orientation resembling this clinical
situation. Sectioning the teeth mesio-distally resembled
treatment; as the shear-bond strength values of the control the preparation of a class II cavity with no margin
sides were significantly greater than that of the test sides bevelling and a primarily longitudinal orientation of
(p ˆ 0.002). enamel prisms.
There was no significant difference between transverse After cutting the specimens with different rotary instru-
and longitudinal prism orientation on shear-bond strength ments, the surfaces were evaluated quantitatively by an opti-
values (p ˆ 0.372). cal laser pick-up system. This type of surface tracing has
some advantages over conventional, contact stylus profilo-
3.3. SEM evaluation metry. The laser is focussed to a diameter of 1 mm, thus
permitting a precise tracing of even relatively smooth
The SEM evaluation of the transition zone between cut surfaces. The diameter of a conventional stylus varies
and etched surfaces showed a modification of the character- between 4 and 20 mm. This could be too inexact for those
istic surface features after the application of phosphoric enamel surfaces in the present study, which were finished to
acid. In most cases, the surface geometry caused by the an Rz of 4 mm or less. Another advantage of the laser is that
rotating instruments continued onto the etched surface in a the contact-free tracing of surfaces eliminates the possibility
reduced intensity; the typical pattern of etched enamel was of surface damage caused by direct contact with the tip of a
superimposed onto the surface irregularities that resulted mechanical pick-up.
from the prior use of different burs. From Fig. 6, an example In addition to Rz, there are several other parameters for
of longitudinally sectioned prisms after preparation with a the characterization of surface roughness. Maximum rough-
coarse diamond, it can be seen that the grooves continued on ness (Rt) and average roughness (Ra) are frequently used in
the literature [10]. It was the aim of the present study to
determine if there was a correlation between surface rough-
ness after cutting and shear-bond strength. Rz was chosen,
because this parameter gives a better indication of the actual
depth of the surface irregularities.
The profilometric evaluation of the prepared enamel
surfaces showed that the roughness varied widely, depend-
ing on the type of instrument, its grain size or number of
blades and on the prism orientation of the enamel speci-
mens. The use of diamond burs resulted in the greatest Rz
values, the tungsten carbide finishing instruments produced
the smoothest surfaces and the stones were between these
two groups.
The results are consistent with the findings of Al-Omari et
al. [11], who concluded that the smoothest surfaces on
Fig. 7. Instrumentation of transversely sectioned enamel prisms with a dentine and enamel were obtained using tungsten carbide
30 mm finishing diamond (left side) and after etching with phosphoric finishing burs. A study investigating the preparation of
acid (right side). dental hard tissue with diamond burs of different grit size
M. Jung et al. / Dental Materials 15 (1999) 250–256 255

bonding process than the additional surface roughness


obtained after the use of rotary instruments.
Finger et al. [15] found similar results for dentin surfaces
and concluded that the type of rotary instrument has little or
no influence on bonding strength of composite to dentin. On
the other hand, Mowery Jr. et al. [16] showed that differ-
ences in dentin surface roughness caused by sandpaper discs
from 60 to 1200 grit had an influence on shear-bond strength
data.
Shear-bond strength tests however, may not be the most
suitable method for investigating the quality of adhesive
bonding. The present data show a high standard deviation,
thus indicating that several tooth-dependent factors such as
varying mineralization or ultrastructural differences in
enamel composition may have influenced the measured
Fig. 8. The use of a Dura-white stone on the enamel with longitudinal prism
shear-bond strength data.
orientation (left side) and after etching with phosphoric acid (right side).
One problem often involved in this type of study is to
achieve a complete wetting of the enamel by the composite.
[12] showed similar results to the present study regarding It has been shown in a previous study with a similar tech-
the roughness after the use of a coarse diamond bur. nique for the placement of composite, that there were no
However, the Rz values caused by the 30 mm finishing signs of trapped air bubbles or other irregularities on the
diamond were much smaller than those of the present failed composite surfaces after the shear tests [17].
data. This inconsistency might be due to the use of a less In the present study, the shear-bond strength values of the
exact mechanical stylus with a tip diameter of 20 mm, which controls were significantly greater than those of the test
was not able to accurately trace the small grooves created by surfaces after preparation. Evidently, any kind of rotary
the finishing diamonds. instrumentation had a weakening effect on the measured
The lowest Rz values were recorded for the surfaces with bond strength. This could be explained by the enamel
transversely sectioned enamel prisms. This could be due to subsurface damage through crack formation after tooth
the fact, that when longitudinally orientated prisms are preparation [13]. Furthermore, the stones that were used at
prepared, a cracking and tearing out of enamel rods might slower speed are rarely perfectly round and concentric.
occur more easily than on the transversely sectioned They can thereby produce a hammering effect upon the
surfaces. This explanation is supported by the findings of surface on which they are used [18]. Consequently, the
Xu et al. [13], who investigated enamel subsurface damage structure of enamel after rotary instrumentation could be
after tooth preparation with diamonds. The cracks in the weakened and therefore adhesive bonding could be
enamel were dependent on the orientation of the prisms impaired. In contrast to the rotary instrumentation, the
and were significantly longer in the direction parallel to application of the abrasive paper disks at low speed was a
the enamel rods. much more gentle and moderate type of treatment, which is
The shear-bond strength data reported in this study varied unlikely to cause any kind of enamel damage.
between 16.8 and 29.4 MPa. These results are consistent Munechika et al. [19] reported greater tensile bond
with those published by several others concerning the bond- strength for transverse than for longitudinal enamel
ing between enamel and composite [5,8,14]. sections. Under the conditions of this study the enamel
The use of rotary instruments on enamel prior to bonding prism orientation had no effect on shear-bond strength.
may have two effects. An increase in roughness results in a One possible reason for this is that the teeth were not
greater area available for bonding and could therefore facil- sectioned in the middle of the approximal surface, but rather
itate the wetting of the etched surface. On the other hand, from cusp-tip to cusp-tip. The prism orientation might there-
deep and narrow grooves could lead to the inclusion of air fore not always have been strictly longitudinal.
bubbles between the enamel and the composite, thus weak-
ening the bond strength. Under the conditions of this study,
there was no correlation between surface roughness caused 5. Conclusion
by rotary instruments and shear-bond strength after acid
etching. Neither the rough nor the smooth surfaces could Under the conditions of the present study varying enamel
improve the bond strength. SEM analysis of prepared and roughness caused by the use of eight different rotary instru-
etched enamel areas demonstrated that the surface irregula- ments had no effect on shear-bond strength of enamel to
rities in most cases largely persisted after etching. This composite after acid etching.
indicates that the microroughness as a result of acid etching The coarse diamond and the Dura-green stone should not
was of greater importance for the quality of the adhesive be used for cutting enamel prior to bonding because of the
256 M. Jung et al. / Dental Materials 15 (1999) 250–256

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[11] W.M. Al-Omari, C.A. Mitchell, L. Cunningham, Surface roughness
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