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The Effect of Enamel Surface Reduction in vitro on the Bonding of Composite Resin to Permanent Human Enamel
Paul M. Schneider, Louise B. Messer and William H. Douglas J DENT RES 1981 60: 895 DOI: 10.1177/00220345810600050801 The online version of this article can be found at: http://jdr.sagepub.com/content/60/5/895

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The Effect of Enamel Surface Reduction in vitro on the Bonding of Composite Resin to Permanent Human Enamel
PAUL M. SCHNEIDER, LOUISE B. MESSER,* and WILLIAM H. DOUGLAS**

Department of Pediatric Dentistry, University of Texas Dental School, San Antonio, Texas 78284, and *Department of Pediatric Dentistry and **Program in Biomaterials, University of Minnesota School of Dentistry, Minneapolis, Minnesota 55455 The shear bond strength between composite resin a prismless layer on deciduous and permanent and human permanent tooth enamel was measured tooth enamel.10-13 Ripa et al.9 and on unabraded tooth surfaces and after mechanical others13,14 have found prismless enamel reduction of 0.1 mm and 0.6 mm of the enamel more prevalent in the cervical than the surface. There was a higher bond strength follow- occlusal areas of teeth, and it has been ing the reduction of 0.1 mm of the surface (p < postulated that this finding is due to the 0.05) and 0.6 mm of the surface (p < 0.01). Mechanical surface reduction was associated with wearing away of the layer on occlusal increased residual composite at the bond site after surfaces by abrasion or attrition. Upon acid-etching, prismless enamel does not debonding. develop a surface as conducive to bonding with resins as does prismatic enamel.15-17 J Dent Res 60(5):895-900, May 1981 When resin is applied to etched prismless Introduction. enamel, there is inadequate resin penetration into the enamel to produce the tags In the past two decades, the clinical repair which aid in bonding.15,18
of fractured incisors has been greatly facilitated by the advent of composite resins and the introduction of acid etching of enamel1 to enhance resin retention. Several different techniques proposed for enamel preparation prior to acid etching include: 1) cleaning the enamel surface with no mechanical preparation;24 2) a scalloped shoulder 1-2 mm beyond the fracture site and approximately half the enamel thickness in depth;5,6 3) a chamfer shoulder;7 and 4) a knife-edged bevel.8 One of the reasons advanced for performing mechanical reduction prior to acid etching is that unprepared enamel surfaces may be resistant to acid conditioning due to the presence of prismless enamel in the superficial layer.7 Ripa et al.9 described a prismless layer of outer enamel on all 28 deciduous and on 70 of the 100 permanent teeth they examined by various microscopic techniques. The layer averaged 30 Mu in thickness and lacked the characteristic prism markings of enamel. Other studies have also demonstrated such

Barnes19 and Galil and Wright20 have investigated the effect of mechanical surface reduction before etching on the microscopic appearance of the enamel after etching. Both studies showed that the surface pattern after etching was more regular and more conducive to resin tag formation on teeth with mechanical reduction than on teeth without such reduction. This finding has

been attributed to the fact that mechanical reduction removes the prismless enamel layer which does not develop a favorable bonding surface when etched.20 Several studies have shown conflicting findings on the effect of mechanical reduction prior to acid etching on the strength of the bond between composite resin and etched enamel.21'24 Conniff and Hamby21 reported that such reduction results in an increase in bond strength, whereas Bozalis et al.22 reported that the bond strength did not differ significantly between samples with and without mechanical reduction. Aker et al.23 described increased bond strength following reduction with a rough

Received for publication May 2, 1980 Accepted for publication July 30, 1980 This study was supported in part by the Minnesota Mining and Manufacturing Co., St. Paul, MN 55101.

diamond instrument but not when a smoother carbide bur was used. In the only study attempting to control depth of enamel reduction, Vahid Golpayegani24 reported substantially reduced bond strength follow895

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was etched for one min (37% w/w H3P04), washed for one min with de-ionized water from a wash bottle, and dried with filtered compressed air. A thin layer of unfilled resin was mixed and applied to the etched surface according to the manufacturer's instructions. A rubber moldt that had previously been fabricated (1 cm diameter, 3 mm thick, with a 2 mm diameter hole through the center) was held in contact with the resin-coated enamel surface using a wooden tongue blade. The blade contained a 6 mm diameter aperture in the end resting on the rubber mold, and the hole in the mold was visible through the tongue blade aperture. A 70 g weight resting on the tongue blade stabilized the blade and underlying mold. The composite resin was mixed according to the manufacturer's instructions and syringed into the hole in the center of the mold, and thereby onto the enamel surface. The material was allowed to set for at least 15 min under a 50 g weight. Any flash that formed under the rubber mold was removed with a

ing removal of two-thirds of the enamel thickness. The purposes of the present study were to observe the effect of differing extents of enamel reduction on the strength of the bond between etched enamel and composite resin, and to assess the amount of residual composite at the bond site following debonding.
Materials and methods.
Tooth selection. - Sixty permanent bicuspids extracted as part of orthodontic treatment from 20 humans aged ten to 21 yr were collected (three teeth per subject). The teeth were stored in de-ionized water at 40C and randomly assigned to one of three experimental groups, each group containing 20 teeth (one from each of the 20 subjects). Composite resin. - The composite resin system used for all samples was Concise with Enamel Bond. All material used was from one batch, and the study was performed within six mo of the date on the package. The material was stored at 4 C, but was placed at room temperature (approximately 20 C) at least three h before use. Tooth preparation. - Group A teeth had no mechanical enamel reduction, but were cleaned with 100 strokes of a soft toothbrush under running tap water. Each group B tooth was mounted in a microtome fitted with a 600 grit carborundum wheel which was cooled and lubricated with water. The tooth was advanced against the wheel until 0.1 mm of enamel was removed as indicated by a gauge which is an integral part of the microtome. Group C teeth were prepared in the same manner as those in Group B, except that 0.6 mm of enamel was removed. Following surface preparation, each tooth was mounted in an acrylic block+ measuring 2 cm wide and 0.5 cm thick with the prepared enamel surface horizontal. Composite application. - The method of preparing a standardized sample of composite was a development of that of Mitchem and Turner.25 The prepared enamel surface

sharp blade. Sample storage. - The samples were stored in de-ionized water for 11-13 d before testing. The teeth were maintained at 40C, except for a period of thermocyclingt between 180C and 500C for 90 s at each temperature (total 150 cycles). Bond strength testing. - The bond strength was measured mechanically// using shear force. The acrylic block was held so that the composite sample was approximately horizontal. A loop of 0.46 mm diameter round wire: was gripped in the upper jaw which was suspended by a universal joint. The wire was placed around the composite sample and held against the tooth surface. Using a cross head speed of 1 mm per min, the machine applied a shear force until the composite fractured from the tooth. The force applied at fracture was recorded automatically. Microscopic examination of fracture
MI 48174

tKerr Syringe Elasticon, Kerr Co., Romulus, Concise with Enamel Bond, 3M Co., St. 4Thermocycling machine custom made at the Paul, MN 55101 University of Minnesota, Minneapolis, MN 55455 #John C. Motter Printing Press Co., York, PA /Instron Testing Machine, Model 1122, Instron (Designer Dr. D.B. Scott, NIH, Bethesda, MD) Corp., Canton, MA 02021 +Kerr Formatray (pour consistency), Kerr Co., :Rocky Mountain Elgiloy, Rocky Mountain,
Romulus, MI 48174
Inc., Denver, CO 80217
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site. - A low power stereoscopic microscope0 with an eyepiece grid in 1 mm2 divisions was used. Using the grid as a reference, the percentage of the bonding site covered by residual composite was estimated. There was no attempt to measure the amount of unfilled resin at the bonding site. Statistical treatment of data. - The shear forces required for fracture in each of the experimental groups were compared using Student's t test for paired data and tested at 0.05 and 0.01 levels of significance.

ference of 4.8 kg), and Groups A and B both showed a similar range (difference of 7.7 kg). Technical problems occurred with three samples from three different subjects as follows: One showed an air bubble at the bond site; one sample showed a flash of composite which had been left untrimmed; and one specimen was dislodged during storage. These samples were excluded from the study. To ensure that each subject had teeth represented in all three groups, the remaining two teeth from each affected subject were also discarded. Results. The mean force required to fracture Bond strength testing. - The Table shows specimens in Group A (7.8 kg 2.3 SD) the force in kg applied to the composite at was significantly lower (p < 0.05) than that the time of its fracture from the enamel required for Group B specimens (9.6 kg + surface, the group medians, the means, and 1.8), and it also was significantly lower the standard deviations. Teeth in Group C (p < 0.01) than that required for Group C (0.6 mm enamel reduction) showed the specimens (10.3 kg 1.4). Forces required to narrowest range of forces required (a dif- fracture specimens in Groups B and C did not differ significantly. A random sample of six composite TABLE FORCE IN KG APPLIED TO COMPOSITE samples had a mean diameter of 1.93 mm + SAMPLE AT MOMENT OF FRACTURE OF 0.008 SD at the bonding site. Using a conCOMPOSITE FROM ENAMEL version factor of kg/cm2 x 0.09807 = MPa, the mean force at fracture for each group Group A Group B Group C was equivalent to: Group A, 26.1 MPa; No 0.1 mm 0.6 mm Subject* Reduction Reduction Reduction Group B, 32.1 MPa; and Group C, 34.5 MPa.
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17

9.8 kg 7.7 9.8

7.7 5.0 6.3 12.2 6.9 5.2 8.4 11.1 9.1 9.0 4.5 7.9 6.7 4.7

9.6 9.0 8.5 13.0 11.0 8.0 9.6 5.3 10.0 10.8 10.4 10.5 12.8 8.3 8.2 8.6

10.2 kg

7.4 kg 8.2 12.2 11.8 11.6 9.5 10.6 9.5 11.4 10.9 10.1 9.9 8.2 10.2 12.1 11.2 9.5

Microscopic examination of bond site. The Figure shows the distribution of residual composite for each specimen in all three groups. The greatest number of residuefree teeth was seen in Group A and the least in Group C. An increasing amount of enamel reduction was associated with an increasing percentage of the bond site being covered with residual composite after fracture. With the exception of one specimen (no. 7 in Group A), all teeth showed the fracture site located within the composite or at the enamel-composite interface. The one exception showed evidence of enamel fracture at the bond site.

perimentation.

Median 7.7 10.2 9.6 Mean 7.8 9.6 10.3 Standard Deviation 2.3 1.8 1.4 *The teeth of three subjects were eliminated due to technical difficulties experienced during ex-

Bausch and Lomb, Inc., Rochester, NY 14602

Discussion. The findings of the present study show that the mechanical removal of as little as 0.1 mm of surface enamel will significantly increase the shear strength of the bond between composite resin and etched permanent enamel. This observation supports the findings of Conniff and Hamby,21 but it
is at variance with those of Bozalis et

al.,22

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1510-

/5

Group A no reduction

maximum

study
ness.

was less than half the enamel thick-

depth of reduction in the present

5-

E~ Ur) 10E o-

r/

Group B
ni

l
Group C
0.6mm reduction

lOnt ifr10-ene
50
4

r n In m 0 5 1015 25 35506675 % of Site With Residual Composite Fig. Percentage of bonding site covered by residual composite.

-I

Aker et al.,23 and Vahid Golpayegani.24 Bozalis et al. 22 did not find significant bond strength differences between groups, possibly because of the low number of five samples per group. Aker et al.23 found no significant increase in bond strength after the enamel surface had been reduced with a carbide bur, which probably left a rougher surface than did the 600 grit carborundum used in the present study. Reasons for their finding no significant difference may also include: a) the small sample size (ten per group) and b) the fact that the depth of reduction was not controlled and may have exceeded that of the present study. Another important aspect of the study by Aker et al. was that they did not report the of the age subjects from whom the sample teeth were extracted. However, the fact that calculus had to be removed from the teeth suggests that they were from older patients. If this is the case, any prismless or other etch-resistant layer on the enamel surface may have been removed by attrition or abrasion. Vahid Golpayegani24 controlled the depth of enamel reduction, stating that it was two-thirds of the enamel thickness; he found a reduced bond strength at this depth. The present study is not directly comparable because, after the maximum 0.6 mm reduction, the enamel remained approximately 1 mm thick. Therefore, the

The results of the present study are a corollary to those of Barnes19 and Galil and Wright.20 Both those studies found that, following mechanical enamel surface reduction, the pattern produced by etching was more conducive to the formation of the resin tags responsible for bonding. The present study has shown that, as well as the improved etch pattern, there is in fact an increased bond strength after mechanical surface reduction. Any study of bonding to unreduced surface enamel must address the problem of how to remove organic integument from the surface. In the present study, the surface was brushed with 100 strokes of a soft toothbrush under running water. This technique was chosen because it is easily standardized and leaves no residue. The effect of a pumice prophylaxis, which has been used in other studies,15'2021 varies with the speed of the instrument used, the pressure applied, and the amount of heat generated on the surface. Also, any residual pumice may interfere with bonding. Although the technique used in the present study may not have removed all organic integument, and the residual integument may have interfered with etching, the magnitude of the bond strength results of Group A teeth indicates that some etching must have occurred. Since Silverstone26 has shown that etching completely removes the most superficial layer of enamel, it seems likely that any residual organic integument will have been separated from the enamel during etching and removed by the washing and drying subsequent to etching. The results of the microscopic examination of the bond site in the present study confirm the bond strength results. The samples with mechanical surface reduction had more residual composite on the bond site than did samples with no surface reduction. Therefore, the strength of the enamelcomposite bond following mechanical reduction was closer to the cohesive strength of the composite than the bond strength on unreduced enamel. A problem when comparing the results of bond strength testing studies by different
authors is that there are no standardized methods either for applying a composite

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sample of controlled size to an enamel surface or of measuring the bond strength. This lack of uniformity in technique may be largely responsible for the widely differing values reported for bond strength. For example, among the values reported for the shear strength of the bond between composite and etched enamel without mechanical reduction are: Bozalis et al.,22 3.9 MPa* (untreated surface, Nuva-Fil composite);** Aker et al.,23 17.1 MPa* (unprepared, Nuva-Fil), and 40.3 MPa* (unprepared Concise); Vahid Golpayegani24 24.6 MPa* (intact surface, Concise ) and the present study, 26.1 MPa (no reduction, Concise). Variables which may be responsible for these differences include: age, fluoride history, and storage time of teeth before testing; the acid concentration, its time and method of application; the time and method of washing and drying; the use of a thin unfilled resin layer on the surface; the type of composite and any pressure during its application; and the method of force application. Until there is a better standardization of this long list of variables, caution should be used in comparing the results of different studies in this field.
Conclusions.
The results of the present in vitro study show that mechanical removal of 0.1 or 0.6 mm of the enamel surface of permanent teeth significantly increases the shear bond strength between etched enamel and composite resin. Correspondingly, following debonding of composite from the enamel, teeth with surface reduction before etching show more residual composite at the bond site than do teeth without mechanical surface reduction.
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**Nuva-Fil, L.D. Caulk Co., Milford, DE 19963

Concise, 3M Co., St. Paul, MN 55101

*Conversion Factor:

psi

x 0.006895

MPa

KINS, W.A.: Clinical Evaluation of Three Acid-etch Composite Resin Systems: Twoyear Report, JADA 97:829-832, 1978. 5. RULE, D.C. and ELLIOTT, B.: Semipermanent Restoration of Fractured Incisors in Young Patients, Br Dent J 139:272-275, 1975. 6. SCHEER, B.: The Restoration of Injured Anterior Teeth in Children by Etch-retained Resin, Br Dent J 139:465-468, 1975. 7. JORDAN, R.E.; SUZUKI, M.; GWINNETT, A.J.; and HUNTER, J.K.: Restoration of Fractured and Hypoplastic Incisors by the Acid Etch Resin Technique: A Three-year Report, JADA 95:795-803, 1977. 8. HILL, F.J. and SOETOPO: A Simplified Acidetch Technique for the Restoration of Fractured Incisors, J Dent 5:207-212, 1977. 9. RIPA, L.W.; GWINNETT, A.J.; and BUONOCORE, M.G.: The "Prismless" Outer Layer of Deciduous and Permanent Enamel, Arch Oral Biol 11:41-48, 1966. 10. GWINNETT, A.J.: The Ultrastructure of the "Prismless" Enamel of Deciduous Teeth, Arch Oral Biol 11:1109-1115, 1966. 11. GWINNETT, A.J.: The Ultrastructure of the "Prismless" Enamel of Permanent Human Teeth, Arch Oral Biol 12:381-387, 1967. 12. TINANOFF, N. and MUELLER, B.; Acid Etch Characteristics of Prismless Enamel, JIntAssoc Dent Child 8:15-19, 1977. 13. HORSTED, M.; FEJERSKOV, O.; JOOST LARSEN, M.; and THYLSTRUP, A.: The Structure of Surface Enamel with Special Reference to Occlusal Surfaces of Primary and Permanent Teeth, Caries Res 10:287-296, 1976. 14. RIPA, L.W.: Sealant Retention on Primary Teeth: A Critique of Clinical and Laboratory Studies, JPedod 3:275-290, 1979. 15. SHEYKHOLESLAM, Z. and BUONOCORE, M.G.: Bonding of Resins to Phosphoric Acidetched Enamel Surfaces of Permanent and Deciduous Teeth, J Dent Res 51:1572-1576, 1972. 16. BRANNSTROM, M. and NORDENVALL, K.J.: The Effect of Acid Etching on Enamel, Dentin, and the Inner Surface of the Resin Restoration: A Scanning Electron Microscopic Investigation, J Dent Res 56:917-923, 1977. 17. NORDENVALL, K.J.: Enamel Bond-composite Fillings in Etched Cavities. The Appearance of Resin Surfaces Facing Enamel and Dentine, Swed DentJ 2:141-150, 1978. 18. GWINNETT, A.J.: Human Prismless Enamel and Its Influence on Sealant Penetration, Arch Oral Biol 18:441-444,1973.

3. WATKINS, J.J. and ANDLAW, R.J.: Restoration of Fractured Incisors with an Ultra-violet Light-polymerized Composite Resin, Br Dent J 142:249-252, 1977. 4. ROBERTS, M.W.; MOFFA, J.P.; and JEN-

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J Dent Res May 1981

19. BARNES, I.E.: The Adaptation of Composite Resins to Tooth Structure. Part 2, Br Dent J 142:185-191, 1977. 20. GALIL, K.A. and WRIGHT, G.Z.: Acid Etching Patterns on Buccal Surfaces of Permanent Teeth, Pediatr Dent 1:230-234, 1979. 21. CONNIFF, J.N. and HAMBY, G.R.: Preparation of Primary Tooth Enamel for Acid Conditioning, JDentChild 43:177-179, 1976. 22. BOZALIS, W.G.; MARSHALL, G.W.; and COOLEY, R.O.: Mechanical Pretreatments and Etching of Primary-tooth Enamel, JDent Child 46:4349, 1979. 23. AKER, D.A.; AKER, J.R.; and SORENSEN, S.E.: Effect of Methods of Tooth Enamel Preparation on the Retentive Strength of

Composite Resins, JADA 99: 185-189, 1979. 24. VAHID GOLPAYEGANI, M.: Effect of Water Immersion on Tensile and Shear Bond Strength of Nuva-Fil (R) and Concise (R) with and without Primer to Three Different Enamel Layers, Rochester, NY: University of Rochester, 1978. M.S. Thesis. 25. MITCHEM, J.C. and TURNER, L.R.: The Retentive Strengths of Acid-etched Retained Resins, JADA 89:1107-1110, 1974. 26. SILVERSTONE, L.M.: The Acid Etch Technique: In vitro Studies with Special Reference to the Enamel Surface and the Enamel-resin Interface, Proc Int Symp Acid Etch Tech, St. Paul: North Central Publishing Co., 1975,
pp. 13-39.

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