Influence of enamel conditioning on bond strength of resinmodified glass ionomer restorative materials and polyacid-modified composites

Thomas Attin, Dr Med Dent, a Wolfgang Buchalla, Dr Med Dent, a and Elmar Hellwig, Prof Dr Med Dent b

University of Freiburg, Freiburg, Germany

This study evaluated e n a m e l b o n d strength of restorative materials containing both glass ionomer and composite components. Three resin-modified glass ionomer restorative materials (Fuji II LC, Vitremer, Photac-Fil), t h r e e polyacid-modified composites (VariGlass VLC, Dyract, Ionosit Fil), a h y b r i d composite (blend-a-lux) a n d a chemical-cured glass-ionomer c e m e n t (ChemFil Superior) w e r e tested for e n a m e l tensile bond strength w i t h and without conditioning of the tooth surfaces. Tensile b o n d strength was determined for five specimens each of conditioned and unconditioned bovine teeth. S p e c i m e n conditioning was performed as r e c o m m e n d e d by the manufacturers. The tensile bond strength was tested with a universal testing machine. Except for the e n a m e l bond strength of ChemFil Superior, all m a t e r i a l s showed greater adhesion to conditioned tooth surfaces than to u n c o n d i t i o n e d specimens. E n a m e l bond strengths of the polyacid-modified composites applied after a p h o s p h o r i c acid etching technique (Ionosit Fil, Dyract, VariGlass) w e r e greater c o m p a r e d with the materials applied after surface conditioning with polyacrylic acid-containing agents. No significant difference was observed b e t w e e n the hybrid composite and the tested materials attached w i t h the p h o s p h o r i c acid etching technique. To improve adhesion of the tested materials to enamel, following the manufacturers' instructions about tooth surface conditioning is recommended. Superior bond strength to e n a m e l was obtained for polyacid-modified composites, w h i c h are attached w i t h the p h o s p h o r i c acid etching t e c h n i q u e and thereby resemble the adhesion patterns of composites. (J Prosthet Dent 1996;76:29-33.)

T h e tight a n d sufficiently strong bonding of a restorative m a t e r i a l to the cavity walls is an i m p o r t a n t aim in restorative dentistry. Bonding to the cavity walls m a y reduce the occurrence of m a r g i n a l gap formation. Moreover, because of tight bonding of restorative material, p r e p a r a t i o n of undercuts m a y be superfluous for retention of the m a t e r i a l in the cavity. Consequently erosion lesions or fractured teeth m a y be restored without u n d e r c u t prepa r a t i o n } The adhesion of a m a t e r i a l to tooth structure is influenced by its flow capacity, volumetric changes, and bond s t r e n g t h to dental h a r d tissues. Several studies proved t h a t glass ionomer cements bond adhesively to tooth structure. 2-7 In these studies conventional glass ionomers or resin-modified glass ionomers t h a t were developed for use as bases or liners were tested. It was found t h a t bond s t r e n g t h to tooth structure is enhanced by the use of conditioning agents before the application of resinmodified glass-ionomer bases or liners. 3 Recently, new types of restorative m a t e r i a l s with both glass ionomer and resin components were introduced. According to McLean et al., s restorative m a t e r i a l s t h a t contain both glass ionom e r and composite components m a y be classified as follows: (1) resin-modified glass ionomers, m a t e r i a l s t h a t

retain a significant acid-base reaction as part of their overall curing process; and (2) polyacid-modified composites, materials that may contain either or both of the essential components of a glass ionomer cement but at levels insufficient to promote the acid-base cure reaction in the dark. These m a t e r i a l s were developed as restorative m a t e r i a l s for class I, III, or V cavities. W h e n these m a t e r i a l s are used for restoration of class I and class III cavities, a tight bonding to enamel is required. For the available materials, two different enamel conditioning procedures are m a i n l y recommended by the manufacturers. They advise either conditioning with an enamel acid etching technique cont a i n i n g phosphoric acid or p r e t r e a t m e n t with polyacrylic acid-containing agents. Little information exists about the enamel bond s t r e n g t h of these materials. The purpose of this study was to investigate the tensile bond s t r e n g t h of resin-modified glass ionomer restorative m a t e r i a l s and polyacid-modified composites for enamel tensile bond s t r e n g t h to conditioned and unconditioned enamel. Thus, this study focuses on the efficacy of the various conditioning systems recommended. MATERIAL AND METHODS

aAssistant Professor, Department of Operative Dentistry. bprofessor and Chairman, Department of Operative Dentistry.

In a pilot study, the m a t e r i a l s with both glass ionomer and resin components were e v a l u a t e d for setting reaction in the d a r k (Table I). Each of two specimens were mixed according to the m a n u f a c t u r e r s ' recommendations and

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Table I. Restorative m a t e r i a l s tested

Material E n a m e l conditioning

Chemical compositiont

Blend-a-lux [93230002]* (Blendax, Mainz, Germany)

(1) Etching Gel (DMG) Application (1 rain) Wash-off (1 min) Drying (2) Prisma Universal Bond 3 Adhesive, LC (10 sec)

1) Phosphoric acid (37%)

Ionosit Fil [921214]* (DMG, Hamburg, Germany)

(1) Etching Gel (DMG) Application (20 sec) Wash-off (1 min) Drying (2) Superlax Mono LC (20 sec)

2) UDMA (50%) TEGDMA (40%) PENTA (5%) Glutaraldehyde (2%) Bis-GMA phosphoric acid ester Amine-campherquinone-catalyst 1) Phosphoric acid (37%)

Dryact [KL 15-72-2]* (DeTrey Dentsply, Konstanz, Germany)

VariGlass VLC [9202265 (powder) 930617 (liquid)]* (DeTrey Dentsply)

Photac-Fil [007 031)* (ESPE, Seefeld, Germany) Vitremer [307067]* (3M, Borken, Germany) Fuji II LC [070523 (powder), 281021 (liquid)]* (GC Dental Int., Leuven, Belgium) ChemFil Superior [19930416]* (DeTrey Dentsply)

(1) Etching Gel (DMG) Application (1 min) Wash-off (1 min) Drying (air-blow) (2) PSA-Liquid (DeTrey) Application, waiting (30 sec) Air-blow LC (10 sec) (1) Etching Gel (DMG) Application (1 min) Wash-off (1 min) Drying (2) Prisma Universal Bond 3 Adhesive, LC (10 sec) Ketac Conditioner (ESPE) Application, waiting (10 sec) Wash-off (30 sec) Drying Vitremer Primer Application (30 sec) Drying (15 sec) LC (20 sec) GC Dentin Conditioner (GC Dent.) Application (20 sec) Wash-off Drying ChemFil Tooth Cleanser (DeTrey) Application (15 sec) Wash-off Air-blow

2) TEGDMA Bis-GMA Polymethacryl polycarbonic acid Oligomaleinic acid Amine-campherquinone-catalyst 1) Phosphoric acid (37.5%) 2) TEGDMA, PENTA, HTDTDMA Amine-campherquinone-catalyst Acetone

1) See above

2) See above Polyacrylic acid (25%)

Polyacrylic acid polymer (12%) HEMA, alcohol

Polyacrylic acid (10%)

Polyacrylic acid (25%)

LC, Light-curing with Optilux 400 (Demetron Research Corp., Danburry, USA); Bis-GMA, bisphenol glycidyl methacrylate; HTDTDMA, hexamethyl tetraoxo dodecanaoxa tetraazadoheptacontan diyldimethacrylate; PENTA, dipentaerythriol penta-acrylate phosphoric acid ester; TEGDMA, triethylene glycoldimethacrylate; UDMA, urethane dimethacrylate.
*Batch No. tComposition according to manufacturer.

subsequently stored in a d a r k room at 20 C. The specimens were stored in a dry atmosphere except those for Dyract material, which were stored in water. Dyract is a single-component m a t e r i a l t h a t is not mixed before appli30

cation. The m a n u f a c t u r e r of Dyract m a t e r i a l suggests t h a t the glass ionomer acid-base reaction of the m a t e r i a l s t a r t s because of the w a t e r contact. After 24 hours of storage, plasticity of the specimens was detected by indenting the
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materials with a plastic scaler. Easily deformed materials were categorized as resin-modified glass ionomer restorative materials. According to these findings, the tested materials were classified as followsS: (1) resin-modified glass ionomer restorative materials, Fuji II LC, Vitremer, and Photac-Fil; a n d (2) polyacid-modified composites, VariGlass VLC, Dyract, a n d Ionosit Fil. A hybrid composite (blend-a-lux) a n d a chemical-cured glass ionomer (ChemFil Superior) were also investigated. The m a n u f a c t u r e r s recommended conditioning of the enamel with a n acid etching technique (with 37% phosphoric acid) for blend-a-lux, Ionosit Fil, Dyract, and VariGlass VLC materials, respectively. The conditioner for Vitremer material consists of polyacrylic acid and a hydrophilic monomer hydroxyethylmethacrylate (HEMA). The enamel conditioning agents of the other materials contained only polyacrylic acid. Sound extracted bovine incisors (n = 80) were stored at room t e m p e r a t u r e in 0.9% sodium chloride solution for up to 1 week before preparation for the bonding tests. The preparation of the teeth included cutting off the roots, removing the pulp tissues, and embedding the crowns, with the exception of the labial surface, in a n epoxy resin (BK, Vosschemie GmbH, Uetersen, Germany). To avoid dehydration of the dentin, cotton-wool soaked with distilled water was placed in the pulp chambers a n d the pulp chambers were closed with wax. The labial surfaces of the specimens were ground flat a n d then finished with 800-grit silicon carbide paper to remove approximately 300 l~m of enamel. Thickness of the removed dental hard tissue was controlled with a micrometer. The enamel was washed with distilled water and dried with air. Ten enamel specimens each were used for the bond test of the respective restorative materials. Five of these 10 enamel specimens were conditioned (Table I); the surfaces of the r e m a i n i n g specimens were not conditioned. A funnel-shaped steel mold was used to form and to hold the restorative materials next to the enamel surface during the time of the experiment. The molds were 4 m m high and could be clamped tightly to the enamel surfaces. The opening at the end of the funnel t h a t contacted the surface of the specimens was 4.3 m m in diameter. Each restorative material was prepared according to the manufacturers, and the materials were condensed into the molds. The light-cured restorative materials were applied with a twostep technique in 2 m m increments. Each i n c r e m e n t was photocured for 60 seconds. The chemical-cured glass ionomer cement (ChemFil Superior) was allowed to set for 5 m i n u t e s and was subsequently varnished with ChemFil varnish. All specimens were t h e n stored in water at 37 C for 24 hours while the molds were still clamped to the teeth. The tensile bond strengths of the restorative materials to the enamel surfaces were tested in a universal testing machine (model UPM 81565, F r a n k GmbH a n d Co., Weinheim, Germany). The specimens were m o u n t e d so t h a t the flattened enamel surface was positioned perpendicular to the moving crosshead of the testing machine. The crossJULY 1996

T a b l e II. Average tensile bond strength to enamel

Tensile b o n d strength ( M P a ) Unconditioned enamel Conditioned enamel Materials applied
X, SD X SD

After acid etching blend-a-lux* -Ionosit Fil* 1.4b, c Dryact* 2.65, c VariGlass VLC* 1.35, c After conditioning with polyacrylic Fuji II LC* 0.8c Photac-Fil* -Vitremer* 4.1a,5 ChemFil Superior 5.9a

-25.3a 1.3 0.3 22.4a, b 0.9 0.2 20.6a, 5 1.5 0.5 17.75 2.4 acid containing agents 0.2 10.6c 3.1 -10.2c 2.2 0.6 6.4c 0.7 1.3 5.2c 1.0

Differences between values in one column with s a m e superscript letter are not statistically significant (level of significance: p < 0.05). *Material with a statistically significant difference between unconditioned a n d conditioned specimens.

head was fixed in a n u n d e r c u t of the mold and allowed the mold to be pulled offofthe tooth. The tensile load required to cause debonding was recorded at a crosshead speed of 1 mm/minute. The bond strength was calculated from the load at which the material debonded, divided by the area of bonded enamel surface (4.3 m m in diameter). After the bonds were broken, the debonded surfaces on the tooth specimens were examined u n d e r a light microscope (40 magnification). The failure modes were classified as follows: adhesive failure at the material-tooth interface (A), cohesive failure within the restorative material (C), and a combination of C a n d A (CA). For each test performed, statistical analysis of comparisons among the materials were achieved by analysis of variance a n d Scheff~'s F-test. Differences between the conditioned a n d unconditioned specimens of the same material were tested with Student's t-test. The level of significance was set at p < 0.05. RESULTS Table II presents the results of the tensile bond strength to enamel. Bond strengths to the unconditioned enamel specimens were not determined for blend-a-lux and Photac-Fil materials because the molds filled with these materials did not attach sufficiently to the specimens after the clamps were removed. With exception of ChemFil Superior cement, all materials yielded a greater bond strength to conditioned enamel as compared with unconditioned enamel. The increases of bond strength as a result of conditioning were statistically significant for all materials. The resin-modified glass ionomer restorative materials a n d the polyacid-modified composites demonstrated lower bond strengths to conditioned enamel when compared with the hybrid composite (blenda-lux) and greater bond strength when compared with the chemical-cured glass ionomer cement (ChemFil Superior).
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Table III. Frequency of failure modes

Conditioned e n a m e l Materials applied
A* Ct CA$

After acid etching blend-a-lux 1 Ionosit Fil 1 Dyract -VariGlass VLC 1 After conditioning with polyacrylic acid containing agents Fuji II LC 3 Photac-Fil 3 Vitremer 4 ChemFil Superior 1
*Adhesive failure a t the material-tooth interface. tCohesive failure within the material. $Combination of C a n d A.

2 1 2 3

2 3 3 1

2 1 ---

-1 1 4

Enamel bond strength of the polyacid-modified composites applied after the acid etching technique (Ionosit Fil, Dyract, VariGlass VLC) were greater compared with the resin-modified glass ionomer restorative materials. Inspection of the debonded unconditioned enamel surfaces revealed exclusively adhesive failures for all materials. The results of the microscopic examination of the debonded surfaces of the conditioned specimens are presented in Table III. The polyacid-modified composites attached with the acid etching technique revealed fewer adhesive failures when compared with the resin-modified glass ionomer restorative materials applied after conditioning with po]yacrylic acid-containing agents. DISCUSSION In this study, bovine teeth were used to evaluate the bond strength of restorative materials bonded to enamel. According to Nakamichi et al., 9 bovine hard tissue can serve as a possible substitute for human teeth in adhesion tests. They found no statistical difference in adhesion of conventional glass ionomer cements and composite materials to bovine enamel and dentin specimens compared with human specimens. In this study the tested materials were allowed to set for 24 hours before determination of bond strength. Both chemical-cured and resin-modified glass ionomer cements undergo chemical reactions after initial setting, thereby increasing their bond strength to tooth structure. 6 A previous study reported that curing contraction of the tested materials increased continuously within 24 hours after mixing and light-curing. 1 The curing contraction may reduce the bond strength of these materials to dental hard tissues. With regard to the prolonged setting reaction and the increasing curing contraction, the bond strength was evaluated 24 hours after initial setting. Conditioning of the enamel specimens created a higher bond strength for all investigated materials except for the chemical-cured cement. All polyacid-modified composites

attached to enamel with the acid etching technique yielded greater bond strengths compared with the resin-modified glass ionomer restorative materials, which were applied after the enamel was conditioned with polyacrylic acid. The frequent occurrences of cohesive or cohesive/adhesive failures after acid etching demonstrated that the enamel tensile bond strengths recorded for these materials were at least partly limited by the tensile strengths of the materials themselves and not exclusively by their bond strength to enamel. By contrast, the resin-modified glass ionomer materials applied after pretreatment with polyacrylic acid-containing agents revealed frequent occurrence of adhesive failures. This finding emphasized that the values recorded for these materials actually reflect bond strength to enamel and not the tensile strength of the materials themselves. The phosphoric acid etching technique is recommended for composite materials and provides a micromechanical interlocking of the composite with the enamel, n By contrast, polyacrylic acid is used for conditioning dentin cavity surfaces before conventional glass ionomer cements are applied. The polyacrylic acid is applied to the cavity surface to remove the smear layer and clean the tooth. This application facilitates a chemical bond between the glass ionomer and the dental hard tissues. 12, 13 According to the manufacturers, the tested materials are actually hybrid systems that combine conventional glass ionomer and light-cured resin chemistries. No significant differences in bond strength were observed between the hybrid composite and the polyacid-modified composites attached with the phosphoric acid etching technique. Moreover both of these materials and the hybrid composite often revealed cohesive or adhesive/cohesive failures. The findings in this study support the claim that the adhesion pattern of the polyacid-modified composites attached with an acid etching technique appears to be more likely caused by the resin component than the glass ionomer component. It is also suggested that their adhesion is the result of micromechanical interlocking instead of a chemical bond to enamel. CONCLUSION Within this experimental population it is highly recommended to follow the manufacturers' instructions for enamel pretreatment to improve adhesion with the tested materials. Polyacid-modified composites are used with the enamel acid etching technique and are preferred for achieving a tight enamel bond compared with resin-modified glass ionomer materials applied after conditioning with polyacrylic acid-containing agents. REFERENCES
1. McLean JW. The clinical use of glass-ionomer cements. D e n t Clin N o r t h A m 1992;36:693-711. 2. Powis DR, Foller~s T, Merson SA, Wilson AD. Improved adhesion of a glass ionomer cement to dentin a n d enamel. J Dent Res 1982;61:141622.

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3. McCaghren RA, Retief DH, Bradley EL, Denys FR. Shear bond strength of light-cured glass-ionomer to enamel and dentin. J Dent Res 1990;69:40-5. 4. Mitra SB. Adhesion to dentin and physical properties of a light-cured glass-ionomer liner/base. J Dent Res 1991;70:72-4. 5. Hinoura K, Miyazaki M, Onose H. Dentin bond strength of light-cured glass-ionomer cements. J Dent Res 1991;70:1542-4. 6. Lin A, McIntyre NS, Davidson RD. Studies on the adhesion of glass-ionomer cements to dentin. J Dent Res 1992;71:1836-41. 7. Eliades G, Palaghias G. In vitro characterization of visible light-cured glass ionomer liners. Dent Mater 1993;9:198-203. 8. McLean JW, Nicholson JW, Wilson AD. Proposed nomenclature for glass-ionomer dental cements and related materials. Quintessence Int 1994;25:587-9. 9. Nakamichi I, Iwaku M, Fusayama T. Bovine teeth as possible substitutes in the adhesion test. J Dent Res 1983;62:1076-81. 10. Attin T, Buchalla W, Kielbassa AM, Hellwig E. Curing shrinkage and volumetric changes of resin-modified glass ionomer restorative materials. Dent Mater 1995;11:359-62.

11. Buonocore MG. Simple method of increasing the adhesion of acrylic filling materials to enamel surfaces. J Dent Res 1955;34:849-53. 12. Wilson AD, Presser HJ. A survey of inorganic and polyelectrolyte cements. Br Dent J 1984;157:449-54. 13. Aboush YE, Jenkins CB. The effect ofpoly(acrylic acid) cleanser on the adhesion of a glass polyalkenoate cement to enamel and dentine. J Dent 1987;15:147-52.

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B o n d i n g o f r e s i n t e e t h to t h e p o l y m e t h y l m e t h a c r y l a t e d e n t u r e b a s e material. Vallittu PK. Acta Odontol Scand 1995;53:99-104. A common type of failure in an acrylic resin denture is between the denture tooth and acrylic resin denture base (PMMA). This in vitro study compared several types of mechanical treatment of the ridge lap area of acrylic resin denture teeth by determining their bond strength to both heat-polymerizing and autopolymerizing PMMA denture base material. Material a n d Methods. Twenty samples each of heat-polymerizing and autopolymerizing PMMA denture base materials were used to bond acrylic resin teeth. Each 20-sample batch was divided into four groups of five samples, depending on how the PMMA denture tooth was modified in the ridge lap area. The modifications were (1) no treatment, (2) ground, (3) ground and two parallel groves placed, and (4) ground with a 1.5 mm retention hole placed. The dentures and teeth were processed according to the manufacturer's directions and then subjected to a three-point loading fracture test. To determine whether the fracture site was adhesive or cohesive, the fracture surface was analyzed both visually and with a scanning electron microscope. Data were collected and results were analyzed to compare the results between the heat and autopolymerizing PMMA samples. Results. The greatest bond strength to both heat-polymerized and autopolymerized PMMA was obtained by placing grooves on the ridge lap area of the acrylic resin denture tooth before processing of the PMMA denture base (p < 0.001). Heat-polymerized PMMA and autopolymerizing PMMA were equal in their adherence to the acrylic resin denture tooth (p > 0.05). Conclusions. Within the limits of this study it is suggested that for both heat-polymerized and autopolymerized PMMA denture base material, proper grinding of the ridge lap of the PMMA denture tooth with placement of two horizontal retention grooves should precede processing, to achieve the greatest bond strength. 19 References. R P R E N N E R

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