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RESEARCH REPORT |
1 Paediatric Dentistry and Orthodontics, Faculty of Dentistry, University of Hong Kong, Prince Philip Dental Hospital, 34 Hospital Road, Hong Kong SAR, China;
2 Department of Oral Biology and Maxillofacial Pathology, Medical College of Georgia, Augusta, GA, USA;
3 Department of Restorative Dentistry, University of Newcastle, Newcastle upon Tyne, UK;
4 Department of Restorative Dentistry, National University of Singapore, Singapore;
5 Department of Dental Materials, University of Granada, Spain; and
6 Electron Microscopy Unit, University of Hong Kong, Hong Kong SAR, China;
* corresponding author, kfctay{at}hknet.com
| ABSTRACT |
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KEY WORDS: glass ionomer spherical bodies water diffusion
| INTRODUCTION |
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To date, both ultrastructural and analytical evidence is available on the existence of an intermediate layer along the GIC-dentin/enamel interfaces that is caused by ion exchange between the material and tooth substrate (Geiger and Weiner, 1993; Ngo et al., 1997; Ferrari and Davidson, 1997; Sennou et al., 1999; Tay et al., 2001a; Yip et al., 2001). Water permeation from dentin into GICs (Watson et al., 1991, 1998) or resin-modified GICs (Sidhu and Watson, 1998) has been observed by dynamic laser confocal microscopy. This phenomenon of localized water sorption has not been previously observed in GIC-bonded dentin. The consequence of such water permeation across the GIC-dentin interface is unknown.
This study used scanning electron microscopy (SEM), field-emission/environmental SEM (FE-ESEM), and transmission electron microscopy (TEM) to examine the regional differences in the ultrastructure of GIC bonded onto moist human dentin. Dentin surfaces bonded with 6 auto-cured GICs were examined along the fractured GIC-dentin interfaces. Additional GIC specimens were fractured 3 mm away from the interfaces, and fractured unbonded GIC samples were used as controls. The null hypothesis tested was that there is no difference among the ultrastructural features of GICs fractured at different locations from the bonded dentin, and fractured unbonded GICs.
| MATERIALS & METHODS |
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Experimental Design
Dentin surfaces were abraded with 180-grit silicon carbide paper and further treated with polyacrylic acid (Cavity Conditioner; GC Corp., Tokyo, Japan) for 10 sec immediately before being bonded with the GICs. Five teeth were prepared for each of the 6 auto-cured GICs tested: Fuji IX GP and Fuji VII (GC Corp.), ChemFlex and Experimental batch K-136 (Dentsply DeTrey, Konstanz, Germany), Ketac-Molar Aplicap (3M ESPE, St. Paul, MN, USA), and Hy-Bond (Shofu, Kyoto, Japan). The GICs were dispensed/mixed and bonded according to the manufacturers instructions, to form 6-mm-high cores over the surfaces of the moist dentin.
Additional GICs were mixed and applied to the surfaces of mylar strips, which were then allowed to cure without being bonded to tooth substrates.
After initial setting, both the bonded and unbonded GICs were covered with a thin layer of light-cured, oxygen-inhibition-layer-free, glaze resin (BisCover, Bisco Inc., Schaumburg, IL, USA), to prevent them from losing or gaining water via external sources. After storage at 37°C and 100% relative humidity for 48 hrs, the bonded specimens were cut occlusogingivally into 0.9 x 0.9 mm beams, following the method used for evaluation of microtensile bond strengths of GICs (Tay et al., 2001a). With this technique, none of the specimens fractured during preparation into beams, confirming our previous experience. Similar beams were prepared from the unbonded GICs.
These beams were sealed in bottles at 100% humidity for 48 hrs before analyses. For SEM examination, 5 beams were randomly selected from the teeth bonded with each GIC, and fractured close to the GIC-dentin interface by three-point bending (razor blade at interface of end-supported beams). We fractured 5 additional bonded beams, at a location that was approximately 3 mm away from the bonded interfaces, by moving the supports. Both the dentin and GIC sides of these beams were air-dried, sputter-coated with gold/palladium, and examined with a SEM (Cambridge Stereoscan 440, Cambridge, UK) operating at 10 kV.
A similar number of beams from each group was used for FE-ESEM examination. The beams were fractured on-site, inserted immediately into the Peltier (cooling) stage of the microscope (Philips XL-30, Eindhoven, The Netherlands), and covered with water to avoid desiccation of the fractured GICs. They were examined at 15 kV, wet and without being coated, with the temperature of the Peltier stage fixed at 4°C and the vapor pressure of the specimen chamber varying between 5.4 and 5.9 Torr to generate a relative humidity of 9699.9%. We used energy-dispersive x-ray (EDX) analysis to determine the composition of various structural phases identified by FE-ESEM along the fractured GIC-dentin interfaces.
To determine the extension of spherical bodies from bonded interfaces, we bonded 2 teeth with Fuji VII to form 6-mm-high cores over the surface of moist dentin, with the surface sealed with glaze resin. Bonded GIC-dentin slabs 2 mm wide were sectioned occluso-gingivally from the bonded teeth. They were polished under wet conditions with 1200-grit SiC paper, followed by 1 µm alpha alumina (Buehler Ltd.). These surfaces were briefly etched for 15 sec with 10% phosphoric acid (Bisco Inc.) to remove the smear layer and to bring the interfaces into relief. Two additional teeth were similarly bonded with Fuji VII, but without the surfaces being sealed with glaze resin. After setting of the GIC, these 2 teeth were immersed in distilled water for 10 min before storage at 100% relative humidity for 48 hrs. GIC-dentin slabs 2 mm wide were similarly prepared and examined by FE-ESEM.
TEM examination was performed only on bonded GIC-dentin interfaces. Two beams were examined for each GIC. Intact beams (i.e., without being fractured) were processed and resin-embedded according to the TEM protocol for GIC examination described by Tay et al.(2001a). Examination of 90-nm-thick sections was performed with a transmission electron microscope (Philips EM208S), operating at 80 kV.
| RESULTS |
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| DISCUSSION |
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EDX and TEM results further confirmed that the shells of these spherical bodies were not simply siliceous hydrogel layers of the FASG fillers, since the latter contained distinct fluoride-rich, electron-dense, "seed-like" phases that are characteristic of the original glass composition (Barry et al., 1979; Tay et al, 2001b). Rather, the eggshell-like structure represents a distinct Si-rich phase that has a composition slightly different from that of the original polyalkenoate matrix. The Si-rich phase is probably formed as a result of water diffusion across the bonded interface, initiating the delayed GI reaction that occurred during the maturation phase of GIC. Since permeation of water into GIC is a diffusion-controlled process, we speculate that a longer storage time will allow more spherical bodies to form. The presence of this secondary phase resembles the silica phase that was observed following the aging of GICs (Wasson and Nicholson, 1993; Matsuya et al., 1996). Undeniably, the EDX used during FE-ESEM examination has a relatively large depth of compositional analysis that may affect the accuracy of our results. However, recent examination of elemental compositions of spherical bodies by TEM/EDX analysis resulted in similar conclusions (Tay, unpublished results).
The difference between the hollow appearance of the spherical bodies, as observed with SEM and TEM, and their solid appearance, under FE-ESEM, may be attributed to the presence of a pool of water within the eggshell-like structure when specimens were examined by the latter technique. When the specimens were examined by conventional SEM, the water probably evaporated from the fractured shells, revealing the original eggshell-like characteristics.
Since the GICs were protected with resin-coatings in the present study, water for the additional GIC reaction could be provided only by the underlying moist dentin. Such a phenomenon parallels what has been recently reported for single-step, self-etch dentin adhesives (Tay et al., 2002), in which water can diffuse from moist dentin through the adhesive layer to form water droplets along the adhesive-composite interface, with the adhesive layer acting as a semi-permeable membrane. Since an intermediate layer (Tanumiharja et al., 2001) is present between dentin and GIC (Fig. 4A
), we hypothesize that a similar osmotic gradient may exist in the ion-rich polyalkenoate matrix that causes permeation of water across the GIC-dentin interface and initiated the additional GI reaction. Although such a hypothesis awaits confirmation, it provides a rationale for why only air-voids were observed when GIC-bonded dentin specimens were fractured at sites farther from the bonded interfaces. It also provides a reasonable explanation for the observed water permeation from dentin into GICs (Watson et al., 1998) during dynamic imaging of GIC-bonded dentin.
The additional Si-rich phase represented by these spherical bodies probably played an important role in strengthening GIC along the bonded interface. Leiskar et al.(2003) reported a continuous increase in shear punch strength for up to 2 wks when Fuji IX GP, that was not initially protected by a resin coating, was exposed to water. Similar results were reported by Miyazaki et al.(1996). The clinical implication is that bonded GICs will continue to draw water from the underlying moist dentin for additional acid-base reactiona process that does not occur in GIC-bonded enamel, due to its lower water content (ten Bosch et al. 2000). The clinical disadvantage is that the GIC may draw water from dentin fast enough to cause the occasional post-operative sensitivity (Christensen, 1990) that is associated with their use.
In conclusion, in the absence of water-sorption from external sources, the existence of a distinct Si-rich phase within the air-voids of GIC-bonded dentin is probably caused by the permeation of water across the GIC-dentin interface, as previously reported by Watson et al.(1998). Since similar water movement across bonded resin-modified GICs has resulted in the formation of an amorphous "absorption layer" (Sidhu and Watson, 1998; Sidhu et al., 1999, 2002), further research should be performed to examine if similar spherical bodies could be seen in this class of restorative material.
| ACKNOWLEDGMENTS |
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Received February 15, 2003; Last revision December 5, 2003; Accepted January 22, 2004
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