ࡱ>     %`bjbjNN xN,,Y&PPPPX$H dTNTNTN8N,O5\PQ"QQQ]]]$hΆPTh6\]h$hΆPPQQ >6}6}6}h PQPQ6}Th6}6}PP6}QP sTNDu6}TTT56}*{6}N}VJ~]$`>6}cd]]]ΆΆ{N]]]5ThThThTh$(C CddD PPPPPP Surface structural changes of feldspathic ceramics before and after immersion in corrosive medium using Atomic Force Microscopy Mehuli K.1, Svetli i V.2, `egota S.2 Vojvodi D1 1University of Zagreb, School of Dental Medicine, Gundulieva 5, 10000 Zagreb, Croatia 2Ruer Boakovi Institute, P.O.Box 180, HR-10002 Zagreb, Croatia e-mail:  HYPERLINK "mailto:mehulic@sfzg.hr" mehulic@sfzg.hr,  HYPERLINK "mailto:svetlicic@irb.hr" svetlicic@irb.hr,  HYPERLINK "mailto:segota@irb.hr" segota@irb.hr Correspondence to: Mehuli Ketij University of Zagreb School of Dental Medicine Department of Prosthodontics, Gundulieva 5, Zagreb, Croatia E-mail:  HYPERLINK "mailto:mehulic@sfzg.hr" mehulic@sfzg.hr Acknowledgments This work was supported by Grants 065-0650446-0435 and, 098-0982934-2744, denis. This work was presented at IV International Congress of Croatian Dental Society. Zagreb, Croatia, November 2008. Abstract Dental ceramics are attractive dental materials as a result of their superior aesthetics and biocompatibility. However, they are brittle and inclined to premature failure, especially if repeated contact strain and moist environment. Chemical stability of dental ceramics is important because it directly affects mechanical properties and aesthetic value of restorations. The aim of this study was to investigate the effects of the corrosive agent, 4% acetic acid, on the surface of glazed and unglazed feldspathic ceramics. Metal-ceramic plates (9.0 * 9.0 * 1.2 mm) composed of Ni-Cr alloy (Wiron 99, Bego Germany) and glazed or unglazed feldspathic ceramics (IPS Classic, Ivoclar-Vivadent, Schaan, Liechtenstein) were prepared according to the manufacturer's instructions. The samples were immersed in 4% acetic acid at 80C and kept there for 16 h (ISO 6872). The surfaces of the samples before and after immersion in the corrosive medium were examined by atomic force microscopy (AFM). The pre and post-corrosion AFM images of the surfaces of the feldspathic ceramics samples clearly show that the glazed surfaces are much less prone to deterioration by corrosion than the unglazed ones. Key words: dental ceramic, Atomic force microscopy, corrosion, surface morphology, microstructure Introduction The oral cavity is a demanding environment due to variations in pH, solution chemistry, wear and mechanical load. Despite dental ceramic material is supposed to have superior chemical stability compared to other biomaterials (1), still it fails to show absolute chemical inertness in aqueous oral cavity environment. This is even more accentuated when exposed for extended periods of time. Ceramics differ in sensitivity to water (2). Water decreases the strength of most ceramics and glasses, the latter being known since 1958. (3, 4) It is better to consider how ceramics react and on which level with regards to corrosive agents. The corrosive stability determines composition (5), especially ingredient purity (6) and material microstructure (3), environmental conditions, exposure time and temperature (7). The volume of voids or pores existing within the material is indicated by porosity with the detrimental effect being acting as a stress concentrator, as well as it decreases the cross-sectional area over which the force is applied and affects the optical properties by scattering light and decreasing translucency. Porosity control is therefore a fundamental consideration during the design or processing dental ceramics (8). Corrosion of dental ceramics can be proved by elution of inorganic ions from the surface (9) and mass los (5). Possible consequences of corrosion include deterioration of mechanical properties, violation of aesthetic appearance (10) increase of surface roughness (11) and consequently increased plaque adhesion (12). The Atomic Force Microscope (AFM) was invented in 1986. It has become a useful tool for examining material structure at both the micron and nanometre scale allowing atomic images of the surface. AFM can be used in many environments (both liquid and ambient) providing a large range of applications namely studies of phenomena such as abrasion, adhesion, cleaning, corrosion, etching, friction, lubrication, plating, and polishing. It is known that the ceramics surface energies are anisotropic due to the mis-orientation of grains and the absorption of impurities (13, 14). The purpose of this research was to evaluate the structural surface changes of glazed and unglazed feldspathic ceramics before and after immersion in corrosive medium, 4% acetic acid, using the atomic force microscopy techniques. Materials and methods Preparation of the specimens Two metal-ceramic plates (9.0 x 9.0 x 1.2mm) composed of Ni-Cr alloy (Wiron 99, Bego Germany) and feldspathic ceramics (IPS Classic, Ivoclar-Vivadent, Schaan, Liechtenstein) were made. Wax patterns were prepared from a modelling pink wax (modelling wax standard, DeguDent GmbH, Germany). Investing, casting and divesting procedures were carried out as well as grinding and cleaning cast surface prior to the oxidation heat procedures as recommended by the manufacturer. Layering ceramics and firing (ceramic oven P 90, Ivoclar-Vivadent, Schaan, Liechtenstein) were performed according to the firing schedule supplied by the producers with one unglazed and one glazed specimen. The fabrication of the test specimens was performed following the routine technique as closely as possible and by one and the same experienced dental technician. No further treatment was performed in this first part of research. AFM analysis For structural observation of these materials, samples were cleaned before and after AFM imagesimaging. The sample surfaces were washed and cleaned by ethyl alcohol and Mili-Q water in order to remove surface impurity and greasiness previous to drying in gentle nitrogen stream. AFM imaging was performed in air (laboratory atmosphere) under controlled temperature and humidity, prior to which, the samples and the cantilever were allowed to equilibrate at room temperature for at least a half an hour. Multimode Scanning Probe Microscope with Nanoscope IIIa controller (Veeco Instruments, Santa Barbara, CA) with a vertical engagement (JV) 125 m scanner was used. Contact mode was applied using silicon nitride probes (NP-20, Veeco, Nom. Freq. 56 kHz, Nom. spring constant of 0.32 N/m). In the contact mode, physical contact between the ceramic surface and the AFM tip is maintained at all times with constant force. The linear scanning rate was optimized between 1.5 and 2 Hz with scan resolution of 512 samples per line. The three-dimensional motion of the cantilever and the AFM tip attached to the piezo corresponds to the surface morphology of the scanned area. The samples were imaged and collected at 512x512 pixels. Five different scan areas (10x10 m, 50x50 m, 100x100 m) were measured from each sample. The roughness analysis was carried out using the offline NanoScope software, version V614r1. Results are presented as 3D-view of height, as well as Ra, Rms, Rz and the Z range values. Ra is the arithmetic average of the absolute values of the surface height deviations measured from the main plane, Rms is root mean square average of height deviations taken from the mean image date plane, Rz is the average difference in height between the five highest peaks and five lowest valley relative to the Mean Plane, the Z range is maximum vertical distance between the highest and lowest data point within the analyzed region and Mean Plane is plane for which the summation of the square of distances from all points on the true profile to the plane is a minimum. Corrosion procedure After the initial surface analysis, the ceramic specimens were transferred to a 4% acetic acid solution at the temperature of 80C and kept there for 16 h (ISO 6872-for hydrolytic resistance for dental ceramic materials) (15). This solution was chosen due to its frequent use in the household, its pH value (pH=2.4) is comparable to the pH value in certain beverages and fruit drinks, as well as in inner plaque areas in vivo (16). Results The structural changes on the surface of glazed and unglazed feldspathic ceramics before and after immersion in corrosive medium (studied in vitro) are presented as 3D topographic images of height data and as surface roughness analyses (Table 1). AFM data were collected as 100 m (100 m surface areas to include all surface features as well as 10 m (10 m surface areas within the flat surface in order to reveal structural changes at nanometre scale after corrosion that could also directly affect the strength and aesthetic value of ceramic materials in clinical applications (Table 2). The pre-corrosion AFM image of feldspathic ceramics displays a dense surface with very little open porosity clearly exposed in unglazed surface (Figure 1 and 2). AFM analysis of pre and post-corrosion conditions produced evidence of a corrosive attack on exposed surfaces, but to varying degrees. Ra value (scan area 100x100 m) for glazed sample decreased after corrosion and was even smaller (38.3 nm) than before immersion (61 nm) in corroding solution. The indication of high peaks dissolving is seen in lower Rz and Z range values. Grain boundaries became less sharp; glass matrix shows a different appearance, smother, glassier. It can be explained as a consequence of dissolution of glass matrices (Figure 3). Surface of the unglazed sample after immersion showed distinct roughness, Ra value before was 70.9 nm, and after 189 nm. Contact surface has become larger and a number of reactive centres have increased. Rz and Z range values in this scan area were less high peak dissolved, whist roughness in micro scale was not the same as relief. The surface is dominated by differently sized porosities (macro and mezzo) and voids in between seemingly intact areas. However, because of surface deterioration inherent porosity opened up and the surface became covered in numerous micro porosities (Figure 4). Real situation can only be seen on scale 10m x 10 m (Table 2). Before immersion both samples have had similar roughness (Ra glazed 5.52 nm, unglazed 5.29 nm). After immersion Ra value of the glazed sample was about half of its former size (2.13 nm); it s surface became flatter, while the Ra value of the unglazed sample surface significantly increased (6.29 nm); the surface became rougher. The surface roughness of the unglazed sample increased approximately three times after immersion, compared to the glazed one. Contrary, the Rz value and Z range of the glazed sample drastically decreased after immersion (11 x) (Rz 1.52 nm, Z range 40 nm); there remained no high peaks at the surface. The Rz and Z range of the unglazed sample showed twice the value after immersion (Rz 13.9 nm, Z range 135 nm). The relationship between Rz glazed and unglazed samples after treatment is extraordinarily immense (about 10 times bigger for unglazed). Z range glazed sample too shows 3 times the value when compared to the unglazed sample. These numbers can be very clearly illustrated with a 3D image (Figure 5-8). Surface of the unglazed sample after immersion has honeycomb structure and such roughness can be detrimental for restoration, antagonistic teeth and the biologic environment. Discussion Dental ceramics are recognized for their biocompatibility and aesthetic features. However, it has been claimed that these materials also possess a few disadvantages, such as their inability to accommodate tensile forces by plastic deformation and to disseminate such stresses in the vicinity of the cracks or defects (17). It is still not elucidated whether the corrosive media deteriorates above mentioned disadvantages. The observed ceramic sample surfaces are described qualitatively and quantitatively. For quantitative evaluation, only the height mode imaging data and thewere analysed using the NanoScope"! software package (Digital Instruments, version V614r1). software package for image analysis are available with the Nanoscope III-AFM instrument. (Veeco Instruments, Santa Barbara, CA). AFM probes the surface forces between a cantilever tip and the sample deposited on a flat substrate. The tip is raster over the analysis area producing a 3D topographic image. Height measurements can be obtained with sub-nanometre precision. A Veeco Multimode AFM was used for measurements operating in contact mode. AFM imaging offers complementary information to the surface topography and often gives better lateral resolution than by SEM(14). In majority of AFM measurements, variations of surface height are major factor which determine the cut off measure. In rougher surfaces the lower cut off limit used for the z-axis is 500 nm (18), but investigated samples in this research were extremely flat. The AFM analyses displayed differences in surface roughness not only between but also within the individual specimen (12). Ceramic material used in this research was feldspathic type. Feldspathic ceramics are composed of feldspathic glass matrix with different volume fractions of crystalline phases, such as undissolved feldspar, leucite crystals and alumina particles. Owing to the heterogeneous microstructure, the surface degrades in a non-uniform manner, resulting in increased coarseness. The post-corrosion surface roughness values of each of the observation areas displayed wide scatter. The surface changes induced by the corrosion process were obviously strongly influenced by the composition and microstructure; the glass-phase ceramics being more prone to dissolution than the crystalline phases (19). In general the increase of crystalline content is accompanied by the increase of strength and fracture toughness. However, in materials with comparable crystalline content, some other factors such as porosity, grain size, shape and orientation are important in determining mechanical properties. From the clinical standpoint, the alignment of elongated grains parallel to the surface is preferred over perpendicular or random alignment, as the greatest resistance to crack propagation through the core ceramics material is achieved (20). In an aqueous environment ceramics will corrode mainly through ion-exchange processes, leaving behind hydrated surface layers of varying depths and compositions. The surface elemental composition will also be affected by corrosion and lead to altered surface free energy and charge (12). Even though ceramic materials are very resistant to degradation, mechanical wear and chemical dissolution may bring about structural surface changes. By increasing the aggressiveness of the corrosive solutions compared to intraoral conditions, the speed of the corrosion process was accelerated. Immersion in artificial saliva at 22C for 22 years would have been required to produce the same degree of dissolution as exposure to 4% acetic acid at 80C for one week (21). Surface irregularities can lead to failure because of crack propagation, and also serve as niche for plaque retention (22). Castellani (23) was found positive correlation between plaque accumulation and increased surface roughness, indicating the importance of surface characteristics (23). The surface roughness decreased at the initial stage of immersion, and then increased due to the surface dissolution (24). The AFM analysis is precise (measurement at nanoscale) as a surface roughness measuring instrument for dental ceramics compared to other methods such as stylus profiling or laser optical profiler (measurement range at 0,01 to 50m) and also the optical micrographs or SEM images allow only a two-dimensional view (18). Glaze except that fills the flaws in material and strengthens it, also reduces the possibility of wearing the opposite teeth by covering hard elements like crystals and pores at the surface of the ceramic materials (25). It is rather important to know that in clinical practice dentists grind fixed partial dentures (FPD) even after cementation for adjusting the premature opposing teeth contacts. Grinded area is impossible to polish well despite the usage of different materials (26). Some parts of occlusal surface of crowns or bridges thus may remain unglazed and rough and the danger of wearing the opposite teeth out is likely to happen. This study clearly demonstrated that corrosion of unglazed ceramic surfaces significantly increased roughness by transforming the surface to the bee-comb feature, which was not the case with the glazed ceramics, which even showed the decrease of surface roughness after corrosion. Conclusion The AFM analyses allowed visualising very fine structural details of different ceramic finishing treatments. This study has shown that the ceramic materials displayed evidence of surface structural changes when subjected to the provocative corrosion environment with increased roughness of unglazed ceramic and decreased roughness of the glazed ceramic surfaces. References 1. Anusavice KJ. Degradability of dental ceramics. Adv Dent Res. 1992;6:82-9. 2. Kelly JR. Dental ceramics: current thinking and trends. Dent Clin N Am. 2004;48:513-30. 3. Hondrum SO. A review of the strength properties of dental ceramics. J Prosthet Dent.1992;67:849-65. 4. Hohmann W. Dentalkeramik auf der Basis hydrothermaler Glaser. Berlin, Germany: Quintessenz Verlag GmbH, 1993. 5. Stefanovi-Cerjan `, `iljeg M, urkovi L, }ivko-Babi J. Kemijska degradacija dentalne keramike. Kem Ind. 2002;51(4):163-7. 6. urkovi L, Fuduri-Jela a M, Kurajica S. Corrosion behavior of alumina ceramics in aqueous HCL and H2SO4 solutions. Corrosion Science. 2008;50:872-78. 7. Jakovac M, }ivko-Babi J, urkovi L, Aurer A. Measurement of ion elution from dental ceramics. J Europ Ceram Soc. 2006;26:1695-700. 8. Albakry M, Guazzato M, Swain MV. Influence of Hot Pressing on the Microstructure and Fracture Toughness of Two Pressable Dental Glass-Ceramics. J Biomed Mater Res Part B: Appl Biomater. 2004; 71B:99-107. 9. }ivko-Babi J, Lisjak D, urkovi L, Jakovac M. Estimation of chemical resistance of dental ceramics by neural network. Dent Mater. 2008;24:18-27. 10. Cheung KC, Darvell BW. Sintering of dental porcelain: effect of time and temperature on appearance and porosity. Dent Mater. 2002;18:163-73. 11. Martinez-Gomis J, Buzar J, Anglada JA, Samso J, Peraire M. Comparative Evaluation of Four Finishing Systems on One Ceramic Surface. Int J prosthodont. 2003;16:744-77. 12. Milleding P, Carlen A, Wennerberg A, Karlsson S. Protein Characterisation of salivary and plasma biofilms formed in vitro on non-corroded and corroded dental ceramic materials. Biomaterials. 2001;22:2545-55. 13. http://www.keele.ac.uk/depts/ch/groups/csg 14. Batina N, Renugopalakrishnan V, Casilas Lavin PN, Guerrero JCH, Morales M, Garduno-Juarez, Lakka SL. Ultrastructure of Dental Enamel afflicted with Hypoplasia: An Atomic Force Microscopic Study. Calcif Tissue Int. 2004;74:294-301. 15. ISO 6872 International Standards for Dental Ceramics. International Organization for Standardization. Geneva, Switzerland, 1995. 16. 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In: Sauer BW, editor. Biomechanical engineering-recent developments. Proc Biomedical Engineering Conf, New York: Pergamon, 1985:152-5. 22. Esquivel-Upshaw JF, Chai J, Sansano S, Shonberg D. Resistance to Staining, flexural Strength, and Chemical Solubility of Core Porcelains for All-Ceramic Crown. Int J Prosthodont. 2001;14:284-8. 23. Castellani D, Bechelli C, Tiscione E, lo Nostro L, Pierleoni PP. In vivo plaque formation on cast ceramic (Dicor) and conventional ceramic. Int J Prosthodont. 1996;9:459-65. 24.  HYPERLINK "http://www.scientific.net/AFM+Study" http://www.scientific.net/AFM+Study. 25. 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Effects of various treatment and glazing (coating) techniques on the roughness and wettability of ceramic dental restorative surfaces. Colloid Surface B. Biointerfaces. 2006;53:254-9. 26. Karan S, Toroglu MS. Porcelain Refinishing with Two Different Polishing Systems after Orthodontic Debonding. Angle Orthodont. 2008;78:947-53. SurfaceRa/nmRms/nmRz/nmZrange/nm Glazed before50m E 50m 100m E 100m34.3 6148.8 91.7127 2271198 1427Glazed after50m E 50m 100m E 100m28.3 38.331.3 47.7102 103768 832Unglazed before50m E 50m 100m E 100m58.7 70.997.7 102164 1621989 1727Unglazed After50m E 50m 100m E 100m87.7 189125 278141 1471394 1389 Table 1. Surface roughness before and after immersion in corrosive medium before AfterglazedunglazedglazedunglazedRa /nm5.525.292.136.29Rms / nm7.396.833.369.27Rz / nm17.97.681.5213.9Z range/nm79.297.140135 Table 2. Surface roughness before and after immersion in corrosive medium, scan area 10 (m 10 (m x 200 nm  SHAPE \* MERGEFORMAT  Figure 1. 3D AFM of the glazed feldspathic ceramic before treatment. Image size100 m x 100 m x 2.0 (m  SHAPE \* MERGEFORMAT  Figure 2. 3D AFM of the unglazed feldspathic ceramic before treatment. Image size100 m x 100 m x 2.0 (m  SHAPE \* MERGEFORMAT  Figure 3. 3D AFM of the glazed feldspathic ceramic after treatment. Image size100 m x 100 m x 2.0 (m  SHAPE \* MERGEFORMAT  Figure 4. 3D AFM of the unglazed feldspathic ceramic after treatment. Image size100 m x 100 m x 2.0 (m  SHAPE \* MERGEFORMAT  Figure5. 3D AFM of the glazed feldspathic ceramic before treatment. Image size10 m x 10 m x 200 nm  SHAPE \* MERGEFORMAT  Figure 6. 3D AFM of the glazed feldspathic ceramic after treatment. Image size10 m x 10 m x 200 nm  SHAPE \* MERGEFORMAT  Figure 7. 3D AFM of the unglazed feldspathic ceramic before treatment. Image size10 m x 10 m x 200 nm  SHAPE \* MERGEFORMAT  Figure 8. 3D AFM of the unglazed feldspathic ceramic after treatment. 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