| The application of the silicon coating modification combined with the silane coupling agent can significantly improve the bonding strength between the zirconia ceramic and the resin cement.The steam phase hydrolysis technique volatilizes water or other liquids by heating,and the high-pressure steam promotes the hydrolysis of the reactant precursors or reacts with them,thereby forming a uniform coating of the shell material on the core material.The electrostatic self-assembly process utilizes the oppositely-charged polyelectrolyte at the solid-liquid interface through electrostatic adsorption to alternately deposit and form a film.In this experiment,a silicon coating was prepared on the surface of zirconia ceramics by vapor phase hydrolysis and electrostatic self-assembly techniques to investigate the preparation process of dental zirconia ceramic surface coatings suitable for clinical application of oral cavity.At the same time,the effects of these two silicon coating technologies on the short-term bonding strength of ceramics and resins were studied.Part One Effect of Vapor Phase Hydrolysis Silicon Coating Modification on the Bond Strength of Zirconia CeramicsObjective:To explore the feasibility of silicon coating modification on zirconia ceramic surface by steam phase hydrolysis method and the influence of its modification on the bonding strength.Methods:The sandblasted zirconia ceramic pieces were divided into 5 groups(n=7)and subjected to the following surface treatments: Ctr: control group;JT: dip coating group;SS: double acid(H2SO4/HNO3)treatment group;SS +JT: diacid(H2SO4/HNO3)treatment + dip coating group;SS+ZQX: diacid(H2SO4/HNO3)treatment + vapor phase hydrolysis group;heat treatment was performed on the zirconia ceramics of the JT and SS+JT groups.Silica gel structure before and after heat treatment of Fourier transform infrared spectrum(FTIR);Scanning electrical microscopy(SEM)and energy dispersive X-ray spectroscopy(EDS)for different treated ceramic surface structures and elements are observed and analyzed.The ceramic/resin bonding test pieces were made and embedded in the self-curing plastic after 24 hours in the water bath,and the shear adhesive strength of each set of test pieces was tested.Stereomicroscopes were used to observe the fracture patterns of each group,and the representative fracture surface morphology of each group was observed by scanning electron microscopy.Results:FTIR shows that Si-O-Si asymmetric stretching peaks,Si-O-Si symmetric stretching peaks and Si-O-Si bending vibration absorption peaks after heat treatment of silica sols are strengthened;SEM shows that the surface of the silicon coating produced by the vapor phase process is uneven In the particle accumulation state,there are pores with different sizes between the particle aggregation states;EDS shows that the content of Si on the surface of the zirconia ceramic after coating is significantly increased.The zirconium oxide ceramic surface prepared by vapor phase hydrolysis of silicon coating can improve the bonding strength of ceramic and resin,compared with other groups are different Statistically significant(P<0.01).Conclusions:The vapor phase hydrolysis method can prepare a silicon coating on the surface of the zirconia ceramic to realize the surface modification of the zirconia ceramics,and the adhesion strength of the zirconia ceramic can be significantly improved compared with the traditional sol-gel method silicon coating.Part Two Effect of silicon coating modification via electrostatic self-assembly on the adhesion strength of zirconia ceramicsObjective:To explore the feasibility of silicon coating modification on zirconia ceramic surface by electrostatic self-assembly silicon coating modification,and the influence of its modification on the bonding strength.Methods:The grit-blasted zirconia ceramic pieces were divided into 7 groups(n=7)and subjected to the following surface treatments respectively: Ctr: control group;JT: dip coating group;Prh: "Piranha" solution treatment group;Prh+JT: "Piranha" solution treatment + dip coating group;Prh+Zzz1: "Piranha" solution treatment + self-assembly layer 1 group;Prh+Zzz2: "Piranha" solution treatment + self-assembled layer 2 group;Prh+Zzz3: "Piranha" solution treatment+self-assembled three-layer groups were subjected to heat treatment on the zirconia ceramics of the JT,Prh+JT,Prh+Zzz1,Prh+Zzz2,and Prh+Zzz3 groups.Infrared spectroscopy analysis of the PDDA/silica sol structure before and after heat treatment;scanning electron microscopy and energy dispersive spectroscopy were used to observe and analyze the ceramic surface structure and elements after different treatments.The ceramic/resin bonding test pieces were made and embedded in the self-curing plastic after 24 hours in the water bath,and the shear adhesive strength of each set of test pieces was tested.Stereomicroscopes were used to observe the fracture patterns of each group,and the representative fracture surface morphology of each group was observed by scanning electron microscopy.Results:Electrostatic self-assembly method was used to prepare silicon coating on the surface of zirconia ceramics.FTIR showed that the FTIR spectra before and after heat treatment of PDDA/silica sol were similar to those of silica sol before and after heat treatment.The SEM shows that the surface of the zirconia ceramics treated differently shows different morphologies,and the surface of the ceramics of the silicon coating group subjected to the electrostatic self-assembly method is uneven.With the increase of the number of coatings,the morphology of gullies gradually becomes wider and shallower from narrow to deep.The number of cracks formed after heat treatment of silicon coating increases and the cracks become wider and deeper.EDS analysis shows that the content of Si on the surface of ceramics after coating significantly increases.The electrostatic self-assembly method modified by silicon coating can significantly improve the bonding strength between ceramic and resin,and has statistical significance with other groups(P<0.01).Conclusions:The electrostatic self-assembly method can produce silicon coating on the surface of zirconia ceramics to achieve surface modification of zirconia ceramics,and can significantly improve the bonding strength of zirconia ceramics,of which the self-assembled two-layer group has the best effect. |
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