钴铬合金基牙科遮色瓷粉的制备与性能研究
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摘要
本论文利用水热法制备的白榴石前驱体与基础熔块合成了含超细白榴石增强型牙科陶瓷材料，对合成过程中白榴石的析晶机理进行了研究。利用X射线衍射仪（XRD）、高温X射线衍射仪（HXRD）、差热仪（DSC-TG）和扫描电子显微镜（SEM）等分析了白榴石前驱体在基础熔块中的析晶温度和相变过程以及白榴石在烤瓷材料中的显微结构。探讨了向牙科烤瓷材料中添加MoO_3和TiO_2粉体对烤瓷-钴铬合金体系高温润湿性、界面反应以及结合性能的影响。采用乳浊剂SnO_2和CeO_2提高烤瓷对钴铬合金基底的遮色性能。对遮色瓷进行了计算机配色研究，建立了遮色瓷配色数据库。
将30wt%的水热法制备的白榴石前驱体与70wt%的高温熔融法制备的基础熔块混合均匀后在750℃制备了含超细白榴石增强型牙科陶瓷材料。基础熔块中存在大量的碱金属和碱土金属氧化物，能够使陶瓷材料在较低温度下得到液相，产生离子空位，增加系统的化学能，XRD结果表明白榴石的析晶温度由1027℃下降到了720℃。白榴石晶体在720℃左右开始析出立方相白榴石，在冷却到室温的过程中立方相白榴石相变为四方相白榴石。从700℃到900℃，与基础熔块混合的白榴石前驱体有一个析晶和分解的平衡状态，当温度达到750℃后白榴石晶体的含量基本保持不变，保证了烤瓷材料性能的稳定。利用这种材料配制的牙科烤瓷材料热处理920℃后，烤瓷材料的表面和断面都观测到了平均粒径为115nm的白榴石晶体，并且这些白榴石晶体均匀的分散在烤瓷基体中，明显提高了烤瓷材料的强度和韧性。
利用高纯的白榴石与基础熔块建立了定量XRD分析的标准曲线，测定了用低温法制备的含超细白榴石晶体的牙科陶瓷材料中白榴石的含量，大致在30-34wt%之间。
利用高温可视炉、扫描电镜以及拉曼光谱研究了烤瓷与钴铬合金的高温润湿性与界面结合机理，发现添加MoO_3和TiO_2粉体到瓷粉中有助于提高金瓷高温润湿性，且得到了配方：2wt%MoO_3,3wt%TiO_2,1wt%SnO_2和94wt%基体瓷粉。添加的TiO_2在高温下可以降低熔融烤瓷的粘度和表面张力，而添加物MoO_3可以促进烤瓷和钴铬合金间的界面反应，因此添加MoO_3和TiO_2的烤瓷材料具有更好的高温润湿性，并且在热处理过程中均形成了含有新物相的过渡层，过渡层的主要成分为铬的氧化物，烤瓷中的成分会向过渡层扩散并发生化学反应。有上述添加物的烤瓷/Co-Cr合金体系中的过渡层比没有添加物的烤瓷/Co-Cr合金体系更宽。试样进行金瓷三点抗弯测试的断裂面都处于金瓷过渡层靠近陶瓷面的部分，断裂后的合金面有陶瓷嵌入，这种断裂方式表明金瓷两相的结合性较好。添加MoO_3和TiO_2的烤瓷/Co-Cr合金体系和未添加的烤瓷/Co-Cr合金体系的三点抗弯强度分别为43±2和38±3MPa，都远高于烤瓷材料国际标准ISO9693中规定的合格强度25MPa。
添加一定量的乳浊剂（SnO_2和CeO_2）可以提高烤瓷对钴铬合金的遮色能力，当添加量为：5wt%SnO_2，3wt%CeO_2时，遮色瓷在烤瓷厚度为0.2±0.02mm时就能达到对钴铬合金的完全遮色。
制备了钒锆黄、锆镨黄、铝锌红和锆钒蓝四种色料的遮色瓷单色色种，建立了配色数据库。并以VitaA2，A3色料为标准进行计算机配色，在多次配色实验，修正后得到了两组配方，与Vita标准色之间的色差分别为1.17和1.12，均小于人眼所能觉察的色差值。
In this research, a superfine leucite-reinforced dental material was prepared byhydrothermally-derived leucite precursor and basic frit. The leucite crystallizationmechanism and phase transition process were investigated. The effect of basic frit onthe crystallization temperature and phase transition process during the leucitecrystallization, as well as the microstructure of leucite crystal in dental porcelain wereanalyzed by X-ray diffractometer (XRD), High-temperature X-ray diffractometer(HXRD), DSC-TG analysis and Scanning Electron Microscopy (SEM). To understandthe wetting and spreading behaviors, the interfacial reactions, and the bondingmechanism of porcelain fused on metal with TiO_2and MoO_3added to the dentalporcelain. The effect of dental porcelain added with SnO_2and CeO_2on color maskingability was investigated. Computer color matching of opaque porcelain was studied,and the opaque porcelain color database was established.
A superfine leucite-reinforced dental material was prepared by heat-treating themixture of30wt%hydrothermally-derived leucite precursor and70wt%basic frit at750℃. The alkali and alkaline earth mental oxides in the basic frit can form liquidphases earlier, create cation vacancies, increase the chemical potential of the system,and thus effectively lower the crystallization temperature of leucite from1027℃to720℃. The cubic leucite was crystallization at720℃and the cubic leucite wouldtransform to tetragonal leucite in the cooling process. There exists a temperature rangefrom700℃to900℃in which leucite crystals are in the equilibrium of forming anddecomposition, when the temperature reached750℃, the content of leucite wasunchanged. The leucite average size in the dental porcelain prepared by the mixture oflow temperature frit and the material is about115nm, and the superfine leuciteparticles are homogeneously distributed in the matrix, which would improve thestrength and toughness of dental materials.
In order to determine the leucite content in the dental material, quantitative XRDanalysis was used. The calibration curve was established by mixing various weight fraction of pure leucite into the basic frit. The leucite content in the dental material isabout30-34wt%.
The high temperature wettability and bonding mechanism of porcelain to Co-Cralloy were investigated by TOMMI optical dimension measurement system, SEM andRaman spectra. The addition of TiO_2and MoO_3in the dental porcelain improved thewettability of the dental porcelain/Co-Cr alloy system, and obtained the formulationwas2wt%MoO_3,3wt%TiO_2,1wt%SnO_2and94wt%porcelain. The addition ofTiO_2can lower the high temperature viscosity of the dental porcelain and theexistence of MoO_3may promote the reaction between dental porcelain and the Co-Cralloy. The high temperature wetting of porcelain to Co-Cr alloy was reactive wetting,an intermediate layer with a new phase was formed, the main component of theintermediate layer was the oxide of chromium, and there existed diffusion andchemical reactions from porcelain to the intermediate layer. The intermediate layer ofthe porcelain added with TiO_2and MoO_3/Co-Cr alloy system is wider than theporcelain without TiO_2and MoO_3/Co-Cr alloy system. The bond strength of theporcelain modified with TiO_2and MoO_3was43±2MPa and that of the unmodifiedporcelain was38±3MPa. The bond strength of two samples is much higher than ISOstandard9693(the acceptable bond strength of metal ceramic restorations is25MPa).The fracture occurred near the porcelain layer, and part of the porcelain wasembedded into the matrix of the Co-Cr alloy.
The addition of SnO_2and CeO_2in dental porcelain can raise the color maskingability, when the adding amount was5wt%SnO_2,3wt%CeO_2, the opaque porcelain(thickness of opaque was0.2±0.02mm) can mask cobalt-chromium alloycompletely.
The monochrome color samples of vanadium-zirconium yellow,zirconium-praseodymium yellow, chromium-aluminium-zincum red andzirconium-vanadium blue were prepared, and the opaque porcelain color database wasestablished. Computer color matching experiments of the opaque porcelain were performed accoding to the database. The chromatic aberration of opaque porcelainsprepared by this work and Vita A2、A3were1.17and1.12, respectively, which wereless than what the human eye can distinguish.
将30wt%的水热法制备的白榴石前驱体与70wt%的高温熔融法制备的基础熔块混合均匀后在750℃制备了含超细白榴石增强型牙科陶瓷材料。基础熔块中存在大量的碱金属和碱土金属氧化物，能够使陶瓷材料在较低温度下得到液相，产生离子空位，增加系统的化学能，XRD结果表明白榴石的析晶温度由1027℃下降到了720℃。白榴石晶体在720℃左右开始析出立方相白榴石，在冷却到室温的过程中立方相白榴石相变为四方相白榴石。从700℃到900℃，与基础熔块混合的白榴石前驱体有一个析晶和分解的平衡状态，当温度达到750℃后白榴石晶体的含量基本保持不变，保证了烤瓷材料性能的稳定。利用这种材料配制的牙科烤瓷材料热处理920℃后，烤瓷材料的表面和断面都观测到了平均粒径为115nm的白榴石晶体，并且这些白榴石晶体均匀的分散在烤瓷基体中，明显提高了烤瓷材料的强度和韧性。
利用高纯的白榴石与基础熔块建立了定量XRD分析的标准曲线，测定了用低温法制备的含超细白榴石晶体的牙科陶瓷材料中白榴石的含量，大致在30-34wt%之间。
利用高温可视炉、扫描电镜以及拉曼光谱研究了烤瓷与钴铬合金的高温润湿性与界面结合机理，发现添加MoO_3和TiO_2粉体到瓷粉中有助于提高金瓷高温润湿性，且得到了配方：2wt%MoO_3,3wt%TiO_2,1wt%SnO_2和94wt%基体瓷粉。添加的TiO_2在高温下可以降低熔融烤瓷的粘度和表面张力，而添加物MoO_3可以促进烤瓷和钴铬合金间的界面反应，因此添加MoO_3和TiO_2的烤瓷材料具有更好的高温润湿性，并且在热处理过程中均形成了含有新物相的过渡层，过渡层的主要成分为铬的氧化物，烤瓷中的成分会向过渡层扩散并发生化学反应。有上述添加物的烤瓷/Co-Cr合金体系中的过渡层比没有添加物的烤瓷/Co-Cr合金体系更宽。试样进行金瓷三点抗弯测试的断裂面都处于金瓷过渡层靠近陶瓷面的部分，断裂后的合金面有陶瓷嵌入，这种断裂方式表明金瓷两相的结合性较好。添加MoO_3和TiO_2的烤瓷/Co-Cr合金体系和未添加的烤瓷/Co-Cr合金体系的三点抗弯强度分别为43±2和38±3MPa，都远高于烤瓷材料国际标准ISO9693中规定的合格强度25MPa。
添加一定量的乳浊剂（SnO_2和CeO_2）可以提高烤瓷对钴铬合金的遮色能力，当添加量为：5wt%SnO_2，3wt%CeO_2时，遮色瓷在烤瓷厚度为0.2±0.02mm时就能达到对钴铬合金的完全遮色。
制备了钒锆黄、锆镨黄、铝锌红和锆钒蓝四种色料的遮色瓷单色色种，建立了配色数据库。并以VitaA2，A3色料为标准进行计算机配色，在多次配色实验，修正后得到了两组配方，与Vita标准色之间的色差分别为1.17和1.12，均小于人眼所能觉察的色差值。
In this research, a superfine leucite-reinforced dental material was prepared byhydrothermally-derived leucite precursor and basic frit. The leucite crystallizationmechanism and phase transition process were investigated. The effect of basic frit onthe crystallization temperature and phase transition process during the leucitecrystallization, as well as the microstructure of leucite crystal in dental porcelain wereanalyzed by X-ray diffractometer (XRD), High-temperature X-ray diffractometer(HXRD), DSC-TG analysis and Scanning Electron Microscopy (SEM). To understandthe wetting and spreading behaviors, the interfacial reactions, and the bondingmechanism of porcelain fused on metal with TiO_2and MoO_3added to the dentalporcelain. The effect of dental porcelain added with SnO_2and CeO_2on color maskingability was investigated. Computer color matching of opaque porcelain was studied,and the opaque porcelain color database was established.
A superfine leucite-reinforced dental material was prepared by heat-treating themixture of30wt%hydrothermally-derived leucite precursor and70wt%basic frit at750℃. The alkali and alkaline earth mental oxides in the basic frit can form liquidphases earlier, create cation vacancies, increase the chemical potential of the system,and thus effectively lower the crystallization temperature of leucite from1027℃to720℃. The cubic leucite was crystallization at720℃and the cubic leucite wouldtransform to tetragonal leucite in the cooling process. There exists a temperature rangefrom700℃to900℃in which leucite crystals are in the equilibrium of forming anddecomposition, when the temperature reached750℃, the content of leucite wasunchanged. The leucite average size in the dental porcelain prepared by the mixture oflow temperature frit and the material is about115nm, and the superfine leuciteparticles are homogeneously distributed in the matrix, which would improve thestrength and toughness of dental materials.
In order to determine the leucite content in the dental material, quantitative XRDanalysis was used. The calibration curve was established by mixing various weight fraction of pure leucite into the basic frit. The leucite content in the dental material isabout30-34wt%.
The high temperature wettability and bonding mechanism of porcelain to Co-Cralloy were investigated by TOMMI optical dimension measurement system, SEM andRaman spectra. The addition of TiO_2and MoO_3in the dental porcelain improved thewettability of the dental porcelain/Co-Cr alloy system, and obtained the formulationwas2wt%MoO_3,3wt%TiO_2,1wt%SnO_2and94wt%porcelain. The addition ofTiO_2can lower the high temperature viscosity of the dental porcelain and theexistence of MoO_3may promote the reaction between dental porcelain and the Co-Cralloy. The high temperature wetting of porcelain to Co-Cr alloy was reactive wetting,an intermediate layer with a new phase was formed, the main component of theintermediate layer was the oxide of chromium, and there existed diffusion andchemical reactions from porcelain to the intermediate layer. The intermediate layer ofthe porcelain added with TiO_2and MoO_3/Co-Cr alloy system is wider than theporcelain without TiO_2and MoO_3/Co-Cr alloy system. The bond strength of theporcelain modified with TiO_2and MoO_3was43±2MPa and that of the unmodifiedporcelain was38±3MPa. The bond strength of two samples is much higher than ISOstandard9693(the acceptable bond strength of metal ceramic restorations is25MPa).The fracture occurred near the porcelain layer, and part of the porcelain wasembedded into the matrix of the Co-Cr alloy.
The addition of SnO_2and CeO_2in dental porcelain can raise the color maskingability, when the adding amount was5wt%SnO_2,3wt%CeO_2, the opaque porcelain(thickness of opaque was0.2±0.02mm) can mask cobalt-chromium alloycompletely.
The monochrome color samples of vanadium-zirconium yellow,zirconium-praseodymium yellow, chromium-aluminium-zincum red andzirconium-vanadium blue were prepared, and the opaque porcelain color database wasestablished. Computer color matching experiments of the opaque porcelain were performed accoding to the database. The chromatic aberration of opaque porcelainsprepared by this work and Vita A2、A3were1.17and1.12, respectively, which wereless than what the human eye can distinguish.
引文
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