牙科Y-TZP陶瓷着色方法及性能研究

发布时间：2018-04-05 11:07

本文选题：共沉淀　切入点：Y-TZP　出处：《浙江大学》2015年硕士论文

【摘要】：随着人们生活质量的不断提高,对牙科修复材料提出了更高的要求。近三十年来,Y-TZP(钇稳定四方相氧化锆多晶体,yttria-stabilized tetragonal zirconia polycrystalline)陶瓷因高强度、美观性及较好的生物相容性得到了学术界和产业界的广泛关注。对于牙科修复体,透光性和色度是最重要的性能指标。然而,Y-TZP陶瓷的颜色与天然牙色存在一定差距。在传统的遮色处理中,饰面层/Y-TZP双瓷层结构在实现色度调控的同时,也损失了一部分透光性和力学性能。因而自着色Y-TZP全瓷冠成为了人们关注的焦点。目前,国内关于着色方法对Y-TZP性能影响的报道很少。本文采用化学共沉淀法制备了ZrO2(3Y)纳米粉。并基于此系统地研究了不同着色方法对着色Y-TZP力学性能、透光性及色度的影响。选用Fe2O3、CeO2为着色剂,着色方法包括：共沉淀原位生成掺杂、着色剂与ZrO2(3Y)粉体机械混合、着色液浸泡ZrO2(3Y)造粒粉体和着色液浸泡Y-TZP素胚。最终取得主要结果如下：(1)采用化学共沉淀制备了ZrO2(3Y)纳米粉。研究发现：PEG-6000添加量为1.4 wt%时,对前驱体悬浊液的分散效果最好,热处理后的粉体粒径约为15 nm。随着热处理温度的提高,ZrO2(3Y)粉体中单斜相的相对含量逐渐增大。Ce02掺杂降低了非晶态ZrO2的晶型转变温度,因而导致单斜相的相对含量增大。(2)研究了Y-TZP的成型制度与烧结性能。研究发现：在干压—冷等静压成型工艺中,相同冷等静压下素胚体积密度随干压压力提高,先降低后增大。可加工指数随预烧结温度提高,先增大后降低。Y-TZP烧成后,进一步提高烧结温度或延长保温时间,可以提高其全透射率。但烧结温度过高时,单斜相的出现及Y3+在晶界处的偏析导致全透射率略有下降,并且显著地降低了力学性能,对致密度的提高没有贡献。综合考虑确定了Y-TZP烧成制度为1470℃/2 h。(3)研究了不同着色方法对Y-TZP力学性能的影响。研究发现：不同着色方法中,共沉淀原位生成法制得的Y-TZP在硬度、断裂韧性及抗弯强度方面均表现良好。较差的成型性能以及机械混合均匀性的局限,导致着色剂与粉体机械混合法中所得Y-TZP的硬度、断裂韧性较低。在浸泡素胚法中,Fe3+强烈水解引起的胶粒团聚,导致Fe203着色Y-TZP的硬度出现明显下降。浸泡粉体法显著降低了Fe203着色Y-TZP的抗弯强度。(4)研究了不同着色方法对Y-TZP透光性、色度的影响。研究发现：Fe203、Ce02掺杂主要降低了Y-TZP在短波段的全透射率。着色剂与粉体机械混合法对Y-TZP全透射率的影响最大,这与该方法中制得Y-TZP致密程度较低、晶粒尺寸分布不均匀有关。共沉淀原位生成法对全透射率的影响最小,所得样品的透射率为四种方法中的最高；Fe203掺杂显著降低了Y-TZP色品指数L*,增大了a*、b8。Ce02掺杂主要增大了b*,对L*、a8影响较小。浸泡素胚法制得的Fe203着色Y-TZP与其他三种着色方法中的相比色差最大,这与Fe3+无法渗透到Y-TZP内部导致其表面Fe203含量较高有关。
[Abstract]:With the improvement of life quality, puts forward higher requirements for dental restorative materials. In the past thirty years, Y-TZP (polycrystalline zirconia, yttria stabilized tetragonal phase oxidation of yttria-stabilized tetragonal zirconia polycrystalline) ceramics with high strength, beautiful appearance and good biocompatibility has been widespread concern in academia and industry for dental restoration, light transmittance and color is the most important performance. However, there is a certain gap between Y-TZP ceramic and natural color. The color in the color shading treatment in traditional decorative layer /Y-TZP double ceramic layer structure to realize color control at the same time, also lost a part of light transmittance and mechanical properties. Therefore since the coloring of Y-TZP all ceramic crown has become the focus of attention. At present, domestic reports about the influence of coloring method on the performance of Y-TZP is few. Using ZrO2 prepared by chemical coprecipitation (3Y) nano powder. Based on the systematic study of the different coloring method on color Y-TZP mechanical properties and effect of color light. Using Fe2O3, CeO2 as colorant, coloring methods include: co precipitation in situ doping, colorant and ZrO2 (3Y) powder mixed coloring solution for ZrO2 (3Y) granulation powder and coloring liquid soak the Y-TZP embryo. Finally the main results are as follows: (1) ZrO2 were prepared by chemical coprecipitation (3Y) nano powder. It is found that the PEG-6000 content is 1.4 wt%, the dispersion of the precursor suspension, after heat treatment of the powder particle size is about 15 nm. with the increase of temperature heat treatment, ZrO2 (3Y) powder in the relative content of monoclinic phase increases.Ce02 doping reduced the crystal amorphous ZrO2 transition temperature, thus leads to the increase of the relative content of monoclinic phase. (2) studied the forming and sintering performance of the Y-TZP system. The study found: in the dry Pressure - cold isostatic pressing, cold isostatic pressing under the same embryo volume density with dry pressure increased, decreased first and then increased. The processability index with pre sintering temperature increase, increased first and then reduced.Y-TZP after firing, to further improve the sintering temperature and holding time can improve the total transmittance. But the sintering when the temperature is too high, the segregation of monoclinic phase and Y3+ in the grain boundary of the transmittance decreased slightly, and significantly reduce the mechanical properties, does not contribute to the increase of density. Considering the determined Y-TZP firing system is 1470 C /2 h. (3) to study the effect of different coloring methods on the mechanical properties of Y-TZP study found that: different coloring method, co precipitation in situ prepared Y-TZP in hardness, bending strength and fracture toughness are good. Poor formability and mechanical mixing limitations, resulting in Y-TZP the colorant and powder mixing method in hardness, fracture toughness is low. In the embryo soaking method, Fe3+ strong hydrolysis caused by particles agglomeration, leading to Fe203 coloring of Y-TZP hardness decreased significantly. Soaking powder method significantly reduced the flexural strength of Fe203 colored Y-TZP. (4) studied coloring method for Y-TZP light transmittance, color effect. The study found: Fe203, Ce02 doped reduced Y-TZP in the short wave transmittance. Effect of colorant and full powder mechanical mixing method for Y-TZP transmission, this method in preparation of Y-TZP dense degree is low, the grain size distribution of the co precipitation method. In situ influence on the transmittance of the minimum transmittance obtained samples was the highest in four ways; Fe203 doping significantly reduced Y-TZP color index L*, increased a*, b8.Ce02 doped b* mainly increased to L*, a8. The influence of the Fe203 coloring Y-TZP produced by soaking embryo embryo is the largest compared with the other three coloring methods, which is related to the fact that Fe3+ can not penetrate into Y-TZP, resulting in higher Fe203 content on the surface.

【学位授予单位】：浙江大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：TQ174.759

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