本文選題：共沉淀　切入點(diǎn)：Y-TZP　出處：《浙江大學(xué)》2015年碩士論文

【摘要】：隨著人們生活質(zhì)量的不斷提高,對(duì)牙科修復(fù)材料提出了更高的要求。近三十年來,Y-TZP(釔穩(wěn)定四方相氧化鋯多晶體,yttria-stabilized tetragonal zirconia polycrystalline)陶瓷因高強(qiáng)度、美觀性及較好的生物相容性得到了學(xué)術(shù)界和產(chǎn)業(yè)界的廣泛關(guān)注。對(duì)于牙科修復(fù)體,透光性和色度是最重要的性能指標(biāo)。然而,Y-TZP陶瓷的顏色與天然牙色存在一定差距。在傳統(tǒng)的遮色處理中,飾面層/Y-TZP雙瓷層結(jié)構(gòu)在實(shí)現(xiàn)色度調(diào)控的同時(shí),也損失了一部分透光性和力學(xué)性能。因而自著色Y-TZP全瓷冠成為了人們關(guān)注的焦點(diǎn)。目前,國內(nèi)關(guān)于著色方法對(duì)Y-TZP性能影響的報(bào)道很少。本文采用化學(xué)共沉淀法制備了ZrO2(3Y)納米粉。并基于此系統(tǒng)地研究了不同著色方法對(duì)著色Y-TZP力學(xué)性能、透光性及色度的影響。選用Fe2O3、CeO2為著色劑,著色方法包括：共沉淀原位生成摻雜、著色劑與ZrO2(3Y)粉體機(jī)械混合、著色液浸泡ZrO2(3Y)造粒粉體和著色液浸泡Y-TZP素胚。最終取得主要結(jié)果如下：(1)采用化學(xué)共沉淀制備了ZrO2(3Y)納米粉。研究發(fā)現(xiàn)：PEG-6000添加量為1.4 wt%時(shí),對(duì)前驅(qū)體懸濁液的分散效果最好,熱處理后的粉體粒徑約為15 nm。隨著熱處理溫度的提高,ZrO2(3Y)粉體中單斜相的相對(duì)含量逐漸增大。Ce02摻雜降低了非晶態(tài)ZrO2的晶型轉(zhuǎn)變溫度,因而導(dǎo)致單斜相的相對(duì)含量增大。(2)研究了Y-TZP的成型制度與燒結(jié)性能。研究發(fā)現(xiàn)：在干壓—冷等靜壓成型工藝中,相同冷等靜壓下素胚體積密度隨干壓壓力提高,先降低后增大�？杉庸ぶ笖�(shù)隨預(yù)燒結(jié)溫度提高,先增大后降低。Y-TZP燒成后,進(jìn)一步提高燒結(jié)溫度或延長(zhǎng)保溫時(shí)間,可以提高其全透射率。但燒結(jié)溫度過高時(shí),單斜相的出現(xiàn)及Y3+在晶界處的偏析導(dǎo)致全透射率略有下降,并且顯著地降低了力學(xué)性能,對(duì)致密度的提高沒有貢獻(xiàn)。綜合考慮確定了Y-TZP燒成制度為1470℃/2 h。(3)研究了不同著色方法對(duì)Y-TZP力學(xué)性能的影響。研究發(fā)現(xiàn)：不同著色方法中,共沉淀原位生成法制得的Y-TZP在硬度、斷裂韌性及抗彎強(qiáng)度方面均表現(xiàn)良好。較差的成型性能以及機(jī)械混合均勻性的局限,導(dǎo)致著色劑與粉體機(jī)械混合法中所得Y-TZP的硬度、斷裂韌性較低。在浸泡素胚法中,Fe3+強(qiáng)烈水解引起的膠粒團(tuán)聚,導(dǎo)致Fe203著色Y-TZP的硬度出現(xiàn)明顯下降。浸泡粉體法顯著降低了Fe203著色Y-TZP的抗彎強(qiáng)度。(4)研究了不同著色方法對(duì)Y-TZP透光性、色度的影響。研究發(fā)現(xiàn)：Fe203、Ce02摻雜主要降低了Y-TZP在短波段的全透射率。著色劑與粉體機(jī)械混合法對(duì)Y-TZP全透射率的影響最大,這與該方法中制得Y-TZP致密程度較低、晶粒尺寸分布不均勻有關(guān)。共沉淀原位生成法對(duì)全透射率的影響最小,所得樣品的透射率為四種方法中的最高；Fe203摻雜顯著降低了Y-TZP色品指數(shù)L*,增大了a*、b8。Ce02摻雜主要增大了b*,對(duì)L*、a8影響較小。浸泡素胚法制得的Fe203著色Y-TZP與其他三種著色方法中的相比色差最大,這與Fe3+無法滲透到Y(jié)-TZP內(nèi)部導(dǎo)致其表面Fe203含量較高有關(guān)。
[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.

【學(xué)位授予單位】：浙江大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2015
【分類號(hào)】：TQ174.759

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