本文選題：釔穩(wěn)定氧化鋯 + 顏色　； 參考：《中國人民解放軍醫(yī)學(xué)院》2014年博士論文

【摘要】：釔穩(wěn)定氧化鋯陶瓷（Y-TZP）在室溫條件下，通過應(yīng)力作用可以發(fā)生馬氏體相變因而具有較佳的力學(xué)特性，其優(yōu)良的生物安全性、耐磨性能和抗腐蝕性能，使Y-TZP成為理想的牙科陶瓷材料，Y-TZP與其它牙科陶瓷材料相比較，具有理想的機械力學(xué)性能。目前未著色Y-TZP呈現(xiàn)出白色或象牙色，半透明性較差，雖然可以模擬天然牙顏色，，但在臨床上并不能滿足口腔醫(yī)生和患者對修復(fù)體美觀性能的要求，Y-TZP的表面常常需要遮色，這會讓材料近一步降低其半透明性，然而如果Y-TZP顏色被調(diào)整到與擬修復(fù)牙齒相接近，這將會讓牙齒配比顏色的過程變得簡單，同時改善Y-TZP的半透明性，將獲得良好的質(zhì)感。Y-TZP著色一般通過兩種方法，一是外著色，將初燒結(jié)Y-TZP塊浸入染色液中浸泡，然后燒結(jié)；另一種方法是內(nèi)著色，在Y-TZP粉體中添加著色劑。將Y-TZP塊放入染色液中浸泡的外著色方法操作簡單，但容易發(fā)生Y-TZP塊著色不均勻，著色結(jié)果受操作影響大，同時不能將同樣的操作程序應(yīng)用于其它品牌。在生產(chǎn)過程中，將著色氧化物加入Y-TZP粉體中的內(nèi)著色方法，可以使Y-TZP塊著色后，顏色準(zhǔn)確均一，并且對Y-TZP半透明性影響較小，目前Y-TZP內(nèi)著色是一種較理想的Y-TZP顏色解決方案。Y-TZP底層材料盡管具有優(yōu)良的機械力學(xué)性能，但是其半透明性能較差。在齒科常用陶瓷中氧化鋯晶體的折射率較高，光的散射大，可見光透射率較低，無法滿足修復(fù)體特別是前牙區(qū)修復(fù)的美學(xué)要求。如果使用Y-TZP制作的基底冠的顏色和半透明性可以與牙體組織的顏色相匹配，那么齒科技師在修復(fù)體制作過程中通過降低飾面瓷的厚度，減少備牙量，最終可以讓修復(fù)體達(dá)到預(yù)期的美學(xué)效果。本論文采用添加著色氧化物粉體的方式對Y-TZP進行內(nèi)著色，試制出了顏色與VITA-3D Master比色板相近的內(nèi)著色Y-TZP修復(fù)體材料，并對其粉體加工工藝、微觀結(jié)構(gòu)和材料光學(xué)性能進行了研究。本研究的主要目的是選取適合的著色氧化物對Y-TZP粉體進行內(nèi)著色，系統(tǒng)研究加工工藝和著色劑對Y-TZP最終顏色和半透明性的影響，Y-TZP顏色參考VITA-3D Master比色板，對顏色進行測定，以期獲得臨床上符合前牙美學(xué)要求的Y-TZP材料。結(jié)果如下： 1.本實驗分析了影響Y-TZP漿料性質(zhì)的漿料固含量、PVA加入量、球磨時間三個因素，分析得出漿料固含量對漿料的流變性具有顯著的影響，PVA加入量、球磨時間長度對Y-TZP漿料的平均粘度和沉降度均沒有顯著的影響。 2.噴霧造粒漿料的粘度和沉降度都是不可忽視的要素，要便于大規(guī)模工業(yè)化的生產(chǎn)需求，漿料的固含量為50wt%。根據(jù)正交試驗結(jié)果以及生產(chǎn)工藝驗證試驗，確定PVA的加入量為3wt%。本實驗主要目的是要試制著色均勻的并有一定半透明性的Y-TZP齒科用修復(fù)材料。根據(jù)工業(yè)化生產(chǎn)經(jīng)驗及生產(chǎn)工藝驗證，確定球磨時間長度為24h。本實驗分析得到的最好噴霧造粒漿料的方案為A3B3C3，即固相含量為50wt%；PVA加入量為3wt%；球磨時間長度為24h。通過工藝驗證，造粒后得到的粉體顆粒大多成球形，邊緣較圓滑，粉體內(nèi)無氣泡、球體幾乎無破碎。 3.未著色Y-TZP、0.15wt%Fe2O3著色Y-TZP、4wt%CeO2著色Y-TZP的造粒粉體顆粒大致分布在40-120μm之間。同時顆粒分布較窄，60-90μm左右的粉體顆粒較多。造粒后的粉體顆粒粒度不是完全一致，有一定的尺寸級配。Fe2O3作為著色劑進行內(nèi)著色對顆粒的粒徑產(chǎn)生一定的影響，D50比未著色的Y-TZP要大，但影響不明顯。 4. Fe2O3、CeO2作為Y-TZP的內(nèi)著色劑，對造粒粉體的流動性、成球性能和預(yù)燒結(jié)體的密度影響不大。 5.0.15wt%Fe2O3著色Y-TZP、4wt%CeO2著色Y-TZP終燒結(jié)后，晶相主要為四方相ZrO2，XRD的衍射峰中均未出現(xiàn)Fe2O3、CeO2峰。0.15wt%Fe2O3著色Y-TZP、4wt%CeO2著色Y-TZP終燒結(jié)后，著色Y-TZP燒結(jié)致密，晶粒大小均勻，晶粒尺寸約為0.5-0.7μm。著色Y-TZP的斷裂方式為穿晶斷裂和沿晶斷裂。 6. Fe2O3添加量的增加，Y-TZP的明度值從84下降到75左右，明度值逐漸下降。伴隨著明度的下降，a*、b*色調(diào)值同時增大，b*值的增幅比a*值大。b*值從10.76增加到23.65。當(dāng)Fe2O3添加量超過0.06wt%后，a*、b*值都有較明顯的增加。Fe2O3對a*值的影響不是很大，對b*值影響較大。隨著CeO2含量的增加，著色Y-TZP的b*增加，但幅度較小，著色作用比較弱。a*值隨著CeO2含量的增加而稍有降低，總體波動范圍不大。CeO2含量的變化對著色Y-TZP的明度影響較小。 7.未著色Y-TZP和著色Y-TZP的可見光透射率具有波長依賴性，在400-700nm可見光區(qū)域內(nèi)，透射率單調(diào)一致，隨波長的增加，透射率也增加。未著色Y-TZP的透射率曲線幾乎為一條直線，可見光透射率明顯高于著色Y-TZP。 8.未著色Y-TZP組和0.03wt%Fe2O3著色Y-TZP組之間有統(tǒng)計學(xué)差異（P＜0.05），0.03wt%Fe2O3著色Y-TZP組和0.15wt%Fe2O3著色Y-TZP組之間有統(tǒng)計學(xué)差異（P＜0.05），未著色Y-TZP組和0.15wt%Fe2O3著色Y-TZP組之間有統(tǒng)計學(xué)差異（P＜0.05）�？梢姽馔干渎�，未著色Y-TZP＞0.03wt%Fe2O3著色Y-TZP＞0.15wt%Fe2O3著色Y-TZP。 9.未著色Y-TZP組和1wt%CeO2著色Y-TZP組之間有統(tǒng)計學(xué)差異（P＜0.05），1wt%CeO2著色Y-TZP組和4wt%CeO2著色Y-TZP組之間有統(tǒng)計學(xué)差異（P＜0.05），未著色Y-TZP組和4wt%CeO2著色Y-TZP組之間有統(tǒng)計學(xué)差異（P＜0.05）�？梢姽馔干渎�，未著色Y-TZP＞1wt%CeO2著色Y-TZP＞4wt%CeO2著色Y-TZP。
[Abstract]:Yttrium stabilized zirconia ceramics (Y-TZP) can have better mechanical properties at room temperature by stress action and thus has better mechanical properties. Its excellent biological safety, wear resistance and corrosion resistance make Y-TZP an ideal dental ceramic. Compared with its dental ceramics, Y-TZP has ideal mechanical mechanics. Performance. The current uncolored Y-TZP presents white or ivory color and is less translucent. Although it can simulate natural tooth color, it does not meet the clinical requirements of the dentist and patient on the aesthetic performance of the prosthesis. The surface of the Y-TZP often requires shade, which will reduce the translucency of the material in a near step, however, if the Y-TZP color is colored The adjustment to the proposed restoration of the teeth will make the process of the color matching of the teeth simpler and improve the translucency of the Y-TZP, and the good texture of the.Y-TZP will be obtained by two methods, one is the external coloring, the initial sinter Y-TZP is soaked in the dyeing solution and then sintered; the other is the internal coloring, in the Y-TZP powder. A coloring agent is added to the body. The external coloring method to immerse the Y-TZP block into the dye is simple, but it is easy to have the uneven coloring of the Y-TZP block, the coloring result is influenced greatly by the operation, and the same operating procedure can not be applied to other brands. In the process of production, the coloring of the colored oxygenate into the Y-TZP powder can be used in the production process. After coloring the Y-TZP block, the color is accurate and uniform, and it has little effect on the translucency of Y-TZP. At present, Y-TZP interior coloring is an ideal Y-TZP color solution,.Y-TZP bottom material, although it has excellent mechanical and mechanical properties, but its translucent performance is poor. If the color and translucency of the base crown made with Y-TZP can match the color of the tooth tissue, the dental technician can reduce the thickness of the veneer porcelain and reduce the amount of tooth preparation in the process of making the prosthesis. The restorative body has achieved the desired aesthetic effect. In this paper, the interior coloring of Y-TZP was made by adding coloring oxide powder, and the interior coloring Y-TZP restorer materials with similar color and VITA-3D Master were produced. The processing technology, microstructure and optical properties of the powder were studied. The main purpose of this study was to study the main purpose of this study. The suitable coloring oxide was selected for internal coloring of Y-TZP powder. The effects of processing technology and colorant on the final color and translucency of Y-TZP were systematically studied. Y-TZP color reference VITA-3D Master was used to determine the color in order to obtain the Y-TZP material which was clinically suitable for the anterior tooth aesthetics. The results were as follows:
1. the experiment analyzed the slurry solid content of the Y-TZP slurry, the amount of PVA and the ball milling time three factors. It was found that the solid content of the slurry had a significant influence on the rheological property of the slurry. The amount of PVA and the length of the ball milling time had no significant influence on the average viscosity and the settlement degree of the Y-TZP slurry.
2. the viscosity and the settlement degree of the spray granulation slurry are all factors which can not be ignored. To facilitate the production demand of large-scale industrialization, the solid content of the slurry is 50wt%. based on the orthogonal test results and the production process verification test. The main purpose of the experiment is to determine the PVA's addition of 3wt%.. The main purpose of this experiment is to try to make a homogeneous and translucent Y with a uniform color. -TZP dental repair materials. According to the industrial production experience and production process verification, the best spray granulation slurry obtained by the ball milling time length is 24h., which is A3B3C3, that is, the solid content is 50wt%, the PVA addition is 3wt%, the ball milling time is 24h. through process verification, and the particle size is large after granulation. It is more spherical, with smooth edges and no bubbles in the powder, and the ball almost has no breakage.
3. uncoloured Y-TZP, 0.15wt%Fe2O3 coloring Y-TZP, and 4wt%CeO2 colored Y-TZP granulation particles are roughly distributed between 40-120 mu m. The particle distribution is narrower and the particle size is more than 60-90 mu m. The particle size of the powder after granulation is not exactly the same, and a certain size graded.Fe2O3 is used as the colorant for inner coloring particles. The diameter has a certain effect. D50 is larger than unstained Y-TZP, but the effect is not obvious.
4. Fe2O3, CeO2 as the internal colorant of Y-TZP, has little effect on the fluidity, pelletizing property and density of pre sintered powders.
After the 5.0.15wt%Fe2O3 coloring Y-TZP and the final sintering of 4wt%CeO2 coloring Y-TZP, the crystal phase is mainly ZrO2 of the Quartet phase, and there is no Fe2O3 in the diffraction peak of XRD, CeO2 peak.0.15wt%Fe2O3 coloring Y-TZP, 4wt%CeO2 coloring Y-TZP after sintering, the coloring is compact and the grain size is uniform, and the fracture mode of grain size inch is about the transgranular fracture. Crack and intergranular fracture.
6. Fe2O3 added, the brightness value of Y-TZP decreased from 84 to about 75, and the brightness value decreased gradually. With the decrease of brightness, a*, b* hue value increased at the same time, the b* value increased from 10.76 to 23.65. when the Fe2O3 added more than 0.06wt%, a*, b* values had a significant increase in the value. With the increase of CeO2 content, the b* of coloring Y-TZP increases with the increase of the content of Y-TZP, but the amplitude is smaller, and the weaker.A* value decreases slightly with the increase of CeO2 content, and the variation of the overall fluctuation range is less.CeO2 content than the brightness of the color Y-TZP.
7. the visible light transmittance of uncoloured Y-TZP and coloring Y-TZP has wavelength dependence. In the 400-700nm visible region, the transmittance is monotonous and the transmittance increases with the increase of wavelength. The transmittance curve of the uncoloured Y-TZP is almost a straight line, and the visible light transmittance is obviously higher than that of the coloring Y-TZP..
There was a statistical difference between the 8. unstained Y-TZP group and the 0.03wt%Fe2O3 colored Y-TZP group (P < 0.05). There was a statistical difference between the 0.03wt%Fe2O3 colored Y-TZP group and the 0.15wt%Fe2O3 coloring Y-TZP group (P < 0.05). There was a statistical difference between the non coloured Y-TZP group and the 0.15wt%Fe2O3 pigmented Y-TZP group (0.05). 2O3 coloring Y-TZP > 0.15wt%Fe2O3 coloring Y-TZP.
There were statistical differences between the 9. unstained Y-TZP group and the 1wt%CeO2 colored Y-TZP group (P < 0.05). There was a statistical difference between the 1wt%CeO2 colored Y-TZP group and the 4wt%CeO2 coloring Y-TZP group (P < 0.05). There was a statistical difference between the non coloured Y-TZP group and the 4wt%CeO2 pigmented Y-TZP group (0.05). %CeO2 coloring Y-TZP.
【學(xué)位授予單位】：中國人民解放軍醫(yī)學(xué)院
【學(xué)位級別】：博士
【學(xué)位授予年份】：2014
【分類號】：R783.1

【參考文獻(xiàn)】

相關(guān)期刊論文 前2條

1 高燕;張富強;黃慧;歸林華;;仿牙色四方多晶氧化鋯陶瓷的制備及色度學(xué)分析[J];上�？谇会t(yī)學(xué);2010年04期

2 張金棟,施劍林;氧化鋁粉料的顆粒級配對成型行為和燒結(jié)行為的影響[J];無機材料學(xué)報;1997年02期

本文編號：1924179