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[不同表面改性对氧化锆陶瓷微观结构和附着力的影响:一项体外研究]

[Effects of different surface modifications on micro-structure and adhesion of zirconia ceramic: an in vitro study].

作者信息

Siwen Li, Shishi Li, Yanhong Wang, Hongmei Ma

机构信息

Dept. of General Dentistry, Hospital of Stomatology, China Medical University, Shenyang 110000, China.

出版信息

Hua Xi Kou Qiang Yi Xue Za Zhi. 2017 Feb 1;35(1):43-50. doi: 10.7518/hxkq.2017.01.006.

Abstract

OBJECTIVE

This study evaluated the effect of different mechanical-chemical surface treatments on the characteristics, microstructure, and composition of zirconia ceramics and on the zirconia-dentin adhesion.

METHODS

The sintered commercial zirconia blocks (IPS e.max ZirCAD) were sectioned into 126 beams (6 mm×6 mm×5 mm) and randomly assigned to seven experimental groups (n=18). The zirconia block specimens were further treated as follows: (A) untreated, as control; (B) sandblasted with 50 μm Al2O3; (C) sandblasted with 50 μm Al2O3+30 μm silica powder; (D) sandblasted with 50 μm Al2O3+30% silica-sol coating; (E) sandblasted with 110 μm Al2O3; (F) sandblasted with 110 μm Al2O3+30 μm silica powder; and (G) sandblasted with 110 μm Al2O3+30% silica-sol coating. The surface roughness (Ra) of zirconia ceramics using X-ray diffraction (XRD), field emission scanning electron microscopy (SEM), and energy dispersive X-ray spectroscopy (EDX) after seven surface treatments was analyzed. Seventy specimens of dentin surfaces were prepared. A dual-cure resin cement was applied into zirconia surfaces with its corresponding adhesive components to dentin. Shear bond strength (SBS) of each sample was measured using a universal testing machine. The data were analyzed by ANOVA using SPSS 17.0 software.

RESULTS

Ra of zirconia were significantly different compared with the control group (P<0.05). The crystalline transformation from tetragonal phase to monoclinic phase was observed after surface modification. Monoclinic volume content of the heat-treated group was highest than that in other groups. The content of element Si in the heat-treated group was higher than that in other treatment groups accompanied by a decrease in elements Zr, Y, and Hf after being treated by two silica-coating methods. Air abrasion significantly increased the micro-cracks in the ceramic surface and caused the grain boundaries to disappear. A serious shrinkage of the thin silica film can be observed after sintering procedure. This process induced cracks and the film to strip away slightly from the surfaces of Y-TZP substrate. The SBS values from large to small were F and G groups, C and D groups, B and E groups (P<0.05), and control group (P<0.05).

CONCLUSIONS: Alumina sandblasting, silica powder abrasion, and silica-sol coating affect the surface morphology, structure, and composition of the tooth. This effect can also achieve the improved micro-mechanical interlocking or chemical bonding and finally increase the bond strength between zirconia and tooth. Alumina sandblasting followed by silica coating is an effective technique to increase the bonding strength between the zirconia ceramic and dentin.
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摘要

目的

本研究评估了不同机械 - 化学表面处理对氧化锆陶瓷的特性、微观结构、组成以及氧化锆与牙本质黏附力的影响。

方法

将烧结后的商用氧化锆块(IPS e.max ZirCAD)切割成126根梁(6毫米×6毫米×5毫米),并随机分为七个实验组(n = 18)。氧化锆块标本进一步处理如下:(A)未处理,作为对照组;(B)用50μm Al₂O₃喷砂;(C)用50μm Al₂O₃ + 30μm二氧化硅粉末喷砂;(D)用50μm Al₂O₃ + 30%硅溶胶涂层喷砂;(E)用110μm Al₂O₃喷砂;(F)用110μm Al₂O₃ + 30μm二氧化硅粉末喷砂;(G)用110μm Al₂O₃ + 30%硅溶胶涂层喷砂。分析了七种表面处理后氧化锆陶瓷的表面粗糙度(Ra),采用X射线衍射(XRD)、场发射扫描电子显微镜(SEM)和能量色散X射线光谱(EDX)进行分析。制备了70个牙本质表面标本。将双固化树脂水门汀应用于氧化锆表面,并将其相应的黏附成分应用于牙本质。使用万能试验机测量每个样品的剪切粘结强度(SBS)。数据使用SPSS 17.0软件通过方差分析进行分析。

结果

与对照组相比,氧化锆的Ra有显著差异(P < 0.05)。表面改性后观察到从四方相到单斜相的晶体转变。热处理组的单斜相体积含量高于其他组。经过两种硅涂层方法处理后,热处理组中元素Si的含量高于其他处理组,同时元素Zr、Y和Hf的含量降低。空气研磨显著增加了陶瓷表面的微裂纹并导致晶界消失。烧结过程后可观察到薄硅膜严重收缩。这个过程导致裂纹,并且薄膜从Y - TZP基体表面略微剥离。SBS值从大到小依次为F组和G组、C组和D组、B组和E组(P < 0.05)以及对照组(P < 0.05)。

结论

氧化铝喷砂、二氧化硅粉末研磨和硅溶胶涂层会影响牙齿的表面形态、结构和组成。这种影响还可以实现改善微机械互锁或化学键合,最终增加氧化锆与牙齿之间的粘结强度。氧化铝喷砂后进行硅涂层是提高氧化锆陶瓷与牙本质之间粘结强度的有效技术。

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