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某些化学表面改性对树脂与氧化锆粘结的影响。

Effects of some chemical surface modifications on resin zirconia adhesion.

作者信息

Liu Dan, Tsoi James Kit-Hon, Matinlinna Jukka Pekka, Wong Hai Ming

机构信息

Dental Materials Science, Faculty of Dentistry, University of Hong Kong, Hong Kong SAR, PR China.

Paediatric Dentistry, Faculty of Dentistry, University of Hong Kong, Hong Kong SAR, PR China.

出版信息

J Mech Behav Biomed Mater. 2015 Jun;46:23-30. doi: 10.1016/j.jmbbm.2015.02.015. Epub 2015 Feb 26.

Abstract

OBJECTIVES

To evaluate the effects of various chemical surface modifications on adhesion between zirconia and resin adhesive.

MATERIAL AND METHODS

Pre-sintered zirconia discs were sectioned from commercial cylindrical blocks and polished with abrasive papers under running tap water. All the discs were randomly divided into five study groups according to the methods of surface treatment, including: the control group (fully sintered, without any modification), group S (fully sintered and sandblasted with silica coated alumina particles), group HN (fully sintered and etched with a blend of mineral acid solution at 100 °C for 25 min), group HF (fully sintered and etched with 48% hydrofluoric acid solution at 100 °C for 25 min), and group Si (coated with silica particles and then fully sintered). The mean value of surface roughness was evaluated before further treatment. Resin stubs (3.6mm in diameter and 3mm in height) were adhered and light cured on each zirconia disc after the application of a silane coupling agent. In each group, all the samples were further divided into three subgroups with each n=12, one for the measurement of initial adhesion strength (shear bond) value and the other two were tested after thermal cycling for 10,000 and 20,000 cycles, respectively. The results were analyzed with two-way ANOVA and Turkey HSD (p<0.05). XRD technique was utilized in the examination of zirconia surface crystallinity. The morphological appearance of zirconia surface after surface treatment was observed with SEM.

RESULTS

The control group showed the lowest initial shear bond strength (SBS) value (16.8 ± 2.4 MPa) and did not survive the aging treatments. All the investigated surface treatments improved resin zirconia bond strength significantly, the group S displaying the highest initial value of 25.1 ± 2.7 MPa. However, the highest resistance to the aging effects of thermal cycling was found in group Si. It was further shown in the XRD examination that only the grit-blasting caused the crystalline transformation from tetragonal phase to monoclinic phase (T → M). On the other hand, such a phase transformation could not be detected in all the other four groups.

SIGNIFICANCE

Resin zirconia adhesion could be effectively improved by both HF etching and silica coating on zirconia surface, without leading to a T → M crystalline phase transformation.

摘要

目的

评估各种化学表面改性对氧化锆与树脂黏结剂之间黏附力的影响。

材料与方法

从市售圆柱形块体上切下预烧结的氧化锆圆盘,并在流水下用砂纸进行抛光。根据表面处理方法,将所有圆盘随机分为五个研究组,包括:对照组(完全烧结,未作任何改性)、S组(完全烧结并用涂覆二氧化硅的氧化铝颗粒喷砂处理)、HN组(完全烧结并用混合无机酸溶液在100℃蚀刻25分钟)、HF组(完全烧结并用48%氢氟酸溶液在100℃蚀刻25分钟)和Si组(涂覆二氧化硅颗粒然后完全烧结)。在进一步处理之前评估表面粗糙度的平均值。在施加硅烷偶联剂后,将树脂短柱(直径3.6mm,高3mm)黏附在每个氧化锆圆盘上并光固化。在每组中,所有样本进一步分为三个亚组,每组n = 12,一个用于测量初始黏附强度(剪切黏结)值,另外两个分别在进行10000次和20000次热循环后进行测试。结果采用双向方差分析和Turkey HSD检验(p < 0.05)。利用XRD技术检测氧化锆表面结晶度。用扫描电子显微镜观察表面处理后氧化锆表面的形态外观。

结果

对照组显示出最低的初始剪切黏结强度(SBS)值(16.8±2.4MPa),并且在老化处理后未能留存。所有研究的表面处理均显著提高了树脂与氧化锆的黏结强度,S组显示出最高的初始值25.1±2.7MPa。然而,Si组对热循环老化效应的抗性最高。XRD检测进一步表明,只有喷砂处理导致了从四方相到单斜相的晶体转变(T→M)。另一方面,在其他四组中均未检测到这种相变。

意义

通过对氧化锆表面进行HF蚀刻和二氧化硅涂覆,可有效提高树脂与氧化锆的黏附力,且不会导致T→M晶体相变。

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