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中华口腔医学研究杂志(电子版) ›› 2016, Vol. 10 ›› Issue (01) : 38 -44. doi: 10.3877/cma.j.issn.1674-1366.2016.01.007

所属专题： 文献；

基础研究

低温时效性对牙科用氧化锆耐磨性能的影响
浩志超1, 刘珂2, 王林霞3, 孟玉坤3,†()   
  1. 1. 510055　广州，中山大学光华口腔医学院·附属口腔医院，广东省口腔医学重点实验室
    2. 272000　济宁医学院附属医院口腔科
    3. 610041　成都，四川大学华西口腔医院，四川大学口腔国家重点实验室
  • 收稿日期:2015-11-22 出版日期:2016-02-01
  • 通信作者: 孟玉坤

Influence of low-temperature degradation and wear cycles on the wear resistance of zirconia

Zhichao Hao1, Ke Liu2, Linxia Wang3, Yukun Meng3,†()   

  1. 1. Guanghua School of Stomatology, Hospital of Stomatology, Sun Yat-sen University, Guangdong Provincial Key Laboratory of Stomotology, Guangzhou 510055, China
    2. First Affiliated Hospital of Jining Medical University, Jining 272000, China
    3. State Key Laboratory of oral diseases, Hospital of West China Hospital of Stomatology, Sichuan University, Chengdu 610041, China
  • Received:2015-11-22 Published:2016-02-01
  • Corresponding author: Yukun Meng
  • About author:
    Corresponding author: Meng Yukun, Email:
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浩志超, 刘珂, 王林霞, 孟玉坤. 低温时效性对牙科用氧化锆耐磨性能的影响[J]. 中华口腔医学研究杂志(电子版), 2016, 10(01): 38-44.

Zhichao Hao, Ke Liu, Linxia Wang, Yukun Meng. Influence of low-temperature degradation and wear cycles on the wear resistance of zirconia[J]. Chinese Journal of Stomatological Research(Electronic Edition), 2016, 10(01): 38-44.

目的

探讨低温时效对牙科用氧化锆耐磨性能的影响。

方法

本实验对偶球为对照氧化锆球和经低温时效处理的氧化锆球（134℃，100 h），对磨材料为牙釉质（n= 8），每个氧化锆对偶球（n= 8）对应1个牙釉质样本。将样本和对偶球固定在磨耗试验仪上，磨耗实验条件：10 000、20 000和50 000个磨耗循环，频率1.2 Hz，载荷49 N。随后用三维轮廓扫描仪确定每组牙釉质样本磨痕的体积损失和深度损失，并测定磨耗前后氧化锆球表面的粗糙度。用微压痕实验方法检测氧化锆球的维氏硬度。应用SPSS 20.0软件包对实验数据进行统计学分析，采用双因素方差分别分析牙釉质样本的深度损失（μm）和体积损失（mm3 × 10-3）以及氧化锆对偶球的粗糙度（μm），采用单因素方差分析氧化锆对偶球硬度结果，选择Tukey HSD检验进行组间两两比较。

结果

实验结果显示，10 000次磨耗循环后低温时效处理组和对照组牙釉质样本的深度损失（1.43 ± 0.07，1.46 ± 0.12）和体积损失（2.36 ± 0.45，2.31 ± 0.34）差异无统计学意义（F深度损失= 0.721，P深度损失= 0.610；F体积损失= 0.0552，P体积损失=0.801）；而经过20 000和50 000次磨耗循环后老化处理组对磨的牙釉质样本深度损失（F20 000= 4.573，P20 000= 0.0364；F50 000= 49.385，P50 000<0.001）和体积损失（F20 000= 5.769，P20 000= 0.0210；F50 000= 61.792，P50 000<0.001）显著低于对偶球为对照组氧化锆球组。10 000和20 000次磨耗后低温时效组的氧化锆球的表面粗糙度（0.0402 ± 0.0055，0.0366 ± 0.0061）与对照组（0.0406 ± 0.0035，0.0391 ± 0.0059）差异均无统计学意义（F10 000= 0.0314，P10 000= 0.873；F20 000= 0.693，P20 000= 0.416），而磨耗50 000次后老化处理组氧化锆球的粗糙度（0.0596 ± 0.0045）显著高于于对照组氧化锆球（0.0386 ± 0.0027），差异有统计学意义（F50 000= 128.793，P<0.001）。低温时效处理组氧化锆的维氏硬度为1257.0 ± 54.5（HV1）显著低于对照组氧化锆球1385.8 ± 28.7（HV1，F= 124.789，P<0.001）。

结论

低温时效处理导致牙科用氧化锆材料硬度降低，耐磨性能下降（20 000和50 000次磨耗循环后）。

关键词: 氧化锆, 低温时效, 磨耗循环, 耐磨性能
Objective

The purpose of this study is to evaluate the influence of low temperature degradation on the wear behavior of zirconia.

Methods

Zirconia balls with and without autoclaving (134℃, 100 h) were used as the antagonist material in this study. Eight specimens of human enamel for each group were tested. For each enamel sample, a zirconia ball was used as the antagonist (n= 8) . The specimens and antagonist balls were subjected to a wear simulator (10 000, 20 000 and 50 000 loading cycles, 1.2 Hz, 49 N) and then the vertical loss and volume loss were measured by a three-dimensional (3D) optical profilometer. Roughness of zirconia balls was measured by the 3D optical profilometer as well. Hardness of the samples was determined using a micro-Vickers hardness tester. The software of SPSS 20.0 was used for statistical analysis. Two-Way ANOVA was performed to analyze the data of vertical loss (μm) and volume loss (mm3 × 10-3) for enamel samples and roughness (μm) of the zirconia balls and data of Vickers hardness were analyzed using One-Way ANOVA. Multiple pair-wise comparison of means was performed with Tukey′s Honestly Significant Difference (HSD) post hoc test (α= 0.05) .

Results

Results showed that human enamel samples opposing the non-aged zirconia balls demonstrated significantly less vertical loss (F20 000= 4.573, P20 000= 0.0364; F50 000= 49.385, P50 000<0.001) and volume loss (F20 000= 5.769, P20 000= 0.0210; F50 000= 61.792, P50 000<0.001) than those against the aged zirconia balls after 20 000 and 50 000 wear test cycles. No significant differences were observed after 10 000 wear test cycles for vertical loss (1.43 ± 0.07, 1.46 ± 0.12) and volume loss (2.36 ± 0.45, 2.31 ± 0.34; Fvertical loss= 0.721, Pvertical loss= 0.610; Fvolume loss= 0.0552, Pvolume loss= 0.801) . No significant differences were found for the roughness among the aged (0.0402 ± 0.0055, 0.0366 ± 0.0061) and non-aged zirconia balls (0.0402 ± 0.0055, 0.0366 ± 0.0061) after 10 000 and 20 000 were test cycles (F10 000= 0.0314, P10 000= 0.873; F20 000= 0.693, P20 000= 0.416) . However, after 50 000 chewing cycles aged zirconia balls (0.0596 ± 0.0045) showed significantly greater roughness than the non-aged ones (0.0386 ± 0.0027; F50 000= 128.793, P<0.001) . Vickers hardness for the aged zirconia balls 1257.0 ± 54.5 (HV1) was significantly lower than for the non-aged group 1385.8 ± 28.7 (HV1, F= 124.789, P<0.001) .

Conclusions

Low temperature degradation results in significant decrease in Vickers hardness for zirconia balls. Aged zirconia balls demonstrate less wear resistance after 20 000 and 50 000 chewing cycles compared to the non-aged zirconia ones.

Key words: Zirconium oxide, Low temperature degradation, Wear cycle, Wear resistance
表1 不同磨耗循环次数后对磨牙釉质样本的深度损失和体积损失（±s）
磨耗次数 样本数 （个） 深度损失（μm） 体积损失(mm3 × 10-3)
对照组 老化处理组 对照组 老化处理组
10 000 48 1.46 ± 0.12 1.43 ± 0.07 2.31 ± 0.34 2.36 ± 0.45
20 000 48 2.30 ± 0.27 2.08 ± 0.17 4.26 ± 0.44 3.34 ± 0.70
50 000 48 4.01 ± 0.39 3.19 ± 0.17 8.63 ± 0.97 5.74 ± 1.13
图1 磨耗后牙釉质样本的表面形貌
图2 扫描电镜观察磨耗实验后氧化锆球表面的形貌
图3 磨耗后氧化锆球表面粗糙度
图4 氧化锆球维氏硬度测量结果（× 40）
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