北京大学学报(医学版) ›› 2018, Vol. 50 ›› Issue (1): 49-52. doi: 10.3969/j.issn.1671-167X.2018.01.008

• 论著 • 上一篇    下一篇

不同表面处理对氧化锆晶相结构及性能的影响

焦洋1, 王继德2, 邓久鹏2△   

  1. (1. 北京大学第一医院口腔科, 北京100034; 2. 华北理工大学口腔医学院修复科, 河北唐山063000)
  • 出版日期:2018-02-18 发布日期:2018-02-18
  • 通讯作者: 邓久鹏 E-mail:jiupeng00261@sina.com

Effect of different surface treatments on the crystal structure and properties of zirconia

JIAO Yang1, WANG Ji-de2, DENG Jiu-peng2△   

  1. (1. Department of Stomatology,Peking University First Hospital, Beijing 100034, China; 2. Department of Prosthodontics,College of Stomatology,North China University of Science and Technology, Tangshan 063000, Hebei, China)
  • Online:2018-02-18 Published:2018-02-18
  • Contact: DENG Jiu-peng E-mail:jiupeng00261@sina.com

摘要: 目的:研究3种不同表面处理方式对氧化锆晶相转变、表面粗糙度、抗剪切及抗折强度的影响。方法:制作氧化锆试件并随机分为4组:(1)空白对照组,试件表面不做任何处理;(2)氧化铝喷砂组,用110 μm氧化铝颗粒距离10 mm垂直喷砂21 s, 气压0.25 MPa; (3)激光蚀刻组,试件表面均匀涂布石墨粉,以2 W(200 mJ/10 Hz)铒:钇铝石榴石 (Er:Yttrium Aluminum Garnet,Er:YAG)激光均匀辐照试件表面30 s;(4)热酸蚀组,将试件置于1 ∶1混合的40%(质量分数)硝酸与68%(质量分数)氢氟酸蚀液密闭反应釜中,100 ℃水浴锅中反应30 min。检测不同表面处理后氧化锆晶相结构、表面粗糙度、抗剪切及抗折强度的改变,所得数据运用SPSS 20.0统计软件进行统计分析。结果:X射线衍射仪图谱(Xray diffractometer,XRD)显示4组试件表面单斜相晶型的体积百分数分别为0.91%、12.50%、6.64%、17.81%,经过3种表面处理后,氧化锆表面发生了程度不等的四方相向单斜相的转变。表面粗糙度:空白对照组(0.29±0.01) μm,氧化铝喷砂组(1.05±0.11) μm,激光蚀刻组(0.73±0.04) μm,热酸蚀组(1.31±0.06) μm,各组间两两比较差异有统计学意义(P<0.05)。剪切强度:空白对照组(7.09±0.46) MPa,氧化铝喷砂组(12.14±1.51) MPa,激光蚀刻组(8.82±0.74) MPa,热酸蚀组(11.97±0.99) MPa,氧化铝喷砂组与热酸蚀组比较差异无统计学意义(P>0.05),其余两两比较差异有统计学意义(P<0.05)。三点弯曲强度:空白对照组(933.70±44.13) MPa,氧化铝喷砂组(850.95±60.66) MPa,激光蚀刻组(771.53±68.08) MPa,热酸蚀组(766.27±57.49) MPa,激光蚀刻组与热酸蚀组比较差异无统计学意义(P>0.05), 其余两两比较差异有统计学意义(P<0.05)。结论:经过不同表面处理后,氧化锆表面发生了程度不等的四方相向单斜相的转变。3种处理工艺均有效提高了氧化锆与树脂水门汀的粘结强度,同时也会导致氧化锆抗折强度的降低。

关键词:  氧化锆, 喷砂, 热酸蚀

Abstract: Objective:To investigate the effects of 3 surface different treatments on the crystal structure, shear bond strength,roughness value and flexural strength of zirconia. Methods: The zirconia spe-cimens were prepared and randomly divided into 4 groups and received the following treatments: (1)blank control group,the specimens without treatments; (2)sandblasting with alumina group, sandblasting the specimens with 110 μm alumina particles for 21 s as working pressure 0.25 MPa and working distance 10 mm; (3)laser etching group, coating the surface of the specimens with graphite powder and using Er:Yttrium Aluminum Garnet (Er:YAG) laser to irradiate the surface 30 s; (4) hot-etching group, putting the specimens in a closed reactor within a 1 ∶1 mixture of 40%(mass traction) nitric acid and 68%(mass traction) hydrofluoric acid liquid, the reaction of 30 min in a water bath at 100 degrees centigrade. The changes of crystal structure, shear bond strength(SBS) and flexural strength of zirconia after different surface treatments were tested. Results: The X-ray diffractometer(XRD) patterns showed that the volume percentage of monoclinic phase of the 4 groups was 0.91%, 12.50%, 6.64% and 17.81% respectively. The roughness value for the four groups  were as follows: blank control group,(0.29±0.01) μm; sandblasting with alumina group, (1.05±0.11) μm; laser etching group, (0.73±0.04) μm; hot-etching group, (1.31±0.06) μm, respectively(P<0.05). Mean SBS was (7.09±0.46) MPa in blank control group, (12.14±1.51) MPa in sandblasting with alumina group, (8.82±0.74) MPa in laser etching group and (11.97±0.99) MPa in hot-etching group. There was no statistically significant difference between sandblasting with alumina group and hot-etching group (P>0.05), but the difference between the other groups were statistically significant(P<0.05). Mean three-point bending was (933.70±44.13) MPa in blank control group, (850.95±60.66) MPa in sandblasting with alumina group, (771.53±68.08) MPa in laser etching group and (766.27±57.49) MPa in hot-etching group. There was no statistically significant difference between sandblasting with alumina group and hot-etching group (P>0.05), but the difference between the other groups were statistically significant(P<0.05). Conclusion: After different surface treatments, the surface of zirconia has changed from tetrago-nal to monoclinic phases in varying degrees. In addition, surface treatments could improve the bond strength of zirconia to resin cement, and also lead to a decrease in the flexural strength of zirconia.

Key words: Zirconia, Sandblasted, Hot-etching

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