华西口腔医学杂志 ›› 2018, Vol. 36 ›› Issue (3): 252-256.doi: 10.7518/hxkq.2018.03.004

• 基础研究 • 上一篇    下一篇

纳米氢氧化锆涂层对10-甲基丙烯酰氧癸二氢磷酸酯提高氧化锆陶瓷粘接强度的影响

陈冰卓1,2, 杨路1,2, 陈莹1,2, 张怀勤1,2, 谢海峰1,2, 何峰1,3   

  1. 1.南京医科大学口腔疾病研究江苏省重点实验室
    2.南京医科大学附属口腔医院口腔修复科
    3.口腔特诊科,南京 210029
  • 收稿日期:2017-08-14 修回日期:2018-04-05 出版日期:2018-06-01 发布日期:2018-06-01
  • 作者简介:

    陈冰卓,硕士,E-mail:125036701@qq.com

  • 基金资助:
    国家自然科学基金(81400539);江苏省自然科学基金(BK20150998,BK20140913);江苏省高校自然科学研究面上项目(15KJB320003);江苏高校优势学科建设工程资助项目(2014-37)

Effects of nano-zirconium hydroxide coating on resin bonding of 10-methacryloxy decyldihydrogen phosphate-conditioned zirconia

Bingzhuo Chen1,2, Lu Yang1,2, Ying Chen1,2, Huaiqin Zhang1,2, Haifeng Xie1,2, Feng He1,3   

  1. 1. Jiangsu Key Laboratory of Oral Diseases, Nanjing Medical University, Nanjing 210029, China
    2. Dept. of Prosthodontics, Affiliated Hospital of Stomatology, Nanjing Medical University, Nanjing 210029, China
    3. Dept. of Specialty, Affiliated Hospital of Stomatology, Nanjing Medical University, Nanjing 210029, China
  • Received:2017-08-14 Revised:2018-04-05 Online:2018-06-01 Published:2018-06-01
  • Supported by:
    The National Natural Science Foundation of China (81400539);Natural Science Foundation of Jiangsu Province (BK20150998, BK20140913);The Natural Science Research in Jiangsu Higher Education Institutions (15KJB320003);Con-struction Project of Dominant Discipline in Jiangsu Higher Education Institutions (2014-37).

摘要:

目的 研究纳米氢氧化锆在氧化锆陶瓷表面形成碱性涂层后对10-甲基丙烯酰氧癸二氢磷酸酯(MDP)与氧化锆陶瓷粘接强度的影响。方法 制作氧化钇稳定四方相氧化锆(Y-TZP)瓷片140枚,氧化铝喷砂后对其表面进行不同的处理,制作粘接试件并测试剪切粘接强度。以X线光电子能谱(XPS)检测Y-TZP陶瓷表面依次经过纳米氢氧化锆涂层和含有MDP的底涂剂处理后的化学键变化。结果 老化前,与对照组相比,两种碱性涂层均能提高短期粘接强度值,纳米氢氧化锆涂层增强效果更显著。老化后,各组粘接强度值差异无统计学意义,但较老化前均显著降低(P<0.05)。XPS在制备纳米氢氧化锆涂层的Y-TZP瓷片表面检测到-OH键,在制备纳米氢氧化锆涂层的Y-TZP陶瓷应用含有MDP的底涂剂处理后检测出-P-O-Zr键。结论 在氧化锆陶瓷表面制备碱性涂层能够使MDP提高氧化锆陶瓷粘接强度。

关键词: 氧化锆, 粘接, 10-甲基丙烯酰氧癸二氢磷酸酯, 纳米氢氧化锆, pH值, 涂层

Abstract:

Objective This study evaluated the influence of alkaline coating of nano-zirconium hydroxide on resin bonding of 10-methacryloxy decyldihydrogen phosphate (MDP)-conditioned zirconia. Methods A total of 140 yttria-stabilized tetragonal zirconia polycrystals (Y-TZP) plates were prepared and sandblasted with alumina particles, and then subjected to different surface treatment. Resin bonding specimens were prepared with a MDP-free resin cement and tested for shear bond strength (SBS). X-ray photoelectron spectroscopy (XPS) was used to investigate the formation of chemical bond on the surface of Y-TZP treated successively with nano-zirconium hydroxide coating and MDP containing primer. Results The two alkaline coatings increased the 24 h SBS compared to control groups, and groups using nano-zirconium hydroxide coating yielded higher SBS. After thermocycling, no statistical difference was observed between groups, but SBS decreased significantly compared to the 24 h SBS (P<0.05). XPS analysis detected -OH bond on the surface of Y-TZP treated with nano-zirconium hydro-xide coating, and -P-O-Zr bond was detected on the surface of Y-TZP treated with nano-zirconium hydroxide coating and MDP-containing primer. Conclusion Alkaline coatings improved the bonding of resin to zirconia conditioned with MDP-containing primers.

Key words: zirconia, bond, 10-methacryloxy decyldihydrogen phosphate, nano zirconium hydroxide, pH value, coating

中图分类号: 

  • R783.2

图 1

纳米氢氧化锆涂层用液在洁净硅片的典型SEM图像左:× 20 000;右:× 80 000。"

图 2

Y-TZP陶瓷表面纳米氢氧化锆涂层的典型SEM图像左:× 50 000;右:× 100 000。"

表 1

各组试件剪切粘接强度"

组别 37 ℃水储24 h 冷热循环20 000次
Ctr 5.95±2.00 2.48±1.72
Zp 9.54±1.74 6.96±1.96
Cp 8.73±2.01 6.15±1.73
ZpZr 12.23±1.91 7.03±1.89
CpZr 13.40±1.89 7.24±1.90
ZpNa 10.95±1.89 7.66±2.02
CpNa 10.29±1.93 7.65±1.96

表 2

各组试件断裂模式"

组别 37 ℃水储24 h 冷热循环20 000次
A B C A B C
Ctr 5 5 0 0 10 0
Zp 10 0 0 10 0 0
Cp 10 0 0 10 0 0
ZpZr 10 0 0 10 0 0
CpZr 9 0 1 10 0 0
ZpNa 10 0 0 10 0 0
CpNa 10 0 0 10 0 0

图 3

Y-TZP瓷片经氢氧化锆溶液处理后的O1s图谱左:对照组;右:Clearfil Ceramic Primer处理组。"

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