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中华口腔医学研究杂志(电子版) ›› 2018, Vol. 12 ›› Issue (04) : 199 -204. doi: 10.3877/cma.j.issn.1674-1366.2018.04.001

所属专题： 文献；

基础研究

固化模式对双固化树脂水门汀微观机械性能及聚合程度的影响
黄沁1, 杨博1, 杨家俊1, 霍兆麟2, 王焱1,†()   
  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. 55455　美国明尼阿波利斯，明尼苏达大学牙学院牙科生物材料及生物力学研究中心
  • 收稿日期:2018-02-05 出版日期:2018-08-01
  • 通信作者: 王焱
  • 基金资助:
    国家自然科学基金(海外及港澳学者合作研究基金项目，81628005)

Effect of curing modes on nano - mechanical properties and monomer conversion of dual - cured resin cements

Qin Huang1, Bo Yang1, Jiajun Yang1, Zhaolin Huo2, Yan Wang1,†()   

  1. 1. Guanghua School of Stomatology, Hospital of Stomatology, Sun Yat-sen University, Guangdong Provincial Key Laboratory of Stomatology, Guangzhou 510055, China
    2. Minnesota Dental Research Center for Biomaterials and Biomechanics, School of Dentistry, University of Minnesota, Minneapolis, MN 55455, USA
  • Received:2018-02-05 Published:2018-08-01
  • Corresponding author: Yan Wang
  • About author:
    Corresponding author: Wang Yan, Email:
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引用本文：

黄沁, 杨博, 杨家俊, 霍兆麟, 王焱. 固化模式对双固化树脂水门汀微观机械性能及聚合程度的影响[J]. 中华口腔医学研究杂志(电子版), 2018, 12(04): 199-204.

Qin Huang, Bo Yang, Jiajun Yang, Zhaolin Huo, Yan Wang. Effect of curing modes on nano - mechanical properties and monomer conversion of dual - cured resin cements[J]. Chinese Journal of Stomatological Research(Electronic Edition), 2018, 12(04): 199-204.

目的

研究不同固化模式对临床常用的两种双固化树脂水门汀表面纳米硬度、弹性模量、压入蠕变等微观机械性能及聚合程度的影响。

方法

采用即刻光照、间歇光照、延迟光照和无光照四种不同的固化模式，分别对RelyX Unicem、PermaCem 2.0两种双固化树脂水门汀进行固化，制备厚度为0.5 mm、直径5 mm的圆形测试试件。室温避光保存24 h后，使用纳米压痕法对表面纳米硬度、弹性模量、压入蠕变等微观机械性能进行测量，使用傅立叶变换红外光谱-衰减全发射法测试材料的转化率。利用SPSS 16.0软件对数据进行分析（α= 0.05）。

结果

固化模式对本实验选用的两种双固化树脂水门汀的表面纳米硬度、弹性模量有显著影响（P<0.001）。对于RelyX Unicem，无光照组的表面纳米硬度、弹性模量最低，分别为（153.1 ± 14.6）MPa和（7.6 ± 0.7）GPa，即刻、间歇、延迟光照组差异无统计学意义。对于PermaCem 2.0，无光照组的表面纳米硬度、弹性模量最低，分别为（244.8 ± 21.1）MPa和（7.3 ± 0.5）GPa，即刻、间歇、延迟光照组差异无统计学意义。固化模式对RelyX Unicem的压入蠕变有显著影响（F= 135.41，P<0.001），对PermaCem 2.0也有显著影响（F= 148.94，P<0.001），其由高到低依次为：无光照组>延迟光照组>即刻、间歇光照组。固化模式对PermaCem 2.0的转化率有显著影响（F= 20.76，P= 0.004），但对RelyX Unicem的转化率无显著影响（F= 0.899，P= 0.447）。

结论

双固化树脂水门汀在无光照时容易固化不全，降低其微观机械性能。即刻、间歇光照比延迟光照更有利于降低树脂水门汀的压入蠕变。固化模式对不同种类的双固化树脂水门汀聚合程度及微观机械性能的影响程度不同。

关键词: 树脂粘固剂, 牙科胶粘剂光固化, 牙科树脂类自固化, 机械性能, 转化率, 固化模式
Objective

To investigate the influence of different curing modes on nanohardness, elastic modulus, indentation creep and monomer conversion of two types of dual-cured resin cements.

Methods

Specimens of 5 mm diameter and 0.5 mm thickness were fabricated with two dual-cured resin cements: RelyX Unicem (RU) and PermaCem 2.0 (PC) , under four different curing modes: immediate light-curing mode (IML) , intermittent light-curing mode (ITL) , delayed light-cuing mode (DL) and chemical curing mode (CC) . After 24 hours′ storage in darkness at room temperature, nanohardness, elastic modulus and indentation creep were measured with a nanoindentation device under a 10 mN load for 20 s holding time. Monomer conversion was measured by Fourier transform infrared spectroscopy- attenuated total reflection. Data were analyzed by SPSS 16.0 software (α=0.05) .

Results

Curing modes showed significant influence on nanohardness and elastic modulus for both RU and PC (P<0.001) . For RU, nanohardness and elastic modulus of CC group were the lowest among the four curing modes, which were (153.1 ± 14.6) MPa and (7.6 ± 0.7) GPa, respectively. For PC, nanohardness and elastic modulus of CC group were the lowest among the four curing modes, which were (244.8 ± 21.1) MPa and (7.3 ± 0.5) GPa, respectively. There were no significant differences in nanohardness and elastic modulus among IML, ITL and DL groups for both RU and PC. Curing modes showed significant influence on indentation creep for RU (F= 135.41, P<0.001) and PC (F= 148.94, P<0.001) , which ranked in the following order: CC>DL>IML, ITL. For RU, there were no significant difference in monomer conversion among the four curing modes (F= 0.899, P= 0.447) . However, there were significant difference in monomer conversion among the four curing modes for PC (F= 20.76, P= 0.004) .

Conclusions

Lack of light activation resulted in an insufficient polymerization and compromised mechanical properties for dual-cured resin cements. Immediate and delayed light curing modes produce higher indentation creep. Curing modes had different levels of impact on the mechanical properties and monomer conversion of dual-cured resin cements with different components.

Key words: Resin cements, Light-curing of dental cements, Self-curing of dental resins, Mechanical properties, Monomer conversion, Curing modes
表1 本实验用双固化树脂水门汀主要成分及比例
材料 成分 填料比例(vol%) 填料粒度（μm）
RelyTM Unicem 有机基质、甲基丙烯酸酯、酸性单体、引发剂、添加剂、无机填料、填料等 50 <9.5
PermaCem 2.0 含钡玻璃的双酚A双甲基丙烯酸缩水甘油酯(Bis-GMA)、着色剂、添加剂及引发剂等 51 0.02 ~ 3.0
表2 本实验分组情况及各组采用的固化模式
组别 固化模式
间歇光照组 光照2 s，避光1 min，光照18 s
即刻光照组 即刻光照20 s
延迟光照组 避光2 min，光照20 s
无光照组 无光照，混合后即刻避光保存
图1 双固化树脂水门汀纳米压痕测试过程中典型的压入载荷与压入深度的曲线关系
表3 不同固化模式下两种双固化树脂水门汀的纳米硬度、弹性模量及压入蠕变（ ± s）
组别 试件数 纳米硬度(MPa) 弹性模量(GPa) 压入蠕变(%)
RU PC RU PC RU PC
即刻光照组 2 385.6 ± 39.5Aa 312.5 ± 31.4Ba 8.0 ± 0.4Aa 8.0 ± 0.5Aa 13.2 ± 1.3Aa 14.4 ± 1.3Ba
间歇光照组 2 379.3 ± 46.2Aa 311.7 ± 39.0Ba 8.3 ± 0.3Aa 8.4 ± 1.0Aa 13.5 ± 0.9Aa 14.8 ± 1.6Ba
延迟光照组 2 353.8 ± 37.2Aa 295.8 ± 39.1Ba 8.1 ± 0.6Aa 7.8 ± 0.5Aa 14.4 ± 0.8Ab 15.9 ± 0.9Bb
无光照组 2 153.1 ± 14.6Ab 244.8 ± 21.1Bb 7.6 ± 0.7Ab 7.3 ± 0.5Ab 16.4 ± 1.7Ac 17.2 ± 1.0Bc
F值 ? 486.21 13.87 11.65 17.92 135.41 148.94
P值 ? <0.001 <0.001 <0.001 <0.001 <0.001 <0.001
表4 不同固化模式下两种双固化树脂水门汀转换率（n = 6，%， ± s）
组别 试件数 RU PC
即刻光照组 6 46.1 ± 2.6Aa 63.6 ± 3.1Ba
间歇光照组 6 45.8 ± 1.8Aa 60.7 ± 4.6Ba
延迟光照组 6 41.4 ± 2.2Aa 58.3 ± 2.7Ba
无光照组 6 37.4 ± 2.6Aa 48.4 ± 2.8Bb
F值 ? 0.899 20.76
P值 ? 0.447 0.004
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