Ilie Nicoleta, Durner Jürgen
Department of Operative/Restorative Dentistry, Periodontology and Pedodontics, Ludwig-Maximilians-Universität München, Goethestr. 70, 80336, Munich, Germany,
Clin Oral Investig. 2014 Jul;18(6):1587-96. doi: 10.1007/s00784-013-1128-7. Epub 2013 Nov 21.
This study aimed to describe the polymerization process and to quantify the parameters of influence in two bulk-fill resin-based composites by comparing two real-time methods: the Fourier transform infrared (FTIR) spectroscopy and the visible light transmission spectrometry.
The degree of conversion (DC) was recorded in real time for 5 min using the attenuated total reflectance FTIR spectroscopy (n = 6) on the lower surface of 2, 4, and 6 mm thick samples irradiated for 20 s. The variation in irradiance was recorded during material irradiation at the bottom of the samples (n = 5). Results were statistically analyzed using one-way and multiple-way ANOVAs with Tukey HSD post hoc test (α = 0.05), partial eta-squared statistics, and Pearson correlation.
No significant difference was found in DC in any materials as a function of incremental thickness, whereas the irradiance passing the specimens differed consistently within both analyzed increments and materials. These data could be described by the superposition of two exponential functions, the first being attributed to the gel phase and the second to the glass phase, resulting in an exponential sum function. DC data were able to calculate the end of the gel phase and the beginning of the glass phase, whereas irradiance measurements were able to detect only the last phase. The polymerization kinetics in the glass phase was less material-dependent as in the gel phase.
The irradiance measurements were more sensitive to variation in thickness, meaning that translucency is continuing to change as a function of thickness at a higher extent than DC.
Knowing the impact of the modulation factors describing the calculated sum exponential function allows the manipulation of the polymerization process at different stages to tailor material properties.
本研究旨在通过比较两种实时方法:傅里叶变换红外(FTIR)光谱法和可见光透射光谱法,描述两种大块充填树脂基复合材料的聚合过程并量化影响参数。
使用衰减全反射傅里叶变换红外光谱法(n = 6)在2、4和6毫米厚的样品下表面对辐照20秒的样品实时记录5分钟的转化率(DC)。在样品底部进行材料辐照期间记录辐照度的变化(n = 5)。使用单向和多向方差分析以及Tukey HSD事后检验(α = 0.05)、偏η²统计和Pearson相关性对结果进行统计学分析。
在任何材料中,转化率均未随增量厚度表现出显著差异,而在两种分析的增量和材料中,透过样品的辐照度始终存在差异。这些数据可以用两个指数函数的叠加来描述,第一个归因于凝胶相,第二个归因于玻璃相,从而得到一个指数和函数。转化率数据能够计算凝胶相的结束和玻璃相的开始,而辐照度测量仅能检测到最后一个阶段。玻璃相中的聚合动力学比凝胶相对材料的依赖性更小。
辐照度测量对厚度变化更敏感,这意味着半透明性随厚度的变化程度比转化率更高。
了解描述计算出的和指数函数的调节因素的影响,有助于在不同阶段控制聚合过程,以调整材料性能。