Cheng Shaodong, Yang Guang, Zhao Yanqi, Peng MingYing, Skibsted Jørgen, Yue Yuanzheng
Electronic Materials Research Laboratory, Key Laboratory of the Ministry of Education &International Center for Dielectric Research, Xi'an Jiaotong University, Xi'an, 710049, China.
State Key Laboratory of Luminescent Materials and Devices, South China University of Technology, Guangzhou, 510640, China.
Sci Rep. 2015 Dec 8;5:17526. doi: 10.1038/srep17526.
Transmission electron microscopy and related analytical techniques have been widely used to study the microstructure of different materials. However, few research works have been performed in the field of glasses, possibly due to the electron-beam irradiation damage. In this paper, we have developed a method based on electron energy loss spectroscopy (EELS) data acquisition and analyses, which enables determination of the boron speciation in a series of ternary alkali borosilicate glasses with constant molar ratios. A script for the fast acquisition of EELS has been designed, from which the fraction of BO4 tetrahedra can be obtained by fitting the experimental data with linear combinations of the reference spectra. The BO4 fractions (N4) obtained by EELS are consistent with those from (11)B MAS NMR spectra, suggesting that EELS can be an alternative and convenient way to determine the N4 fraction in glasses. In addition, the boron speciation of a CeO2 doped potassium borosilicate glass has been analyzed by using the time-resolved EELS spectra. The results clearly demonstrate that the BO4 to BO3 transformation induced by the electron beam irradiation can be efficiently suppressed by doping CeO2 to the borosilicate glasses.
透射电子显微镜及相关分析技术已被广泛用于研究不同材料的微观结构。然而，在玻璃领域开展的研究工作较少，这可能是由于电子束辐照损伤所致。在本文中，我们开发了一种基于电子能量损失谱（EELS）数据采集与分析的方法，该方法能够测定一系列具有恒定摩尔比的三元碱硼硅酸盐玻璃中的硼形态。设计了一个用于快速采集EELS的脚本，通过将实验数据与参考光谱的线性组合进行拟合，可从中获得BO4四面体的比例。通过EELS获得的BO4比例（N4）与来自（11）B MAS NMR光谱的结果一致，这表明EELS可以作为一种替代且便捷的方法来测定玻璃中的N4比例。此外，利用时间分辨EELS光谱分析了CeO2掺杂的硼酸钾硅酸盐玻璃的硼形态。结果清楚地表明，通过向硼硅酸盐玻璃中掺杂CeO2，可以有效抑制电子束辐照引起的BO4向BO3的转变。
