光谱学与光谱分析, 2013, 33 (3): 704, 网络出版: 2013-03-27   

有机硼酸盐插层Zn/Al-LDH的红外和拉曼光谱特征

Raman and Infrared Spectrograms of Organic Borate Intercalated Hydrotalcite
作者单位
中国地质大学材料科学与工程学院, 北京100083
摘要
研究了碳酸根和硼酸根的二元锌铝水滑石的X射线衍射, 拉曼和红外光谱特征。 采用一步水热共沉淀法, 分别制得结晶良好的层间为碳酸根和硼酸根的二元锌铝水滑石。 X射线衍射分析显示, 硼酸根插层后水滑石(003)特征衍射峰向小角度移动, 峰型尖锐, 水滑石通道高度从0.28 nm增加至0.42 nm; 红外光谱和拉曼光谱特征表明, 硼酸根插层后, 碳酸根的红外和拉曼特征峰消失。 层间硼酸根以B3O3(OH)-4, B4O5(OH)2-4和B(OH)-4三种形式存在。 随层间离子的不同, 与羟基相关的红外光谱和拉曼光谱峰位均有所改变。 研究结果表明以硼酸三正丁酯为插层剂, 可获得单一相、 纯度较高的硼酸根型锌铝水滑石, 拉曼光谱可准确探测水滑石层间阴离子变化对其结构和性能的影响。
Abstract
The pattern of X-ray diffraction, the Raman and infrared spectra of organic borate intercalated hydrotalcite were discussed. The well crystallized zinc-aluminum layered double hydroxides (Zn-Al LDHs) intercalated by carbonate ions and borate ions were respectively prepared by co-precipitation method. Patterns of X-ray diffraction showed that the (003) reflection of borate-LDHs was sharp and symmetric and shifted to lower angle than that of carbonate-LDHs. The gallery height of borate-LDHs increased from 0.28 nm to 0.42 nm after intercalation, indicating that interlayered carbonate ions were substituted by borate anions. The Raman and IR spectra showed that specific bands of carbonate ions in the borate-LDHs disappeared, but with the presence of B3O3(OH)-4, B4O5(OH)2-4 and B(OH)-4 in the interlayer galleries. The hydroxide interlayer anions had a significant influence on the band positions in Raman and infrared spectra of modes related to the hydroxyl group. Our results indicate that single phase and pure borate-pillared LDHs can be obtained using tributyl orthoborate as intercalating agents, and the change in the structure and nature of hydrotalcite can be detected precisely by Raman spectroscopy.
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张婧宇, 白志民, 赵栋. 有机硼酸盐插层Zn/Al-LDH的红外和拉曼光谱特征[J]. 光谱学与光谱分析, 2013, 33(3): 704. ZHANG Jing-yu, BAI Zhi-min, ZHAO Dong. Raman and Infrared Spectrograms of Organic Borate Intercalated Hydrotalcite[J]. Spectroscopy and Spectral Analysis, 2013, 33(3): 704.

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