Direct Detection of Al-O-Al Structure in Aluminosilicate Specimens: A Use of Homo-Nuclear DQMAS NMR

作者:Lin, Xiongchao*; Ideta, Keiko; Miyawaki, Jin; Wang, Yonggang; Nishiyama, Yusuke; Yoon, Seongho; Mochida, Isao
来源:Applied Magnetic Resonance, 2014, 45(2): 111-123.
DOI:10.1007/s00723-013-0504-4

摘要

A general strategy of Al-O-Al structure in various aluminosilicate was evaluated by combining triple-quantum magic angle spinning (3QMAS) and double-quantum homo-nuclear correlation under magic angle spinning (DQMAS) solid-state nuclear magnetic resonance (NMR) measurements with the aid of high magnetic field NMR (800 MHz for H-1 Larmor frequency). The results show that in many cases the direct detection of Al-O-Al sites in aluminosilicate crystals and glasses is possible; hence the extent of aluminum avoidance can be directly elucidated. Specifically, experimental evidence of Al-O-Al linkages in several aluminosilicate materials with Si/Al > 1 was straightforwardly confirmed; and the existence of Al-O-Al is considered to have little correlation with the Si/Al ratio, but it may be strongly related to the cation and local structural arrangement. In addition, the presence of tri-clusters of (Si, Al)O-4-tetrahedra in aluminosilicate framework was proposed, which was thought to act as nuclei for formation and incorporation of cations to achieve charge neutrality.