Chinese Journal of Magnetic Resonance ›› 2010, Vol. 27 ›› Issue (3): 436-444.

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Preparation of CsH2PO4 and CsH5(PO4)2 Investigated with Multinuclear Solid-State NMR Spectroscopy

Seen Ae CHAE1, Young Eun LEE1, Oc Hee HAN1,2*, Sang Geul LEE1   

  1. 1. Daegu Center, Korea Basic Science Institute, Daegu, 702-701, Republic of Korea; 2. Graduate School of Analytical Science and Technology, Chungnam National University, Daejeon, 305-764, Republic of Korea
  • Received:2010-07-16 Online:2010-09-05 Published:2010-09-05

Abstract:

We attempted to prepare CsH2PO4 (CDP) and CsH5(PO4)2 (CPDP), compounds known to be promising solid acid electrolytes for fuel cells. The CDP and CPDP mixture was crystallized from an aqueous solution of Cs2CO3∶H3PO4, in a molar ratio of 1∶4, while the mixture of CDP and Cs2HPO4·1.5H2O (H-DCHP) was obtained from the aqueous solution in a molar ratio of 1∶2. Methanol washing was most effective in separating the CDP from the mixture. The 133Cs and 31P MAS NMR spectra of CDP, CPDP, and H-DCHP, and the 1H MAS NMR spectra of CPDP and H-DCHP were reported for the first time and the peaks corresponding to each compound assigned. Herein, we demonstrated multinuclear SS-NMR to be a very useful tool to control the quality of the syntheses of solid acid electrolytes by identification of the electrolytes synthesized and the by-products produced in the process of the syntheses.

Key words: solid-state NMR, solid acid electrolyte, CsH2PO4, CsH5(PO4)2, 133Cs MAS NMR,  31P MAS NMR,  1H MAS NMR

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