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Published October 18, 2012 | Published + Supplemental Material
Journal Article Open

In Situ NMR Study on the Interaction between LiBH_4–Ca(BH_4)_2 and Mesoporous Scaffolds

Abstract

We discuss the use of nuclear magnetic resonance (NMR) spectroscopy to investigate the physical state of the eutectic composition of LiBH_(4)–Ca(BH_4)_2 (LC) infiltrated into mesoporous scaffolds and the interface effect of various scaffolds. Eutectic melting and the melt infiltration of mixed borohydrides were observed through in situ NMR. In situ and ex situ NMR results for LC mixed with mesoporous scaffolds indicate that LiBH_4 and Ca(BH_4)_2 exist as an amorphous mixture inside of the pores after infiltration. Surprisingly, the confinement of the eutectic LC mixture within the mesopores is initiated below the melting temperature, which indicates a certain interaction between the borohydrides and the mesoporous scaffolds. The confined borohydrides remain inside of the pores after cooling. These phenomena were not observed in microporous or nonporous materials, and this observation highlights the importance of the pore structure of the scaffolds. Such surface interactions may be associated with a faster dehydrogenation of the nanoconfined borohydrides.

Additional Information

© 2012 American Chemical Society. Received: August 16, 2012; Accepted: September 24, 2012; Published: September 24, 2012. We thank Mr. Yashodhan Bhawe and Dr. Mark E. Davis at the California Institute of Technology for their support in zeolite materials and helpful discussions. This work has been sponsored by the Korea Research Council of Fundamental Science and Technology. The NMR facility at the California Institute of Technology was supported by the National Science Foundation (NSF) under Grant Number 9724240 and partially supported by the MRSEC Program of the NSF under Award Number DMR-520565.

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Published - jz301199y.pdf

Supplemental Material - jz301199y_si_001.pdf

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