1H and 2H NMR studies of cyclohexane nanocrystals in controlled pore glasses

The formation and behaviour of cyclohexane and cyclohexane- d 12 nanocrystals in mesoporous solids of well-defined dimensional constraints are studied by 1H and 2H NMR. The NMR line widths, spin–spin relaxation times ( T 2), spin–lattice relaxation times ( T 1) and diffusivities ( D) were measured a...

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Bibliographic Details
Published in:Journal of molecular structure 2004-12, Vol.708 (1), p.23-31
Main Authors: Aksnes, D.W., Førland, K., Kimtys, L.
Format: Article
Language:English
Subjects:
Confined cyclohexane
Dynamic NMR
Nanocrystals
Pore glass
Relaxation
Self-diffusion
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Summary:The formation and behaviour of cyclohexane and cyclohexane- d 12 nanocrystals in mesoporous solids of well-defined dimensional constraints are studied by 1H and 2H NMR. The NMR line widths, spin–spin relaxation times ( T 2), spin–lattice relaxation times ( T 1) and diffusivities ( D) were measured as a function of temperature, and the results are discussed with reference to the values obtained for the bulk materials. The confined solids exhibit substantial changes in the phase behaviour and molecular dynamics. Thus, the line-shape measurements reveal a two-phase system consisting of a highly mobile component at the surface of the pore and a plastically crystalline phase in the centre of the pore. The liquid-like surface layer in the mesopores is observable well below the reduced transition temperature of the confined cyclohexane. However, the T 2 and diffusion measurements show that the mobile phase also embraces a minor component attributed to non-frozen liquid in pockets or offshoots.
ISSN:0022-2860
1872-8014
DOI:10.1016/j.molstruc.2004.02.055