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Crystallographic and transport studies on AsF5 intercalated graphite from 4.2 to 295 K. I. Structural ordering and phase separation

Published online by Cambridge University Press:  31 January 2011

M. Lelaurain
Affiliation:
Laboratoire de Chimie du solide Minéral, Service de Chimie Minérale Appliquée, UA CNRS 158, Université de Nancy 1, BP239,54506 Vandoeuvre les Nance, France
J. F. Marêché
Affiliation:
Laboratoire de Chimie du solide Minéral, Service de Chimie Minérale Appliquée, UA CNRS 158, Université de Nancy 1, BP239,54506 Vandoeuvre les Nance, France
E. McRae
Affiliation:
Laboratoire de Chimie du solide Minéral, Service de Chimie Minérale Appliquée, UA CNRS 158, Université de Nancy 1, BP239,54506 Vandoeuvre les Nance, France
G. Furdin
Affiliation:
Laboratoire de Chimie du solide Minéral, Service de Chimie Minérale Appliquée, UA CNRS 158, Université de Nancy 1, BP239,54506 Vandoeuvre les Nance, France
A. Hérold
Affiliation:
Laboratoire de Chimie du solide Minéral, Service de Chimie Minérale Appliquée, UA CNRS 158, Université de Nancy 1, BP239,54506 Vandoeuvre les Nance, France
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Abstract

A study of the (00l), (hk0), and (hkl) reflections of stage 1 AsF5 intercalated graphite between 4.2 and 295 K has been done using synchrotron radiation for single-crystal samples and a linear detector setup for those based on highly oriented pyrographite (HOPG). The nature and temperature dependence of the structural ordering allow the materials to be classified into (at least) two types related to the degree to which the AsF5 has been converted into AsF6 and AsF3. At 295 K a small amount of in-plane order is detected within the essentially two-dimensional (2-D) liquid intercalate attributed to small quantities of AsF5 and AsF6 − AsF5-ordered phases. Lowering the temperature leads to increased phase separation through crystallization and to changes in the in-plane unit cells associated with each. The most marked structural change is an incommensurate-to-commensurate (I⇉C) transformation within the AsF5 phase, which starts at 215 ± 5 K. No new structural order is detected below 180 K. The (00l) studies give clear confirmation of the existence of separate phases with different values of interplanar distance. A smaller number of stage 2 compounds were examined. The most clearly different feature is that the I⇉C transformation is downshifted by ∼ 70 K. At room temperature, the stacking sequences are A/A/A … for stage 1 and A/AB/BC/CA … for stage 2.

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Copyright
Copyright © Materials Research Society 1988

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Crystallographic and transport studies on AsF5 intercalated graphite from 4.2 to 295 K. I. Structural ordering and phase separation
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Crystallographic and transport studies on AsF5 intercalated graphite from 4.2 to 295 K. I. Structural ordering and phase separation
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Crystallographic and transport studies on AsF5 intercalated graphite from 4.2 to 295 K. I. Structural ordering and phase separation
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