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A cell for the in situ study of electrocrystallization
Author(s) -
Parkin Andrew,
Johnstone Stuart F.,
Mount Andrew R.,
Parsons Simon,
Pulham Colin R.,
Sanders David
Publication year - 2004
Publication title -
journal of applied crystallography
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 1.429
H-Index - 162
ISSN - 1600-5767
DOI - 10.1107/s0021889803029625
Subject(s) - in situ , diffractometer , materials science , diffraction , single crystal , electrode , phase (matter) , oxide , nanotechnology , optics , crystallography , chemistry , crystal structure , metallurgy , physics , organic chemistry
A new cell for studying electrocrystallization in situ on a diffractometer is reported. The construction of the cell is described in detail. The working electrode, fabricated from a propelling pencil lead encased in glass, was designed to sit in the path of the incident X‐ray beam so that processes occurring at its tip could be studied using diffraction methods. Practical difficulties of both design and data collection are discussed, as well as advantages and limitations of the method. In a series of proof‐of‐concept experiments, the cell has been applied to the in situ study of silver, both by powder and single‐crystal methods. A new silver oxide perchlorate phase, Ag 7 O 8 ClO 4 , was also identified using the cell; use of the same growth conditions ex situ enabled a sample of this new phase to be isolated.