Dynamic in situ electrochemical neutron reflectivity measurements.
We report the first dynamic in situ electrochemical neutron reflectivity (NR) measurements on electroactive films. By using a boxcar integration strategy within a cyclic voltammetric experiment, it is possible to acquire neutron reflectivity data associated with narrow, defined windows of potential. Accumulation of data from repetitive cycles allows one to build up potential- (time-) resolved profiles. The effective time resolution is now on the order of seconds, as compared to ca. 1 h using conventional methodology, making in situ NR a practical technique for dynamic electrochemical studies. Illustrative data for polyvinylferrocene films reveal hysteresis in (de)swelling, incomplete desolvation upon reduction, and transient salt retention, all of which respond to time-scale variations.
Cooper
Jonathan M
JM
Department of Electronics, University of Glasgow, Glasgow G12 8LT, Scotland, U.K.
Cubitt
Robert
R
Dalgliesh
Robert M
RM
Gadegaard
Nikolaj
N
Glidle
Andrew
A
Hillman
A Robert
AR
Mortimer
Roger J
RJ
Ryder
Karl S
KS
Smith
Emma L
EL