TY - JOUR
T1 - A flow cell for transient voltammetry and in situ grazing incidence X-ray diffraction characterization of electrocrystallized cadmium(II) tetracyanoquinodimethane
AU - Veder, Jean Pierre
AU - Nafady, Ayman
AU - Clarke, Graeme
AU - Williams, Ross P.
AU - De Marco, Roland
AU - Bond, Alan M.
N1 - Funding Information:
The Australian Research Council (ARC) is acknowledged for financial support. The SR-GIXRD work was performed at the Australian National Beamline Facility (ANBF) with support from the Australian Synchrotron Research Program, which is funded by the Commonwealth of Australia under the Major National Research Facilities Program. We also thank Drs. Garry Foran and James Hester at the ANBF for support with the SR-GIXRD studies. One of us (J.P.V.) is grateful to Curtin University for a post-graduate scholarship, as well as the Australian Institute of Nuclear Science and Engineering (AINSE) for a postgraduate research award, and Mr. William Rickard in Applied Physics at Curtin University for assistance with the SEM research.
PY - 2011/1/1
Y1 - 2011/1/1
N2 - An easy to fabricate and versatile cell that can be used with a variety of electrochemical techniques, also meeting the stringent requirement for undertaking cyclic voltammetry under transient conditions in in situ electrocrystallization studies and total external reflection X-ray analysis, has been developed. Application is demonstrated through an in situ synchrotron radiation-grazing incidence X-ray diffraction (SR-GIXRD) characterization of electrocrystallized cadmium (II)-tetracyanoquinodimethane material, Cd(TCNQ)2, from acetonitrile (0.1 mol dm-3 [NBu 4][PF6]). Importantly, this versatile cell design makes SR-GIXRD suitable for almost any combination of total external reflection X-ray analysis (e.g., GIXRF and GIXRD) and electrochemical perturbation, also allowing its application in acidic, basic, aqueous, non-aqueous, low and high flow pressure conditions. Nevertheless, the cell design separates the functions of transient voltammetry and SR-GIXRD measurements, viz., voltammetry is performed at high flow rates with a substantially distended window to minimize the IR (Ohmic) drop of the electrolyte, while SR-GIXRD is undertaken using stop-flow conditions with a very thin layer of electrolyte to minimize X-ray absorption and scattering by the solution.
AB - An easy to fabricate and versatile cell that can be used with a variety of electrochemical techniques, also meeting the stringent requirement for undertaking cyclic voltammetry under transient conditions in in situ electrocrystallization studies and total external reflection X-ray analysis, has been developed. Application is demonstrated through an in situ synchrotron radiation-grazing incidence X-ray diffraction (SR-GIXRD) characterization of electrocrystallized cadmium (II)-tetracyanoquinodimethane material, Cd(TCNQ)2, from acetonitrile (0.1 mol dm-3 [NBu 4][PF6]). Importantly, this versatile cell design makes SR-GIXRD suitable for almost any combination of total external reflection X-ray analysis (e.g., GIXRF and GIXRD) and electrochemical perturbation, also allowing its application in acidic, basic, aqueous, non-aqueous, low and high flow pressure conditions. Nevertheless, the cell design separates the functions of transient voltammetry and SR-GIXRD measurements, viz., voltammetry is performed at high flow rates with a substantially distended window to minimize the IR (Ohmic) drop of the electrolyte, while SR-GIXRD is undertaken using stop-flow conditions with a very thin layer of electrolyte to minimize X-ray absorption and scattering by the solution.
KW - Electrochemical surface and interface analysis
KW - Electrocrystallization
KW - In situ external reflection X-ray analysis
KW - Synchrotron radiation-grazing incidence X-ray diffraction
UR - http://www.scopus.com/inward/record.url?scp=78650515462&partnerID=8YFLogxK
U2 - 10.1016/j.electacta.2010.09.106
DO - 10.1016/j.electacta.2010.09.106
M3 - Article
SN - 0013-4686
VL - 56
SP - 1546
EP - 1553
JO - Electrochimica Acta
JF - Electrochimica Acta
IS - 3
ER -