10.1002/cctc.201901530
ChemCatChem
FULL PAPER
H. S. Gao, L. Bai, J. L. Han, B. B. Yang, S. J. Zhang, X. P.
Zhang, Chem. Commun. 2018, 54, 12671-12685.
for 24 h. The final products were centrifuged, washed with ethanol
and deionized water for 3 times, respectively and then lyophilised.
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Electrochemical Measurement
To obtain the In2S3/CP working electrodes, 2.0 mg of the prepared
In2S3 above was suspended in 240 μL ethanol and 40 μL Nafion
D−521 to form a homogeneous ink assisted by ultrasound. Then,
the ink was spread onto CP (1×1 cm2) surface by a micropipette,
and finally dried under room temperature. The electrolysis
experiments were conducted in a typical H−type cell separated by
Nafion 117 membrane on an electrochemical workstation (CHI
660E, Shanghai CH Instruments Co., China). Carbon paper
spread with catalyst was used as working electrode. Ag/Ag+ (0.01
M AgClO4 in 0.1 M TBAP−MeCN) electrode and a platinum gauze
were used as reference electrode and counter electrode,
respectively. Before the experiment, the electrolyte was bubbled
with CO2 (30 mL/min) for at least 30 min to form CO2 saturated
solution and slight magnetic stirring was applied in electrolyte
during experiment for better mixing. Linear sweep voltammetry
(LSV) measurements were recorded at a scan rate of 20 mV s−1
and the potential range is from −0.9 to −2.4 V. All potentials in this
study were measured against the Ag/Ag+ reference electrode and
each current density was normalized by electrode geometric area.
0.1 ML H2SO4 aqueous solution was used as anodic electrolyte
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hexafluorophosphate ([Bmim][PF6])/MeCN−H2O mixture solution
containing 30 wt% [Bmim]PF6, 65 wt% MeCN, and 5 wt% H2O
was used as cathodic electrolyte.
The electrochemical active surface area is proportional to Cdl
value. Cdl was determined by the capacitive current associated
with double−layer charging from the scan−rate dependence of
cyclic voltammogram which ranged from −0.04 to −0.20 V (vs.
Ag/Ag+) with different scan rates were 10, 20, 40 and 80 mV s−1.
The electrochemical impedance spectroscopic (EIS) was carried
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open circuit potential (OCP) within the frequency extent of 100 to
100000 Hz and at an amplitude of 5 mV.
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Acknowledgements
This work is financially supported by the National Key R&D
Program of China (2018YFB0605802), the National Natural
Science Foundation of China (21838010, 51574215), the
program of Beijing Municipal Natural Science Foundation
(2182072, 2182071), the Beijing hundreds of leading talents
training project of science and technology (Z171100001117154),
and the DNL Cooperation Fund, CAS (DNL 180406)
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Keywords: CO2 reduction• Ionic liquid • Indium sulfide • facet
sensitivity • electrocatalyst
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