Amorphous Vanadium Oxide/Carbon Composite Positive Electrode for ...
Supporting Information
Amorphous Vanadium Oxide/Carbon Composite Positive Electrode for Rechargeable Aluminum Battery Masanobu Chiku*, Hiroki Takeda, Shota Matsumura, Eiji Higuchi and Hiroshi Inoue
Department of Applied Chemistry, Graduate School of Engineering,
Osaka Prefecture University, Sakai, Osaka 599-8531, Japan
.Corresponding author: [email protected]
Experimentals
Dipropylsulfone (Tokyo Chemical Industry) and all other chemicals (Wako Pure Chemical) were used as received without any purification. A Molybdenum plate was
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purchased from Nilaco Corporation. Ketjen black (EC600JD) was purchased from Lion Corporation.
Amorphous V2O5/C was prepared by referring to Kudo et al.1, 2 250 mg of vanadium powder was dissolved into 25 mL of 30 wt. % hydrogen peroxide solution in an ice bath. Then 750 mg of ketjen black (KB) was added into the solution. The temperature of the resultant suspension was gradually raised up to 60 ºC and held at this temperature to dry it up. The residue was clashed with mortar and heat-treated at 200 ºC for 10 h. The resultant powder is named V2O5/C hereafter. 45 mg of V2O5/C was mixed with 5 mg of PTFE, followed by pressing at 5.9 MPa for 1 min to form a pellet of 13 mm in diameter. KB electrode was formed as follow; 25 mg of KB and 5 mg of PTFE were mixed and pressed at 5.9 MPa for 1 min to form a pellet of 13 mm in diameter.
All electrochemical measurements were performed with glass cells. A mixture of aluminum chloride, dipropylsulfone and toluene (1:10:5 in mole ratio) was used as an electrolyte solution for rechargeable Al battery in the present study. A Mo plate (1.3 cm × 1.3 cm) was used as current collector, and immersed in conc. HCl for several seconds before use. An Al plate (10 mm in diameter) was used as counter and reference
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electrodes for all electrochemical experiments. A glass fiber filter was used as separator. In an Ar-filled glove box, a test cell was assembled and placed in a glass bottle with electrical contact point, and then the bottle was sealed. CV and charge/discharge tests were performed at 30 ºC with SI1287 potentiostat (Solartron) and HJ1001SM8 charge/discharge system (Hokuto Denko), respectively.
X-ray diffraction (XRD) spectra were measured by using an X-ray diffractometer (Shimadzu, XRD-6100, 50 kV, 30 mA) equipped with a Cu Kα source (λ= 0.1541nm). X-ray photoelectron spectroscopy (XPS) was performed to identify the vanadium valence by using ESCA-3200 (Shimadzu) equipped with a MgKα source. The contents of V5+, V4+ and V3+ were evaluated by deconvoluting the V 2P3/2 spectrum3 after the first discharge and charge at C/40.
Scanning electron microscope (SEM)
images and Energy dispersion X-ray analysis (EDX) were taken with an S-4500 field-emission SEM (Hitachi) and EDAX (Ametec). Nitrogen adsorption-desorption experiments were performed to determine the surface area of KB and V2O5/C with Micromeritics ASAP 2020 analyzer using Brunauer-Emmett-Teller (BET) gas adsorption method. Transmission Electron Microscope (TEM) images were taken by JEM-2100F (Hitachi). TEM samples were as prepared V2O5/C and after 3 cycle charge/discharged V2O5/C.
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TEM images of V2O5/C
Figure S1 TEM images of V2O5/C (a, b) before and (c, d) after charge discharge cycle.
CV of Al plate electrode
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Figure S2 CV of Al plate electrode.
References;
(1) Imamura, D.; Miyayama, M.; Hibino, M.; Kudo, T. Mg Intercalation Properties into V2O5 gel/Carbon Compositesunder High-Rate Condition. J. Electrochem. Soc., 2003, 150, A753-A758
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(2) Kudo, T.; Ikeda, Y.; Watanabe, T.; Hibino, M.; Miyayama, M.; Abe, H.; Kajita, K. Amorphous V2O5/Carbon Composites as Electrochemical Supercapacitor Electrodes. Solid State Ionics, 2002, 152-153, 833-841
(3) Hryha, E.; Rutqvist, E. Nyborg, L. Stoichiometric Vanadium Oxides Studied by XPS. Surf. Interface Anal. 2012, 44, 1022-1025
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Amorphous Vanadium Oxide/Carbon Composite Positive Electrode for Rechargeable Aluminum Battery Masanobu Chiku*, Hiroki Takeda, Shota Matsumura, Eiji Higuchi and Hiroshi Inoue
Department of Applied Chemistry, Graduate School of Engineering,
Osaka Prefecture University, Sakai, Osaka 599-8531, Japan
.Corresponding author: [email protected]
Experimentals
Dipropylsulfone (Tokyo Chemical Industry) and all other chemicals (Wako Pure Chemical) were used as received without any purification. A Molybdenum plate was
S-1
purchased from Nilaco Corporation. Ketjen black (EC600JD) was purchased from Lion Corporation.
Amorphous V2O5/C was prepared by referring to Kudo et al.1, 2 250 mg of vanadium powder was dissolved into 25 mL of 30 wt. % hydrogen peroxide solution in an ice bath. Then 750 mg of ketjen black (KB) was added into the solution. The temperature of the resultant suspension was gradually raised up to 60 ºC and held at this temperature to dry it up. The residue was clashed with mortar and heat-treated at 200 ºC for 10 h. The resultant powder is named V2O5/C hereafter. 45 mg of V2O5/C was mixed with 5 mg of PTFE, followed by pressing at 5.9 MPa for 1 min to form a pellet of 13 mm in diameter. KB electrode was formed as follow; 25 mg of KB and 5 mg of PTFE were mixed and pressed at 5.9 MPa for 1 min to form a pellet of 13 mm in diameter.
All electrochemical measurements were performed with glass cells. A mixture of aluminum chloride, dipropylsulfone and toluene (1:10:5 in mole ratio) was used as an electrolyte solution for rechargeable Al battery in the present study. A Mo plate (1.3 cm × 1.3 cm) was used as current collector, and immersed in conc. HCl for several seconds before use. An Al plate (10 mm in diameter) was used as counter and reference
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electrodes for all electrochemical experiments. A glass fiber filter was used as separator. In an Ar-filled glove box, a test cell was assembled and placed in a glass bottle with electrical contact point, and then the bottle was sealed. CV and charge/discharge tests were performed at 30 ºC with SI1287 potentiostat (Solartron) and HJ1001SM8 charge/discharge system (Hokuto Denko), respectively.
X-ray diffraction (XRD) spectra were measured by using an X-ray diffractometer (Shimadzu, XRD-6100, 50 kV, 30 mA) equipped with a Cu Kα source (λ= 0.1541nm). X-ray photoelectron spectroscopy (XPS) was performed to identify the vanadium valence by using ESCA-3200 (Shimadzu) equipped with a MgKα source. The contents of V5+, V4+ and V3+ were evaluated by deconvoluting the V 2P3/2 spectrum3 after the first discharge and charge at C/40.
Scanning electron microscope (SEM)
images and Energy dispersion X-ray analysis (EDX) were taken with an S-4500 field-emission SEM (Hitachi) and EDAX (Ametec). Nitrogen adsorption-desorption experiments were performed to determine the surface area of KB and V2O5/C with Micromeritics ASAP 2020 analyzer using Brunauer-Emmett-Teller (BET) gas adsorption method. Transmission Electron Microscope (TEM) images were taken by JEM-2100F (Hitachi). TEM samples were as prepared V2O5/C and after 3 cycle charge/discharged V2O5/C.
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TEM images of V2O5/C
Figure S1 TEM images of V2O5/C (a, b) before and (c, d) after charge discharge cycle.
CV of Al plate electrode
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Figure S2 CV of Al plate electrode.
References;
(1) Imamura, D.; Miyayama, M.; Hibino, M.; Kudo, T. Mg Intercalation Properties into V2O5 gel/Carbon Compositesunder High-Rate Condition. J. Electrochem. Soc., 2003, 150, A753-A758
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(2) Kudo, T.; Ikeda, Y.; Watanabe, T.; Hibino, M.; Miyayama, M.; Abe, H.; Kajita, K. Amorphous V2O5/Carbon Composites as Electrochemical Supercapacitor Electrodes. Solid State Ionics, 2002, 152-153, 833-841
(3) Hryha, E.; Rutqvist, E. Nyborg, L. Stoichiometric Vanadium Oxides Studied by XPS. Surf. Interface Anal. 2012, 44, 1022-1025
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