Nano flower-shaped NiCoP supercapacitor electrode material, preparation method and application thereof
A technology of supercapacitors and electrode materials, which is applied in the manufacture of hybrid capacitor electrodes and hybrid/electric double-layer capacitors, etc., can solve the problems of poor conductivity and structural instability of metal-organic frameworks, and achieve improved conductivity and structural stability. Conductivity, the effect of improving performance
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[0031] A kind of preparation method of nano flower shape NiCoP supercapacitor electrode material, comprises the following steps:
[0032] S1. The preparation of the metal-organic framework material comprises the following steps:
[0033] 290mg Ni(NO 3 ) 2 ·6H 2 O, 125mg Co(NO 3 ) 2 ·6H 2 O, 50 mg H 4DOBDC and 1.5g of PVP were uniformly dispersed in 30ml of ethanol, distilled water and DMF with a volume ratio of 1:1:1 and stirred evenly; ℃ for hydrothermal reaction, the reaction time is 12 hours, after the reaction is completed, a turbid solution is obtained; the precipitation is collected by centrifugation at 7000r / min for 3 minutes, and the precipitation is washed with ethanol and distilled water in turn to remove the residual reagents and by-products; finally, at 70 Vacuum drying at ℃ to obtain the Ni / Co-MOFs precursor;
[0034] S2, the synthesis of three-dimensional nano flower-like double metal phosphide NiCoP, comprising the following steps:
[0035] Under an ult...
Embodiment 1
[0039] 290mg Ni(NO 3 ) 2 ·6H 2 O, 125mg Co(NO 3 ) 2 ·6H 2 O, 50 mg H 4 DOBDC and 1.5g PVP were uniformly dispersed in 30ml mixed solution (volume ratio of ethanol:distilled water:DMF was 1:1:1) and stirred evenly. The clarified solution was transferred to an autoclave, and then placed in a blast drying oven for hydrothermal reaction at a reaction temperature of 160° C. for 12 hours. After the reaction was completed, the precipitate was collected from the turbid solution by centrifugation (7000r / min, 3min), and the precipitate was washed with ethanol and distilled water in order to wash away residual reagents and by-products. Finally, the Ni / Co-MOFs precursor, that is, the Ni / Co metal-organic framework material, was obtained by vacuum drying at 70 °C.
Embodiment 2
[0042] NiCoP composites were prepared by low-temperature phosphating of Ni / Co-MOFs in a tube furnace under an ultrapure Ar atmosphere. Ni / Co-MOFs (20mg) precursor and NaH 2 PO 2 2H 2 O points (120mg) were placed in two porcelain boats with NaH 2 PO 2 2H 2 The porcelain boat of O is located upstream of the ultrapure Ar gas flow, and the porcelain boat with Ni / Co-MOFs precursor is located at the upstream of the NaH 2 PO 2 2H 2 Downstream of the porcelain boat of O; then, the Ni / Co-MOFs precursor was heated to 300 °C for 2 h at a rate of 3 °C / min. After cooling to room temperature, a black and black three-dimensional nanoflower-like bimetallic phosphide NiCoP is obtained, which is denoted as NiCoP.
[0043] The nickel mesh is used as the current collector, and the nickel mesh does not provide electrochemical performance. According to the mass ratio, NiCoP: polyvinylidene fluoride: acetylene black = 8:1:1 (where: the amount of NiCoP is 30mg) mixed and transferred to 30ml ...
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