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Preparation method for NiCo2S4@NiCo2O4 nanoneedle composite catalytic electrode with core-shell structure

A technology of catalytic electrode and core-shell structure, which is applied in the field of electrocatalysis, can solve the problems of unfavorable electrocatalytic performance, poor stability and electronic conductivity, unfavorable commercial application, etc., and achieve favorable electrocatalytic performance and high stability and electron conductivity, the effect of low electrode cost

Inactive Publication Date: 2016-08-17
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The materials used in this patent are metals or alloys, and contain precious metals, which are not conducive to commercial applications, and wet chemical reduction is used to prepare powdery materials, which have weak stability and electronic conductivity, which is not conducive to the improvement of electrocatalytic performance.

Method used

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  • Preparation method for NiCo2S4@NiCo2O4 nanoneedle composite catalytic electrode with core-shell structure
  • Preparation method for NiCo2S4@NiCo2O4 nanoneedle composite catalytic electrode with core-shell structure
  • Preparation method for NiCo2S4@NiCo2O4 nanoneedle composite catalytic electrode with core-shell structure

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Wash the 4cm×1cm nickel foil with acetone, ethanol, and distilled water successively, and ultrasonically clean each for 15min until the surface is clean, then blow dry with nitrogen gas for use. Weigh 0.1426g NiCl 2 ·6H 2 O, 0.2852g CoCl 2 ·6H 2O and 0.4324g urea (the molar ratio is 1:2:12); they are dissolved in the mixed solution of 24mL water and ethanol (the volume ratio is 1:1); Transfer to a 30mL reactor and place in an oven at 95°C for 10h. After the reaction, the reactor was cooled to room temperature, and the Ni-Co composite precursor was taken out, washed with distilled water and ethanol in turn, and dried in a vacuum oven at 60° C. for 2 hours. Transfer 22.5mL of sodium sulfide solution (concentration 0.1-0.4mol / L) to a 30mL reactor, put the prepared Ni-Co composite precursor into the reactor, and place it in an oven at 120°C for vulcanization reaction, keeping 4-16h. After the vulcanization reaction is over, wait for the reactor to cool down to room te...

Embodiment 2

[0030] NiCo is prepared in Example 1 2 S 4 @NiCo 2 o 4 The electrochemical properties of the nanoneedle composite catalytic electrode were tested in 1M KOH solution.

[0031] Using a three-electrode electrochemical measurement system, on the CHI660c electrochemical workstation, the prepared NiCo 2 S 4 @NiCo 2 o 4 The nanoneedle composite catalytic electrode is the working electrode, the platinum wire electrode is the counter electrode, and the saturated calomel electrode (SCE) is the reference electrode. The linear sweep voltammetry curve (LSV) of the measurement electrode is shown in image 3 . The specific test conditions are as follows: the electrolyte is 1mol L -1 KOH solution; the potential window is 0-0.8V; the scan rate is 0.005V / s. from image 3 It can be seen in the synthesized NiCo 2 S 4 @NiCo 2 o 4 The nanoneedle composite catalytic electrode shows good catalytic performance in the process of water oxidation, and the current density has reached 120mA c...

Embodiment 3

[0033] NiCo is prepared in Example 1 2 S 4 @NiCo 2 o 4 Nanoneedle composite catalytic electrode at 1mol L -1 The stability of the electrode during water oxidation was tested in KOH solution.

[0034] Using a three-electrode electrochemical measurement system, on a CHI660c electrochemical workstation, the prepared core-shell structure NiCo 2 S 4 @NiCo 2 o 4 The nanoneedle composite catalytic electrode is the working electrode, the platinum wire electrode is the counter electrode, and the saturated calomel electrode (SCE) is the reference electrode. The stability of the electrode is measured by a multi-step current method, see Figure 4 . The specific test conditions are as follows: the electrolyte is 1mol L -1 KOH solution; the current value setting range is 0.005-0.05A, the current interval of each step is 0.005A, and the holding time of each step is 500s. from Figure 4 It can be seen that within about 1.5h, the catalytic performance of the catalyst is basically no...

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Abstract

The invention relates to a preparation method for a NiCo2S4@NiCo2O4 nanoneedle composite catalytic electrode with a core-shell structure. The NiCo2S4@NiCo2O4 nanoneedle composite catalytic electrode grows in situ on the surface of nickel foil through two steps of the hydrothermal process. Compared with the prior art, the electrocatalytic electrode prepared through the method has the advantages that the electrical conductivity of a spinel oxide NiCo2O4 and the electrocatalytic water oxidation property are greatly improved through construction of the double-component core-shell structure, the advantages of being large in current density, high in electrocatalytic efficiency, stable in catalytic property and the like are achieved, only 290-mV overpotential needs to be supplied, the current density can reach 10 mA.cm<-2>, and the initial oxygen evolution potential is 0.46 V vs SCE. In addition, the electrode is simple in preparation method and low in preparation cost and has the potential application value in the energy and environment fields such as water decomposition hydrogen production and carbon dioxide reduction.

Description

technical field [0001] The invention relates to the technical field of electrocatalysis, in particular to a high-efficiency core-shell structure NiCo for promoting water oxidation 2 S 4 @NiCo 2 o 4 Preparation method of nano needle composite catalytic electrode. Background technique [0002] In recent years, in order to solve the increasingly serious energy crisis, environmental pollution, greenhouse effect and other problems in human society, the development of clean energy with sustainable development characteristics has become a popular scientific research topic. Among many new energy sources, solar energy has been paid more and more attention due to its advantages such as huge energy, inexhaustibility, and no pollution. If we could harness 1% of this energy, it would be possible to meet the energy needs of the entire world. Solar energy is obviously different from petroleum, coal and other fossil fuels. Solar energy is easy to obtain, and its use will neither pollut...

Claims

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Application Information

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IPC IPC(8): C02F1/46C02F1/72
CPCC02F1/4672
Inventor 史慧杰王英玲赵国华
Owner TONGJI UNIV
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