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One-step electrodeposition method to prepare 3D needle-like nickel-cobalt double metal oxide nanoclusters

A technology of double metal oxide and electrodeposition method, which is applied in the direction of nanotechnology, nanotechnology, hybrid/electric double layer capacitor manufacturing, etc., can solve the problems of reducing the capacitance performance of materials, uncontrollable reaction process, and large influence of substrate capacitance. To achieve the effect of increasing the specific capacitance value and cycle stability, the reaction process is intuitive and controllable, and the loading capacity is increased

Active Publication Date: 2021-05-28
SHAANXI TECHN INST OF DEFENSE IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, when using the hydrothermal template-assisted method to prepare electrode materials with different shapes, the shape of the sample is difficult to control. The existence of the template will increase the dead volume of the electrode and reduce the capacitive performance of the material.
Therefore, it is necessary to remove the template twice, but this not only increases the operation steps of the experiment, but also causes secondary damage to the electrode structure due to multiple reactions
[0003] For the problem of preparing 3D Ns-Ni-Co LDH by the template-assisted method, the following methods are currently used to solve the problem: (1) directly use the hydrothermal method to prepare without additional template assistance, but the reaction process is uncontrollable and the sample morphology is difficult. To achieve a 3D needle-like nanocluster structure, at the same time, the requirements for the reaction container are more stringent; (2) use a solvent with a lower concentration to dissolve the template, although the damage to the substrate is reduced, but the removal of the template is not complete, and the capacitance of the substrate Greater impact

Method used

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  • One-step electrodeposition method to prepare 3D needle-like nickel-cobalt double metal oxide nanoclusters
  • One-step electrodeposition method to prepare 3D needle-like nickel-cobalt double metal oxide nanoclusters
  • One-step electrodeposition method to prepare 3D needle-like nickel-cobalt double metal oxide nanoclusters

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 1. Cut the nickel foam into a square sheet with a specification of 1cm×1cm×0.25cm, and then at room temperature, first place the cut foam nickel in 3mol / L acetone aqueous solution for 30min, and then place it in a 6% mass concentration Soak in hydrochloric acid for 30 minutes. After soaking, use absolute ethanol and deionized water to wash the foamed nickel repeatedly several times, and dry the cleaned foamed nickel in a vacuum oven at 70°C for 3 hours.

[0029] 2. Soak the nickel foam after vacuum drying in step 1 in 20mL pretreatment solution, which contains 0.375mmol / L Ni(NO 3 ) 2 , 0.75mmol / L Co(NO 3 ) 2 , 1.125mmol / L NH 4 NO 3 , an aqueous solution with a volume concentration of 2.5% dimethyl sulfoxide, heated and reacted in an oil bath at 100°C for 30 minutes, and after the reaction was completed, the sample was repeatedly ultrasonically cleaned several times with deionized water and absolute ethanol, and then the sample was placed in a 60°C oven Dry for 2 ho...

Embodiment 2

[0035] 1. Cut the nickel foam into a square sheet with a specification of 1cm×1cm×0.25cm, and then at room temperature, first place the cut foam nickel in 3mol / L acetone aqueous solution for 30min, and then place it in a 6% mass concentration Soak in hydrochloric acid for 30 minutes. After soaking, use absolute ethanol and deionized water to wash the foamed nickel repeatedly several times, and dry the cleaned foamed nickel in a vacuum oven at 70°C for 3 hours.

[0036] 2. Soak the nickel foam after vacuum drying in step 1 in 20mL pretreatment solution, which contains 0.375mmol / LNi(NO 3 ) 2 , 0.75mmol / L Co(NO 3 ) 2 , 1.125mmol / L NH 4 NO 3 , an aqueous solution with a volume concentration of 2.5% dimethyl sulfoxide, heated and reacted in an oil bath at 100°C for 10 minutes, and after the reaction was completed, the sample was repeatedly ultrasonically cleaned several times with deionized water and absolute ethanol, and then the sample was placed in a 60°C oven Dry for 2 hou...

Embodiment 3

[0040] 1. Cut the nickel foam into a square sheet with a specification of 1cm×1cm×0.25cm, and then at room temperature, first place the cut foam nickel in 3mol / L acetone aqueous solution for 30min, and then place it in a 6% mass concentration Soak in hydrochloric acid for 30 minutes. After soaking, use absolute ethanol and deionized water to wash the foamed nickel repeatedly several times, and dry the cleaned foamed nickel in a vacuum oven at 70°C for 3 hours.

[0041] 2. Soak the nickel foam after vacuum drying in step 1 in 20mL pretreatment solution, which contains 0.375mmol / L Ni(NO 3 ) 2 , 0.75mmol / L Co(NO 3 ) 2 , 1.125mmol / L NH 4 NO 3 , an aqueous solution with a volume concentration of 2.5% dimethyl sulfoxide, heated and reacted in an oil bath at 100°C for 60 minutes, and after the reaction was completed, the sample was repeatedly ultrasonically cleaned several times with deionized water and absolute ethanol, and then the sample was placed in a 60°C oven Dry for 2 ho...

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Abstract

The invention discloses a method for preparing 3D acicular nickel-cobalt double metal oxide nanoclusters by a one-step electrodeposition method. The method uses pretreated nickel foam as a substrate and vertically grows on the surface of the substrate by a one-step constant current electrodeposition method. Acicular Ni-Co double metal oxide, the electrode material prepared by this method has good contact with the substrate, and does not need to use any binder and conductive agent, and the substrate foam nickel has both self-supporting effect and good conductivity. At the same time, the fine pore structure on the surface of the pretreated nickel foam not only has the template effect, but also has a certain capacitance contribution when the template can increase the loading capacity of the active material per unit area, without secondary removal, and the preparation method is simple and efficient. It also provides a novel research idea for the preparation of wire electrode materials, which has certain universality.

Description

technical field [0001] The invention belongs to the technical field of supercapacitors, and in particular relates to a method for preparing 3D needle-shaped nickel-cobalt double metal oxide nanoclusters by a one-step electrodeposition method. Background technique [0002] Spinel binary metal oxide NiCo 2 o 4 , with low production cost, high theoretical specific capacitance (1370F / g), and abundant redox electron pairs (Ni 2+ / Ni 3+ and Co 2+ / Co 3+ ) and other characteristics have attracted widespread attention. It has been found that the morphology, conductivity, and porosity of electrode materials play a key role in improving the electrochemical performance of supercapacitors. Among them, the change of material morphology is particularly important because electrode materials with hierarchical / porous structures or three-dimensional (3D) array structures can increase the specific surface area of ​​electrode materials, improve the contact area between electrodes and elec...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01G11/86H01G11/46H01G11/26H01G11/24C25D9/04C25D5/40C25D5/50B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00C25D5/40C25D5/50C25D9/04H01G11/24H01G11/26H01G11/46H01G11/86Y02E60/13
Inventor 刘沛静辛福恩
Owner SHAANXI TECHN INST OF DEFENSE IND