In-situ preparation method of three-dimensional conductive MOF@MXene composite electrode

A composite electrode and in-situ preparation technology, which is applied in the manufacture of hybrid capacitor electrodes, hybrid/electric double layer capacitors, etc., can solve problems such as poor electrical conductivity, achieve uniform distribution of components, mild conditions, excellent electrochemical activity and The effect of stability

Active Publication Date: 2020-12-08
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] In order to overcome the problem of poor conductivity of MOF, the present invention provides an in-situ preparation method of a three-dimensional conductive MOF@MXene composite electrode. The process is efficient and stable, the process flow is simple, and energy is effectively saved. The prepared three-dimensional conductive MOF@MXene Composite powders can be used as supercapacitor electrode materials to achieve stable and efficient energy storage

Method used

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  • In-situ preparation method of three-dimensional conductive MOF@MXene composite electrode
  • In-situ preparation method of three-dimensional conductive MOF@MXene composite electrode

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Effect test

Embodiment 1

[0025] A three-dimensional Ni 3 (HITP) 2 In situ preparation method of @MXene composite electrode and supercapacitor application, including the following steps: (1) Multilayer Ti 3 C 2 T x Preparation of powder: add 1 g Ti to a round bottom centrifuge tube 3 AlC 2 solid and 10 mL HF (40wt%), stirred at 35 °C for 24 h, after the reaction, washed 6 times with deionized water until the pH dropped to 6, and the obtained product was vacuum-dried at 60 °C for 24 h. 3 C 2 T x powder;

[0026] (2) Ti 3 C 2 T x Preparation of -COOH: Add 300 mg multilayer Ti to a 100 mL glass vial 3 C 2 T x Powder, 5 g of chloroacetic acid and 300 mL of 0 °C aqueous solution were stirred at room temperature for 1 h, then 32 mL of 6 M NaOH aqueous solution was added, and the reaction was stirred at a constant temperature in a water bath at 60 °C for 3 h. After the reaction, centrifuged and washed 6 times, vacuum dried to obtain Ti 3 C 2 T x - COOH powder;

[0027] (3) Three-dimensional ...

Embodiment 2

[0031] A three-dimensional Ni 3 (HITP) 2 @Ti 2 CT x The in-situ preparation method and supercapacitor application of composite electrodes include the following steps: (1) multilayer Ti 2 CT x Preparation of powder: add 1 g Ti to a round bottom centrifuge tube 2 AlC solids and 5 mL HF (40%wt) were stirred at 35 °C for 5 h. After the reaction, they were washed with deionized water for 6 times until the pH dropped to 7. The obtained product was vacuum-dried at 60 °C for 24 h. 2 CT x powder;

[0032] (2) Ti 2 CT x Preparation of -COOH: Add 12 mg multilayer Ti to a 100 mL glass vial 2 CT x Powder, 3 g of chloroacetic acid and 300 mL of 0 °C aqueous solution were stirred at room temperature for 1 h, then 32 mL of 1 M NaOH aqueous solution was added, and the reaction was stirred at a constant temperature in a water bath at 60 °C for 1 h. After the reaction, centrifuged and washed 6 times, vacuum dried to obtain Ti 3 C 2 T x - COOH powder;

[0033] (3) Three-dimensional...

Embodiment 3

[0035] A three-dimensional Ni 3 (HITP) 2 @V 2 CT x The in-situ preparation method and supercapacitor application of composite electrodes include the following steps: (1) multilayer V 2 CT x Preparation of powder: add 1 g of V to a round bottom centrifuge tube 2 AlC solid and 20 mL HF (40%wt), stirred at 35 °C for 10 h, after the reaction, washed 6 times with deionized water until the pH dropped to 7, and the obtained product was vacuum-dried at 60 °C for 24 h with multilayer V 2 CT x powder;

[0036] (2)V 2 CT x - Preparation of COOH: Add 300 mg multilayer V in a 100 mL glass vial 2 CT x Powder, 300 mg of chloroacetic acid and 300 mL of 0 ℃ aqueous solution were stirred at room temperature for 1 h, then 32 mL of 10 M NaOH aqueous solution was added, and the reaction was stirred at a constant temperature in a 60 ℃ water bath for 12 h. After the reaction, centrifuged and washed 6 times, vacuum dried to get V 2 CT x - COOH powder;

[0037] (3) Three-dimensional Ni...

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Abstract

The invention relates to the field of the synthesis of composite materials, and provides an in-situ preparation method of a three-dimensional conductive MOF@MXene composite electrode in order to solvethe problem of poor conductivity of MOFs, which comprises the following steps: adding MAX phase powder into an HF solution, etching for 5-24 hours, centrifugally washing with deionized water until the pH value of the upper solution is 6-7, and carrying out vacuum drying to obtain multilayer MXene powder; uniformly dispersing the powder in the deionized water, adding chloroacetic acid, stirring atroom temperature, adding a NaOH solution, carrying out stirring reaction for 1-12 hours, carrying out centrifugal washing, and carrying out vacuum drying to obtain MXene-COOH powder; dispersing the powder into the deionized water, adding a metal salt, a ligand and ammonia water in order, carrying out air-blowing stirring reaction at 50-70 DEG C, and finally, carrying out centrifugal washing and drying to obtain the three-dimensional conductive MOF@MXene composite powder. The method is efficient and stable in process and simple in process, the prepared composite powder can serve as a super-capacitor electrode material, and the stable and efficient energy storage is achieved.

Description

technical field [0001] The invention relates to the field of synthesis of composite materials, in particular to an in-situ preparation method of a three-dimensional conductive MOF@MXene composite electrode. Background technique [0002] Electrochemical double-layer capacitors (EDLCs) have high power density and excellent cycle performance, and have become a research hotspot in recent years. They have great prospects in smart grids, electric vehicles and other application fields, and are even eager to compete for the market of traditional batteries. state. The active electrode materials of capacitors are represented by activated carbon, carbon nanotubes, porous graphene, metal oxides / hydroxides, etc., which have the characteristics of large porosity and high specific surface area, which is conducive to increasing the contact between active substances and solutions and improving energy storage. efficiency. For example, an invention patent with publication number CN103828002A...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01G11/86H01G11/30H01G11/24
CPCH01G11/86H01G11/30H01G11/24Y02E60/13
Inventor 曹澥宏高鑫隆施文慧毋芳芳阮鹏超
Owner ZHEJIANG UNIV OF TECH
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