Preparation method based on solid-phase reaction for capacitor electrode material

A capacitor electrode and solid-state reaction technology, which is applied in hybrid capacitor electrodes, hybrid/electric double-layer capacitor manufacturing, vanadium halides, etc., can solve the problems of restricting electrochemical performance, high electrode resistance, and poor conductivity of cobalt tetraoxide

Active Publication Date: 2015-06-24
SUZHOU INST OF NANO TECH & NANO BIONICS CHINESE ACEDEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the poor conductivity and high electrode resistance of cobalt tetraoxide, its electrochemical performance as an electrode material is severely restricted.

Method used

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  • Preparation method based on solid-phase reaction for capacitor electrode material
  • Preparation method based on solid-phase reaction for capacitor electrode material
  • Preparation method based on solid-phase reaction for capacitor electrode material

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Experimental program
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Effect test

Embodiment 1

[0044] Such as figure 1 Shown, this capacitor electrode material preparation method based on solid phase reaction comprises the following steps:

[0045] 1. First, weigh the raw materials cobalt acetate tetrahydrate and oxalic acid dihydrate in a molar ratio of 1:1, for example, weigh 0.747g of cobalt acetate tetrahydrate and 0.378g of oxalic acid dihydrate, and grind them in an agate mortar for 0.5h respectively , to ensure that the reactants are fully refined; 2, then, take graphene oxide 0.06g (the amount of graphene oxide is preferably 5% to 30% of the quality of the final cobalt tetroxide obtained, and the present embodiment takes 0.06g to be about the final obtained 25% of the quality of tricobalt tetroxide), mixed evenly with the above-mentioned ground cobalt acetate tetrahydrate, and then ground for about 0.25h; Until the gas with a pungent smell is released, a black paste precursor is obtained, the main component of which is a cobalt oxalate-graphene oxide mixture. ...

Embodiment 2

[0054] Such as figure 1 As shown, the method for preparing the capacitor electrode material in this embodiment differs in step 2:

[0055] The precursor was placed in a tube furnace, raised from room temperature to 300° C. over 0.5 h, and continued to be calcined at this temperature for 0.5 h to obtain a black tricobalt tetroxide-graphene composite material. Comparing the three cobalt tetroxide-graphene composites calcined under two kinds of temperature conditions, its properties are as follows: image 3 As shown, the integral area of ​​the cyclic voltammetry curve of the sample at the calcination temperature of 275°C is greater than that at the calcination temperature of 300°C, indicating that the specific capacitance of the sample at the calcination temperature of 275°C is greater than that at the calcination temperature of 300°C.

Embodiment 3

[0057] The capacitor electrode material preparation method of the present embodiment, see Figure 4 , including the following steps:

[0058] 1. First weigh the raw materials cobalt acetate tetrahydrate and citric acid monohydrate in a molar ratio of 1:1, for example, weigh 0.747g of cobalt acetate tetrahydrate and 0.627g of citric acid monohydrate, and grind them in an agate mortar 1h to ensure that the reactant is fully refined; 2. Then, take 0.072g of graphene oxide (according to 30% of the mass of cobalt tetroxide finally obtained), mix it with the above-mentioned ground cobalt acetate tetrahydrate, and then grind for about 0.5h; 3. Finally, continue grinding with the above-mentioned ground citric acid monohydrate for 0.5h at room temperature until the gas without pungent odor in the mixture is released, and a black paste precursor is obtained, the main component is cobalt citrate-graphite oxide Alkene mixture.

[0059] A chemical reaction occurs in the above grinding, s...

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Abstract

The invention discloses a preparation method based on a solid-phase reaction for a capacitor electrode material. The preparation method comprises the following steps of: 1) adequately mixing and grinding cobalt acetate, oxalic acid and oxidized graphene to obtain an cobalt oxalate-oxidized graphene mixture; and 2) calcining the cobalt oxalate-oxidized graphene mixture aforementioned to obtain a cobaltosic oxide-graphene electrode material, wherein the dosage ratio by mole of cobalt acetate to oxalic acid is 1: 1, and the dosage of oxidized graphene is 5-30% of the mass of the finally obtained cobaltosic oxide; additionally, the selected ligand can also be citric acid and hexamethylenetetramine except oxalic acid; a solvent is not used in the solid-phase reaction of the preparation method disclosed by the invention, so that the side reactions generated in a water-phase reaction are avoided, the yield and the purity are increased, the reaction conditions are easy to control, and the operation is simple and practicable; and moreover, via the introduction of the graphene material, a novel way is provided for an oxide material with bad electrical conductivity, good energy storage property, and high theoretical specific capacitance in the field of capacitors, and the graphene material has important theoretical and practical application significance.

Description

technical field [0001] The invention relates to the technical field of nanomaterial preparation, in particular to a method for preparing a capacitor electrode material. Background technique [0002] Supercapacitor is an energy storage device with energy storage performance between conventional capacitors and batteries. It has the advantages of fast charging speed, high power density, long cycle life, and environmental friendliness, which fully makes up for the shortcomings of conventional capacitors and batteries. Cobalt tetroxide, a transition metal oxide, has attracted widespread attention in the field of supercapacitor materials due to its high theoretical specific capacitance, good charge-discharge stability, simple preparation method, and wide range of raw material sources. However, due to the poor conductivity and high electrode resistance of cobalt tetroxide, its electrochemical performance as an electrode material is severely restricted. The traditional synthesis me...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G51/04C01G31/04H01G11/86H01G11/24
Inventor 田靖陈名海
Owner SUZHOU INST OF NANO TECH & NANO BIONICS CHINESE ACEDEMY OF SCI
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