Carbon-coated iron-based prussian blue and preparation method thereof and sodium ion battery

A carbon-coated iron-based, Prussian blue technology, used in battery electrodes, secondary batteries, circuits, etc., can solve the problem of not achieving complete carbon coating, and achieve excellent cycle stability, less contact, and good rate performance. Effect

Active Publication Date: 2018-07-31
张五星
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method can improve the conductivity of Prussian blue to a certain extent, but it has not achieved complete carbon coating, the improvement of its conductivity is limited, the required carbon content is high, and the side reaction between Prussian blue and organic electrolyte will still occur. Inhibit its performance as a sodium ion cathode material

Method used

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  • Carbon-coated iron-based prussian blue and preparation method thereof and sodium ion battery
  • Carbon-coated iron-based prussian blue and preparation method thereof and sodium ion battery
  • Carbon-coated iron-based prussian blue and preparation method thereof and sodium ion battery

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preparation example Construction

[0027] The preparation method of the carbon-coated iron-based Prussian blue of the present invention utilizes uniform carbon-coated nano-metal or metal oxide as a precursor, and then adopts a liquid phase reaction to make a uniform carbon-coated metal M source (M is Fe, Mn, Co, Ni) react with sodium ferrocyanide solution to obtain carbon-coated iron-based Prussian blue, which specifically includes the following steps:

[0028] S1: Synthesis of uniform carbon-coated metals or metal oxides as metal M sources;

[0029] S2: Stir and disperse the product of step S1 in water or an organic solvent (ethylene glycol, acetonitrile, N-methylpyrrolidone, etc.), or add an appropriate amount of additives to assist the reaction (such as sodium citrate, etc.).

[0030] S3: Take a certain amount of sodium ferrocyanide to prepare a solution, then mix and react with the solution of S2, and finally obtain carbon-coated Prussian blue.

Embodiment 1

[0031] Example 1: Synthesis of carbon-coated iron Prussian blue (NaxFeFe(CN) in aqueous solution 6 )

[0032] Specifically include the following steps:

[0033] S1: Prussian blue (Fe) with a purity greater than 99% 4 [Fe(CN) 6 ] 3 ) placed in a container filled with an inert atmosphere, and heat-treated at 650° C. for 10 h, and cooled to room temperature to obtain carbon-coated nano-iron powder.

[0034] S2: 0.1 g of the product of step S1 was vigorously stirred and dispersed in 50 ml of aqueous solution (0.2 wt%).

[0035] S3: Take 2mmol of sodium ferrocyanide to prepare a 50ml solution (0.04mol / L). Then mix with the solution of S2.

[0036] S4: Add 0.8754ml (37wt% HCL) dropwise to the mixed solution obtained in S3, and react in a water bath at 60°C for 72h to obtain carbon-coated Prussian blue.

[0037] figure 1 The XRD diffraction collection of patterns of the carbon-coated Prussian blue powder prepared for this implementation example, by and XRD standard PDF card (...

Embodiment 2

[0039] Embodiment 2: Synthesis of carbon-coated ferromanganese Prussian blue (NaxMnFe(CN) in ethylene glycol solution 6 )

[0040] Specifically include the following steps:

[0041] S1: heat-treat nano-manganese monoxide (MnO) powder in an acetylene atmosphere at 600°C for 2 hours for carbon coating;

[0042] S2: 0.5 g of the product of step S1 was vigorously stirred and dispersed in 50 ml of ethylene glycol solution (10 wt%).

[0043] S3: Take 6 mmol of sodium ferrocyanide and prepare 50 ml of ethylene glycol solution (0.12 mol / L). Then mix with the solution of S2.

[0044] S4: Add 10ml of glacial acetic acid dropwise to the mixed solution prepared in S3, and react for 72h in a water bath at 80°C to obtain carbon-coated ferromanganese Prussian blue.

[0045]In the present invention, for Na x MFe(CN) 6 The form of metal source (M) (metal element or oxide, etc.), the mass ratio of carbon-coated metal source and sodium ferrocyanide reaction, the amount of acid added, react...

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Abstract

The invention discloses a preparation method of carbon-coated iron-based prussian blue. The preparation method comprises the following steps of S1, synthesizing uniform and carbon-coated metal or metal oxide to be used as a metal M source; S2, taking the product in the step S1, performing strong stirring and enabling the product to be dispersed into water or an organic solvent to form a solution;S3, taking sodium ferrocyanide, and preparing into a solution, and enabling the solution to be mixed with the solution obtained in the step S2; and S4, adding an additive to the solution obtained in the step S3, and performing a reaction at a proper temperature to obtain the carbon-coated iron-based prussian blue. The invention also discloses the carbon-coated iron-based prussian blue. The invention also discloses a sodium ion battery. According to the preparation method disclosed in the invention, the uniform and carbon-coated nanometer metal source and sodium ferrocyanide are reacted to obtain iron-based prussian blue in in-situ growth in the carbon raw material, and the surface is uniformly coated with carbon, so that prussian blue is more excellent in conductivity, and less in contactwith an electrolyte, thereby suppressing a secondary reaction between prussian blue and the electrolyte in a high potential.

Description

technical field [0001] The invention belongs to the technical field of preparation of carbon-coated iron-based Prussian blue composites, and more specifically relates to a carbon-coated iron-based Prussian blue, a preparation method thereof, and an application thereof in anode materials for sodium-ion batteries. Background technique [0002] Iron-based Prussian Blue (Na x MFe(CN) 6 , 0≤x≤2, M is Ni, Fe, Mn, Ni and other transition metal elements), with a cubic framework, in which M and Fe alternately occupy the apex positions of the cube and are connected by cyano groups (CN). The metal-organic framework structure of Prussian blue and its derivatives can provide enough space for the transport of sodium ions, so it is an ideal choice for the cathode material of sodium-ion batteries. [0003] The traditional synthesis method of iron-based Prussian blue is the aqueous co-precipitation method. At room temperature, the salt solution of metal M is added dropwise to the solution...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/36H01M4/58H01M4/62H01M10/054
CPCH01M4/366H01M4/58H01M4/625H01M4/628H01M10/054H01M2004/021H01M2004/028Y02E60/10
Inventor 张五星龚文哲薛丽红
Owner 张五星
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