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Preparation method and application of in-situ carbon-compounded prussian blue type compound thin film

A Prussian blue, in-situ composite technology, applied in the field of energy material preparation and electrochemistry, can solve the problems of high internal vacancy and water content, poor electronic conductivity of materials, insufficient contact, etc., to increase the integrity of the crystal structure and reduce the vacancy. and the effect of improving water content and electrode conductivity

Inactive Publication Date: 2015-01-07
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] However, in practical application, the Prussian blue complexes still have the following two deficiencies: first, the sodium ion content in the complexes prepared by the general method is too low, and the internal vacancies and water content are high, which makes the charge and discharge capacity far lower. Lower than the theoretical value, and the cycle performance is poor; second, the electronic conductivity of the material itself is poor, resulting in poor rate performance
The above two reasons restrict the full play of its electrochemical performance.
In addition, from the perspective of the electrode preparation process, firstly, the active material and the conductive agent in the electrode prepared by the traditional coating method are difficult to mix uniformly, resulting in insufficient contact with each other, resulting in poor conductivity of the electrode; secondly, the coating film Active substances in the method are easily interfered by foreign substances such as conductive agents and binders, which will greatly affect the full play of their intrinsic properties.

Method used

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  • Preparation method and application of in-situ carbon-compounded prussian blue type compound thin film

Examples

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preparation example Construction

[0024] The preparation method of the Prussian blue compound thin film of in-situ composite carbon comprises the following steps:

[0025] 1) Ultrasonic dispersion of carbon materials in NaCl solution;

[0026] 2) Weigh the transition metal cyano complex, reducing agent and inorganic acid in proportion and add them to the above solution;

[0027] 3) Electrolysis of water for 3 to 5 minutes to clean the surface of the ITO conductive substrate;

[0028] 4) Under the constant voltage condition of -2.0-2.0V relative to the standard Ag / AgCl electrode, a Prussian blue compound film with in-situ composite carbon was formed on the ITO conductive substrate.

[0029] The mole fraction ratio of the transition metal cyano complex, inorganic acid, reducing agent and carbon material is 1:(0.1-30):(0.1-10):(0.1-20).

[0030] The carbon material is selected from at least one of Ketjen black, acetylene black, carbon black, Super P, graphene, carbon nanotubes, mesophase microspheres or pyrolyt...

Embodiment 1

[0041] In this example, an in-situ composite carbon Prussian blue thin film positive electrode material was prepared by an electrochemical deposition method. The molar ratio of each substance required for the reaction is Na 4 Fe(CN) 6 : HCl: Ketjen Black: Sodium Borohydride = 1:5:1:0.2. The specific steps are:

[0042] 1) Ultrasonic dispersion of Ketjen black in 1.0M NaCl solution;

[0043] 2) Weigh Na in proportion 4 Fe(CN) 6 , HCl and sodium borohydride were added to the above solution;

[0044] 3) Electrolysis of water for 3 to 5 minutes to clean the surface of the ITO conductive substrate;

[0045] 4) Under the constant voltage condition of -0.5V relative to the standard Ag / AgCl electrode, a Prussian blue film of in-situ composite carbon was formed on the ITO substrate, and finally the film was peeled off the substrate with a microknife for future use.

[0046] Analyze the crystal structure of product with powder X-ray diffractometer (Rigaku D / Max-2550pc, CuK ray), ...

Embodiment 2

[0051] The preparation method of this example is the same as that of Example 1, but the carbon material is acetylene black, and the reducing agent is sodium citrate. The molar ratio of each substance required for the reaction is Na 4 Fe(CN) 6 : HCl: acetylene black: sodium citrate=1:10:2:0.5. The specific steps are:

[0052] 1) Ultrasonic dispersion of acetylene black in 1.0M NaCl solution;

[0053] 2) Weigh Na in proportion 4 Fe(CN) 6 , HCl and sodium citrate were added to the above solution;

[0054] 3) Electrolysis of water for 3 to 5 minutes to clean the surface of the ITO conductive substrate;

[0055] 4) Under the constant voltage condition of -1.0V relative to the standard Ag / AgCl electrode, a Prussian blue film of in-situ composite carbon was generated on the ITO substrate, and finally the film was peeled off the substrate with a microknife for future use.

[0056] The assembly process and testing method of the button cell are the same as in Example 1.

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Abstract

The invention discloses a preparation method and application of an in-situ carbon-compounded prussian blue type compound thin film. The preparation method comprises the following steps: (1) carrying out ultrasonic dispersion on carbon materials in a NaCl solution; (2) weighing transition metal cyano complexes, a reducing agent and inorganic acid in a ratio and adding into the solution; (3) electrolyzing for 3-5 minutes in water to clean the surface of an ITO conducting substrate; and (4) generating the in-situ carbon-compounded prussian blue type compound thin film on the ITO conducting substrate under a constant-voltage condition relative to voltage from -2.0V to 2.0V of a standard Ag / AgCl electrode. According to the preparation method and the application, the film is formed in one step, the preparation method is rapid and simple and low in cost and the electrical conductivity of the obtained compound material is greatly improved; and the content of sodium is high, and vacancy and the water content are low. As a sodium-ion battery positive electrode material, the material has the characteristics of high specific capacity, high cycling stability, excellent rate performance and the like, and has a bright prospect in large-scale development and application of sodium-ion batteries.

Description

technical field [0001] The invention relates to a preparation method and application of a Prussian blue compound thin film of in-situ composite carbon, belonging to the fields of energy material preparation and electrochemistry. Background technique [0002] Lithium-ion batteries have shown broad application prospects in portable electronic devices and electric vehicles due to their advantages such as high specific capacity, high power density, stable discharge, and environmental friendliness. However, the reserves of lithium resources in the earth's crust are limited, and the price of lithium raw materials continues to rise, hindering the sustainable development of lithium-ion batteries. In addition to having a similar working principle to lithium-ion batteries, sodium-ion batteries also have the advantages of abundant resources and low cost, and are considered to be an ideal choice for next-generation energy storage power sources. In the current reports on sodium-ion batt...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/1393H01M4/583
CPCH01M4/1393H01M4/583H01M2004/028Y02E60/10
Inventor 姜银珠于胜兰李勇
Owner ZHEJIANG UNIV
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