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Preparation method of iron carbide composite electrode material coated with nitrogen and sulfur doped with carbon

A composite electrode and carbon coating technology, applied in nanotechnology for materials and surface science, battery electrodes, circuits, etc., can solve the problem of uneven distribution of iron carbide particles, cumbersome preparation process operations, difficult to control doping methods, etc. The problem is that the synthesis process is easy to control, the process is simple, and the preparation cost is low.

Inactive Publication Date: 2019-05-07
GUANGXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In order to solve the problems of harsh reaction conditions, cumbersome preparation process operation, difficult control of doping methods and uneven distribution of iron carbide particles in the preparation method of the above-mentioned iron carbide and nitrogen-sulfur-doped carbon composite electrode material, the present invention invents a method for preparing nitrogen-sulfur A method for doping a carbon-coated iron carbide composite electrode material, thereby providing a method for preparing a nitrogen-sulfur-doped carbon-coated iron carbide composite electrode material with low production cost, simple operation steps, and good controllability

Method used

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  • Preparation method of iron carbide composite electrode material coated with nitrogen and sulfur doped with carbon
  • Preparation method of iron carbide composite electrode material coated with nitrogen and sulfur doped with carbon
  • Preparation method of iron carbide composite electrode material coated with nitrogen and sulfur doped with carbon

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Embodiment 1

[0027] The preparation method of nitrogen-sulfur-doped carbon-coated iron carbide composite electrode material, the specific operation steps are as follows:

[0028] (1) Get ferric chloride hexahydrate 2mmol, thiourea 100mmol and glucose 1mmol respectively according to ferric chloride hexahydrate, thiourea and glucose into a molar ratio of 2:100:1, and ferric chloride hexahydrate, thiourea Mix with glucose, and dissolve in 100ml of deionized water and ethanol in a solvent mixed at a volume ratio of 2:1, stir evenly and heat to 90°C to evaporate the solvent until dry powder is obtained;

[0029] (2) Put the dry powder obtained in step (1) into a tube furnace for heat treatment in argon. The heating rate of the heat treatment is 2°C / min, and the temperature is raised to 800°C, kept for 1 hour, and then cooled to room temperature to obtain black Powder; wherein, the inert atmosphere flow rate is controlled at 60cc / min;

[0030] (3) Add the black powder obtained after cooling in ...

Embodiment 2

[0032] The preparation method of nitrogen-sulfur-doped carbon-coated iron carbide composite electrode material, the specific operation steps are as follows:

[0033] (1) According to ferric nitrate nonahydrate, thiourea and glucose into a molar ratio of 1:100:1, take 1 mmol of ferric nitrate nonahydrate, 100 mmol of thiourea and 1 mmol of glucose respectively, mix ferric nitrate nonahydrate, thiourea and glucose, and dissolve In a solvent composed of 100ml of deionized water and ethanol in a volume ratio of 1:1, stir evenly and heat to 90°C to evaporate the solvent until a dry powder is obtained;

[0034] (2) Put the dry powder obtained in step (1) into a tube furnace for heat treatment in argon. The heating rate of the heat treatment is 5°C / min, and the temperature is raised to 900°C, kept for 1 hour, and then cooled to room temperature to obtain black Powder; wherein, the inert atmosphere flow rate is controlled at 80cc / min;

[0035] (3) Add the black powder obtained after ...

Embodiment 3

[0037] The preparation method of nitrogen-sulfur-doped carbon-coated iron carbide composite electrode material, the specific operation steps are as follows:

[0038] (1) Get ferric chloride hexahydrate 5mmol, thiourea 100mmol and glucose 1mmol respectively according to ferric chloride hexahydrate, thiourea and glucose into a molar ratio of 5:100:1, and ferric chloride hexahydrate, thiourea Mix with glucose, and dissolve in 100ml of deionized water and ethanol in a solvent with a volume ratio of 1:1, stir evenly and heat to 90°C to evaporate the solvent until a dry powder is obtained;

[0039] (2) Put the dry powder obtained in step (1) into a tube furnace for heat treatment in an inert atmosphere of argon. The heating rate of the heat treatment is 10°C / min, and the temperature is raised to 1000°C, kept for 1 hour, and then cooled to room temperature. Obtain black powder; Wherein, inert gas flow rate is controlled at 30cc / min;

[0040](3) Add the black powder obtained after co...

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Abstract

The invention discloses a preparation method of an iron carbide composite electrode material coated with nitrogen and sulfur doped with carbon. The method comprises the following steps of: (1) mixingan iron-containing compound, thiourea and glucose, dissolving the mixture into a solvent for stirring and heating until dried powder is obtained; (2) performing heat treatment in an inert atmosphere for cooling to obtain black powder; (3) adding an acid solution for heating and stirring, filtering to remove filter residues to wash until the solvent is neutral, cooling and drying the residue obtained after washing to obtain an iron carbide composite electrode material coated with nitrogen and sulfur doped with carbon. The method is simple in process, greatly limits the agglomeration of the ironcarbide nanoparticles, is easy to control of the synthesis process and low in manufacturing cost, and can be applied to fields of energy storage and conversion research such as lithium ion batteries,electrocatalytic oxygen reduction.

Description

technical field [0001] The invention relates to a preparation method of an electrode material, in particular to a preparation method of a nitrogen-sulfur-doped carbon-coated iron carbide composite electrode material. Background technique [0002] More than 20 years ago, lithium-ion batteries opened a new chapter in energy storage [Science.1994, 264, 1115], and were widely used in portable electronic devices, electric vehicles and other energy devices, and have always been a research hotspot in academia and industry [Chem . Rev., 2004, 104, 4271]. Iron carbide (Fe 3 C) It has abundant reserves, low price, and can catalyze and promote the reversible formation / decomposition of solid electrolyte interface (SEI) film, thereby improving the electrochemical performance of lithium-ion batteries. However, when iron carbide is used as an electrode material, the repeated intercalation and extraction of lithium ions will cause a large volume change in the material during charge and di...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/36H01M4/587H01M4/62H01M10/0525B82Y30/00
CPCY02E60/10
Inventor 沈培康陈海军马旭东
Owner GUANGXI UNIV
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