Preparation method of boron-nitrogen dual-ingredient self-doping three-dimensional drape graphene electrode material

A graphene electrode and self-doping technology, which is applied in graphene, battery electrodes, chemical instruments and methods, etc., can solve the problems of harsh reaction equipment and reaction conditions, difficult doping methods and types, and cumbersome preparation process steps. Achieve the effects of easy realization of reaction conditions, easy control of doping amount and type, and simple reaction equipment

Inactive Publication Date: 2017-03-08
GUANGXI UNIV
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  • Abstract
  • Description
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Problems solved by technology

[0005] The present invention provides a simple and feasible method for solving the problems in the preparation method of boron-nitrogen binary doped graphene, such as harsh reaction equipment and reaction conditions, cumbersome preparation process steps, large environmental pollution, and difficult control of doping methods and types. Method for preparing boron-nitrogen binary self-doped three-dimensional wrinkled graphene with aminoborane compound and using it as electrode material

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  • Preparation method of boron-nitrogen dual-ingredient self-doping three-dimensional drape graphene electrode material
  • Preparation method of boron-nitrogen dual-ingredient self-doping three-dimensional drape graphene electrode material
  • Preparation method of boron-nitrogen dual-ingredient self-doping three-dimensional drape graphene electrode material

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Embodiment 1

[0028] A method for preparing a boron-nitrogen binary self-doped three-dimensional wrinkled graphene electrode material, the operation steps are as follows:

[0029] (1) Mix 0.2 mol of borane-tert-butylamine complex with 0.1 mol of catalyst metal salt cobalt chloride, dissolve in 60 ml of ethanol, keep the temperature below 90° C., heat and stir until dry powder is obtained;

[0030] (2) heat-treating the dry powder obtained in step (1) at a temperature of 1000° C. for 1 hour in nitrogen, and then cooling to room temperature; wherein, the nitrogen gas introduced is to ensure that the heat treatment process is in an oxygen-free state;

[0031] (3) Add the substance obtained after cooling in step (2) to 500mL 3mol / L hydrochloric acid solution, heat and stir at 50°C for 8 hours, filter, wash the filter residue with deionized water until neutral, dry at 80°C for 24h, remove the residue in the filter residue Moisture, that is, boron and nitrogen binary self-doped three-dimensional ...

Embodiment 2

[0033] A method for preparing a boron-nitrogen binary self-doped three-dimensional wrinkled graphene electrode material, the operation steps are as follows:

[0034] (1) Mix 0.3 mol of trimethylamine-borane complex and 0.1 mol of catalyst metal salt cobalt sulfate, and dissolve in 60 ml of methanol, keep the temperature below 90°C and heat and stir until dry powder is obtained;

[0035] (2) Keeping the dry powder obtained in step (1) at a temperature of 800°C in argon for heat treatment for 3.5 hours, and then cooling to room temperature; wherein, the argon gas introduced is to ensure that the heat treatment process is an oxygen-free state;

[0036] (3) Add the substance obtained after cooling in step (2) to 500mL 3mol / L nitric acid solution, heat and stir at 35°C for 12 hours, filter, wash the filter residue with deionized water until neutral, dry at 80°C for 24 hours, remove the filter residue internal moisture, that is, boron and nitrogen binary self-doped three-dimensional...

Embodiment 3

[0038] A method for preparing a boron-nitrogen binary self-doped three-dimensional wrinkled graphene electrode material, the operation steps are as follows:

[0039] (1) 0.03mol trimethylamine-borane complex, 0.04mol dimethylaminoborane and 0.03mol borane ammonium complex with 0.01mol catalyst metal salt cobalt nitrate, 0.01mol acetic acid Cobalt, 0.02mol of ferric chloride, 0.01mol of ferric sulfate, 0.015mol of ferric oxalate, 0.025mol of ferric acetate, and 0.01mol of ferrous chloride were mixed and dissolved in 60ml of methanol and ethanol mixture (methanol+ethanol, volume Mixing ratio of 1:1), keep the temperature below 90°C, heat and stir until dry powder is obtained;

[0040] (2) Keeping the dry powder obtained in step (1) at a temperature of 1200° C. for heat treatment for 0.5 hours in hydrogen, and then cooling to room temperature; wherein, the hydrogen gas introduced is to ensure that the heat treatment process is in an oxygen-free state;

[0041] (3) Add the substa...

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Abstract

The invention discloses a preparation method of a boron-nitrogen dual-ingredient self-doping three-dimensional drape graphene electrode material. The method comprises the following operation steps: (1) an amino boron hydride compound and catalyst metal salt are mixed, and are dissolved in a solvent; heating and stirring are performed until dry powder is obtained; (2) heat treatment is performed in inert gas; then, the powder is cooled to room temperature; (3) an acid solution is added; heating, stirring and filtering are performed; filter residue is cleaned to a neutral state; drying is performed to obtain boron-nitrogen dual-ingredient self-doping three-dimensional drape graphene. The preparation method has the advantages that the steps are fewer; reaction equipment is simple; the reaction conditions are easily realized; the graphene doping amount and type can be easily controlled; the cost is low; the large-scale preparation is easy; the prepared boron-nitrogen dual-ingredient self-doping three-dimensional drape graphene has high activity and good stability, and shows good electrochemical performance in lithium ion battery negative electrodes and fuel oxygen reduction catalysts; huge economic benefits and values are realized.

Description

technical field [0001] The invention relates to the fields of graphene, lithium-ion batteries and fuel cells, in particular to a method for preparing a boron-nitrogen binary self-doped three-dimensional wrinkled graphene electrode material Background technique [0002] Graphene, a carbon atomic layer structure composed of a layer of honeycomb six-membered rings closely connected, has been used in fuel cells, lithium-ion batteries, The potential application value of supercapacitors has been highly valued by countries all over the world [Chem.Soc.Rev.2010,39,4146; EnergEnviron Sci.2011,4,668]. However, the surface of graphene is inert, and the lithium ion storage capacity and electrocatalytic activity of pure graphene are often unsatisfactory [Chem.Soc.Rev.2014,43,7067; Acs Catal.2015,5,5207]. Doping graphene with nitrogen atoms and boron atoms can effectively increase the lithium ion storage active sites and oxygen reduction catalytic active sites, improve the conductivity o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/184H01M4/587H01M4/90
CPCC01B2204/22C01P2004/03C01P2004/04C01P2004/80H01M4/587H01M4/9083Y02E60/10Y02E60/50
Inventor 朱金良沈培康黄士志潘智毅张伶俐
Owner GUANGXI UNIV
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