Preparation method and application of cubic molybdenum nitride

A technology of molybdenum nitride and body shape is applied in the preparation of cube-shaped molybdenum nitride and the application field of negative electrode materials of lithium ion batteries, which can solve the problems of high oxygen content in products, unsuitable molybdenum nitride, long preparation period, etc. Achieve uniform particle size, low equipment requirements, and good crystal morphology

Active Publication Date: 2021-08-31
HUBEI ENG UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

These methods in the preparation of Mo 2 There are many shortcomings in N negative electrode materials: such as long preparation period, complicated process, and the use of NH 3 problem, and the product has a high oxygen content
However, it is difficult to synthesize bulk molybdenum nitride by conventional methods. The pressure of this preparation method reaches 4-5GPa, and the conditions are harsh, and the prepared molybdenum nitride is not suitable for application in lithium-ion battery anode materials.

Method used

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  • Preparation method and application of cubic molybdenum nitride
  • Preparation method and application of cubic molybdenum nitride
  • Preparation method and application of cubic molybdenum nitride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] A cubic Mo2 The preparation method of N, its step is as follows:

[0036] 0.5g of ammonium molybdate tetrahydrate, 10g urea and 0.6g melamine are added respectively in the ethanol solution prepared by 24g dehydrated alcohol and 10g distilled water and stirred evenly to obtain respectively the ethanol solution of ammonium molybdate tetrahydrate, the ethanol solution of urea and The ethanol solution of melamine, then the three bottles of solutions were mixed, and the mixed solution was obtained after stirring for 12 hours; the obtained mixed solution was aged at room temperature for 24 hours to form a sol; the obtained product was freeze-dried to form a solid, and then the obtained solid was placed in the air Pre-calcined at 300°C for 2h under the condition, then heat-treated at 400°C for 0.5h, and cooled to room temperature to obtain the precursor powder. The obtained powder was calcined at 700 °C for 2 h under nitrogen atmosphere, and cooled to room temperature to obtai...

Embodiment 2

[0038] A cubic Mo 2 The preparation method of N, its step is as follows:

[0039] The tetrahydrate ammonium molybdate of 0.7g, 10g urea and 0.45g melamine are added respectively in the ethanol solution prepared by 24g dehydrated alcohol and 10g distilled water and stir, obtain the ethanol solution of tetrahydrate ammonium molybdate, the ethanol solution of urea and The ethanol solution of melamine, then the three bottles of solutions were mixed, and the mixed solution was obtained after stirring for 12 hours; the obtained mixed solution was aged at room temperature for 24 hours to form a sol; the obtained product was freeze-dried to form a solid, and then the obtained solid was placed in the air Pre-calcined at 300°C for 2h under the condition, then heat-treated at 400°C for 0.5h, and cooled to room temperature to obtain the precursor powder. The obtained powder was calcined at 800 °C for 2 h under a nitrogen atmosphere, and cooled to room temperature to obtain Mo 2 N electr...

Embodiment 3

[0041] A cubic Mo 2 The preparation method of N, its step is as follows:

[0042] 0.9g of ammonium molybdate tetrahydrate, 10g urea and 0.45g melamine are added respectively in the ethanol solution prepared by 24g dehydrated alcohol and 10g distilled water and stirred evenly, obtain the ethanol solution of ammonium molybdate tetrahydrate, the ethanol solution of urea and The ethanol solution of melamine, then the three bottles of solutions were mixed, and the mixed solution was obtained after stirring for 12 hours; the obtained mixed solution was aged at room temperature for 36 hours to form a sol; the obtained product was freeze-dried to form a solid, and then the obtained solid was placed in the air Pre-calcined at 300°C for 2h under the condition, then heat-treated at 400°C for 0.5h, and cooled to room temperature to obtain the precursor powder. The obtained powder was calcined at 900 °C for 2 h under nitrogen atmosphere, and cooled to room temperature to obtain Mo 2 N el...

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Abstract

The invention discloses a preparation method and application of cubic molybdenum nitride, and belongs to the field of lithium ion battery electrode materials. The preparation method comprises the following steps: S1, mixing an ethanol solution of urea, an ethanol solution of melamine and an ethanol solution of ammonium molybdate tetrahydrate, and stirring to obtain a mixed solution, wherein the mass ratio of ammonium molybdate tetrahydrate to urea to melamine in the mixed solution is (5-11): 100: (3-6); S2, aging the mixed solution at room temperature to form sol/gel, and freeze-drying to form a solid; S3, pre-sintering the obtained solid, and then carrying out heat treatment to obtain precursor powder; and S4, roasting the obtained precursor powder in a nitrogen atmosphere, and cooling to room temperature to obtain the molybdenum nitride electrode material. The nanoscale molybdenum nitride powder product is obtained through a simple process, has a cubic structure, is small in grain size and uniform in granularity, and has excellent cycle performance and relatively high specific capacity when being used as a lithium ion battery negative electrode material.

Description

technical field [0001] The invention relates to the technical field of preparation of lithium-ion battery electrode materials, in particular to a preparation method of cubic molybdenum nitride and its application in lithium-ion battery negative electrode materials. Background technique [0002] Among the key materials for manufacturing lithium-ion batteries, negative electrode materials are an important factor in determining their performance and price. At present, the commercialized negative electrode materials are mainly graphite-based carbon materials, but the theoretical capacity of graphite-based carbon materials is only 372mAh / g. At the same time, it is prone to lithium precipitation during high-current charging and discharging, resulting in poor safety and limiting the use of lithium-ion batteries. develop. So now more and more people are studying some transition metal compounds to replace graphite electrode materials. Molybdenum nitride (Mo 2 N) has the advantages...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/06H01M4/58H01M10/0525
CPCC01B21/062H01M4/58H01M10/0525H01M2004/021H01M2004/027C01P2002/72C01P2004/04C01P2006/40C01P2004/38C01P2004/52Y02E60/10
Inventor 付争兵杜逸轩杨雄杜军丁瑜余佳阁
Owner HUBEI ENG UNIV
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