Preparation method of spinel-type porous high entropy oxide material

A spinel-type, oxide-based technology, applied in chemical instruments and methods, nanotechnology for materials and surface science, nickel compounds, etc., to achieve low energy consumption and low production costs

Active Publication Date: 2018-11-16
ANHUI UNIVERSITY OF TECHNOLOGY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The technical problem to be solved by the present invention is to overcome the deficiencies of the prior art, such as the preparation of high-entropy oxide powder materials by mechanical alloying method and pyrolysis spraying method, and provide a kind of energy s

Method used

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  • Preparation method of spinel-type porous high entropy oxide material
  • Preparation method of spinel-type porous high entropy oxide material
  • Preparation method of spinel-type porous high entropy oxide material

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Experimental program
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Effect test

Embodiment 1

[0025] Weigh 14.55g of Co(NO 3 ) 2 ·6H 2 O, 20.008g of Cr(NO 3 ) 3 9H 2 O, 20.2g of Fe(NO 3 ) 3 9H 2 O, 12.55g of Mn(NO 3 ) 2 4H 2 O and 14.54g of Ni(NO 3 ) 2 ·6H 2O was dissolved in 50mL of distilled water and stirred evenly to obtain a mixed solution containing metal salts; then 48.03g of citric acid and 0.72g of ammonium nitrate were weighed and added to the above mixed solution, after stirring evenly, the pH of the mixed solution was adjusted to 8 with ammonia water to obtain a transparent Then heat the above transparent sol in an oil bath at 150°C to remove the solvent water to obtain a loose, foamy gel; finally place the above gel in a muffle furnace at 300°C for 30 minutes to obtain the final product . XRD spectrum ( figure 1 ) shows that the prepared (CoCrFeMnNi) 3 o 4 The high-entropy oxide material is a spinel structure, and the SEM picture ( figure 2 ) shows that the prepared (CoCrFeMnNi) 3 o 4 The average particle size of the high-entropy oxide...

Embodiment 2

[0027] Weigh 29.01g of Co(NO 3 ) 2 ·6H 2 O, 40.02g of Cr(NO 3 ) 3 9H 2 O, 40.4g of Fe(NO 3 ) 3 9H 2 O, 25.10g of Mn(NO 3 ) 2 4H 2 O and 29.08g of Ni(NO 3 ) 2 ·6H 2 O was dissolved in a solvent composed of 42.5mL of distilled water and 7.5mL of ethanol, and stirred evenly to obtain a mixed solution containing metal salts; Adjust the pH of the mixed solution to 6 to obtain a transparent sol; then heat the above transparent sol in an oil bath at 120°C to remove solvent water and obtain a loose, foamy gel; finally place the above gel on the input power React in a microwave oven of 700W for 10 minutes to obtain the final product. SEM image ( image 3 ) shows that the prepared (CoCrFeMnNi) 3 o 4 The average particle size of the high-entropy oxide material is 90nm, the morphology is spherical and has a porous structure.

Embodiment 3

[0029] Weigh 21.83g of Co(NO 3 ) 2 ·6H 2 O, 30.01g of Cr(NO 3 ) 3 9H 2 O, 30.3g of Fe(NO 3 ) 3 9H 2 O, 18.83g of Mn(NO 3 ) 2 4H 2 O and 21.81g of Ni(NO 3 ) 2 ·6H 2 O was dissolved in 42.5mL of ethanol and 7.5mL of distilled water, and stirred evenly to obtain a mixed solution containing metal salts; then 101.34g of glucose and 3.04g of ammonium acetate were weighed and added to the above mixed solution, and after stirring evenly, the pH of the mixed solution was adjusted with ammonia water to 7. Obtain a transparent sol; then heat the above transparent sol in a water bath at 80°C to remove the solvent water to obtain a loose, foamy gel; finally place the above gel in a muffle furnace at 500°C for 10 minutes, A spherical spinel type (CoCrFeMnNi) with an average particle size of 130nm was obtained 3 o 4 High entropy oxide powder material.

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Abstract

Belonging to the field of inorganic oxide powder materials, the invention discloses a preparation method of a spinel-type porous high entropy oxide material. The method is low temperature combustion synthesis method. Specifically, a metal nitrate is adopted as the metal source, one of or a mixture of several of citric acid, ethylenediamine tetraacetic acid, hexamethylenetetramine and glucose is adopted as the fuel, by controlling the concentration of the metal salt raw materials, the fuel type and adding amount, the combustion improver type and adding amount, and the ignition way, the granularity, morphology and other characteristics of the spinel-type transition metal high entropy oxide (CoCrFeMnNi)3O4 nanopowder can be regulated. The preparation method adopts liquid phase compounding toensure molecular level uniform mixing of the raw materials, and the product achieves stoichiometric ratio. At the same time, the method has the advantages of energy saving, high production efficiency,green and environmental protection, no need for complicated post-treatment and the like. The high entropy oxide powder prepared by the method provided by the invention has high purity and uniform particle size distribution.

Description

technical field [0001] The invention belongs to the field of inorganic oxide powder materials, and in particular relates to a preparation method of a high-entropy oxide material for a negative electrode material of a lithium ion battery, specifically having spinel-type porous (CoCrFeMnNi) 3 o 4 Preparation methods of high-entropy oxide materials. Background technique [0002] Due to its light weight, small size, high energy density, and good cycle performance, lithium-ion batteries are widely favored by portable electronic products such as mobile phones, notebook computers, and new energy vehicles. Lithium-ion battery anode materials play an important role in improving battery capacity and cycle performance, and their performance directly affects the performance of lithium-ion batteries. The current commercial lithium-ion battery anode material is generally graphite-based carbon anode material, but its theoretical specific capacity is only 372mAhg -1 And it is not conduci...

Claims

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Application Information

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IPC IPC(8): C01G53/00B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00C01G53/00C01P2002/32C01P2002/72C01P2004/03C01P2004/32C01P2004/62C01P2004/64
Inventor 冒爱琴项厚政林娜俞海云郑翠红闫勇
Owner ANHUI UNIVERSITY OF TECHNOLOGY
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