Preparation method of spinel-type spherical high-entropy oxide material for lithium ion battery anode material

A technology for lithium-ion batteries and negative electrode materials, applied in the field of 3O4 high-entropy oxide materials and their preparation, to achieve the effects of high efficiency, mild reaction, and simple process

Active Publication Date: 2018-12-04
衢州市衢发瑞新能源材料有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is to design a novel lithium-ion battery negative electrode material, a kind of (CoCrCuFeNi) with spinel crystal structure and spherical shape 3 o 4 High-entropy oxide material; at the same time overcome the shortcomings of the prior art preparation, provide a preparation method of high-entropy oxide powder material with low energy consumption, high production efficiency, green environmental protection, and no complicated post-processing of the product

Method used

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  • Preparation method of spinel-type spherical high-entropy oxide material for lithium ion battery anode material
  • Preparation method of spinel-type spherical high-entropy oxide material for lithium ion battery anode material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Weigh an equimolar amount of 11.90g of CoCl 2 ·6H 2 O, 13.32g of CrCl 3 ·6H 2 O, 7.95g of CuCl 2 2H 2 O, 13.52 g of FeCl 3 ·6H 2 O and 11.89 g of NiCl 2 ·6H 2 O five kinds of metal salts, dissolve them in 250mL distilled water, mix well and use as oxidation solution; weigh 20.4g of NaOH and dissolve in 1700mLH 2 After adding 26.35g of sodium thiosulfate and 0.14g of surfactant polyvinylpyrrolidone in O, mix well and use it as a reducing solution; drop the above oxidation solution into the reducing solution at a speed of 15mL / min, and Magnetic stirring at a reaction temperature of ℃, continued stirring for 30 minutes after the dropwise addition, aging for 30 minutes, centrifuged and calcined in a muffle furnace at 300 ℃ to obtain the final product. XRD spectrum ( figure 1 ) shows that the prepared (CoCrCuFeNi) 3 o 4 The high-entropy oxide material is a spinel structure, and the SEM picture ( figure 2 ) shows that the prepared (CoCrCuFeNi) 3 o 4 The averag...

Embodiment 2

[0023] Weigh 43.66g of Co(NO 3 ) 2 ·6H 2 O, 60.18g of Cr(NO 3 ) 3 9H 2 O, 36.24g of Cu(NO 3 ) 2 ·3H 2 O, 60.6g of Fe(NO 3 ) 3 9H 2 O and 43.62g of Ni(NO 3 ) 2 ·6H 2 O five kinds of metal salts, dissolve them in 250mL distilled water, mix well and use as oxidation solution; weigh 75g of NaOH and dissolve in 2500mLH 2 After adding 28.37g of sodium borohydride and 1.78g of surfactant polyethylene glycol, mix well and use it as a reducing solution; drop the above oxidation solution into the reducing solution at a speed of 30mL / min, and in 20 Magnetic stirring at the reaction temperature of ℃, continue to stir for 40 minutes after the dropwise addition and age for 60 minutes, and then calcined in a muffle furnace at 500 ℃ after centrifugation to obtain a spherical (CoCrCuFeNi) with a spinel structure and an average particle size of 110 nm. 3 o 4 High entropy oxide materials.

Embodiment 3

[0025] Weigh an equimolar amount of 11.24g of CoSO 4 ·7H 2 O, 6.60g of Cr(OH)SO 4 , 9.99g of CuSO 4 ·5H 2 O, 11.12g of FeSO 4 ·7H 2 O and 10.51 g NiSO 4 ·6H 2O five kinds of metal salts, dissolve them in 200mL distilled water, mix well and use as oxidation solution; weigh 16g of NaOH and dissolve in 320mLH 2 After adding 6.05g of sodium borohydride and 1.03g of surfactant sorbitol, mix well and use it as a reducing solution; add the above-mentioned oxidizing solution to the reducing solution dropwise at a speed of 10mL / min, and heat Stir magnetically at the reaction temperature, continue to stir for 60 minutes after the dropwise addition, and age for 40 minutes. After centrifugation, it is calcined in a muffle furnace at 400 ° C to obtain a spherical (CoCrCuFeNi) with a spinel structure and an average particle size of 75 nm. 3 o 4 High entropy oxide materials.

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Abstract

The invention discloses a preparation method of a spinel-type spherical high-entropy oxide material for a lithium ion battery anode material and belongs to the field of lithium ion battery anode materials. The preparation method integrates chemical reduction and low temperature thermal treatment and particularly includes: with chlorides, sulfates, nitrates, carbonates, acetates and oxalates of cobalt, chromium, copper, iron and nickel being metal sources and sodium borohydride and sodium hydrosulfite being reducing agents, calcining the products, subjected to a redox reaction, in a device at 300-500 DEG C to obtain the target product. Through liquid-phase burdening, it is guaranteed that the raw materials are blended at molecular level, thus achieving stoichiometric ratio of the product; meanwhile, the method is simple in process, is gentle in reactions, is short in time and high in efficiency, and has no special demands on calcining equipment. The high-entropy oxide powder is high inpurity, is small in particle size and has high initial discharge capacity and great cycle performance.

Description

technical field [0001] The invention belongs to the field of negative electrode materials for lithium ion batteries, in particular to a (CoCrCuFeNi) with a spinel crystal structure and a spherical shape 3 o 4 High-entropy oxide materials and methods for their preparation. Background technique [0002] Lithium-ion battery is the latest generation battery after nickel-chromium and nickel-metal hydride batteries. It is light in weight, small in size, high in energy density, good in cycle performance and low in self-discharge rate. Widely favored in new energy vehicles and other fields. A key to the successful application of lithium-ion batteries is the negative electrode intercalation and deintercalation of lithium compounds. Therefore, as one of the four major components of lithium batteries, negative electrode materials play an important role in improving the capacity and cycle performance of batteries, and their performance directly affects the performance of lithium-ion ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/36H01M4/48H01M4/52H01M10/0525
CPCH01M4/364H01M4/483H01M4/523H01M10/0525Y02E60/10
Inventor 冒爱琴权峰王飘飘俞海云郑翠红林娜
Owner 衢州市衢发瑞新能源材料有限公司
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