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Method for preparing ferrous silicate lithium/carbon composite positive pole material with micropore spherical structure

A technology of lithium ferrous silicate and positive electrode materials, which is applied in the direction of structural parts, battery electrodes, electrical components, etc., can solve the problems of low electronic conductivity and poor diffusion performance, and achieve uniform grain distribution, high rate performance, good The effect of cycle performance

Active Publication Date: 2015-02-18
HUNAN UNIV OF ARTS & SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to improve Li 2 FeSiO 4 Low electronic conductivity, poor diffusion performance, etc., the present invention proposes a method for preparing lithium ferrous silicate / carbon composite positive electrode material with microporous spherical structure, in order to improve its specific capacity under high rate conditions

Method used

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  • Method for preparing ferrous silicate lithium/carbon composite positive pole material with micropore spherical structure
  • Method for preparing ferrous silicate lithium/carbon composite positive pole material with micropore spherical structure
  • Method for preparing ferrous silicate lithium/carbon composite positive pole material with micropore spherical structure

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preparation example Construction

[0020] 1) Preparation of gel: Switching citric acid and lithium hydroxide to add water and stir dissolved; add iron oxalic acid metal iron, adjust the solution pH to 7-8, 80-95 ° C, the oil bath is insulated for 24-72hSoluble; add nano -silica, ultrasonic 20-60min, stir at room temperature for 1 to 3h to make gel.Among them, lithium hydroxide, iron and nano -nano -sanxia silicon Murbi is measured by li: Fe: Si = 2: 1: 1; the proportion of citric acid and iron oxalic acid metal acid is: 0.9 ~ 1.7.

[0021] 2) Dry: Step 1) The gel is sprayed to dry at 100-120 ° C to get a siliconic metal iron / carbon composite front drive body.

[0022] 3) High -temperature cracking: Step 2) The lithium silicate lithium Iron / carbon composite front -drive body is heat -treated in the atmosphere of the atmosphere to the reaction to complete.Among them, the thermal treatment was baked for 8-12 hours at 600 to 800 ° C.

Embodiment 1

[0023] Example 1 li 2 Feesio 4 / C compound positive material preparation

[0024] Illects 0.052mol citric acid and 0.08mol lithium hydroxide add 500ml of water, and the magnetic force is dissolved; add 0.04 mol oxalic acid sub -iron, regulate the pH of the solution to 7-8, and the oil bath is formed by the oil bath at 90 ° C to form a dark green solution; add0.04mol nano -nano -sanxide, ultrasonic 20min, stirred 1h at 25 ° C to make gel; spray the gel at 108 ° C to get a lithium silicon / carbon composite front drive;The composite front -wheel drive is treated at 700 ° C for 10h in the atmosphere.Through element analysis and testing, LI 2 Feesio 4 The content of carbon in the composite positive material is about 14.6%.See figure 1 , Scan the electronic microscope map, see figure 2 As well as image 3 Essence

Embodiment 2

[0025] Example 2 li 2 Feesio 4 / C compound positive material preparation

[0026]Talking about 0.06mol citric acid and 0.08mol lithium hydroxide add 500ml of water, and the magnetic mixing is dissolved; add 0.04 mol oxalic acid sub -iron, regulate the pH of the solution to 7-8, and the oil bath is formed after 36h at 90 ° C; add the dark green solution; add0.04mol nano -nano -sanxide, ultrasonic 20min, stirred 1h at 25 ° C to make gel; spray the gel at 108 ° C to get a lithium silicon / carbon composite front drive;The composite front -wheel drive is treated at 700 ° C for 10h in the atmosphere.Through element analysis and testing, LI obtained 2 Feesio 4 The content of carbon in the composite positive material is about 16.7%.See figure 1 , Scan the electronic microscope map, see figure 2 As well as image 3 Essence

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Abstract

The invention discloses a method for preparing a ferrous silicate lithium / carbon composite positive pole material with a micropore spherical structure. The method particularly comprises the following steps of (1) adding citric acid and lithium hydroxide into water, and stirring for dissolution; adding ferrous oxalate, regulating the pH of a solution to 6-8, carrying out oil bath at 80-95 DEG C, and keeping temperature for 24-72 hours to form a deep green solution; adding nanometer silicon dioxide, carrying out ultrasonography for 20-60 minutes, and stirring at room temperature for 1-3 hours to prepare gel; (2) spray-drying the gel at 100-120 DEG C to obtain a ferrous silicate lithium / carbon composite precursor; (3) calcining the ferrous silicate lithium / carbon composite precursor in argon at 600-800 DEG C for 8-12 hours to obtain the ferrous silicate lithium / carbon composite positive pole material with the micropore spherical structure. The method disclosed by the invention is simple and safe in process and low in cost. The obtained ferrous silicate lithium / carbon composite positive pole material has the advantages of fine granules, uniformity in distribution, excellent microstructure and preferable electrochemical property.

Description

Technical field [0001] The present invention involves the field of lithium -ion battery manufacturing technology, especially a method of siliconicate iconic / carbon composite positive materials that prepare a microporous ball structure. Background technique [0002] Based on the aspects of resources, environmental protection and safety performance, new lithium -ion battery positive materials with low development costs, high safety and environment -friendly are the focus of people's research.Since the first report 4 Since then, the Iron Facin ionic compound has received great attention as potential lithium ion batteries.Li 2 Feesio 4 It is also attractive to have the characteristics of rich minerals, good structural stability, and good environmental compatibility.And under specific conditions, a higher actual ratio (340 mAH G-1) can be obtained, so the material is considered to be one of the potential lithium-ion batteries.However, li 2 Feesio 4 Low electronic conductivity (10 -14 ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/36
CPCH01M4/364H01M4/5825Y02E60/10
Inventor 黄小兵张园梦任杰王云周诗彪陈远道刘北平
Owner HUNAN UNIV OF ARTS & SCI
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