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Preparation method of Li2FeSiO4 cathode material used for controlling Fe3P

A technology of lithium ferrous silicate and cathode material, applied in silicate, alkali metal silicate, battery electrodes, etc., to achieve the effect of simple preparation process, good discharge performance, and voltage increase

Inactive Publication Date: 2010-06-16
FUJIAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Mix the above reactants to get the initial reaction mixture

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Take anhydrous lithium carbonate (Li 2 CO 3 ) 35.1 g, ferrous oxalate (FeC 2 o 4 2H 2 O) 170.5 grams, tetraethyl orthosilicate (C 8 h 12 o 8 Si) 264 grams, phosphorous acid (H 3 PO 3 ) 0.082 grams. Add 4.35 grams of polypropylene, then add 5600ml of deionized water, mix with a ball mill at a speed of 100rpm for 10 minutes, heat in a water bath at 40°C for 10 hours, and then mix with a ball mill at a speed of 100rpm for 3 hours. Medium dry. The dried powder is placed in a nitrogen atmosphere, and pre-sintered at 200° C. for 3 hours to obtain a matrix pre-sintered material. 55ml of the mixed solution of deionized water and methanol (mixing volume ratio 1:0.10) added to the precursor calcined material was ball milled at a speed of 100rpm for 3 hours, and dried in a vacuum at a temperature of 50°C and a pressure of 200Pa. The dried powder is placed in a nitrogen atmosphere and sintered at 550° C. for 3 hours to prepare lithium ferrous silicate containing controll...

Embodiment 2

[0025] Lithium hydroxide (LiOH·H 2 O) 46.2 grams, ferrous sulfate heptahydrate (FeSO 4 ·7H 2 O) 305.8 grams, metasilicate (H 2 SiO 3 )54.7 g, 0.1% phosphorous acid (H 3 PO 3 ) 246000 grams. Add 54.5 grams of polyvinyl alcohol, then add 4080 ml of a mixture of deionized water and ethanol (mixing volume ratio 1:100), mix with a ball mill at a speed of 1000 rpm for 4 hours, heat in a water bath at 90 ° C for 3 hours, and then use a speed of 800 rpm Ball milled and mixed for 12 hours, and dried in a vacuum at a temperature of 120° C. and a pressure of 10132 Pa. The dried powder is placed in a carbon monoxide atmosphere, pre-sintered at 500° C. for 12 hours, and cooled to room temperature to prepare a matrix pre-sintered material. Add 4206ml of a mixture of deionized water and ethanol (mixing volume ratio 1:0.50) to the pre-calcined matrix, ball mill at a speed of 900rpm for 12 hours, and dry in a vacuum at a temperature of 120°C and a pressure of 10132Pa. The dried powder ...

Embodiment 3

[0027] Take lithium acetate dihydrate (CH 3 COOLi·2H 2 O) 96.9 grams, ferrous chloride tetrahydrate (FeCl 2 4H 2 O) 218.8 grams, nano silicon dioxide (SiO 2 ) 48.1 grams, 90% phosphorous acid (H 3 PO 3 ) 18.2 grams. Add 26.6 g of glucose, and then add 3769 mL of a mixture of deionized water and acetone (mixing volume ratio 1:10), mix by ball milling at 200 rpm for 4 hours, and heat in a water bath at 60° C. for 4 hours. Then, it was mixed by ball milling at a speed of 500 rpm for 10 hours, and dried in a vacuum at a temperature of 100° C. and a pressure of 100 Pa. The dried powder is placed in an atmosphere of a mixture of hydrogen and nitrogen (volume ratio 1:100), pre-sintered at 400° C. for 10 hours, and cooled to room temperature to prepare a matrix pre-sintered material. Add 2090 ml of a mixture of deionized water and acetone (mixing volume ratio 1:1) to the matrix calcined material, ball mill at a speed of 500 rpm for 10 hours, and dry under vacuum at a temperatur...

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Abstract

The invention relates to a preparation method of Li2FeSiO4 cathode material used for controlling Fe3P. The technical scheme comprises the following steps: weighting lithium salt or hydrate of lithium salt, ferrous salt or hydrate of ferrous salt, silicon compound and phosphorous acid or aqueous solution of phosphorous acid according to a molar ratio of the reactants that Li<+>:Fe<2+>:Si:H3PO3=0.95-1.10:0.95-1.10:0.70-0.999:0.001-0.429, mixing the reactants, then adding carbon-containing compound which accounts for 1wt%-20wt% of anhydrous reactants and wet grinding medium which accounts for 0.10-10 times of anhydrous reactants by volume, mixing with a ball mill, heating with water bath, mixing with a ball mill again, heating and drying in vacuum, and then using the two-stage sintering process or temperature programmed two-stage sintering process to prepare Li2FeSiO4 with controllable Fe3P under inert atmosphere or weak reduction atmosphere. The material prepared by the method of the invention has better discharge performance, the discharge capacity is significantly increased in 2.9V zone and the cycle performance is good under 0.3C current.

Description

technical field [0001] The invention belongs to the technical field of lithium ion battery electrode materials, and relates to a preparation method of a lithium ferrous silicate positive electrode material that can be used for lithium ion batteries, lithium batteries, polymer lithium ion batteries and supercapacitors. technical background [0002] Lithium-ion batteries are widely used in mobile communications, notebook computers, portable electric tools, and are also the preferred power source for electric vehicles. The main factor affecting the performance and price ratio of lithium-ion batteries is its cathode material. Since 2000, Armand et al. [patent US 6085015] applied for a patent for the preparation of lithium ferrous silicate and Nytén et al. [Nyten A, et al., Electrochem.Commun., 2005, 7 (2): 156-160.] reported silicon Since the orthorhombic structure of lithium ferrous acid, the research of lithium ferrous silicate has attracted attention. Lithium ferrous silica...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/32H01M4/58
CPCY02E60/12Y02E60/10
Inventor 童庆松陈梅蓉黄行康常美娟黄维静吴阳李秀华
Owner FUJIAN NORMAL UNIV
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