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Preparation method of ferrous silicate lithium doped anode material

A technology for lithium ferrous silicate and positive electrode materials, applied in the direction of silicate, alkali metal silicate, battery electrodes, etc., can solve problems such as poor discharge performance, achieve low raw material cost, simple preparation process, and good discharge performance Effect

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

[0006] As a result of the Li prepared by the above method 2 FeSiO 4 The discharge performance at a lower rate is still poor. In recent years, attempts have been made to further improve the electrochemical performance of lithium ferrous silicate by doping.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Weigh lithium carbonate (Li 2 CO 3 ) 70g, ferrous oxalate dihydrate (FeC 2 o 4 2H 2 O) 170g, silicon dioxide (SiO 2 )60g, sodium phosphite monohydrate (NaH 2 PO 3 ·H 2 O) 0.15g, add 2.67g polypropylene. Then add 38mL of deionized water, mix it with a ball mill at a speed of 100 rpm for 20 minutes, heat it in a water bath at 45°C for 1 hour, and then mix it with a ball mill at a speed of 100 rpm for 3 hours. dry conditions. The dried powder is placed in a nitrogen atmosphere, pre-sintered at 200° C. for 3 hours, and cooled to room temperature to prepare a matrix pre-sintered material. Add 48mL of propanol to the precursor calcined material, ball mill for 3 hours at a speed of 100 rpm, and dry in a vacuum at a temperature of 55°C and a pressure of 20Pa. The dried powder was placed in a nitrogen atmosphere and sintered at 550° C. for 3 hours to prepare doped lithium ferrous silicate. The electrode material has good discharge performance, the discharge capacity i...

Embodiment 2

[0025] Lithium hydroxide monohydrate (LiOH·H 2 O) 46g, ferrous acetate tetrahydrate ((CH 3 COO) 2 Fe·4H 2 O) 270g, tetramethyl orthosilicate (Si(OCH 3 ) 4 ) 122g, magnesium phosphite (Mg(H 2 PO 3 ) 2 ) 18.6g, add 3.6g sucrose. Then add 5164mL of ethanol, mix with ball mill at 100 rpm for 3 hours, heat in water bath at 95°C for 1 hour, then ball mill with 1000 rpm for 3 hours, and dry in vacuum at temperature 135°C and pressure 10132Pa . 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 precursor pre-sintered material. Put 5164mL of propanol in the matrix calcined material, ball mill it at 1000 rpm for 12 hours, and dry it in a vacuum at a temperature of 135°C and a pressure of 100Pa. The dried powder is placed in a carbon monoxide atmosphere and sintered at 850° C. for 24 hours to prepare doped lithium ferrous silicate. The electrode material has good discharge performance, t...

Embodiment 3

[0027] Weigh lithium acetate (CH 3 COOLi) 63g, ferrous sulfate heptahydrate (FeSO 4 ·7H 2 O) 306g, hexamethyldisilazane ((CH 3 ) 3 SiNHSi(CH 3 ) 3 ) 145g, cobalt phosphite monohydrate (Co(H 2 PO 3 ) 3 ·H 2 (2) 45.8g, add 125g flour, add the mixed solution (volume ratio 1: 100) of 3885mL deionized water and acetone again, mix 3 hours with the rotating speed ball mill of 500 rev / mins, heat 12 hours in the water bath of 85 ℃, Then, it was ball milled at a speed of 500 rpm for 10 hours, and then dried in a vacuum at a temperature of 125° C. and a pressure of 500 Pa. The dried powder is placed in a carbon dioxide atmosphere, heated from room temperature to 200 °C at a heating rate of 0.5 °C / min, held for 3 hours for pre-sintering, and cooled to room temperature to prepare the matrix pre-sintered material. Add 78mL of deionized water to the matrix calcined material, perform ball milling at a speed of 100 rpm for 3 hours, and dry in a vacuum at a temperature of 55°C and a p...

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Abstract

The invention discloses a preparation method of a ferrous silicate lithium doped anode material. The preparation method comprises the following steps of: weighing lithium salt, ferrous silicate salt, a silicon compound and phosphate according to the mole ratio being (0.95-1.10):(0.95-1.10):(0.80-0.999):(0.001-0.286) of lithium ions to ferrous silicate ions to silicon atoms to phosphorous acid radical ions in an initial reactant and mixing the compounds to obtain an initial reaction mixture; adding a carbon-containing compound which is 1-30 percent of the weight of an anhydrous state compound of the initial reaction mixture and a wet milling medium which is 0.10-10 times of the volume of the anhydrous state compound; ball milling and mixing and heating in a water bath; ball mixing and mixing gain; finally drying; placing the dried powder in an inert atmosphere or a weakly reducing atmosphere; and preparing doped ferrous silicate lithium by adopting a two-stage sintering method or a two stage program temperature-rising sintering method. The electrode material has better discharge performance; the discharge capacity of the prepared sample in a 3.0V zone is remarkably increased; and the prepared sample has excellent circulating performance under the current of 0.3C multiplying power, which lays a sound foundation for the industry.

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 doped 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, and portable electric tools. The main factor affecting the performance and price ratio of lithium-ion batteries is its cathode material. Since Armand et al. [patent US6085015] applied for a patent for the preparation of lithium ferrous silicate in 2000, Nytén et al. [Nyten A, et al., Electrochem.Commun., 2005, 7 (2): 156-160.] reported silicon Since the phase structure of lithium ferrous acid, the research of lithium ferrous silicate has attracted attention. Lithium ferrous silicate positive electrode material has the advantages of wide sour...

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李变云吴阳李秀华
Owner FUJIAN NORMAL UNIV
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