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Method for synthesizing lithium iron phosphate by ultrasonic spray solid-phase sintering

A technology of lithium ferrous phosphate and solid phase sintering method, which is applied to chemical instruments and methods, phosphorus compounds, structural parts, etc., to achieve the effects of improving processing performance and electrochemical performance, uniform particle size distribution, and high reactivity

Active Publication Date: 2013-03-27
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to overcome the shortcomings of the existing high-temperature solid-phase sintering method, and provide a method for synthesizing lithium ferrous phosphate by ultrasonic spray-solid-phase sintering method, so as to achieve uniform particle size distribution and effectively improve the cycle performance of the battery And rate performance and tap density, the processing performance is significantly improved

Method used

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  • Method for synthesizing lithium iron phosphate by ultrasonic spray solid-phase sintering
  • Method for synthesizing lithium iron phosphate by ultrasonic spray solid-phase sintering
  • Method for synthesizing lithium iron phosphate by ultrasonic spray solid-phase sintering

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Embodiment 1

[0024] (1) Weigh 166.85 g of ferrous sulfate heptahydrate and 52.810 g of diammonium hydrogen phosphate, respectively dissolve them in 1.0 L of deionized water, stir to dissolve them; mix ferrous sulfate solution and diammonium hydrogen phosphate solution At the same time, add it into a reactor with an ultrasonic device at a rate of 800 mL / h, control the reaction temperature at 80 °C, and react for 1 h at a stirring speed of 800 r / min to obtain a gray-white ferrous phosphate suspension; Then add 20.80g of lithium dihydrogen phosphate, 14.80g of lithium carbonate, 6.04g of glucose, 90.05g of oxalic acid, 0.2g of titanium oxide and 0.2g of manganese acetate tetrahydrate, and spray-dry during intensive stirring and mixing, with a feed rate of 800 mL / h, the dry air inlet temperature is 220°C, and the air outlet temperature is 120°C to obtain the lithium iron phosphate precursor, and then pretreat at 300°C for 4h under the protection of a high-purity nitrogen atmosphere; take 90g o...

Embodiment 2

[0027] (2) Weigh 172.82 g of ferrous nitrate hexahydrate and 59.60 g of ammonium phosphate, respectively dissolve them in 12.0L of deionized water, and add ferrous nitrate solution and ammonium phosphate solution at the same time at a rate of 1000 mL / h Into a reactor equipped with an ultrasonic device, control the reaction temperature to 50 °C, and react for 0.5 h under the condition of a stirring speed of 400 r / min to obtain a suspension close to white ferrous phosphate; then add 23.20 g of lithium phosphate, 6.28 g sucrose, 15.0 g acetylene black, 5.0 g acetic acid, 0.3 g niobium oxide and 0.1 g cobalt acetate tetrahydrate were spray-dried in the process of intensive stirring and mixing, and the feed rate was 1200 mL / h, and the drying inlet air temperature was 150°C, the air outlet temperature is 100°C, to obtain the complex precursor of lithium iron phosphate containing composite carbon sources and composite metal elements, and then pretreat at 200°C for 2 hours under the pr...

Embodiment 3

[0030] (3) Weigh 104.40 g of ferrous acetate and 46.0 g of ammonium dihydrogen phosphate, and dissolve them in 0.3 L of deionized water respectively. Speed ​​into the reactor with an ultrasonic device, control the reaction temperature at 90 °C, and react for 8 h under the condition of a stirring speed of 1200 r / min to obtain a suspension of gray ferrous phosphate; then add 23.00 g of dihydrogen phosphate Ammonium, 30.60 g lithium oxalate, 10.0 g malic acid, 10.0 g graphite, 10.0 g phenolic resin, 0.2 g magnesium oxide, and 0.2 g aluminum oxide; spray-dried during intensive mixing with a feed rate of 400 mL / h , the dry air inlet temperature is 250°C, and the air outlet temperature is 150°C to obtain the precursor of lithium iron phosphate, and then pretreat at 400°C for 8 hours under the protection of a high-purity nitrogen atmosphere; take 90g of pretreated ferrous phosphate Lithium sample, add 25.0g malic acid and 35.0g phenolic resin to the sample, through high-speed mechani...

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Abstract

The invention relates to a method for synthesizing lithium iron phosphate by ultrasonic spray solid-phase sintering, mechanically activating a water solution, in which the chemical stoichiometric ratio of ferrous ions to phosphate ions is 3:2, at 50-90 DEG C at the rate of 400-1200 rpm under the ultrasonic action for 0.5-8 hours; adding a lithium source compound, a phosphorus source compound, a composite carbon source and a composite metal compound; carrying out ultrasonic spray drying in the reinforced stirring and mixing process; in a protective atmosphere, pretreating the lithium iron phosphate precursor at 200-400 DEG C for 2-8 hours; adding the carbon source, which accounts for 5-40 wt% of the lithium iron phosphate precursor; and carrying out mechanical ball milling, and roasting toobtain the lithium iron phosphate. The lithium iron phosphate provided by the invention has the advantages of uniform particle size distribution and high reaction activity (remaining 98.42% after 200circulations); the 1C discharge is 97.3% of 0.1C discharge; the tap density is 1.42g / cm<3>; the specific area is reduced to 10.0m<2> / g; and thus, the lithium iron phosphate greatly enhances the processability and electrochemical properties of the product.

Description

technical field [0001] The invention relates to a method for preparing lithium iron phosphate by an ultrasonic spray solid-phase sintering method. Background technique [0002] LiFePO 4 It is a new type of cathode material for lithium-ion batteries. It has excellent charge and discharge platform, good cycle performance, low price, high theoretical capacity, and environmental friendliness. It is considered to be the most promising cathode material for lithium-ion batteries and is expected to be used in lithium-ion batteries On electric vehicles, its prospects are immeasurable. The preparation of lithium iron phosphate cathode material can be simply divided into solid-phase method and liquid-phase method. The existing solid phase methods mainly include high temperature solid phase sintering method and carbothermal reduction method. Among them, the high-temperature solid-phase sintering method is to use ferrous iron as a raw material and make finished products through sint...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/45H01M4/58
CPCY02E60/12Y02E60/10
Inventor 张宝张佳峰彭春丽
Owner CENT SOUTH UNIV
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