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Method for covering lithium iron phosphate conducting layer by use of radio frequency plasma enhanced chemical vapor deposition

A technology of radio frequency plasma and lithium iron phosphate, applied in electrochemical generators, circuits, electrical components, etc., can solve the problems of long time, high energy consumption, high heat treatment temperature of the coated metal conductive layer, etc., and achieve short reaction time, The effect of low reaction temperature and good crystal structure development

Active Publication Date: 2014-07-30
SIHUI DABOWEN IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The heat treatment temperature of the general pyrolysis method to coat the metal conductive layer is high, the time is long, and the energy consumption is large.

Method used

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  • Method for covering lithium iron phosphate conducting layer by use of radio frequency plasma enhanced chemical vapor deposition
  • Method for covering lithium iron phosphate conducting layer by use of radio frequency plasma enhanced chemical vapor deposition
  • Method for covering lithium iron phosphate conducting layer by use of radio frequency plasma enhanced chemical vapor deposition

Examples

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Effect test

Embodiment 1

[0020] Weigh ferrous phosphate, lithium hydroxide, and phosphoric acid according to the molar ratio Li:Fe:P=1:1:1, dissolve them in an appropriate amount of deionized water, and transfer them to a polytetrafluoroethylene hydrothermal reaction tank, and seal them. Put the reaction tank in a blast drying oven, and conduct a hydrothermal reaction at 160°C for 48 hours under the blast state. After natural cooling, use deionized water to wash repeatedly by centrifugation, and vacuum-dry the separated powder at 80°C for 10 hours. Obtain lithium iron phosphate. The prepared sample LiFePO 4 Placed in Shenyang Xinlantian Plasma Enhanced Chemical Vapor Deposition System. Vacuum down to 1×10 -1 Pa. Filled with SiH 4 +H 2 (SiH 4 :H 2 =1:9 volume ratio) gas, the flow rate is controlled at 40sccm, and the total pressure of the reaction chamber is maintained at 10Pa. The output power of the RF plasma power supply is 200W. The reaction time was controlled at 30min. After the reactio...

Embodiment 2

[0022] Weigh ferrous phosphate, lithium acetate, and phosphoric acid according to the molar ratio Li:Fe:P=1:1:1, dissolve them with appropriate amount of deionized water, and transfer them to a polytetrafluoroethylene hydrothermal reaction tank, and seal them. Place the reaction tank in a blast drying oven, and conduct a hydrothermal reaction at 180°C for 24 hours under the blast state. After natural cooling, use deionized water to repeatedly centrifuge and clean, and vacuum-dry the separated powder at 80°C for 5 hours. Obtain lithium iron phosphate. The prepared sample LiFePO 4 Placed in Shenyang Xinlantian Plasma Enhanced Chemical Vapor Deposition System. Vacuum down to 1×10 -1 Pa. charge GeH 4 +Ar(GeH 4 :Ar=1:20 volume ratio) gas, the flow rate is controlled at 100sccm, and the total pressure of the reaction chamber is maintained at 200Pa. The output power of the RF plasma power supply is 100W. The reaction time was controlled at 60min. After the reaction is complet...

Embodiment 3

[0024] Weigh ferrous sulfate, lithium chloride, and ammonium dihydrogen phosphate according to the molar ratio Li:Fe:P=1:1:1, dissolve them in appropriate amount of deionized water, and transfer them to a polytetrafluoroethylene hydrothermal reaction tank, seal . Place the reaction tank in a blast drying oven, and conduct a hydrothermal reaction at 200°C for 18 hours under the blast state. After natural cooling, use deionized water to wash repeatedly by centrifugation, and vacuum-dry the separated powder at 80°C for 15 hours. Obtain lithium iron phosphate. The prepared sample LiFePO 4 Placed in Shenyang Xinlantian Plasma Enhanced Chemical Vapor Deposition System. Vacuum down to 1×10 -1 Pa. Charge BH 3 +N 2 (BH 3 :N 2 =1:15 volume ratio) gas, the flow rate is controlled at 70sccm, and the total pressure of the reaction chamber is maintained at 500Pa. The output power of the RF plasma power supply is 60W. The reaction time was controlled at 90min. After the reaction i...

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Abstract

The invention discloses a method for covering a lithium iron phosphate conducting layer by use of radio frequency plasma enhanced chemical vapor deposition. The method comprises the following steps: putting lithium iron phosphate in a reaction chamber and performing a reaction on the lithium iron phosphate for 10-20 minutes in the presence of radio frequency plasmas in a diluted reactant gas, wherein the total pressure of the reaction chamber is kept in a range of 10-1000Pa, the electrical output power of the radio frequency plasmas is in the range of 60-400W, the diluted reactant gas is formed by mixing a diluent gas and a reactant gas in a volume ratio of (5-20):1, the reactant gas is one or mixed gases of any two of silane, SiH3Cl, SiH2Cl2, borane, germane and phosphorane, and the diluent gas is any one of hydrogen, nitrogen, helium, neon, argon, krypton and xenon; therefore, the conducting layer covered lithium iron phosphate is obtained. Compared with conventional chemical vapor deposition, the method has the advantages of high reactivity, low reaction temperature and short reaction time.

Description

Technical field: [0001] The invention belongs to the technical field of preparation technology of positive electrode materials of lithium ion batteries, and in particular relates to a method for realizing the coating of lithium iron phosphate conductive layer by radio frequency plasma enhanced chemical vapor deposition. Background technique: [0002] The demand for lithium-ion batteries in modern society has increased rapidly, especially electric vehicles have put forward higher requirements for lithium-ion batteries. Cathode materials have always been the bottleneck restricting the development of lithium-ion batteries. To develop lithium-ion batteries with high safety, high energy density, high power, long cycle life, environmental protection and low price, we must first develop environmentally friendly, rich raw material resources, comprehensive Cathode material with excellent electrochemical performance. Lithium iron phosphate (LiFePO 4 ) is a third-generation lithium-i...

Claims

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Application Information

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IPC IPC(8): H01M4/58
CPCH01M4/366H01M4/5825H01M10/0525Y02E60/10
Inventor 闵德刘丽英陈彦伟
Owner SIHUI DABOWEN IND CO LTD
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