PVDF/li1.3al0.3ti1.7(po4)3 solid dual-phase electrolyte film material and preparation method

A technology of electrolyte film and film material, which is applied in the field of solid dual-phase electrolyte film and its manufacturing, can solve the problems of high cost, long process flow, and complicated operation, and achieve the effects of enhanced retention capacity, simple synthesis process, and low reaction temperature

Inactive Publication Date: 2011-12-28
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the plasticization / extraction method can improve the microporous structure of the polymer membrane, and the ionic conductivity of the electrolyte can also meet the requirements of battery applications, but this method has problems such as long process flow, complicated operation, and high cost.

Method used

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  • PVDF/li1.3al0.3ti1.7(po4)3 solid dual-phase electrolyte film material and preparation method
  • PVDF/li1.3al0.3ti1.7(po4)3 solid dual-phase electrolyte film material and preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Li(CH 3 COO)·2H 2 O and Al(NO 3 ) 3 9H 2 O is added to ethylene glycol methyl ether, and after it is completely dissolved, add PO(OC 4 h 9 ) 3 , and then add Ti(OC 4 h 9 ) 4 And keep stirring, Li(CH 3 COO)·2H 2 O, Al(NO 3 ) 3 9H 2 O, Ti(OC 4 h 9 ) 4 , PO(OC 4 h 9 ) 3 According to the ratio of the amount of substances added, the ratio of the amount of the substance is 1.35:0.3:1.7:3, the obtained solution is heated at a constant temperature of 140°C for 4 hours to form a gel, and the dry gel is calcined in the air at 850°C for 4 hours, and after cooling in the furnace Ball milling and sieving to obtain Li with a particle size of less than 2 μm 1.3 al 0.3 Ti 1.7 (PO 4 ) 3 powder.

[0017] Mix and stir PVDF and DMAC to prepare a solution containing 20% ​​PVDF, and use DMAC to dissolve Li 1.3 al 0.3 Ti 1.7 (PO 4 ) 3 Powder dispersion, adjusted to contain 50% Li 1.3 al 0.3 Ti 1.7 (PO 4 ) 3 slurry, then press Li 1.3 al 0.3 Ti 1.7 (PO 4 )...

Embodiment 2

[0020] Li(CH 3 COO)·2H 2 O and Al(NO 3 ) 3 9H 2 O is added to ethylene glycol methyl ether, and after it is completely dissolved, add PO(OC 4 h 9 ) 3 , and then add Ti(OC 4 h 9 ) 4 And keep stirring, Li(CH 3 COO)·2H 2 O, Al(NO 3 ) 3 9H 2 O, Ti(OC 4 h 9 ) 4 , PO(OC 4 h 9 ) 3 According to the ratio of the amount of substances added, it is 1.50:0.3:1.7:3, and the obtained solution is heated at a constant temperature of 120°C for 4 hours to form a gel, and the dry gel is calcined in the air at 810°C for 6 hours. Ball milling and sieving to obtain Li with a particle size of less than 2 μm 1.3 al 0.3 Ti 1.7 (PO 4 ) 3 powder.

[0021] Mix and stir PVDF and DMAC to prepare a solution containing 10% PVDF, and use DMAC to dissolve Li 1.3 al 0.3 Ti 1.7 (PO 4 ) 3 Powder dispersion, adjusted to contain 50% Li 1.3 al 0.3 Ti 1.7 (PO 4 ) 3 slurry, then press Li 1.3 al 0.3 Ti 1.7 (PO 4 ) 3 PVDF-DMAC solution and Li 1.3 al 0.3 Ti 1.7 (PO 4 ) 3 - DMAC...

Embodiment 3

[0024] Li(CH 3 COO)·2H 2 O and Al(NO 3 ) 3 9H 2 O is added to ethylene glycol methyl ether, and after it is completely dissolved, add PO(OC 4 h 9 ) 3 , and then add Ti(OC 4 h 9 ) 4 And keep stirring, Li(CH 3 COO)·2H 2 O, Al(NO 3 ) 3 9H 2 O, Ti(OC 4 h 9 ) 4 , PO(OC 4 h 9 ) 3 According to the ratio of the amount of substances added, it is 1.45:0.3:1.7:3, and the obtained solution is heated at a constant temperature of 140°C for 2 hours to form a gel, and the dry gel is calcined in air at 875°C for 3 hours. Ball milling and sieving to obtain Li with a particle size of less than 2 μm 1.3 al 0.3 Ti 1.7 (PO 4 ) 3 powder.

[0025] Mix and stir PVDF and DMAC to prepare a solution containing 15% PVDF, and use DMAC to dissolve Li 1.3 al 0.3 Ti 1.7 (PO 4 ) 3 Powder dispersion, adjusted to contain 30% Li 1.3 al 0.3 Ti 1.7 (PO 4 ) 3 slurry, then press Li 1.3 al 0.3 Ti 1.7 (PO 4 ) 3 PVDF-DMAC solution and Li 1.3 al 0.3 Ti 1.7 (PO 4 ) 3 - DMAC slu...

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Abstract

The invention relates to a solid-state diphase electrolyte thin-film material and a preparation method thereof, wherein the thin-film material is a composite material of Li1.3 Al0.3 Ti1.7 (PO4) 3 and polyvinylidene fluoride, and the mass ratio of Li1.3 Al0.3 Ti1.7 (PO4) 3 to polyvinylidene fluoride is 0.03-0.1:1. The preparation method comprises the following steps of: synthesizing Li1.3 Al0.3 Ti1.7 (PO4) 3 powder with high ion conductivity from Li (CH3COO).2H2O, Al (NO3) 3.9H2O, PO (OC4H9) 3 and Ti (OC4H9) 4 by a sol-gel method; then respectively mixing the PVDF and the Li1.3 Al0.3 Ti1.7 (PO4) 3 powder with an organic solvent and coating after uniformly stirring; controlling the temperature and volatilizing the solvent to form a thin film, and then drying the thin film in vacuum to obtain the PVDF / Li1.3 Al0.3 Ti1.7 (PO4) 3 diphase electrolyte thin-film material. The PVDF / Li1.3 Al0.3 Ti1.7 (PO4) 3 diphase electrolyte thin-film material has the advantages of good mechanical strength and flexibility, high ion conductivity, good electrochemical properties and easy realization of industrial production.

Description

technical field [0001] The invention relates to a solid two-phase electrolyte film and a manufacturing method thereof, belonging to the field of materials. Background technique [0002] With the increasingly prominent problems of environmental pollution, energy crisis and resource shortage, countries all over the world are paying more and more attention to the development of high-efficiency, clean, renewable energy and electric vehicles and other related technologies. [0003] As a form of energy in chemical power sources, lithium-ion batteries have the advantages of high working voltage, high energy density, light weight, small size, long cycle life, and environmental protection. They are used in mobile electronic appliances, electric tools, large energy storage, and electric transportation Power supply and other aspects have broad application prospects. However, the current liquid lithium-ion batteries contain a large amount of highly flammable liquid organic electrolytes...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L27/16C08K3/32C08J5/18H01M10/058
CPCY02E60/12Y02E60/10Y02P70/50
Inventor 郭华军李新海杨波王志兴彭文杰胡启阳张云河
Owner CENT SOUTH UNIV
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