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Production method of lithium secondary battery drop water ferric fluoride anode material

A technology for lithium secondary batteries and positive electrode materials, applied in electrode manufacturing, battery electrodes, fluoride preparation, etc., can solve the problems of time and energy consumption, product shape dependence, high consumables, etc., and achieve uniform distribution and regular surface morphology , the effect of high yield

Inactive Publication Date: 2009-07-22
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this kind of reaction is time-consuming and energy-consuming, and the consumption of materials is high, and the shape of the obtained product depends on the original form of the iron compound material powder

Method used

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  • Production method of lithium secondary battery drop water ferric fluoride anode material
  • Production method of lithium secondary battery drop water ferric fluoride anode material
  • Production method of lithium secondary battery drop water ferric fluoride anode material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Weigh FeCl at a molar ratio of 1:4 3 and about 25g of ammonia water, mix the two materials evenly in an aqueous solution at room temperature, filter with suction to obtain a ferric-alkaline mixture, add 40% hydrofluoric acid to the ferric-alkaline mixture at a molar ratio of 1:4, and put it into a special airtight plastic container Insulated at 50°C for 40 hours to make it evenly mixed. Then remove the excess product from the reaction, wash the remaining material with ethanol and dry it in the air atmosphere for 24 hours, then vacuum-dry the material at 50°C for 36 hours; take out the product, crush it and ball mill it to 5-10 μm in a ball mill , through a 300-mesh sieve to obtain FeF with a purity greater than 95% 3 (H 2 O) 0.33 product.

Embodiment 2

[0027] Weigh Fe at a molar ratio of 1:8.5 2 (SO 4 ) 3 and about 25g of sodium hydroxide, the two materials are mixed uniformly in aqueous solution at normal temperature, and the water generated is removed by suction filtration to obtain a ferric-alkali mixture, which is added with 10% hydrofluoric acid in a molar ratio of 1:7, and put Put it into a special airtight plastic container and keep it warm at 75°C for 30 hours to make it mix evenly. Then the excess product of the reaction was removed, and the remaining material was washed with ethanol and dried in an air atmosphere for 30 hours, and then the material was vacuum-dried at 90° C. for 64 hours; the product was taken out, pulverized and ball-milled in a ball mill to 5 ~10μm, through 200 mesh sieve, get FeF with purity greater than 95% 3 (H 2 O) 0.33 product.

Embodiment 3

[0029] Weigh FeNO at a molar ratio of 1:6 3and about 25g of KOH, the two materials are uniformly mixed in an aqueous solution at normal temperature, and the generated water is removed by suction filtration to obtain a ferric-alkaline mixture. The ferric-alkaline mixture is added with 30% hydrofluoric acid in a molar ratio of 1:9, and put into In a special airtight plastic container, keep warm at 90°C for 36 hours to make it evenly mixed. Then the excess product of the reaction was removed, and the remaining material was washed with ethanol and dried in an air atmosphere for 10 hours, and then the material was vacuum-dried at 190°C for 24 hours; the product was taken out, crushed and ball-milled in a ball mill to 5 ~10μm, through 400 mesh sieve, get FeF with purity greater than 95% 3 (H 2 O) 0.33 product.

[0030] figure 1 FeF prepared for the present invention 3 (H 2 O) 0.33 The X-ray Diffraction Spectrum. It can be seen from the figure that the prepared FeF 3 (H 2 ...

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Abstract

The invention discloses a preparation method for lithium secondary battery micro water ferric fluoride anode materials, wherein, firstly, teracidic malysite and alkali are uniformly mixed in an aqueous solution under normal temperature in proportion from 1 to 1 - 1 to 10; water is removed after sucking filtration; iron-alkali mixture is obtained after drying for 1 to 48 hours; secondly, the iron-alkali mixture and 5 to 40 percent hydrofluoric acids are uniformly reacted in a plastic sealed container in proportion from 1 to 1 - 1 to 10, and heat preservation is performed for 1 to 48 hours under the temperature of 40 to 100 DEG C; thirdly, mixture is filtered, cleaned by utilization of ethanol and dried for 1 to 36 hours in the air; fourthly, the mixture is dried for 1 to 72 hours under vacuum state of 50 to 250 DEG C; fifthly, the mixture is crushed in a ball mill and passes through a 100 to 400 mesh sieve, and then a ferric fluoride product is obtained. The invention has the advantages that: firstly, systematic temperature is automatically controlled, and technological parameters are determined through precise calculation on the basis; secondly, yield of the method is high and product purity is larger than 95 percent. Obtained FeF3 (H2O) 0.33 has an integrated orthorhombic system structure, regular surface topography, small grain diameter and uniform distribution, and good discharge performance. The method is a novel and practical technological line for preparation of the FeF3 (H2O) 0.33.

Description

technical field [0001] The invention relates to a preparation method of ferric fluoride. Background technique [0002] The energy problem is a common problem faced by mankind in the 21st century. Electric energy is the most convenient form of energy. In order to store electric energy and meet the needs of the rapid development of the electronics industry and the development of electric vehicles, various types of batteries have emerged as the times require. Lithium secondary batteries are favored by the world for their excellent characteristics such as high reversible capacity, high voltage, high cycle performance, and high energy density. They are known as the leading power source in the 21st century, and their application fields continue to expand. However, the competition in the lithium secondary battery industry is very fierce. Finding new electrode materials with high performance and low cost is a powerful means to further reduce battery costs and enhance competitiveness...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/04H01M4/58C01B9/08
CPCY02E60/10
Inventor 王先友伍文王欣胡涛曹俊琪
Owner XIANGTAN UNIV
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