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Carbon solid acid and aluminic acid ester doped ferric fluoride anode material with titanium-phosphate-lithium three-component surface modification, and preparation method of anode material

A technology of acid aluminate and lithium titanium phosphate, applied in battery electrodes, electrochemical generators, electrical components, etc., can solve the problems of high reaction activation energy, high conversion reaction, high voltage difference, etc., to improve ion conductivity and electronic conductivity, strong activity, and the effect of improving electrochemical performance

Inactive Publication Date: 2014-03-26
NINGBO UNIV
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AI Technical Summary

Problems solved by technology

However, the attachment of carbon materials on the surface of positive electrode material particles mainly depends on physical adsorption, and it is difficult to form a complete carbon conductive link.
Secondly, the higher capacity of the material needs to be released at a higher temperature (50-70°C). The main reason is that the activation energy of the conversion reaction in the second stage is very high, and a higher temperature is required to overcome the activation energy and have Faster reaction speed, in addition, the voltage difference between the charge platform and discharge platform of the material is very high, which is also a manifestation of high reaction activation energy and poor reaction reversibility
Finally, because FeF 3 The material is slightly soluble in cold water, so it is usually prepared by the ethanol liquid phase method, which requires a large amount of ethanol during the synthesis process, which is not economical
Not suitable for industrial applications

Method used

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  • Carbon solid acid and aluminic acid ester doped ferric fluoride anode material with titanium-phosphate-lithium three-component surface modification, and preparation method of anode material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Embodiment 1: Al 2 o 3 : SiO 2 : TiO 2 : NH 4 h 2 PO 4 : Li 2 CO 3 Mix evenly at a ratio of 0.05:0.2:1.9:2.8:0.65 (molar ratio), add 3.5% of 95% ethanol, and ball mill in a ball mill at a speed of 110 rpm for 12 hours. After ball milling, the pressure is 15Pa at 65°C Dry in a vacuum oven for 2.5 hours, take it out and re-grind it in an agate mortar for 15 minutes. The ground powder is heated to 650°C at a rate of 6°C / min and kept for 6 hours to make Li 1.3 Al 0.1 Ti 1.9 Si 0.2 P 2.8 o 12 Solid electrolyte powder. Place 5g of glucose in an oven at 90°C to dry for 5 hours, then carbonize at a constant temperature of 700°C in a muffle furnace for 6 hours, place it in a crucible after cooling, add 12mL of concentrated sulfuric acid and sulfonate it in an oven at 150°C for 1 hour to obtain carbon solid acid; the Fe(NO 3 ) 3 9H 2 O and ammonium fluoride (1.0:3.1 molar ratio) with 3.2% by weight Li 1.3 Al 0.1 Ti 1.9 Si 0.2 P 2.8 o 12 Solid electrolyte po...

Embodiment 2

[0020] Embodiment 2: Al 2 o 3 : SiO 2 : TiO 2 : NH 4 h 2 PO 4 : Li 2 CO 3 Mix evenly at a ratio of 0.05:0.2:1.9:2.8:0.65 (molar ratio), add 8% of 95% ethanol, and ball mill in a ball mill at a speed of 450 rpm for 45 hours. After ball milling, the pressure is 80Pa at 75°C Dry it in a vacuum oven for 8 hours, take it out and re-grind it in an agate mortar for 25 minutes, and heat the ground powder to 900°C at a rate of 25°C / min for 15 hours to make Li 1.3 Al 0.1 Ti 1.9 Si 0.2 P 2.8 o 12 Solid electrolyte powder. Place 20g of glucose in an oven at 120°C to dry for 10 hours, then carbonize at a constant temperature of 900°C in a muffle furnace for 10 hours, place it in a crucible after cooling, add 15mL of concentrated sulfuric acid, and sulfonate it in an oven at 190°C for 5 hours to obtain carbon Solid acid; FeCl 3 ·6H 2 O and ammonium fluoride (1.0:3.6 molar ratio) with 13% by weight Li 1.3 Al 0.1 Ti 1.9 Si 0.2 P 2.8 o 12 Solid electrolyte powder, 15% by ...

Embodiment 3

[0021] Embodiment 3: Al 2 o 3 : SiO 2 : TiO 2 : NH 4 h 2 PO 4 : Li 2 CO 3 Mix evenly at a ratio of 0.05:0.2:1.9:2.8:0.65 (molar ratio), add 5% of 95% ethanol, and ball mill in a ball mill at a speed of 200 rpm for 25 hours. After ball milling, the pressure is 60Pa at 70°C Dry it in a vacuum oven for 7 hours, take it out and re-grind it in an agate mortar for 20 minutes. The ground powder is heated to 750°C at a rate of 20°C / min and kept for 12 hours to make Li 1.3 Al 0.1 Ti 1.9 Si 0.2 P 2.8 o 12 Solid electrolyte powder. Place 10g of glucose in an oven at 100°C to dry for 7 hours, then carbonize at a constant temperature of 800°C in a muffle furnace for 7 hours, place it in a crucible after cooling, add 12mL of concentrated sulfuric acid, and sulfonate it in an oven at 170°C for 3 hours to obtain carbon solid acid; the Fe 2 (SO 4 ) 3 9H 2 O and ammonium fluoride (molar ratio 1.0:3.5) with 7% by weight Li 1.3 Al 0.1 Ti 1.9 Si 0.2 P 2.8 o 12 Solid electro...

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Abstract

The invention provides a preparation method of carbon solid acid and aluminic acid ester doped ferric fluoride anode material with titanium-phosphate-lithium three-component surface modification. The preparation method comprises the following steps: ball-milling sulfonated carbon solid acid, aluminic acid ester and titanium-phosphate-lithium doped with silicon and aluminum Li[1.3]A1[0.1]Ti[1.9]Si[0.2]P[2.8]O[12] and synthetic raw materials in a high-energy ball mill for a period of time and carrying out heat treatment. The preparation method is characterized in that sulfonated solid acid is coordinated through iron ions to form an integrated electron conduction link; reactive group alkoxy of an aluminic acid ester coupling reagent is adopted to rapidly hydrolyze into hydroxyl to be combined with the ionic conductive agent Li[1.3]A[10.1]Ti[1.9]Si[0.2]P[2.8]O[12] and combined with a sulfo group on the sulfonated carbon solid acid in a condensation manner at the same time, so as to combine the conductive agent sulfonated carbon solid acid and the ionic conductive agent Li[1.3]A[10.1]Ti[1.9]Si[0.2]P[2.8]O[12] on the surfaces of FeF3 particles, so that an electron and ionic conduction circuit is formed, the ionic conductivity and the electronic conductivity of the FeF3 material are improved greatly, and thus the electrochemical performance of the material is improved.

Description

technical field [0001] The invention relates to the technical field of a method for manufacturing a high-capacity lithium iron fluoride cathode material. Background technique [0002] Lithium-ion secondary batteries have absolute advantages such as high volume, high weight-to-energy ratio, high voltage, low self-discharge rate, no memory effect, long cycle life, and high power density. Currently, the global mobile power market has an annual share of more than 30 billion US dollars and Gradually grow at a rate of more than 10%. Especially in recent years, with the gradual depletion of fossil energy, new energy sources such as solar energy, wind energy, and biomass energy have gradually become alternatives to traditional energy sources. Among them, wind energy and solar energy are intermittent, and a large amount of energy is used simultaneously to meet the needs of continuous power supply. Energy storage batteries; urban air quality problems caused by automobile exhaust are ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/36H01M4/58H01M4/62
CPCH01M4/366H01M4/58H01M4/624H01M10/0525Y02E60/10
Inventor 冯琳水淼徐晓萍郑卫东高珊舒杰任元龙程亮亮
Owner NINGBO UNIV
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