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Carboxyl carbon, titanate and doped titanium lithium phosphate three-component surface modified iron fluoride cathode material and preparation method thereof

A carbon titanate, lithium titanium phosphate technology, applied in battery electrodes, electrochemical generators, electrical components and other directions, to achieve the effect of improving ionic conductivity and electronic conductivity, and improving electrochemical performance

Active Publication Date: 2014-01-01
沛县度创科技发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] In view of the existing background technology, the present invention proposes a three-component surface-modified ferric fluoride positive electrode material and a preparation method of carboxyl carbon titanate doped titanium lithium phosphate

Method used

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  • Carboxyl carbon, titanate and doped titanium lithium phosphate three-component surface modified iron fluoride cathode material and preparation method thereof

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Experimental program
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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 in 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 the 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. Dissolve 5 g of glucose in 30 mL of distilled water and add 5% acrylic acid by weight, stir evenly, pour into a polytetrafluoroethylene substrate hydrothermal reaction kettle, keep the temperature at 180°C for 17 hours, open the reaction kettle, and wash twice with ethanol , placed in a 90°C oven and dried for 5 hours to obtain carboxyl carbon; 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...

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 in 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 the ball milling, the pressure is 80Pa at 75°C Dry in a vacuum oven for 8 hours, take it out and re-grind it in an agate mortar for 25 minutes. The ground powder is heated to 900°C at a rate of 25°C / min and kept 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. Dissolve 20g of glucose in 45mL of distilled water and add 9% by weight of acrylic acid, stir evenly, pour into a polytetrafluoroethylene substrate hydrothermal reaction kettle, keep the temperature at 205°C for 23 hours, open the reaction kettle, and wash with ethanol for 5 times , placed in a 120°C oven and dried for 10 hours to obtain carboxyl carbon; FeCl 3 ·6H 2 O and ammonium fluoride (1.0:3.6 molar ratio) with 13% by weight Li 1.3 al ...

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 in 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 the ball milling, the pressure is 60Pa at 70°C Dry 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. Dissolve 12g of glucose in 40mL of distilled water and add 7% acrylic acid by weight, stir evenly and pour into a polytetrafluoroethylene substrate hydrothermal reaction kettle, keep the temperature at 190°C for 20 hours, open the reaction kettle, and wash with ethanol 4 times , placed in a 105°C oven and dried for 7 hours to obtain carboxyl carbon; the Fe 2 (SO 4 ) 3 9H 2 O and ammonium fluoride (molar ratio 1.0:3.5) with 7% by weight Li ...

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Abstract

The invention discloses a carboxyl carbon, titanate and doped titanium lithium phosphate three-component surface modified iron fluoride cathode material and a preparation method thereof. The preparation method is characterized by comprising the following steps: ball-milling carboxyl carbon, titanate and silicon / aluminum-doped titanium lithium phosphate Li1.3Al0.1Ti1.9Si0.2P2.8O12 as well as a synthetic raw material in a high-energy ball mill for a period of time, and carrying out heat treatment to obtain the FeF3 cathode material. Carboxyl carbon coordinates with FeF3 iron ions through carboxyl to form firm bonding; carboxyl carbon is a good electron conductor and is helpful for forming a complete conductive link; Li1.3Al0.1Ti1.9Si0.2P2.8O12 is a good lithium ion conductor; a complete lithium ion conductive link is formed for guaranteeing Li1.3Al0.1Ti1.9Si0.2P2.8O12 to be closely contacted with the FeF3 material through lone pair electrons; the electron conductor-carboxyl carbon and the lithium ion conductor-Li1.3Al0.1Ti1.9Si0.2P2.8O12 are bonded on the FeF3 particle surface by coordinating and bonding reactive groups-fluorine ions of titanate with titanium ions, hydrolyzing alkoxy into hydroxy and bonding hydroxy with Li1.3Al0.1Ti1.9Si0.2P2.8O12, so that a complete electron and ion conductive link is formed, the ion conductivity and the electron conductivity of the FeF3 material are greatly improved, and 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 the absolute advantages of high volume, 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 becomi...

Claims

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Application Information

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IPC IPC(8): H01M4/58
CPCY02E60/12H01M4/362H01M4/582H01M4/624H01M10/0525Y02E60/10
Inventor 阮洁超水淼徐晓萍郑卫东高珊舒杰冯琳任元龙程亮亮
Owner 沛县度创科技发展有限公司
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