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A kind of carbon solid acid titanate doped lithium titanium phosphate three-component surface-modified iron fluoride cathode material and preparation method

A technology of acid titanate and lithium titanium phosphate, which is applied in the field of high-capacity lithium iron fluoride cathode material manufacturing to achieve the effect of improving electrochemical performance, increasing ionic conductivity and electronic conductivity

Active Publication Date: 2016-08-17
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 carbon solid acid titanate doped lithium titanium phosphate

Method used

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  • A kind of carbon solid acid titanate doped lithium titanium phosphate three-component surface-modified iron fluoride cathode material and preparation method

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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 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 10mL 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 The solid electroly...

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 discloses a carbon solid acid, 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 carbon solid acid, 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. Sulfonated carbon solid acid coordinates with FeF3 iron ions through sulfonic acid groups to form firm bonding; sulfonated carbon solid acid 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-sulfonated carbon solid acid 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 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 Patents(China)
IPC IPC(8): H01M4/36H01M4/58H01M4/62
CPCH01M4/362H01M4/582H01M4/624H01M10/0525Y02E60/10
Inventor 汪卓彬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