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Surface modified ferric fluoride cathode material containing three components, such as carbon-based solid acid, aluminium zirconium coupling agent and doped titanium lithium phosphate, and preparation method thereof

An acid aluminum zirconate, lithium titanium phosphate technology, applied in battery electrodes, electrical components, circuits, etc., to achieve the effect of improving ionic conductivity and electronic conductivity, and improving electrochemical performance

Active Publication Date: 2014-04-02
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 aluminum zirconate doped lithium titanium phosphate

Method used

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  • Surface modified ferric fluoride cathode material containing three components, such as carbon-based solid acid, aluminium zirconium coupling agent and doped titanium lithium phosphate, and preparation method thereof

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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 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 for 12 hours at a speed of 110 rpm in a ball mill. After the ball mill finishes, 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 wt% Li 1.3 Al 0.1 Ti 1.9 Si 0.2 P 2.8 o 12 Solid electro...

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 for 45 hours at a speed of 450 rpm in a ball mill. After the ball mill finishes, 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. 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 in molar ratio) with 13% by weight Li 1.3 Al 0.1 Ti 1.9 Si 0.2 P 2.8 o 12 Solid elec...

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% 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 0 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 (1.0:3.5 molar ratio) with 7 wt% Li 1.3 Al 0.1 Ti 1.9 Si 0.2 P 2.8 o 12 Solid electrolyte p...

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Abstract

The invention provides a preparation method of surface modified ferric fluoride cathode material containing three components, such as carbon-based solid acid, aluminium zirconium coupling agent and doped titanium lithium phosphate. The preparation method is as follows: sulfonated carbon-based solid acid, aluminium zirconium coupling agent, silicon and aluminium doped titanium lithium phosphate Li1.3A10.1Ti1.9Si0.2P2.8O12 and synthetic raw materials are added into a bowl mill for ball milling for a period of time and are subjected to heat treatment. Electronic good conductor sulfonated carbon-based solid acid is coordinated with FeF3 iron ion by sulfonic group, and firm combination is good for forming a complete electronic conductive link; many alkyloxy of the aluminium zirconium bimetallic coupling agent with many active point locations are hydrolyzed into hydroxyl, thereby the aluminium zirconium bimetallic coupling agent is bonded with lithium ion good conductor Li1.3A10.1Ti1.9Si0.2P2.8O12 and is bonded with sulfonic group in sulfonated carbon-based solid acid by polycondensation; simultaneously zirconium is an electron acceptor, and can coordinate with fluorinion in the surface of the FeF3 particles, so the electron conductive agent sulfonated carbon-based solid acid and the lithium ion conductive agent Li1.3A10.1Ti1.9Si0.2P2.8O12 are bonded in the surface of the FeF3 particle, and a complete electron and ion conductive link is formed, thereby improving ion conductivity and electron conductivity of FeF3 material, and improving electrochemistry performance of the material.

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): H01M4/36H01M4/58H01M4/62
CPCH01M4/582H01M4/624Y02E60/10
Inventor 程亮亮水淼徐晓萍郑卫东高珊舒杰冯琳任元龙
Owner 沛县度创科技发展有限公司
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