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Silane doped lithium titanium phosphate two-component surface modified ferric fluoride anode material and preparation method

A technology of lithium titanium phosphate and surface modification, which is applied in the direction of battery electrodes, electrochemical generators, electrical components, etc., can solve the problems of high reaction activation energy, high conversion reaction, poor economy, etc., to overcome the ion conductivity Extremely low, the effect of improving electrochemical performance

Active Publication Date: 2014-01-08
沛县度创科技发展有限公司
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  • Abstract
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  • Application Information

AI Technical Summary

Problems solved by technology

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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  • Silane doped lithium titanium phosphate two-component surface modified ferric fluoride anode material and preparation method

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 in a ratio of 0.05: 0.1: 1.9: 2.9: 0.6 (molar ratio), add 3% of 95% ethanol, and ball mill in a ball mill at a speed of 100 rpm for 10 hours. After the ball milling, the pressure is 10Pa at 60°C Dry in a vacuum oven for 2 hours, take it out and re-grind it in an agate mortar for 10 minutes. The ground powder is heated to 600°C at a rate of 5°C / min and kept for 5 hours to make Li 1.2 Al 0.1 Ti 1.9 Si 0.1 P 2.9 o 12 Solid electrolyte powder. Fe(NO 3 ) 3 9H 2 O and ammonium fluoride (1.0:3.0 molar ratio) with 3 wt% Li 1.2 Al 0.1 Ti 1.9 Si 0.1 P 2.9 o 12 The solid electrolyte powder, 0.5% by weight of Tween-80 and 0.5% by weight of anilinomethyltriethoxysilane were ball-milled at room temperature for 5 hours under the protection of high-purity nitrogen in a high-energy ball mill, and then the materials were taken out. Under the protection of the mixed gas of % hydrogen and 95...

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: 0.1: 1.9: 2.9: 0.6 (molar ratio), add 8% 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 90Pa 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 1.2 Al 0.1 Ti 1.9 Si 0.1 P 2.9 o 12 Solid electrolyte powder. FeCl 3 ·6H 2 O and ammonium fluoride (1.0:3.6 in molar ratio) with 13% by weight Li 1.2 Al 0.1 Ti 1.9 Si 0.1 P 2.9 o 12 Solid electrolyte powder, 2.8% by weight of span-60 and 3.0% by weight of N-β(aminoethyl)-γ-aminopropyltrimethoxysilane were ball milled in a high-energy ball mill under the protection of high-purity nitrogen at room temperature for 20 After 1 hour, the material was taken out, heated to 450 degrees under the protec...

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: 0.1: 1.9: 2.9: 0.6 (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 700°C at a rate of 20°C / min and kept for 12 hours to make Li 1.2 Al 0.1 Ti 1.9 Si 0.1 P 2.9 o 12 Solid electrolyte powder. Will Fe 2 (SO 4 ) 3 9H 2 O and ammonium fluoride (1.0:3.5 molar ratio) with 7 wt% Li 1.2 Al 0.1 Ti 1.9 Si 0.1 P 2.9 o 12 The solid electrolyte powder, the tx-10 with a weight percentage of 2.0% and the hexamethylenediaminomethyltriethoxysilane with a weight percentage of 2.1% were ball milled at room temperature for 15 hours under the protection of high-purity nitrogen in a high-energy ball mill, and then the materials were taken out an...

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Abstract

The invention provides a silane doped lithium titanium phosphate two-component surface modified ferric fluoride anode material and a preparation method. The preparation method is characterized by ball-milling an amino-containing silane coupling agent, silicon and aluminium doped lithium titanium phosphate Li1.2Al0.1Ti1.9Si0.1P2.9O12 and synthetic raw materials in a high energy ball mill for a period of time and carrying out heat treatment, thus obtaining the FeF3 anode material. The anode material and the preparation method have the advantages that FeF3 is stronger Lewis acid and can form coordination with the amino capable of providing lone pair electrons in the silane coupling agent, thus forming strong bonding, and meanwhile, hydroxyl formed by hydrolyzing alkoxy in the silane coupling agent strongly interacts with surface hydroxyll on Li1.2Al0.1Ti1.9Si0.1P2.9O12 and is subjected to polycondensation; therefore under the action of aminosilane, doped lithium titanium phosphate Li1.2Al0.1Ti1.9Si0.1P2.9O12 is bonded on the surfaces of FeF3 anode particles, so that the particles of doped lithium titanium phosphate Li1.2Al0.1Ti1.9Si0.1P2.9O12 and the FeF3 anode form good contact, and Li1.2Al0.1Ti1.9Si0.1P2.9O12 is a good lithium ion conductor and has ionic conductivity 103-104 times that of lithium cobalt oxide; therefore the defect that the ionic conductivity of the FeF3 anode material is extremely low can be overcome and the electrochemical performance of the FeF3 material can be 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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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/36H01M4/58H01M4/62
CPCY02E60/12H01M4/362H01M4/582H01M4/624H01M10/0525Y02E60/10
Inventor 水淼徐晓萍陈姝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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