Aluminum zirconate-doped lithium titanium phosphate two-component surface-modified ferric fluoride positive electrode material and preparation method thereof

A technology of aluminum zirconate and surface modification, which is applied in the direction of battery electrodes, electrochemical generators, electrical components, etc., can solve the problems of high conversion reaction, high reaction activation energy, and poor economy, so as to improve the electrochemical performance. performance, overcoming the effect of extremely low ionic conductivity

Active Publication Date: 2016-05-25
刘焕礼
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  • Abstract
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  • Application Information

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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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  • Aluminum zirconate-doped lithium titanium phosphate two-component surface-modified ferric fluoride positive electrode material 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 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. 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 powder, 0.6% by weight of Tween-80 and 0.6% by weight of aluminum-zirconium coupling agent of brand name C are ball milled at room temperature for 5 hours under the protection of high-purity nitrogen in a high-energy ball mill. Under the protection of the mixed gas of % hydrogen and 95% argon, th...

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. 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 The solid electrolyte powder, 2.8% by weight of span-60 and 3.0% by weight of the aluminum-zirconium coupling agent of the trade name CPM are ball milled at room temperature for 20 hours under the protection of high-purity nitrogen in a high-energy ball mill, and the material is taken out at 5% Under the protection of the ...

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 the 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. Will 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 electrolyte powder, 2.0% by weight of tx-10 and 2.1% by weight of the commercial brand of aluminum-zirconium coupling agent CPG are ball milled at room temperature for 15 hours under the protection of high-purity nitrogen in a high-energy ball mill, and the material is taken out at 5% Under the protect...

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Abstract

The invention discloses an aluminum zirconium acid ester-doped titanium phosphate dual-component surface-modified ferric fluoride anode material and a preparation method. The method is characterized by comprising the following steps: loading aluminum zirconium acid ester, silicon / aluminium-doped titanium phosphate Li1.3Al0.1Ti1.9Si0.2P2.8O12, and a synthetic raw materials into a high-energy ball mill, ball-milling for a certain period, and performing heat treatment to obtain the FeF3 anode material. The aluminum zirconium acid ester is a bimetal coupling agent, has multiple active sites, and bonds with Li1.3Al0.1Ti1.9Si0.2P2.8O12 by hydrolysis of multiple alkoxyl groups into hydroxyl groups while having condensation polymerization with hydroxyl groups on the surface of the FeF3 anode material, and zirconium is an electron acceptor, can coordinate with fluorine ions on surfaces of FeF3 particles, therefore, under the action of the aluminum zirconium acid ester, doped titanium phosphate Li1.3Al0.1Ti1.9Si0.2P2.8O12 is bonded to the surfaces of the FeF3 anode particles with good contact between particles, and Li1.3Al0.1Ti1.9Si0.2P2.8O12 is a good lithium ion conductor, and the ionic conductivity of Li1.3Al0.1Ti1.9Si0.2P2.8O12 is 103-104 times of that of lithium cobalt oxide. Therefore, the defect that the FeF3 anode material has an extremely-low ionic conductivity can be overcome, and the electrochemical properties of the FeF3 material are 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 Patents(China)
IPC IPC(8): H01M4/58
CPCH01M4/362H01M4/582H01M4/624H01M10/0525Y02E60/10
Inventor 水淼徐晓萍陈姝郑卫东高珊舒杰冯琳任元龙程亮亮
Owner 刘焕礼
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