A borate-doped titanium lithium phosphate two-component surface-modified iron fluoride positive electrode material and preparation method thereof

A surface modification, lithium titanium phosphate technology, applied in 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 ionic conductivity Very low, improved electrochemical performance

Inactive Publication Date: 2016-05-11
NINGBO UNIV
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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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  • A borate-doped titanium lithium phosphate two-component surface-modified iron 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 the 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. Dry in a vacuum oven at 15 Pa for 2.5 hours, take it out and re-grind it in an agate mortar for 15 minutes, and heat up the ground powder to 650°C at a rate of 6°C / min for 6 hours to make Li 1.3 Al 0.1 Ti 1.9 8i 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 The solid electrolyte powder, Tween-80 with 0.6% by weight and diethanolamine borate with 0.6% by weight 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 % argon, the temperature is raised to 300 degrees and the temperature is kept at 2 hours, and the...

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 the ratio of 0.05:0.2:1.9:2.8:0.65 (molar ratio), add 8% 95% ethanol, and ball mill for 45 hours at a speed of 450 rpm in a ball mill. Dry in an 80Pa vacuum oven for 8 hours, take it out and re-grind in an agate mortar for 25 minutes, and the ground powder is heated to 900℃ at a rate of 25℃ / 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 aminotriethyl borate were ball milled at room temperature for 20 hours under the protection of high-purity argon in a high-energy ball mill, and then the materials were taken out and mixed with 5% hydrogen and Under the protection of a mixed gas of 95% argon, the temperature was raised to 450 ...

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. Dry in a vacuum oven at 60 Pa for 7 hours, take it out and re-grind in an agate mortar for 20 minutes, and 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 The solid electrolyte powder, tx-10 with a weight percentage of 2.0% and 2-methylamino-5-pyridine borate 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. Under the protection of a mixed gas of 5% hydrogen and...

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Abstract

The invention provides a borate doped lithium titanium phosphate two-component surface modified ferric fluoride anode material and a preparation method. The preparation method is characterized by ball-milling borate, silicon and aluminium doped lithium titanium phosphate Li1.3Al0.1Ti1.9Si0.2P2.8O12 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 reactive groups of borate, namely amino groups on borate, are subjected to coordination bonding with fluorine ions on FeF3 material particle surfaces and meanwhile specific groups in borate strongly interact with surface hydroxyl on Li1.3Al0.1Ti1.9Si0.2P2.8O12 and then are subjected to polycondensation; therefore under the action of borate, doped lithium titanium phosphate Li1.3Al0.1Ti1.9Si0.2P2.8O12 is bonded on the surfaces of FeF3 anode particles, so that the particles of doped lithium titanium phosphate Li1.3Al0.1Ti1.9Si0.2P2.8O12 and the FeF3 anode form good contact, and Li1.3Al0.1Ti1.9Si0.2P2.8O12 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 Patents(China)
IPC IPC(8): H01M4/62H01M4/58
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 NINGBO UNIV
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