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Method for preparing lithium vanadium phosphoric acid of anode material of lithium ion battery under high pressure

A lithium-ion battery, lithium vanadium phosphate technology, applied in battery electrodes, chemical instruments and methods, circuits, etc., can solve the problems of slow reaction rate, high reaction temperature, large volume change, etc., to avoid pretreatment steps, reaction The effect of temperature reduction and simple and easy process

Inactive Publication Date: 2006-12-06
广州鸿森材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, LiMn 2 o 4 There are two main defects: First, the cycle performance is relatively poor, which is mainly attributed to LiMn 2 o 4 During the charge and discharge process, the volume change is large and the Mn 4+ / Mn 3+ John~Teller effect in the conversion process; second, the capacity loss at higher temperature, which is mainly due to the Mn 3+ Disproportionation and Mn 2+ Easily soluble in electrolyte
[0008] However, at present, lithium vanadium phosphate cathode material is only in the initial stage of further research on its structure, and its synthesis and preparation methods have not yet been carried out specific and extensive research work, and there are only a few reports on the synthesis of high-performance lithium vanadium phosphate cathode materials
prepared a lithium vanadium phosphate positive electrode material with excellent cycle performance, but hydrogen was used as a reducing atmosphere during the preparation process, which was relatively expensive, and due to the low diffusion rate of hydrogen, the reaction rate was slow, and large-scale production was difficult.
Huang et al. added carbon glue to the raw materials to form a carbon coating with a nano-network structure in the product, thereby improving the cycle performance and rate performance of the product, but the preparation of carbon glue is difficult and there is no industrialization. products, it is impossible to apply this method to practice
[0009] As far as the current research progress is concerned, there are still no good measures to improve a series of difficulties brought about by low reaction diffusion rate, slow reaction rate, high reaction temperature, and large-scale production difficulties in reducing atmospheres.

Method used

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  • Method for preparing lithium vanadium phosphoric acid of anode material of lithium ion battery under high pressure
  • Method for preparing lithium vanadium phosphoric acid of anode material of lithium ion battery under high pressure
  • Method for preparing lithium vanadium phosphoric acid of anode material of lithium ion battery under high pressure

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Embodiment 1

[0029] Will Li 2 CO 3 , V 2 o 5 and NH 4 h 2 PO 4 Weigh 200g according to the stoichiometric ratio of Li:V:P=3:2:3, mix evenly, and ball mill on a planetary ball mill for 7h; then pretreat at 300°C for 5h under air atmosphere, and after natural cooling, the powder is obtained Shape product; Add low molecular weight phenolic resin 50g as carbon source in above-mentioned powdery product, ball mill 12h again in planetary ball mill, in N 2 In gas atmosphere, sintering is carried out at 900° C. for 12 h under 1 MPa pressure to obtain carbon-coated lithium vanadium phosphate positive electrode material.

[0030] The XRD pattern of the product is shown in figure 1 In the curve a, it can be seen from the figure that the pure-phase monoclinic lithium vanadium phosphate positive electrode material is synthesized by using the solid-state sintering method. There is no impurity peak in the spectrum, and the product has high purity. The scanning electron micrograph of the product is...

Embodiment 2

[0032] LiNO 3 、VO 2 and (NH 4 ) 2 HPO 4 Weigh 50 g according to the stoichiometric ratio of Li: V: P = 3.06: 2: 3, mix them uniformly, and ball mill them on a planetary ball mill for 12 hours; then carry out pretreatment at 200° C. for 8 hours in an air atmosphere, and after natural cooling, obtain Powdered product; then add 10 g of acetylene black to the above powdered product as a carbon source, ball mill again in a planetary ball mill for 24 hours, and sinter at 500 °C for 8 hours in an Ar gas atmosphere under a pressure of 10 MPa to obtain a carbon-coated Lithium vanadium phosphate cathode material.

[0033] The XRD pattern of the product is shown in figure 1 In the middle b curve, it can be seen from the figure that there is no impurity in the product, and it is a pure-phase monoclinic lithium vanadium phosphate positive electrode material. The first charge and discharge curve of the lithium vanadium phosphate positive electrode material is shown in Figure 5 , the...

Embodiment 3

[0035] LiCH 3 COO, V 2 o 3 and (NH 4 ) 3 PO 4 Weigh 100g according to the stoichiometric ratio of Li:V:P=3.1:2:3, mix it evenly, and ball mill it on a planetary ball mill for 20h; then under air atmosphere, carry out pretreatment at 400°C for 12h, after natural cooling, to obtain Powdered product; then add 1 g of graphite to the above powdered product as a carbon source, ball mill again in a planetary ball mill for 20 hours, and sinter at 600°C for 2 hours in a He gas atmosphere to obtain carbon-coated phosphoric acid Lithium vanadium cathode material.

[0036] The XRD pattern of the product is shown in figure 1 In the curve c, it can be seen from the figure that there is no impurity in the product, and it is a pure-phase monoclinic lithium vanadium phosphate positive electrode material. The first charge and discharge curve of the lithium vanadium phosphate positive electrode material is shown in Figure 6 , when the charging and discharging voltages are 3-4.3V, 3-4.5V...

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Abstract

This invention relates to a high-pressure method for preparing vanadium lithium phosphate used as the anode material for lithium ion batteries. The method comprises: (1) mixing lithium salt, vanadium salt and phosphate uniformly, and ball-milling for 7-24 h; (2) preheating in the air at 200-500 deg.C for 2-12 h to obtain vanadium lithium phosphate. The method has such advantages of simple process, abundant raw materials, no need for reductive gas protection during reaction, short reaction time and low reaction temperature. The product has high capacity and good recycling property, and can be used as the anode material for lithium ion batteries.

Description

technical field [0001] The invention relates to a method for preparing a positive electrode material of a battery, in particular to a method for synthesizing a high-performance lithium vanadium phosphate positive electrode material in a high-pressure atmosphere. Background technique [0002] Lithium-ion batteries have many advantages: high working voltage, usually the voltage of a single lithium-ion battery is 3.6V, while the voltage of MH~Ni, Cd~Ni batteries is 1.2V, a difference of 3 times; small size, light weight, specific energy High (specific energy is 3 times that of lead-acid batteries and 2 times that of various nickel batteries); long cycle life, much higher than other batteries; safe and fast charging, low self-discharge rate; no memory effect, long use time. [0003] Therefore, since 1991, when SONY Company introduced commercialized lithium-ion batteries, the research on lithium-ion batteries has been in the ascendant. Currently, most mobile phones, notebook com...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/45H01M4/58
CPCY02E60/10Y02P20/129
Inventor 申国培赵彦明付鹏
Owner 广州鸿森材料有限公司
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