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Preparation method of phosphate anode material

A positive electrode material and phosphate technology, which is applied in the field of preparation of phosphate-based positive electrode materials, can solve problems such as large resistance, reduced product performance, and instability, and achieve the effects of improving discharge performance, reducing reaction resistance, and uniform doping

Active Publication Date: 2015-07-01
常州普格纳能源材料有限公司
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

[0005] In order to solve the problem of the introduction of impurity elements and the relatively large resistance of the doping reaction kinetic process in the synthesis of materials by solid-state method, resulting in the degradation and instability of product performance, the present invention proposes a preparation method for phosphate-based positive electrode materials, which can effectively improve Improve the discharge performance of the product while improving the stability of the product

Method used

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Experimental program
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Effect test

Embodiment 1

[0022] (1) Mg 3 (PO 4 ) 2 with MnPO 4 The precursor was mixed and ball-milled for 5 hours at a molar ratio of 0.1:1 to obtain a mixture;

[0023] (2) Pre-sintering the mixture in nitrogen at 400°C for 7 hours to obtain a pre-sintered product;

[0024] (3) The pre-sintered product was mixed with lithium carbonate and graphene for 5 hours, wherein the mol ratio of the pre-sintered product and lithium carbonate was 1: 1, and the addition of graphene was 10% of the pre-sintered product quality;

[0025] (4) sintering the ball-milled product in step (3) at 500° C. for 14 hours in nitrogen to obtain a sintered product;

[0026] (5) The sintered product is finely crushed and sieved to obtain magnesium-doped LiMnPO 4 Cathode material.

[0027] With the doping LiMnPO that embodiment 1 obtains 4 The discharge curve of the lithium-ion battery as the positive electrode material is as follows: figure 1 shown; the transmission electron microscope picture of the positive electrode ma...

Embodiment 2

[0029] (1) Nb 3 (PO 4 ) 5 with FePO 4 The precursor was mixed and ball-milled for 2 hours at a molar ratio of 0.01:1 to obtain a mixture;

[0030] (2) Pre-sintering the mixture in argon at 300° C. for 12 hours to obtain a pre-sintered product;

[0031] (3) The pre-sintered product was mixed with lithium hydroxide, glucose and sucrose and ball milled for 8 hours, wherein the molar ratio of the pre-sintered product to lithium hydroxide was 1: 0.95, and the amount of glucose and sucrose added was 1 / 2 of the pre-sintered product quality. 3%, wherein the mass ratio of glucose to sucrose is 1:1;

[0032] (4) sintering the ball-milled product in step (3) at 700° C. for 24 hours in argon to obtain a sintered product;

[0033] (5) The sintered product is finely crushed and sieved to obtain niobium-doped LiF e PO 4 Cathode material.

Embodiment 3

[0035] (1) Put Ti 3 (PO 4 ) 4 with CoPO 4 The precursor was mixed and ball-milled for 8 hours at a molar ratio of 0.05:1 to obtain a mixture;

[0036] (2) Pre-sintering the mixture in nitrogen at 450° C. for 2 hours to obtain a pre-sintered product;

[0037] (3) The pre-sintered product was mixed with lithium oxalate and superconducting carbon black and ball milled for 2 hours, wherein the mol ratio of the pre-sintered product to lithium oxalate was 1: 1.05, and the addition of superconducting carbon black was 1 / 2 of the pre-sintered product quality 15%;

[0038] (4) sintering the ball-milled product in step (3) at 900° C. for 4 hours in nitrogen to obtain a sintered product;

[0039] (5) The sintered product is finely crushed and sieved to obtain titanium-doped LiCoPO 4 Cathode material.

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Abstract

The invention relates to the technical field of lithium ion batteries and provides a preparation method of a phosphate anode material, in order to solve the problem that product property is reduced and unstable since impurity elements are introduced during raw material solid phase method synthesis and resistance is relatively large in the dynamical process of doping reaction. The preparation method comprises the following steps: (1) carrying out mixed ball milling on a phosphate and a precursor for 2-8 hours to obtain a mixture; (2) pre-sintering the mixture in inert gas at 300-450 DEG C for 2-12h, thus obtaining a pre-sintered product; (3) carrying out mixed ball milling on the pre-sintered product, a lithium source and a carbon source for 2-8h; (4) sintering the product obtained after ball milling in the step (3) in inert gas at 500-900 DEG C for 4-24h, thus obtaining a sintering product; and (5) fine crushing the sintered product and sieving to obtain the phosphate anode material. With adoption of the preparation method disclosed by the invention, the discharge performance of the product is improved effectively and the homogeneity and stability of the product are also enhanced.

Description

technical field [0001] The invention relates to the technical field of lithium ion batteries, in particular to a method for preparing a phosphate-based positive electrode material. Background technique [0002] Lithium-ion batteries are mainly composed of four parts: positive electrode material, negative electrode material, electrolyte, and diaphragm material, and the performance of the positive electrode material directly determines the performance of the lithium-ion battery. Phosphate-based cathode materials have high safety performance and cycle life, and at the same time have the advantages of non-toxic, non-polluting, wide source of raw materials, and low price. They are ideal cathode materials for the new generation of lithium-ion batteries. However, the electron conductance and ion conductance of the phosphate-based positive electrode material are very low, which is not suitable for charging and discharging with a large current, which hinders its application. Both th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/45H01M4/58
CPCY02E60/10
Inventor 吴雪峰金传洪
Owner 常州普格纳能源材料有限公司
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