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Phosphate material having mesoporous structure for lithium secondary batteries and preparation method thereof

A technology of mesoporous structure and mesoporous materials, applied in secondary batteries, electrode manufacturing, battery electrodes, etc., can solve the problems of low electrode density and poor rate characteristics, achieve high power density, improve rate performance, and reduce consumption Effect

Inactive Publication Date: 2009-09-23
INST OF PHYSICS - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to overcome the disadvantages of poor rate characteristics and low density of pole pieces when existing LiMPO4 materials are used as positive electrode materials for secondary lithium batteries

Method used

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  • Phosphate material having mesoporous structure for lithium secondary batteries and preparation method thereof
  • Phosphate material having mesoporous structure for lithium secondary batteries and preparation method thereof
  • Phosphate material having mesoporous structure for lithium secondary batteries and preparation method thereof

Examples

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Effect test

Embodiment 1

[0043] Embodiment 1, prepare the mesoporous structure pure phase LiFePO that is used for secondary lithium battery of the present invention , prepared this sample reference as attached figure 1 and 2 .

[0044] The mesoporous structure pure phase LiFePO4 of this embodiment can be prepared by the following steps. First, weigh 1.02g of LiAc 2H2O, 2.48g of Fe(Ac)2 4H2O and 0.98g of H3PO4, add them into a beaker filled with 200ml of ethylene glycol, and stir for 30 minutes with a magnetic stirrer until uniformly dispersed. Add NH4·H2O to adjust the pH value to 7-8, continue magnetic stirring for 0.5 hours until a sol is formed, and heat-treat the sol in high-purity Ar gas (the heat treatment step is: heat the sol at 120°C for 3 hours, then raise the temperature to 140°C ℃ until it becomes a xerogel), and the xerogel is sintered under the protection of high-purity Ar gas (the sintering step is: take 3 hours to heat up from room temperature to 700 ° C, keep the temperature at 700 ...

Embodiment 2

[0048] Example 2. Preparation of the mesoporous cathode material LiCoPO4 for secondary lithium batteries of the present invention. The prepared sample is referred to as attached image 3 and 4 .

[0049] Mesoporous cathode material LiCoPO4 can be prepared by the following steps. First, weigh 1.05g of LiAc 2H2O, 2.51g of Co(Ac)2 4H2O and 0.98g of H3PO4, add them into a beaker containing 80ml of ethylene glycol, stir for 30 minutes with a magnetic stirrer until uniformly dispersed, Add NH4·H2O to adjust the pH value to 7-8, continue magnetic stirring for 0.5 hours until a sol is formed, and heat-treat the sol in air (the heat-treatment step is: heat the sol at 120°C for 1 hour, then raise the temperature to 140°C until it becomes into a xerogel), and sinter the xerogel in air (the sintering step is: take 3 hours to heat up from room temperature to 700°C, keep the temperature at 700°C for 12 hours, and then cool to room temperature for 5 hours). The scanning electron microgra...

Embodiment 3

[0053] Example 3, mesoporous structure doped lithium iron phosphate material

[0054] Doped lithium iron phosphate Li0.99Na0.01FePO4 can be prepared by the following steps. First, weigh 1.02g of LiAc·2H2O, 2.46g of Fe(Ac)2·4H2O, 0.035g of NaAc·3H2O and 0.98g of H3PO4, add them to a beaker containing 50ml of ethylene glycol, and use a magnetic stirrer Stir for 1 hour until uniformly dispersed, add NH4·H2O to adjust the pH value to 7-8, continue magnetic stirring for 1.5 hours until a sol is formed, and heat-treat the sol in high-purity Ar gas (the heat treatment step is: heat the sol at 150°C for 5 hours, and then heated up to 170°C until it becomes a xerogel), the xerogel is sintered under the protection of high-purity Ar gas (the sintering step is: use 2 hours to heat up from room temperature to 700°C, and keep the temperature at 700°C for 12 hours , and cooled to room temperature for another 3 hours). The obtained mesoporous structure Li0.99Na0.01FePO4 has an average prima...

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Abstract

The invention relates to a phosphate material having a mesoporous structure for lithium secondary batteries and a preparation method thereof. The material having a mesoporous structure is secondary particles which have a mesoporous spherical or spheroid shape and are formed by the agglomeration of primary particles; the chemical composition of the material having the mesoporous structure is represented by the formula of LixAaMmBbPOzNn; the average particle diameter of the primary particles is 10nm to 1mum, the average particle diameter of the secondary particles is 100nm to 50mum, the average pore diameter of mesopores is 2 to 500nm; and the material having the mesoporous structure also comprises a layer of 2 to 100nm thick carbon coated outside the secondary particles and on the inner walls of the mesopores, wherein the content of the carbon accounts for 1 to 20 weight percent of the total weight of a substrate. The material is prepared by the steps of: firstly preparing pure-phase phosphate LiMPO4 or doped LiMPO4 sol; secondly, forming dry gel through heat treatment; and finally, forming the agglomerate secondary particles through sintering at high temperature. The phosphate material having the mesoporous structure can be directly used in secondary lithium batteries as an anode active material and can also be used by being mixed with the prior anode material as an additive. The material having the mesoporous structure can improve the rate performance and energy density of the prior anode material and batteries. The secondary lithium batteries containing the phosphate material having the mesoporous structure has high power density and high safety.

Description

technical field [0001] The present invention relates to a kind of anode material for secondary lithium battery, in particular to a kind of olivine or NASICON type lithium transition metal phosphate positive electrode material with mesoporous structure for secondary lithium battery and its preparation method. Background technique [0002] In 1996, J. Barker et al. first proposed the application of NASICON-type phosphate material Li3V2(PO4)3 as anode material for secondary lithium battery in US Patent No. 5,871,866. In 1997, J.B. Goodenough et al. proposed in the US patent USA 5,910,382 that LiFePO4 was used as the positive electrode material of the secondary lithium battery. In the same year, M. Armand et al. disclosed in US Patent USA6,514,640 that LiFePO4 was doped with iron and replaced with phosphorus. The main advantages of materials such as LiFePO4 are that these materials have low raw material prices, abundant storage, no pollution to the environment, and stable chem...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/58H01M4/48C01B25/45H01M4/04H01M10/40
CPCY02E60/12Y02E60/10
Inventor 禹习谦王小建黄学杰
Owner INST OF PHYSICS - CHINESE ACAD OF SCI
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