Method for preparing spinel-doped lithium-enriched lithium manganate anode material through doping zirconium

A technology of lithium-rich lithium manganese oxide and positive electrode materials, applied in battery electrodes, electrical components, circuits, etc., can solve problems such as poor discharge performance, weak structural stability, and attenuation of cycle performance, and achieve low raw material cost and stable structure The effect of high stability and wide source of raw materials

Active Publication Date: 2014-02-12
贵州唯特高新能源科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0016] Although the above preparation method can improve the electrochemical performance of the sample, however, due to the currently prepared spinel Li 4 mn 5 o 12 The stability of the structure is still not strong during charge and discharge, and there are problems such as poor discharge performance under low temperature and high current discharge conditions, and obvious attenuation of cycle performance under high temperature.

Method used

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  • Method for preparing spinel-doped lithium-enriched lithium manganate anode material through doping zirconium
  • Method for preparing spinel-doped lithium-enriched lithium manganate anode material through doping zirconium

Examples

Experimental program
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Effect test

Embodiment 1

[0034] Lithium hydroxide, manganese carbonate, and zirconium acetate were weighed respectively according to the molar ratio of lithium ion, manganese ion, and zirconium ion being 1:1.15:0.08.

[0035] Mix the weighed lithium hydroxide, manganese carbonate and zirconium acetate, add distilled water 6 times the volume of the total solid volume, and use a super energy ball mill for wet grinding and mixing for 10 hours to prepare precursor 1. Precursor 1 was placed at 180°C and 1000 Pa, and dried in vacuum to prepare Precursor 2. Precursor 2 was placed in an oxygen-enriched air atmosphere with an oxygen volume content of 51%, sintered at 260°C for 10 hours, and then heated from 260°C to 500°C at a heating rate of 5°C / min, and kept at the temperature for sintering for 15 hours. Hetero-spinel lithium-rich lithium manganese oxide cathode material.

[0036] Compared with other inventive methods, the raw material cost of the present invention is lower, the source of raw materials is w...

Embodiment 2

[0038] Weigh lithium carbonate, manganese carbonate, and zirconium oxide respectively according to the molar ratio of lithium ion, manganese ion, and zirconium ion being 0.95: 1.05: 0.20.

[0039] Mix the weighed lithium carbonate, manganese carbonate, and zirconia, add deionized water that is 1 times the volume of the total solid volume, and use an ordinary ball mill for wet grinding and mixing for 3 hours to prepare precursor 1. Precursor 1 was placed at 80° C. and 10 Pa, and dried in vacuum to prepare Precursor 2 . Precursor 2 was placed in an oxygen-enriched air atmosphere with an oxygen volume content of 22%, sintered at 150°C for 3 hours, then heated from 150°C to 400°C at a heating rate of 1°C / min, and kept at the temperature for sintering for 3 hours to prepare the doped Hetero-spinel lithium-rich lithium manganese oxide cathode material.

[0040] Compared with other inventive methods, the raw material cost of the present invention is lower, and the stability of the z...

Embodiment 3

[0042] Lithium citrate, manganese chloride, and zirconium nitrate were weighed respectively according to the molar ratio of lithium ion, manganese ion, and zirconium ion being 1.06: 1.15: 0.05.

[0043] Mix the weighed lithium citrate, manganese chloride and zirconium nitrate, add methanol 12 times the volume of the total solid volume, and wet grind and mix for 15 hours with a wet grinder to prepare precursor 1. Precursor 1 was vacuum-dried at 280° C. and 10132 Pa to prepare Precursor 2 . Precursor 2 was placed in an oxygen-enriched air atmosphere with an oxygen volume content of 99%, sintered at 300°C for 15 hours, and then heated from 300°C to 600°C at a heating rate of 30°C / min, and kept at the temperature for sintering for 24 hours. Hetero-spinel lithium-rich lithium manganese oxide cathode material.

[0044] Compared with other inventive methods, the raw material cost of the present invention is lower, the source of raw materials is wide, and the structural stability of ...

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Abstract

The invention relates to a method for preparing a spinel-doped lithium-enriched lithium manganate anode material through doping zirconium. The method is characterized by respectively weighing compounds of lithium, manganese and zirconium according to the fact that the mol ratio of lithium ions (x) to manganese ions (y) to zirconium ions (z) is (0.95-1.06):(1.05-1.20):(0.05-0.20); y+z is greater than or equals to 1.20 and is less than or equals to 1.25. The compounds of the lithium, the manganese and the zirconium are mixed and added with wet milling mediums to prepare a precursor 1; the precursor 1 is dried to prepare a precursor 2; the LixMnyZrzO12 spinel-doped lithium-enriched lithium manganate anode material is prepared by the precursor 2 through the two-stage sintering method. Zirconium-doped samples prepared by the invention are high in structure stability, so that the lithium ions are conveniently embedded in and released out when charging and discharging, and excellent foundation is laid for the industrialization.

Description

technical field [0001] The invention belongs to the technical field of battery electrode material preparation, and in particular relates to a preparation method of a lithium-rich spinel lithium manganate positive electrode material that can be used for lithium batteries, lithium ion batteries, polymer batteries and supercapacitors. technical background [0002] Lithium-ion batteries have the advantages of high battery voltage, high energy density, no memory effect, long cycle life, and low self-discharge. The performance of positive electrode materials plays a decisive role in the performance of lithium-ion batteries. [0003] Manganese-based cathode materials have the advantages of low price, green and pollution-free, and are the research focus of lithium-ion batteries. Among the manganese-based cathode materials, spinel LiMn has been studied more. 2 o 4 , layered LiMnO 2 and layered solid solution cathode materials. Among them, layered LiMnO 2 The stability of the str...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/505
CPCY02E60/122H01M4/505H01M4/62Y02E60/10
Inventor 童庆松潘国涛姜祥祥朱德钦蔡斌黄能贵王浪
Owner 贵州唯特高新能源科技有限公司
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