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Method for preparing lithium-enriched solid solution cathode material by doping iron, copper and tin ions

A positive electrode material and solid solution technology, which is applied in the field of preparation of doped lithium-rich solid solution positive electrode materials, can solve the problems of poor electrochemical performance consistency of reaction products, uneven mixing of reactants, etc., and achieve excellent discharge performance, low raw material cost, and cycle good performance effect

Active Publication Date: 2013-01-16
DYNABAT NEW ENERGY SCI & TECH CO CLD FUJIAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The ordinary solid-state sintering method simply mixes the reaction products by ball milling, and then sinters the preparation process. There are problems such as uneven mixing of reactants and poor consistency of electrochemical properties of reaction products.

Method used

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  • Method for preparing lithium-enriched solid solution cathode material by doping iron, copper and tin ions

Examples

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Comparison scheme
Effect test

Embodiment 1

[0032] Weigh lithium carbonate, nickel carbonate, manganese carbonate, cobalt carbonate, Fe 2 o 3 and formic acid.

[0033] Nickel carbonate, manganese carbonate, cobalt carbonate and Fe 2 o 3 Mix, add deionized water 15 times the volume of the total solid volume, add formic acid, wet mill and mix for 15 hours with an ordinary ball mill, then add lithium carbonate, wet mill and mix for 15 hours to obtain precursor 1; precursor 1 at 80 ° C, Precursor 2 was prepared by drying under a vacuum condition of 10 Pa. Precursor 2 was placed in a pure oxygen atmosphere, sintered at 550°C for 15 hours, and cooled to a room to obtain a precursor calcined material; the precursor calcined material was crushed and passed through a 200-mesh sieve, placed in an air atmosphere, and sintered at 1050°C sintering at lower temperature for 24 hours, the prepared composition is 0.30 Li 2 MnO 3 0.70 Li[Ni 0.30 mn 0.40 co 0.225 Fe 0.075 ]O 2 lithium-rich solid solution cathode material. When...

Embodiment 2

[0036] According to the molar ratio of lithium ion, nickel ion, manganese ion, cobalt ion, ferrous ion, oxalic acid is 1.57: 0.215: 0.742: 0.0344: 0.0086:1, weigh basic lithium carbonate, basic nickel carbonate, basic manganese carbonate , basic cobalt carbonate, FeO and oxalic acid.

[0037] Mix the weighed basic nickel carbonate, basic manganese carbonate, basic cobalt carbonate and FeO, add 1 / 10 times the volume of ethanol of the total volume of the solid, add glycine, and use a super energy ball mill to wet mix for 3 hours, then Add basic lithium carbonate, and use a super-energy ball mill to mix for 3 hours to obtain precursor 1; dry precursor 1 at 80° C. under a vacuum condition of 10132 Pa to prepare dry precursor 2. Precursor 2 was placed in an oxygen-enriched air gas atmosphere with an oxygen volume content of 22%, sintered at 300°C for 3 hours, and then placed in another sintering furnace with an air atmosphere, and sintered at 1050°C for 3 hours, the preparation com...

Embodiment 3

[0040] Weigh lithium hydroxide, nickel carbonate, manganese carbonate, basic cobalt carbonate, Cu (OH) 2 , formic acid.

[0041] Nickel carbonate, manganese carbonate, basic cobalt carbonate and Cu(OH) 2 Mix, add acetone 15 times the volume of the total solid volume, add formic acid, wet grind and mix for 3 hours with a wet grinder, then add lithium hydroxide, and mix with a wet grinder for 3 hours to obtain precursor 1; at 280 ° C Precursor 2 was prepared by drying in a vacuum at a pressure of 10132 Pa. Precursor 2 was placed in a pure oxygen atmosphere, sintered at 550 °C for 15 hours, and then placed in another sintering furnace with a pure oxygen atmosphere, and sintered at 800 °C for 24 hours to prepare a composition of 0.25 Li 2 MnO 3 0.75 Li[Ni 0.15 mn 0.40 co 0.30 Cu 0.15 ]O 2 lithium-rich solid solution cathode material. When the prepared sample is charged and discharged at 45°C, in the voltage range from 4.6 to 2.5V, and at a current of 0.8C, the discharge ...

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Abstract

The invention provides a method for preparing a lithium-enriched solid solution cathode material by doping iron, copper and tin ions, which is characterized in that a preparation process is formed by the following steps of: mixing a nickel compound, a manganese compound, a cobalt compound and an M compound, which are weighed to form a mixture 1; adding a wet milling medium and organic weak acid; carrying out wet milling and mixing and adding a lithium compound; after carrying out the wet milling and the mixing, utilizing a vacuum drying or spraying drying method to treat a precursor 1 to prepare a dry precursor 2; putting the precursor 2 into air, oxygen-enriched gas or pure oxygen atmosphere; and utilizing a two-section sintering method or a two-time subsection sintering method to prepare the lithium-enriched solid solution cathode material of xLi2MnO3*(1-x)Li[NiyMnzCokMq]O2. An electrode material prepared by the method disclosed by the invention is uniformly formed and has a very good discharging performance; and particularly, the electrode material has the excellent circulating discharging performance under a large-current condition.

Description

technical field [0001] The invention belongs to the technical field of battery electrode material preparation, and in particular relates to a method for preparing a doped lithium-rich solid solution positive electrode material that can be used for lithium batteries, lithium ion batteries, polymer batteries and supercapacitors. technical background [0002] Spinel LiMn 2 o 4 It has the characteristics of high working voltage, low price, and environmental friendliness, but the reversible capacity of the positive electrode material is low, and the discharge point capacity is only 90-100mAh / g when charging and discharging at a rate of 1C; at high temperatures, the discharge capacity of the positive electrode material will change with the Rapid decay with the charge-discharge cycle. [0003] Lithium-rich solid solution cathode material Li 2 MnO 3 ·Li[Ni 1 / 3 co 1 / 3 mn 1 / 3 ]O 2 It shows the advantages of high specific capacity, good thermal stability, and good cycle perform...

Claims

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Application Information

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IPC IPC(8): H01M4/505H01M4/525
CPCY02E60/122Y02E60/10
Inventor 童庆松肖斌蔡斌周惠韩铭黄娟姜祥祥潘樱
Owner DYNABAT NEW ENERGY SCI & TECH CO CLD FUJIAN
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