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Method for preparing lithium-rich solid solution cathode material by virtue of metal reduction process

A positive electrode material and solid solution technology, which is applied in the field of preparation of lithium-rich solid solution positive electrode materials, can solve problems such as the inability to eliminate the influence of dissolved oxygen in water, and achieve excellent discharge performance, less time-consuming, and a wide range of raw material sources.

Active Publication Date: 2013-01-16
FUJIAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

When ammonia water is used as a precipitant, excess ammonia reacts with cobalt ions to form Co(NH 3 ) 6 2+ Ions can be oxidized by oxygen in the air (Editor-in-Chief of Wuhan University, Analytical Chemistry (2nd Edition), Higher Education Press, October 1982, Beijing: Page 14 to Page 17), therefore, using hydroxide co-precipitation The sintering precursor prepared by the method is a compound of trivalent manganese and divalent manganese, or even a compound of trivalent cobalt and divalent cobalt, although some documents use nitrogen gas when preparing hydroxide precipitation to solve this problem The method of protecting the precipitation, however, the method of protecting the precipitation with nitrogen can only eliminate the influence of oxygen in the air, but cannot exclude the influence of oxygen dissolved in water

Method used

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  • Method for preparing lithium-rich solid solution cathode material by virtue of metal reduction process

Examples

Experimental program
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Effect test

Embodiment 1

[0036] The preparation process consists of the following steps:

[0037] (1) Weigh lithium hydroxide, nickel hydroxide, manganese acetate, cobalt hydroxide, and zinc powder according to the molar ratio of lithium ion, nickel ion, manganese ion, cobalt ion, and zinc powder to 1.35: 0.195: 0.506: 0.319: 0.0325 . The total weight of reactants is the total weight of lithium hydroxide, nickel hydroxide, manganese acetate, cobalt hydroxide and zinc powder. The weight ratio of the total weight of reactants to deionized water is 5:50 (equivalent to (2·(1-x)·y+4·(x+z-x·z)+3·(1-x)·k+2· (1-x) q-x-3)=0.0868)

[0038] (2) Zinc powder is mixed with deionized water, and then mixed with nickel hydroxide, manganese acetate, and cobalt hydroxide that have been weighed, mixed for 1 hour by wet grinding, and ammonia water is added to make the solution acidity pH 10, and lithium hydroxide that has been weighed is added , wet grinding and mixing for 1 hour to prepare a reaction mixture solution ...

Embodiment 2

[0041] The preparation process consists of the following steps:

[0042] (1) Weigh lithium nitrate, nickel oxalate, manganese sulfate, cobalt chloride and magnesium metal according to the molar ratio of lithium ions, nickel ions, manganese ions, cobalt ions, and metal magnesium powder is 1.15: 0.0425 : 0.354 : 0.51 : 0.0085 Powder (equivalent to (2 · (1-x) · y + 4 · (x+z-x · z) + 3 · (1-x) · k + 2 · (1-x) · q -x-3) = -0.10); the total reactant is the total weight of lithium nitrate, nickel oxalate, manganese sulfate, cobalt chloride and metal magnesium powder, and the ethanol is weighed according to the total reactant and ethanol weight ratio of 5:1.

[0043] (2) Metal magnesium powder is mixed with ethanol, then mixed into the nickel oxalate, manganese sulfate and cobalt chloride taken by weighing, wet milling and mixing for 15 hours, adding ammonia water to make the solution acidity pH 13.5, adding lithium nitrate taken by weighing, wet milling Mix for 15 hours to prepare a...

Embodiment 3

[0046] The preparation process consists of the following steps:

[0047] (1) Weigh lithium iodide, nickel nitrate, manganese oxalate, cobalt oxalate, and aluminum powder according to the molar ratio of lithium ions, nickel ions, manganese ions, cobalt ions, and metal aluminum powder to 1.6 : 0.18: 0.77 : 0.02 : 0.04, respectively. The total weight of the reactant is the total weight of lithium iodide, nickel nitrate, manganese oxalate, cobalt oxalate and metal aluminum powder, according to the total weight of the reactant and methanol weight ratio is 1:1 weighing methanol (equivalent to (2.(1 -x) y + 4 (x+z-x z) + 3 (1-x) k + 2 (1-x) q -x-3)=-0.02).

[0048] (2) Mix the metal aluminum powder with methanol, then mix the weighed nickel nitrate, manganese oxalate and cobalt oxalate, wet mill and mix for 1 hour, add ammonia water to make the solution acidity pH 10, add the weighed lithium iodide, wet mill Mix for 1 hour to prepare a reaction mixture solution containing precipitat...

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Abstract

The invention relates to a method for preparing lithium-rich solid solution cathode material by virtue of a metal reduction process, and the method comprises the following steps of: respectively weighing compounds of lithium, nickel, manganese and cobalt as well as a metal reducing agent M according to the molar ratio of (1+x):(1-x)* y:(x+z-x*z):(1-x)* k:(1-x)* q among lithium ionic, nickel ionic, manganese ionic, cobalt ionic and the metal reducing agent M; mixing the metal reducing agent M with a wet grinding medium, and then mixing the compounds of nickel, manganese and cobalt into the obtained mixture; performing wet grinding, mixing and adding ammonia water and the compound of lithium to prepare a reaction mixed solution; drying and putting the product at a certain atmosphere; and finally, adopting a two-stage sintering method or two times of multi-step sintering method to prepare the lithium-rich solid solution cathode material with the composition of xLi2MnO3(1-x)Li(Niy Mnz Cok Mq)O2. The prepared electrode material is uniform in composition, has excellent discharge property, and has better discharge cycle performance especially under the condition of large current.

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 lithium-rich solid solution positive electrode material that can be used for lithium batteries, lithium ion batteries, polymer batteries and supercapacitors. Background technique [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 performance, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/48H01G11/30
CPCY02E60/12Y02E60/10
Inventor 童庆松周惠王浪韩铭姜祥祥潘樱蔡斌任瑗瑗黄能贵
Owner FUJIAN NORMAL UNIV
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