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Method ofr prpearing high-lithium ion content laminated lithium manganate anode material

A technology with ion content and shape of lithium manganate, applied in the field of lithium ion battery material preparation, can solve the problems of limited mixing uniformity of precursor raw materials, expensive LiI, difficult mass production, etc., and achieves high first irreversible specific capacity and simple process. , the effect of low cost

Inactive Publication Date: 2006-01-11
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the high-temperature solid-state reaction method is used to synthesize the precursor raw materials to a limited degree of uniformity. In addition, the price of LiI is relatively expensive, and it is difficult to produce in batches.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Na 2 CO 3 , MnCO 3 , Co(NO 3 ) 2 ·6H 2 O and citric acid are mixed according to the ratio of Na / Mn / Co / citric acid=1.1 / 0.7 / 0.3 / 2.1 (molar ratio), dissolved in deionized water, and prepared as Na + The concentration is 4mol·L -1 The solution was placed in a vacuum drying oven preheated to 150°C for 2 hours to obtain a fluffy xerogel, which was pretreated in a muffle furnace at 400°C for 5 hours to remove organic matter. Calcined at 800°C for 6 hours in a Furnace to obtain the precursor.

[0015] LiNO 3 Mix with LiCl at 88 / 12 (mass ratio), heat to 350°C to melt, add the precursor according to precursor / molten salt = 1 / 5 (molar ratio), ion exchange for 4 hours, quickly pour 3 times the melting Dissolve the excess lithium salt in deionized water with the volume of salt, wash thoroughly with deionized water and acetone in turn, filter with suction, and then vacuum dry in a vacuum oven at 100°C for 10 hours to obtain the target product.

[0016] ICP and XRD tests show...

Embodiment 2

[0018] Na 2 CO 3 , MnCO 3 , Co(NO 3 ) 2 ·6H 2 O and citric acid are mixed according to the ratio of Na / Mn / Co / citric acid=1.3 / 0.85 / 0.15 / 2.3 (molar ratio), dissolved in deionized water, and prepared as Na + The concentration is 2mol L -1 The solution was placed in a vacuum drying oven preheated to 120 ° C for 6 hours to obtain a fluffy dry gel, which was pretreated in a muffle furnace at 450 ° C for 3 hours to remove organic matter, taken out and ground and then placed in a vacuum oven Calcined at 900°C for 4 hours in a Furnace to obtain the precursor.

[0019] LiNO 3 Mix with LiCl at 88 / 12 (mass ratio), heat to 330°C to melt, add the precursor according to precursor / molten salt = 1 / 10 (molar ratio), ion exchange for 3 hours, quickly pour 5 times the melting Dissolve the excess lithium salt in deionized water with the volume of salt, wash thoroughly with deionized water and acetone in turn, filter with suction, and then vacuum dry in a vacuum oven at 110°C for 8 hours to...

Embodiment 3

[0022] Na 2 CO 3 , MnCO 3 , Ni(NO 3 ) 2 ·6H 2 O and citric acid are mixed according to the ratio of Na / Mn / Ni / citric acid=1.3 / 0.7 / 0.3 / 2.3 (molar ratio), dissolved in deionized water, and made into Na + The concentration is 3mol L -1 The solution was placed in a vacuum drying oven preheated to 140°C for 6 hours to obtain a fluffy xerogel, which was pretreated in a muffle furnace at 400°C for 5 hours to remove organic matter, taken out and ground and then placed in a vacuum oven. Calcined at 800°C for 4 hours in a Furnace to obtain the precursor.

[0023] LiNO 3 Mix with LiCl at 88 / 12 (mass ratio), heat to 300°C to melt, add the precursor according to precursor / molten salt = 1 / 15 (molar ratio), ion exchange for 2 hours, and quickly pour into 5 times the melting The excess lithium salt was dissolved in deionized water with the volume of salt, washed thoroughly with deionized water and acetone in turn, filtered with suction, and then vacuum-dried in a vacuum oven at 120°C f...

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PUM

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Abstract

This invention provides a method for preparing 02 structure laminated lithium manganate positive material (Lix [Mn1-yMy]O2), M is ions of Co or Ni, which applies a method for citric acid colloidal sol-gel to prepare a precursor with high content of Na ions of p2 structure laminated Nax[Mn1-yMy] O2 gets the product by the exchange reaction of molten salt ions. The advantage is that said positive material does not turn to the structure of spinel while charging and discharging so as to have good electrochemical circulation performance.

Description

technical field [0001] The invention belongs to the technical field of preparation of lithium ion battery materials, and in particular provides an O2 structure layered lithium manganate positive electrode material Li with high lithium ion content. x [Mn 1-y m y ]O 2 The preparation method, wherein M is Co, Ni and other metal ions, 0.15≤y≤0.30, x≥0.85. Background technique [0002] Lithium manganate LiMnO 2 As a cathode material for lithium-ion batteries, it has the advantages of abundant resources, low price, and high specific capacity, but its structure is unstable and its electrochemical cycle stability is poor. In lithium manganese oxide LiMnO 2 doped with a certain amount of other metal ions, such as Co 3+ , Ni 3+ , Cr 3+ , Al 3+ etc., to obtain layered Li x [Mn 1-y m y ]O 2 (M=Co, Ni, Cr, Al, etc.), which can improve the stability of its structure during charging and discharging, and thus improve its electrochemical cycle stability. [0003] Layered Li x ...

Claims

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Application Information

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IPC IPC(8): H01M4/04H01M4/48H01M4/58C01D15/00C01G1/02C01G45/00H01M4/505
CPCY02E60/10
Inventor 杨文胜陈冬梅段雪肖寒
Owner BEIJING UNIV OF CHEM TECH
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