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Method for preparing composite dopant LiMn2O4 by one-step sintering solid-phase reaction

A technology of compound doping lithium manganate and solid-phase reaction, applied in structural parts, electrical components, battery electrodes, etc., can solve problems such as increasing production costs, achieve performance improvement, promote solid-phase reaction, and improve electrochemical performance Effect

Active Publication Date: 2012-09-12
QINGDAO QIANYUN HIGH TECH NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For solid-phase synthesis, two-step sintering is usually used, which increases production costs to a certain extent

Method used

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  • Method for preparing composite dopant LiMn2O4 by one-step sintering solid-phase reaction
  • Method for preparing composite dopant LiMn2O4 by one-step sintering solid-phase reaction
  • Method for preparing composite dopant LiMn2O4 by one-step sintering solid-phase reaction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) Weigh 715 g of lithium carbonate and 58 g of aluminum hydroxide into a high-speed mixing granulator and mix for 30 minutes.

[0023] (2) Add 44 g of cobalt tetroxide and mix for 30 minutes.

[0024] (3) Finally, 3183g of manganese dioxide is added and mixed for 60 minutes.

[0025] (4) Add 3% polyvinyl alcohol for granulation, and the moisture content is 12%.

[0026] (5) Dry the pellets at 100°C, fully dry and sinter it, increase the temperature from room temperature to 350°C for 1 hour, keep it at this temperature for 4 hours, then raise it to 950°C for 5 hours, then lower it to 650°C for 2 hours and keep it for 15 hours. Cool down naturally.

[0027] (6) The calcined material is broken, sieved, and various performance tests are performed. The results are as follows Figure 1-Figure 3 Shown.

Embodiment 2

[0029] (1) Weigh 686 g of lithium hydroxide and 48 g of cobalt tetroxide into a high-speed mixing granulator and mix for 20 minutes.

[0030] (2) Add 36 g of aluminum hydroxide and mix for 20 minutes.

[0031] (3) Finally, add 3118g of trimanganese tetroxide and mix for 40 minutes.

[0032] (4) Add 3% polyvinyl alcohol for granulation, and the moisture content is 15%.

[0033] (5) Dry the pellets at 150°C, fully dry and sinter it, increase the temperature from room temperature to 350°C for 1 hour, keep it at this temperature for 4 hours, then raise it to 950°C for 5 hours, then lower it to 650°C for 2 hours and keep it for 15 hours. Cool down naturally.

[0034] (6) The calcined materials are broken, sieved, and various performance tests are performed.

Embodiment 3

[0036] (1) Weigh 729 g of lithium nitrate and 60 g of aluminum hydroxide into a high-speed mixing granulator and mix for 10 minutes.

[0037] (2) Add 48 g of cobalt tetroxide and mix for 10 minutes.

[0038] (3) Finally, 3183g of manganese dioxide is added and mixed for 30 minutes.

[0039] (4) Add 3% polyvinyl alcohol for granulation, and the moisture content is 14%.

[0040] (5) Dry the pellets at 200°C, fully dry and sinter it, increase the temperature from room temperature to 350°C for 1 hour, keep it at this temperature for 4 hours, then raise it to 950°C for 5 hours, then lower it to 650°C for 2 hours and keep it for 15 hours. Cool down naturally.

[0041] (6) The calcined materials are broken, sieved, and various performance tests are performed.

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Abstract

The invention discloses a method for preparing composite dopant LiMn204 by one-step sintering solid-phase reaction. The method includes the following steps of (1) weighing a lithium source compound and one of dopant compounds to be placed in a high-speed mixed granulator with the mixing time set as 10-30 minutes according to a molar ratio of 0.5-0.6 of lithium to manganese; (2) adding another dopant compound to be mixed with the mixture with the mixing time set as 10-30 minutes; (3) adding the lithium source compound to be mixed fully with the mixing time set as 30-60 minutes; (4) adding binder to granulate all reactants by weight ratio after the reactants are mixed evenly; (5) feeding and drying fillings in a dryer; (6) placing the fillings in an atmosphere furnace to calcine after drying is completed; and (7) crushing and screening calcined fillings and performing each performance detection. Another substance is added to be mixed after each substance is added and is mixed for certain time, so that evenness of mixing materials is improved, solid-phase reaction is facilitated, and electrochemical performance of materials is improved. The method for preparing the composite dopant LiMn204 by the one-step sintering solid-phase reaction is simple in manufacturing process, capable of improving performance of the materials, and suitable for mass production of industrialization.

Description

Technical field [0001] The invention relates to the technical field of lithium ion battery cathode materials, in particular to a method for preparing composite doped lithium manganate by one-step sintering solid phase reaction. Background technique [0002] As spinel LiMn 2 O 4 It has the advantages of higher specific energy, low cost, low pollution, etc., and is the most promising cathode material for the next generation of lithium-ion batteries, but its poor cycle performance limits its application. The current research on this material is focusing on LiMn 2 O 4 Modification to improve LiMn 2 O 4 Many studies have shown that the use of doped Fe, Co, Ni, Zn, Mg and other metal elements to form LiM x Mn 2-x O 4 (M is a doping element) to stabilize the spinel structure is the most effective way to solve the decline of the cycle capacity of this cathode material. [0003] The current industrial production method of lithium manganate is mainly high temperature solid phase method. For...

Claims

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Application Information

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IPC IPC(8): H01M4/505
CPCY02E60/10
Inventor 孙琦张连君孙慧英
Owner QINGDAO QIANYUN HIGH TECH NEW MATERIAL
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