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Preparation methods of spherical lithium manganate for lithium-ion power battery and precursor of spherical lithium manganate

A spherical lithium manganate and power battery technology, which is applied to battery electrodes, manganate/permanganate, circuits, etc., can solve the problems of increased cost and difficulty in process control, lack of oxygen and large voids in materials, and damage to physical and chemical properties of materials. Performance and other issues, to achieve the effect of controllable powder particle size, good cycle performance and high temperature performance

Active Publication Date: 2013-09-25
QINGDAO HUAGUAN HENGYUAN LI TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But directly react with manganese oxalate and lithium carbonate or lithium hydroxide, need certain O in the reaction process 2 partial pressure and generate large amounts of CO 2 Gas, which may cause the material to lack oxygen and have too many voids, thereby destroying the physical and chemical properties of the material and causing fluctuations in the performance of the material. In addition, complexing agents need to be added during the reaction process, which increases the cost and difficulty of process control.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] In the present invention, the configuration method of the precursor is carried out according to the following steps:

[0020] (1) Configure 0.1 mol / L MnSO respectively 4 solution and 1mo1 / L of NH 4 HCO 3 solution.

[0021] (2) MnSO 4 The solution was poured into a stirred reactor, and then the NH 4 HCO 3 Add the solution dropwise into the reaction kettle at a speed of 10 ml / min, continuously stir at a speed of 100 r / min, control the temperature of the water bath at 40°C, continue stirring for half an hour after the titration is completed, and filter it after aging for 12 hours. Repeated washing until the pH of the filtrate was about 7.0, and air-dried at 110°C for 12 hours to obtain spherical MnCO3 .

[0022] (3) According to the molar ratio of AL and Mn of 0.04:1.96, the 3 and MnCO 3 Mixing and preheating at low temperature, the heat treatment procedure is two-stage sintering: 300°C, 4h, then 600°C, 8h, the obtained precursor after sintering is Mn doped with Al...

Embodiment 2

[0028] In the present invention, the configuration method of the precursor is carried out according to the following steps:

[0029] (1) Configure 0.5 mol / L MnSO 4 solution and 1mo1 / L of NH 4 HCO 3 solution.

[0030] (2) MnSO 4 The solution was poured into a stirred reactor, and the NH 4 HCO 3 The solution was added dropwise into the reactor at a rate of 5 ml / min. Stir continuously at a speed of 200r / min, control the reaction water bath temperature at 50°C, continue to stir for half an hour after titration to fully proceed the reaction, filter after aging for 10 hours, wash repeatedly with distilled water until the pH value of the filtrate is about 7.0, and store at 110°C Blow drying for 12 hours to obtain spherical MnCO 3 .

[0031] (3) According to the molar ratio of Mg and Mn 0.04:1.96, Mg(NO3) 2 and MnCO 3 Mixing and pretreatment at low temperature, the heat treatment program is two-stage sintering: 300°C, 4h, then 600°C, 8h, the obtained precursor after sinterin...

Embodiment 3

[0036] In the present invention, the configuration method of the precursor is carried out according to the following steps:

[0037] (1) Configure 1mol / L MnSO 4 solution and 2mo1 / L of NH 4 HCO 3 solution.

[0038] (2) MnSO 4 The solution was poured into a stirred reactor, and the NH 4 HCO 3 Add the solution dropwise into the reactor at 3 ml / min, stir continuously at a speed of 300r / min, control the temperature of the water bath at 30°C, continue stirring for half an hour after the titration is completed to fully proceed the reaction, filter after aging for 8 hours, and wash repeatedly with distilled water Until the pH value of the filtrate is about 7.0, air-dry at 110°C for 12 hours to obtain spherical MnCO 3 .

[0039] (3) Mg(NO 3 ) 2 and MnCO 3 Mixing and pretreatment at low temperature, the heat treatment program is two-stage sintering: 300°C, 4h, then 600°C, 8h; the resulting sintered precursor is Mn doped with Mg 2 o 3 - MgO precursors.

[0040] In the presen...

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PUM

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Abstract

The invention discloses preparation methods of a spherical lithium manganate for a lithium-ion power battery and a precursor of the spherical lithium manganate. The preparation method for the precursor is carried out as the following steps: (1) preparing a manganese salt water solution; (2) preparing a precipitant water solution; (3) injecting the prepared solutions in the step (1) and the step (2) to a reaction kettle with a stirrer and a constant-temperature water bath; (4) mixing the obtained MnCO3 and a compound containing an element M based on a mol ratio of M to Mn described in the invention, sintering and obtaining the precursor. The preparation method of the spherical lithium manganate is carried out as the following steps: mixing the precursor and Li2CO3, sintering and obtaining an M-doped spherical spinel lithium manganate. Compared with the prior art, the method of the invention has the advantages that: (1) impurity content is low, discharge plateau is high, specific capacity is high, cycle performance is good, high-temperature performance is good and tap density is high; and (2) raw material price and production cost are low, powder particle size can be controlled, microscale additive disperses uniformly, particle size distribution is concentrate, and microscopic morphology is spherical or spheroidic.

Description

technical field [0001] The invention relates to a method for synthesizing a positive electrode material of a lithium-ion secondary battery, in particular to a method for preparing spherical lithium manganate for a lithium-ion power battery. Background technique [0002] In 1978, Armand proposed that both the positive and negative electrodes use TiS which can allow lithium ions to be intercalated and extracted. 2 Concentration battery is formed. During the charging and discharging process of this kind of battery, lithium ions are intercalated and extracted between the two electrodes, which is vividly called a "rocking chair" lithium-ion secondary battery. However, the battery voltage is only 0~2V, which does not have the high voltage characteristics of lithium batteries. In early 1980, LiCoO was discovered 2 with TiS 2 The same layered structure, in the same year, Oxford University Goodendugh et al. proposed to use LiCoO 2 , LiNiO 2 , LiMn 2 o 4 As the positive el...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/505C01G45/12
CPCY02E60/10
Inventor 胡章勇
Owner QINGDAO HUAGUAN HENGYUAN LI TECH
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