Preparation method of bulky-grain spinel lithium manganate material

A technology of spinel lithium manganese oxide and large particles, applied in electrical components, battery electrodes, circuits, etc., can solve problems such as inappropriate high-temperature calcination process, harmful cycle life due to oxygen deficiency, and unimproved cycle life, etc., to achieve Low cost, complete crystal grains, and excellent high and low temperature cycle life

Inactive Publication Date: 2012-04-18
UNIV OF SCI & TECH BEIJING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] Generally, increasing the sintering temperature and increasing the sintering time are the most effective methods to increase the particle size of the material and reduce the specific surface area, but for lithium manganate materials, it must be calcined at a high temperature above 900 ° C for more than 10 hours to effectively reduce its specific surface area, but high temperature The degree of oxygen defici

Method used

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  • Preparation method of bulky-grain spinel lithium manganate material
  • Preparation method of bulky-grain spinel lithium manganate material
  • Preparation method of bulky-grain spinel lithium manganate material

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Embodiment 1

[0029] The raw materials used are industrial-grade manganese dioxide, lithium carbonate and aluminum hydroxide, and the final ratio is Li 1.05 mn 1.77 Al 0.18 Ox, first mix manganese dioxide and aluminum hydroxide evenly according to the ratio, sinter at 1100°C for 10 hours, cool to 200°C, and mix with lithium carbonate after crushing, sinter at 800°C for 10 hours and slowly cool to 200°C, and then crush Milling and grading the powder can obtain the desired spinel lithium manganese oxide.

[0030] The raw material manganese dioxide used is flake (such as figure 1 ), wide particle size distribution (such as figure 2 ), the product obtained by sintering in the first stage is tested by XRD, such as image 3 As shown, the product is trimanganese tetraoxide. Figure 4 It can be seen from the SEM image that the grains have a complete crystal shape and a particle size of about 8 microns. Figure 5 Is the particle size distribution, it can be seen that the particle size distri...

Embodiment 2

[0034] The raw materials used are industrial-grade manganese dioxide, lithium carbonate and tricobalt tetroxide, and the final ratio is Li 1.1 mn 1.72 co 0.18 Ox, first mix manganese dioxide and tricobalt tetroxide evenly according to the proportion, sinter at 1100°C for 10 hours, cool in the air, mix with lithium hydroxide after crushing, sinter at 800°C for 10 hours and slowly cool to 200°C, then crush and make powder , powder classification, that is, to obtain the desired spinel lithium manganese oxide.

[0035]

Embodiment 3

[0037] The raw materials used are industrial-grade manganese carbonate, lithium carbonate, aluminum hydroxide and yttrium oxide, and the final ratio is Li 1.1 mn 1.72 Al 0.13 Y 0.05 Ox, first mix manganese tetraoxide, aluminum hydroxide and yttrium oxide evenly according to the proportion, sinter at 1200°C for 10h, and cool in the air after cooling to 1000°C, mix with lithium hydroxide after crushing, and sinter at 800°C After 10 hours of slow cooling to 200°C, it was crushed to make powder, and the powder was classified to obtain the desired spinel lithium manganese oxide.

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Abstract

The invention discloses a preparation method of a bulky-grain spinel lithium manganate material, which belongs to the field of electrochemical materials. The bulky-grain spinel lithium manganate material is prepared through carrying out high-temperature sintering on a raw material such as manganese dioxide or manganese carbonate as with a doped element M to be converted into uniformly-doped bulky-grain mangano-manganic oxide, using the bulky-grain mangano-manganic oxide as the raw material of a Mn source, mixing the bulky-grain mangano-manganic oxide with an original material of Li, and sintering the obtained mixture. The mangano-manganic oxide prepared by the invention has a good crystalline grain shape; the grain size is in normal distribution; after the bulky-grain mangano-manganic oxide is used as the raw material of the Mn source and mixed with the original material of the Li, a bulky-grain lithium manganate product with a low surface area can be obtained without the obtained miture at a temperature which exceeds 900 DEG C; and the problem that oxygen loss is caused when the bulky-grain lithium manganate is prepared by high sintering exceeding 900 DEG C is solved. The lithium manganate prepared by the method has uniform granularity; the average grain size of the lithium manganate can be controlled in a range of 5-15 mum through the process; the specific surface area is between 0.2 m<2>/g and 0.6 m<2>/g; crystalline grains are complete; and the high-low temperature cycle service is excellent. The method provided by the invention has a simple process and low cost, and is applicable to industrial production.

Description

technical field [0001] The invention relates to a preparation method of a large-grain spinel lithium manganese oxide material, which belongs to the technical fields of electrochemistry, powder metallurgy and electronic products. Background technique [0002] Cathode materials are an important part of secondary lithium-ion batteries, and their performance and cost play a key role in the development and application of lithium-ion batteries. In the cost of lithium battery preparation, the positive electrode material accounts for the largest proportion, more than 30%. The positive electrode materials that have been developed so far mainly include layered lithium cobaltate, lithium nickelate, multi-component positive electrode, lithium manganate with spinel structure and lithium iron phosphate with olivine structure. The positive electrode materials of the above systems have their own advantages and disadvantages, and different systems are suitable for different battery products...

Claims

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Application Information

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IPC IPC(8): H01M4/58
CPCY02E60/12Y02E60/10
Inventor 李平曲选辉翟福强范丽珍万琦尹海清
Owner UNIV OF SCI & TECH BEIJING
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