CN1526647A - Prepn of nano lithium cobaltate particle - Google Patents
Prepn of nano lithium cobaltate particle Download PDFInfo
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- CN1526647A CN1526647A CNA031512119A CN03151211A CN1526647A CN 1526647 A CN1526647 A CN 1526647A CN A031512119 A CNA031512119 A CN A031512119A CN 03151211 A CN03151211 A CN 03151211A CN 1526647 A CN1526647 A CN 1526647A
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- lithium cobaltate
- lithium
- molecular weight
- particle
- cobaltate particle
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Abstract
The present invention discloses preparation process of nano lithium cobaltate particle. It is one wet chemical process including dissolving monohydrate of lithium hydroxide and soluble cobalt salt, introducing organic dispersant to prevent aggregate of the primary particles, spray drying or fast solution evaporating to obtain dry powder, and heat treatment at 500-1000 deg.c to obtain 10-100 nm lithium cobaltate particle. The nano lithium cobaltate product of the present invention may be used widely in the production of lithium cell, non-water electrolyte, etc.
Description
Technical field
The present invention relates to prepare the method for nano lithium cobaltate particle.
Background technology
Along with the development of information industry and the progress of science and technology, have higher requirement to battery in fields such as the energy-storage battery of movable electrical appliances, electric vehicle engineering, big power station, ups power, Medical Instruments power supply and outer space.And secondary lithium battery have the operating voltage height, in light weight, specific energy is big, self-discharge is little, have extended cycle life, memory-less effect, advantage such as low in the pollution of the environment, is a kind of extraordinary selection.Positive pole material of secondary lithium battery commonly used at present mainly contains LiCoO
2, LiNiO
2And LiMn
2O
4Deng, LiNiO wherein
2Synthesis technique be difficult to control, easily form non-stoichiometric compound.And LiMn
2O
4Structure irreversible conversion easily takes place in charging and discharging process, cycle life is poor.And LiCoO
2Operating voltage height, discharge steadily, moderate, practicality is best.Cobalt acid lithium generally adopts solid phase method synthetic, but because the limitation of this traditional method, be difficult to obtain the purity height, the nonstoichiometry skew is little, granularity is little and the desirable powder of narrower particle size distribution, especially nano particle.And too high synthesis temperature and generated time also can influence its chemical property.
Summary of the invention
The purpose of this invention is to provide a kind of method for preparing nano lithium cobaltate particle, to simplify technology, to reduce cost, obtain the purity height, disperse better and the nano lithium cobaltate particle of narrow particle size distribution.
The method for preparing nano lithium cobaltate particle of the present invention is to adopt wet chemical method.Promptly by the cobalt salt dissolving with a hydronium(ion) oxidation lithium and solubility, add organic dispersing agent, spray-dried or quick evaporate to dryness solution and thermal treatment finally form nano lithium cobaltate particle.Its concrete steps are as follows:
1) a hydronium(ion) oxidation lithium is dissolved in is mixed with the solution that concentration is 0.2mol/L～4.0mol/L in the deionized water;
2) with the cobalt salt of above-mentioned solution in 1: 1 ratio of lithium cobalt mol ratio dissolving solubility, 1%～15% ratio adds organic dispersing agent by weight then;
3) dry or be preheated in 150～350 ℃ the Stainless Steel Disc evaporate to dryness solution fast at 100～250 ℃ of temperature range internal sprayings, obtain the dry glue powder end;
4) with the dry glue powder end 500～1000 ℃ of following thermal treatments 2～7 hours, get final product.
Above-mentioned solubility cobalt salt can be cobaltous acetate or Xiao Suangu.Organic dispersing agent can be the polyacrylic acid of molecular weight between 200～30000, molecular weight between 200～40000 polyoxyethylene glycol or molecular weight at 1000～30000 polyvinyl alcohol.
The present invention adopts wet-chemical to make a kind of nano oxidized lithium particle comparatively easily in conjunction with heat-treating methods, and its granular size is between the 10-100 nanometer, and granularity can be controlled by the variation of experiment condition.Owing to adopt organic dispersing agent, solved the problem that primary particle is easy to reunite in the solvent evaporation process effectively, adopt spray-drying process and quick evaporate to dryness solution method in the preparation process, solved the problem of particle agglomeration in the drying process effectively, so the grain graininess of preparing is even, substantially do not reunite, can be widely used in the scientific research and the production of aspects such as lithium cell, nonaqueous electrolyte.In addition, adopt a hydronium(ion) oxidation lithium as raw material, and follow-up thermal treatment temp is lower, therefore has lower cost.
Embodiment
Further specify the present invention below in conjunction with example.
Embodiment 1
One hydronium(ion) oxidation lithium is dissolved in the solution that forms 0.3mol/L in the deionized water, then therein in 1: 1 ratio of lithium cobalt mol ratio dissolving Xiao Suangu (Co (NO
3)
2), adding molecular weight by weight 5% ratio therein again is 3000 polyacrylic acid, forms the dry glue powder ends 200 ℃ of following spraying dryings then, with the dry glue powder end 700 ℃ of following thermal treatments 3 hours, particle diameter at the cobalt acid lithium particle of 30～40nm.
Embodiment 2
One hydronium(ion) oxidation lithium is dissolved in the solution that forms 1mol/L in the deionized water, then therein in 1: 1 ratio of lithium cobalt mol ratio dissolving Xiao Suangu (Co (NO
3)
2), adding molecular weight by weight 9% ratio therein again is 6000 polyoxyethylene glycol, forms the dry glue powder ends 200 ℃ of following spraying dryings then, with the dry glue powder end 800 ℃ of following thermal treatments 4 hours, particle diameter at the cobalt acid lithium particle of 20～50nm.
Embodiment 3
One hydronium(ion) oxidation lithium is dissolved in the solution that forms 0.5mol/L in the deionized water, then therein in 1: 1 ratio of lithium cobalt mol ratio dissolving Xiao Suangu (Co (NO
3)
2), adding molecular weight by weight 5% ratio therein again is 3000 polyacrylic acid, then in being preheated to 150 ℃ Stainless Steel Disc fast evaporate to dryness solution form the dry glue powder end, with the dry glue powder end 700 ℃ of following thermal treatments 4 hours, particle diameter at the cobalt acid lithium particle of 40～60nm.
Embodiment 4
One hydronium(ion) oxidation lithium is dissolved in the solution that forms 1mol/L in the deionized water, then therein in 1: 1 ratio of lithium cobalt mol ratio dissolving cobaltous acetate (Co (CH
3COO)
2), adding molecular weight by weight 8% ratio therein again is 6000 polyvinyl alcohol, then in being preheated to 150 ℃ Stainless Steel Disc fast evaporate to dryness solution form the dry glue powder end, with the dry glue powder end 800 ℃ of following thermal treatments 4 hours, particle diameter at the cobalt acid lithium particle of 60～80nm.
Claims (3)
1. a method for preparing nano lithium cobaltate particle is characterized in that comprising the steps:
1) a hydronium(ion) oxidation lithium is dissolved in is mixed with the solution that concentration is 0.2mol/L～4.0mol/L in the deionized water;
2) with the cobalt salt of above-mentioned solution in 1: 1 ratio of lithium cobalt mol ratio dissolving solubility, 1%～15% ratio adds organic dispersing agent by weight then;
3) dry or be preheated in 150～350 ℃ the Stainless Steel Disc evaporate to dryness solution fast at 100～250 ℃ of temperature range internal sprayings, obtain the dry glue powder end;
4) with the dry glue powder end 500～1000 ℃ of following thermal treatments 2～7 hours, get final product.
2. the method for preparing nano lithium cobaltate particle according to claim 1 is characterized in that said solubility cobalt salt is cobaltous acetate or Xiao Suangu.
3. the method for preparing nano lithium cobaltate particle according to claim 1, it is characterized in that said organic dispersing agent is the polyacrylic acid of molecular weight between 200～30000, molecular weight between 200～40000 polyoxyethylene glycol or molecular weight at 1000～30000 polyvinyl alcohol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03151211 CN1244499C (en) | 2003-09-23 | 2003-09-23 | Prepn of nano lithium cobaltate particle |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03151211 CN1244499C (en) | 2003-09-23 | 2003-09-23 | Prepn of nano lithium cobaltate particle |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1526647A true CN1526647A (en) | 2004-09-08 |
| CN1244499C CN1244499C (en) | 2006-03-08 |
Family
ID=34286966
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 03151211 Expired - Fee Related CN1244499C (en) | 2003-09-23 | 2003-09-23 | Prepn of nano lithium cobaltate particle |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1244499C (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104577067A (en) * | 2015-01-11 | 2015-04-29 | 方美卿 | Method for preparing fluorinated carbon black coated lithium cobalt oxide cathode material |
| CN110311128A (en) * | 2019-07-10 | 2019-10-08 | 深圳市本征方程石墨烯技术股份有限公司 | A kind of lithium cobaltate cathode material and preparation method thereof of graphene doping |
-
2003
- 2003-09-23 CN CN 03151211 patent/CN1244499C/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104577067A (en) * | 2015-01-11 | 2015-04-29 | 方美卿 | Method for preparing fluorinated carbon black coated lithium cobalt oxide cathode material |
| CN104577067B (en) * | 2015-01-11 | 2017-04-05 | 贵州中伟正源新材料有限公司 | A kind of preparation method of the lithium cobaltate cathode material that perfluorocarbon black-envelope covers |
| CN110311128A (en) * | 2019-07-10 | 2019-10-08 | 深圳市本征方程石墨烯技术股份有限公司 | A kind of lithium cobaltate cathode material and preparation method thereof of graphene doping |
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| Publication number | Publication date |
|---|---|
| CN1244499C (en) | 2006-03-08 |
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Owner name: SHANGHAI HUASHI NANO MATERIALS CO., LTD. Free format text: FORMER OWNER: WENG WENJIAN; HUANG DEHUAN; HAN GAORONG Effective date: 20061020 |
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Effective date of registration: 20061020 Address after: 201108 Shanghai Huashi nanometer material Co., Ltd. A building, Xin Mei Industrial Zone, No. 260, Cao Cao Road, Shanghai, Minhang District Patentee after: Shanghai Huashi Nano Material Co., Ltd. Address before: 310031 No. 20, Zhejiang Road, Hangzhou, Zhejiang, Xihu District Co-patentee before: Huang Dehuan Patentee before: Weng Wenjian Co-patentee before: Han Gaorong |
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Owner name: SHANGHAI GUANGLI NANOMETER SCIENCE CO., LTD. Free format text: FORMER OWNER: SHANGHAI HUASHI NANO MATERIALS CO., LTD. Effective date: 20070615 |
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Owner name: SHANGHAI GUANG-LI INVESTMENT MANAGEMENT CO., LTD. Free format text: FORMER OWNER: SHANGHAI GUANG-LI NANO TECHNOLOGY CO., LTD. Effective date: 20090828 |
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Effective date of registration: 20090828 Address after: Room 506, Zhi Lou building, No. 3217 Hongmei Road, Shanghai Patentee after: Shanghai Guang Li Cci Capital Ltd Address before: No. 1900, Hongqiao Road, Shanghai, 5009 Patentee before: Shanghai broad force Nanometer Technology Co., Ltd. |
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Granted publication date: 20060308 Termination date: 20110923 |