CN102275996A - Preparation method for nano spinel lithium manganate of lithium ion battery anode material - Google Patents
Preparation method for nano spinel lithium manganate of lithium ion battery anode material Download PDFInfo
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- CN102275996A CN102275996A CN2010101998924A CN201010199892A CN102275996A CN 102275996 A CN102275996 A CN 102275996A CN 2010101998924 A CN2010101998924 A CN 2010101998924A CN 201010199892 A CN201010199892 A CN 201010199892A CN 102275996 A CN102275996 A CN 102275996A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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Abstract
The invention relates to a preparation method for nano spinel lithium manganate of a lithium ion battery anode material. The method is characterized by: adopting lithium hydroxide as lithium source; dissolving the lithium hydroxide; mixing the dissolved lithium hydroxide and high-purity electrolyzed manganese dioxide adopted as a manganese source material, followed by carrying out stirring for 0.5-2 hours at a temperature of 50-100 DEG C or adopting the ultrasonic technology to carry out treatment to provide a spare use; slowly adding an aqueous solution of a weak reducing agent of an alcohol or glucose to the mixed solution comprising the lithium hydroxide and the electrolyzed manganese dioxide in a dropwise manner, then holding the temperature to 50-100 DEG C and carrying out stirring treatment for 6-20 hours, followed by carrying out completely mixing, reacting, cooling, aging for several hours, filtering and drying to obtain a precursor mixture; carrying out ball milling treatment for the precursor mixture to provide a spare use; placing the precursor mixture in the environment having the temperature of 650-950 DEG C, and carrying out insulation synthesis for 8-36 hours in the air atmosphere, followed by cooling to obtain the product. According to the present invention, the method synthesizes the advantages of the liquid-phase method and the solid-phase method; the nano spinel lithium manganate is an anode material having characteristics of simple and convenient production process, low production cost, stable chemical property, high specific capacity, low cost and good safety.
Description
Technical field
The invention belongs to anode material for lithium-ion batteries, be specifically related to a kind of manufacture method with nano spinel structure lithium manganate.
Background technology
Lithium manganate (LiMn with spinel structure
2O
4) because have the voltage height, have extended cycle life, cost is low, aboundresources and nontoxicity, thereby becomes one of the most promising positive electrode material of lithium ion battery of new generation, and particle diameter is at the LiMn of nanometer range
2O
4Because of material particle size is little, lithium ion embeds in granule interior/migration path weak point when taking off embedding, to improving LiMn
2O
4High rate charge-discharge performance, utilization ratio (specific storage) aspect positive effect is arranged.
Spinel type LiMn
2O
4At present the synthetic method that adopts mainly contains three kinds of solid phase methods, liquid phase method, vapor phase process.It is synthesis material that solid-phase synthesis adopts powder solid, because solid phase diffusion speed and material blended ununiformity, general requirement higher reaction temperatures and long reaction times, be easy to generate the Li-Mn-O by product of other component, the preparation product also exists than big difference on composition, structure, size-grade distribution, causes the chemical property of material wayward.Vapor phase process is difficult to realize industrialization control also because there is the problem of step complexity, condition harshness, only rests on the laboratory study stage at present.
Most representative cryochemistry synthesis method is a sol-gel method in the liquid phase method at present.Sol-gel method has advantages such as the synthesis temperature of reduction, shortening reaction times, narrow diameter distribution, and synthesis step is many, the shortcoming of complex process but also exist, and is difficult at LiMn
2O
4Large-scale production in to use.
Summary of the invention
The manufacture method that the purpose of this invention is to provide a kind of lithium ion cell nano spinel lithium manganate; this method synthesis the advantage of liquid phase method and solid phase method; technology is simple, convenient, be easy to industrial scale production; production cost is low, and can guarantee institute's tool stable electrochemical property, specific storage height, the positive electrode material that cost is low, security is good.
The method that the present invention prepares the lithium ion cell nano spinel lithium manganate is as follows:
(1) be the lithium source with the lithium hydroxide, after the dissolving, mix for the manganese source material, under 50-100 ℃ of temperature, stirred 0.5-2 hour with high purity electrolytic manganese dioxide as the manganese source material, this step or adopt ultrasonic technology to handle, standby;
(2) with the aqueous solution of weak reductants such as alcohol or glucose, slowly be added drop-wise in the mixed solution of lithium hydroxide and electrolytic manganese dioxide, in 50-100 ℃ of temperature stir process 6-20h, thorough mixing, reaction, cooling, ageing a few hours, obtain precursor mixture after filtration, the drying, carry out ball-milling processing in this step or with presoma, standby;
(3) precursor mixture is placed under 650-950 ℃ the high temperature, insulation is synthetic 8-36 hour in air atmosphere, promptly gets product after the cooling.
Embodiment
Embodiments of the invention 1:
75.4gLiOH is dissolved in the 10L water, add 156.6g electrolytic manganese dioxide (EMD) then, the slurry that obtains was stirred 0.5 hour under 50-100 ℃ of temperature, then 7.5g glucose is dissolved in the 500mL water, join while stirring in the above-mentioned slurry, add 4L water then, reaction continues at 100 ℃ of temperature stir process 6h, at last with the slurry cooling that obtains, ageing a few hours.Under 750 ℃ high temperature, insulation is synthetic 36 hours in air atmosphere, promptly gets product after the cooling.
Embodiments of the invention 2:
75.4gLiOH is dissolved in the 10L water, add 156.6g electrolytic manganese dioxide (EMD) then, the slurry that obtains was stirred 0.5 hour under 50-100 ℃ of temperature, then 7.5g glucose is dissolved in the 500mL water, join while stirring in the above-mentioned slurry, add 4L water then, reaction continues at 100 ℃ of stir process 6h, and adopt ultrasonication 10-20min, at last with the slurry cooling that obtains, ageing a few hours.Under 750 ℃ high temperature, insulation is synthetic 36 hours in air atmosphere, promptly gets product after the cooling.
Embodiments of the invention 3:
75.4gLiOH is dissolved in the 10L water, add 156.6g electrolytic manganese dioxide (EMD) then, the slurry that obtains was stirred 0.5 hour at 50-100 ℃, then 7.5g glucose is dissolved in the 500mL water, join while stirring in the above-mentioned slurry, add 4L water then, reaction continues at 100 ℃ of stir process 6h, and adopt ultrasonication 10-20min, at last with the slurry cooling that obtains, ageing a few hours.Under 750 ℃ high temperature, insulation is synthetic 36 hours in air atmosphere, promptly gets product after the cooling behind the dry back employing high energy ball mill processing 10-30min.
Claims (5)
1. the preparation method of a lithium ion anode material nano spinel lithium manganate is characterized in that:
(1) be the lithium source with the lithium hydroxide, after the dissolving, mix for the manganese source material, under 50-100 ℃ of temperature, stirred 0.5-2 hour, or adopt ultrasonic technology to handle with the high purity electrolytic manganese dioxide, standby;
(2) with the aqueous solution of alcohol or glucose weak reductant, slowly be added drop-wise in the mixed solution of lithium hydroxide and electrolytic manganese dioxide, keep 50-100 ℃ of temperature stir process 6-20h, thorough mixing, reaction, cooling, ageing a few hours, obtain precursor mixture after filtration, the drying, presoma is carried out ball-milling processing, standby;
(3) precursor mixture is placed under 650-950 ℃ the high temperature, insulation is synthetic 8-36 hour in air atmosphere, promptly gets product after the cooling.
2. a kind of manufacture method with nano spinel structure lithium manganate according to claim 1 is characterized in that: lithium hydroxide described in the manufacture method step (1) and Manganse Dioxide at first fully stir in liquid phase environment.
3. a kind of manufacture method with nano spinel structure lithium manganate according to claim 1 is characterized in that: lithium hydroxide described in the manufacture method step (1) and Manganse Dioxide mixed solution adopt ultrasonic wave to handle 10-20min.
4. a kind of manufacture method with nano spinel structure lithium manganate according to claim 1 is characterized in that: the weak reductant described in the manufacture method step (2) is ethanol or methyl alcohol or the organic weak reductant of glucose in the alcohols.
5. a kind of manufacture method with nano spinel structure lithium manganate according to claim 1 is characterized in that the precursor mixture described in the manufacture method step (2) adopts ball-milling processing 20-30min.
Priority Applications (1)
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| CN2010101998924A CN102275996A (en) | 2010-06-09 | 2010-06-09 | Preparation method for nano spinel lithium manganate of lithium ion battery anode material |
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| CN2010101998924A CN102275996A (en) | 2010-06-09 | 2010-06-09 | Preparation method for nano spinel lithium manganate of lithium ion battery anode material |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103022469A (en) * | 2012-12-13 | 2013-04-03 | 青岛乾运高科新材料股份有限公司 | Method for preparing lithium manganate anode material through ultrasonic wave activation technology |
| CN103219509A (en) * | 2013-04-19 | 2013-07-24 | 四川大学 | Preparation method of lithium manganese oxide spinel positive material |
| CN103296253A (en) * | 2013-05-24 | 2013-09-11 | 遵义师范学院 | Preparation method of nano lithium manganate used as anode material for lithium ion battery |
| CN103490056A (en) * | 2013-09-24 | 2014-01-01 | 四川国理锂材料有限公司 | Method for producing lithium manganate as lithium battery cathode material through wet mixing |
| WO2014012258A1 (en) * | 2012-07-20 | 2014-01-23 | 深圳市德方纳米科技有限公司 | Auto-thermal evaporative liquid-phase synthesis method for cathode material for battery |
| CN113461065A (en) * | 2021-06-21 | 2021-10-01 | 中国计量大学 | Preparation method of lithium manganate catalyst for formaldehyde degradation |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101017892A (en) * | 2006-06-26 | 2007-08-15 | 兰州大学 | Positive material for the lithium ion battery and preparing method |
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2010
- 2010-06-09 CN CN2010101998924A patent/CN102275996A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101017892A (en) * | 2006-06-26 | 2007-08-15 | 兰州大学 | Positive material for the lithium ion battery and preparing method |
Non-Patent Citations (2)
| Title |
|---|
| V. GANESH KUMAR ET AL.: "An Aqueous Reduction Method To Synthesize Spinel-LiMn2O4 Nanoparticles as a Cathode Material for Rechargeable Lithium-Ion Batteries", 《CHEM. MATER.》 * |
| 姚耀春等: "超声空化预处理对尖晶石LiMn2O4性能的影响", 《电池》 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2014012258A1 (en) * | 2012-07-20 | 2014-01-23 | 深圳市德方纳米科技有限公司 | Auto-thermal evaporative liquid-phase synthesis method for cathode material for battery |
| CN103022469A (en) * | 2012-12-13 | 2013-04-03 | 青岛乾运高科新材料股份有限公司 | Method for preparing lithium manganate anode material through ultrasonic wave activation technology |
| CN103022469B (en) * | 2012-12-13 | 2015-09-23 | 青岛乾运高科新材料股份有限公司 | Ultrasonic activation technology prepares the method for manganate cathode material for lithium |
| CN103219509A (en) * | 2013-04-19 | 2013-07-24 | 四川大学 | Preparation method of lithium manganese oxide spinel positive material |
| CN103219509B (en) * | 2013-04-19 | 2015-04-01 | 四川大学 | Preparation method of lithium manganese oxide spinel positive material |
| CN103296253A (en) * | 2013-05-24 | 2013-09-11 | 遵义师范学院 | Preparation method of nano lithium manganate used as anode material for lithium ion battery |
| CN103490056A (en) * | 2013-09-24 | 2014-01-01 | 四川国理锂材料有限公司 | Method for producing lithium manganate as lithium battery cathode material through wet mixing |
| CN103490056B (en) * | 2013-09-24 | 2015-11-25 | 四川国理锂材料有限公司 | Material by wet type mixing produces the method for anode material of lithium battery LiMn2O4 |
| CN113461065A (en) * | 2021-06-21 | 2021-10-01 | 中国计量大学 | Preparation method of lithium manganate catalyst for formaldehyde degradation |
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Application publication date: 20111214 |