CN101567442A - Method for preparing spinel lithium titanate - Google Patents
Method for preparing spinel lithium titanate Download PDFInfo
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- CN101567442A CN101567442A CNA2009101342471A CN200910134247A CN101567442A CN 101567442 A CN101567442 A CN 101567442A CN A2009101342471 A CNA2009101342471 A CN A2009101342471A CN 200910134247 A CN200910134247 A CN 200910134247A CN 101567442 A CN101567442 A CN 101567442A
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- lithium titanate
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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
Abstract
A method for preparing the spinel lithium titanate belongs to the field of the battery. The aim of the invention is to provide a method for preparing the spinel lithium titanate. The essential point of the technical scheme of the invention is that the molecular formula of the spinel lithium titanate is LixTi1.25-yMyO3/wz according to the method for preparing the spinel lithium titanate. The method for preparing comprises the following steps: (1) after mixing a lithium source and a titanium source with the atomic ratio between lithium and titanium for 0.6-1 into an organic solvent for executing ball milling for 8-24 hours, drying; (2) executing heat treatment to the dried object prepared in the step (1) at the temperature of 300-600 DEG C for 10-24 hours, cooling by radiation; and (3) mixing and executing ball milling to the material obtained in the step (2) and the coating material for 8-24 hours, and after sintering under the protection of nitrogen in the temperature of 700-1000 DEG C for 10-24 hours, cooling and sieving for obtaining the spinel lithium titanate of the invention. The method of the invention is used for preparing the lithium cell.
Description
Technical field:
The present invention relates to the manufacture method of the electrode formed by active material, especially for the preparation method of the spinel lithium titanate of lithium electricity secondary battery cathode material.
Background technology:
The high specific energy of lithium ion battery, high voltage and oligosaprobic characteristic make it become present mobile phone, the good power supply of notebook computer and video camera, and be one of important candidate of following electric powered motor power supply.At present in the commercial lithium ion battery metal oxide-type of commercialization or the part electrode material, lithium-titanium composite oxide Li
4Ti
5O
12Can make lithium ion battery negative material, has spinel structure, the end of the eighties, the positive electrode of Ceng Zuowei lithium ion battery was studied, but because it is on the low side and energy density is also lower (theoretical capacity is 175mAh/g) with respect to the lithium current potential, thereby reduced people's research interest.There are some researches show Li afterwards
4Ti
5O
12Its skeleton structure changes hardly in charge and discharge process, need to generate passivating film unlike material with carbon element, for the first time efficiency for charge-discharge is up to more than 90%, and is a kind of zero strain material, keep crystalchecked in the charge and discharge process, have excellent cycle performance.Especially under the requirement of fast charging and discharging, its skeleton structure crystalchecked that changes has hardly solved problems such as the quick charge of present electric powered motor power supply and long-term use.
Summary of the invention:
The preparation method who the purpose of this invention is to provide a kind of spinel lithium titanate, it is good, safe and specific capacity is big that the spinel lithium titanate made from this method has excellent cyclical stability, fast charging and discharging, anti-over-charging performance and a thermal stability as lithium cell cathode material.Technical scheme of the present invention is, a kind of preparation method of spinel lithium titanate, and the molecular formula that it is characterized in that spinel lithium titanate is Li
xTi
1.25-yM
yO
3/ w
zM is the doping vario-property material in the formula, and W is a clad material, 0.5≤x≤1.5,0＜y≤0.5,0＜z≤0.5, its preparation methods steps has: (1) is with lithium: the atomic ratio of titanium is to be distributed to behind the lithium source of 0.6-1 and titanium source and the doping vario-property agent mixing to carry out ball milling 8-24 hour in the organic solvent, oven dry, described doping vario-property agent are one or two or more kinds the mixture in the following oxide: Mn, Cr, Co, Cu, Ni, V, Mo, Zn, Al, Mg, B, Zr, Nb, doping is 0-0.5; (2) the oven dry thing that work step (1) is made natural cooling after heat-treating 10-24 hour under 300-600 ℃; (3) material that work step (2) is obtained and clad material carried out mixing and ball milling 8-24 hour; under nitrogen protection with 700-1000 ℃ under carry out sintering 10-24 hour after; cooling is sieved and is obtained spinelle of the present invention and meet lithium titanate, and described clad material is glucose, sucrose, furfural resin, pitch or polyacrylamide.The present invention has fast charging and discharging, good cycling stability compared with the prior art, anti-over-charging is electrical and Heat stability is good and the big remarkable advantage of specific capacity.
Embodiment:
Adopt titanium dioxide and inorganic lithium salt as raw material, the doping vario-property agent is mixed and is formed, and the microscopic feature with sphere or class sphere comprises the porous nano passage in the particle, be synthetic medium with watery fusion salt.Coat the back with the nano-sized carbon clad material again and form second particle, by solid phase reaction synthetic spinel type lithium titanate takes place.In preparation process, the diffusion velocity of reactant in watery fusion salt is apparently higher than in traditional solid phase environment, and this is fast reaction speed effectively, reduces reaction temperature, shortens the reaction time, energy savings; And the advantage of this method is integrated conventional high-temperature solid phase method and sol-gel process, the product purity height, cost is lower, is easy to realize large-scale industrial production.The spinel lithium titanate pattern rule of the present invention's preparation, even particle size distribution, crystal formation are grown complete, show the chemical property of excellence as the negative pole of lithium secondary battery.
The present invention has following examples:
[embodiment 1] Li
0.6Ti
1.2Cr
0.05O
3/ w
0.1
First treatment step, wherein the atomic ratio with lithium and titanium is that Li/Ti is lithium carbonate, titanium dioxide and the chromium oxide y=0.05 mixture mixing of x=0.6, be distributed to spirit solvent carry out ball milling 12 hours, the oven dry.
Second treatment step wherein will be heat-treated under 300 ℃ 12 hours at the oven dry thing that described first treatment step obtains.
The 3rd treatment step wherein will obtain the heat treatment material and glucose z=0.1 carried out mixing and ball milling after 12 hours at described second treatment step, under nitrogen protection after carrying out sintering under 750 ℃ 12 hours, cool off 300 mesh sieves.
[embodiment 2] Li
0.6Ti
1.2Cr
0.05O
3/ w
0.2
First treatment step, wherein the atomic ratio with lithium and titanium is that Li/Ti is lithium hydroxide, metatitanic acid and the zirconia y=0.1 mixture mixing of x=1.3, be distributed to acetone solvent carry out ball milling 18 hours, the oven dry.
Second treatment step wherein will be heat-treated under 500 ℃ 16 hours at the oven dry thing that described first treatment step obtains.
The 3rd treatment step wherein will obtain the heat treatment material and furfural resin z=0.2 carried out mixing and ball milling after 10 hours at described second treatment step, under nitrogen protection after carrying out sintering under 800 ℃ 18 hours, cool off 300 mesh sieves.
[embodiment 3] Li
0.6Ti
1.2Cr
0.05O
3/ w
0.4
First treatment step, wherein the atomic ratio with lithium and titanium is that Li/Ti is lithium nitrate, titanium tetrachloride and the zinc oxide y=0.2 mixture mixing of x=1.0, be distributed to spirit solvent carry out ball milling 24 hours, the oven dry.
Second treatment step wherein will be heat-treated under 600 ℃ 24 hours at the oven dry thing that described first treatment step obtains.
The 3rd treatment step wherein will obtain the heat treatment material and pitch z=0.3 carried out mixing and ball milling after 12 hours at described second treatment step, under nitrogen protection after carrying out sintering under 900 ℃ 12 hours, cool off 300 mesh sieves.
[embodiment 4] Li
0.6Ti
1.2Cr
0.05O
3/ w
0.5
First treatment step, wherein the atomic ratio with lithium and titanium is that Li/Ti is lithium acetate, titanium dioxide and the aluminium oxide y=0.08 mixture mixing of x=0.9, be distributed to acetone solvent carry out ball milling 16 hours, the oven dry.
Second treatment step wherein will be heat-treated under 400 ℃ 18 hours at the oven dry thing that described first treatment step obtains.
The 3rd treatment step wherein will obtain the heat treatment material and polyacrylamide z=0.5 carried out mixing and ball milling after 12 hours at described second treatment step, under nitrogen protection after carrying out sintering under 1000 ℃ 24 hours, cool off 300 mesh sieves.
[embodiment 5] Li
0.6Ti
1.2Cr
0.05O
3/ w
0.3
First treatment step wherein is that Li/Ti is that lithium carbonate, titanium dioxide and molybdenum oxide, the niobium oxide of x=0.8 is respectively 0.1,0.2 mixture mixing with the atomic ratio of lithium and titanium, is distributed to spirit solvent carry out ball milling 12 hours, oven dry.
Second treatment step wherein will be heat-treated under 600 ℃ 12 hours at the oven dry thing that described first treatment step obtains.
The 3rd treatment step wherein will obtain the heat treatment material and sucrose z=0.3 carried out mixing and ball milling after 18 hours at described second treatment step, under nitrogen protection after carrying out sintering under 850 ℃ 24 hours, cool off 300 mesh sieves.
[embodiment 6] Li
0.6Ti
1.2Cr
0.05O
3/ w
0.35
First treatment step wherein is that Li/Ti is that lithium hydroxide, metatitanic acid and oxidation brill, nickel oxide, the manganese oxide of x=1.1 all is 0.1 mixture mixing with the atomic ratio of lithium and titanium, is distributed to spirit solvent carry out ball milling 24 hours, oven dry.
Second treatment step wherein will be heat-treated under 550 ℃ 18 hours at the oven dry thing that described first treatment step obtains.
The 3rd treatment step wherein will obtain the heat treatment material and glucose z=0.35 carried out mixing and ball milling after 12 hours at described second treatment step, under nitrogen protection after carrying out sintering under 950 ℃ 18 hours, cool off 300 mesh sieves.
[embodiment 7] Li
0.6Ti
1.2Cr
0.05O
3/ w
0.4
First treatment step wherein is that Li/Ti is that lithium nitrate, titanium dioxide and cupric oxide, vanadic oxide, magnesium oxide, the boron oxide of x=1.05 all is 0.05 mixture mixing with the atomic ratio of lithium and titanium, is distributed to spirit solvent carry out ball milling 18 hours, oven dry.
Second treatment step wherein will be heat-treated under 600 ℃ 24 hours at the oven dry thing that described first treatment step obtains.
The 3rd treatment step wherein will obtain the heat treatment material and glucose z=0.4 carried out mixing and ball milling after 12 hours at described second treatment step, under nitrogen protection after carrying out sintering under 700 ℃ 24 hours, cool off 300 mesh sieves.
The compound lithium titanate material of the spinelle of method for preparing is done negative pole and ferrousphosphate lithium material is done positive pole, with the vinylidene is the pole plate binding agent, make the positive plate and the negative plate of lithium ion battery respectively, with the microporous polypropylene membrane is electrode diaphragm, is dimethyl carbonate with the volume ratio: diethyl carbonate: the 1M lithium hexafluoro phosphate of ethylene carbonate=1: 1: 1 is that electrolyte is assembled into lithium ion battery.
The spinel lithium titanate material of method for preparing is done negative pole and ferrousphosphate lithium material is done positive pole, with the vinylidene is the pole plate binding agent, make the positive plate and the negative plate of lithium ion battery respectively, with the microporous polypropylene membrane is electrode diaphragm, is dimethyl carbonate with the volume ratio: diethyl carbonate: the 1M lithium hexafluoro phosphate of ethylene carbonate=1: 1: 1 is that electrolyte is assembled into lithium ion battery.
Battery performance of the foregoing description such as following table:
Claims (1)
1, a kind of preparation method of spinel lithium titanate, the molecular formula that it is characterized in that spinel lithium titanate is Li
xTi
1.25-yM
yO
3/ w
zM is the doping vario-property material in the formula, and W is a clad material, 0.5≤x≤1.5,0＜y≤0.5,0＜z≤0.5, its preparation methods steps has: (1) is with lithium: the atomic ratio of titanium is to be distributed to behind the lithium source of 0.6-1 and titanium source and the doping vario-property agent mixing to carry out ball milling 8-24 hour in the organic solvent, oven dry, described doping vario-property agent are one or two or more kinds the mixture in the following oxide: Mn, Cr, Co, Cu, Ni, V, Mo, Zn, Al, Mg, B, Zr, Nb, doping is 0-0.5; (2) the oven dry thing that work step (1) is made natural cooling after heat-treating 10-24 hour under 300-600 ℃; (3) material that work step (2) is obtained and clad material carried out mixing and ball milling 8-24 hour; under nitrogen protection with 700-1000 ℃ under carry out sintering 10-24 hour after; cooling is sieved and is obtained spinelle of the present invention and meet lithium titanate, and described clad material is glucose, sucrose, furfural resin, pitch or polyacrylamide.
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|---|---|---|---|
| CNA2009101342471A CN101567442A (en) | 2008-07-28 | 2009-04-10 | Method for preparing spinel lithium titanate |
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|---|---|---|---|
| CN200810140968.9 | 2008-07-28 | ||
| CN200810140968 | 2008-07-28 | ||
| CNA2009101342471A CN101567442A (en) | 2008-07-28 | 2009-04-10 | Method for preparing spinel lithium titanate |
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Cited By (23)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102054963A (en) * | 2010-07-22 | 2011-05-11 | 中信国安盟固利动力科技有限公司 | Titanium acid lithium battery cathode material containing rare metal elements |
| CN102315427A (en) * | 2010-06-29 | 2012-01-11 | 比亚迪股份有限公司 | Cathode active substance for lithium ion secondary battery, preparation method and lithium ion secondary battery |
| CN102496706A (en) * | 2011-12-09 | 2012-06-13 | 东莞市迈科科技有限公司 | Modified lithium titanate and preparation method thereof |
| CN102969492A (en) * | 2012-12-04 | 2013-03-13 | 广州有色金属研究院 | Carbon-coated doping modified lithium titanate and preparation method thereof |
| CN103004005A (en) * | 2010-07-28 | 2013-03-27 | Nec能源元器件株式会社 | Lithium ion secondary battery |
| CN103022497A (en) * | 2011-09-22 | 2013-04-03 | 株式会社东芝 | Active material, method of manufacturing the same, nonaqueous electrolyte battery and battery pack |
| CN103078087A (en) * | 2013-01-30 | 2013-05-01 | 新乡远东电子科技有限公司 | Preparation method of lithium titanate/carbon nano tube composite cathode material |
| CN103151521A (en) * | 2013-02-22 | 2013-06-12 | 中国科学院过程工程研究所 | Positive electrode material of lithium ion battery and preparing method thereof |
| CN103647066A (en) * | 2013-11-15 | 2014-03-19 | 成都兴能新材料有限公司 | Preparation method of lithium titanate anode material containing chromium |
| CN104037414A (en) * | 2014-06-20 | 2014-09-10 | 上海动力储能电池***工程技术有限公司 | Modified lithium-titanate material for lithium ion battery and preparation method of modified lithium-titanate material |
| CN104269547A (en) * | 2014-10-10 | 2015-01-07 | 西安中科新能源科技有限公司 | Preparation method of carbon-coating vanadium-doped titanic oxide |
| TWI501458B (en) * | 2013-06-28 | 2015-09-21 | ||
| CN104979542A (en) * | 2014-04-11 | 2015-10-14 | 上海杉杉科技有限公司 | Modified lithium titanate composite material, preparation method and application thereof |
| CN105406051A (en) * | 2014-09-16 | 2016-03-16 | 河南科隆新能源有限公司 | Composite lithium titanate preparation method |
| CN105449187A (en) * | 2015-12-20 | 2016-03-30 | 华南理工大学 | Preparation method of high-performance co-doped lithium titanate electrode material |
| CN106384819A (en) * | 2016-11-07 | 2017-02-08 | 珠海格力电器股份有限公司 | Carbon-coated lithium titanate material and preparation method thereof as well as lithium-ion battery |
| CN106531987A (en) * | 2016-10-19 | 2017-03-22 | 深圳市沃特玛电池有限公司 | Preparation method of lithium titanate material |
| CN107482208A (en) * | 2017-10-10 | 2017-12-15 | 合肥国轩高科动力能源有限公司 | A kind of method of modifying of nickel ion doped |
| CN108649213A (en) * | 2018-05-23 | 2018-10-12 | 大连理工大学 | A kind of method that ion doping assisted Solid-state method prepares nano lithium titanate |
| CN109659517A (en) * | 2018-11-29 | 2019-04-19 | 郑州中科新兴产业技术研究院 | A kind of preparation method of high-performance lithium titanate composite material |
| CN110323433A (en) * | 2019-07-10 | 2019-10-11 | 银隆新能源股份有限公司 | A kind of lithium titanate composite material and preparation method thereof, lithium ion battery and preparation method thereof |
| CN110918044A (en) * | 2019-12-02 | 2020-03-27 | 尚鹏 | Doped lithium-rich spinel type titanium lithium oxide adsorption material and preparation method thereof |
| CN113871589A (en) * | 2021-09-16 | 2021-12-31 | 南开大学 | Lithium-rich manganese-based positive electrode material coated with lithium titanate assisted by molten salt and preparation method thereof |
-
2009
- 2009-04-10 CN CNA2009101342471A patent/CN101567442A/en active Pending
Cited By (30)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102315427A (en) * | 2010-06-29 | 2012-01-11 | 比亚迪股份有限公司 | Cathode active substance for lithium ion secondary battery, preparation method and lithium ion secondary battery |
| CN102054963A (en) * | 2010-07-22 | 2011-05-11 | 中信国安盟固利动力科技有限公司 | Titanium acid lithium battery cathode material containing rare metal elements |
| CN103004005A (en) * | 2010-07-28 | 2013-03-27 | Nec能源元器件株式会社 | Lithium ion secondary battery |
| CN103022497A (en) * | 2011-09-22 | 2013-04-03 | 株式会社东芝 | Active material, method of manufacturing the same, nonaqueous electrolyte battery and battery pack |
| CN102496706A (en) * | 2011-12-09 | 2012-06-13 | 东莞市迈科科技有限公司 | Modified lithium titanate and preparation method thereof |
| CN102969492B (en) * | 2012-12-04 | 2014-11-12 | 广州有色金属研究院 | Carbon-coated doping modified lithium titanate and preparation method thereof |
| CN102969492A (en) * | 2012-12-04 | 2013-03-13 | 广州有色金属研究院 | Carbon-coated doping modified lithium titanate and preparation method thereof |
| CN103078087A (en) * | 2013-01-30 | 2013-05-01 | 新乡远东电子科技有限公司 | Preparation method of lithium titanate/carbon nano tube composite cathode material |
| CN103078087B (en) * | 2013-01-30 | 2015-11-18 | 新乡远东电子科技有限公司 | A kind of preparation method of lithium titanate/carbon nano tube composite cathode material |
| CN103151521A (en) * | 2013-02-22 | 2013-06-12 | 中国科学院过程工程研究所 | Positive electrode material of lithium ion battery and preparing method thereof |
| CN103151521B (en) * | 2013-02-22 | 2015-12-23 | 中国科学院过程工程研究所 | A kind of anode material for lithium-ion batteries and preparation method thereof |
| TWI501458B (en) * | 2013-06-28 | 2015-09-21 | ||
| CN103647066A (en) * | 2013-11-15 | 2014-03-19 | 成都兴能新材料有限公司 | Preparation method of lithium titanate anode material containing chromium |
| CN104979542B (en) * | 2014-04-11 | 2019-10-29 | 上海杉杉科技有限公司 | A kind of modified lithium titanate composite material and preparation method and application |
| CN104979542A (en) * | 2014-04-11 | 2015-10-14 | 上海杉杉科技有限公司 | Modified lithium titanate composite material, preparation method and application thereof |
| CN104037414A (en) * | 2014-06-20 | 2014-09-10 | 上海动力储能电池***工程技术有限公司 | Modified lithium-titanate material for lithium ion battery and preparation method of modified lithium-titanate material |
| CN105406051A (en) * | 2014-09-16 | 2016-03-16 | 河南科隆新能源有限公司 | Composite lithium titanate preparation method |
| CN104269547A (en) * | 2014-10-10 | 2015-01-07 | 西安中科新能源科技有限公司 | Preparation method of carbon-coating vanadium-doped titanic oxide |
| CN105449187A (en) * | 2015-12-20 | 2016-03-30 | 华南理工大学 | Preparation method of high-performance co-doped lithium titanate electrode material |
| CN106531987A (en) * | 2016-10-19 | 2017-03-22 | 深圳市沃特玛电池有限公司 | Preparation method of lithium titanate material |
| CN106384819A (en) * | 2016-11-07 | 2017-02-08 | 珠海格力电器股份有限公司 | Carbon-coated lithium titanate material and preparation method thereof as well as lithium-ion battery |
| CN107482208A (en) * | 2017-10-10 | 2017-12-15 | 合肥国轩高科动力能源有限公司 | A kind of method of modifying of nickel ion doped |
| CN107482208B (en) * | 2017-10-10 | 2019-09-27 | 合肥国轩高科动力能源有限公司 | A kind of method of modifying of nickel ion doped |
| CN108649213A (en) * | 2018-05-23 | 2018-10-12 | 大连理工大学 | A kind of method that ion doping assisted Solid-state method prepares nano lithium titanate |
| CN109659517A (en) * | 2018-11-29 | 2019-04-19 | 郑州中科新兴产业技术研究院 | A kind of preparation method of high-performance lithium titanate composite material |
| CN110323433A (en) * | 2019-07-10 | 2019-10-11 | 银隆新能源股份有限公司 | A kind of lithium titanate composite material and preparation method thereof, lithium ion battery and preparation method thereof |
| CN110323433B (en) * | 2019-07-10 | 2022-12-20 | 银隆新能源股份有限公司 | Lithium titanate composite material and preparation method thereof, lithium ion battery and preparation method thereof |
| CN110918044A (en) * | 2019-12-02 | 2020-03-27 | 尚鹏 | Doped lithium-rich spinel type titanium lithium oxide adsorption material and preparation method thereof |
| CN113871589A (en) * | 2021-09-16 | 2021-12-31 | 南开大学 | Lithium-rich manganese-based positive electrode material coated with lithium titanate assisted by molten salt and preparation method thereof |
| CN113871589B (en) * | 2021-09-16 | 2023-10-24 | 南开大学 | Lithium-rich manganese-based positive electrode material coated by molten salt-assisted lithium titanate and preparation method thereof |
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Open date: 20091028 |