CN105406051A - Composite lithium titanate preparation method - Google Patents
Composite lithium titanate preparation method Download PDFInfo
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- CN105406051A CN105406051A CN201410473412.7A CN201410473412A CN105406051A CN 105406051 A CN105406051 A CN 105406051A CN 201410473412 A CN201410473412 A CN 201410473412A CN 105406051 A CN105406051 A CN 105406051A
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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
The invention relates to a composite lithium titanate preparation method, which comprises: 1) uniformly mixing a lithium source compound, a titanium source compound and the compound of a doped modifier M according to a molar ratio of Li to Ti to M of (0.6-1):1:(0.06-0.3), dispersing in an organic solvent, carrying out ball milling for 6-12 h, sintering for 6-12 h at a temperature of 80-120 DEG C, and drying; 2) carrying out a heat treatment on the dried product obtained in the step 1) for 8-20 h at a temperature of 400-600 DEG C, and naturally cooling; and 3) carrying out mixing ball milling on the treated material obtained in the step 2) and a cladding material for 6-12 h according to a weight ratio of 100:(5-20), sintering for 8-20 h at a temperature of 700-950 DEG C under the protection of nitrogen, cooling, and screening with a 300 mesh sieve. According to the present invention, the preparation method has characteristics of rapid reaction, high product purity, low cost, and easy large-scale industrial production achieving.
Description
Technical field
The invention belongs to lithium battery material field, be specifically related to a kind of preparation method of compound lithium titanate.
Background technology
In recent years, the research and development of lithium ion battery is worldwide paid attention to widely and is paid close attention to.The high specific energy of lithium ion battery, high voltage and oligosaprobic characteristic make it become current mobile phone, the good power supply of notebook computer and video camera, and are one of important candidates of following electric powered motor power supply.In current commercialization or part commercial lithium ion battery metal oxide-type electrode material, lithium-titanium composite oxide Li
4ti
5o
12lithium ion battery negative material can be made, there is spinel structure, the end of the eighties, the positive electrode of Zeng Zuowei lithium ion battery was studied, but because its and energy density on the low side relative to lithium current potential also lower (theoretical capacity is 175mAh/g), thus decreases the research interest of people.There are some researches show Li afterwards
4ti
5o
12in charge and discharge process, its skeleton structure changes hardly, need to generate passivating film unlike material with carbon element, first time, efficiency for charge-discharge was up to more than 90%, and was a kind of zero strain material, keep crystalchecked in charge and discharge process, there is good cycle performance.Especially, under the requirement of fast charging and discharging, its skeleton structure changes crystalchecked hardly, solves the problem such as quick charge and Long-Time Service of current electric powered motor power supply.At present, the synthetic method of lithium titanate is many, usually has solid reaction process, high-energy ball milling method and sol-gel process.But Li prepared by said method
4ti
5o
12still there is certain defect in the cycle performance of material.
Because the conductivity of lithium titanate itself is very poor, when high power charging-discharging, capacity can not well be brought into play, therefore needs to improve its conductivity and cycle performance by doping, coated etc. to its modification.
Summary of the invention
The object of this invention is to provide a kind of preparation method with the compound lithium titanate of high-rate discharge ability and excellent cycle performance.
The preparation method of a kind of compound lithium titanate of the present invention comprises the following steps:
1) be (0.6-1): 1:(0.06-0.3 by the compound of Li source compound, titanium source compound and doping vario-property agent M according to Li:Ti:M mol ratio) mix, be distributed to organic solvent and carry out ball milling 6-12 hour, at 80-120 DEG C, then sinter oven dry in 6-12 hour;
2) by step 1) drying object that obtains heat-treats after 8-20 hour and naturally cools at 400-600 DEG C;
3) by step 2) the heat treatment material that obtains and clad material 100:(5-20 by weight) carry out mixing and ball milling 6-12 hour, then in nitrogen protection, after carrying out sintering 8-20 hour at 700-950 DEG C, cooled 300 mesh sieves.
Described Li source compound is lithium nitrate, lithium acetate, lithium carbonate or lithium hydroxide.
Described titanium source compound is titanium dioxide, metatitanic acid, titanium tetrachloride or butyl titanate.
The compound of described doping vario-property agent M is at least one in the oxide of Al, Mg, B, Zr, Nb, Mn, Cr, Co, Si, Ni, V, Mo, Zn.
Described clad material is at least one in polyacrylamide, carboxymethyl cellulose, glucose, sucrose, furfural resin, pitch.
Described organic solvent is alcohol, isopropyl alcohol or acetone.
The molecular formula of the product that described preparation method obtains is Li
xti
1.25-ym
yo
3, 0.5≤x≤1.5,0≤y≤0.5.
The preparation method of compound lithium titanate of the present invention, is formed the electrode material of good conductivity, improves its high rate capability by coated or doping; The nanochannel of particle adds the effective affecting acreage of electrode and the passage of lithium ion turnover, and make electrode material have very high reversible electrochemical capacity, less specific area improves its initial coulomb efficiency and cyclical stability.
The compound lithium titanate of spinelle with uniform properties Sum fanction crystal face that the preparation method of compound lithium titanate of the present invention obtains reveals significant stability and its high rate capability, the nanochannel of particle adds the effective affecting acreage of electrode and the passage of lithium ion turnover, electrode material is made to have very high reversible electrochemical capacity, less specific area improves its initial coulomb efficiency and cyclical stability, crystal structure does not damage by lithium embedding/deintercalation, and have stable service life cycle, high rate during charging-discharging significantly improves.
Embodiment
By the following examples detailed process of the present invention is described further.
Embodiment 1
The preparation method of compound lithium titanate comprises the following steps:
1) be that 0.6:1:0.06 mixes by lithium carbonate, titanium dioxide and chromium oxide according to Li:Ti:Cr mol ratio, be distributed to spirit solvent and carry out ball milling 8 hours, then 80 DEG C of sintering are dried for 6 hours;
2) by step 1) drying object that obtains heat-treats after 10 hours and naturally cools at 400 DEG C;
3) by step 2) the heat treatment material that obtains and glucose by weight 100:10 carry out mixing and ball milling after 10 hours, at 750 DEG C, carry out sintering under nitrogen protection after 15 hours, cooled 300 mesh sieves.
Embodiment 2
The preparation method of compound lithium titanate comprises the following steps:
1) be that 0.8:1:0.1 mixes by lithium carbonate, titanium dioxide and zirconia according to Li:Ti:Zr mol ratio, be distributed to acetone solvent and carry out ball milling 12 hours, then 90 DEG C of sintering are dried for 8 hours;
2) by step 1) drying object that obtains heat-treats after 18 hours and naturally cools at 500 DEG C;
3) by step 2) the heat treatment material that obtains and furfural resin by weight 100:20 carry out mixing and ball milling after 10 hours, at 800 DEG C, carry out sintering under nitrogen protection after 16 hours, cooled 300 mesh sieves.
Embodiment 3
The preparation method of compound lithium titanate comprises the following steps:
1) be that 1:1:0.2 mixes by lithium nitrate, titanium tetrachloride and zinc oxide according to Li:Ti:Zn mol ratio, be distributed to spirit solvent and carry out ball milling 8 hours, then 100 DEG C of sintering are dried for 8 hours;
2) by step 1) drying object that obtains heat-treats after 20 hours and naturally cools at 600 DEG C;
3) by step 2) the heat treatment material that obtains and pitch by weight 100:10 carry out mixing and ball milling after 12 hours, at 900 DEG C, carry out sintering under nitrogen protection after 18 hours, cooled 300 mesh sieves.
Embodiment 4
The preparation method of compound lithium titanate comprises the following steps:
1) be that 0.9:1:0.08 mixes by lithium acetate, titanium dioxide and aluminium oxide according to Li:Ti:Al mol ratio, be distributed to acetone solvent and carry out ball milling 7 hours, then 120 DEG C of sintering are dried for 10 hours;
2) by step 1) drying object that obtains heat-treats after 19 hours and naturally cools at 450 DEG C;
3) will in step 2) obtain be my heat treatment material and polyacrylamide by weight 100:18 carry out mixing and ball milling after 12 hours, at 900 DEG C, carry out sintering under nitrogen protection after 20 hours, cooled 300 mesh sieves.
Embodiment 5
The preparation method of compound lithium titanate comprises the following steps:
1) be that 0.8:1:0.1:0.2 mixes by lithium carbonate, titanium dioxide, molybdenum oxide and niobium oxide according to Li:Ti:Mo:Nb mol ratio, be distributed to spirit solvent and carry out ball milling 9 hours, then 110 DEG C of sintering are dried for 12 hours;
2) by step 1) drying object that obtains heat-treats after 12 hours and naturally cools at 550 DEG C;
3) by step 2) the heat treatment material that obtains and sucrose by weight 100:12 carry out mixing and ball milling after 11 hours, at 850 DEG C, carry out sintering under nitrogen protection after 20 hours, cooled 300 mesh sieves.
Embodiment 6
The preparation method of compound lithium titanate comprises the following steps:
1) be that 0.85:1:0.1:0.1:0.1 mixes by lithium hydroxide, metatitanic acid, cobalt oxide, nickel oxide and manganese oxide according to Li:Ti:Co:Ni:Mn mol ratio, be distributed to isopropanol solvent and carry out ball milling 10 hours, then 95 DEG C of sintering are dried for 12 hours;
2) by step 1) drying object that obtains heat-treats after 18 hours and naturally cools at 480 DEG C;
3) by step 2) the heat treatment material that obtains and glucose by weight 100:8 carry out mixing and ball milling after 10 hours, at 950 DEG C, carry out sintering 18 hours under nitrogen protection, cooled 300 mesh sieves.
Embodiment 7
The preparation method of compound lithium titanate comprises the following steps:
1) be that 0.75:1:0.5:0.5:0.5 mixes by lithium nitrate, butyl titanate, silica, vanadic oxide, magnesium oxide and boron oxide according to Li:Ti:V:Mg:B mol ratio, be distributed to spirit solvent and carry out ball milling 12 hours, then 105 DEG C of sintering are dried for 8 hours;
2) by step 1) drying object that obtains heat-treats after 20 hours and naturally cools at 500 DEG C;
3) by step 2) the heat treatment material that obtains and carboxymethyl cellulose by weight 100:5 carry out mixing and ball milling after 12 hours, at 700 DEG C, carry out sintering under nitrogen protection after 20 hours, cooled 300 mesh sieves.
The compound lithium titanate material of spinelle preparation method of the present invention obtained does negative pole, ferrousphosphate lithium material does positive pole, take vinylidene as pole plate binding agent, make positive plate and the negative plate of lithium ion battery respectively, being electrode diaphragm with microporous polypropylene membrane, take volume ratio as dimethyl carbonate: diethyl carbonate: the 1M lithium hexafluoro phosphate of ethylene carbonate=1:1:1 is that electrolyte is assembled into lithium ion battery.Performance test is carried out to obtained lithium ion battery, the results are shown in Table 1, the discharge capacity first of lithium ion battery is 155-170mAh/g, 10C charge/discharge capacity is 130-142mAh/g, discharge platform voltage is 1.97-2.01V, and 1000 circulation volume conservation rates are 91-97%.
Table 1
The preparation method of compound lithium titanate of the present invention, doping vario-property agent doping composition, there is spherical or that class is spherical microscopic feature, porous nano passage is comprised in particle, take low temperature molten salt as synthetic medium, use the coated rear formation second particle of nano-carbon coated material again, by there is solid state reaction kinetics spinel type lithium titanate.In preparation process, the diffusion velocity of reactant in low temperature molten salt is apparently higher than in conventional solid environment, and this can fast reaction speed effectively, reduces reaction temperature, Reaction time shorten, energy savings; And the method is integrated with the advantage of conventional high-temperature solid phase method and sol-gel process, and product purity is high, and cost is lower, be easy to realize large-scale industrial production.The pattern rule of the spinel lithium titanate that preparation method of the present invention obtains, even particle size distribution, crystal formation are complete, and the negative pole as lithium secondary battery shows excellent chemical property.
Claims (7)
1. a preparation method for compound lithium titanate, is characterized in that comprising the following steps:
1) be (0.6-1): 1:(0.06-0.3 by the compound of Li source compound, titanium source compound and doping vario-property agent M according to Li:Ti:M mol ratio) mix, be distributed to organic solvent and carry out ball milling 6-12 hour, at 80-120 DEG C, then sinter oven dry in 6-12 hour;
2) by step 1) drying object that obtains heat-treats after 8-20 hour and naturally cools at 400-600 DEG C;
3) by step 2) the heat treatment material that obtains and clad material 100:(5-20 by weight) carry out mixing and ball milling 6-12 hour, then in nitrogen protection, after carrying out sintering 8-20 hour at 700-950 DEG C, cooled 300 mesh sieves.
2. the preparation method of compound lithium titanate according to claim 1, is characterized in that: described Li source compound is lithium nitrate, lithium acetate, lithium carbonate or lithium hydroxide.
3. the preparation method of compound lithium titanate according to claim 1, is characterized in that: described titanium source compound is titanium dioxide, metatitanic acid, titanium tetrachloride or butyl titanate.
4. the preparation method of compound lithium titanate according to claim 1, is characterized in that: the compound of described doping vario-property agent M is at least one in the oxide of Al, Mg, B, Zr, Nb, Mn, Cr, Co, Si, Ni, V, Mo, Zn.
5. the preparation method of compound lithium titanate according to claim 1, is characterized in that: described clad material is at least one in polyacrylamide, carboxymethyl cellulose, glucose, sucrose, furfural resin, pitch.
6. the preparation method of compound lithium titanate according to claim 1, is characterized in that: described organic solvent is alcohol, isopropyl alcohol or acetone.
7. the preparation method of compound lithium titanate according to claim 1, is characterized in that: the molecular formula of the product that described preparation method obtains is Li
xti
1.25-ym
yo
3, 0.5≤x≤1.5,0≤y≤0.5.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105870437A (en) * | 2016-05-10 | 2016-08-17 | 北京泰和九思科技有限公司 | Shape-controllable nano lithium titanate composite and preparation method thereof and lithium ion battery |
| CN106159250A (en) * | 2016-08-15 | 2016-11-23 | 四川兴能新材料有限公司 | A kind of metatitanic acid is the lithium titanate electrode material in titanium source and preparation method thereof |
| CN106252644A (en) * | 2016-08-26 | 2016-12-21 | 浙江长兴金太阳电源有限公司 | A kind of preparation method of lithium ion battery thulium doped titanic acid lithium anode material |
| CN107331869A (en) * | 2017-01-21 | 2017-11-07 | 深圳市瑞能达科技有限公司 | It is a kind of to lift the compound additive of lithium titanate electric material cryogenic property |
| CN108682832A (en) * | 2018-06-11 | 2018-10-19 | 四会市恒星智能科技有限公司 | Lithium battery composite negative pole material and preparation method thereof |
| CN109301236A (en) * | 2018-08-17 | 2019-02-01 | 中北润良新能源汽车(徐州)股份有限公司 | A kind of solid reaction process improving 1.55V lithium titanate battery capacity |
| CN109319830A (en) * | 2018-11-13 | 2019-02-12 | 北方奥钛纳米技术有限公司 | Lithium titanate material and preparation method thereof, negative electrode tab, battery |
| 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 |
| CN110459750A (en) * | 2019-08-21 | 2019-11-15 | 宋婷 | A kind of cathode material of lithium-ion power battery and preparation method thereof |
| CN113594437A (en) * | 2021-07-21 | 2021-11-02 | 安徽天时新能源科技有限公司 | Negative active material of low-temperature lithium battery and preparation method thereof |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105870437A (en) * | 2016-05-10 | 2016-08-17 | 北京泰和九思科技有限公司 | Shape-controllable nano lithium titanate composite and preparation method thereof and lithium ion battery |
| CN106159250A (en) * | 2016-08-15 | 2016-11-23 | 四川兴能新材料有限公司 | A kind of metatitanic acid is the lithium titanate electrode material in titanium source and preparation method thereof |
| CN106252644A (en) * | 2016-08-26 | 2016-12-21 | 浙江长兴金太阳电源有限公司 | A kind of preparation method of lithium ion battery thulium doped titanic acid lithium anode material |
| CN107331869A (en) * | 2017-01-21 | 2017-11-07 | 深圳市瑞能达科技有限公司 | It is a kind of to lift the compound additive of lithium titanate electric material cryogenic property |
| CN108682832A (en) * | 2018-06-11 | 2018-10-19 | 四会市恒星智能科技有限公司 | Lithium battery composite negative pole material and preparation method thereof |
| CN109301236A (en) * | 2018-08-17 | 2019-02-01 | 中北润良新能源汽车(徐州)股份有限公司 | A kind of solid reaction process improving 1.55V lithium titanate battery capacity |
| CN109319830A (en) * | 2018-11-13 | 2019-02-12 | 北方奥钛纳米技术有限公司 | Lithium titanate material and preparation method thereof, negative electrode tab, battery |
| 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 |
| CN110459750A (en) * | 2019-08-21 | 2019-11-15 | 宋婷 | A kind of cathode material of lithium-ion power battery and preparation method thereof |
| CN113594437A (en) * | 2021-07-21 | 2021-11-02 | 安徽天时新能源科技有限公司 | Negative active material of low-temperature lithium battery and preparation method thereof |
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Application publication date: 20160316 |