CN102522536A - Template synthesis method for lithium-ion anode material lithium titanate - Google Patents
Template synthesis method for lithium-ion anode material lithium titanate Download PDFInfo
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Abstract
The invention discloses a template synthesis method for a lithium-ion anode material lithium titanate. The preparation method comprises the following steps of: preparing nanometre TiO2 by P123, X titanium compound, TEOS (tetraethyl orthosilicate), HCl and H2O of certain proportion; and mixing and ball-milling, sintering, cooling and grinding nanometre TiO2 and lithium compound to acquire a lithium titanate product. The invention prepares nanometre titanium dioxide by a template method, achieves the preparation for nanometre lithium titanate material by controlling sintering conditions, and improves rate capability and cycle performances of the nanometre lithium titanate material; the lithium titanate anode material prepared by the method has such characteristics as high purity, small and uniform particles, high charge-discharge specific capacity, high charge-discharge efficiency, good cycle performances, good safety and the like.
Description
Technical field
The present invention relates to a kind of lithium ion battery negative material, especially use template to prepare lithium titanate anode material, belong to electrochemical material preparation and new energy field.
Background technology
Along with progressively riseing of international petroleum Gas Prices, energy problem has been the significant problem that is related to national economy of countries in the world top concern.Along with the continuous development of human social economy with science and technology; Reducing day by day of non-renewable energy resources such as petroleum gas become the restriction mankind's socio-economic development, kept the important obstruction of human society existence, so develops the common recognition that new forms of energy have become countries in the world.
R and D for new energy materials are the focuses in energy research field always.In recent years, the electronics and the information industry development are swift and violent, and the electronic product function is maked rapid progress, and is increasingly high to the performance requirement of power supply, and are accompanied by the development of new-energy automobile industries such as electric automobile, and the jumbo secondary cell exploitation of high-performance is extremely urgent.
Lithium ion battery is on the lithium metal secondary battery basis, to develop and next secondary cell of new generation; Replacing nickel-cadmium cell and metal-hydrogen nickel battery gradually; Have operating voltage height, in light weight, outstanding advantages such as specific energy is big, self discharge is little, have extended cycle life, memory-less effect, non-environmental-pollution; Being electronic installation miniaturization and ideal sources such as video camera, mobile phone, notebook computer and Portable Measurement Instrument, also is the first-selected power supply of the light-duty high-energy power power supply of following used for electric vehicle.Electrode material is the basis of development lithium ion battery, and Development of New Generation high energy positive and negative pole material is current important process.
At present the negative material of lithium ion battery adopts various embedding lithium material with carbon elements mostly, but the current potential of the current potential of carbon electrode and lithium metal is very approaching, and when battery overcharge, carbon electrodes is prone to the precipitating metal lithium, can form dendrite and causes short circuit; Be prone to cause thermal runaway etc. when temperature is too high.Lithium ion can make the material with carbon element structure be damaged, thereby cause the decay of capacity inserting times without number and taking off in the embedding process simultaneously.Therefore, searching can embed lithium under the positive slightly current potential of carbon negative pole current potential, and new negative material cheap and easy to get, safe and reliable and height ratio capacity is a problem highly significant.The titanyl compounds also is one type of negative material studying often now, comprises TiO
2, LiTi
2O
4, Li
4Ti
5O
12, Li
2Ti
3O
7, K
xTi
8O
16, and their doping vario-property material.
Spinel lithium titanate is as lithium ion battery negative material, and the current potential of lithium electrode is 1.55 V (vs Li/Li relatively
+), theoretical capacity is 175 mAh/g, actual specific capacity has reached 150-160 mAh/g.Li
+Inserting and taking off embedding does not almost influence material structure; Have that coulombic efficiency height, cycle performance are good, discharging voltage balance, embedding lithium current potential is high and be difficult for causing that lithium metal separates out; Can have good fail safe in the interval use of the electrolytical burning voltage of most liquid; Also be a kind of " zero strain " material, and material source is wide, clean environment firendly, has possessed the characteristic that the essential charging times of lithium ion battery of future generation is more, charging process is faster, safer.In addition, it also has tangible charge and discharge platform, and the platform capacity can reach more than 90% of discharge capacity, discharges and recharges characteristics such as tangible voltage jump is arranged when finishing,
But high potential brings, and the voltage of battery is low, (intrinsic conductivity is 10 to poorly conductive
-9S/cm), heavy-current discharge be prone to produce problem such as bigger polarization and the commercialization that limited it is used, thereby how to improve the specific discharge capacity of material when high power charging-discharging and become the research emphasis that many researchers mainly concentrate.At present, the high rate performance that improves lithium titanate mainly contains two kinds of approach, and the one, prepare nano level lithium titanate particle; The 2nd, to its mix, coated modified carbon etc.
At present, the preparation lithium titanate mainly adopts high temperature solid-state method in the industry, is with TiO
2With Li
2CO
3Or raw material such as LiOH 800-1000 ℃ synthetic down, general 12-24h of reaction time, it is simple that this method has technology; Be easy to large-scale production, but that shortcoming is the particle diameter of product is wayward, and is micron order mostly; Uniformity is relatively poor, compares with micro crystal, and coarse grained lithium ion insertion reaction path is longer; Be unfavorable for high current charge-discharge, high rate capability is poor.
Method about preparing nanoscale metatitanic acid lithium material is a lot, but does not find as yet at present to utilize P123 to prepare the research of nanoscale metatitanic acid lithium material as template.
Summary of the invention
The present invention aims to provide a kind of template synthesis method of ion cathode material lithium lithium titanate, this method through control lithium titanium when sintering condition realize the preparation of nano barium titanate lithium material improving high rate performance and cycle performance.Characteristics such as the gained material purity is high, particle is little and be evenly distributed, charging and discharging capacity is high, charge efficiency is high, good cycle, fail safe are good, and this preparation technology is simple, cost is low, the preparation process is easy to control.
The present invention adopts following technical scheme to achieve these goals:
The template synthesis method of ion cathode material lithium lithium titanate is characterized in that may further comprise the steps:
(1) preparation nanoscale TiO
2:
A: be 0.0172 P123:X titanium compound in molar ratio: (1-X) TEOS:6HCl:208.33H
2O, wherein X is respectively 0,0.02,0.04,0.06,0.08, takes by weighing stoichiometric P123, uses deionized water dissolving, is stirred to dissolving fully;
B: in above-mentioned solution, add titanium compound, continue to stir 1-3h, add the hydrochloric acid of 2mol/L again, low-grade fever stirs 1-3h;
C: under agitation slowly drip TEOS, after dropwising, continue to stir 23-25h, be transferred in the stainless steel cauldron that polytetrafluoroethylene is a lining crystallization 24-48h under the 80-120 ℃ of condition then;
D: products therefrom, is dried down for 55-65 ℃ to neutral with deionized water wash;
E: with synthetic material in Muffle furnace with 2-6 ℃ of programming rate to 540-560 ℃, insulation 4-6h promptly obtains nanoscale TiO
2
(2) preparation lithium titanate:
A: Li:Ti is that 4.0-4.4:5 takes by weighing the nanoscale TiO that a certain amount of lithium compound and step (1) obtain in molar ratio
2, be dissolved in the solvent, mixing and ball milling 2.5-3.5h, drying and grinding obtains mixture;
B: with gained mixture 750-850 ℃ of following sintering 8-12h in tube furnace, cooling is ground, and promptly gets the lithium titanate product.
The template synthesis method of described ion cathode material lithium lithium titanate is characterized in that: said titanium compound is selected from one or more in Titanium Nitrate, metatitanic acid tetrem fat, metatitanic acid methyl esters, tetraisopropyl titanate, titanium tetrachloride, butyl titanate and the titanyl sulfate.
The template synthesis method of described ion cathode material lithium lithium titanate is characterized in that: said lithium compound is selected from one or more in lithium carbonate, lithium hydroxide, lithium acetate, lithium oxalate, lithium nitrate, lithia, the lithium fluoride.
The template synthesis method of described ion cathode material lithium lithium titanate is characterized in that: described solvent is selected from absolute ethyl alcohol, ethylene glycol or cyclohexane.
Beneficial effect of the present invention:
The present invention through control lithium titanium when sintering condition realize the preparation of nano barium titanate lithium material improving high rate performance and cycle performance.Characteristics such as the gained material purity is high, particle is little and be evenly distributed, charging and discharging capacity is high, charge efficiency is high, good cycle, fail safe are good, and this preparation technology is simple, cost is low, the preparation process is easy to control.
Description of drawings
Fig. 1 is the surface topography of the nano lithium titanate that makes among the embodiment 1.
Fig. 2 is the X-ray diffracting spectrum of the lithium titanate material of embodiment 1 preparation.
Fig. 3 is the charging and discharging curve of lithium titanate electrode material under different multiplying of embodiment 1 preparation, and charge-discharge magnification is 1C, 2C, 5C, 10C.
Embodiment
Embodiment 1:
A. be 0.0172 P123:0.04 butyl titanate: 0.96TEOS:6HCl:208.33H according to mol ratio
2O takes by weighing stoichiometric P123, uses deionized water dissolving, is stirred to dissolving fully; Add, continue to stir 3h, add the hydrochloric acid of 2mol/L again, low-grade fever stirs 3h; Slowly drip TEOS, after dropwising, continue to stir 24h, be transferred in the stainless steel cauldron that polytetrafluoroethylene is a lining crystallization 48h under 100 ℃ of conditions then; Products therefrom, is dried down for 60 ℃ to neutral with deionized water wash; With synthetic material in Muffle furnace with 5 ℃ of programming rates to 550 ℃, insulation 5h promptly obtains nanoscale TiO
2
B. Li:Ti is that 4.2:5 takes by weighing the nanoscale TiO that a certain amount of lithium carbonate and steps A obtain in molar ratio
2, be dissolved in the anhydrous ethanol solvent, mixing and ball milling 3 hours, drying and grinding obtains mixture; With gained mixture 850 ℃ of following sintering 12h in tube furnace, cooling is ground, and promptly obtains the lithium titanate product.The surface topography of this lithium titanate material is as shown in Figure 1, can find out that lithium titanate demonstrates good particle.Its X-ray diffracting spectrum is as shown in Figure 2, and can find out does not have tangible impurity peaks in this spectrogram, shows that prepared material is pure phase lithium titanate.
Embodiment 2:
A. be 0.0172P123:0.02 butyl titanate: 0.98TEOS:6HCl:208.33H according to mol ratio
2O takes by weighing stoichiometric P123, uses deionized water dissolving, is stirred to dissolving fully; Add butyl titanate, continue to stir 2h, add the hydrochloric acid of 2mol/L again, low-grade fever stirs 2h; Slowly drip TEOS, dropwise, continue to stir 24h, be transferred in the stainless steel cauldron that polytetrafluoroethylene is a lining crystallization 24h under 90 ℃ of conditions then; Products therefrom, is dried down for 60 ℃ to neutral with deionized water wash; With synthetic material in Muffle furnace with 5 ℃ of programming rates to 550 ℃, insulation 5h promptly obtains nanoscale TiO
2
B. Li:Ti is that 4.2:5 takes by weighing the nanoscale TiO that a certain amount of lithium carbonate and steps A obtain in molar ratio
2, be dissolved in the anhydrous ethanol solvent, mixing and ball milling 3h, drying and grinding obtains mixture; With gained mixture 850 ℃ of following sintering 10h in tube furnace, cooling is ground, and promptly obtains the lithium titanate product.
Embodiment 3:
A. be 0.0172P123:0.06 butyl titanate: 0.94TEOS:6HCl:208.33H according to mol ratio
2O takes by weighing stoichiometric P123, uses deionized water dissolving, is stirred to dissolving fully; Add butyl titanate, continue to stir 3h, add the hydrochloric acid of 2mol/L again, low-grade fever stirs 3h, slowly drips TEOS, after dropwising, continues to stir 24h, is transferred in the stainless steel cauldron that polytetrafluoroethylene is a lining crystallization 48h under 120 ℃ of conditions then; Products therefrom, is dried down for 60 ℃ to neutral with deionized water wash; With synthetic material in Muffle furnace with 3 ℃ of programming rates to 550 ℃, insulation 5h promptly obtains nanoscale TiO
2
B. Li:Ti is that 4.2:5 takes by weighing the nanoscale TiO that a certain amount of lithium carbonate and steps A obtain in molar ratio
2, be dissolved in the anhydrous ethanol solvent, mixing and ball milling 3 hours, drying and grinding obtains mixture; With gained mixture 780 ℃ of following sintering 12h in tube furnace, cooling is ground, and promptly gets the lithium titanate product.
Embodiment 4:
A. be 0.0172P123:0.08 butyl titanate: 0.92TEOS:6HCl:208.33H according to mol ratio
2O takes by weighing stoichiometric P123, uses deionized water dissolving, is stirred to dissolving fully; Add butyl titanate, continue to stir 2h, add the hydrochloric acid of 2mol/L again, low-grade fever stirs 3h, slowly drips TEOS, after dropwising, continues to stir 24h, is transferred in the stainless steel cauldron that polytetrafluoroethylene is a lining crystallization 48h under 100 ℃ of conditions then; Products therefrom, is dried down for 60 ℃ to neutral with deionized water wash; With synthetic material in Muffle furnace with 3 ℃ of programming rates to 550 ℃, insulation 5h promptly obtains nanoscale TiO
2
B. Li:Ti is that 4.2:5 takes by weighing the nanoscale TiO that a certain amount of lithium carbonate and steps A obtain in molar ratio
2, be dissolved in the anhydrous ethanol solvent, mixing and ball milling 3 hours, drying and grinding obtains mixture; With gained mixture 750 ℃ of following sintering 8h in tube furnace, cooling is ground, and promptly gets the lithium titanate product.
Embodiment 5:
A. be 0.0172P123:0.04 tetraisopropyl titanate: 0.96TEOS:6HCl:208.33H according to mol ratio
2O takes by weighing stoichiometric P123, uses deionized water dissolving, is stirred to dissolving fully; Add tetraisopropyl titanate, continue to stir 3h, add the hydrochloric acid of 2mol/L again, low-grade fever stirs 3h, slowly drips TEOS, after dropwising, continues to stir 24h, is transferred in the stainless steel cauldron that polytetrafluoroethylene is a lining crystallization 48h under 100 ℃ of conditions then; Products therefrom, is dried down for 60 ℃ to neutral with deionized water wash; With synthetic material in Muffle furnace with 3 ℃ of programming rates to 550 ℃, insulation 5h promptly obtains nanoscale TiO
2
B. Li:Ti is that 4.2:5 takes by weighing the nanoscale TiO that a certain amount of lithium carbonate and steps A obtain in molar ratio
2, be dissolved in the anhydrous ethanol solvent, mixing and ball milling 3h, drying and grinding obtains mixture; With gained mixture 850 ℃ of following sintering 12h in tube furnace, cooling is ground, and promptly gets the lithium titanate product.
Embodiment 6:
A. be 0.0172P123:0.02 tetraisopropyl titanate: 0.98TEOS:6HCl:208.33H according to mol ratio
2O takes by weighing stoichiometric P123, uses deionized water dissolving, is stirred to dissolving fully; Add tetraisopropyl titanate, continue to stir 3h, add the hydrochloric acid of 2mol/L again, low-grade fever stirs 2h, slowly drips TEOS, after dropwising, continues to stir 24h, is transferred in the stainless steel cauldron that polytetrafluoroethylene is a lining crystallization 48h under 90 ℃ of conditions then; Products therefrom, is dried down for 60 ℃ to neutral with deionized water wash; With synthetic material in Muffle furnace with 3 ℃ of programming rates to 550 ℃, insulation 5h promptly obtains nanoscale TiO
2
B. Li:Ti is that 4.2:5 takes by weighing the nanoscale TiO that a certain amount of lithium carbonate and steps A obtain in molar ratio
2, be dissolved in the anhydrous ethanol solvent, mixing and ball milling 3h, drying and grinding obtains mixture; With gained mixture 850 ℃ of following sintering 8h in tube furnace, cooling is ground, and promptly gets the lithium titanate product.
The lithium titanate material and the metal lithium sheet of gained in the foregoing description are assembled into battery and carry out charge-discharge test with 1C, 2C, 5C, 10C multiplying power respectively.Wherein the prepared lithium titanate material charging and discharging curve of embodiment 1 is as shown in Figure 3; Can find out; The 1C specific discharge capacity is 169.99 mAh/g, and the 2C specific discharge capacity is 162.36 mAh/g, and the 5C specific discharge capacity is 149.60 mAh/g; The 10C specific discharge capacity is 122.84 mAh/g, demonstrates good high rate performance.
Embodiment result shows, through template synthesis of nano titanium dioxide, and further prepares lithium titanate material, compares with the micron lithium titanate of commonsense method preparation, and its high rate performance has obtained obvious improvement.Wherein be 0.0172 P123:0.04 titanium compound: 0.96TEOS:6HCl:208.33H in molar ratio
2The TiO of O preparation
2, and the lithium titanate material that further obtains at 850 ℃ of following sintering 12h, charge-discharge performance is good, shows excellent chemical property, is good lithium ion battery negative material.
In the foregoing description; Butyl titanate and tetraisopropyl titanate have only been enumerated in the titanium source; Lithium carbonate has only been enumerated in the lithium source, and solvent has only been enumerated the situation of absolute ethyl alcohol, selects other titanium sources such as Titanium Nitrate, metatitanic acid tetrem fat, metatitanic acid methyl esters, titanium tetrachloride and titanyl sulfate etc. for use; Select other lithium sources such as lithium hydroxide, lithium acetate, lithium oxalate, lithium nitrate, lithia and lithium fluoride etc. for use, solvent such as ethylene glycol are similar with the experimental result that cyclohexane is produced.
Claims (4)
1. the template synthesis method of an ion cathode material lithium lithium titanate is characterized in that may further comprise the steps:
(1) preparation nanoscale TiO
2:
A: be 0.0172 P123:X titanium compound in molar ratio: (1-X) TEOS:6HCl:208.33H
2O, wherein X is respectively 0,0.02,0.04,0.06,0.08, takes by weighing stoichiometric P123, uses deionized water dissolving, is stirred to dissolving fully;
B: in above-mentioned solution, add titanium compound, continue to stir 1-3h, add the hydrochloric acid of 2mol/L again, low-grade fever stirs 1-3h;
C: under agitation slowly drip TEOS, after dropwising, continue to stir 23-25h, be transferred in the stainless steel cauldron that polytetrafluoroethylene is a lining crystallization 24-48h under the 80-120 ℃ of condition then;
D: products therefrom, is dried down for 55-65 ℃ to neutral with deionized water wash;
E: with synthetic material in Muffle furnace with 2-6 ℃ of programming rate to 540-560 ℃, insulation 4-6h promptly obtains nanoscale TiO
2
(2) preparation lithium titanate:
A: Li:Ti is that 4.0-4.4:5 takes by weighing the nanoscale TiO that a certain amount of lithium compound and step (1) obtain in molar ratio
2, be dissolved in the solvent, mixing and ball milling 2.5-3.5h, drying and grinding obtains mixture;
B: with gained mixture 750-850 ℃ of following sintering 8-12h in tube furnace, cooling is ground, and promptly gets the lithium titanate product.
2. according to the template synthesis method of claims 1 described ion cathode material lithium lithium titanate, it is characterized in that: said titanium compound is selected from one or more in Titanium Nitrate, metatitanic acid tetrem fat, metatitanic acid methyl esters, tetraisopropyl titanate, titanium tetrachloride, butyl titanate and the titanyl sulfate.
3. according to the template synthesis method of claims 1 described ion cathode material lithium lithium titanate, it is characterized in that: said lithium compound is selected from one or more in lithium carbonate, lithium hydroxide, lithium acetate, lithium oxalate, lithium nitrate, lithia, the lithium fluoride.
4. the template synthesis method of ion cathode material lithium lithium titanate according to claim 1 is characterized in that: described solvent is selected from absolute ethyl alcohol, ethylene glycol or cyclohexane.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102903899A (en) * | 2012-07-20 | 2013-01-30 | 合肥国轩高科动力能源有限公司 | Method for synthesizing SiO2 lithium ion battery cathode material lithium titanate |
| CN102945952A (en) * | 2012-12-05 | 2013-02-27 | 吉林大学 | Method for preparing anode material carbon coated lithium titanate for lithium ion power batteries |
| CN103682294A (en) * | 2012-09-24 | 2014-03-26 | 中信国安盟固利动力科技有限公司 | Preparation method for synthesizing lithium titanate nanosphere |
| CN106145184A (en) * | 2016-06-21 | 2016-11-23 | 河南师范大学 | One has the high activity { TiO of 111} exposure high preferred orientation2the preparation method of microsphere |
| CN106450262A (en) * | 2016-10-28 | 2017-02-22 | 上海纳米技术及应用国家工程研究中心有限公司 | Hollow-sphere-shaped lithium titanate anode material and preparation method and application thereof |
| CN113964315A (en) * | 2021-10-14 | 2022-01-21 | 北京师范大学 | Preparation method and application of large-size two-dimensional lithium titanate nanosheet |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102903899A (en) * | 2012-07-20 | 2013-01-30 | 合肥国轩高科动力能源有限公司 | Method for synthesizing SiO2 lithium ion battery cathode material lithium titanate |
| CN103682294A (en) * | 2012-09-24 | 2014-03-26 | 中信国安盟固利动力科技有限公司 | Preparation method for synthesizing lithium titanate nanosphere |
| CN103682294B (en) * | 2012-09-24 | 2016-08-03 | 中信国安盟固利动力科技有限公司 | A kind of preparation method synthesizing lithium titanate nanosphere |
| CN102945952A (en) * | 2012-12-05 | 2013-02-27 | 吉林大学 | Method for preparing anode material carbon coated lithium titanate for lithium ion power batteries |
| CN106145184A (en) * | 2016-06-21 | 2016-11-23 | 河南师范大学 | One has the high activity { TiO of 111} exposure high preferred orientation2the preparation method of microsphere |
| CN106450262A (en) * | 2016-10-28 | 2017-02-22 | 上海纳米技术及应用国家工程研究中心有限公司 | Hollow-sphere-shaped lithium titanate anode material and preparation method and application thereof |
| CN106450262B (en) * | 2016-10-28 | 2019-04-16 | 上海纳米技术及应用国家工程研究中心有限公司 | A kind of hollow sphere pattern lithium titanate anode material and preparation method and application |
| CN113964315A (en) * | 2021-10-14 | 2022-01-21 | 北京师范大学 | Preparation method and application of large-size two-dimensional lithium titanate nanosheet |
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Address after: 230000 Yaohai Industrial Park, Anhui, Hefei No. D weft Road, No. 7 Applicant after: Hefei Guoxuan High-Tech Power Energy Co., Ltd. Address before: 230000 Yaohai Industrial Park, Anhui, Hefei No. D weft Road, No. 7 Applicant before: Hefei Guoxuan High-Tech Power Energy Co., Ltd. |
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Free format text: CORRECT: APPLICANT; FROM: HEFEI GUOXUAN HIGH-TECH POWER ENERGY CO., LTD. TO: HEFEI GUOXUAN HIGH-TECH POWER ENERGY CO., LTD. |
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Application publication date: 20120627 |