CN102442695A - Preparation method of lithium titanate material of lithium ion battery - Google Patents
Preparation method of lithium titanate material of lithium ion battery Download PDFInfo
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- CN102442695A CN102442695A CN2010105050545A CN201010505054A CN102442695A CN 102442695 A CN102442695 A CN 102442695A CN 2010105050545 A CN2010105050545 A CN 2010105050545A CN 201010505054 A CN201010505054 A CN 201010505054A CN 102442695 A CN102442695 A CN 102442695A
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- lithium titanate
- ion battery
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- lithium ion
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- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 55
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 239000000463 material Substances 0.000 title claims abstract description 29
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000001816 cooling Methods 0.000 claims abstract description 18
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 9
- 229910003002 lithium salt Inorganic materials 0.000 claims abstract description 6
- 159000000002 lithium salts Chemical class 0.000 claims abstract description 6
- 239000000654 additive Substances 0.000 claims abstract description 5
- 230000000996 additive effect Effects 0.000 claims abstract description 5
- 238000010792 warming Methods 0.000 claims description 16
- 239000003795 chemical substances by application Substances 0.000 claims description 9
- 238000005245 sintering Methods 0.000 claims description 9
- 238000001291 vacuum drying Methods 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- 239000010405 anode material Substances 0.000 claims description 8
- 239000006185 dispersion Substances 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 8
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- -1 acetate compound Chemical class 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 claims 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims 1
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims 1
- 150000001875 compounds Chemical class 0.000 claims 1
- YNQRWVCLAIUHHI-UHFFFAOYSA-L dilithium;oxalate Chemical compound [Li+].[Li+].[O-]C(=O)C([O-])=O YNQRWVCLAIUHHI-UHFFFAOYSA-L 0.000 claims 1
- PQVSTLUFSYVLTO-UHFFFAOYSA-N ethyl n-ethoxycarbonylcarbamate Chemical compound CCOC(=O)NC(=O)OCC PQVSTLUFSYVLTO-UHFFFAOYSA-N 0.000 claims 1
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims 1
- GLXDVVHUTZTUQK-UHFFFAOYSA-M lithium hydroxide monohydrate Substances [Li+].O.[OH-] GLXDVVHUTZTUQK-UHFFFAOYSA-M 0.000 claims 1
- 229940040692 lithium hydroxide monohydrate Drugs 0.000 claims 1
- FUJCRWPEOMXPAD-UHFFFAOYSA-N lithium oxide Chemical compound [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 claims 1
- 229910001947 lithium oxide Inorganic materials 0.000 claims 1
- 150000002823 nitrates Chemical class 0.000 claims 1
- 238000002156 mixing Methods 0.000 abstract description 8
- 238000010438 heat treatment Methods 0.000 abstract description 5
- 238000009826 distribution Methods 0.000 abstract description 3
- 239000002243 precursor Substances 0.000 abstract description 3
- 239000002245 particle Substances 0.000 abstract description 2
- 238000000227 grinding Methods 0.000 abstract 2
- 239000002270 dispersing agent Substances 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 239000007773 negative electrode material Substances 0.000 abstract 1
- 239000004408 titanium dioxide Substances 0.000 abstract 1
- 238000011068 loading method Methods 0.000 description 7
- 238000000034 method Methods 0.000 description 7
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- 229910010413 TiO 2 Inorganic materials 0.000 description 6
- 230000014759 maintenance of location Effects 0.000 description 6
- 238000000498 ball milling Methods 0.000 description 5
- 238000005303 weighing Methods 0.000 description 5
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 4
- 230000010354 integration Effects 0.000 description 4
- 238000004581 coalescence Methods 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 230000003245 working effect Effects 0.000 description 2
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 2
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910013553 LiNO Inorganic materials 0.000 description 1
- 229910013870 LiPF 6 Inorganic materials 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 1
- 239000006230 acetylene black Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- WYYQVWLEPYFFLP-UHFFFAOYSA-K chromium(3+);triacetate Chemical compound [Cr+3].CC([O-])=O.CC([O-])=O.CC([O-])=O WYYQVWLEPYFFLP-UHFFFAOYSA-K 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- PDKHNCYLMVRIFV-UHFFFAOYSA-H molybdenum;hexachloride Chemical compound [Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[Mo] PDKHNCYLMVRIFV-UHFFFAOYSA-H 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229920003987 resole Polymers 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 238000003836 solid-state method Methods 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000011010 synthetic spinel Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
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Abstract
The invention discloses a preparation method of a lithium titanate material of a lithium ion battery, which comprises the following steps: a: mixing lithium salt and titanium dioxide according to a molar ratio of 0.84, adding a dispersing agent, grinding and mixing, and then drying in vacuum to obtain a precursor; b: heating the prepared precursor to 800-950 ℃ under the condition of nitrogen or air according to the heating rate of 1-10 ℃/min, and reacting for 12-24 h; c: and cooling the sintered product, adding an additive, grinding and mixing, heating to 400-600 ℃ at a heating rate of 1-10 ℃/min under the condition of nitrogen or air, preserving heat for 2-10 h, cooling and crushing to obtain the lithium titanate negative electrode material of the lithium ion battery. The lithium titanate prepared by the preparation method has uniform particle size distribution, greatly improves the electronic conductivity of the material, and effectively improves the rate charge-discharge performance and the cycle stability of the material.
Description
Technical field
The present invention relates to a kind of preparation method of lithium cell lithium titanate material, belong to the lithium secondary battery technical field of material.
Background technology
Spinel type lithium titanate (Li
4Ti
5O
12) voltage is 1.55V, as lithium ion battery negative material remarkable advantages is arranged: lithium titanate is a kind of zero strain material, embeds and to deviate from the process volume change of material very little at lithium ion; The stability of crystalline structure has improved the cycle performance and the work-ing life of electrode; Having reduced the specific storage of bringing with the cycle index increase decays significantly; The chemical diffusion coefficient that lithium titanate is high makes that this negative material can quick, many cycle charge-discharges.The specific conductivity of pure lithium titanate material commonly used is lower, and high rate capability is relatively poor, therefore need carry out modification to material.
The lithium titanate related patent U.S. Patent No. has: publication number is the preparation method of CN1978524A quick charging battery material of lithium titanate/coalescence benzene mixture; Its preparation method is with the precursor of lithium source, titanium, homemade coalescence benzene or synthetic resol; Obtain lithium titanate composite material through high-temperature heat treatment; 0.3C the multiplying power first discharge specific capacity is 155-162mAh/g, 9C multiplying power first discharge specific capacity is at 95-110mAh/g.Publication number is the lithium titanate of CN101402469A with a step solid phase method synthetic spinel structure, at 700-1300 ℃ of TR reaction 4-36h, makes lithium titanate recycle ratio capacity and reaches 100-160mAh/g.Patent publication No. is that CN101456581A is a raw material with titanium oxide, lithium salts, rare earth oxide, and high temperature solid-state method synthesizes the lithium cell cathode material lithium titanate, and specific storage is up to 173mAh/g first for 0.2C, and cycle performance is excellent.
Summary of the invention
The purpose of this invention is to provide a kind of electronic conduction ability that can improve lithium titanate material, the preparation method of the rate charge-discharge performance of raising lithium titanate material and the lithium ion battery lithium titanate material of cyclical stability.
Its technical scheme is: a kind of preparation method of lithium ion battery lithium titanate material is characterized in that comprising the steps:
A: lithium salts and titanium oxide are pressed 0.84 mixed in molar ratio, add the dispersion agent ground and mixed, vacuum-drying then obtains presoma;
B:, under nitrogen or air conditions, be warming up to 800~950 ℃ and react 12~24h with the temperature rise rate of the presoma that makes by 1~10 ℃/min;
C: after the cooling of the product behind the sintering; Add the additive ground and mixed therein; Again with the temperature rise rate of 1~10 ℃/min, under nitrogen or air conditions, be warming up to 400~600 ℃ and be incubated 2~10h, cooling back powder essence promptly gets lithium titanate anode material for lithium ion battery.
Its technique effect is: the present invention is owing to improve its conductivity through in sintering process, adding additive agent modified lithium titanate material; So the lithium titanate even particle size distribution for preparing, improved the electronic conduction ability of material greatly, effectively raised the rate charge-discharge performance and the cyclical stability of material.Through detecting: charge/discharge capacity reaches 173.5mAh/g under the 0.5C multiplying power, and charge/discharge capacity is 162.6mAh/g during 1C, and the 10C charge/discharge capacity is 131.5mAh/g, and 100 capability retentions of each multiplying power circulation are all more than 98%.Compare with pure lithium titanate, the lithium titanate after the modification has higher capacity, better cyclical stability and longer work-ing life under big electric current; And its technology is simple, is fit to suitability for industrialized production.
Description of drawings
Fig. 1 is an X-ray diffracting spectrum of executing the lithium titanate for preparing in the example 1;
Fig. 2 is the SEM figure that executes the lithium titanate of preparation in the example 1;
Fig. 3 is the first charge-discharge curve of executing under each multiplying power of lithium titanate of preparation in the example 1;
Fig. 4 is the high rate performance figure that executes the lithium titanate of preparation in the example 1.
Embodiment
Embodiment 1.
Get 200g Li
2CO
3, 500g anatase titanium dioxide TiO
2, add absolute ethyl alcohol as dispersion agent, ground and mixed, vacuum-drying then obtains presoma;
With the temperature rise rate of the presoma that makes, under nitrogen, be warming up to 900 ℃ and react 20h by 5 ℃/min;
With after the product behind the sintering cooling, add aluminum nitrate therein, ground and mixed again with the temperature rise rate of 5 ℃/min, is warming up to 500 ℃ and be incubated 10h under nitrogen, and cooling back powder essence obtains lithium titanate anode material for lithium ion battery.
The above-mentioned lithium titanate sample that makes through the X-ray diffraction analysis, is obtained the XRD figure spectrum of lithium titanate as shown in Figure 1, and as can be seen from the figure, the XRD figure of this sample and lithium titanate standard are basic identical, the appearance at inclusion-free peak.
Can find out on the SEM electromicroscopic photograph of Fig. 2 that the lithium titanate material distribution uniform does not have obvious agglomeration, median size is about 2.0 μ m, and its porous pattern is beneficial to the circulation of material.
The above-mentioned lithium titanate sample that makes, acetylene black, pvdf (PVDF) are mixed by 90: 5: 5 mass ratio, roll film forming, behind 80 ℃ of vacuum-drying 10h, be assembled into half-cell, electrolytic solution is LiPF
6(EC: DEC=1: 1).Adopt the Land battery test system, TV is 1.0-2.5V, and is as shown in Figure 3; Loading capacity reaches 173.5mAh/g first under the 0.5C multiplying power; During 1C first loading capacity reach 162.6mAh/g, 10C loading capacity first is 131.5mAh/g, and is visible with the prepared lithium titanate of present embodiment during as lithium ion battery negative material; Its charging and discharging capacity is high, and big multiplying power discharging property is superior.
Can find out among the high rate performance figure of prepared lithium titanate in the present embodiment like Fig. 4: when being used as lithium ion battery negative material with the prepared lithium titanate of present embodiment, under different multiplying powers, 20 times circulation back capability retention all remains on more than 98%.
Embodiment 2.
Take by weighing 129.5g LiOH, 500g anatase titanium dioxide TiO
2, add acetone as dispersion agent, put into the ball mill mixing and ball milling 5 hours, vacuum-drying then obtains presoma; With the temperature rise rate of the presoma that makes, under air, be warming up to 950 ℃ and react 12h by 8 ℃/min; After the cooling of product behind the sintering, add the 6.2g manganous nitrate therein, ground and mixed again with the temperature rise rate of 8 ℃/min, is warming up to 600 ℃ and be incubated 5h under air, and cooling back powder essence obtains lithium titanate anode material for lithium ion battery.
With reference to embodiment 1, carry out the Integration Assembly And Checkout of battery with identical method, the prepared lithium titanate of present embodiment under the 0.5C multiplying power first loading capacity be 170mAh/g, 20 times circulation back capability retention is 98.3%.
Embodiment 3.
Take by weighing 372.7g LiNO
3, 500g anatase titanium dioxide TiO
2Put into the ball mill mixing and ball milling 6 hours with water, vacuum-drying then obtains presoma; With the temperature rise rate of the presoma that makes, under air, be warming up to 800 ℃ and react 20h by 1 ℃/min; After the cooling of product behind the sintering, add the 26.1g chromium acetate therein, ground and mixed again with the temperature rise rate of 1 ℃/min, is warming up to 450 ℃ and be incubated 8h under air, and cooling back powder essence obtains lithium titanate anode material for lithium ion battery.
With reference to embodiment 1, carry out the Integration Assembly And Checkout of battery with identical method, the prepared lithium titanate of present embodiment under the 0.5C multiplying power first loading capacity be 171.2mAh/g, 20 times circulation back capability retention is 98.6%.
Embodiment 4:
Take by weighing 200g Li
2CO
3, 500g anatase titanium dioxide TiO
2And acetone (dispersion agent) put into the ball mill mixing and ball milling 5 hours, and vacuum-drying then obtains presoma; With the temperature rise rate of the presoma that makes, under nitrogen, be warming up to 800 ℃ and react 24h by 5 ℃/min; After the cooling of product behind the sintering, add the 21g zirconium white therein, ground and mixed again with the temperature rise rate of 5 ℃/min, is warming up to 600 ℃ and be incubated 6h under nitrogen gas, and cooling back powder essence obtains lithium titanate anode material for lithium ion battery.
With reference to embodiment 1, carry out the Integration Assembly And Checkout of battery with identical method, the prepared lithium titanate of present embodiment under the 0.5C multiplying power first loading capacity be 174.7mAh/g, 20 times circulation back capability retention is 99.1%.
Take by weighing 129.5g LiOH, 500g anatase titanium dioxide TiO
2, as dispersion agent, put into the ball mill mixing and ball milling 6 hours with absolute ethyl alcohol, vacuum-drying then obtains presoma; With the temperature rise rate of the presoma that makes, under air, be warming up to 950 ℃ and react 20h by 2 ℃/min; After the cooling of product behind the sintering, add the 31.5g molybdenum chloride therein, ground and mixed again with the temperature rise rate of 2 ℃/min, is warming up to 550 ℃ and be incubated 6h under air, and cooling back powder essence obtains lithium titanate anode material for lithium ion battery.
Embodiment 6.
Take by weighing 200g Li
2CO
3, 500g anatase titanium dioxide TiO
2, as dispersion agent, put into the ball mill mixing and ball milling 6 hours with acetone, vacuum-drying obtains presoma; With the temperature rise rate of the presoma that makes, under air, be warming up to 850 ℃ and react 15h by 8 ℃/min; After the cooling of product behind the sintering, add the 7g zinc chloride therein, ground and mixed again with the temperature rise rate of 8 ℃/min, is warming up to 500 ℃ and be incubated 6h under air, and cooling back powder essence obtains lithium titanate anode material for lithium ion battery.
With reference to embodiment 1, carry out the Integration Assembly And Checkout of battery with identical method, the prepared lithium titanate of present embodiment under the 0.5C multiplying power first loading capacity be 170.6mAh/g, 20 times circulation back capability retention is 98.5%.
Claims (4)
1. the preparation method of a lithium ion battery lithium titanate material is characterized in that comprising the steps:
A: lithium salts and titanium oxide are pressed 0.84 mixed in molar ratio, add the dispersion agent ground and mixed, vacuum-drying then obtains presoma;
B:, under nitrogen or air conditions, be warming up to 800~950 ℃ and react 12~24h with the temperature rise rate of the presoma that makes by 1~10 ℃/min;
C: after the cooling of the product behind the sintering; Add the additive ground and mixed therein; Again with the temperature rise rate of 1~10 ℃/min, under nitrogen or air conditions, be warming up to 400~600 ℃ and be incubated 2~10h, cooling back powder essence promptly gets lithium titanate anode material for lithium ion battery.
2. the preparation method of lithium ion battery lithium titanate material according to claim 1 is characterized in that: said lithium salts is one or more in Quilonum Retard, Lithium Hydroxide MonoHydrate, Lithium Oxide 98min, lithium nitrate or the lithium oxalate.
3. the preparation method of lithium ion battery lithium titanate material according to claim 1 is characterized in that: described dispersion agent is a kind of in absolute ethyl alcohol, water or the acetone.
4. the preparation method of lithium ion battery lithium titanate material according to claim 1; It is characterized in that: the said additive that in step C, adds is a kind of in nitrate salt, muriate, oxide compound, carbonate, oxalate or the acetate compound, and add-on is the 0.1-5% of lithium salts and titanium oxide mole number.
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Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102997651A (en) * | 2012-11-30 | 2013-03-27 | 龙能科技(苏州)有限公司 | Pusher furnace for preparing lithium titanate negative electrode materials of lithium ion battery and method |
CN103011265A (en) * | 2012-12-26 | 2013-04-03 | 彩虹集团公司 | Preparation method of lithium titanate |
CN104916846A (en) * | 2015-07-03 | 2015-09-16 | 中国第一汽车股份有限公司 | Preparation method of nano-micron morphology Zn-doped lithium titanate for lithium-ion battery |
CN105098168A (en) * | 2015-09-18 | 2015-11-25 | 孟红琳 | Preparation method of power lithium battery anode material |
CN106159223A (en) * | 2016-07-01 | 2016-11-23 | 天津普兰能源科技有限公司 | A kind of preparation method of lithium titanate material |
CN109473654A (en) * | 2018-11-22 | 2019-03-15 | 成都先进金属材料产业技术研究院有限公司 | Li4Ti5O12- TiN-TiC material and preparation method thereof |
CN109704395A (en) * | 2018-12-28 | 2019-05-03 | 北方奥钛纳米技术有限公司 | Preparation method, lithium titanate material and the battery of lithium titanate material |
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Cited By (10)
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CN102997651A (en) * | 2012-11-30 | 2013-03-27 | 龙能科技(苏州)有限公司 | Pusher furnace for preparing lithium titanate negative electrode materials of lithium ion battery and method |
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CN103011265A (en) * | 2012-12-26 | 2013-04-03 | 彩虹集团公司 | Preparation method of lithium titanate |
CN104916846A (en) * | 2015-07-03 | 2015-09-16 | 中国第一汽车股份有限公司 | Preparation method of nano-micron morphology Zn-doped lithium titanate for lithium-ion battery |
CN105098168A (en) * | 2015-09-18 | 2015-11-25 | 孟红琳 | Preparation method of power lithium battery anode material |
CN106159223A (en) * | 2016-07-01 | 2016-11-23 | 天津普兰能源科技有限公司 | A kind of preparation method of lithium titanate material |
CN109473654A (en) * | 2018-11-22 | 2019-03-15 | 成都先进金属材料产业技术研究院有限公司 | Li4Ti5O12- TiN-TiC material and preparation method thereof |
CN109704395A (en) * | 2018-12-28 | 2019-05-03 | 北方奥钛纳米技术有限公司 | Preparation method, lithium titanate material and the battery of lithium titanate material |
CN111403724A (en) * | 2020-04-21 | 2020-07-10 | 旭派电源有限公司 | Modified N, P co-doped lithium titanate negative electrode material and preparation method thereof |
CN111403724B (en) * | 2020-04-21 | 2022-03-29 | 旭派电源有限公司 | Modified N, P co-doped lithium titanate negative electrode material and preparation method thereof |
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