CN100345766C - Process for preparing nano lithium titanium oxide material by low temp. solid phase reaction - Google Patents
Process for preparing nano lithium titanium oxide material by low temp. solid phase reaction Download PDFInfo
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- CN100345766C CN100345766C CNB2006100111211A CN200610011121A CN100345766C CN 100345766 C CN100345766 C CN 100345766C CN B2006100111211 A CNB2006100111211 A CN B2006100111211A CN 200610011121 A CN200610011121 A CN 200610011121A CN 100345766 C CN100345766 C CN 100345766C
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- 239000000463 material Substances 0.000 title claims abstract description 18
- 238000003746 solid phase reaction Methods 0.000 title claims abstract description 8
- FDLZQPXZHIFURF-UHFFFAOYSA-N [O-2].[Ti+4].[Li+] Chemical compound [O-2].[Ti+4].[Li+] FDLZQPXZHIFURF-UHFFFAOYSA-N 0.000 title description 2
- 238000004519 manufacturing process Methods 0.000 title 1
- 238000000034 method Methods 0.000 claims abstract description 20
- 238000002360 preparation method Methods 0.000 claims abstract description 15
- 239000000843 powder Substances 0.000 claims abstract description 14
- 239000004570 mortar (masonry) Substances 0.000 claims abstract description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000000047 product Substances 0.000 claims abstract description 7
- 239000012467 final product Substances 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 4
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 4
- 239000010439 graphite Substances 0.000 claims abstract description 4
- 239000002002 slurry Substances 0.000 claims abstract description 4
- 239000013078 crystal Substances 0.000 claims description 3
- 235000011194 food seasoning agent Nutrition 0.000 claims description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 2
- 206010013786 Dry skin Diseases 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- 238000000967 suction filtration Methods 0.000 claims 1
- 238000005406 washing Methods 0.000 claims 1
- 239000003990 capacitor Substances 0.000 abstract description 14
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 5
- 230000015572 biosynthetic process Effects 0.000 abstract description 5
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 5
- 238000003786 synthesis reaction Methods 0.000 abstract description 5
- 238000006243 chemical reaction Methods 0.000 abstract description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 239000002243 precursor Substances 0.000 abstract 3
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 abstract 2
- 229910002986 Li4Ti5O12 Inorganic materials 0.000 abstract 1
- 229910010479 Li4Ti5O2 Inorganic materials 0.000 abstract 1
- 239000007832 Na2SO4 Substances 0.000 abstract 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 abstract 1
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 abstract 1
- 229910001626 barium chloride Inorganic materials 0.000 abstract 1
- 238000001514 detection method Methods 0.000 abstract 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 abstract 1
- 239000007773 negative electrode material Substances 0.000 abstract 1
- 229910000029 sodium carbonate Inorganic materials 0.000 abstract 1
- 235000017550 sodium carbonate Nutrition 0.000 abstract 1
- 229910052938 sodium sulfate Inorganic materials 0.000 abstract 1
- 235000011152 sodium sulphate Nutrition 0.000 abstract 1
- 239000010936 titanium Substances 0.000 description 19
- 238000007599 discharging Methods 0.000 description 8
- 238000010532 solid phase synthesis reaction Methods 0.000 description 8
- 239000011734 sodium Substances 0.000 description 5
- 239000008151 electrolyte solution Substances 0.000 description 4
- 239000000376 reactant Substances 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- 238000003980 solgel method Methods 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000006230 acetylene black Substances 0.000 description 2
- 239000013543 active substance Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000006258 conductive agent Substances 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000007669 thermal treatment Methods 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 206010016654 Fibrosis Diseases 0.000 description 1
- 229910013684 LiClO 4 Inorganic materials 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 239000002033 PVDF binder Substances 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000009194 climbing Effects 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000004761 fibrosis Effects 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920000767 polyaniline Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000007614 solvation Methods 0.000 description 1
- 238000001228 spectrum 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
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
- 229910000349 titanium oxysulfate Inorganic materials 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 230000001052 transient effect Effects 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
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Abstract
The present invention provides a method for preparing a Li4Ti5O12 material by adopting low-temperature solid-phase reaction, which belongs to the technical field of the preparation of electrochemical capacitors and lithium ion battery negative electrode materials. The present invention can prepare a precursor by two steps that hydrous TiOSO4.2H2O and anhydrous Na2CO3 are respectively ground in a mortar for 30 to 60 minutes in a stoichiometric ratio for reaction, the obtained product is washed by water, and is pumped and filtered, Na2SO4 is washed away, detection is carried out by BaCl2 until SO4 (2-) does not exist, a pure TiOCO3 slurry material is obtained, and then a TiOCO3 powder body is obtained after a natural drying process; the TiOCO3 powder body, powder graphite of which the content is from 6 to 10 percent, and LiOH. H2O are mixed in a certain stoichiometric ratio and are ground in the mortar for 30 to 60 minutes, the mixture is dried at a temperature of 100 to 150 DEG C, and then the precursor is prepared out. The prepared precursor is calcined for 8 to 24 hours at the temperature of 500 to 800 DEG C, and then the final product Li4Ti5O2 is obtained. The present invention has the advantages of simple operation and low synthesis temperature, which greatly reduces energy consumption.
Description
Technical field
The invention belongs to electrochemical capacitor and lithium ion battery negative material preparing technical field, particularly provide a kind of employing low-temperature solid phase reaction to prepare Li
4Ti
5O
12The method of material is used as electrochemical capacitor and lithium ion battery negative material.
Technical background
Along with the rise of environmental-protecting type electric automotive research, electrochemical capacitor has become another research focus behind lithium ion battery as a kind of energy storage device with high power density.It and secondary cell combination are used, can satisfy electromobile starting preferably, quicken, during climbing to high-power requirement, and reclaim the transient energy that electromobile when brake produces rapidly, make secondary cell maintain work under the more stable current status all the time, prolong its cycle life.
In order to satisfy in the practical application load to the whole requirement of power-supply system energy density and power density, people begin to design novel asymmetric electrochemical capacitor, be hybrid electrochemical capacitor again, a utmost point that is electrical condenser is a double layer electrodes, and another pseudo capacitance electrode very, as the C/KOH/ polyaniline, C/KOH/Ni (OH)
2Etc. the system hybrid electrochemical capacitor.Hybrid electrochemical capacitor also can constitute Li by lithium ion intercalated material and double layer electrodes material
4Ti
5O
12Be that a kind of lithium inserts the zero strain material, has superior cycle performance, can be used to replace a utmost point of gac double layer capacitor, bring into play the advantage of its relative height ratio capacity, the big order of magnitude of its chemical diffusion coefficient ratio carbon electrode material becomes ideal hybrid electrochemical capacitor negative material simultaneously.
Present Li
4Ti
5O
12Synthetic method adopt solid reaction process and sol-gel method mostly.
Li
4Ti
5O
12The high temperature solid-state synthesis technique similar to other composite oxide of metal, usually with Detitanium-ore-type TiO
2And LiOHH
2O (or Li
2CO
3) be raw material, form product by high temperature (800-1000 ℃), long thermal treatment.High temperature solid phase synthesis is simple to operate, is easy to push to industrialization.But shortcoming also is conspicuous, and is not enough as mixture homogeneity, and diffusion process is difficult to carry out smoothly, needs the long thermal treatment of high temperature, the energy consumption height.
Synthesis temperature is low, particle size is little, homogeneity is good, specific surface area is big and the crystallization degree advantages of higher is widely adopted gradually owing to having for the sol-gel method liquid phase synthesizing method, the existing literature report sol-gel methodes that adopt more.Can prepare the Li of nanoscale with sol-gel technique
4Ti
5O
12Powder body material.But synthesis technique complexity.
Adopt the synthetic Li of low temperature solid phase method
4Ti
5O
12Combine the advantage of above two kinds of methods, when the preparation presoma, form liquid film and make reactants dissolved at reaction-ure surface by the crystal water in the reactant.Lysed reactant has mass transfer velocity faster in liquid film, accelerated speed of response.The existence of trace solvent does not change the direction and the limit of reaction, only plays the effect of quickening and reducing temperature of reaction.This is because trace solvent can not be with the complete solvation of reactant, so the tremendous influence of solvent can not occur at this in the solution.
In article of delivering and patent, do not see at present the report that adopts with same raw materials of the present invention and synthetic this material of method as yet.
Summary of the invention
The object of the present invention is to provide a kind of employing low-temperature solid phase reaction to prepare Li
4Ti
5O
12The method of material has solved the synthetic Li of high temperature solid-state
4Ti
5O
12Temperature height in the negative material process, the time is long, the problem that energy consumption is high; Solve complex process cost problem of higher in collosol and gel and the hydro-thermal building-up process.
The present invention adopts the low-temperature solid phase reaction method, prepares presoma in two steps.
1, preparation presoma: the first step will contain the titanyl sulfate (TiOSO of crystal water respectively
42H
2O) with anhydrous sodium carbonate (Na
2CO
3) in mortar, ground 30-60 minute by stoichiometric ratio, it is reacted.Its mol ratio TiOSO
42H
2O: Na
2CO
3=1: 0.8～1.2, products therefrom is washed, filtered, wash Na off
2SO
4, use BaCl
2Detect, up to no SO
4 2-, obtain purified TiOCO
3Slurry obtains TiOCO after the seasoning
3Powder; Second step was with TiOCO
3Powder and 6～10% be the LiOHH of powder graphite and stoichiometric ratio
2O mixes, and grinds 30-60 minute in mortar.Its mol ratio TiOCO
3: LiOHH
2O=5: 3.8～4.6, mixture is prepared presoma 100～150 ℃ of dryings.
2, product preparation: the presoma for preparing was obtained final product Li in 8～24 hours 500～800 ℃ of roastings
4Ti
5O
12
At preparation Li
4Ti
5O
12Step in, can be at TiOCO
3Middle V, the Ag of stoichiometric ratio, acetate or the oxide compound of Al, Fe of adding.Obtain final product Li
4M
xTi
5-xO
12, x=0～0.1 wherein.
The invention has the advantages that: simple to operate, synthesis temperature is low, can reach the performance of liquid phase synthetic materials simultaneously.
Description of drawings
Fig. 1 is the Li of low-heat solid phase synthesis of the present invention
4Ti
5O
12XRD figure is by embodiment 1 preparation.
Fig. 2 is the Li of low-heat solid phase synthesis of the present invention
4Ti
5O
12XRD figure, by embodiment 2 preparations,
Fig. 3 is standard Li
4Ti
5O
12
Fig. 4 is the Li of low-heat solid phase synthesis of the present invention
4Ti
5O
12The discharge curve of different multiplying is prepared by embodiment 1 method.Capacitor anode is a gac, and electrolytic solution is 1MLiClO
4-PC, charging and discharging currents density from 175mA/g (1C) to 1750mA/g (10C), charging/discharging voltage scope 2.7-1.5V.X-coordinate is specific storage (mAh/g), and ordinate zou is voltage (V).
Fig. 5 is the Li of low-heat solid phase synthesis of the present invention
4Ti
5O
12The discharge curve of different multiplying is prepared by embodiment 2 methods.Capacitor anode is a gac, and electrolytic solution is 1MLiClO
4-PC, charging and discharging currents density from 175mA/g (1C) to 1750mA/g (10C), charging/discharging voltage scope 2.7-1.5V.X-coordinate is specific storage (mAh/g), and ordinate zou is voltage (V).
Fig. 6 is the Li of low temperature solid phase synthesis of the present invention
4Ti
5O
12Sample different multiplying loading capacity and cycle diagram, capacitor anode are gac, and electrolytic solution is 1MLiClO
4-PC, charging and discharging currents density from 175mA/g (1C) to 3500mA/g (20C), charging/discharging voltage scope 2.7-1.5V.X-coordinate is a cycle index, and ordinate zou is specific storage (mAh/g).(label 600-is by embodiment 1 preparation, and label 625-is by embodiment 2 preparations)
Embodiment
Further specify method of the present invention by the following examples.
1, preparation TiOCO
3Powder
Embodiment 1:
1) takes by weighing TiOSO respectively by 1: 1 mol ratio
42H
2O 4.898g and Na
2CO
32.65g in mortar, ground 60 minutes, be mixed into thick;
2) products therefrom is washed, is filtered with deionized water, washes Na off
2SO
4, filter 3 times repeatedly, and use BaCl
2Detect, up to no SO
4 =, obtain purified TiOCO
3Slurry obtains TiOCO after the seasoning
3Powder;
3) take by weighing 2gTiOCO respectively
3Powder, 0.129g micro powder graphite and 0.57gLiOHH
2O mixes, and grinds 60 minutes in mortar.Its mol ratio TiOCO
3: LiOHH
2O=5: 4., mixture is prepared presoma in 120～℃ drying.
4) presoma is put into crucible oven, be warming up to 600 ℃ of insulation 12h, cool to room temperature by 5 ℃/min, behind mistake 140 mesh sieves, 600 ℃ of temper 8 hours with 5 ℃/min.
Embodiment 2:
1)-3) go on foot with embodiment 1,
4) presoma is put into crucible oven, is warming up to 625 ℃ of insulation 12h with 5 ℃/min, cools to room temperature by 5 ℃/min, behind mistake 140 mesh sieves, 600 ℃ of temper 8 hours.
2, the preparation of electrode film
It is anodal that the experiment electrical condenser adopts gac to do, and positive pole is pressed active substance: conductive agent (acetylene black): tackiness agent (tetrafluoroethylene)=87: 10: the 3wt% mixed is even, adds small amount of ethanol, to promote the snappiness of PTFE fibrosis, intensifier electrode film.Be rolled into the film that thickness is about 0.35mm with manual rolling machine, be pressed on the nickel foam collector with the pressure of 2MPa again and make positive pole.
Negative pole is pressed Li
4Ti
5O
12: conductive agent (acetylene black): tackiness agent (polyvinylidene difluoride (PVDF))=83: 10: the 7wt% mixed evenly is applied on the Al paper tinsel, the about 20 μ m of thickness, and dry back makes with the compacting of electronic pair of roller roll forming machine.
The positive and negative electrode sheet is standby at 125 ℃ of vacuum-drying 24h.For guaranteeing that the two stored energy capacitance of positive and negative electrode is complementary, the mass ratio of active substance is about 5: 1 in the positive and negative electrode.
3, the assembling of electrical condenser and test:
Mixed capacitor is assembled in the argon gas glove box, 1M LiClO
4/ PC makes electrolytic solution.Charging/discharging voltage scope 2.5～1.5V, charging and discharging currents are respectively 1C (175mA/g)～20C (3500mA/g)
By the XRD figure of Fig. 1 as seen, institute two sample diffraction peaks of synthetic position is consistent with the diffraction peak of standard spectrum, illustrates to have formed good spinel structure.
As seen adopt the Li of low-temperature solid-phase synthesis method preparation by Fig. 2 and Fig. 3
4Ti
5O
12Material has the performance of good high rate capability.
Claims (2)
1, a kind of employing low-temperature solid phase reaction prepares Li
4Ti
5O
12The method of material is characterized in that:
A, presoma preparation:
The first step will contain the TiOSO of crystal water respectively
42H
2O and anhydrous Na
2CO
3In mortar, ground 30-60 minute by stoichiometric ratio, it is reacted; ,, wash Na off with products therefrom washing, suction filtration
2SO
4, use BaCl
2Detect, up to no SO
4 2-, obtain purified TiOCO
3Slurry obtains TiOCO after the seasoning
3Powder; Second step was with TiOCO
3Powder and 6～10% micro powder graphite and the LiOHH of stoichiometric ratio
2O mixes, and grinds 30-60 minute in mortar; TiOCO is compared in its metering
3: LiOHH
2O=5: 4, mixture is prepared presoma 100～150 ℃ of dryings;
B, product preparation: the presoma for preparing was obtained final product Li in 8～24 hours 500～800 ℃ of roastings
4Ti
5O
12
2, employing low-temperature solid phase reaction according to claim 1 prepares Li
4Ti
5O
12The method of material is characterized in that: at preparation Li
4Ti
5O
12Step in, at TiOCO
3Middle V, the Ag of stoichiometric ratio, acetate or the oxide compound of Al, Fe of adding; Obtain final product Li
4M
xTi
5-xO
12, x=0～0.1 wherein.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100111211A CN100345766C (en) | 2006-01-06 | 2006-01-06 | Process for preparing nano lithium titanium oxide material by low temp. solid phase reaction |
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|---|---|---|---|
| CNB2006100111211A CN100345766C (en) | 2006-01-06 | 2006-01-06 | Process for preparing nano lithium titanium oxide material by low temp. solid phase reaction |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1792815A CN1792815A (en) | 2006-06-28 |
| CN100345766C true CN100345766C (en) | 2007-10-31 |
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ID=36804488
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100411994C (en) * | 2006-07-07 | 2008-08-20 | 清华大学 | Process for preparing carbon-doped spherical Li4Ti5O12 |
| CN102259911B (en) * | 2011-06-29 | 2013-03-27 | 上海空间电源研究所 | Method for preparing nano lithium titanate anode material for lithium ion battery |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001213622A (en) * | 2000-01-26 | 2001-08-07 | Toho Titanium Co Ltd | Process of producing lithium titanate, lithium ion battery and electrode thereof |
| US6475673B1 (en) * | 1999-02-16 | 2002-11-05 | Toho Titanium Co., Ltd. | Process for producing lithium titanate and lithium ion battery and negative electrode therein |
| US20030017104A1 (en) * | 2001-07-20 | 2003-01-23 | Altair Nanomaterials Inc. | Process for making lithium titanate |
| US20040217335A1 (en) * | 2003-04-29 | 2004-11-04 | Hans-Josef Sterzel | Preparation of nanocrystalline lithium titanate spinels |
-
2006
- 2006-01-06 CN CNB2006100111211A patent/CN100345766C/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6475673B1 (en) * | 1999-02-16 | 2002-11-05 | Toho Titanium Co., Ltd. | Process for producing lithium titanate and lithium ion battery and negative electrode therein |
| JP2001213622A (en) * | 2000-01-26 | 2001-08-07 | Toho Titanium Co Ltd | Process of producing lithium titanate, lithium ion battery and electrode thereof |
| US20030017104A1 (en) * | 2001-07-20 | 2003-01-23 | Altair Nanomaterials Inc. | Process for making lithium titanate |
| US20040217335A1 (en) * | 2003-04-29 | 2004-11-04 | Hans-Josef Sterzel | Preparation of nanocrystalline lithium titanate spinels |
Non-Patent Citations (1)
| Title |
|---|
| 锂离子电池负极材料钛酸锂的研究进展 高剑，等，电池，第35卷第5期 2005 * |
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