CN103730637B - A kind of alternating voltage method prepares the method for lithium ionic cell cathode material lithium titanate - Google Patents
A kind of alternating voltage method prepares the method for lithium ionic cell cathode material lithium titanate Download PDFInfo
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- CN103730637B CN103730637B CN201410012477.1A CN201410012477A CN103730637B CN 103730637 B CN103730637 B CN 103730637B CN 201410012477 A CN201410012477 A CN 201410012477A CN 103730637 B CN103730637 B CN 103730637B
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- titanium
- lithium titanate
- lithium
- alternating voltage
- cathode material
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 75
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 71
- 238000000034 method Methods 0.000 title claims abstract description 41
- 239000010406 cathode material Substances 0.000 title claims abstract description 15
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000010936 titanium Substances 0.000 claims abstract description 26
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 25
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 11
- 239000002105 nanoparticle Substances 0.000 claims abstract description 10
- 239000008151 electrolyte solution Substances 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- SWAIALBIBWIKKQ-UHFFFAOYSA-N lithium titanium Chemical compound [Li].[Ti] SWAIALBIBWIKKQ-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims abstract description 5
- 230000007935 neutral effect Effects 0.000 claims abstract description 5
- 239000012266 salt solution Substances 0.000 claims abstract description 5
- 239000002245 particle Substances 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 9
- 238000005868 electrolysis reaction Methods 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 8
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 238000000967 suction filtration Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000011780 sodium chloride Substances 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 14
- 230000002441 reversible effect Effects 0.000 abstract description 8
- 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
- 230000014759 maintenance of location Effects 0.000 abstract description 4
- 238000007599 discharging Methods 0.000 description 5
- 238000007600 charging Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000004070 electrodeposition Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 206010013786 Dry skin Diseases 0.000 description 2
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 230000036632 reaction speed Effects 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 1
- 239000002033 PVDF binder Substances 0.000 description 1
- 239000006230 acetylene black Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000006258 conductive agent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 description 1
- 229910052939 potassium sulfate Inorganic materials 0.000 description 1
- 235000011151 potassium sulphates Nutrition 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/003—Titanates
- C01G23/005—Alkali titanates
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
A kind of alternating voltage method of the present invention prepares the method for lithium ionic cell cathode material lithium titanate.The method is electrolyte solution with neutral salt solution, take pure metallic titanium as cathode and anode, and apply alternating voltage (10 ~ 220V), metallic titanium is dispersed into Titanium dioxide nanoparticle colloidal sol.Titanium oxide sol is separated, cleans and dry rear and Li
2cO
3mix in the ratio of lithium titanium mol ratio 0.8 ~ 0.9, in tube furnace, namely 700 ~ 900 DEG C of heat treatments obtain lithium titanate in 3 ~ 24 hours.The lithium titanate of the present invention's synthesis, with lithium metal for be prepared into battery to electrode, 0.5C reversible capacity reaches 161mAh/g, and after charge and discharge cycles 100 is enclosed, capacity is 157mAh/g, and capability retention is 97.5%; 10C reversible capacity reaches 141mAh/g, and after charge and discharge cycles 100 is enclosed, capacity can also reach 127mAh/g.The inventive method preparation section is simple, and the lithium titanate of preparation has excellent cycle performance and high-rate discharge ability, can be widely used in various portable electric appts and the lithium ion battery needed for various electric motor car.
Description
Technical field
The present invention relates to new material and field of lithium ion battery, be specifically related to a kind of preparation method of lithium ionic cell cathode material lithium titanate, namely alternating voltage method prepares lithium titanate.
Background technology
Novel lithium titanate (Li
4ti
5o
12) negative material is a kind of composite oxides by lithium metal and electronegative potential transition metals Ti.As lithium ion battery negative material, Li
4ti
5o
12maximum feature is exactly its " zero strain ".In charge and discharge cycles, this " zero strain " can be avoided due to the flexible back and forth of electrode material and cause structural damage, greatly improves cycle performance and the useful life of electrode, has extraordinary overcharging resisting, crosses and put feature.Secondly, Li
4ti
5o
12operating potential opposing metallic lithium be 1.55V, far above the deposition potential of lithium metal, avoid the safety problem analysed lithium and cause in actual applications.The most important thing is that lithium titanate can carry out high power fast charging and discharging, is one of ideal candidates negative material of environmental-protecting type electric car driving power of future generation, communications service, energy-accumulating power station etc.
But current business-like lithium titanate great majority adopt solid phase method with the larger titanium dioxide of particle for precursor power, and the lithium titanate prepared need carry out multistep screening, and preparation technology is quite complicated, and the high-power charging and discharging capabilities of prepared lithium titanate is poor.
The present invention will provide a kind of method of high efficiency alternating voltage synthesis lithium titanate, and prepared lithium titanate is applied to lithium ion battery negative material and has excellent cycle performance and high-rate charge-discharge capability.
Summary of the invention
The object of the invention is to provide a kind of method preparing lithium ionic cell cathode material lithium titanate, and lithium titanate of negative pole material prepared by the method has excellent cycle performance and high-rate charge-discharge capability.
To achieve the above object of the invention, the present invention proposes following technical scheme:
A kind of alternating voltage method prepares the method for lithium ionic cell cathode material lithium titanate, being electrolyte solution with neutral salt solution, take pure metallic titanium as cathode and anode, applies alternating voltage, metallic titanium is dispersed into Titanium dioxide nanoparticle colloidal sol, is then separated by titanium oxide sol, cleans and dry rear and Li
2cO
3mix, namely heat treatment obtain lithium titanate.
Described Titanium dioxide nanoparticle particle size <100nm.
Described neutral salt solution comprises NaNO
3, NaCl, Na
2sO
4, KNO
3, KCl or K
2sO
4the mixture of one or more.
In described solution, electrolytical concentration is not less than 0.5mol/L.
Titanium form is any one in titanium silk, titanium sheet, target titanium.
Described alternating voltage is 10 ~ 220V, and electrolysis time is 1 ~ 24 hour.
The method be separated by titanium oxide is centrifugal or suction filtration, and the material for cleaning is deionized water.
Titanium oxide and Li
2cO
3the lithium titanium mol ratio of mixing is 0.8 ~ 0.9.
Heat treated temperature is 700 ~ 900 DEG C, and the heat treated time is 3 ~ 24 hours.
Owing to have employed above scheme, the lithium titanate of the present invention's synthesis possesses following advantage:
With lithium metal for be prepared into battery to electrode, 0.5C reversible capacity reaches 161mAh/g, and after charge and discharge cycles 100 is enclosed, capacity is 157mAh/g, and capability retention is 97.5%; 10C reversible capacity reaches 141mAh/g, and after charge and discharge cycles 100 is enclosed, capacity can also reach 127mAh/g.The inventive method preparation section is simple, and the lithium titanate of preparation has excellent cycle performance and high-rate discharge ability, can be widely used in various portable electric appts and the lithium ion battery needed for various electric motor car.
The titanium oxide of visible nm regime of the present invention is that the lithium titanate that precursor power goes out has excellent cycle performance and high-rate discharge ability, and what current business-like method adopted is micron order titanium oxide, and the lithium titanate performance prepared is not ideal enough.The alternating voltage method that the present invention creates for the applicant, also not being disclosed alternating voltage method prepares nano-metal-oxide at present, different with alternating current electro-deposition, electro-deposition deposits to above electrode by the metal of the slaine in solution, and the present invention take pure metallic titanium as anode and cathode, disperse in the solution Titanium is oxidized to nanometer shape titanium oxide under alternating voltage after; Moreover, Titanium is very stable metal, conventional electrolysis mode also cannot convert it into the titan oxide particles of nm regime, electrolysis (i.e. anodic oxidation) as traditional can only grow titanium oxide in surface of metal titanium, adhere to very firm, be difficult to peel off from titanium substrate, be difficult to commercial and produce; Alternating voltage method of the present invention is had any different in the electrolysis tech of routine, and Titanium can be oxidized and peel off and become Titanium dioxide nanoparticle by this special sine voltage, and conventional method anodic oxidation, and electro-deposition etc. all cannot realize.
Accompanying drawing explanation
Alternating voltage method synthesis lithium titanate precursor schematic diagram in Fig. 1 embodiment 1;
The XRD collection of illustrative plates of the lithium titanate of preparation in Fig. 2 embodiment 1;
The TEM figure of the lithium titanate of preparation in Fig. 3 embodiment 1;
The lithium titanate 0.5C of preparation in Fig. 4 embodiment 1 circulates and business-like lithium titanate 0.5C circulation and coulombic efficiency figure (b) in coulombic efficiency figure (a) and comparative example;
The lithium titanate 10C of preparation in Fig. 5 embodiment 1 circulates and business-like lithium titanate 10C circulation and coulombic efficiency figure (b) in coulombic efficiency figure (a) and comparative example;
Fig. 6 is the SEM figure of commercialization lithium titanate in comparative example;
In Fig. 7 embodiment 2, the lithium titanate TEM of preparation schemes;
In Fig. 8 embodiment 3, the lithium titanate TEM of preparation schemes.
Embodiment
Following examples are to explain the present invention in more detail, but these embodiments do not form any restriction to the present invention, and the present invention can implement by the either type described in summary of the invention.
Embodiment 1
As shown in Figure 1, with 3mol/LNaNO
3solution is electrolyte solution, with pure metallic titanium silk for cathode and anode, applies alternating voltage 30V electrolysis 5 hours, metallic titanium is dispersed into the Titanium dioxide nanoparticle colloidal sol that particle diameter is less than 100nm, then titanium oxide sol suction filtration is separated, with deionized water rinsing six times, after 50 DEG C of dryings and Li
2cO
3the ratio being 0.85 in lithium titanium mol ratio mixes, and in tube furnace, namely 800 DEG C of heat treatments obtain lithium titanate in 15 hours.From Fig. 2 and XRD standard card JCPDS49-0207, the lithium titanate of synthesis is pure phase, without other impurity.TEM(Fig. 3) show, synthesized lithium titanate particle diameter 50 ~ 70nm.
By lithium titanate powder, conductive agent acetylene black and binding agent PVDF(are dissolved in 1-METHYLPYRROLIDONE) 80:10:10 mixed grinding uniformly slurry in mass ratio, be applied on clean Copper Foil and make electrode film, then predrying at 75 DEG C, then vacuumize obtains negative plate at 100 DEG C.Do electrode with lithium sheet, adopt 1mol/LLiPF
6/ ethylene carbonate (EC)+dimethyl carbonate (DMC) (volume ratio=1:1) is as electrolyte.CR2016 button cell is assembled in argon gas glove box.Adopt CT2001A type constant current charge-discharge instrument (the blue electricity in Wuhan) to carry out constant current cycle performance test, charging and discharging currents density is 0.5C (87.5mA/g) and 10C (1750mA/g), and charging/discharging voltage scope control is between 1 ~ 3V.Fig. 4 (a) is circulation-specific capacity, the efficiency chart under 0.5C current density, and initial coulomb efficiency is 83%, and circulation coulombic efficiency subsequently can reach more than 99.5%; Reversible capacity reaches 161mAh/g, and after charge and discharge cycles 100 is enclosed, capacity is 157mAh/g, and capability retention is 97.5%; Fig. 5 (a) is circulation-specific capacity, the efficiency chart under high current density 10C, and initial coulomb efficiency is 84%, and circulation coulombic efficiency subsequently can reach more than 99.5%; Reversible capacity reaches 141mAh/g, and after charge and discharge cycles 100 is enclosed, capacity can also reach 127mAh/g.
Comparative example
Business-like lithium titanate (Jie Wei Momentum Ind LLC, prepared by solid phase method, as shown in Figure 6, particle size is about 1.5 μm to surface topography) is prepared electrode plates according to the preparation technology of electrode in embodiment 1 and is assembled into button cell.Fig. 4 (b) is circulation-specific capacity, the efficiency chart under 0.5C current density, and reversible capacity is 145mAh/g, and after charge and discharge cycles 100 is enclosed, capacity is 136mAh/g, and capability retention is 93.8%; Fig. 5 (b) is circulation-specific capacity, the efficiency chart under high current density 10C, and reversible capacity is 102mAh/g, and after charge and discharge cycles 100 is enclosed, capacity is 88mAh/g.Compared with the lithium titanate prepared in embodiment 1, lithium titanate prepared by its cyclical stability and high rate during charging-discharging Xun Benfa far away.
Embodiment 2
As shown in Figure 1, with 3mol/LNaNO
3solution is electrolyte solution, with pure metallic titanium silk for cathode and anode, apply alternating voltage 60V electrolysis 2 hours (reaction speed comparatively embodiment 1 is fast), metallic titanium is dispersed into Titanium dioxide nanoparticle colloidal sol, then titanium oxide sol suction filtration is separated, with deionized water rinsing six times, after 50 DEG C of dryings and Li
2cO
3the ratio being 0.85 in lithium titanium mol ratio mixes, and in tube furnace, namely 800 DEG C of heat treatments obtain lithium titanate in 15 hours.TEM(Fig. 7) show, synthesized lithium titanate is reunited comparatively serious, and particle diameter is 30 ~ 65nm about.
Embodiment 3
With 3mol/LNaCl solution for electrolyte solution, with pure metallic titanium silk for cathode and anode, apply alternating voltage 30V electrolysis 1 hour, metallic titanium is dispersed into Titanium dioxide nanoparticle colloidal sol.Ultrasonic collection is also cleaned, and other subsequent preparation process is with embodiment 1.TEM(Fig. 8) show, synthesized lithium titanate particle diameter 40 ~ 70nm, some is reunited.
Embodiment 4
Electrolyte solution is replaced by Na
2sO
4, KNO
3, KCl or K
2sO
4solution, other process is with embodiment 1.Product can be prepared, cell reaction speed KNO in this several solns
3the fastest in solution, the slowest in potassium sulfate.
Claims (9)
1. an alternating voltage method prepares the method for lithium ionic cell cathode material lithium titanate, it is characterized in that, take neutral salt solution as electrolyte solution, take pure metallic titanium as cathode and anode, apply sine wave AC voltage, Titanium is oxidized and is peeled off and becomes Titanium dioxide nanoparticle, metallic titanium is dispersed into Titanium dioxide nanoparticle colloidal sol, is then separated by titanium oxide sol, cleans and dry rear and Li
2cO
3mix, namely heat treatment obtain lithium titanate.
2. alternating voltage method according to claim 1 prepares the method for lithium ionic cell cathode material lithium titanate, it is characterized in that, described Titanium dioxide nanoparticle particle size <100nm.
3. alternating voltage method according to claim 1 prepares the method for lithium ionic cell cathode material lithium titanate, it is characterized in that, described neutral salt solution comprises NaNO
3, NaCl, Na
2sO
4, KNO
3, KCl or K
2sO
4the mixture of one or more.
4. the alternating voltage method according to claim 1 or 3 prepares the method for lithium ionic cell cathode material lithium titanate, it is characterized in that, in described solution, electrolytical concentration is not less than 0.5mol/L.
5. alternating voltage method according to claim 1 prepares the method for lithium ionic cell cathode material lithium titanate, it is characterized in that, Titanium form is any one in titanium silk, titanium sheet, target titanium.
6. alternating voltage method prepares the method for lithium ionic cell cathode material lithium titanate according to claim 1 or 5, it is characterized in that, described alternating voltage is 10 ~ 220V, and electrolysis time is 1 ~ 24 hour.
7. alternating voltage method according to claim 1 prepares the method for lithium ionic cell cathode material lithium titanate, it is characterized in that, the method be separated by titanium oxide is centrifugal or suction filtration, and the material for cleaning is deionized water.
8. alternating voltage method according to claim 1 prepares the method for lithium ionic cell cathode material lithium titanate, it is characterized in that, titanium oxide and Li
2cO
3the lithium titanium mol ratio of mixing is 0.8 ~ 0.9.
9. alternating voltage method according to claim 1 prepares the method for lithium ionic cell cathode material lithium titanate, it is characterized in that, heat treated temperature is 700 ~ 900 DEG C, and the heat treated time is 3 ~ 24 hours.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410012477.1A CN103730637B (en) | 2014-01-10 | 2014-01-10 | A kind of alternating voltage method prepares the method for lithium ionic cell cathode material lithium titanate |
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| CN103730637B true CN103730637B (en) | 2016-04-20 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101054711A (en) * | 2007-05-10 | 2007-10-17 | 复旦大学 | Method of preparing titanium dioxide thin film by oxidizing metallic titanium using alternating current |
| CN101580273A (en) * | 2009-06-12 | 2009-11-18 | 清华大学 | High energy density spinel structural lithium titanate material and preparation method thereof |
| CN101759227A (en) * | 2008-12-24 | 2010-06-30 | 比亚迪股份有限公司 | Lithium titanate composite material and preparation method thereof |
| CN102496705A (en) * | 2011-12-09 | 2012-06-13 | 东莞市迈科科技有限公司 | Preparation method of spinel lithium titanate |
| CN103097588A (en) * | 2010-07-19 | 2013-05-08 | 莱顿大学 | Process to prepare metal nanoparticles or metal oxide nanoparticles |
-
2014
- 2014-01-10 CN CN201410012477.1A patent/CN103730637B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101054711A (en) * | 2007-05-10 | 2007-10-17 | 复旦大学 | Method of preparing titanium dioxide thin film by oxidizing metallic titanium using alternating current |
| CN101759227A (en) * | 2008-12-24 | 2010-06-30 | 比亚迪股份有限公司 | Lithium titanate composite material and preparation method thereof |
| CN101580273A (en) * | 2009-06-12 | 2009-11-18 | 清华大学 | High energy density spinel structural lithium titanate material and preparation method thereof |
| CN103097588A (en) * | 2010-07-19 | 2013-05-08 | 莱顿大学 | Process to prepare metal nanoparticles or metal oxide nanoparticles |
| CN102496705A (en) * | 2011-12-09 | 2012-06-13 | 东莞市迈科科技有限公司 | Preparation method of spinel lithium titanate |
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Effective date of registration: 20161130 Address after: Tianfu Huayang street of Chengdu city in Sichuan province 610000 China Xilu No. 44 1 floor Patentee after: CHENGDU YUNJIN ENERGY TECHNOLOGY CO.,LTD. Address before: 410000 room 41, building 502, sunshine one hundred and thirty, Changsha, Hunan, Yuelu District Patentee before: Ji Xiaobo |
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Granted publication date: 20160420 |