WO2009074208A2 - Materiau d'electrode negative pour batteries li-ion - Google Patents
Materiau d'electrode negative pour batteries li-ion Download PDFInfo
- Publication number
- WO2009074208A2 WO2009074208A2 PCT/EP2008/009763 EP2008009763W WO2009074208A2 WO 2009074208 A2 WO2009074208 A2 WO 2009074208A2 EP 2008009763 W EP2008009763 W EP 2008009763W WO 2009074208 A2 WO2009074208 A2 WO 2009074208A2
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- active material
- material according
- carbon
- lithium
- phase
- Prior art date
Links
Classifications
-
- 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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/009—Compounds containing, besides iron, two or more other elements, with the exception of oxygen or hydrogen
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/40—Cobaltates
- C01G51/42—Cobaltates containing alkali metals, e.g. LiCoO2
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/006—Compounds containing, besides nickel, two or more other elements, with the exception of oxygen or hydrogen
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/40—Nickelates
- C01G53/42—Nickelates containing alkali metals, e.g. LiNiO2
-
- 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
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/50—Solid solutions
- C01P2002/52—Solid solutions containing elements as dopants
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
-
- 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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
-
- 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
Definitions
- the present invention relates to lithium batteries, accumulators or batteries, and more particularly to an active material for the rechargeable battery negative electrode.
- Li-ion type batteries are intended for new applications (portable electronics, wireless tools, hybrid vehicles) that always require more power and energy to meet the needs. They must be stable with long cycle and calendar life. Finally, they must meet societal requirements related to safety and the protection of the environment.
- Graphite is commonly used as a negative electrode for Li-ion batteries.
- lithium titanate oxide ramsdellite, Li 2 Ti 3 O 7
- Such a negative electrode material operates at a voltage higher than that of carbon (> 1V), thus ensuring better operational safety.
- it is less subject to polarization, that is to say the difference between potential charge and discharge, that the graphite and is therefore suitable for use requiring high power.
- the capacity of this material is however relatively low, reaching about 130 Ah / kg at low speed (C / 15) and 100 Ah / kg at high speed (1 C), but has the advantage of having excellent reversibility during fast cycling.
- the reversible capacity at low speed can now reach 140 Ah / kg, thanks to an additional substitution by one or two of the following elements: Ti 3+ ,
- the present invention proposes to further improve the substituted ramsdellite, so as to obtain an improved specific capacity, while preserving the other qualities of the existing poly-substituted product.
- the present invention specifically relates to a negative electrode material that meets the aforementioned needs.
- the invention relates to an active material for lithium battery electrode comprising a phase having the general formula Li 2 + v -4 cCcTi 3 -WFe x MyM ' z O 7 - ⁇ , in which M and M 1 are metal ions groups 2 to 15 having an ionic radius between 0.5 and 0.8 ⁇ in octahedral oxygen environment, v, w, x, y, z and ⁇ being linked by the relationships:
- the M and M 'ions can be selected from the list composed of Ti 3+ , Co 2+ , Co 3+ , Ni 2+ , Ni 3+ Cu 2+ , Mg 2+ , Al 3+ , In 3+ , Sn 4+ , Sb 3+ , and Sb 5+ .
- M is preferably Ni 2+ and M 'of Al 3+ .
- Another subject of the invention relates to a process for synthesizing the active material defined above, and comprising the steps of:
- the cooling of the ceramic phase is at least 100 ° C / min, from the synthesis temperature to less than 400 ° C.
- the invention also relates to the use of the active material defined above for the manufacture of batteries, accumulators or lithium batteries.
- the invention finally also relates to batteries, accumulators or lithium batteries comprising the active material defined above.
- the material of the invention has mass and volume capacities of up to 190 Ah / kg, ie 602 Ah / m 3 , ie higher than those of the state of the art, while retaining the previously acquired advantages. , especially:
- the ramsdellite structure consists of a network comprising Ti and Li atoms in an octahedral environment of oxygen and channels partially occupied by Li atoms in a tetrahedral environment. This arrangement leaves a large number of vacant tetrahedral sites in the channels and the Li / gap distribution can vary depending on the synthesis conditions.
- the substitution metals occupy the octahedral sites of the network.
- the first step of the process according to the invention comprises a reactive mixture of compounds.
- Solid precursors in the form of fine powder, are selected and mixed.
- This mixture preferably comprises oxides of Ti and Fe, as well as those of metals M and M '.
- Other precursors are also suitable, these being organic and / or inorganic compounds capable of forming Me-O-Me bonds (where Me is a metal) by condensation or hydrolysis / condensation.
- oxides, carbonates, acetates, hydroxides, chlorides (eg AlCl 3 ), nitrates, Me-oxoalkoxides this list not being exhaustive and the man of the profession will be able to complete it.
- As for lithium it may be provided by another precursor, such as an oxide, hydroxide, or chloride. Li 2 CO 3 is however preferred.
- the mixture will also comprise carbon or carbon precursors which will be the simplest hydrocarbon phases such as monosaccharides or monosaccharides, for example glucose, fructose, sucrose, ascorbic acid, and polysaccharides corresponding to the condensation of monosaccharides. as starch, cellulose and glycogen.
- carbon or carbon precursors which will be the simplest hydrocarbon phases such as monosaccharides or monosaccharides, for example glucose, fructose, sucrose, ascorbic acid, and polysaccharides corresponding to the condensation of monosaccharides. as starch, cellulose and glycogen.
- the proportion of each of the metals in the precursor mixture corresponds to the stoichiometric proportion of the target material, leading to the formation of the composite.
- the proportion of carbon will be calculated taking into account the losses of CO and CO 2 by oxidation. This proportion may be increased if excess grain is desired at the grain boundaries.
- the second step of the process according to the invention comprises a heat treatment.
- the heat treatment is carried out under a controlled atmosphere (eg N 2 , Ar); it is carried out at a temperature which can be between 980 ° C and 1050 ° C, preferably between 1:30 and 2 h, to obtain good crystallinity, correlated with a limited particle size.
- a controlled atmosphere eg N 2 , Ar
- the rise in temperature to reach the reaction stage can be carried out in a single fast step because it makes it possible to minimize side reactions and the formation of undesirable titanates.
- the last step is to cool the material quickly.
- the manufacturing process as a whole is fast and has a reduced implementation cost.
- Figure 1 Photos of scanning electron microscopy of Li 2 Ti 3 O 7 substituted Fe, Ni, Al material without carbon (a) and with different carbon levels, of 0.14 (b), 0.27 (c) and 0.68 (d) mole per mole of synthesized material.
- FIG. 2 Comparison of infrared spectroscopy bands between the different materials substituted Fe, Ni, Al synthesized without carbon (a) and with different carbon levels, of 0.14 (b), 0.27 (c) and 0.68 (d) mole per mole of synthesized material.
- Figure 3 Galvanic charge / discharge curves in the C / 15 regime of Li 2 Ti 3 O 7 material substituted Fe, Ni, Al without carbon (a) and with 0.27 (b) mole of carbon per mole of synthesized material.
- Reactive grinding of Li 2 CO 3 compounds (0.7235 g), nanotallic TiO 2 anatase (1.2028 g), Fe 2 O 3 (0.021 g), NiO (0.0393 g) and finally Al 2 O 3 (0.0134 g) is performed in a Pulverisette ® 7 (duration 15 min; speed 8) with agate balls and a ball weight ratio / mass product equal to 10.
- the heat treatment is performed in nacelle under Ar one step. A ramp of 7 ° C / min is applied up to a synthesis temperature of 980 ° C, this temperature being maintained for 1h30.
- the cooling is carried out rapidly, under argon, so as to freeze the high temperature structure.
- Sucrose is added as carbon precursor, representing 5, 10 and 15% by mass relative to the total weight weighed before synthesis. Refer to Table 1 for different carbon levels.
- a reagent grinding of the compounds Li 2 CO 3, TiO 2 anatase nanosized, Fe 2 O 3, NiO, Al 2 O 3 in stoichiometric amounts, and sucrose is carried out in a Pulverisette ® 7 (duration 15 min; rate 8) with agate balls and a bead / mass mass ratio of product equal to 10.
- the heat treatment is carried out as in Example 1.
- Figure 1 shows the photos of scanning microscopy of the various synthesized examples.
- the IR spectra of FIG. 2 show (bd) for the products prepared according to examples 2 to 4, the presence of vibration bands between 1430 and 1500 cm -1 , characteristic of the CO 3 2 "group . This confirms the substitution of carbon in the ramsdellite structure.
- the product prepared according to Example 4 shows (d) also vibration bands at about 1650 cm -1, which correspond to the conjugated CC bonds which belong to the surface carbon.
- the electrochemical tests are performed in a half-cell with two electrodes, the negative of which is a lithium metal washer.
- the positive comprises a mixture of 85% by weight of active material, 5% by weight of carbon black and 10% by weight of PTFE binder.
- the electrolyte used is LiPF 6 (1 M) in ethylene carbonate, dimethyl carbonate and propylene carbonate (1: 3: 1).
- the cycling is carried out in galvanostatic mode at 25 ° C between 1 and 2.5 V vs. Li / Li + at diets of C / 15 and 1 C.
- FIG. 3 (a) shows the charge and discharge (vs. Li) curves of the carbon-free material, prepared according to example 1.
- FIG. 3 (b) corresponds to the material with carbon, according to example 3. These measurements are performed in galvanostatic mode at a C / 15 rate between 1 and 2.5 V vs Li / Li + .
- the observed capacity for the carbon-free material is 130 Ah / kg.
- the curve shows a shoulder between 1.4 and 2.5 V. Thanks to the carbon, the values of the reversible capacities are improved, reaching here 180 Ah / kg, with a low irreversible capacity of 8 Ah / kg, and a low polarization of 67 mV.
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
Description
Claims
Priority Applications (7)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
KR1020107013399A KR101439586B1 (ko) | 2007-12-10 | 2008-11-19 | Li-이온 배터리용 음극 물질 |
CN2008801200794A CN101918317B (zh) | 2007-12-10 | 2008-11-19 | 用于锂离子电池的负极材料 |
CA2708708A CA2708708C (fr) | 2007-12-10 | 2008-11-19 | Materiau d'electrode negative pour batteries li-ion |
BRPI0821589A BRPI0821589A2 (pt) | 2007-12-10 | 2008-11-19 | material ativo para um eletrodo de bateria de lítio, método para sintetizar o material sintético, uso, e, célula, acumulador ou bateria de lítio contendo um material ativo |
US12/746,319 US8486309B2 (en) | 2007-12-10 | 2008-11-19 | Negative electrode material for Li-ion batteries |
EP08859157A EP2231524A2 (fr) | 2007-12-10 | 2008-11-19 | Materiau d'electrode negative pour batteries li-ion |
JP2010537271A JP5389046B2 (ja) | 2007-12-10 | 2008-11-19 | Liイオン電池のための負電極材料 |
Applications Claiming Priority (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP07291475.7 | 2007-12-10 | ||
EP07291475 | 2007-12-10 | ||
US633008P | 2008-01-07 | 2008-01-07 | |
US61/006.330 | 2008-01-07 |
Publications (2)
Publication Number | Publication Date |
---|---|
WO2009074208A2 true WO2009074208A2 (fr) | 2009-06-18 |
WO2009074208A3 WO2009074208A3 (fr) | 2009-09-17 |
Family
ID=39885000
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/EP2008/009763 WO2009074208A2 (fr) | 2007-12-10 | 2008-11-19 | Materiau d'electrode negative pour batteries li-ion |
Country Status (9)
Country | Link |
---|---|
US (1) | US8486309B2 (fr) |
EP (1) | EP2231524A2 (fr) |
JP (1) | JP5389046B2 (fr) |
KR (1) | KR101439586B1 (fr) |
CN (1) | CN101918317B (fr) |
BR (1) | BRPI0821589A2 (fr) |
CA (1) | CA2708708C (fr) |
TW (1) | TWI462378B (fr) |
WO (1) | WO2009074208A2 (fr) |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP2415105A1 (fr) * | 2009-03-30 | 2012-02-08 | Umicore | Matériau actif négatif haute tension pour batterie au lithium rechargeable |
WO2014006600A1 (fr) | 2012-07-06 | 2014-01-09 | Saint-Gobain Centre De Recherches Et D'etudes Europeen | Produit fondu a base de lithium |
WO2014006599A1 (fr) | 2012-07-06 | 2014-01-09 | Saint-Gobain Centre De Recherches Et D'etudes Europeen | Produit fondu a base de lithium |
US20150044576A1 (en) * | 2012-02-29 | 2015-02-12 | Robert Bosch Gmbh | all-solid-state cell |
Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2011165372A (ja) * | 2010-02-05 | 2011-08-25 | Nippon Telegr & Teleph Corp <Ntt> | リチウム二次電池用負極材料とその製造方法およびリチウム二次電池 |
US7909576B1 (en) * | 2010-06-24 | 2011-03-22 | General Electric Company | Fastening device for rotor blade component |
JP5662261B2 (ja) * | 2011-06-20 | 2015-01-28 | 日本電信電話株式会社 | リチウム二次電池用負極材料製造方法及びリチウム二次電池 |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2003030283A1 (fr) * | 2001-10-02 | 2003-04-10 | Valence Technology, Inc. | Pile au lithium a base de titanates de metal de transition lithie |
WO2004100292A1 (fr) * | 2003-05-09 | 2004-11-18 | Umicore | Electrode negative pour batteries au lithium |
Family Cites Families (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH11283624A (ja) * | 1998-03-31 | 1999-10-15 | Matsushita Electric Ind Co Ltd | リチウム二次電池およびその製造方法 |
JP2001185141A (ja) | 1999-12-22 | 2001-07-06 | Kyocera Corp | リチウム電池 |
JP2002008658A (ja) | 2000-06-27 | 2002-01-11 | Toyota Central Res & Dev Lab Inc | リチウム二次電池電極活物質用リチウムチタン複合酸化物およびその製造方法 |
CA2327370A1 (fr) * | 2000-12-05 | 2002-06-05 | Hydro-Quebec | Nouvelle methode de fabrication de li4ti5o12 pur a partir du compose ternaire tix-liy-carbone: effet du carbone sur la synthese et la conductivite de l'electrode |
EP1261050A1 (fr) * | 2001-05-23 | 2002-11-27 | n.v. Umicore s.a. | Poudre de phosphate de lithium et d'un métal de transition pour piles rechargeables |
CN100448071C (zh) * | 2003-03-18 | 2008-12-31 | 黄穗阳 | 锂电池正极材料及其制备方法 |
-
2008
- 2008-11-19 WO PCT/EP2008/009763 patent/WO2009074208A2/fr active Application Filing
- 2008-11-19 KR KR1020107013399A patent/KR101439586B1/ko not_active IP Right Cessation
- 2008-11-19 CN CN2008801200794A patent/CN101918317B/zh not_active Expired - Fee Related
- 2008-11-19 US US12/746,319 patent/US8486309B2/en not_active Expired - Fee Related
- 2008-11-19 EP EP08859157A patent/EP2231524A2/fr not_active Withdrawn
- 2008-11-19 JP JP2010537271A patent/JP5389046B2/ja not_active Expired - Fee Related
- 2008-11-19 BR BRPI0821589A patent/BRPI0821589A2/pt not_active IP Right Cessation
- 2008-11-19 CA CA2708708A patent/CA2708708C/fr not_active Expired - Fee Related
- 2008-12-09 TW TW097147837A patent/TWI462378B/zh not_active IP Right Cessation
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2003030283A1 (fr) * | 2001-10-02 | 2003-04-10 | Valence Technology, Inc. | Pile au lithium a base de titanates de metal de transition lithie |
WO2004100292A1 (fr) * | 2003-05-09 | 2004-11-18 | Umicore | Electrode negative pour batteries au lithium |
EP1623473B1 (fr) * | 2003-05-09 | 2006-06-21 | Umicore | Electrode negative pour batteries au lithium |
Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP2415105A1 (fr) * | 2009-03-30 | 2012-02-08 | Umicore | Matériau actif négatif haute tension pour batterie au lithium rechargeable |
JP2012522339A (ja) * | 2009-03-30 | 2012-09-20 | ユミコア ソシエテ アノニム | 再充電可能なリチウム電池のための高電圧負極活性材料 |
EP2415105B1 (fr) * | 2009-03-30 | 2013-10-23 | Umicore | Matériau actif négatif haute tension pour une batterie au lithium rechargeable |
US8628694B2 (en) | 2009-03-30 | 2014-01-14 | Umicore | High voltage negative active material for a rechargeable lithium battery |
US20150044576A1 (en) * | 2012-02-29 | 2015-02-12 | Robert Bosch Gmbh | all-solid-state cell |
US9647265B2 (en) * | 2012-02-29 | 2017-05-09 | Robert Bosch Gmbh | All-solid state cell |
WO2014006600A1 (fr) | 2012-07-06 | 2014-01-09 | Saint-Gobain Centre De Recherches Et D'etudes Europeen | Produit fondu a base de lithium |
WO2014006599A1 (fr) | 2012-07-06 | 2014-01-09 | Saint-Gobain Centre De Recherches Et D'etudes Europeen | Produit fondu a base de lithium |
Also Published As
Publication number | Publication date |
---|---|
EP2231524A2 (fr) | 2010-09-29 |
KR101439586B1 (ko) | 2014-09-11 |
JP5389046B2 (ja) | 2014-01-15 |
KR20100113488A (ko) | 2010-10-21 |
CN101918317B (zh) | 2013-03-27 |
TW200941801A (en) | 2009-10-01 |
WO2009074208A3 (fr) | 2009-09-17 |
US20110042628A1 (en) | 2011-02-24 |
BRPI0821589A2 (pt) | 2015-09-29 |
TWI462378B (zh) | 2014-11-21 |
CA2708708C (fr) | 2013-11-05 |
US8486309B2 (en) | 2013-07-16 |
CA2708708A1 (fr) | 2009-06-18 |
CN101918317A (zh) | 2010-12-15 |
JP2011507166A (ja) | 2011-03-03 |
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