JP2014535145A - リチウム空気電池用の水性電解液 - Google Patents
リチウム空気電池用の水性電解液 Download PDFInfo
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- 239000003792 electrolyte Substances 0.000 title claims abstract description 36
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims abstract description 131
- 239000000654 additive Substances 0.000 claims abstract description 45
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 43
- 230000000996 additive effect Effects 0.000 claims abstract description 40
- 239000007864 aqueous solution Substances 0.000 claims abstract description 35
- 238000000034 method Methods 0.000 claims abstract description 12
- 239000007784 solid electrolyte Substances 0.000 claims abstract description 9
- 238000007599 discharging Methods 0.000 claims abstract description 5
- 239000007788 liquid Substances 0.000 claims abstract description 5
- 229910001416 lithium ion Inorganic materials 0.000 claims description 31
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 28
- 229910052760 oxygen Inorganic materials 0.000 claims description 28
- 239000001301 oxygen Substances 0.000 claims description 28
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 27
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims description 22
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 22
- 239000008151 electrolyte solution Substances 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 7
- 229920000620 organic polymer Polymers 0.000 claims description 5
- 239000005518 polymer electrolyte Substances 0.000 claims description 5
- 150000001768 cations Chemical class 0.000 claims description 4
- 239000013078 crystal Substances 0.000 claims description 4
- 150000008044 alkali metal hydroxides Chemical class 0.000 claims description 3
- 238000010924 continuous production Methods 0.000 claims description 3
- 239000007772 electrode material Substances 0.000 claims description 2
- 229920005597 polymer membrane Polymers 0.000 claims description 2
- FUJCRWPEOMXPAD-UHFFFAOYSA-N lithium oxide Chemical compound [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 claims 2
- 229910001947 lithium oxide Inorganic materials 0.000 claims 2
- 150000001450 anions Chemical class 0.000 claims 1
- 239000000243 solution Substances 0.000 description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 16
- 238000006243 chemical reaction Methods 0.000 description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 10
- 230000000694 effects Effects 0.000 description 10
- 229910000831 Steel Inorganic materials 0.000 description 9
- 239000010959 steel Substances 0.000 description 9
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 8
- 229910052799 carbon Inorganic materials 0.000 description 8
- 239000000203 mixture Substances 0.000 description 7
- 229920006395 saturated elastomer Polymers 0.000 description 7
- 238000006722 reduction reaction Methods 0.000 description 6
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical group [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 5
- 229910001413 alkali metal ion Inorganic materials 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 5
- 239000004744 fabric Substances 0.000 description 5
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 5
- 229910052700 potassium Inorganic materials 0.000 description 5
- 239000011591 potassium Substances 0.000 description 5
- 229910001414 potassium ion Inorganic materials 0.000 description 5
- 239000002244 precipitate Substances 0.000 description 5
- 230000009467 reduction Effects 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 4
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 239000012528 membrane Substances 0.000 description 4
- 229910052759 nickel Inorganic materials 0.000 description 4
- 229910010293 ceramic material Inorganic materials 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 230000002401 inhibitory effect Effects 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 239000011149 active material Substances 0.000 description 2
- 229910052783 alkali metal Inorganic materials 0.000 description 2
- 150000001340 alkali metals Chemical class 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- -1 hydroxyl ions Chemical class 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000003760 magnetic stirring Methods 0.000 description 2
- 239000007773 negative electrode material Substances 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000007790 solid phase Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical group C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229910012305 LiPON Inorganic materials 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000004931 aggregating effect Effects 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000005349 anion exchange Methods 0.000 description 1
- 239000012736 aqueous medium Substances 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 229910000428 cobalt oxide Inorganic materials 0.000 description 1
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 1
- 230000002542 deteriorative effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 230000009931 harmful effect Effects 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 239000000138 intercalating agent Substances 0.000 description 1
- 229910003002 lithium salt Inorganic materials 0.000 description 1
- 159000000002 lithium salts Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 150000002926 oxygen Chemical class 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 239000011253 protective coating Substances 0.000 description 1
- 238000012552 review Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000005063 solubilization Methods 0.000 description 1
- 230000003381 solubilizing effect Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000002226 superionic conductor Substances 0.000 description 1
- BHZCMUVGYXEBMY-UHFFFAOYSA-N trilithium;azanide Chemical compound [Li+].[Li+].[Li+].[NH2-] BHZCMUVGYXEBMY-UHFFFAOYSA-N 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
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Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M12/00—Hybrid cells; Manufacture thereof
- H01M12/02—Details
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/24—Alkaline accumulators
- H01M10/26—Selection of materials as electrolytes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M12/00—Hybrid cells; Manufacture thereof
- H01M12/04—Hybrid cells; Manufacture thereof composed of a half-cell of the fuel-cell type and of a half-cell of the primary-cell type
- H01M12/06—Hybrid cells; Manufacture thereof composed of a half-cell of the fuel-cell type and of a half-cell of the primary-cell type with one metallic and one gaseous electrode
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M12/00—Hybrid cells; Manufacture thereof
- H01M12/08—Hybrid cells; Manufacture thereof composed of a half-cell of a fuel-cell type and a half-cell of the secondary-cell type
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
- H01M10/0566—Liquid materials
- H01M10/0567—Liquid materials characterised by the additives
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M2220/00—Batteries for particular applications
- H01M2220/20—Batteries in motive systems, e.g. vehicle, ship, plane
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M2220/00—Batteries for particular applications
- H01M2220/30—Batteries in portable systems, e.g. mobile phone, laptop
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M2300/00—Electrolytes
- H01M2300/0002—Aqueous electrolytes
- H01M2300/0014—Alkaline electrolytes
-
- 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
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Hybrid Cells (AREA)
- Cell Separators (AREA)
- Secondary Cells (AREA)
Abstract
Description
本発明は、電気化学的デバイス(具体的には水性電解液を有するリチウム空気型の電池)並びに本発明のリチウム空気電池を用いて電気エネルギーの蓄電および放電を行う方法に関する。
〔背景技術〕
電池の単位質量当たりのエネルギー密度(Wh/kgと表される)は、今もなお、携帯電気機器(例えば携帯電子機器または電気自動車など)への電池の利用を制限する主な要因となっている。これら電池の限られたエネルギー密度は、主に、電池材料の性能に起因している。一般的に、現在利用可能な負極材料のうち最も良好な負極材料の比容量は300Ah/kg〜350Ah/kgである。これが正極材料になると、比容量は僅か100Ah/kg〜150Ah/kg程度となる。
〔発明の概要〕
本発明の対象は、リチウム金属を含む負極区画と、水酸化リチウムを含有する水溶液と接している、少なくとも1つの空気正極を備える正極区画と、前記正極区画から前記負極区画を気体および液体を通さないように隔てる固体電解質とを備え、水酸化リチウムを含有する前記水溶液は、リチウムイオンの溶解度を低下させる少なくとも1つの添加剤をさらに含んでいるリチウム空気電池である。
〔図面の簡単な説明〕
実施例および添付の図面に照らせば、本発明はより良く理解されるであろう。なお、実施例は本発明を限定するものではなく、その一例に過ぎない。添付の図面では:
図1は、溶液中のLi+イオンの飽和濃度をK+イオンの濃度の関数として示すグラフ(理論上の濃度およびICP−AESで実際に測定した濃度)である。
〔実施例〕
(電解液の調整)
水酸化リチウムで飽和し、本発明の添加剤(本実施例ではカリウム)を1M〜8Mの異なる濃度で含む水溶液を以下の手順に従い調製した。
こうして調整した電解質をICP−AES法により分析した。K0LiSat溶液に関しては電解質を1000倍の間で希釈し、K8LiSat混合体に関しては電解質を10,000倍の間で希釈した。ICP−AES(Inductively Coupled Plasma-Atomic Emission Spectrometry)分析方法の詳細はKlaus G. Heumannによる“Handbook of Elemental Speciation: Techniques and Methodology”に記載されている。
316Lスチール織物上において、操作から30分経過後に33mA.cm−2の酸素放出反応電位を測定した。電極表面の触媒層の発達に起因した変化による擾乱を回避するために、各回毎に新たな電極を使用した。
0.19cm2の幾何学的表面積を有する回転ディスク電極(turning disk electrode:TDE)上において、316Lスチールの電極の電極触媒性能の測定を準定常モードで記録した(T=25℃;vb=0.1mVs−1;Sgeo=0.19cm2)。
値=((K0LiSatのηO2)−(KxLiSatのηO2))/K0LiSatのηO2
結論としては、上記水性電解液中に添加剤を使用することは、過電圧を著しく低減し、したがって、水性電解液を設けたリチウム空気電池を含む種類のシステムの電流下における酸素放出電極のエネルギー損失を著しく低減する。
Claims (10)
- リチウム金属を含む負極区画と、
水酸化リチウムを含む水溶液と接している、少なくとも1つの空気正極を備える正極区画と、
前記負極区画を前記正極区画から気体および液体を通さないように分離する固体電解質と、を備え、
水酸化リチウムを含む前記水溶液は、リチウムイオンの溶解度を低減させる少なくとも1つの添加剤をさらに含んでいるリチウム空気電池。 - 上記添加剤を含む上記水溶液中の水酸化リチウムの溶解限度は、4mol/L未満であり、より好ましくは3mol/L未満であり、さらに好ましくは1mol/L〜2mol/Lであることを特徴とする請求項1に記載のリチウム空気電池。
- リチウムイオンの溶解度を低減させる上記添加剤はアルカリ金属水酸化物であることを特徴とする請求項1または2に記載のリチウム空気電池。
- リチウムイオンの溶解度を低減させる上記添加剤は、水酸化カリウムおよび水酸化ナトリウムから成る群から選択され、
上記添加剤は、好ましくは水酸化カリウムであることを特徴とする請求項3に記載のリチウム空気電池。 - 上記固体電解質の表面上に酸化リチウムが結晶層を密に形成することを防止する手段を備える請求項1〜4の何れか1項に記載のリチウム空気電池。
- 上記固体電解質の表面上に酸化リチウムが結晶層を密に形成することを防止する上記手段は、カチオン伝導性の有機高分子電解質であることを特徴とする請求項5に記載のリチウム空気電池。
- 上記水酸化リチウムを含む水溶液と接する酸素放出正極をさらに備える請求項1〜6の何れか1項に記載のリチウム空気電池。
- 上記空気正極は、電極材と電解液を含む上記水溶液との間を分離するアニオン交換性の高分子膜をさらに備えることを特徴とする請求項1〜7の何れか1項に記載のリチウム空気電池。
- 請求項1〜8の何れか1項に記載のリチウム空気電池を使用して電気エネルギーの蓄電および放電を行う方法であって、
(a)負極区画に含まれるリチウム金属が正極区画の水溶液中にて酸化し、水酸化リチウムの形態で沈殿する充電工程および、
(b)前記負極側で還元されるリチウムイオンを遊離化するために前記水酸化リチウムが可溶化する再充電工程、
という連続する工程を含む方法。 - リチウム空気電池のエネルギー効率を向上させることを目的とした、リチウムイオンの溶解度を低減させる少なくとも1つの添加剤の使用法であって、
前記添加剤は、前記リチウム空気電池の電解液を構成する、水酸化リチウムを含む水溶液中に含まれていることを特徴とする使用法。
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR1160224A FR2982427B1 (fr) | 2011-11-09 | 2011-11-09 | Electrolyte aqueux pour batterie lithium-air |
FR1160224 | 2011-11-09 | ||
PCT/FR2012/052576 WO2013068694A1 (fr) | 2011-11-09 | 2012-11-08 | Electrolyte aqueux pour batterie lithium-air |
Publications (2)
Publication Number | Publication Date |
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JP2014535145A true JP2014535145A (ja) | 2014-12-25 |
JP5851624B2 JP5851624B2 (ja) | 2016-02-03 |
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Application Number | Title | Priority Date | Filing Date |
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JP2014540539A Active JP5851624B2 (ja) | 2011-11-09 | 2012-11-08 | リチウム空気電池用の水性電解液 |
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Country | Link |
---|---|
US (1) | US9461348B2 (ja) |
EP (1) | EP2777090B1 (ja) |
JP (1) | JP5851624B2 (ja) |
KR (1) | KR101632676B1 (ja) |
CN (1) | CN103931049B (ja) |
CA (1) | CA2854049C (ja) |
ES (1) | ES2569255T3 (ja) |
FR (1) | FR2982427B1 (ja) |
SG (1) | SG11201402072WA (ja) |
WO (1) | WO2013068694A1 (ja) |
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US10535901B2 (en) | 2015-04-06 | 2020-01-14 | The Trustees Of Princeton University | Alkaline battery electrolyte useful for a rechargeable alkaline electrochemical cell |
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SG11201402072WA (en) | 2014-09-26 |
CN103931049B (zh) | 2017-05-24 |
US20150140453A1 (en) | 2015-05-21 |
WO2013068694A1 (fr) | 2013-05-16 |
CA2854049A1 (fr) | 2013-05-16 |
JP5851624B2 (ja) | 2016-02-03 |
ES2569255T3 (es) | 2016-05-09 |
EP2777090A1 (fr) | 2014-09-17 |
KR101632676B1 (ko) | 2016-06-22 |
FR2982427A1 (fr) | 2013-05-10 |
EP2777090B1 (fr) | 2016-02-10 |
CA2854049C (fr) | 2017-04-18 |
CN103931049A (zh) | 2014-07-16 |
FR2982427B1 (fr) | 2013-12-20 |
KR20140074392A (ko) | 2014-06-17 |
US9461348B2 (en) | 2016-10-04 |
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