WO2014092312A1 - 이온성 액체를 포함하는 고체 전해질 - Google Patents
이온성 액체를 포함하는 고체 전해질 Download PDFInfo
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- WO2014092312A1 WO2014092312A1 PCT/KR2013/008738 KR2013008738W WO2014092312A1 WO 2014092312 A1 WO2014092312 A1 WO 2014092312A1 KR 2013008738 W KR2013008738 W KR 2013008738W WO 2014092312 A1 WO2014092312 A1 WO 2014092312A1
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- Prior art keywords
- solid electrolyte
- gel
- ionic liquid
- type solid
- metal oxide
- Prior art date
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- 239000007784 solid electrolyte Substances 0.000 title claims abstract description 51
- 239000002608 ionic liquid Substances 0.000 title claims abstract description 41
- -1 silane compound Chemical class 0.000 claims abstract description 40
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 26
- 229910000077 silane Inorganic materials 0.000 claims abstract description 26
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 23
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 10
- 229910052736 halogen Inorganic materials 0.000 claims abstract description 6
- 150000002367 halogens Chemical class 0.000 claims abstract description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 6
- 239000001257 hydrogen Substances 0.000 claims abstract description 6
- 229910003002 lithium salt Inorganic materials 0.000 claims description 15
- 159000000002 lithium salts Chemical class 0.000 claims description 15
- 239000002253 acid Substances 0.000 claims description 11
- 239000003990 capacitor Substances 0.000 claims description 10
- 125000004432 carbon atom Chemical group C* 0.000 claims description 8
- 238000006460 hydrolysis reaction Methods 0.000 claims description 8
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 7
- 229910052744 lithium Inorganic materials 0.000 claims description 7
- 150000001768 cations Chemical class 0.000 claims description 6
- 150000001450 anions Chemical class 0.000 claims description 5
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims description 5
- RAXXELZNTBOGNW-UHFFFAOYSA-O Imidazolium Chemical compound C1=C[NH+]=CN1 RAXXELZNTBOGNW-UHFFFAOYSA-O 0.000 claims description 4
- 229910013063 LiBF 4 Inorganic materials 0.000 claims description 4
- 229910013870 LiPF 6 Inorganic materials 0.000 claims description 4
- RWRDLPDLKQPQOW-UHFFFAOYSA-O Pyrrolidinium ion Chemical compound C1CC[NH2+]C1 RWRDLPDLKQPQOW-UHFFFAOYSA-O 0.000 claims description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 3
- 229910015015 LiAsF 6 Inorganic materials 0.000 claims description 3
- 229910013372 LiC 4 Inorganic materials 0.000 claims description 3
- 229910013872 LiPF Inorganic materials 0.000 claims description 3
- 229910012513 LiSbF 6 Inorganic materials 0.000 claims description 3
- 101150058243 Lipf gene Proteins 0.000 claims description 3
- NQRYJNQNLNOLGT-UHFFFAOYSA-O Piperidinium(1+) Chemical compound C1CC[NH2+]CC1 NQRYJNQNLNOLGT-UHFFFAOYSA-O 0.000 claims description 3
- NVIANCROYQGROD-UHFFFAOYSA-N bis(fluorosulfonyl)azanide Chemical compound FS(=O)(=O)[N-]S(F)(=O)=O NVIANCROYQGROD-UHFFFAOYSA-N 0.000 claims description 3
- DWYMPOCYEZONEA-UHFFFAOYSA-L fluoridophosphate Chemical compound [O-]P([O-])(F)=O DWYMPOCYEZONEA-UHFFFAOYSA-L 0.000 claims description 3
- KTQDYGVEEFGIIL-UHFFFAOYSA-N n-fluorosulfonylsulfamoyl fluoride Chemical compound FS(=O)(=O)NS(F)(=O)=O KTQDYGVEEFGIIL-UHFFFAOYSA-N 0.000 claims description 3
- 125000001153 fluoro group Chemical group F* 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 6
- 230000008901 benefit Effects 0.000 abstract description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052799 carbon Inorganic materials 0.000 abstract description 3
- 150000002431 hydrogen Chemical class 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 11
- 239000003792 electrolyte Substances 0.000 description 10
- 238000000034 method Methods 0.000 description 10
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 8
- 238000001879 gelation Methods 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 5
- 238000005259 measurement Methods 0.000 description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 description 3
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 3
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 3
- 229910001416 lithium ion Inorganic materials 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 2
- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- 150000001408 amides Chemical class 0.000 description 2
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000002484 cyclic voltammetry Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000008151 electrolyte solution Substances 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 description 2
- 239000003063 flame retardant Substances 0.000 description 2
- 235000019253 formic acid Nutrition 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- TZIHFWKZFHZASV-UHFFFAOYSA-N methyl formate Chemical compound COC=O TZIHFWKZFHZASV-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000005486 organic electrolyte Substances 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- ZXMGHDIOOHOAAE-UHFFFAOYSA-N 1,1,1-trifluoro-n-(trifluoromethylsulfonyl)methanesulfonamide Chemical compound FC(F)(F)S(=O)(=O)NS(=O)(=O)C(F)(F)F ZXMGHDIOOHOAAE-UHFFFAOYSA-N 0.000 description 1
- DOYSIZKQWJYULQ-UHFFFAOYSA-N 1,1,2,2,2-pentafluoro-n-(1,1,2,2,2-pentafluoroethylsulfonyl)ethanesulfonamide Chemical compound FC(F)(F)C(F)(F)S(=O)(=O)NS(=O)(=O)C(F)(F)C(F)(F)F DOYSIZKQWJYULQ-UHFFFAOYSA-N 0.000 description 1
- WNXJIVFYUVYPPR-UHFFFAOYSA-N 1,3-dioxolane Chemical compound C1COCO1 WNXJIVFYUVYPPR-UHFFFAOYSA-N 0.000 description 1
- IQQRAVYLUAZUGX-UHFFFAOYSA-N 1-butyl-3-methylimidazolium Chemical compound CCCCN1C=C[N+](C)=C1 IQQRAVYLUAZUGX-UHFFFAOYSA-N 0.000 description 1
- OGLIVJFAKNJZRE-UHFFFAOYSA-N 1-methyl-1-propylpiperidin-1-ium Chemical compound CCC[N+]1(C)CCCCC1 OGLIVJFAKNJZRE-UHFFFAOYSA-N 0.000 description 1
- YQFWGCSKGJMGHE-UHFFFAOYSA-N 1-methyl-1-propylpyrrolidin-1-ium Chemical compound CCC[N+]1(C)CCCC1 YQFWGCSKGJMGHE-UHFFFAOYSA-N 0.000 description 1
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- UINDRJHZBAGQFD-UHFFFAOYSA-O 2-ethyl-3-methyl-1h-imidazol-3-ium Chemical compound CCC1=[NH+]C=CN1C UINDRJHZBAGQFD-UHFFFAOYSA-O 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 1
- 229910013684 LiClO 4 Inorganic materials 0.000 description 1
- 229910013131 LiN Inorganic materials 0.000 description 1
- RJUFJBKOKNCXHH-UHFFFAOYSA-N Methyl propionate Chemical compound CCC(=O)OC RJUFJBKOKNCXHH-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 description 1
- KXKVLQRXCPHEJC-UHFFFAOYSA-N acetic acid trimethyl ester Natural products COC(C)=O KXKVLQRXCPHEJC-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 125000005210 alkyl ammonium group Chemical group 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 239000000010 aprotic solvent Substances 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 239000011245 gel electrolyte Substances 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 150000003949 imides Chemical class 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 150000002596 lactones Chemical class 0.000 description 1
- 239000011244 liquid electrolyte Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229940017219 methyl propionate Drugs 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000011255 nonaqueous electrolyte Substances 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 150000004756 silanes Chemical class 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000000527 sonication Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- ZMANZCXQSJIPKH-UHFFFAOYSA-O triethylammonium ion Chemical compound CC[NH+](CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-O 0.000 description 1
- 238000002525 ultrasonication Methods 0.000 description 1
Images
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
- 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
- H01M10/0565—Polymeric materials, e.g. gel-type or solid-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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/06—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/54—Electrolytes
- H01G11/56—Solid electrolytes, e.g. gels; Additives therein
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/022—Electrolytes; Absorbents
- H01G9/025—Solid electrolytes
-
- 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
- H01M10/052—Li-accumulators
-
- 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
-
- 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
- H01M2300/0017—Non-aqueous electrolytes
- H01M2300/0025—Organic electrolyte
- H01M2300/0045—Room temperature molten salts comprising at least one organic ion
-
- 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
- H01M2300/0017—Non-aqueous electrolytes
- H01M2300/0065—Solid electrolytes
-
- 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
- H01M2300/0085—Immobilising or gelification of electrolyte
-
- 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
- H01M2300/0088—Composites
- H01M2300/0091—Composites in the form of mixtures
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- 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
-
- 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
- Y02E60/13—Energy storage using capacitors
Definitions
- the present invention relates to a solid electrolyte applied to an electrochemical double layer capacitor (EDLC) or a lithium secondary battery, and provides a flexible gel-type solid electrolyte.
- EDLC electrochemical double layer capacitor
- the present invention relates to a solid electrolyte applied to an electrochemical double layer capacitor (EDLC) or a lithium secondary battery, and provides a flexible gel-type solid electrolyte.
- Organic electrolytes used in lithium secondary batteries or electric double layer capacitors are polar aprotic organic solvents that are easy to dissolve lithium salts and are difficult to be electrolyzed, such as carbonates such as ethylene carbonate and propylene carbonate, dimethyl carbonate and methyl ethyl.
- Carbonate esters such as a carbonate and diethyl carbonate
- Lactones such as (gamma) -butyrolactone and 3-methyl- (gamma) -valerolactone
- ester such as methyl formate, methyl acetate, and methyl propionate
- 1,2-dimethoxy A liquid electrolyte in which lithium salts such as LiPF 6 , LiBF 4 , LiN (CF 3 SO 2 ) 2 , LiClO 4 , and LiCF 3 SO 3 are dissolved in organic solvents such as ethers such as ethane, tetrahydrofuran and dioxolane.
- the organic electrolyte has high ion conductivity, there are problems in the process due to volatility, low stability due to decomposition reaction at the electrode, and liquid state.
- ionic liquid is a room temperature molten salt composed of cations and anions, and has the characteristics of non-volatile, flame retardant, non-flammable, wide potential window and chemical stability. I am getting it.
- the ionic liquid is also liquid at room temperature, there is a disadvantage in that processability is poor when applied as an electrolyte.
- Japanese Laid-Open Patent Publication No. 2010-225511 proposes a gel electrolyte having improved durability formed by embedding an ionic liquid in porous particles.
- the solid electrolyte prepared using only porous metal oxide has a problem in that it is not flexible and easily broken when applied to an external impact or a product.
- the present invention is a solid electrolyte used in a lithium ion secondary battery or an electrochemical double layer capacitor (EDLC), a gel-type solid electrolyte having improved flexibility while maintaining the advantages of the conventional ionic liquid. To provide.
- EDLC electrochemical double layer capacitor
- the present invention provides a gel-type solid electrolyte comprising an ionic liquid in a porous metal oxide prepared from a silane compound represented by Formula 1 below:
- R 1 and R 2 are each independently an alkyl group having 1 to 3 carbon atoms
- R 3 , R 4 And R 5 are independently of each other hydrogen, a halogen element or an alkyl group having 1 to 5 carbon atoms,
- the porous metal oxide includes 30 to 50 wt% of the silane compound having 2 ⁇ x + y ⁇ 3 in Formula 1.
- the porous metal oxide is formed from a hydrolysis reaction in the presence of an acid of the silane compound of formula (1).
- the acid is used in the range of 1 to 50 parts by volume based on the entire silane compound of formula (1).
- the porous metal oxide includes a structure represented by the following formula:
- R in the above formula 3 , R 4 And R 5 are independently of each other hydrogen, a halogen element or an alkyl group having 1 to 5 carbon atoms.
- the ionic liquid includes imidazolium, ammonium, pyrrolidinium or piperidinium as a cation, and bis (fluorosulfonyl) imide as an anion.
- bis (fluorosulfonyl) imide bis (fluorosulfonyl) amide
- fluoroborate or fluorophosphate.
- the ionic liquid is included in the range of 100 to 200 parts by weight based on 100 parts by weight of the porous metal oxide.
- the solid electrolyte is LiPF 6 , LiBF 4 , LiAsF 6 , LiSbF 6 , LiCF 3 SO 3 , LiC 2 F 5 SO 3 , LiC 4 F 9 SO 3 , LiN (CF 3 SO 2 ) 2 , LiN (C At least one lithium salt selected from the group consisting of 2 F 5 SO 2 ) 2 , LiC (CF 3 SO 2 ) 3 , and LiPF 2 ⁇ (COO) 2 ⁇ 2 .
- the lithium salt is contained in 5 to 40% by weight based on the total solid electrolyte.
- the present invention provides a lithium secondary battery including the solid electrolyte.
- the present invention provides an electric double layer capacitor comprising the solid electrolyte.
- the processability of the ionic liquid can be improved by providing a gel-like solid electrolyte having improved flexibility including the ionic liquid. Therefore, the electrolyte may be advantageously used in the manufacturing process of the lithium secondary battery or the electric double layer capacitor to take advantage of the ionic liquid.
- FIG. 1 illustrates a manufacturing process of a solid electrolyte according to an embodiment of the present invention.
- FIG. 2 shows a device for measuring the ionic conductivity of a solid electrolyte of the present invention.
- Figure 3 shows a device for measuring the capacity in an electric double layer capacitor to which the solid electrolyte of the present invention is applied.
- the present invention provides a gel-type solid electrolyte with improved flexibility while retaining the benefits of an ionic liquid by effectively internalizing the ionic liquid into a porous metal oxide.
- the porous metal oxide is prepared from a silane compound represented by Formula 1 below:
- R 1 and R 2 are each independently an alkyl group having 1 to 3 carbon atoms
- R 3 , R 4 And R 5 are independently of each other hydrogen, a halogen element or an alkyl group having 1 to 5 carbon atoms,
- the silane compound forms a silane oxide compound having a network structure by a hydrolysis reaction.
- the present invention is characterized by using a silane compound containing a vinyl group in the case of 2 ⁇ x + y ⁇ 3 in the above formula (1) as a porous metal oxide for embedding the ionic liquid.
- Silane compounds comprising such vinyl groups are included between silane oxide compounds to form as follows, for example, as part of a network structure:
- the network structure is formed from the hydrolysis reaction of the silane compound of Formula 1, wherein the silane compound containing a vinyl group in the middle of the structure is introduced to terminate the network structure Will be achieved.
- the silane compound containing a vinyl group in the middle of the structure is introduced to terminate the network structure Will be achieved.
- the network structure is continuously generated, and thus the viscosity of the obtained material continues to increase, resulting in a hard state that is difficult to process.
- the vinyl group induces the termination of this network structure so that a result of a flexible state which is easy to process is obtained. Therefore, the use of a silane compound containing a vinyl group in the present invention is a means for forming a skeleton of a flexible solid electrolyte.
- the present invention provides a solid electrolyte comprising an ionic liquid embedded in a porous metal oxide obtained from a hydrolysis reaction of a silane compound represented by Chemical Formula 1.
- the porous metal oxide is preferably a silane compound containing a vinyl group, that is, 30 to 50% by weight of the silane compound in the case of 2 ⁇ x + y ⁇ 3 in the formula (1).
- the silane compound containing a vinyl group is used in an amount less than the above range, the effect of improving the flexibility is insignificant, resulting in poor workability, such as being broken in the process for use as a solid electrolyte.
- the gelation is not achieved to the desired level because this is also poor workability.
- the reaction proceeds preferably under acidic conditions for the hydrolysis reaction.
- an acid organic acids such as formic acid, hydrochloric acid, sulfuric acid, phosphoric acid, nitric acid and acetic acid can be used.
- the amount of these acids to be used is preferably in the range of 1 to 50 parts by volume based on the entire silane compound of formula (1). If the amount of the acid is less than the above range, hydrolysis does not occur to the desired level, and if the amount of the acid is used above the above range, the viscosity of the gel-like porous metal oxide obtained becomes too high, making it difficult to later mix with the ionic liquid.
- the solution is sonicate the solution so that hydrolysis occurs uniformly and effectively in the reaction product containing the silane compound of Formula 1 and an acid.
- Ultrasonication may be performed for 1 to 20 minutes at 40KHz. After sonication, the solution is cooled at 0 ° C to 10 ° C for 1 minute to 120 minutes.
- the ionic liquid is then added to allow the gel to proceed. That is, in the present invention, the gel-type solid electrolyte is hydrolyzed by the silane compound of Chemical Formula 1 to form a porous metal oxide having a network structure, and at the same time an ionic liquid is impregnated, so that the ionic liquid is contained in the porous metal oxide structure. It is manufactured in the form.
- the ionic liquid is an ionic substance in a molten state at room temperature (25 ° C.), and may be used without limitation as long as it includes a cation and an anion.
- Ionic liquids include, but are not limited to, imidazolium, ammonium, pyrrolidinium, or piperidinium, but are not limited to bis, including but not limited to cations. Fluorosulfonyl) imide, bis (fluorosulfonyl) amide, fluoroborate, or fluorophosphate.
- the cation include, for example, alkylammonium such as triethylammonium, imidazolium such as ethylmethylimidazolium and butylmethylimidazolium, pyrrolidinium such as 1-methyl-1-propylpyrrolidinium, or the like. Methyl propyl piperidinium is mentioned.
- anion examples include bis (trifluoromethylsulfonyl) imide (bis), bis (pentafluoroethylsulfonyl) amide (bis) (pentafluoroethylsufonyl) amide (BETI), tetra Fluoroborate (BF 4 ), or hexafluorophosphate (PF 6 ).
- the ionic liquid can be used alone as an electrolyte without using a separate solvent.
- the ionic liquid is preferably included in the solid electrolyte in the range of 100 to 200 parts by weight based on 100 parts by weight of the porous metal oxide.
- the solid electrolyte of the present invention is finally obtained by drying at room temperature for 1 hour or more or by heat treatment for 5 to 10 minutes in a temperature range of 300 ° C to 600 ° C.
- the electrolyte thus obtained is easy to process because it is a gel-like solid with improved flexibility. Therefore, it can be easily used as a solid electrolyte in the manufacturing process of a lithium secondary battery or an electric double layer capacitor.
- the solid electrolyte of the present invention is LiPF 6 , LiBF 4 , LiAsF 6 , LiSbF 6 , LiCF 3 SO 3 , LiC 2 F 5 SO 3 , LiC 4 F 9 SO 3 , LiN (CF 3 SO 2 ) 2 , LiN ( One or more lithium salts selected from the group consisting of C 2 F 5 SO 2 ) 2 , LiC (CF 3 SO 2 ) 3 , and LiPF 2 ⁇ (COO) 2 ⁇ 2 may be further included.
- the solid electrolyte containing lithium salt may be used as an electrolyte of a lithium ion battery. In this case, the lithium salt is preferably contained in 5 to 40% by weight based on the entire solid electrolyte.
- the lithium salt is preferably added together with the ionic liquid during the process of adding the ionic liquid to the reactant including the silane compound, the vinyl silane compound and the acid so that the gelation for forming the solid electrolyte proceeds. That is, lithium salt is included with the ionic liquid in the porous metal oxide structure.
- the lithium salt is dissolved in an ionic liquid in an Ar atmosphere glove box using a stirrer for at least 24 hours, and then an ionic liquid in which lithium salt is dissolved is added to the gelation process.
- a gel solid electrolyte containing a ionic liquid is synthesized.
- the lithium salt may be used in the form of an electrolyte solution dissolved in a solvent such as dimethyl carbonate (DMC), diethyl carbonate (DEC), methyl ethyl carbonate (MEC), ethylene carbonate (EC), propylene carbonate (PC), and mixtures thereof.
- DMC dimethyl carbonate
- DEC diethyl carbonate
- MEC methyl ethyl carbonate
- EC ethylene carbonate
- PC propylene carbonate
- TMOS tetramethoxysilane
- Triethoxyvinylsilane triethoxy vinylyl
- the obtained product was dried at room temperature for 1 hour to finally obtain a gel solid electrolyte.
- a solid electrolyte was obtained by performing the same process except using 2 mL of tetramethoxysilane in place of 1 mL of tetramethoxysilane (TMOS) and 1 mL of triethoxyvinylsilane.
- TMOS tetramethoxysilane
- conductivity measurement cell Inserting the solid electrolyte (1) in the two stainless steel electrodes (2) conductivity measurement cell (Swagelok cell) consists of, as first measuring the ionic conductivity shown in Figure 2 and then to 2 ⁇ 10 -2 Hz from 10 6 Conductance was measured up to the Hz range to measure conductivity.
- BMIMBF 4 ionic liquid butylmethyl imidazolium tetrafluoroborate
- the solid electrolyte of the Example and the comparative example was produced in the frame of 70 mm (width) x 150 mm (length) x 30 mm (thickness), respectively. Then, the center of the sample was fixed and the angle until the crack appeared by applying a force of 10 N in the same direction at both ends was measured.
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Abstract
Description
이온전도도 ( mS/cm ) | |
BMIMBF4 | 1.70 |
실시예 | 0.44 |
비교예 | 0.43 |
Capacitance (F/g) | |
BMIMBF4 | 30 |
실시예 | 25 |
비교예 | 22 |
깨짐(crack)각도 | |
실시예 | 40 |
비교예 | 2 |
Claims (11)
- 하기 화학식 1로 표현되는 실란 화합물로부터 제조되는 다공성 금속산화물 내에 이온성 액체를 포함시킨 것을 특징으로 하는 겔형의 고체 전해질:[화학식 1]Si(R1)x(OR2)y(CR3=CR4R5)(4-x-y)상기 식에서,R1 및 R2는 서로 독립적으로 탄소수 1 내지 3의 알킬기이고,R3, R4 및 R5는 서로 독립적으로 수소, 할로겐 원소 또는 탄소수 1 내지 5의 알킬기이며,0≤x≤3의 정수이고,1≤y≤4의 정수이며,2≤x+y≤4의 정수이다.
- 제1항에서,상기 다공성 금속산화물은 상기 화학식 1에서 2≤x+y≤3인 실란 화합물을 30 내지 50 중량% 포함하는 것을 특징으로 하는 겔형의 고체 전해질.
- 제1항에서,상기 다공성 금속산화물은 화학식 1의 실란 화합물의 산(acid) 존재하에서의 가수분해 반응으로부터 형성되는 것을 특징으로 하는 겔형의 고체 전해질.
- 제3항에서,상기 산은 화학식 1의 실란 화합물 전체에 대하여 1 내지 50 부피부의 범위로 사용되는 것을 특징으로 하는 겔형의 고체 전해질.
- 제1항에서,상기 이온성 액체는 양이온으로 이미다졸륨(imidazolium), 암모늄(ammonium), 피롤리디늄(pyrrolidinium) 및 피페리디늄(piperidinium)로 이루어지는 군에서 선택된 1종 이상을 포함하고, 음이온으로 비스(플루오로설포닐)이미드(bis(fluorosulfonyl)imide), 비스(플루오로설포닐)아미드(bis(fluorosufonyl)amide), 플루오로보레이트(fluoroborate) 및 플루오로포스페이트(fluorophosphate)로 이루어지는 군에서 선택된 1종 이상을 포함하는 것을 특징으로 하는 겔형의 고체 전해질.
- 제1항에서,상기 이온성 액체는 다공성 금속산화물 100 중량부에 대하여, 100 내지 200 중량부의 범위로 포함되는 것을 특징으로 하는 겔형의 고체 전해질.
- 제1항에서,상기 고체 전해질은 LiPF6, LiBF4, LiAsF6, LiSbF6, LiCF3SO3, LiC2F5SO3, LiC4F9SO3, LiN(CF3SO2)2, LiN(C2F5SO2)2, LiC(CF3SO2)3, 및 LiPF2{(COO)2}2으로 이루어지는 그룹에서 선택되는 1종 이상의 리튬염을 추가로 포함하는 것을 특징으로 하는 겔형의 고체 전해질.
- 제8항에서,상기 리튬염은 고체 전해질 전체에 대하여 5 내지 40 중량%로 포함되는 것을 특징으로 하는 겔형의 고체 전해질.
- 제1항 내지 제9항 중 어느 한 항의 고체 전해질을 포함하는 것을 특징으로 하는 리튬이차전지.
- 제1항 내지 제9항 중 어느 한 항의 고체 전해질을 포함하는 전기 이중층 캐패시터.
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