JP2022548332A - 電気化学デバイス用電解質配合物 - Google Patents
電気化学デバイス用電解質配合物 Download PDFInfo
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- tetrafluoroborate
- difluoromethane
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- 239000003792 electrolyte Substances 0.000 title claims abstract description 38
- 239000000203 mixture Substances 0.000 title claims description 20
- 238000009472 formulation Methods 0.000 title description 8
- 239000002904 solvent Substances 0.000 claims abstract description 44
- 150000003839 salts Chemical class 0.000 claims abstract description 38
- 239000003990 capacitor Substances 0.000 claims abstract description 27
- RWRIWBAIICGTTQ-UHFFFAOYSA-N difluoromethane Chemical compound FCF RWRIWBAIICGTTQ-UHFFFAOYSA-N 0.000 claims description 90
- -1 fluoroethylene, difluoroethylene Chemical group 0.000 claims description 36
- NBVXSUQYWXRMNV-UHFFFAOYSA-N monofluoromethane Natural products FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 claims description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 12
- NPNPZTNLOVBDOC-UHFFFAOYSA-N 1,1-difluoroethane Chemical compound CC(F)F NPNPZTNLOVBDOC-UHFFFAOYSA-N 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 6
- 239000006229 carbon black Substances 0.000 claims description 2
- 239000002041 carbon nanotube Substances 0.000 claims description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 2
- 239000003575 carbonaceous material Substances 0.000 claims description 2
- 229910021389 graphene Inorganic materials 0.000 claims description 2
- 229910002804 graphite Inorganic materials 0.000 claims description 2
- 239000010439 graphite Substances 0.000 claims description 2
- XPDWGBQVDMORPB-UHFFFAOYSA-N Fluoroform Chemical compound FC(F)F XPDWGBQVDMORPB-UHFFFAOYSA-N 0.000 claims 2
- LVGUZGTVOIAKKC-UHFFFAOYSA-N 1,1,1,2-tetrafluoroethane Chemical compound FCC(F)(F)F LVGUZGTVOIAKKC-UHFFFAOYSA-N 0.000 claims 1
- UJPMYEOUBPIPHQ-UHFFFAOYSA-N 1,1,1-trifluoroethane Chemical compound CC(F)(F)F UJPMYEOUBPIPHQ-UHFFFAOYSA-N 0.000 claims 1
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 claims 1
- HRYZWHHZPQKTII-UHFFFAOYSA-N chloroethane Chemical compound CCCl HRYZWHHZPQKTII-UHFFFAOYSA-N 0.000 claims 1
- 229960003750 ethyl chloride Drugs 0.000 claims 1
- UHCBBWUQDAVSMS-UHFFFAOYSA-N fluoroethane Chemical compound CCF UHCBBWUQDAVSMS-UHFFFAOYSA-N 0.000 claims 1
- NBVXSUQYWXRMNV-OUBTZVSYSA-N fluoromethane Chemical group F[13CH3] NBVXSUQYWXRMNV-OUBTZVSYSA-N 0.000 claims 1
- 150000008282 halocarbons Chemical class 0.000 claims 1
- GTLACDSXYULKMZ-UHFFFAOYSA-N pentafluoroethane Chemical compound FC(F)C(F)(F)F GTLACDSXYULKMZ-UHFFFAOYSA-N 0.000 claims 1
- 229920006395 saturated elastomer Polymers 0.000 claims 1
- 239000007787 solid Substances 0.000 claims 1
- 239000007789 gas Substances 0.000 description 38
- 235000002639 sodium chloride Nutrition 0.000 description 38
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 12
- 238000012360 testing method Methods 0.000 description 11
- 238000000034 method Methods 0.000 description 9
- 150000001768 cations Chemical class 0.000 description 5
- AFVFQIVMOAPDHO-UHFFFAOYSA-N Methanesulfonic acid Chemical compound CS(O)(=O)=O AFVFQIVMOAPDHO-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000012983 electrochemical energy storage Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 2
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 150000001450 anions Chemical class 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- UCQFCFPECQILOL-UHFFFAOYSA-N diethyl hydrogen phosphate Chemical compound CCOP(O)(=O)OCC UCQFCFPECQILOL-UHFFFAOYSA-N 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-M hydrogensulfate Chemical compound OS([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-M 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- YACKEPLHDIMKIO-UHFFFAOYSA-N methylphosphonic acid Chemical compound CP(O)(O)=O YACKEPLHDIMKIO-UHFFFAOYSA-N 0.000 description 2
- 239000012046 mixed solvent Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- KTQDYGVEEFGIIL-UHFFFAOYSA-N n-fluorosulfonylsulfamoyl fluoride Chemical compound FS(=O)(=O)NS(F)(=O)=O KTQDYGVEEFGIIL-UHFFFAOYSA-N 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
- PWZSCBSKFVJMJH-UHFFFAOYSA-N 1,1-diethylpyrrolidin-1-ium Chemical compound CC[N+]1(CC)CCCC1 PWZSCBSKFVJMJH-UHFFFAOYSA-N 0.000 description 1
- GARJMFRQLMUUDD-UHFFFAOYSA-N 1,1-dimethylpyrrolidin-1-ium Chemical compound C[N+]1(C)CCCC1 GARJMFRQLMUUDD-UHFFFAOYSA-N 0.000 description 1
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 description 1
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 206010011878 Deafness Diseases 0.000 description 1
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 239000002033 PVDF binder Substances 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 101150071882 US17 gene Proteins 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- RPXKKUZDTAOVEQ-UHFFFAOYSA-N boric acid;oxalic acid Chemical compound OB(O)O.OC(=O)C(O)=O.OC(=O)C(O)=O RPXKKUZDTAOVEQ-UHFFFAOYSA-N 0.000 description 1
- 229920006184 cellulose methylcellulose Polymers 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 229940021013 electrolyte solution Drugs 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- KVURXUSSSJWASD-UHFFFAOYSA-N fluoro(dioxido)borane tetrabutylazanium Chemical compound [O-]B([O-])F.[O-]B([O-])F.[O-]B([O-])F.[O-]B([O-])F.[O-]B([O-])F.[O-]B([O-])F.CCCC[N+](CCCC)(CCCC)CCCC.CCCC[N+](CCCC)(CCCC)CCCC.CCCC[N+](CCCC)(CCCC)CCCC.CCCC[N+](CCCC)(CCCC)CCCC.CCCC[N+](CCCC)(CCCC)CCCC.CCCC[N+](CCCC)(CCCC)CCCC.CCCC[N+](CCCC)(CCCC)CCCC.CCCC[N+](CCCC)(CCCC)CCCC.CCCC[N+](CCCC)(CCCC)CCCC.CCCC[N+](CCCC)(CCCC)CCCC.CCCC[N+](CCCC)(CCCC)CCCC.CCCC[N+](CCCC)(CCCC)CCCC KVURXUSSSJWASD-UHFFFAOYSA-N 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 150000003949 imides Chemical class 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229940098779 methanesulfonic acid Drugs 0.000 description 1
- 229910052759 nickel Inorganic materials 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
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- PNGLEYLFMHGIQO-UHFFFAOYSA-M sodium;3-(n-ethyl-3-methoxyanilino)-2-hydroxypropane-1-sulfonate;dihydrate Chemical compound O.O.[Na+].[O-]S(=O)(=O)CC(O)CN(CC)C1=CC=CC(OC)=C1 PNGLEYLFMHGIQO-UHFFFAOYSA-M 0.000 description 1
- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
- DZLFLBLQUQXARW-UHFFFAOYSA-N tetrabutylammonium Chemical compound CCCC[N+](CCCC)(CCCC)CCCC DZLFLBLQUQXARW-UHFFFAOYSA-N 0.000 description 1
- CBXCPBUEXACCNR-UHFFFAOYSA-N tetraethylammonium Chemical compound CC[N+](CC)(CC)CC CBXCPBUEXACCNR-UHFFFAOYSA-N 0.000 description 1
- QEMXHQIAXOOASZ-UHFFFAOYSA-N tetramethylammonium Chemical compound C[N+](C)(C)C QEMXHQIAXOOASZ-UHFFFAOYSA-N 0.000 description 1
- OSBSFAARYOCBHB-UHFFFAOYSA-N tetrapropylammonium Chemical compound CCC[N+](CCC)(CCC)CCC OSBSFAARYOCBHB-UHFFFAOYSA-N 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- SEACXNRNJAXIBM-UHFFFAOYSA-N triethyl(methyl)azanium Chemical compound CC[N+](C)(CC)CC SEACXNRNJAXIBM-UHFFFAOYSA-N 0.000 description 1
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- H01M10/00—Secondary cells; Manufacture thereof
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- 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
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Abstract
Description
本出願は、2019年9月30日に出願された米国仮特許出願第62/908515号、2019年10月7日に出願された米国仮特許出願第62/911505号、および2019年10月7日に出願された米国仮特許出願第62/911508号に対する優先権を主張するものであり、これらの出願のそれぞれは、参照によりその全体が組み込まれる。
図2は、ジフルオロメタン中の1.0M SBPBF4から構成される電気化学デバイスについての様々な温度での放電曲線を示す。
図3は、種々の温度におけるジフルオロメタン中の1.0M SBPBF4から構成される電気化学デバイスについてのキャパシタンス対放電速度を示す。
図4は、ジフルオロメタン中の1.0M SBPBF4から構成され、+85℃で1500時間2.7Vに保持された電気化学デバイスの静電容量対時間を示す。
図5は、+85℃で1500時間、2.7Vに保持された、ジフルオロメタン中の1.0M SBPBF4から構成される電気化学デバイスのDCR抵抗対時間を示す。
図6は、種々の温度におけるジフルオロメタン中の1.0M TBABF4から構成される電気化学デバイスについての静電容量対放電速度を示す。
図7は、種々の温度におけるジフルオロメタン中の0.3M TEABF4および0.7M TBABF4から構成される電気化学デバイスについての静電容量対放電速度を示す。
図8は、+20℃でジフルオロメタン中0.3M TEABF4から構成された電気化学デバイスの静電容量対放電速度を示す。
電気化学キャパシタデバイスを、ジフルオロメタン(DFM)中の1.0M SBPBF4からなる液化ガス電解液を用いて試験した。デバイスを3.0Vに60分間充電し、様々な温度で5Aの速度で放電した。+85℃から-55℃まで良好に機能し、その温度範囲にわたってキャパシタンスまたはインピーダンスの変化はほとんどなかった。78℃の低温では、若干の容量低下を示したが、それでも、最新の電気化学キャパシタと比較すると、低温で優れた性能を示した。最も驚くべきことは、キャパシタが3.0Vおよび+85℃で短時間良好に機能する能力であり、この予想外の性能は、3.0Vおよび+85℃で数分または数時間保持した場合でさえ急速な劣化を示す最新技術のキャパシタの性能よりも優れている。これは、短期間の高温が予想される領域に適用される。性能測定基準を以下の表1に記載し、放電曲線を図2に示す。
電気化学キャパシタデバイスを、ジフルオロメタン(DFM)中の1.0M SBPBF4からなる液化ガス電解液を用いて試験した。デバイスを、-60℃、+20℃、および+85℃において40Ampまでの様々な放電速度で試験した。各温度で試験した電流に対しての感知できる変化はなく、各温度での高性能を示すことがわかった。各温度でのキャパシタンス対温度データを図3にプロットする。
電気化学キャパシタデバイスを、ジフルオロメタン(DFM)中の1.0M SBPBF4からなる液化ガス電解液を用いて試験した。デバイスを2.7V及び+85℃で加速寿命試験した。デバイスを試験期間中この温度で保持し、100時間間隔で放電させてキャパシタンスをチェックし、その直後に2.7Vに充電し戻した。キャパシタンス及びDCR対時間データをそれぞれ図4及び5に示す。一般に、セルは、この「直流寿命」試験に合格し、1500時間の試験で静電容量が7%低下し、DCR(抵抗値)が26%上昇した。一般に、この「直流寿命」試験では、静電容量が20%未満、DCRが50%未満の低下で合格となる。この驚くべき結果は、SBPBF4塩及びジフルオロメタン液化ガス溶媒系の優れた安定性を示す。以前には、別の電解液が、1500時間にわたって+85℃で2.7Vの性能のこの組み合わせを示したことは決してない。他の溶媒(例えば、アセトニトリル)中で使用される同じ塩が、ジフルオロメタンなどの新しい液化ガス溶媒中で非常に良好に機能することは、当業者には明らかではない。この性能を示すためには実験試験が必要であり、本明細書で初めて開示され、塩と溶媒とのこの独特の組み合わせがデバイスの性能を著しく向上させることが示される。
比較試験として、ジフルオロメタン(DFM)中の1.0M TBABF4からなる液化ガス電解液を用いて電気化学キャパシタデバイスを試験した。デバイスは、-60及び+20℃で40Aまでの様々な放電速度で試験した。20℃では5Aから40Aへの放電で容量が6%低下するが、低温では容量が大幅に低下する。各温度での容量対放電電流を図6に示す。セルは、-60℃の温度で高いDCRで非常に不十分に機能した。これは、良好な低温性能に必要とされるのは液化ガス溶媒ジフルオロメタンでも塩の良好な溶解性でもなく、開示されたSBPBF4塩及びジフルオロメタン溶媒の場合のように、塩及び溶媒の正しい組み合わせでもあることを示す。さらに、図3に示した性能と比較すると、SBPBF4塩の静電容量とTBABF4塩の静電容量とでは、SBPBF4塩の方が高くなっている。これは、小さいサイズのカチオンが、炭素電極上のより多くのナノ細孔にアクセスすることができ、デバイスキャパシタンスを増加させるためである。これらの異なる測定基準は、実際の電池性能を決定するために実験が行われない限り、明白ではないであろう。
比較試験として、ジフルオロメタン(DFM)中の0.3TEABF4および0.7M TBABF4からなる液化ガス電解質を用いて電気化学キャパシタデバイスを試験した。このデバイスは、-60℃と+20℃において、最大40Aまでのさまざまな放電速度でテストされた。+20℃での5Aから40Aへの放電では容量の低下はほとんどないか全くないが、より低い温度では容量の大幅な低下がある。各温度での容量対放電電流を図7に示す。+85℃の温度で高いDCRを有する電池の性能は非常に悪かった。
比較試験として、液化ガスを用いて電気化学キャパシタ装置を試験した。電解質ジフルオロメタン(DFM)中に0.3TEABF4を含む。デバイスを、+20℃で40Aまでの様々な放電速度で試験した。放電電流のレベルが増加すると、キャパシタンスが著しく低下する。キャパシタンス対放電電流を図8に示す。電池は、-60℃及び+85℃の極端な温度で高いDCRで非常に不十分に機能した。
比較試験として、DFM中の1.0M SBPBF4、DFM中の1.0M TBABF4、DFM中の0.3TEABF4+0.7M TBABF4、及びジフルオロメタン(DFM)中の0.3M TEABF4から構成される液化ガス電解液を用いて、いくつかの電気化学キャパシタデバイスを試験した。各セルについて、DCR抵抗を測定し、その結果を下記表2に示す。明らかに、DFM中にSBPBF4塩を有するセルは、+20℃および-60℃の両方で試験したセルの最も低い耐性を有した。
Claims (2)
- 電気化学キャパシタであって、
圧縮ガス溶媒と、1つ以上の固体または液体の塩との混合物を含むイオン伝導性電解質であって、前記圧縮ガス溶媒が、293.15Kの室温で100kPa超の蒸気圧を有する少なくとも第1の成分を含み、前記第1の成分が、フルオロメタン、ジフルオロメタン、1,1-ジフルオロエタン、トリフルオロメタン、フルオロエタン、、トリフルオロエタン、テトラフルオロエタン、ペンタフルオロエタン、フルオロエチレン、ジフルオロエチレン、トリフルオロエチレン、テトラフルオロエチレン、クロロメタン、クロロエタン、クロロエテン、飽和ハロゲン化炭化水素、及び、不飽和ハロゲン化炭化水素、ならびにそれらの異性体からなる群から選択され、
1つ以上の塩がスピロ-(1,1´)-ビピロリジニウムテトラフルオロボレート、ジメチルピロリジニウムテトラフルオロボレートからなる群から選択される。エチルメチルピロリジニウムテトラフルオロボレート、ジエチルピロリジニウムテトラフルオロボレート、ジプロピルピロリジニウムテトラフルオロボレート、およびジブチルピロリジニウムテトラフルオロボレート、ならびにこれらの異性体および組み合わせであり、
293.15Kの室温で100kPaより高い圧力に圧縮ガス溶媒を維持する加圧条件下でイオン伝導性電解質を封入するハウジングと、
前記イオン伝導性電解質と接触する少なくとも2つの伝導性電極と、
を含むことを特徴とする電気化学キャパシタ。 - 一方または両方の電極が、活性炭、グラファイト、カーボンブラック、グラフェン、およびカーボンナノチューブからなる群から選択される炭素材料から構成される、請求項1に記載の電気化学キャパシタ。
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