JP2023546706A - リチウム二次電池用正極、この製造方法及びこれを含むリチウム二次電池 - Google Patents
リチウム二次電池用正極、この製造方法及びこれを含むリチウム二次電池 Download PDFInfo
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- JP2023546706A JP2023546706A JP2023524812A JP2023524812A JP2023546706A JP 2023546706 A JP2023546706 A JP 2023546706A JP 2023524812 A JP2023524812 A JP 2023524812A JP 2023524812 A JP2023524812 A JP 2023524812A JP 2023546706 A JP2023546706 A JP 2023546706A
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- secondary battery
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- 229910052788 barium Inorganic materials 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- IWOUKMZUPDVPGQ-UHFFFAOYSA-N barium nitrate Chemical compound [Ba+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O IWOUKMZUPDVPGQ-UHFFFAOYSA-N 0.000 description 1
- 229910052790 beryllium Inorganic materials 0.000 description 1
- ATBAMAFKBVZNFJ-UHFFFAOYSA-N beryllium atom Chemical compound [Be] ATBAMAFKBVZNFJ-UHFFFAOYSA-N 0.000 description 1
- QQHZPQUHCAKSOL-UHFFFAOYSA-N butyl nitrate Chemical compound CCCCO[N+]([O-])=O QQHZPQUHCAKSOL-UHFFFAOYSA-N 0.000 description 1
- 229920005549 butyl rubber Polymers 0.000 description 1
- 229910052792 caesium Inorganic materials 0.000 description 1
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 150000001721 carbon Chemical class 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002301 cellulose acetate Polymers 0.000 description 1
- 229920006217 cellulose acetate butyrate Polymers 0.000 description 1
- AJAFRMGZWFDZAS-UHFFFAOYSA-M cesium;nitrite Chemical compound [Cs+].[O-]N=O AJAFRMGZWFDZAS-UHFFFAOYSA-M 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000007607 die coating method Methods 0.000 description 1
- 238000003618 dip coating Methods 0.000 description 1
- NJLLQSBAHIKGKF-UHFFFAOYSA-N dipotassium dioxido(oxo)titanium Chemical compound [K+].[K+].[O-][Ti]([O-])=O NJLLQSBAHIKGKF-UHFFFAOYSA-N 0.000 description 1
- VUPKGFBOKBGHFZ-UHFFFAOYSA-N dipropyl carbonate Chemical compound CCCOC(=O)OCCC VUPKGFBOKBGHFZ-UHFFFAOYSA-N 0.000 description 1
- 238000007606 doctor blade method Methods 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 238000006056 electrooxidation reaction Methods 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
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- IDNUEBSJWINEMI-UHFFFAOYSA-N ethyl nitrate Chemical compound CCO[N+]([O-])=O IDNUEBSJWINEMI-UHFFFAOYSA-N 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 229910052730 francium Inorganic materials 0.000 description 1
- KLMCZVJOEAUDNE-UHFFFAOYSA-N francium atom Chemical compound [Fr] KLMCZVJOEAUDNE-UHFFFAOYSA-N 0.000 description 1
- 229910003472 fullerene Inorganic materials 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 238000007756 gravure coating Methods 0.000 description 1
- NDEMNVPZDAFUKN-UHFFFAOYSA-N guanidine;nitric acid Chemical compound NC(N)=N.O[N+]([O-])=O.O[N+]([O-])=O NDEMNVPZDAFUKN-UHFFFAOYSA-N 0.000 description 1
- 239000001863 hydroxypropyl cellulose Substances 0.000 description 1
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- 150000003949 imides Chemical class 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 229920000126 latex Polymers 0.000 description 1
- 239000004816 latex Substances 0.000 description 1
- 229910001547 lithium hexafluoroantimonate(V) Inorganic materials 0.000 description 1
- 229910001540 lithium hexafluoroarsenate(V) Inorganic materials 0.000 description 1
- IDNHOWMYUQKKTI-UHFFFAOYSA-M lithium nitrite Chemical compound [Li+].[O-]N=O IDNHOWMYUQKKTI-UHFFFAOYSA-M 0.000 description 1
- FUJCRWPEOMXPAD-UHFFFAOYSA-N lithium oxide Chemical compound [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 description 1
- 229910001947 lithium oxide Inorganic materials 0.000 description 1
- MHCFAGZWMAWTNR-UHFFFAOYSA-M lithium perchlorate Chemical compound [Li+].[O-]Cl(=O)(=O)=O MHCFAGZWMAWTNR-UHFFFAOYSA-M 0.000 description 1
- 229910001486 lithium perchlorate Inorganic materials 0.000 description 1
- GLNWILHOFOBOFD-UHFFFAOYSA-N lithium sulfide Chemical compound [Li+].[Li+].[S-2] GLNWILHOFOBOFD-UHFFFAOYSA-N 0.000 description 1
- 229910001537 lithium tetrachloroaluminate Inorganic materials 0.000 description 1
- 229910001496 lithium tetrafluoroborate Inorganic materials 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- YQCIWBXEVYWRCW-UHFFFAOYSA-N methane;sulfane Chemical compound C.S YQCIWBXEVYWRCW-UHFFFAOYSA-N 0.000 description 1
- LRMHVVPPGGOAJQ-UHFFFAOYSA-N methyl nitrate Chemical compound CO[N+]([O-])=O LRMHVVPPGGOAJQ-UHFFFAOYSA-N 0.000 description 1
- KKQAVHGECIBFRQ-UHFFFAOYSA-N methyl propyl carbonate Chemical compound CCCOC(=O)OC KKQAVHGECIBFRQ-UHFFFAOYSA-N 0.000 description 1
- 239000002121 nanofiber Substances 0.000 description 1
- 150000002826 nitrites Chemical class 0.000 description 1
- 150000002828 nitro derivatives Chemical class 0.000 description 1
- LYGJENNIWJXYER-UHFFFAOYSA-N nitromethane Chemical compound C[N+]([O-])=O LYGJENNIWJXYER-UHFFFAOYSA-N 0.000 description 1
- VLZLOWPYUQHHCG-UHFFFAOYSA-N nitromethylbenzene Chemical compound [O-][N+](=O)CC1=CC=CC=C1 VLZLOWPYUQHHCG-UHFFFAOYSA-N 0.000 description 1
- 239000000615 nonconductor Substances 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- TXQBMQNFXYOIPT-UHFFFAOYSA-N octyl nitrate Chemical compound CCCCCCCCO[N+]([O-])=O TXQBMQNFXYOIPT-UHFFFAOYSA-N 0.000 description 1
- 150000002898 organic sulfur compounds Chemical class 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 229920002755 poly(epichlorohydrin) Polymers 0.000 description 1
- 229920003207 poly(ethylene-2,6-naphthalate) Polymers 0.000 description 1
- 229920000927 poly(p-phenylene benzobisoxazole) Polymers 0.000 description 1
- 229920001197 polyacetylene Polymers 0.000 description 1
- 229920002401 polyacrylamide Polymers 0.000 description 1
- 229920000767 polyaniline Polymers 0.000 description 1
- 229920001230 polyarylate Polymers 0.000 description 1
- 229920002857 polybutadiene Polymers 0.000 description 1
- 229920001707 polybutylene terephthalate Polymers 0.000 description 1
- 229920005646 polycarboxylate Polymers 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 239000011112 polyethylene naphthalate Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920000193 polymethacrylate Polymers 0.000 description 1
- 229920006380 polyphenylene oxide Polymers 0.000 description 1
- 229920000069 polyphenylene sulfide Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920000128 polypyrrole Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 229920001021 polysulfide Polymers 0.000 description 1
- 239000005077 polysulfide Substances 0.000 description 1
- 150000008117 polysulfides Polymers 0.000 description 1
- 229920000123 polythiophene Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 229920002689 polyvinyl acetate Polymers 0.000 description 1
- 239000011118 polyvinyl acetate Substances 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 229920002717 polyvinylpyridine Polymers 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 235000010289 potassium nitrite Nutrition 0.000 description 1
- 239000004304 potassium nitrite Substances 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- JNTOKFNBDFMTIV-UHFFFAOYSA-N propyl nitrate Chemical compound CCCO[N+]([O-])=O JNTOKFNBDFMTIV-UHFFFAOYSA-N 0.000 description 1
- XLABPPWWFVQMBZ-UHFFFAOYSA-O pyridin-1-ium;nitrate Chemical compound [O-][N+]([O-])=O.C1=CC=[NH+]C=C1 XLABPPWWFVQMBZ-UHFFFAOYSA-O 0.000 description 1
- 229910052705 radium Inorganic materials 0.000 description 1
- HCWPIIXVSYCSAN-UHFFFAOYSA-N radium atom Chemical compound [Ra] HCWPIIXVSYCSAN-UHFFFAOYSA-N 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007763 reverse roll coating Methods 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 229910052701 rubidium Inorganic materials 0.000 description 1
- IGLNJRXAVVLDKE-UHFFFAOYSA-N rubidium atom Chemical compound [Rb] IGLNJRXAVVLDKE-UHFFFAOYSA-N 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000002109 single walled nanotube Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical compound O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 0.000 description 1
- 125000000472 sulfonyl group Chemical group *S(*)(=O)=O 0.000 description 1
- 125000005463 sulfonylimide group Chemical group 0.000 description 1
- 150000003464 sulfur compounds Chemical class 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
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Abstract
Description
前記正極集電体の一面に形成された湿式正極活物質層;及び
前記湿式正極活物質層の上に形成された乾式正極活物質層;を含み、
前記湿式正極活物質層は、硫黄‐炭素複合体、バインダー及び導電材を含み、
前記乾式正極活物質層は、炭素含有硫黄溶融物で構成されたものである、リチウム二次電池用正極を提供する。
(2)前記湿式正極活物質層の一面にフリースタンディングフィルム型正極材である乾式正極活物質層を附着する段階;を含むリチウム二次電池用正極の製造方法を提供する。
本発明は湿式正極活物質層及び乾式正極活物質層を含むリチウム二次電池用正極に係り、前記リチウム二次電池用正極は、正極集電体;前記正極集電体の一面に形成された湿式正極活物質層;及び前記湿式正極活物質層の上に形成された乾式正極活物質層;を含み、前記湿式正極活物質層は、硫黄‐炭素複合体、バインダー及び導電材を含み、前記乾式正極活物質層は炭素含有硫黄溶融物で構成されたものである。
本発明は、また、リチウム二次電池用正極の製造方法に係り、前記リチウム二次電池用正極の製造方法は、(1)硫黄‐炭素複合体、バインダー及び導電材を含む正極スラリーを正極集電体に一面に塗布し、湿式正極活物質層を形成する段階;及び(2)前記湿式正極活物質層の一面にフリースタンディングフィルム型正極材である乾式正極活物質層を附着する段階;を含むものである。
また、本発明は前記リチウム二次電池用正極を含むリチウム二次電池を提供する。
硫黄(S)と炭素ナノチューブ(CNT)を固体状態で65:35の重量比で均一に混合し、100rpmの条件で1時間ボールミーリングして混合物を製造した。
(1)正極製造
前記製造例1で得た硫黄‐炭素複合体(S‐CNT)、導電材及びバインダーを90:5:5の重量比で混合してスラリーを製造した後、20μm厚さのアルミニウム集電体上にコーティング後、乾燥及び圧延して湿式正極活物質層を形成した。この時、前記導電材は比表面積300m2で、粒子の大きさ20μmであるCNTを使用し、前記バインダーはスチレン‐ブタジエンゴム(styrene butadiene rubber;SBR)を使用した。
前記製造された正極と厚さ150μmのリチウム金属を負極で準備した。
乾式正極活物質層を形成せず、湿式正極活物質層のみを形成したことを除いて、実施例1と同様の方法で正極及びリチウム‐硫黄二次電池を製造した。
湿式正極活物質層を形成せず、乾式正極活物質層をアルミニウム集電体の一面に形成したことを除いて実施例1と同様の方法で正極及びリチウム‐硫黄二次電池を製造した。この時、前記アルミニウム集電体上にバインダーである SBR(Styrene Butadiene Rubber)塗布した後、前記乾式正極活物質層を接着させた。
バインダーを使わないことを除いて、比較例2と同様に実施して、アルミニウム集電体上に乾式活物質層を接着させた。
前記実施例及び比較例で製造されたポーチセル形態のリチウム二次電池に対し、下のような方法で、容量、公称電圧、水分含量及び寿命特性を測定したし、その結果を下記切符1に記載した。
25℃で、0.1C充電/0.1C放電2.5サイクル後、0.2C充電/0.2C放電3サイクル後、0.2C充電/0.3C放電条件にして、25℃及び45℃の温度で容量を測定した。
公称電圧とは、電力系統で与えられた電圧系統を呼ぶための呼称電圧値であって、一般的に起電力よりやや低い値を持ち、通常放電曲線の中心値(mean value of discharge voltage)を意味する。
水分測定機器(Metrohm 901KF Tirando)を利用して水分含量を測定した。
容量保存率が初期容量の80%になる地点を寿命の最終サイクルにした。
20:湿式正極活物質層
30:乾式正極活物質層
Claims (14)
- 正極集電体;
前記正極集電体の一面に形成された湿式正極活物質層;及び
前記湿式正極活物質層上に形成された乾式正極活物質層;を含み、
前記湿式正極活物質層は、硫黄‐炭素複合体、バインダー及び導電材を含み、
前記乾式正極活物質層は硫黄溶融物内に多孔性炭素材が分散された、炭素含有硫黄溶融物で構成されたものである、リチウム二次電池用正極。 - 前記湿式正極活物質層は、硫黄‐炭素複合体40重量%ないし80重量%、バインダー1重量%ないし30重量%、及び導電材0.5重量%ないし30重量%を含むものである、請求項1に記載のリチウム二次電池用正極。
- 前記湿式正極活物質層のローディング量は0.1mAh/cm2ないし0.5mAh/cm2、前記湿式正極活物質層のローディング量は前記乾式正極活物質層のローディング量の2%ないし20%である、請求項1に記載のリチウム二次電池用正極。
- 前記湿式正極活物質層の気孔率は30%ないし90%である、請求項1に記載のリチウム二次電池用正極。
- 前記湿式正極活物質層の密度は0.2g/cm3ないし1.4g/cm3である、請求項1に記載のリチウム二次電池用正極。
- 前記乾式正極活物質層の気孔率は68%以下である、請求項1に記載のリチウム二次電池用正極。
- 前記乾式正極活物質層は内部接着力が10gf/cm以上である、請求項1に記載のリチウム二次電池用正極。
- (1)硫黄‐炭素複合体、バインダー及び導電材を含む正極スラリーを正極集電体の一面に塗布し、湿式正極活物質層を形成する段階;及び
(2)前記湿式正極活物質層の一面にフリースタンディングフィルム型正極材である乾式正極活物質層を附着する段階;を含む、リチウム二次電池用正極の製造方法。 - 前記フリースタンディングフィルム型正極材である乾式正極活物質層は、
(a)硫黄と多孔性炭素材を混合する段階;
(b)前記(a)段階で形成された混合物を熱処理する段階;及び
前記(b)段階で形成された硫黄‐炭素複合体を容器に充填させた後、加圧して炭素含有硫黄溶融物を形成する段階;を含む工程によって製造される、請求項8に記載のリチウム二次電池用正極の製造方法。 - 前記熱処理は130℃ないし170℃の温度条件下で遂行される、請求項9に記載のリチウム二次電池用正極の製造方法。
- 前記加圧は0.8MPaないし15MPaの圧力条件下で遂行される、請求項9に記載のリチウム二次電池用正極の製造方法。
- 請求項1に記載のリチウム二次電池用正極;
リチウム金属またはリチウム合金を含む負極;
前記正極と負極の間に位置する分離膜;及び
前記正極、負極及び分離膜が含浸された電解質を含むリチウム二次電池。 - 前記リチウム二次電池はリチウム‐硫黄二次電池である、請求項12に記載のリチウム二次電池。
- 前記正極は硫黄のローディング量が3.0mAh/cm2ないし5.0mAh/cm2である、請求項12に記載のリチウム二次電池。
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