JP6337777B2 - セパレータ、電極素子、蓄電デバイスおよび前記セパレータの製造方法 - Google Patents
セパレータ、電極素子、蓄電デバイスおよび前記セパレータの製造方法 Download PDFInfo
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- JP6337777B2 JP6337777B2 JP2014551936A JP2014551936A JP6337777B2 JP 6337777 B2 JP6337777 B2 JP 6337777B2 JP 2014551936 A JP2014551936 A JP 2014551936A JP 2014551936 A JP2014551936 A JP 2014551936A JP 6337777 B2 JP6337777 B2 JP 6337777B2
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- QHGJSLXSVXVKHZ-UHFFFAOYSA-N dilithium;dioxido(dioxo)manganese Chemical compound [Li+].[Li+].[O-][Mn]([O-])(=O)=O QHGJSLXSVXVKHZ-UHFFFAOYSA-N 0.000 description 1
- YNQRWVCLAIUHHI-UHFFFAOYSA-L dilithium;oxalate Chemical compound [Li+].[Li+].[O-]C(=O)C([O-])=O YNQRWVCLAIUHHI-UHFFFAOYSA-L 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
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- KLKFAASOGCDTDT-UHFFFAOYSA-N ethoxymethoxyethane Chemical compound CCOCOCC KLKFAASOGCDTDT-UHFFFAOYSA-N 0.000 description 1
- 229940093499 ethyl acetate Drugs 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 125000001153 fluoro group Chemical group F* 0.000 description 1
- WBJINCZRORDGAQ-UHFFFAOYSA-N formic acid ethyl ester Natural products CCOC=O WBJINCZRORDGAQ-UHFFFAOYSA-N 0.000 description 1
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- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
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- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 229910003437 indium oxide Inorganic materials 0.000 description 1
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 1
- 239000010954 inorganic particle Substances 0.000 description 1
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- 229910052742 iron Inorganic materials 0.000 description 1
- WDAXFOBOLVPGLV-UHFFFAOYSA-N isobutyric acid ethyl ester Natural products CCOC(=O)C(C)C WDAXFOBOLVPGLV-UHFFFAOYSA-N 0.000 description 1
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- JMMWKPVZQRWMSS-UHFFFAOYSA-N isopropanol acetate Natural products CC(C)OC(C)=O JMMWKPVZQRWMSS-UHFFFAOYSA-N 0.000 description 1
- 229940011051 isopropyl acetate Drugs 0.000 description 1
- GWYFCOCPABKNJV-UHFFFAOYSA-N isovaleric acid Chemical compound CC(C)CC(O)=O GWYFCOCPABKNJV-UHFFFAOYSA-N 0.000 description 1
- 150000002596 lactones Chemical class 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 150000002642 lithium compounds Chemical class 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
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 1
- CUONGYYJJVDODC-UHFFFAOYSA-N malononitrile Chemical compound N#CCC#N CUONGYYJJVDODC-UHFFFAOYSA-N 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- CSSYKHYGURSRAZ-UHFFFAOYSA-N methyl 2,2-difluoroacetate Chemical compound COC(=O)C(F)F CSSYKHYGURSRAZ-UHFFFAOYSA-N 0.000 description 1
- CXHHBNMLPJOKQD-UHFFFAOYSA-M methyl carbonate Chemical compound COC([O-])=O CXHHBNMLPJOKQD-UHFFFAOYSA-M 0.000 description 1
- ANGDWNBGPBMQHW-UHFFFAOYSA-N methyl cyanoacetate Chemical compound COC(=O)CC#N ANGDWNBGPBMQHW-UHFFFAOYSA-N 0.000 description 1
- 229940017219 methyl propionate Drugs 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- PYLWMHQQBFSUBP-UHFFFAOYSA-N monofluorobenzene Chemical compound FC1=CC=CC=C1 PYLWMHQQBFSUBP-UHFFFAOYSA-N 0.000 description 1
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- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 239000010450 olivine Substances 0.000 description 1
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- 239000011368 organic material Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 150000003014 phosphoric acid esters Chemical class 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
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- WYVAMUWZEOHJOQ-UHFFFAOYSA-N propionic anhydride Chemical compound CCC(=O)OC(=O)CC WYVAMUWZEOHJOQ-UHFFFAOYSA-N 0.000 description 1
- FVSKHRXBFJPNKK-UHFFFAOYSA-N propionitrile Chemical compound CCC#N FVSKHRXBFJPNKK-UHFFFAOYSA-N 0.000 description 1
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- APSBXTVYXVQYAB-UHFFFAOYSA-M sodium docusate Chemical compound [Na+].CCCCC(CC)COC(=O)CC(S([O-])(=O)=O)C(=O)OCC(CC)CCCC APSBXTVYXVQYAB-UHFFFAOYSA-M 0.000 description 1
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- 229910052717 sulfur Inorganic materials 0.000 description 1
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- DQWPFSLDHJDLRL-UHFFFAOYSA-N triethyl phosphate Chemical compound CCOP(=O)(OCC)OCC DQWPFSLDHJDLRL-UHFFFAOYSA-N 0.000 description 1
- WVLBCYQITXONBZ-UHFFFAOYSA-N trimethyl phosphate Chemical compound COP(=O)(OC)OC WVLBCYQITXONBZ-UHFFFAOYSA-N 0.000 description 1
- XZZNDPSIHUTMOC-UHFFFAOYSA-N triphenyl phosphate Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)(=O)OC1=CC=CC=C1 XZZNDPSIHUTMOC-UHFFFAOYSA-N 0.000 description 1
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- 239000011787 zinc oxide Substances 0.000 description 1
Images
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- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
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- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
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- H—ELECTRICITY
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- H—ELECTRICITY
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- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
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- H—ELECTRICITY
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H—ELECTRICITY
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- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/489—Separators, membranes, diaphragms or spacing elements inside the cells, characterised by their physical properties, e.g. swelling degree, hydrophilicity or shut down properties
- H01M50/497—Ionic conductivity
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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
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
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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
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Description
特許文献2:特許第4831937号公報
特許文献3:特開2004−269579号公報
特許文献4:特表2005−503652号公報
セパレータは、少なくとも無機材料を用いて形成された層を含む基材を有している。セパレータは、電解液とともに正極と負極の間に存在して、正極と負極との短絡を防止しつつ、イオン伝導性を有するように構成される。基材に含まれる無機材料からなる層は電気伝導性を有していないが、セパレータ自体はイオン伝導性を有している。また、セパレータは、電解液に侵されにくいことが好ましい。さらに、セパレータに必要な強度および形状保持性は、基材が担う。よって、基材に含まれる層は、セパレータが、イオン伝導性を有し、電解液に侵されにくく、かつ必要な強度および形状保持性を有するように構成されるようなものであれば、どのような無機材料を含んでいてもよい。基材が少なくとも無機材料で形成された層を有することで、セパレータとして必要な機械的強度を確保しつつ、加熱時の熱収縮がほとんど生じない、温度変化による寸法安定性に優れたセパレータを得ることができる。
(1)無機系または有機系のバインダ溶液に無機繊維を分散させたものを基材の表面に塗布し、バインダを固化する方法。
(2)熱可塑性樹脂をあらかじめ無機繊維の表面に付着させておき、熱可塑性樹脂を加熱溶融することによって、無機繊維同士を熱溶着する方法。
(3)無機繊維層に繊維状または粉末状の熱可塑性樹脂を添加し、熱可塑性樹脂を加熱溶融することによって無機繊維同士を熱溶着する方法。
(4)基材の表面に熱可塑性樹脂による接着層を形成し、その上に無機繊維層を形成した後、熱可塑性樹脂を加熱溶融することによって、基材と無機繊維層とを熱溶着する方法。
(5)溶融した熱可塑性樹脂を基材に浸透させ、熱可塑性樹脂が溶融した状態で基材の上に無機繊維を分散させ、熱可塑性樹脂を固化させる方法。
本発明は、上述した本発明によるセパレータと、セパレータを間において対向配置された正極および負極と、を有する電極素子に関する。また、本発明は、上記電極素子と、電解液と、これら電極素子および電解液を内包する外装体と、を有する蓄電デバイスに関する。
本実施形態のリチウム二次電池は、負極活物質を有する負極を備える。負極活物質は負極用結着材によって負極集電体上に結着されることができる。
正極は、例えば、正極活物質が正極用結着剤によって正極集電体を覆うように結着されてなる。
本実施形態で用いる電解液は、リチウム塩(支持塩)と、この支持塩を溶解する非水溶媒を含む非水電解液を用いることができる。
外装体としては、電解液に安定で、かつ十分な水蒸気バリア性を持つものであれば、適宜選択することができる。例えば、積層ラミネート型の二次電池の場合、外装体としては、アルミニウム、シリカをコーティングしたポリプロピレン、ポリエチレン等のラミネートフィルムを用いることができる。特に、体積膨張を抑制する観点から、アルミニウムラミネートフィルムを用いることが好ましい。また、外装体は、単一の部材で構成してもよいし、図1に示したように複数の部材(外装材21、22)を組み合わせて構成してもよい。
<電池の作製>
(正極作製方法)
正極活物質として、リチウムマンガン複合酸化物(LiMn2O4)材料を85質量%、導電助剤としてアセチレンブラックを7質量%、バインダとしてポリフッ化ビニリデン8質量%とを混合し、これをN−メチルピロリドン(NMP)に分散させてスラリーとした後、正極集電体としてのアルミニウム箔(15μm)に塗布し、乾燥させた。乾燥後、電極をプレス処理し、処理後の厚さが80μmになるように作製した。活物質塗布部分は幅100mm、長さ200mmとした。
負極活物質として、黒鉛材料を90質量%、バインダとしてポリフッ化ビニリデン10質量%とを混合し、N−メチルピロリドン(NMP)に分散させてスラリーとした後、負極集電体として10μmの銅箔に塗布し、乾燥させた。乾燥後、電極をプレス処理し、処理後の厚さが65μmになるように作製した。活物質塗布部分は幅102mm、長さ202mmとした。
基材に含まれる複数の開口を有して形成された層を構成するものとして、厚さが20μm、目開きの大きさがおよそ100μm×100μm、ガラス繊維の直径が2〜3μmの、平織のガラスクロスを用意した。基材の上に設ける無機繊維層の材料として、繊維の直径が3μmから5μmのグラスウールを用意した。グラスウールは長さが1mm未満になるように切断した。
上述のようにして得られた負極、正極およびセパレータを、負極・セパレータ・正極・セパレータ・負極・セパレータ・正極・セパレータ・負極の順に積層して、電極素子を作製した。
体積比で、EC/PC/DMC/EMC/DEC=20/20/20/20/20からなるカーボネート系非水電解液を調製し、さらに、支持塩としてのLiPF6を1モル/リットルの濃度で溶解して、電解液を形成した。
上記電極素子を外装体としてのアルミラミネートフィルムで包み、内部に電解液を注液した後、0.1気圧の減圧雰囲気下で封止することで、二次電池を作製した。
実施例1において、ガラス繊維を固定するバインダ溶液をポリビニルアルコール(PVA)の2%水溶液とした。グラスウールを分散したPVA水溶液をガラスクロスの片側表面から浸透させ、室温で乾燥した後、PVAの耐水性、耐溶剤性を上げるために、140℃で20分間熱処理を行った。このようにして作製したセパレータの厚さは、30μmであった。その他のセパレータ作製条件、二次電池の作製条件は実施例1と同一とし、作製した二次電池は、実施例1と同様の評価を行った。
実施例1で用いたのと同じガラスクロスに、厚さ10μmのポリエチレンフィルムを重ねて180℃で20分加熱した。この処理により、溶融したポリエチレンをガラスクロスに浸透させた。次に、このガラスクロスの表面に、実施例1と同じく切断したグラスウールを散布した。切断したグラスウールを散布したガラスクロスを180℃で10分間加熱したところ、再度溶融したポリエチレンにより、グラスウールがガラスクロスに固定された。また、室温まで冷却した後、ガラスクロスに固定されなかったグラスウールを除去した。このようにして作製したセパレータの厚さは、28μmであった。よって、ガラス繊維層の厚さは8μmとなる。この他は実施例1と同じ条件で二次電池を作製し、作製した二次電池について実施例1と同様の評価を行なった。
ガラスクロス単体をセパレータとした。セパレータにガラスクロスを用いた以外は、実施例1と同じ条件で二次電池を作製し、作製した二次電池について実施例1と同様の評価を行なった。
ガラスクロスに、実施例1と同じく切断したグラスウールをPVA15%水溶液に分散した溶液を塗布し、室温乾燥の後、140℃で20分間の熱処理を行ったものをセパレータとした。ガラスクロスの目開きは、PVA被膜で閉塞されていた。このようにして作製したセパレータの厚さは、30μmであった。セパレータ以外は、実施例1と同じ条件で二次電池を作製し、作製した二次電池について実施例1と同様の評価を行なった。
10 電極素子
11 外装材
12 外装材
13 負極タブ
14 正極タブ
21 負極
21a 負極集電体
21b 負極活物質
22 正極
22a 正極集電体
22b 正極活物質
23 セパレータ
23a 基材
23a1 縦糸
23a2 横糸
23b 無機繊維層
Claims (6)
- 正極と負極とを対向配置させた電極素子用のセパレータであって、
複数の開口を有して形成された、少なくとも無機繊維から作られた織物または編物からなる層を含む基材と、
前記基材の片面または両面に、前記開口を閉塞することなく前記開口を覆うように前記基材に積層された無機繊維層と、
を有し、前記基材および前記無機繊維層の両方がバインダによって固定され、かつ、全体の厚さが100μm以下であるセパレータ。 - 前記無機繊維から作られた織物または編物からなる層はガラスクロスである請求項1に記載のセパレータ。
- 前記無機繊維層はガラス繊維を含む請求項1または2に記載のセパレータ。
- 請求項1から3の何れか一項に記載のセパレータと、
前記セパレータを間において対向配置された正極および負極と、
を有する電極素子。 - 請求項4に記載の電極素子と、
電解液と、
前記電極素子および前記電解液を内包する外装体と、
を有する蓄電デバイス。 - 正極と負極とを対向配置させた電極素子用のセパレータの製造方法であって、
複数の開口を有して形成された、少なくとも無機繊維から作られた織物または編物からなる層を含む基材を用意する工程と、
前記基材および前記無機繊維層の両方をバインダで固定して前記基材の片面または両面に無機繊維層を積層する工程と、
を有し、セパレータ全体の厚さが100μm以下となるように前記基材および前記無機繊維層の厚さを選択する製造方法。
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