JP6792248B2 - エネルギー貯蔵デバイス用集電体、エネルギー貯蔵デバイス用電極及びエネルギー貯蔵デバイス - Google Patents
エネルギー貯蔵デバイス用集電体、エネルギー貯蔵デバイス用電極及びエネルギー貯蔵デバイス Download PDFInfo
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- JP6792248B2 JP6792248B2 JP2017530803A JP2017530803A JP6792248B2 JP 6792248 B2 JP6792248 B2 JP 6792248B2 JP 2017530803 A JP2017530803 A JP 2017530803A JP 2017530803 A JP2017530803 A JP 2017530803A JP 6792248 B2 JP6792248 B2 JP 6792248B2
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- SEGJNMCIMOLEDM-UHFFFAOYSA-N n-methyloctan-1-amine Chemical compound CCCCCCCCNC SEGJNMCIMOLEDM-UHFFFAOYSA-N 0.000 description 1
- QWERMLCFPMTLTG-UHFFFAOYSA-N n-methyltetradecan-1-amine Chemical compound CCCCCCCCCCCCCCNC QWERMLCFPMTLTG-UHFFFAOYSA-N 0.000 description 1
- HKUFIYBZNQSHQS-UHFFFAOYSA-N n-octadecyloctadecan-1-amine Chemical compound CCCCCCCCCCCCCCCCCCNCCCCCCCCCCCCCCCCCC HKUFIYBZNQSHQS-UHFFFAOYSA-N 0.000 description 1
- 125000003935 n-pentoxy group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])O* 0.000 description 1
- JACMPVXHEARCBO-UHFFFAOYSA-N n-pentylpentan-1-amine Chemical compound CCCCCNCCCCC JACMPVXHEARCBO-UHFFFAOYSA-N 0.000 description 1
- 125000004123 n-propyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 150000005002 naphthylamines Chemical class 0.000 description 1
- 229910021382 natural graphite Inorganic materials 0.000 description 1
- 150000002829 nitrogen Chemical class 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- FJDUDHYHRVPMJZ-UHFFFAOYSA-N nonan-1-amine Chemical compound CCCCCCCCCN FJDUDHYHRVPMJZ-UHFFFAOYSA-N 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- IOQPZZOEVPZRBK-UHFFFAOYSA-N octan-1-amine Chemical compound CCCCCCCCN IOQPZZOEVPZRBK-UHFFFAOYSA-N 0.000 description 1
- 125000002347 octyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 125000002524 organometallic group Chemical group 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000003002 pH adjusting agent Substances 0.000 description 1
- 239000006174 pH buffer Substances 0.000 description 1
- GPNDARIEYHPYAY-UHFFFAOYSA-N palladium(ii) nitrate Chemical compound [Pd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O GPNDARIEYHPYAY-UHFFFAOYSA-N 0.000 description 1
- CXZOCEZMGWOOFD-UHFFFAOYSA-N phenanthren-1-amine Chemical class C1=CC2=CC=CC=C2C2=C1C(N)=CC=C2 CXZOCEZMGWOOFD-UHFFFAOYSA-N 0.000 description 1
- KIHQWOBUUIPWAN-UHFFFAOYSA-N phenanthren-9-amine Chemical compound C1=CC=C2C(N)=CC3=CC=CC=C3C2=C1 KIHQWOBUUIPWAN-UHFFFAOYSA-N 0.000 description 1
- 229940117803 phenethylamine Drugs 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- XKJCHHZQLQNZHY-UHFFFAOYSA-N phthalimide Chemical compound C1=CC=C2C(=O)NC(=O)C2=C1 XKJCHHZQLQNZHY-UHFFFAOYSA-N 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229920001983 poloxamer Polymers 0.000 description 1
- 229920003207 poly(ethylene-2,6-naphthalate) Polymers 0.000 description 1
- 229920002492 poly(sulfone) Polymers 0.000 description 1
- 229920006122 polyamide resin Polymers 0.000 description 1
- 229920000767 polyaniline Polymers 0.000 description 1
- 239000004631 polybutylene succinate Substances 0.000 description 1
- 229920002961 polybutylene succinate Polymers 0.000 description 1
- 229920001707 polybutylene terephthalate Polymers 0.000 description 1
- 239000004632 polycaprolactone Substances 0.000 description 1
- 229920001610 polycaprolactone Polymers 0.000 description 1
- 229920005668 polycarbonate resin Polymers 0.000 description 1
- 239000004431 polycarbonate resin Substances 0.000 description 1
- 229920001225 polyester resin Polymers 0.000 description 1
- 239000004645 polyester resin Substances 0.000 description 1
- 239000011112 polyethylene naphthalate Substances 0.000 description 1
- 239000009719 polyimide resin Substances 0.000 description 1
- 239000004626 polylactic acid Substances 0.000 description 1
- 229920005596 polymer binder Polymers 0.000 description 1
- 239000002491 polymer binding agent Substances 0.000 description 1
- 229920005672 polyolefin resin Polymers 0.000 description 1
- 229920006324 polyoxymethylene Polymers 0.000 description 1
- 229920000069 polyphenylene sulfide Polymers 0.000 description 1
- 229920000128 polypyrrole Polymers 0.000 description 1
- 229920005990 polystyrene resin 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
- 239000007774 positive electrode material Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- NTTOTNSKUYCDAV-UHFFFAOYSA-N potassium hydride Chemical compound [KH] NTTOTNSKUYCDAV-UHFFFAOYSA-N 0.000 description 1
- 229910000105 potassium hydride Inorganic materials 0.000 description 1
- 150000003138 primary alcohols Chemical class 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- SCUZVMOVTVSBLE-UHFFFAOYSA-N prop-2-enenitrile;styrene Chemical compound C=CC#N.C=CC1=CC=CC=C1 SCUZVMOVTVSBLE-UHFFFAOYSA-N 0.000 description 1
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 description 1
- LLHKCFNBLRBOGN-UHFFFAOYSA-N propylene glycol methyl ether acetate Chemical compound COCC(C)OC(C)=O LLHKCFNBLRBOGN-UHFFFAOYSA-N 0.000 description 1
- 125000003373 pyrazinyl group Chemical group 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 125000000714 pyrimidinyl group Chemical group 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 1
- 125000002943 quinolinyl group Chemical group N1=C(C=CC2=CC=CC=C12)* 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 239000012744 reinforcing agent Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- SVOOVMQUISJERI-UHFFFAOYSA-K rhodium(3+);triacetate Chemical compound [Rh+3].CC([O-])=O.CC([O-])=O.CC([O-])=O SVOOVMQUISJERI-UHFFFAOYSA-K 0.000 description 1
- SONJTKJMTWTJCT-UHFFFAOYSA-K rhodium(iii) chloride Chemical compound [Cl-].[Cl-].[Cl-].[Rh+3] SONJTKJMTWTJCT-UHFFFAOYSA-K 0.000 description 1
- 238000007788 roughening Methods 0.000 description 1
- 229910001925 ruthenium oxide Inorganic materials 0.000 description 1
- OJLCQGGSMYKWEK-UHFFFAOYSA-K ruthenium(3+);triacetate Chemical compound [Ru+3].CC([O-])=O.CC([O-])=O.CC([O-])=O OJLCQGGSMYKWEK-UHFFFAOYSA-K 0.000 description 1
- YBCAZPLXEGKKFM-UHFFFAOYSA-K ruthenium(iii) chloride Chemical compound [Cl-].[Cl-].[Cl-].[Ru+3] YBCAZPLXEGKKFM-UHFFFAOYSA-K 0.000 description 1
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 description 1
- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- BHRZNVHARXXAHW-UHFFFAOYSA-N sec-butylamine Chemical compound CCC(C)N BHRZNVHARXXAHW-UHFFFAOYSA-N 0.000 description 1
- QZAYGJVTTNCVMB-UHFFFAOYSA-N serotonin Chemical compound C1=C(O)C=C2C(CCN)=CNC2=C1 QZAYGJVTTNCVMB-UHFFFAOYSA-N 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 229910001923 silver oxide Inorganic materials 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- ODZPKZBBUMBTMG-UHFFFAOYSA-N sodium amide Chemical class [NH2-].[Na+] ODZPKZBBUMBTMG-UHFFFAOYSA-N 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 239000012312 sodium hydride Substances 0.000 description 1
- 229910000104 sodium hydride Inorganic materials 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 125000006850 spacer group Chemical group 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
- 239000001384 succinic acid Substances 0.000 description 1
- 150000004763 sulfides Chemical class 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 150000003462 sulfoxides Chemical class 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 150000003464 sulfur compounds Chemical class 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- KKEYFWRCBNTPAC-UHFFFAOYSA-L terephthalate(2-) Chemical compound [O-]C(=O)C1=CC=C(C([O-])=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-L 0.000 description 1
- 229920006027 ternary co-polymer Polymers 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- AOCSUUGBCMTKJH-UHFFFAOYSA-N tert-butyl n-(2-aminoethyl)carbamate Chemical compound CC(C)(C)OC(=O)NCCN AOCSUUGBCMTKJH-UHFFFAOYSA-N 0.000 description 1
- POHWAQLZBIMPRN-UHFFFAOYSA-N tert-butyl n-(3-aminopropyl)carbamate Chemical compound CC(C)(C)OC(=O)NCCCN POHWAQLZBIMPRN-UHFFFAOYSA-N 0.000 description 1
- ZFQWJXFJJZUVPI-UHFFFAOYSA-N tert-butyl n-(4-aminobutyl)carbamate Chemical compound CC(C)(C)OC(=O)NCCCCN ZFQWJXFJJZUVPI-UHFFFAOYSA-N 0.000 description 1
- YBRBMKDOPFTVDT-UHFFFAOYSA-N tert-butylamine Chemical compound CC(C)(C)N YBRBMKDOPFTVDT-UHFFFAOYSA-N 0.000 description 1
- 125000005931 tert-butyloxycarbonyl group Chemical group [H]C([H])([H])C(OC(*)=O)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- CBXCPBUEXACCNR-UHFFFAOYSA-N tetraethylammonium Chemical compound CC[N+](CC)(CC)CC CBXCPBUEXACCNR-UHFFFAOYSA-N 0.000 description 1
- CZDYPVPMEAXLPK-UHFFFAOYSA-N tetramethylsilane Chemical compound C[Si](C)(C)C CZDYPVPMEAXLPK-UHFFFAOYSA-N 0.000 description 1
- OSBSFAARYOCBHB-UHFFFAOYSA-N tetrapropylammonium Chemical compound CCC[N+](CCC)(CCC)CCC OSBSFAARYOCBHB-UHFFFAOYSA-N 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000010023 transfer printing Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- IFXORIIYQORRMJ-UHFFFAOYSA-N tribenzylphosphane Chemical compound C=1C=CC=CC=1CP(CC=1C=CC=CC=1)CC1=CC=CC=C1 IFXORIIYQORRMJ-UHFFFAOYSA-N 0.000 description 1
- IMFACGCPASFAPR-UHFFFAOYSA-N tributylamine Chemical compound CCCCN(CCCC)CCCC IMFACGCPASFAPR-UHFFFAOYSA-N 0.000 description 1
- TUQOTMZNTHZOKS-UHFFFAOYSA-N tributylphosphine Chemical compound CCCCP(CCCC)CCCC TUQOTMZNTHZOKS-UHFFFAOYSA-N 0.000 description 1
- DANYXEHCMQHDNX-UHFFFAOYSA-K trichloroiridium Chemical compound Cl[Ir](Cl)Cl DANYXEHCMQHDNX-UHFFFAOYSA-K 0.000 description 1
- WLPUWLXVBWGYMZ-UHFFFAOYSA-N tricyclohexylphosphine Chemical compound C1CCCCC1P(C1CCCCC1)C1CCCCC1 WLPUWLXVBWGYMZ-UHFFFAOYSA-N 0.000 description 1
- ABVVEAHYODGCLZ-UHFFFAOYSA-N tridecan-1-amine Chemical compound CCCCCCCCCCCCCN ABVVEAHYODGCLZ-UHFFFAOYSA-N 0.000 description 1
- BDZBKCUKTQZUTL-UHFFFAOYSA-N triethyl phosphite Chemical compound CCOP(OCC)OCC BDZBKCUKTQZUTL-UHFFFAOYSA-N 0.000 description 1
- YFTHZRPMJXBUME-UHFFFAOYSA-N tripropylamine Chemical compound CCCN(CCC)CCC YFTHZRPMJXBUME-UHFFFAOYSA-N 0.000 description 1
- KCTAHLRCZMOTKM-UHFFFAOYSA-N tripropylphosphane Chemical compound CCCP(CCC)CCC KCTAHLRCZMOTKM-UHFFFAOYSA-N 0.000 description 1
- QFKMMXYLAPZKIB-UHFFFAOYSA-N undecan-1-amine Chemical compound CCCCCCCCCCCN QFKMMXYLAPZKIB-UHFFFAOYSA-N 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 239000002966 varnish Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000003232 water-soluble binding agent Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Images
Classifications
-
- 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
- H01G11/66—Current collectors
- H01G11/68—Current collectors characterised by their material
-
- 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
- H01G11/66—Current collectors
- H01G11/70—Current collectors characterised by their structure
-
- 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
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/64—Carriers or collectors
- H01M4/66—Selection of materials
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Cell Electrode Carriers And Collectors (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
Description
1.(a)熱可塑性樹脂、(b)アンモニウム基を分子末端に有し、重量平均分子量(Mw)が1,000〜5,000,000のハイパーブランチポリマー及び(c)金属微粒子を含む樹脂組成物をエレクトロスピニング法で紡糸してなるナノファイバー集合体を無電解銅めっき処理してなる導電性ナノファイバー集合体を備えるエネルギー貯蔵デバイス用集電体。
2.(a)熱可塑性樹脂、(b)アンモニウム基を分子末端に有し、Mwが1,000〜5,000,000のハイパーブランチポリマー及び(c)金属微粒子を含んで構成される、平均直径が50〜2,000nmのナノファイバーの集合体と、その表面の一部又は全部に形成された銅めっき層と、を備える導電性ナノファイバー集合体を備えるエネルギー貯蔵デバイス用集電体。
3.(c)金属微粒子に、(b)ハイパーブランチポリマーのアンモニウム基が付着して複合体を形成している1又は2のエネルギー貯蔵デバイス用集電体。
4.(b)ハイパーブランチポリマーが、式[1]で表されるものである1〜3のいずれかのエネルギー貯蔵デバイス用集電体。
5.(b)ハイパーブランチポリマーが、式[3]で表されるものである4のエネルギー貯蔵デバイス用集電体。
6.(c)金属微粒子が、鉄(Fe)、コバルト(Co)、ニッケル(Ni)、銅(Cu)、パラジウム(Pd)、銀(Ag)、スズ(Sn)、白金(Pt)及び金(Au)からなる群より選択される少なくとも一種の金属の微粒子である1〜5のいずれかのエネルギー貯蔵デバイス用集電体。
7.(c)金属微粒子が、パラジウム微粒子である6のエネルギー貯蔵デバイス用集電体。
8.(c)金属微粒子の平均粒径が、1〜100nmである1〜6のいずれかのエネルギー貯蔵デバイス用集電体。
9.(a)熱可塑性樹脂が、フッ化ビニリデン−ヘキサフルオロプロピレン共重合体である1〜7のいずれかのエネルギー貯蔵デバイス用集電体。
10.前記導電性ナノファイバー集合体の体積抵抗値が、1×104Ω・cm以下である1〜9のいずれかのエネルギー貯蔵デバイス用集電体。
11.前記導電性ナノファイバー集合体のみからなる1〜10のいずれかのエネルギー貯蔵デバイス用集電体。
12.更に、導電性基材を備える1〜10のいずれかのエネルギー貯蔵デバイス用集電体。
13.前記導電性基材が、銅又は銅を含む合金である12のエネルギー貯蔵デバイス用集電体。
14.前記導電性ナノファイバー集合体が、前記導電性基材の片面又は両面に形成されている12又は13のエネルギー貯蔵デバイス用集電体。
15.1〜14のいずれかのエネルギー貯蔵デバイス用集電体を備えるエネルギー貯蔵デバイス用電極。
16.15のエネルギー貯蔵デバイス用電極を備えるエネルギー貯蔵デバイス。
17.(a)熱可塑性樹脂と、(b)アンモニウム基を分子末端に有し、Mwが1,000〜5,000,000のハイパーブランチポリマーと、(c)金属微粒子とを含む樹脂組成物をエレクトロスピニング法にて導電性基材の片面又は両面に付着させてナノファイバー集合体を含む積層体を作製する工程、及び
前記工程で得られた積層体を無電解銅めっき処理する工程
を含むエネルギー貯蔵デバイス用集電体の製造方法。
また、紡糸材料として特定のハイパーブランチポリマーと金属微粒子を配合した熱可塑性樹脂を用いて静電紡糸し、得られたナノファイバーを無電解銅めっき浴に浸すという簡便な工程にて、電気伝導性に優れる導電性ナノファイバーを備える集電体を容易に得ることができる。このため、従来の無電解めっき処理に必要とされた煩雑な前処理工程の必要性や、製造工程の複雑化、高コスト化といった問題に煩わされることがない。
本発明のエネルギー貯蔵デバイス用集電体は、(a)熱可塑性樹脂、(b)アンモニウム基を分子末端に有し、Mwが1,000〜5,000,000のハイパーブランチポリマー及び(c)金属微粒子を含む樹脂組成物をエレクトロスピニング法で紡糸してなるナノファイバー集合体を無電解銅めっき処理してなる導電性ナノファイバー集合体を備えるものである。その構成としては、前記(a)〜(c)成分を含んで構成される、平均直径が50〜2,000nmのナノファイバーの集合体と、その表面の一部又は全部に形成された銅めっき層と、を備える導電性ナノファイバー集合体を備えるものである。
<(a)熱可塑性樹脂>
(a)熱可塑性樹脂としては特に限定されないが、例えば、ポリエチレン(PE)、ポリプロピレン(PP)、エチレン−酢酸ビニル共重合体(EVA)、エチレン−ビニルアルコール共重合体(EVOH)、ポリビニルアルコール(PVA)、エチレン−アクリル酸エチル共重合体(EEA)、ポリフッ化ビニリデン(PVDF)、フッ化ビニリデン−ヘキサフルオロプロピレン共重合体(PVDF/HFP)等のポリオレフィン系樹脂;ポリスチレン(PS)、ハイインパクトポリスチレン(HIPS)、アクリロニトリル−スチレン共重合体(AS)、アクリロニトリル−ブタジエン−スチレン共重合体(ABS)、スチレン−ブタジエン−スチレン共重合体(SBS)、メタクリル酸メチル−スチレン共重合体(MS)等のポリスチレン系樹脂;ポリカーボネート樹脂;塩化ビニル樹脂;ポリアミド樹脂;ポリイミド樹脂;ポリウレタンエラストマー(PUE)等のポリウレタン樹脂;ポリメチルメタクリレート(PMMA)等の(メタ)アクリル樹脂;ポリアクリロニトリル(PAN);ポリエチレンテレフタレート(PET)、ポリブチレンテレフタレート、ポリエチレンナフタレート、ポリブチレンナフタレート、ポリ乳酸(PLA)、ポリ−3−ヒドロキシ酪酸、ポリカプロラクトン、ポリブチレンサクシネート、ポリエチレンサクシネート/アジペート等のポリエステル樹脂;ポリエチレンオキシド(PEO);ポリフェニレンエーテル樹脂;変性ポリフェニレンエーテル樹脂;ポリアセタール樹脂;ポリエーテルスルホン(PES)樹脂、ポリスルホン樹脂;ポリフェニレンサルファイド樹脂;ポリビニルアルコール樹脂;ポリグルコール酸;変性でんぷん;酢酸セルロース、三酢酸セルロース;キチン、キトサン;リグニン等が挙げられる。中でも、(a)熱可塑性樹脂として、PVDF、PVDF/HFP、ポリウレタン樹脂等を用いることが好ましい。
(b)ハイパーブランチポリマーは、アンモニウム基を分子末端に有し、かつMwが1,000〜5,000,000であるポリマーであり、具体的には下記式[1]で表されるものが挙げられる。
(c)金属微粒子としては特に限定されず、金属種としては鉄(Fe)、コバルト(Co)、ニッケル(Ni)、銅(Cu)、パラジウム(Pd)、銀(Ag)、スズ(Sn)、白金(Pt)、金(Au)等が挙げられ、これらの金属の1種類でもよいし、2種以上の合金でもよい。中でも好ましい金属微粒子としては、パラジウム微粒子が挙げられる。なお、金属微粒子として、前記金属の酸化物を用いてもよい。
使用する溶媒としては、金属イオンとハイパーブランチポリマーとを必要濃度以上に溶解できる溶媒であれば特に限定されないが、具体的には、メタノール、エタノール、1−プロパノール、2−プロパノール等のアルコール類;塩化メチレン、クロロホルム等のハロゲン化炭化水素類;THF、2−メチルテトラヒドロフラン、テトラヒドロピラン等の環状エーテル類;アセトニトリル、ブチロニトリル等のニトリル類;DMF、NMP等のアミド類;ジメチルスルホキシド等のスルホキシド類等、及びこれらの溶媒の混合溶媒が挙げられ、好ましくは、アルコール類、ハロゲン化炭化水素類、環状エーテル類が挙げられ、より好ましくは、エタノール、2−プロパノール、クロロホルム、THF等が挙げられる。
<紡糸工程>
本発明の導電性ナノファイバーの製造方法における紡糸工程は、(a)熱可塑性樹脂、(b)ハイパーブランチポリマー及び(c)金属微粒子を含む樹脂組成物を紡糸材料として、エレクトロスピニング法に従い、ナノファイバーを作製する工程である。実際には、前記樹脂組成物を溶媒に溶解又は分散してワニスの形態とし、これを静電紡糸して集合体(不織布)状のナノファイバーを作製する工程である。
この工程は、前述の紡糸工程で作製したナノファイバーを無電解銅めっき処理する工程である。なお前述の紡糸工程にて作製されたナノファイバーは、繊維表面部(界面)に前記ハイパーブランチポリマー及び金属微粒子(これらから形成された複合体)が存在した状態にある。このため、エッチング、コンディショニング、キャタライジング、アクセラレーティングといった各処理からなるめっき前処理を必要とすることなく、エレクトロスピニング法によって得られたナノファイバーをそのまま無電解銅めっき処理に供することができる。
本発明のエネルギー貯蔵デバイス用電極は、前記導電性ナノファイバー集合体を備えるエネルギー貯蔵デバイス用集電体上に、活物質及び溶媒、並びに必要に応じて、電極層の導電性向上のために炭素等からなる導電助剤、バインダー等を含む電極スラリーを塗布して薄膜を形成することで作製することができる。
本発明のエネルギー貯蔵デバイスは、前述した電極を備えるものであり、より具体的には、少なくとも一対の正負極と、これら各極間に介在するセパレータと、電解質とを備えて構成され、正負極の少なくとも一方が、前述したエネルギー貯蔵デバイス用電極から構成される。
装置:東ソー(株)製HLC-8220GPC
カラム:昭和電工(株)製Shodex(登録商標)KF-804l + KF-803l
カラム温度:40℃
溶媒:テトラヒドロフラン
検出器:UV(254nm)、RI
(2)1H−NMRスペクトル
装置:日本電子(株)製JNM-L400
溶媒:CDCl3
内部標準:テトラメチルシラン(0.00ppm)
(3)13C−NMRスペクトル
装置:日本電子(株)製JNM-ECA700
溶媒:CDCl3
緩和試薬:トリスアセチルアセトナートクロム(Cr(acac)3)
基準:CDCl3(77.0ppm)
(4)ICP発光分析(誘導結合プラズマ発光分析)
装置:(株)島津製作所製ICPM-8500
(5)透過型電子顕微鏡(TEM)画像
装置:(株)日立ハイテクノロジーズ製H-8000
(6)エレクトロスピニング
インフュージョンポンプ(シリンジポンプ):(有)メルクエスト製FP-1000
高圧電源:松定プレシジョン(株)製HR-40R0.75
(7)走査型電子顕微鏡(SEM)画像
装置:(株)キーエンス製3Dリアルサーフェスビュー顕微鏡VE-9800
(8)ナノファイバーマットの厚み測定
装置:(株)ミツトヨ製マイクロメータMDQ-30
(9)体積抵抗値測定
装置:(株)三菱化学アナリテック製ロレスタ(登録商標)AX MCP-T370
(10)充放電測定装置(二次電池評価)
装置:東洋システム(株)製TOSCAT 3100
HPS:ハイパーブランチポリスチレン(日産化学工業(株)製ハイパーテック(登録商標)HPS-200)
IPA:2−プロパノール
IPE:ジイソプロピルエーテル
PVDF/HFP:フッ化ビニリデン−ヘキサフルオロプロピレン共重合体(アルドリッチ社製 製品番号:427160、Mw(GPC):400,000、Mn:130,000)
DMF:N,N−ジメチルホルムアミド
別の300mLの反応フラスコに、ジチオカルバメート基を分子末端に有するハイパーブランチポリマーHPS15g及びクロロホルム150gを仕込み、窒素気流下均一になるまで攪拌した。
前記0℃に冷却した塩化スルフリル/クロロホルム溶液中に、窒素気流下、HPS/クロロホルム溶液が仕込まれた前記300mLの反応フラスコから、送液ポンプを用いて、該溶液を反応液の温度が−5〜5℃となるように60分間かけて加えた。添加終了後、反応液の温度を−5〜5℃に保持しながら6時間攪拌した。
更にこの反応液へ、シクロヘキセン(東京化成工業(株)製)16gをクロロホルム50gに溶かした溶液を、反応液の温度が−5〜5℃となるように加えた。添加終了後、この反応液をIPA1,200gに添加してポリマーを沈殿させた。この沈殿をろ取して得られた白色粉末をクロロホルム100gに溶解し、これをIPA500gに添加してポリマーを再沈殿させた。この沈殿物を減圧ろ過し、真空乾燥して、塩素原子を分子末端に有するハイパーブランチポリマー(HPS−Cl)8.5gを白色粉末として得た(収率99%)。
得られたHPS−Clの1H−NMRスペクトルを図1に示す。ジチオカルバメート基由来のピーク(4.0ppm、3.7ppm)が消失していることから、得られたHPS−Clは、HPS分子末端のジチオカルバメート基がほぼ全て塩素原子に置換されていることが明らかとなった。また、得られたHPS−ClのGPCによるポリスチレン換算で測定されるMwは14,000、Mw/Mnは2.9であった。
液温30℃まで冷却後、溶媒を留去した。得られた残渣を、クロロホルム60gに溶解し、この溶液をIPE290gに添加して再沈精製した。析出したポリマーを減圧ろ過し、50℃で真空乾燥して、ジメチルオクチルアンモニウム基を分子末端に有するハイパーブランチポリマー(HPS−N(Me)2OctCl)9.3gを白色粉末として得た。
得られたHPS−N(Me)2OctClの13C−NMRスペクトルを図2に示す。ベンゼン環のピークと、オクチル基末端のメチル基のピークから、得られたHPS−N(Me)2OctClは、HPS−Cl分子末端の塩素原子がほぼ定量的にアンモニウム基に置換されていることが明らかとなった。また、HPS−ClのMw(14,000)及びアンモニウム基導入率(100%)から算出されるHPS−N(Me)2OctClのMwは、28,000となった。
凝縮器を設置した300mLの反応フラスコに、酢酸パラジウム(川研ファインケミカル(株)製)2.1g及びクロロホルム20gを仕込み、均一になるまで攪拌した。この溶液へ、製造例2で製造したHPS−N(Me)2OctCl 9.0gをクロロホルム135gに溶解させた溶液を、滴下ロートを使用して加えた。この滴下ロート内を、エタノール45gを使用して前記反応フラスコへ洗い込んだ。この混合物を、60℃で8時間攪拌した。
液温30℃まで冷却後、この反応混合物を0℃のIPE2,000gに添加して再沈精製した。析出したポリマーを減圧ろ過し、60℃で真空乾燥して、アンモニウム基を分子末端に有するハイパーブランチポリマーとPd粒子との複合体(Pd[HPS−N(Me)2OctCl])9.8gを黒色粉末として得た。
ICP発光分析の結果から、得られたPd[HPS−N(Me)2OctCl]のPd含有量は、10質量%であった。また、TEM画像から、そのPd粒子径は、およそ2〜4nmであった。
500mLのフラスコに、イオン交換水210mL、スルカップ(登録商標)PSY-1A(上村工業(株)製)25mL、スルカップ(登録商標)PSY-1B(上村工業(株)製)10mL、及び37%ホルムアルデヒド水溶液(東京化成工業(株)製)をイオン交換水で2倍に希釈したもの5mLを順次仕込んだ。この溶液へ界面活性剤としてアデカ(登録商標)プルロニックL-34((株)ADEKA製)0.025gを加えて、無電解銅めっき液とした。
PVDF/HFP100質量部、製造例3で製造したPd[HPS−N(Me)2OctCl]3質量部(Pdとして0.3質量部)、及びDMF400質量部を均一に混合し、樹脂組成物(紡糸材料)を調製した。
この組成物を、エレクトロスピニング装置を用いて、印加電圧19.5kV、紡糸距離20cm、紡糸量0.6mL/hとして紡糸し、マット状のナノファイバーの集合体(以下、ナノファイバーマットと称する。)を作製した。得られたナノファイバーマットをSEMで観察し、ナノファイバー径(平均直径)を算出したところ、0.27μmであった。ナノファイバー径は、異なる5箇所のSEM画像から無作為に選択した100本のナノファイバーの直径を計測し、その平均値とした。
次に、このナノファイバーマットを、無電解銅めっき液に33℃で90分浸漬した。その後、取り出したナノファイバーマットを水洗し、50℃で60分乾燥した。得られた無電解銅めっき処理したナノファイバーマットのナノファイバー径を、前述と同様に算出したところ、0.95μmであった。また、ナノファイバーマットの体積抵抗値を測定した結果、3.96×10-5Ω・cmであった。得られた無電解銅めっき処理したナノファイバーマットのSEM画像を図3に示す。なお、ナノファイバーマットの厚みは、60μmであった。
活物質としてケイ素(Si)((株)高純度化学研究所製SIE23PB、24.0g)、バインダーとしてポリアクリル酸の水溶液(アルドリッチ社製、8質量%、25.5g)、増粘材としてナトリウムカルボキシメチルセルロース(NaCMC、アズワン(株)製、CMF-150、0.360g)、及び導電助剤としてアセチレンブラック(AB)(電気化学工業(株)製、デンカブラック、3.59g)を、ビーズミル(ジルコニアビーズ、φ0.5mm、2,000rpm、30分)にて混合し、電極スラリー(固形分濃度50質量%、Si:PAA:NaCMC:AB=80:6.8:1.2:12(質量比))を作製した。
得られた電極スラリーを、ドクターブレード法によりナノファイバーマット上に均一(ウェット膜厚25μm)に展開後、80℃で30分、次いで120℃で30分乾燥して導電性結着層上に活物質層を形成し、電極を作製した。得られた電極のSEM画像を図4に示す。図3と4の比較で明らかなように、電極に含まれるSiやABは、ナノファイバーマットに存在する空隙よりも小さく、一部内部に充填されていることがわかった。
電極中のケイ素の質量は、電極を直径10mmの円盤状に打ち抜き、得られた質量から、スラリーを塗布していない部分の基材を直径10mmの円盤状に打ち抜き、得られた質量を差し引き、更にケイ素の質量比を乗じることで算出した結果、1.93mgであった。
打ち抜いた電極を15時間100℃で真空乾燥し、アルゴンで満たされたグローブボックスに移した。
2032型のコインセル(宝泉(株)製)のワッシャーとスペーサーが溶接されたフタに、直径14mmに打ち抜いたリチウム箔(本荘ケミカル(株)製、厚み0.17mm)を6枚重ねたものを設置し、その上に、電解液(キシダ化学(株)製、エチレンカーボネート:ジエチルカーボネート(1:1、体積比)、電解質であるリチウムヘキサフルオロホスフェートを1mol/L含む)を24時間以上染み込ませた、直径16mmに打ち抜いたセパレータ(セルガード(株)製、2400)を一枚重ねた。更に上から、活物質を塗布した面を下にして電極を重ねた。電解液を1滴滴下したのち、ケースとガスケットを乗せて、コインセルかしめ機で密封した。その後24時間静置し、試験用の二次電池とした。
リチウムイオン電池の基材として、ナノファイバーマットのかわりに厚み18μmの銅箔を使用し、ウェット膜厚50μmとした以外は、実施例1で用いた電極スラリーをそのまま用い、実施例1と同様の方法でリチウムイオン二次電池を作製した。電極中のケイ素の重量は、1.44mgであった。
リチウムイオン電池の基材として、ナノファイバーマットのかわりに厚み18μmの銅箔を使用し、ウェット膜厚100μmとした以外は、実施例1で用いた電極スラリーをそのまま用い、実施例1と同様の方法でリチウムイオン二次電池を作製した。電極中のケイ素の重量は、3.10mgであった。
・電流:0.1C定電流充放電(1サイクル目のみ0.01Vでの定電流定電圧充電、Siの容量を4200mAh/gとした)
・カットオフ電圧:1.50V−0.01V
・充電容量:活物質の重量を基準とし、2,000mAh/gまで
・温度:室温
Claims (14)
- (a)熱可塑性樹脂、(b)アンモニウム基を分子末端に有し、重量平均分子量が1,000〜5,000,000のハイパーブランチポリマー及び(c)鉄(Fe)、コバルト(Co)、ニッケル(Ni)、銅(Cu)、パラジウム(Pd)、銀(Ag)、スズ(Sn)、白金(Pt)及び金(Au)からなる群より選択される少なくとも一種の金属微粒子を含んで構成され、(c)金属微粒子に(b)ハイパーブランチポリマーのアンモニウム基が付着して複合体を形成している、平均直径が50〜2,000nmのナノファイバーの集合体と、その表面の一部又は全部に形成された銅めっき層と、を備える導電性ナノファイバー集合体を備えるエネルギー貯蔵デバイス用集電体。
- (b)ハイパーブランチポリマーが、式[1]で表されるものである請求項1記載のエネルギー貯蔵デバイス用集電体。
- (c)金属微粒子が、パラジウム微粒子である請求項1〜3のいすれか1項記載のエネルギー貯蔵デバイス用集電体。
- (c)金属微粒子の平均粒径が、1〜100nmである請求項1〜4のいずれか1項記載のエネルギー貯蔵デバイス用集電体。
- (a)熱可塑性樹脂が、フッ化ビニリデン−ヘキサフルオロプロピレン共重合体である請求項1〜5のいずれか1項記載のエネルギー貯蔵デバイス用集電体。
- 前記導電性ナノファイバー集合体の体積抵抗値が、1×104Ω・cm以下である請求項1〜6のいずれか1項記載のエネルギー貯蔵デバイス用集電体。
- 前記導電性ナノファイバー集合体のみからなる請求項1〜7のいずれか1項記載のエネルギー貯蔵デバイス用集電体。
- 更に、導電性基材を備える請求項1〜7のいずれか1項記載のエネルギー貯蔵デバイス用集電体。
- 前記導電性基材が、銅又は銅を含む合金である請求項9記載のエネルギー貯蔵デバイス用集電体。
- 前記導電性ナノファイバー集合体が、前記導電性基材の片面又は両面に形成されている請求項9又は10記載のエネルギー貯蔵デバイス用集電体。
- 請求項1〜11のいずれか1項記載のエネルギー貯蔵デバイス用集電体を備えるエネルギー貯蔵デバイス用電極。
- 請求項12記載のエネルギー貯蔵デバイス用電極を備えるエネルギー貯蔵デバイス。
- (a)熱可塑性樹脂と、(b)アンモニウム基を分子末端に有し、重量平均分子量が1,000〜5,000,000のハイパーブランチポリマー並びに(c)鉄(Fe)、コバルト(Co)、ニッケル(Ni)、銅(Cu)、パラジウム(Pd)、銀(Ag)、スズ(Sn)、白金(Pt)及び金(Au)からなる群より選択される少なくとも一種の金属微粒子からなる複合体であって、(c)金属微粒子に(b)ハイパーブランチポリマーのアンモニウム基が付着して形成された複合体とを含む樹脂組成物をエレクトロスピニング法にて導電性基材の片面又は両面に付着させてナノファイバー集合体を含む積層体を作製する工程、及び
前記工程で得られた積層体を無電解銅めっき処理する工程
を含むエネルギー貯蔵デバイス用集電体の製造方法。
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