JPWO2019189146A1 - リチウムイオン二次電池、及びその作動方法 - Google Patents
リチウムイオン二次電池、及びその作動方法 Download PDFInfo
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- JPWO2019189146A1 JPWO2019189146A1 JP2020510889A JP2020510889A JPWO2019189146A1 JP WO2019189146 A1 JPWO2019189146 A1 JP WO2019189146A1 JP 2020510889 A JP2020510889 A JP 2020510889A JP 2020510889 A JP2020510889 A JP 2020510889A JP WO2019189146 A1 JPWO2019189146 A1 JP WO2019189146A1
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- Japan
- Prior art keywords
- sulfur
- mass
- secondary battery
- negative electrode
- lithium
- Prior art date
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- Granted
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- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 28
- 238000011017 operating method Methods 0.000 title description 2
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- 238000000034 method Methods 0.000 claims abstract description 28
- 239000011149 active material Substances 0.000 claims abstract description 22
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 14
- 239000011593 sulfur Substances 0.000 claims abstract description 14
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- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 4
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- 101710102978 Protein associated with UVRAG as autophagy enhancer Proteins 0.000 description 1
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- 238000001816 cooling Methods 0.000 description 1
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- 238000007723 die pressing method Methods 0.000 description 1
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- 239000006185 dispersion Substances 0.000 description 1
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- KLKFAASOGCDTDT-UHFFFAOYSA-N ethoxymethoxyethane Chemical compound CCOCOCC KLKFAASOGCDTDT-UHFFFAOYSA-N 0.000 description 1
- HHEIMYAXCOIQCJ-UHFFFAOYSA-N ethyl 2,2-dimethylpropanoate Chemical compound CCOC(=O)C(C)(C)C HHEIMYAXCOIQCJ-UHFFFAOYSA-N 0.000 description 1
- IJUHLFUALMUWOM-UHFFFAOYSA-N ethyl 3-methoxypropanoate Chemical compound CCOC(=O)CCOC IJUHLFUALMUWOM-UHFFFAOYSA-N 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- UKFXDFUAPNAMPJ-UHFFFAOYSA-N ethylmalonic acid Chemical compound CCC(C(O)=O)C(O)=O UKFXDFUAPNAMPJ-UHFFFAOYSA-N 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 229920001973 fluoroelastomer Polymers 0.000 description 1
- KGPPDNUWZNWPSI-UHFFFAOYSA-N flurotyl Chemical compound FC(F)(F)COCC(F)(F)F KGPPDNUWZNWPSI-UHFFFAOYSA-N 0.000 description 1
- 229910003472 fullerene Inorganic materials 0.000 description 1
- 239000006232 furnace black Substances 0.000 description 1
- 239000002241 glass-ceramic Substances 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 229910052735 hafnium Inorganic materials 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 239000002608 ionic liquid Substances 0.000 description 1
- 150000002500 ions Chemical class 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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- HSZCZNFXUDYRKD-UHFFFAOYSA-M lithium iodide Inorganic materials [Li+].[I-] HSZCZNFXUDYRKD-UHFFFAOYSA-M 0.000 description 1
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- ZQXSMRAEXCEDJD-UHFFFAOYSA-N n-ethenylformamide Chemical compound C=CNC=O ZQXSMRAEXCEDJD-UHFFFAOYSA-N 0.000 description 1
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- 239000011331 needle coke Substances 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 239000010955 niobium Substances 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
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- RKEWSXXUOLRFBX-UHFFFAOYSA-N pimavanserin Chemical compound C1=CC(OCC(C)C)=CC=C1CNC(=O)N(C1CCN(C)CC1)CC1=CC=C(F)C=C1 RKEWSXXUOLRFBX-UHFFFAOYSA-N 0.000 description 1
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- 229940005642 polystyrene sulfonic acid Drugs 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
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- 229920001289 polyvinyl ether Polymers 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
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- 239000004576 sand Substances 0.000 description 1
- 229910052706 scandium Inorganic materials 0.000 description 1
- 239000011163 secondary particle Substances 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
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- MBDNRNMVTZADMQ-UHFFFAOYSA-N sulfolene Chemical compound O=S1(=O)CC=CC1 MBDNRNMVTZADMQ-UHFFFAOYSA-N 0.000 description 1
- FFFHXSGSMLTXFJ-UHFFFAOYSA-N tert-butyl propyl carbonate Chemical compound CCCOC(=O)OC(C)(C)C FFFHXSGSMLTXFJ-UHFFFAOYSA-N 0.000 description 1
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- YFHICDDUDORKJB-UHFFFAOYSA-N trimethylene carbonate Chemical compound O=C1OCCCO1 YFHICDDUDORKJB-UHFFFAOYSA-N 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
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- 229910052727 yttrium Inorganic materials 0.000 description 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N zinc oxide Inorganic materials [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 1
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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/137—Electrodes based on electro-active polymers
-
- 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
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- 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
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/44—Methods for charging or discharging
-
- 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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/60—Selection of substances as active materials, active masses, active liquids of organic compounds
-
- 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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/60—Selection of substances as active materials, active masses, active liquids of organic compounds
- H01M4/602—Polymers
- H01M4/604—Polymers containing aliphatic main chain polymers
-
- 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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
-
- 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
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Secondary Cells (AREA)
Abstract
Description
また本発明は、硫黄変性ポリアクリロニトリルを活物質とする負極を有する、リチウムイオン二次電池の作動方法であって、負極の充電下限電位を0.1V(vs.Li/Li+)以上で、1.0V(vs.Li/Li+)未満とする、リチウムイオン二次電池の作動方法を提供するものである。
ポリアクリロニトリル粉末(シグマアルドリッチ製、平均粒径200μm)10質量部及び硫黄粉末(シグマアルドリッチ製、平均粒径200μm)30質量部を、乳鉢を用いて混合した。ポリアクリロニトリルの硫黄変性には特開2013−054957号公報の実施例に準じた反応装置を用いた。この混合物を特開2013−054957号公報の実施例に記載されたものと同様の円筒状ガラスビンに入れ、ガラスビンの下部をルツボ型電気炉に入れ、窒素気流下に発生する硫化水素を除去しながら400℃で1時間加熱した。冷却後、生成物をガラスチューブオーブンに入れ、真空吸引しつつ250℃で3時間加熱することにより単体硫黄を除去した。得られた硫黄変性ポリアクリロニトリルを、乳鉢を用いて、平均粒子径が10μmになるまで粉砕し硫黄変性ポリアクリロニトリル粉末PANS1を得た。PANS1の硫黄含量は38質量%である。
単体硫黄の除去温度を250℃から200℃に変更した以外は製造例1と同様の操作を行い硫黄変性ポリアクリロニトリル粉末PANS2を得た。PANS2の硫黄含量は55質量%である。なお、製造例2の単体硫黄の除去条件は特許文献3に記載の条件と同様であり、PANS2の硫黄含量は特許文献3記載の硫黄変性ポリアクリロニトリルと同等であるものと考えられる。
〔負極1〜10の製造〕
電極活物質として、PANS1又はPANS2(表1参照)を92.0質量部、導電助剤として3.5質量部のアセチレンブラック(電気化学工業製)、1.5質量部のカーボンナノチューブ(昭和電工製、商品名 VGCF)、バインダーとして1.5質量部のスチレン−ブタジエンゴム(40質量%水分散液、日本ゼオン製)、1.5質量部のカルボキシメチルセルロースナトリウム(ダイセルファインケム製)、及び100質量部の水を、自転・公転ミキサーを用いて分散しスラリーを調製した。このスラリー組成物を、ドクターブレード法によりステンレス箔(厚さ10μm)の集電材に電極合剤層の厚さが下記表1の値となるように塗布し、90℃で3時間乾燥した。その後、この電極を所定の大きさにカットし、120℃で2時間真空乾燥を行い、円盤状電極を作製した。
正極活物質として、LiNi1/3Co1/3Mn1/3O2(日本化学産業製、以下、NCMと略記)を90質量部、導電助剤として5質量部のアセチレンブラック(電気化学工業製)、バインダーとして5質量部のポリフッ化ビニリデン(クレハ製)、及び溶媒として100質量部のN−メチルピロリドンを、自転・公転ミキサーを用いて分散しスラリーを調製した。このスラリー組成物を、ドクターブレード法によりアルミニウム箔(厚さ20μm)の集電材に電極合剤層の厚さが62μmとなるように塗布し、90℃で3時間乾燥した。その後、この電極を所定の大きさにカットし、120℃で2時間真空乾燥を行い、円盤状の正極を作製した。正極容量は、負極の充電下限電位がいずれの場合においても、正極の充電上限電位が4.2V(vs.Li/Li+)になるようにした。
エチレンカーボネート50体積%、ジエチルカーボネート50体積%からなる混合溶媒に、LiPF6を1.0mol/Lの濃度で溶解し電解質溶液を調製した。
PANS1又は2を活物質とする負極1〜10、及び、NCMを活物質とする正極を、セパレータ(セルガード社製、商品名:セルガード2325)を挟んでケース内に保持した。その後、先に調製した非水電解質をケース内に注入し、ケースを密閉、封止して、非水電解質二次電池(φ20mm、厚さ3.2mmのコイン型)である電池1〜10を製作した。また、負極1〜10の初回充電時の下位電位の確認を行うため、三極セルキット(東洋システム社製)を用いて、負極1〜10、NCM正極、ガラスフィルターセパレータ、リチウム金属参照極、及び、先に調製した非水電解質から構成された三極セルを作製した。
三極セルを25℃の恒温槽にいれ、充電レート0.1CでNCM正極の電位が4.2V(vs.Li/Li+)になるまで充電し、その際の負極1〜10の電位が表2の値であることを確認した。
また、非水電解質二次電池を25℃の恒温槽に入れ、充電レート0.1Cで負極の充電下限電位が表2の値になるまで充電し、放電レート0.1Cで、電池電圧が0.8Vまで放電する充放電サイクルを50回行った。充放電サイクル10回目のPANS負極重量当たりの放電容量、及び充放電サイクル10回目のPANS負極重量当たりの放電容量に対する50回目の放電容量の比を表2に示す。この比の値が大きいほどサイクル特性に優れることを示す。
Claims (4)
- 硫黄変性ポリアクリロニトリルを活物質とする負極を有する、リチウムイオン二次電池であって、負極の充電下限電位が0.1V(vs.Li/Li+)以上で、1.0V(vs.Li/Li+)未満である、リチウムイオン二次電池。
- 硫黄変性ポリアクリロニトリルの硫黄含有量が、25質量%〜60質量%である請求項1記載のリチウムイオン二次電池。
- 硫黄変性ポリアクリロニトリルを活物質とする負極を有する、リチウムイオン二次電池の作動方法であって、負極の充電下限電位を0.1V(vs.Li/Li+)以上で、1.0V(vs.Li/Li+)未満とする、リチウムイオン二次電池の作動方法。
- 硫黄変性ポリアクリロニトリルの硫黄含有量が、25質量%〜60質量%である請求項3記載のリチウムイオン二次電池の作動方法。
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