JP5792975B2 - リチウムのプリドープ方法 - Google Patents
リチウムのプリドープ方法 Download PDFInfo
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- JP5792975B2 JP5792975B2 JP2011070772A JP2011070772A JP5792975B2 JP 5792975 B2 JP5792975 B2 JP 5792975B2 JP 2011070772 A JP2011070772 A JP 2011070772A JP 2011070772 A JP2011070772 A JP 2011070772A JP 5792975 B2 JP5792975 B2 JP 5792975B2
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- 229910052744 lithium Inorganic materials 0.000 title claims description 155
- 238000000034 method Methods 0.000 title claims description 69
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims description 67
- 239000000463 material Substances 0.000 claims description 103
- 239000002904 solvent Substances 0.000 claims description 81
- 238000004898 kneading Methods 0.000 claims description 70
- 238000002156 mixing Methods 0.000 claims description 67
- 239000012530 fluid Substances 0.000 claims description 5
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims 1
- 229910000077 silane Inorganic materials 0.000 claims 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 22
- 229910001416 lithium ion Inorganic materials 0.000 description 22
- 239000000203 mixture Substances 0.000 description 22
- 238000003860 storage Methods 0.000 description 22
- 238000004519 manufacturing process Methods 0.000 description 19
- 239000011888 foil Substances 0.000 description 17
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 16
- 239000002002 slurry Substances 0.000 description 16
- 238000006243 chemical reaction Methods 0.000 description 15
- 239000003990 capacitor Substances 0.000 description 14
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- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 9
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- -1 alkyl lithium Chemical compound 0.000 description 6
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- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 229920003026 Acene Polymers 0.000 description 4
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 description 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- 238000009835 boiling Methods 0.000 description 4
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- 238000000576 coating method Methods 0.000 description 4
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- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 description 4
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
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- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical class O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 0.000 description 3
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- 229910000838 Al alloy Inorganic materials 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 229910012851 LiCoO 2 Inorganic materials 0.000 description 2
- MZRVEZGGRBJDDB-UHFFFAOYSA-N N-Butyllithium Chemical compound [Li]CCCC MZRVEZGGRBJDDB-UHFFFAOYSA-N 0.000 description 2
- JFBZPFYRPYOZCQ-UHFFFAOYSA-N [Li].[Al] Chemical compound [Li].[Al] JFBZPFYRPYOZCQ-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 239000011324 bead Substances 0.000 description 2
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- 239000011889 copper foil Substances 0.000 description 2
- 150000005676 cyclic carbonates Chemical class 0.000 description 2
- NNBZCPXTIHJBJL-UHFFFAOYSA-N decalin Chemical compound C1CCCC2CCCCC21 NNBZCPXTIHJBJL-UHFFFAOYSA-N 0.000 description 2
- SBZXBUIDTXKZTM-UHFFFAOYSA-N diglyme Chemical compound COCCOCCOC SBZXBUIDTXKZTM-UHFFFAOYSA-N 0.000 description 2
- 230000008034 disappearance Effects 0.000 description 2
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 description 2
- SNRUBQQJIBEYMU-UHFFFAOYSA-N dodecane Chemical compound CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 2
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- 239000011261 inert gas Substances 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
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- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 2
- TZIHFWKZFHZASV-UHFFFAOYSA-N methyl formate Chemical compound COC=O TZIHFWKZFHZASV-UHFFFAOYSA-N 0.000 description 2
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- BQCIDUSAKPWEOX-UHFFFAOYSA-N 1,1-Difluoroethene Chemical compound FC(F)=C BQCIDUSAKPWEOX-UHFFFAOYSA-N 0.000 description 1
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 description 1
- 238000004438 BET method Methods 0.000 description 1
- HGVAXMJKHJAZGW-UHFFFAOYSA-N CC=C.F.F.F.F.F.F.F Chemical group CC=C.F.F.F.F.F.F.F HGVAXMJKHJAZGW-UHFFFAOYSA-N 0.000 description 1
- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 description 1
- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 description 1
- MBMLMWLHJBBADN-UHFFFAOYSA-N Ferrous sulfide Chemical compound [Fe]=S MBMLMWLHJBBADN-UHFFFAOYSA-N 0.000 description 1
- 229910004764 HSV900 Inorganic materials 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229920006370 Kynar Polymers 0.000 description 1
- 229910000733 Li alloy Inorganic materials 0.000 description 1
- 229910015643 LiMn 2 O 4 Inorganic materials 0.000 description 1
- 241000512299 Nerita Species 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- KXKVLQRXCPHEJC-UHFFFAOYSA-N acetic acid trimethyl ester Natural products COC(C)=O KXKVLQRXCPHEJC-UHFFFAOYSA-N 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 239000003125 aqueous solvent Substances 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 150000005678 chain carbonates Chemical class 0.000 description 1
- 239000011315 coal-based isotropic pitch Substances 0.000 description 1
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- 230000018109 developmental process Effects 0.000 description 1
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
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- 150000002148 esters Chemical class 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 229920001973 fluoroelastomer Polymers 0.000 description 1
- 239000011245 gel electrolyte Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000012770 industrial material Substances 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
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- 238000009830 intercalation Methods 0.000 description 1
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- 239000001989 lithium alloy Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 1
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 239000011255 nonaqueous electrolyte Substances 0.000 description 1
- 239000005486 organic electrolyte Substances 0.000 description 1
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- 125000003367 polycyclic group Chemical group 0.000 description 1
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- PXXNTAGJWPJAGM-UHFFFAOYSA-N vertaline Natural products C1C2C=3C=C(OC)C(OC)=CC=3OC(C=C3)=CC=C3CCC(=O)OC1CC1N2CCCC1 PXXNTAGJWPJAGM-UHFFFAOYSA-N 0.000 description 1
Classifications
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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
- 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
-
- 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
- Y02E60/13—Energy storage using capacitors
Landscapes
- Electric Double-Layer Capacitors Or The Like (AREA)
- Battery Electrode And Active Subsutance (AREA)
Description
また、電極内にリチウム金属粉末を混合する、あるいは、特許文献7に記載されているようにリチウム金属粉末を負極上に均一に分散させ、注液後、電極上で局部電池を構成し電極内に均一に吸蔵する方法が開示されている。更に、特許文献8には、負極中にポリマー被覆Li微粒子を混合し負極を製造し、キャパシタを組み立て後、電解液を含浸させることにより、ポリマー被覆Li微粒子のうちポリマー部分を電解液に溶出させ、Li金属と負極のカーボンを導通(短絡)させることにより負極のカーボン中にLiをドープさせる方法も開示されている。
すなわち本発明は、以下の構成からなることを特徴とし、上記課題を解決するものである。
(2)前記リチウムドープ可能材料とリチウム金属を溶剤の存在下において混練混合する工程において、リチウム金属を複数回にわたって加えることを特徴とする前記(1)に記載のリチウムのプリドープ方法。
(多環芳香族系炭化水素:PAHsの合成)
石炭系等方性ピッチ(軟化点280℃)を、コーヒーミルで粉砕し、粒度1mm以下のピッチ原料を得た。該ピッチ粉末1000gをステンレス鋼製の皿に入れ、電気炉(炉内有効寸法300mm×300mm×300mm)内に設置して、熱反応を行った。熱反応は、窒素雰囲気下で行い、窒素流量を10リットル/分とした。熱反応に際しては、室温から100℃/時間の速度で680℃(炉内温)まで昇温した後、この温度で4時間保持し、続いて自然冷却により、60℃まで冷却し、反応生成物を電気炉から取り出した。得られた生成物は、原料の形状を留めず、不定形な不溶不融性固体であった。収量は790gであり、収率は79重量%であった。
上記PAHs、アセチレンブラックを170℃で10時間真空乾燥した後、水分100ppm以下のドライエアー中で、PAHs5g、アセチレンブラック0.5gを混合し、水分30ppm以下のプロピレンカーボネート(沸点242℃)5.0gを加え、自公転ミキサー(シンキー製:あわとり練太郎AR−250:容器100ml)を用いて混練混合した。得られた高粘度混合物(流動性なし)に30μmのリチウム金属箔をカットしたものを約0.07g加え、自公転ミキサーを用いて自転速度2000rpm、公転速度2000rpmの条件で2分間、混練混合した。その後、リチウム金属の消失を確認しながら、リチウム金属箔を約0.07gずつ加え、上記条件で2分間混練混合する操作を繰り返し、総計0.5gの所定量のリチウム金属(PAHsの重量に対し380mAh/gに相当)を混練混合した。
実施例1に記載のPAHs、アセチレンブラックを170℃で10時間真空乾燥した後、水分100ppm以下のドライエアー中で、PAHs5g、アセチレンブラック0.5gを混合し、水分30ppm以下のプロピレンカーボネート(沸点242℃)7.7gを加え、自公転ミキサー(シンキー製:あわとり練太郎AR−250:容器100ml)を用いて混練混合した。容器にジルコニア製ボール(10mmφ)2個を入れ、得られた流動性のある混合物に30μmのリチウム金属箔をカットしたものを約0.07g加え、400G以上の遠心力で混練混合可能な上記自公転ミキサーを用いて自転速度2000rpm、公転速度2000rpmの条件で2分間、混練混合した。リチウム金属の消失を確認しながら、次のリチウム金属箔を約0.07gずつ加え、上記条件で2分間混練混合する操作を繰り返し、総計0.5gのリチウム金属(PAHsの重量に対し380mAh/gに相当)を混練混合した。この混練混合時の温度は40℃程度であり、著しい発熱は見られなかった。終了後、加えたリチウム金属箔はほぼ完全に消失していた。本実施例ではリチウムの小片がごく微量残る状態であったが、380mAh/gという実用的プリドープ量を短時間でプリドープ可能であった。
Claims (2)
- リチウムをリチウムドープ可能材料にプリドープする方法であって、リチウムドープ可能材料とリチウム金属を溶剤の存在下において混練混合することによりリチウムをリチウムドープ可能材料にプリドープする工程を含み、前記リチウムドープ可能材料とリチウム金属を溶剤の存在下において混練混合する工程において、粘度の高い流動性のない状態で、ボールとの衝突、摩擦なしに混練混合する工程の後、粘度の高い流動性のない状態又は溶剤を添加し粘度を低下させた流動性のある状態で、ボールとの衝突、摩擦による混練混合する工程を含むことを特徴とするリチウムのプリドープ方法。
- 前記リチウムドープ可能材料とリチウム金属を溶剤の存在下において混練混合する工程において、リチウム金属を複数回にわたって加えることを特徴とする請求項1に記載のリチウムのプリドープ方法。
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JP5792975B2 true JP5792975B2 (ja) | 2015-10-14 |
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Families Citing this family (11)
Publication number | Priority date | Publication date | Assignee | Title |
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JP5760593B2 (ja) * | 2011-03-30 | 2015-08-12 | Tdk株式会社 | 活物質の製造方法、電極及びリチウムイオン二次電池 |
PL3043412T3 (pl) | 2013-09-02 | 2021-02-08 | Mitsubishi Gas Chemical Company, Inc. | Bateria z elektrolitem stałym i sposób wytwarzania materiału aktywnego elektrody |
WO2016073438A1 (en) * | 2014-11-03 | 2016-05-12 | 24M Technologies, Inc. | Pre-lithiation of electrode materials in a semi-solid electrode |
US10580592B2 (en) | 2015-09-28 | 2020-03-03 | Jsr Corporation | Method for manufacturing electrode material, cell, and capacitor; and device for manufacturing electrode material |
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