JP2010538424A - リチウムイオン用途のための安定化リチウム金属粉末、組成物および製造方法 - Google Patents
リチウムイオン用途のための安定化リチウム金属粉末、組成物および製造方法 Download PDFInfo
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- JP2010538424A JP2010538424A JP2010522937A JP2010522937A JP2010538424A JP 2010538424 A JP2010538424 A JP 2010538424A JP 2010522937 A JP2010522937 A JP 2010522937A JP 2010522937 A JP2010522937 A JP 2010522937A JP 2010538424 A JP2010538424 A JP 2010538424A
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- 239000000843 powder Substances 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims description 14
- 239000000203 mixture Substances 0.000 title description 16
- 229910001416 lithium ion Inorganic materials 0.000 title description 12
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title description 11
- 238000004519 manufacturing process Methods 0.000 title description 4
- 229920000642 polymer Polymers 0.000 claims abstract description 47
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 70
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- 238000002844 melting Methods 0.000 claims description 7
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- 229920000468 styrene butadiene styrene block copolymer Polymers 0.000 claims description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000010439 graphite Substances 0.000 claims description 2
- 229910002804 graphite Inorganic materials 0.000 claims description 2
- 229910021450 lithium metal oxide Inorganic materials 0.000 claims description 2
- 239000000463 material Substances 0.000 claims 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims 1
- 229910001128 Sn alloy Inorganic materials 0.000 claims 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims 1
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- 229910052718 tin Inorganic materials 0.000 claims 1
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- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims 1
- 229910001887 tin oxide Inorganic materials 0.000 claims 1
- 229910000314 transition metal oxide Inorganic materials 0.000 claims 1
- 238000002161 passivation Methods 0.000 abstract description 2
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- 238000003860 storage Methods 0.000 description 20
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 18
- 239000002904 solvent Substances 0.000 description 17
- 239000002245 particle Substances 0.000 description 15
- 238000003756 stirring Methods 0.000 description 11
- 229910052786 argon Inorganic materials 0.000 description 10
- 238000000576 coating method Methods 0.000 description 10
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- 229910000856 hastalloy Inorganic materials 0.000 description 7
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- 238000012360 testing method Methods 0.000 description 5
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- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 3
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- 238000013019 agitation Methods 0.000 description 3
- 210000004027 cell Anatomy 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
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- 238000001816 cooling Methods 0.000 description 3
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 3
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
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- 238000012546 transfer Methods 0.000 description 3
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical compound C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 2
- 229910018871 CoO 2 Inorganic materials 0.000 description 2
- 229910012851 LiCoO 2 Inorganic materials 0.000 description 2
- 229910013290 LiNiO 2 Inorganic materials 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- 239000012300 argon atmosphere Substances 0.000 description 2
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- 239000012467 final product Substances 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 239000013529 heat transfer fluid Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000012454 non-polar solvent Substances 0.000 description 2
- 239000002798 polar solvent Substances 0.000 description 2
- 229920002959 polymer blend Polymers 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 229920004943 Delrin® Polymers 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229910018119 Li 3 PO 4 Inorganic materials 0.000 description 1
- 229910010093 LiAlO Inorganic materials 0.000 description 1
- 229910013641 LiNbO 3 Inorganic materials 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 229910006404 SnO 2 Inorganic materials 0.000 description 1
- 229920002125 Sokalan® Polymers 0.000 description 1
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 1
- GEIAQOFPUVMAGM-UHFFFAOYSA-N ZrO Inorganic materials [Zr]=O GEIAQOFPUVMAGM-UHFFFAOYSA-N 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
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- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Inorganic materials [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 231100000989 no adverse effect Toxicity 0.000 description 1
- 125000002524 organometallic group Chemical group 0.000 description 1
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
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- 238000003786 synthesis reaction Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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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
- 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
- H01M4/134—Electrodes based on metals, Si or alloys
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/102—Metallic powder coated with organic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/16—Metallic particles coated with a non-metal
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
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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
- 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
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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
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
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- H—ELECTRICITY
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/381—Alkaline or alkaline earth metals elements
- H01M4/382—Lithium
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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
Abstract
Description
本出願は、2007年8月31日に出願された米国仮出願第60/969,267号の利益を主張し、その内容全体が引用することにより本明細書に組み入れられる:。
電池グレードのリチウム金属(405g)を2×2インチの断片に切断し、一定流量の乾燥アルゴン下、室温で、固定高速撹拌機モータに接続された撹拌シャフトが取り付けられた4インチの上部を有する3リットルのステンレス鋼フラスコ反応器に投入した。反応器に上部マントルヒーターおよび底部マントルヒーターを取り付けた。次に反応器を組み立て、1041.4gのペネテック(Penetek)(商標)油(ペンレコ(Penreco))、ペンゾイル・プロダクツ・カンパニー(Penzoil Products Company)の一部門)を加えた。次に反応器を約200℃まで加熱し、250rpm〜800rpmの範囲内の穏やかな撹拌を維持することですべての金属を溶融させ、アルゴン流を加熱ステップ全体にわたって維持した。次に混合物を高速(最高10,000rpm)で2分間撹拌した。オレイン酸8.1gを反応器中に投入し、さらに3分間高速撹拌した後、5.1gのCO2を加えた。次に高速撹拌を停止し、マントルヒーターを取り外し、分散体を約50℃まで冷却し、貯蔵瓶に移した。さらに、アルゴン気流下、密閉した焼結ガラスフィルタ漏斗中で、リチウム分散体を濾過し、ヘキサンで3回洗浄し、n−ペンタンで1回洗浄して、炭化水素油媒体を除去した。漏斗をヒートガンで加熱して微量の溶媒を除去し、得られた易流動性粉末を蓋がきつく閉まる貯蔵瓶に移した。
アルゴン雰囲気下、室温で、ペネテック(商標)鉱油(4449g)および1724gの電池グレードのリチウム金属を15リットルのジャケット付き分散反応器に加えた。次に、ジャケット内に高温の伝熱流体を圧送することによって、反応器を室温から200℃まで加熱した。加熱中、伝熱を促進するため、分散撹拌機を低速に維持した。反応器内部の温度が200℃に達した後、分散撹拌機速度を5000rpmまで増加させた。3.5分間の高速撹拌の後、36gのオレイン酸を反応器中に投入し、高速撹拌をさらに4.5分間続けた後、22gのCO2ガスを加えた。さらに4分間の高速撹拌の後、高速撹拌機を停止し、反応器の内容物を室温まで冷却した。この冷却プロセス中、低速撹拌を使用して懸濁液中での分散を維持した。アルゴン圧力下でリチウム分散体をバッチフィルタに移し、鉱油を流出させた。フィルタ中の分散体をヘキサンで4回洗浄し、続いて乾燥アルゴンをフィルタを通過するように吹き付けて、残留する揮発性有機物を除去した。乾燥した安定化ポリマーコーティングリチウム分散体を最終生成物としてフィルタから取り出した。
Claims (9)
- 実質的に連続なポリマー層でコーティングされた安定化リチウム金属粉末であって、前記ポリマーが、ポリウレタン、ポリテトラフルオロエチレン、ポリフッ化ビニル、ポリ塩化ビニル、ポリスチレン、ポリエチレン、ポリプロピレン、ポリホルムアルデヒド、スチレン−ブタジエン−スチレンブロックポリマー、エチレン酢酸ビニル、エチレンアクリル酸コポリマー、ポリエチレンオキシド、ポリイミド、ポリチオフェン、ポリ(パラ−フェニレン)、ポリアニリン、ポリ(p−フェニレンビニレン)、シリカチタニア系コポリマー、不飽和ポリカルボン酸、およびポリシロキサンからなる群より選択される、安定化リチウム金属粉末。
- 前記実質的に連続なポリマー層が、25〜200nmの厚さを有する請求項1に記載の安定化リチウム金属粉末。
- 無機コーティング層をさらに含む請求項2に記載の安定化リチウム金属粉末。
- 電気化学系内でリチウム吸収または脱着が可能なホスト材料を含むアノードであって、請求項3に記載のポリマーがコーティングされ安定化されたリチウム金属粉末が前記ホスト材料中に分散しているアノード。
- 前記ホスト材料が、炭素質材料、ケイ素、スズ、酸化スズ、複合スズ合金、遷移金属酸化物、リチウム金属窒化物、黒鉛、カーボンブラック、およびリチウム金属酸化物からなる群より選択される少なくとも1種類の材料を含む請求項4に記載のアノード。
- 前記実質的に連続なポリマー層が、25〜200nmの厚さを有する請求項5に記載のアノード。
- 25〜200nmの厚さを有する実質的に連続なポリマー層がコーティングされた安定化リチウム金属粉末。
- 電気化学系内でリチウムの吸収または脱着が可能なホスト材料を含むアノードであって、請求項7に記載のポリマーがコーティングされ安定化されたリチウム金属粉末が前記ホスト材料中に分散しているアノード。
- a)リチウム金属を炭化水素油と接触させるステップと、
b)前記リチウム金属および炭化水素油を前記リチウム金属の融点よりも高温に加熱するステップと、
c)前記加熱されたリチウム金属および炭化水素油を、前記リチウム金属を前記油中に分散させるのに十分な条件にさらすステップと、
d)前記リチウム金属上に実質的に連続なポリマー層を設けるために、前記リチウム金属を、ポリウレタン、ポリテトラフルオロエチレン、ポリフッ化ビニル、ポリ塩化ビニル、ポリスチレン、ポリエチレン、ポリプロピレン、(ポリホルムアルデヒド)、スチレン−ブタジエン−スチレンブロックポリマー、エチレン酢酸ビニル、エチレンアクリル酸コポリマー、ポリエチレンオキシド、ポリイミド、ポリチオフェン、ポリ(パラ−フェニレン)、ポリアニリン、ポリ(p−フェニレンビニレン)、シリカチタニア系コポリマー、不飽和ポリカルボン酸、およびポリシロキサンからなる群より選択されるポリマーと、前記リチウム金属の融点と前記ポリマーの融点との間の温度で接触させるステップと
を含む、リチウム分散体の形成方法。
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US20170149052A1 (en) | 2017-05-25 |
CN101790806A (zh) | 2010-07-28 |
DE112008002212T5 (de) | 2010-07-08 |
GB2490433A (en) | 2012-10-31 |
US11171323B2 (en) | 2021-11-09 |
GB201211010D0 (en) | 2012-08-01 |
RU2010112410A (ru) | 2011-10-10 |
CA2696771A1 (en) | 2009-03-05 |
JP6001596B2 (ja) | 2016-10-05 |
EP2463940A1 (en) | 2012-06-13 |
US20180261829A1 (en) | 2018-09-13 |
JP2014167936A (ja) | 2014-09-11 |
GB201000554D0 (en) | 2010-03-03 |
GB2490433B (en) | 2013-02-27 |
GB2463217A (en) | 2010-03-10 |
GB2463217B (en) | 2013-02-13 |
KR20100081304A (ko) | 2010-07-14 |
EP2186151A1 (en) | 2010-05-19 |
JP5548126B2 (ja) | 2014-07-16 |
WO2009029270A1 (en) | 2009-03-05 |
US20090061321A1 (en) | 2009-03-05 |
CA2696771C (en) | 2016-05-24 |
CN105618735A (zh) | 2016-06-01 |
EP2463940B1 (en) | 2014-07-02 |
EP2186151B1 (en) | 2013-12-04 |
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