JP2019526915A - 多孔質ケイ素材料および導電性ポリマーバインダー電極 - Google Patents
多孔質ケイ素材料および導電性ポリマーバインダー電極 Download PDFInfo
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- 229910021426 porous silicon Inorganic materials 0.000 title claims abstract description 81
- 229920005598 conductive polymer binder Polymers 0.000 title claims abstract description 46
- 239000002210 silicon-based material Substances 0.000 title 1
- 239000002131 composite material Substances 0.000 claims abstract description 57
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910001416 lithium ion Inorganic materials 0.000 claims abstract description 21
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000004519 manufacturing process Methods 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims description 27
- 229910052799 carbon Inorganic materials 0.000 claims description 20
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 19
- 229910052710 silicon Inorganic materials 0.000 claims description 19
- 239000010703 silicon Substances 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 11
- 239000012876 carrier material Substances 0.000 claims description 10
- 239000011241 protective layer Substances 0.000 claims description 8
- 239000002002 slurry Substances 0.000 claims description 8
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- 239000002904 solvent Substances 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 3
- 239000008240 homogeneous mixture Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000002409 silicon-based active material Substances 0.000 claims description 3
- 239000000758 substrate Substances 0.000 claims description 3
- 239000010409 thin film Substances 0.000 claims description 3
- 238000000151 deposition Methods 0.000 claims description 2
- 239000011230 binding agent Substances 0.000 abstract description 13
- CERQOIWHTDAKMF-UHFFFAOYSA-M Methacrylate Chemical compound CC(=C)C([O-])=O CERQOIWHTDAKMF-UHFFFAOYSA-M 0.000 abstract description 3
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 abstract description 2
- 238000006138 lithiation reaction Methods 0.000 description 24
- 239000011149 active material Substances 0.000 description 17
- 239000000463 material Substances 0.000 description 12
- 239000010410 layer Substances 0.000 description 10
- 239000000654 additive Substances 0.000 description 9
- 239000011856 silicon-based particle Substances 0.000 description 9
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- 230000000996 additive effect Effects 0.000 description 7
- 230000001351 cycling effect Effects 0.000 description 7
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- 229910052744 lithium Inorganic materials 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 238000007086 side reaction Methods 0.000 description 6
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 5
- 239000002482 conductive additive Substances 0.000 description 5
- 238000000157 electrochemical-induced impedance spectroscopy Methods 0.000 description 5
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
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- 238000006731 degradation reaction Methods 0.000 description 4
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- SBLRHMKNNHXPHG-UHFFFAOYSA-N 4-fluoro-1,3-dioxolan-2-one Chemical compound FC1COC(=O)O1 SBLRHMKNNHXPHG-UHFFFAOYSA-N 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 description 3
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
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- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 description 2
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- BBEAQIROQSPTKN-UHFFFAOYSA-N pyrene Chemical compound C1=CC=C2C=CC3=CC=CC4=CC=C1C2=C43 BBEAQIROQSPTKN-UHFFFAOYSA-N 0.000 description 2
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- 230000006641 stabilisation Effects 0.000 description 2
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- 229920003048 styrene butadiene rubber Polymers 0.000 description 2
- 229920002153 Hydroxypropyl cellulose Polymers 0.000 description 1
- 229910012851 LiCoO 2 Inorganic materials 0.000 description 1
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- 229920002125 Sokalan® Polymers 0.000 description 1
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- 229920005994 diacetyl cellulose Polymers 0.000 description 1
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- GVEPBJHOBDJJJI-UHFFFAOYSA-N fluoranthrene Natural products C1=CC(C2=CC=CC=C22)=C3C2=CC=CC3=C1 GVEPBJHOBDJJJI-UHFFFAOYSA-N 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000001863 hydroxypropyl cellulose Substances 0.000 description 1
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- 238000002847 impedance measurement Methods 0.000 description 1
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- 238000010902 jet-milling Methods 0.000 description 1
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- 239000007788 liquid Substances 0.000 description 1
- 229910000625 lithium cobalt oxide Inorganic materials 0.000 description 1
- 229910021450 lithium metal oxide Inorganic materials 0.000 description 1
- BFZPBUKRYWOWDV-UHFFFAOYSA-N lithium;oxido(oxo)cobalt Chemical compound [Li+].[O-][Co]=O BFZPBUKRYWOWDV-UHFFFAOYSA-N 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
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Classifications
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/621—Binders
- H01M4/622—Binders being polymers
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- 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
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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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- 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
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- H01M4/04—Processes of manufacture in general
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- H01M4/00—Electrodes
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- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/133—Electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- 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
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Abstract
Description
本明細書に記述されかつ特許請求の範囲に記載される本発明は、一部、契約No.DE−AC02−05CH11231の下、米国エネルギー省によって供給された資金を利用して行われた。政府は、本発明において、ある一定の権利を有する。
電極組成物:
全ての電極積層体は、導電性ポリマーバインダーおよびケイ素活性材料でできている。多孔質Siは市販されており、VestaSiおよび他の供給源から入手することができる。ミクロサイズの非多孔質Siは市販されており、Alfa Aesarから入手することができる。ピレン系導電性バインダーは、米国特許第9,153,353号に記載されているように合成した。
全ての電極積層体を、ミツトヨのドクターブレードおよびヨシミツ精機の真空ドローダウン・コータを使用して、活物質を単位面積当たりほぼ同じ負荷まで、20μmの厚さの電池・グレードのCuシート上に流延した。被膜および積層体を、溶媒のほとんどが蒸発しかつ乾燥したように見えるまで、最初に赤外線ランプの下で1時間乾燥した。被膜および積層体を、10−2torrの動的真空の下で24時間、130℃でさらに乾燥した。被膜および積層体の厚さを、精度が±1μmのミツトヨ・マイクロメータで測定した。4.8mAh/com2までのいくつかの負荷および厚さを行い、電極も、連続的に調節可能な隙間を備えたInternationalRollingMill製のカレンダ機を使用して加圧し、および非加圧状態にした。
コインセルの組立ては、標準の2325コインセル・ハードウェアを使用して行った。1.47cmの直径のディスクを積層体から打ち抜いて、作用電極としてコインセル・アセンブリに使用した。リチウム箔(FMCコーポレーションから得られた)を、対電極を作製するのに使用した。対電極を、1.5cmの直径のディスクに切断した。作用電極を、コインセル・アセンブリの外殻の中心に配置し、2滴の30%FEC、1.2MLiPF6をBASFから購入したEC/DEC=3/7電解質に溶かしたものを添加して、電極を濡らした。直径2cmのCelgard2400多孔質ポリエチレン・セパレータを、作用電極の最上部に配置した。さらに3滴の電解質を、セパレータに添加した。対電極を、セパレータの最上部に配置した。作用電極の上方に対称的に対電極を位置合わせするのに、特に注意を払った。ステンレス鋼スペーサおよびBellevilleバネを、対電極の最上部に配置した。プラスチック・グロメットを、電極アセンブリの外縁の最上部に配置し、カナダのNationalResearchCouncilにより製造された特注の圧着機で密接に圧着した。セル製作手順の全体は、Ar雰囲気グローブ・ボックス内で行った。
コインセル性能を、MaccorSeries4000電池試験システムにより、30℃の熱チャンバ内で評価した。一定の充電容量サイクリングでは、コインセルを、計算された特定の容量に該当するある程度まで最初にリチウム化し、次いで元の1Vまで脱リチウム化した。より低いカットオフ電圧は、10mVに設定された。材料の容量を、理論容量、および電極内で使用される材料の量に基づいて計算した。
Claims (25)
- 比容量が500から2200mAh/gの間である多孔質ケイ素と導電性ポリマーバインダーとを含み、導電性ポリマーバインダーが下記式の繰り返し単位を有するポリマー組成物からなる群から選択される:
リチウムイオン電池に使用される複合電極。 - 前記m/n比が7/3である、請求項1に記載の複合電極。
- 前記導電性ポリマーバインダーが、約1〜20質量%までの量で存在する、請求項1に記載の複合電極。
- 前記導電性ポリマーバインダーが、約5〜12質量%の量で存在する、請求項1に記載の複合電極。
- 前記導電性ポリマーバインダーが、約5質量%の量で存在する、請求項1に記載の複合電極。
- 前記電極が、約80〜約99質量%の多孔質ケイ素からなる、請求項1に記載の複合電極。
- 前記電極が、約0.5〜5質量%の導電性炭素をさらに含む、請求項1に記載の複合電極。
- 前記多孔質ケイ素が保護層で被覆されている、請求項1に記載の複合電極。
- 前記多孔質ケイ素が導電性キャリア材料上に堆積されている、請求項1に記載の複合電極。
- 前記多孔質ケイ素が導電性キャリア材料上に堆積され、保護層で被覆されている、請求項1に記載の複合電極。
- 前記多孔質ケイ素が導電性キャリア材料上に堆積され、保護層で被覆されており、前記多孔質ケイ素の空隙に対するケイ素の体積比が1:1である、請求項1に記載の複合電極。
- 前記多孔質ケイ素が、約10〜99質量%のSiおよび約1〜90質量%のCを含む、請求項1に記載の複合電極。
- リチウムイオン電池に使用するための複合電極を製造する方法であって、
溶媒および導電性ポリマーバインダーとの溶液を形成するステップ;
この溶液に多孔質ケイ素活物質を添加してスラリーを形成するステップ;
スラリーを混合して均質混合物を形成するステップ;
このようにして得られた混合物の薄膜を基板の上に堆積させるステップ;そして
得られた複合体を乾燥して前記電極を形成するステップ、
を含む、前記製造方法。 - 導電性ポリマーバインダーが、以下の式の繰り返し単位を有するポリマー組成物からなる群から選択される:
請求項13に記載の方法。 - 前記m/n比が7/3である、請求項14に記載の方法。
- 前記導電性ポリマーバインダーが、約1〜20質量%までの量で存在する、請求項13に記載の方法。
- 前記導電性ポリマーバインダーが、約5〜12質量%の量で存在する、請求項13に記載の方法。
- 前記導電性ポリマーバインダーが、約5質量%の量で存在する、請求項13に記載の方法。
- 前記電極が、約80〜99質量%の多孔質ケイ素からなる、請求項13に記載の方法。
- 前記電極が、約0.5〜5質量%の導電性炭素をさらに含む、請求項13に記載の方法。
- 前記多孔質ケイ素が保護層で被覆されている、請求項13に記載の方法。
- 前記多孔質ケイ素が導電性キャリア材料上に堆積されている、請求項13に記載の方法。
- 前記多孔質ケイ素が導電性キャリア材料上に堆積され、保護層で被覆されている、請求項13に記載の方法。
- 前記多孔質ケイ素が導電性キャリア材料上に堆積され、保護層で被覆されており、前記多孔質ケイ素の空隙に対するケイ素の体積比が1:1である、請求項13に記載の方法。
- 前記多孔質ケイ素が、約10〜99質量%のSiおよび約1〜90質量%のCを含む、請求項13に記載の方法。
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PCT/EP2017/071864 WO2018046385A1 (en) | 2016-09-09 | 2017-08-31 | Porous silicon materials and conductive polymer binder electrodes |
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WO2023002756A1 (ja) * | 2021-07-20 | 2023-01-26 | パナソニックIpマネジメント株式会社 | 負極活物質および電池 |
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US10403897B2 (en) | 2017-05-19 | 2019-09-03 | Bayerische Motoren Werke Aktiengesellschaft | Conductive polymer binder for a novel silicon/graphene anode in lithium ion batteries |
CN109148886B (zh) * | 2018-08-28 | 2021-06-11 | 合肥国轩高科动力能源有限公司 | 粘结剂及其制备方法、锂离子电池负极片 |
US11205778B2 (en) | 2019-06-12 | 2021-12-21 | The Regents Of The University Of California | Conductive polymer emulsion |
CN111769285B (zh) * | 2020-07-01 | 2022-04-01 | 苏州凌威新能源科技有限公司 | 锂电池负极胶粘剂及负极片 |
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