JP2023506269A - リチウム補充材料及びその製造方法、負極、並びにリチウムイオン電池 - Google Patents
リチウム補充材料及びその製造方法、負極、並びにリチウムイオン電池 Download PDFInfo
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- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 338
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 318
- 239000000463 material Substances 0.000 title claims abstract description 99
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 42
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 9
- 239000002245 particle Substances 0.000 claims abstract description 150
- 239000004020 conductor Substances 0.000 claims abstract description 73
- 238000000034 method Methods 0.000 claims abstract description 24
- 239000007773 negative electrode material Substances 0.000 claims abstract description 24
- 239000006185 dispersion Substances 0.000 claims description 98
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 58
- 239000002048 multi walled nanotube Substances 0.000 claims description 52
- 239000002041 carbon nanotube Substances 0.000 claims description 41
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 41
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 41
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 41
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 36
- 229920002545 silicone oil Polymers 0.000 claims description 36
- 238000002161 passivation Methods 0.000 claims description 30
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 20
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 20
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 20
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 18
- 239000001569 carbon dioxide Substances 0.000 claims description 18
- 238000001816 cooling Methods 0.000 claims description 16
- 239000003575 carbonaceous material Substances 0.000 claims description 14
- 239000004094 surface-active agent Substances 0.000 claims description 12
- 229910021389 graphene Inorganic materials 0.000 claims description 10
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 9
- 239000004917 carbon fiber Substances 0.000 claims description 9
- 239000002109 single walled nanotube Substances 0.000 claims description 9
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 claims description 8
- 239000002612 dispersion medium Substances 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 5
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 4
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 4
- 229930195733 hydrocarbon Natural products 0.000 claims description 4
- 150000002430 hydrocarbons Chemical class 0.000 claims description 4
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 4
- 239000004215 Carbon black (E152) Substances 0.000 claims description 3
- 150000002148 esters Chemical class 0.000 claims description 3
- 150000002170 ethers Chemical class 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 238000002844 melting Methods 0.000 claims description 3
- 230000008018 melting Effects 0.000 claims description 3
- 239000003960 organic solvent Substances 0.000 claims description 3
- 239000012188 paraffin wax Substances 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 abstract description 32
- 239000002184 metal Substances 0.000 abstract description 32
- 230000015572 biosynthetic process Effects 0.000 abstract description 9
- 230000008569 process Effects 0.000 abstract description 9
- 210000001787 dendrite Anatomy 0.000 abstract description 7
- 238000010521 absorption reaction Methods 0.000 abstract description 6
- 230000000149 penetrating effect Effects 0.000 abstract description 2
- 238000003756 stirring Methods 0.000 description 44
- 239000002923 metal particle Substances 0.000 description 19
- 239000007789 gas Substances 0.000 description 17
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 16
- 238000010438 heat treatment Methods 0.000 description 16
- 238000009775 high-speed stirring Methods 0.000 description 16
- 239000012265 solid product Substances 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 14
- 238000001514 detection method Methods 0.000 description 14
- 239000000203 mixture Substances 0.000 description 12
- 229910002804 graphite Inorganic materials 0.000 description 5
- 239000010439 graphite Substances 0.000 description 5
- 239000011230 binding agent Substances 0.000 description 4
- 239000003921 oil Substances 0.000 description 4
- 230000009469 supplementation Effects 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 239000011149 active material Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000011267 electrode slurry Substances 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 239000011888 foil Substances 0.000 description 3
- 230000035515 penetration Effects 0.000 description 3
- 230000005501 phase interface Effects 0.000 description 3
- 238000003825 pressing Methods 0.000 description 3
- 239000007790 solid phase Substances 0.000 description 3
- 230000032258 transport Effects 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- UBAZGMLMVVQSCD-UHFFFAOYSA-N carbon dioxide;molecular oxygen Chemical compound O=O.O=C=O UBAZGMLMVVQSCD-UHFFFAOYSA-N 0.000 description 2
- 239000006258 conductive agent Substances 0.000 description 2
- 239000011889 copper foil Substances 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 230000037427 ion transport Effects 0.000 description 2
- 230000002427 irreversible effect Effects 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 241000872198 Serjania polyphylla Species 0.000 description 1
- 239000006230 acetylene black Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 210000004027 cell Anatomy 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000008094 contradictory effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000003137 locomotive effect Effects 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- 239000006250 one-dimensional material Substances 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 239000005486 organic electrolyte Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000007784 solid electrolyte Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
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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
- H01M4/36—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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- 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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- H01M10/058—Construction or manufacture
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- 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
- H01M10/446—Initial charging measures
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- H01M4/0404—Methods of deposition of the material by coating on electrode collectors
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- H01M4/04—Processes of manufacture in general
- H01M4/0438—Processes of manufacture in general by electrochemical processing
- H01M4/044—Activating, forming or electrochemical attack of the supporting material
- H01M4/0445—Forming after manufacture of the electrode, e.g. first charge, cycling
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Abstract
Description
好ましくは、前記炭素材料は、カーボンナノチューブであり、前記カーボンナノチューブは、単層カーボンナノチューブ及び/又は多層カーボンナノチューブであり、好ましくは、多層カーボンナノチューブであり、及び/又は、前記カーボンナノチューブは、チューブ径が5nm~100nmであり、好ましくは、10nm~30nmであり、長さが10μm~80μmであり、好ましくは、30μm~50μmである。
前記金属リチウム粒子の表面には、不動態化層があり、前記不動態化層の厚さは、5nm~100nmであり、前記不動態化層は、炭酸リチウム、フッ化リチウム、及びパラフィンのうちの少なくとも1つを含む。
S2では、前記混合後の材料を金属リチウムが凝固するまで冷却し、固液分離を行う。
前記第1の分散液は、界面活性剤をさらに含み、前記界面活性剤は、ポリビニルピロリドン、ドデシルベンゼンスルホン酸ナトリウム、及びセチルトリメチルアンモニウムブロミドから選択された少なくとも1つであり、好ましくは、ポリビニルピロリドンであり、前記金属リチウムと前記界面活性剤との重量比は、1:(0.002~0.05)であり、好ましくは、1:(0.005~0.02)であり、及び/又は、
前記第1の分散液及び前記第2の分散液の分散媒は、不活性有機溶媒であり、前記第1の分散液及び前記第2の分散液の分散媒は、それぞれ独立して、炭化水素、エステル、エーテル、及びシリコーンオイルから選択された少なくとも1つであり、及び/又は、
前記第1の分散液と前記第2の分散液との体積比は、1:(0.1~10)であり、好ましくは、1:(0.5~3)であり、前記金属リチウムと前記導電材料との重量比は、100:(0.1~3)であり、好ましくは、100:(0.5~1)である。
S2では、上記混合後の材料を金属リチウムが凝固するまで冷却し、固液分離を行う。
(比較例1)
(比較例2)
(比較例3)
(試験例)
Claims (15)
- 金属リチウム粒子及び導電材料を含むリチウム補充材料であって、
前記導電材料は、前記金属リチウム粒子に埋め込まれた内蔵部分、及び、前記金属リチウム粒子の外部に位置する露出部分を含み、前記導電材料の電子伝導度は、100S/cmよりも大きいことを特徴とする、リチウム補充材料。 - 前記導電材料は、炭素材料であり、前記炭素材料は、カーボンナノチューブ、炭素繊維、及びグラフェンから選択された少なくとも1つであり、好ましくは、前記炭素材料は、カーボンナノチューブであり、前記カーボンナノチューブは、単層カーボンナノチューブ、及び/又は、多層カーボンナノチューブであり、好ましくは、多層カーボンナノチューブである、請求項1に記載のリチウム補充材料。
- 前記カーボンナノチューブは、チューブ径が5nm~100nmであり、好ましくは、10nm~30nmであり、前記カーボンナノチューブは、長さが10μm~80μmであり、好ましくは、30μm~50μmである、請求項2に記載のリチウム補充材料。
- 100重量部の前記金属リチウム粒子に対して、前記導電材料の含有量は、0.1~3重量部であり、好ましくは、0.5~1重量部である、請求項1に記載のリチウム補充材料。
- 前記金属リチウム粒子の平均粒径は、20μm~40μmである、請求項1に記載のリチウム補充材料。
- 前記金属リチウム粒子の表面には、不動態化層があり、前記不動態化層は、炭酸リチウム、フッ化リチウム、及びパラフィンのうちの少なくとも1つを含む、請求項1に記載のリチウム補充材料。
- 前記不動態化層の厚さは、5nm~100nmである、請求項6に記載のリチウム補充材料。
- リチウム補充材料の製造方法であって、
溶融金属リチウムを含有する第1の分散液と、電子伝導度が100S/cmよりも大きい導電材料を含有する第2の分散液とを、金属リチウムの溶融温度で混合し、混合後の材料を得るS1と、
前記混合後の材料を金属リチウムが凝固するまで冷却し、固液分離を行い、リチウム補充材料を得るS2と、を含む、リチウム補充材料の製造方法。 - 前記金属リチウムと前記導電材料との重量比は、100:(0.1~3)であり、好ましくは、100:(0.5~1)である請求項8に記載の方法。
- 前記第1の分散液は、界面活性剤をさらに含み、
前記界面活性剤は、ポリビニルピロリドン、ドデシルベンゼンスルホン酸ナトリウム、及びセチルトリメチルアンモニウムブロミドから選択された少なくとも1つであり、好ましくは、ポリビニルピロリドンである、請求項8に記載の方法。 - 前記金属リチウムと前記界面活性剤との重量比は、1:(0.002~0.05)であり、好ましくは、1:(0.005~0.02)である、請求項10に記載の方法。
- 前記第1の分散液及び前記第2の分散液の分散媒は、不活性有機溶媒であり、前記第1の分散液及び前記第2の分散液の分散媒は、それぞれ独立して、炭化水素、エステル、エーテル、及びシリコーンオイルから選択された少なくとも1つである、請求項8に記載の方法。
- 前記第1の分散液と前記第2の分散液との体積比は、1:(0.1~10)であり、好ましくは、1:(0.5~3)である、請求項8に記載の方法。
- ステップS1では、前記第1の分散液と前記第2の分散液とを混合した後、二酸化炭素を導入するステップをさらに含む、請求項8~13のいずれか一項に記載の方法。
- 負極は、集電体、負極活物質、及び請求項1~7のいずれか一項に記載のリチウム補充材料を含むことを特徴とする、リチウムイオン電池。
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CN201911296454.7A CN112993251B (zh) | 2019-12-16 | 2019-12-16 | 一种补锂材料及其制备方法、负极和锂离子电池 |
CN201911296454.7 | 2019-12-16 | ||
PCT/CN2020/128047 WO2021120927A1 (zh) | 2019-12-16 | 2020-11-11 | 一种补锂材料及其制备方法、负极和锂离子电池 |
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CN113782823B (zh) * | 2021-08-12 | 2023-07-04 | 浙江锋锂新能源科技有限公司 | 一种用于固态锂电池的补锂功能电解质膜的制备方法 |
CN114975858A (zh) * | 2022-06-17 | 2022-08-30 | 珠海冠宇电池股份有限公司 | 一种负极片和应用该负极片的补锂方法 |
WO2024073001A1 (en) * | 2022-09-28 | 2024-04-04 | Applied Materials, Inc. | Alkali metal oxide and hydroxide reduction in the film by ex¬ situ surface passivated layer |
CN116053708B (zh) * | 2023-03-29 | 2023-07-04 | 安迈特科技(北京)有限公司 | 一种用于锂电池的补锂复合隔膜、锂电池及其制备方法 |
CN116741986B (zh) * | 2023-08-07 | 2023-12-19 | 合肥国轩高科动力能源有限公司 | 锂离子电池正极补锂复合材料及其制备方法和应用 |
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JP2018534747A (ja) * | 2015-10-28 | 2018-11-22 | エルジー・ケム・リミテッド | 導電材分散液およびこれを用いて製造したリチウム二次電池 |
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CN107305941B (zh) * | 2016-04-21 | 2019-12-27 | 中国科学院苏州纳米技术与纳米仿生研究所 | 锂-碳复合材料、其制备方法与应用以及锂补偿方法 |
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