JP7416521B2 - リチウム金属電極の製造方法およびリチウム金属二次電池 - Google Patents
リチウム金属電極の製造方法およびリチウム金属二次電池 Download PDFInfo
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- JP7416521B2 JP7416521B2 JP2022525898A JP2022525898A JP7416521B2 JP 7416521 B2 JP7416521 B2 JP 7416521B2 JP 2022525898 A JP2022525898 A JP 2022525898A JP 2022525898 A JP2022525898 A JP 2022525898A JP 7416521 B2 JP7416521 B2 JP 7416521B2
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- Prior art keywords
- lithium metal
- fluorine
- lithium
- metal electrode
- lubricant composition
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Images
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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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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
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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
- H01M4/139—Processes of manufacture
- H01M4/1395—Processes of manufacture of electrodes based on metals, Si or alloys
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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
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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
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Description
[化学式1]
CF3-O-[CF(CF3)-CF2O]x-[CF2O]y-CF3
前記化学式1中、x、yはそれぞれ独立して1~20の整数である。
*-[CF2-O]m-[CF2-CF2-O]n-*
前記化学式2中、m~nはそれぞれ独立して1~100の整数である。
また、前記潤滑剤組成物は、粘度が0.5~100cpであることが好ましい。
また、本発明のリチウム金属電極の製造方法によると、圧延工程時に保護膜が形成されるため、保護膜を形成するための別のコーティング工程が要らず、そのため工程性および経済性に優れる。
先ず、本発明に係るリチウム金属電極の製造方法について説明する。
図1には、本発明に係るリチウム金属電極の製造方法が示されている。
前記フッ素系溶媒は、後述するフッ素系化合物との相溶性に優れるため、フッ素系化合物を円滑に溶解させることで、潤滑剤組成物がリチウム金属ストリップ上に円滑に塗布されるようにする。
また、前記フッ素系溶媒は、蒸気圧(vapor pressure)が0.1~30kPa、好ましくは1~20kPa、より好ましくは2~10kPaの溶媒であることが好ましい。
CF3-O-[CF(CF3)-CF2O]x-[CF2O]y-CF3
前記化学式1中、x、yはそれぞれ独立して1~20の整数であり、好ましくは1~8の整数、より好ましくは1~4の整数であってもよい。
本発明において、前記フッ素系化合物は、フッ素原子を含み、重量平均分子量(Mw)が100~100,000g/mol、好ましくは2,000~20,000g/mol、より好ましくは5,000g/mol~10,000g/molのオリゴマーまたは重合体であってもよい。フッ素系化合物の重量平均分子量が過度に小さいと、リチウム金属ストリップ上に高分子膜が円滑に形成されないため、潤滑性能が低下し、重量平均分子量が過度に大きいと、潤滑剤組成物の粘度が高くなるため、リチウム金属ストリップ上に噴射または塗布が円滑に行われない。
[化学式2]
*-[CF2-O]m-[CF2-CF2-O]n-*
前記化学式2中、m~nはそれぞれ独立して1~100の整数、好ましくは20~80の整数、より好ましくは40~60の整数であってもよい。
また、前記潤滑剤組成物は、前記フッ素系化合物を1~10重量%、好ましくは1~5重量%、より好ましくは2~4重量%の量で含んでもよい。
次に、本発明に係るリチウム金属電池について説明する。
本発明に係るリチウム金属電池は、前記方法により製造されたリチウム金属電極を含む。具体的には、本発明に係るリチウム金属電池は、正極、負極、および電解質を含み、前記負極として、リチウム金属薄膜と、前記リチウム金属薄膜の表面に形成され、LiFを含む保護膜とを含むものであってもよい。また、本発明に係るリチウム金属電池は、必要に応じて、セパレータをさらに含んでもよい。
以下、本発明のリチウム金属電池の各構成についてさらに詳しく説明する。
前記負極は、本発明の方法により製造されたリチウム金属電極であり、リチウム金属薄膜と、前記リチウム金属薄膜の表面に形成された保護膜とを含む。
前記正極は、リチウム金属電池に用いられる多様な正極が用いられてもよい。例えば、前記正極は、正極集電体上に正極活物質層が積層された形態であってもよい。
前記正極活物質としては、リチウム金属電池に用いられる一般的な正極活物質が用いられてもよく、例えば、硫黄含有化合物が用いられてもよい。
導電材は、集電体(Current collector)から電子が正極活物質まで移動する経路の役割をして電子伝導性を付与するだけでなく、電解質と正極活物質を電気的に連結して電解質中に溶けているリチウムイオン(Li+)が硫黄まで移動して反応するようにする経路の役割を同時にする。
前記電解質としては、二次電池に用いられる液体電解質、有機固体電解質、無機固体電解質などが用いられてもよく、その種類が特に制限されるものではない。
例えば、前記液体電解質は、有機溶媒およびリチウム塩を含んでもよい。
前記セパレータは、負極と正極を分離しリチウムイオンの移動通路を提供するものであり、通常、二次電池においてセパレータとして用いられるものであれば特に制限されずに使用可能であり、特に電解質のイオン移動に対して低抵抗であり、且つ、電解液含湿能力に優れることが好ましい。
また、通常の多孔性不織布、例えば、高融点のガラス繊維、ポリエチレンテレフタレート繊維などからなる不織布が用いられてもよい。
フッ素系溶媒CF3-O-[CF(CF3)-CF2O]2-CF2O-CF3(沸点105℃、蒸気圧:2.5kPa)とフッ素系化合物Fomblin(R) Z15(製造会社:Solvay、重量平均分子量8,000g/mol)を97.6:2.4の重量比で混合し、潤滑剤組成物を製造した。製造された潤滑剤組成物の粘度をBrokfield社の粘度測定装置(モデル名:DV2TLV)を用いて20℃で測定し、測定された粘度は1.2cpであった。
フッ素系溶媒CF3-O-[CF(CF3)-CF2O]2-CF2O-CF3(沸点105℃、蒸気圧:2.5kPa)とフッ素系化合物Fomblin(R) Z15(製造会社:Solvay、重量平均分子量8,000g/mol)を96:4の重量比で混合し、潤滑剤組成物を製造した。製造された潤滑剤組成物の粘度をBrokfield社の粘度測定装置(モデル名:DV2TLV)を用いて20℃で測定し、測定された粘度は1.5cpであった。
フッ素系溶媒CF3-O-[CF(CF3)-CF2O]2-CF2O-CF3(沸点105℃、蒸気圧:2.5kPa)とフッ素系化合物Fomblin(R) Z25(製造会社:Solvay、重量平均分子量9,500g/mol)を97.6:2.4の重量比で混合し、潤滑剤組成物を製造した。製造された潤滑剤組成物の粘度をBrokfield社の粘度測定装置(モデル名:DV2TLV)を用いて20℃で測定し、測定された粘度は1.4cpであった。
実施例1の潤滑剤組成物の代わりに、炭素数8の鎖式飽和炭化水素であるオクタンを潤滑剤として用いたことを除いては、実施例1と同様の方法によりリチウム金属電極を製造した。
<正極の製造>
正極活物質として硫黄-炭素複合体(S:C=7:3の重量比)を90重量部、導電材としてデンカブラック5重量部、バインダーとしてスチレン-ブタジエンゴムとカルボキシメチルセルロースを7:3の重量比で混合した混合物5重量部を混合し、正極スラリー組成物を製造した。
実施例1~3および比較例1により製造されたそれぞれのリチウム金属電極を用いてリチウム金属電極/セパレータ/リチウム金属電極構造の対称電池を製造し、電解質0.1mlを注入した。
15:リチウム金属薄膜
20:潤滑剤組成物
25:保護膜
30:圧延ローラ
Claims (8)
- リチウム金属ストリップ(strip)を提供するステップと、
前記リチウム金属ストリップ上にフッ素系溶媒およびフッ素系化合物を含む潤滑剤組成物を提供し圧延するステップと、を含み、
前記フッ素系溶媒は、下記[化学式1]で表される化合物であり、
前記フッ素系化合物は、下記[化学式2]で表される単位を含む、リチウム金属電極の製造方法。
[化学式1]
CF 3 -O-[CF(CF 3 )-CF 2 O] x -[CF 2 O] y -CF 3
前記化学式1中、x、yはそれぞれ独立して1~20の整数である。
[化学式2]
*-[CF 2 -O] m -[CF 2 -CF 2 -O] n -*
前記化学式2中、m~nはそれぞれ独立して1~100の整数である。 - 前記フッ素系溶媒は、沸点が150℃以下であり、蒸気圧が0.1kPa~30kPaである、請求項1に記載のリチウム金属電極の製造方法。
- 前記フッ素系溶媒は、沸点が50℃~130℃であり、蒸気圧が1kPa~20kPaである、請求項1に記載のリチウム金属電極の製造方法。
- 前記フッ素系溶媒は、沸点が80℃~120℃であり、蒸気圧が2kPa~10kPaである、請求項1に記載のリチウム金属電極の製造方法。
- 前記フッ素系化合物は、重量平均分子量が100g/mol~100,000g/molである、請求項1に記載のリチウム金属電極の製造方法。
- 前記フッ素系化合物は、重量平均分子量が2,000g/mol~20,000g/molである、請求項1に記載のリチウム金属電極の製造方法。
- 前記潤滑剤組成物は、フッ素系溶媒90~99重量%、およびフッ素系化合物1~10重量%を含む、請求項1に記載のリチウム金属電極の製造方法。
- 前記潤滑剤組成物は、粘度が0.5~100cpである、請求項1に記載のリチウム金属電極の製造方法。
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EP4037022A1 (en) | 2022-08-03 |
CN114556624A (zh) | 2022-05-27 |
WO2021256829A1 (ko) | 2021-12-23 |
KR20210155086A (ko) | 2021-12-22 |
JP2023500528A (ja) | 2023-01-06 |
US20230006211A1 (en) | 2023-01-05 |
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