JP7038947B2 - リチウム金属と無機物複合層を用いた前リチウム化 - Google Patents
リチウム金属と無機物複合層を用いた前リチウム化 Download PDFInfo
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Description
<負極の製造>
負極活物質としてSiOが92重量%、デンカブラック(Denka Black、導電剤)3重量%及びSBR(結合剤)3.5重量%、及びCMC(増粘剤)1.5重量%を水に添加して負極混合物スラリーを製造した。
銅集電体の一面に前記負極混合物スラリーをコーティングし、それを乾燥及び圧延した後、一定の大きさにパンチングして負極を製造した。
SiO負極表面にリチウム金属-Al2O3の複合層を形成するため、リチウム金属粉末(粒径:5~50μm)30重量%、Al2O3粉末(粒径:0.5~1μm)66重量%及びバインダー4質量%をn-ヘキサン溶液に入れて分散させ、スラリーを製造した。この時、溶媒と固形分の混合比率は、溶媒35vol%、固形分65vol%とした。前記のように製造されたスラリーをSiO電極表面に塗布し、乾燥して5μmの平均厚さを有するリチウム金属-Al2O3複合層を形成させた。
カウンター(counter)電極(対向電極)にリチウム金属箔(150μm)を使用し、前記負極と前記カウンター電極との間にポリオレフィンセパレータを介在させた後、エチレンカーボネート(EC)、エチルメチルカーボネート(DEC)を50:50の体積比で混合した溶媒に1Mの六フッ化リン酸リチウム(LiPF6)が溶解された電解液を注入してコイン型ハーフ電池を製造した。
Al2O3の代わりに酸化マグネシウム(MgO)を用いたことを除いては、実施例1と同様の方法で電池を製造した。
Al2O3の代わりに二酸化ジルコニウム(ZrO2)を使用したことを除いては、実施例1と同様の方法で電池を製造した。
リチウム金属-無機物複合層の厚さを3μmに調節したことを除いては、実施例1と同様の方法で電池を製造した。
リチウム金属-無機物複合層の厚さを8μmに調節したことを除いては、実施例1と同様の方法で電池を製造した。
リチウム金属粉末及びAl2O3粉末の重量比を20:76に変更したことを除いては、実施例1と同様の方法で電池を製造した。
リチウム金属粉末及びAl2O3粉末の重量比を35:61に変更したことを除いては、実施例1と同様の方法で電池を製造した。
負極に前記実施例の平均厚さ5μmのリチウム金属-Al2O3の複合層が形成されたSiO電極の代わりに何らかの処理もしていないSiO電極を使用したことを除いては、実施例1と同様の方法で電池を製造した。
溶融されたリチウムに粉末形態のMgOを入れ、それを押出して実施例1のSiO負極表面にコーティングしたことを除いては、実施例1と同様に電池を製造した。この時、リチウム及びMgOの重量比は8:2であり、コーティング厚さは20μmであった。
リチウム金属-無機物複合層の厚さを30μmに調節したことを除いては、実施例1と同様の方法で電池を製造した。
前記実施例及び比較例で製造したコイン型ハーフ電池に対して電気化学充放電器を利用して充放電可逆性のテストを行った。最初のサイクルの充電時に0.005V(vs.Li/Li+)の電圧まで0.1C-rateの電流密度で電流を加えて充電し、放電時に同じ電流密度で1.5V(vs.Li/Li+)の電圧まで放電を実施した。この時、充電容量と放電容量を測定し、その比率(放電容量/充電容量*100)を計算して表1に示した。
示差走査熱量測定(differential scanning calorimetry)を実施するために実施例及び比較例のコイン型ハーフ電池を前記のように1サイクル充放電した後、2回目のサイクルで0.005Vまで充電して活性化させた負極を掻き出した。こうして得た充填された負極パウダー13mgに電解液0.1mlを添加してDSC装置(mettle Toledo)にローディングした。こうしてローディングされたサンプルを10℃/minの昇温速度で加熱してカロリーを測定し、その結果を表1に示した。
200: リチウム金属-無機物の混合溶液、リチウム金属-無機物複合層
210: 無機物粉末
220: リチウム金属粉末
300: 前リチウム化された負極
400: 無機物層
Claims (5)
- リチウム金属粉末20~40重量部、無機物粉末50~80重量部及びバインダー1~10重量部を溶媒に入れて分散させ、混合溶液を製造する段階と、
負極に前記混合溶液を使用して、リチウム金属-無機物複合層を形成させる段階と、を含み、
前記無機物粉末はアルミナ(Al 2 O 3 )、二酸化チタン(TiO 2 )、二酸化ジルコニウム(ZrO 2 )、二酸化ケイ素(SiO 2 )、酸化スズ(SnO 2 )、酸化セリウム(CeO 2 )、酸化マグネシウム(MgO)、酸化カルシウム(CaO)及びイットリア(Y 2 O 3 )の中から選ばれた1種または2種以上である、二次電池用負極の前リチウム化方法。 - 前記リチウム金属-無機物複合層の厚さは0.5~20μmであることを特徴とする、請求項1に記載の二次電池用負極の前リチウム化方法。
- 前記リチウム金属-無機物複合層を形成する方法は、塗布、スプレー、ラミネーションの中から選ばれた1つの方法であることを特徴とする、請求項1または2に記載の二次電池用負極の前リチウム化方法。
- 前記リチウム金属-無機物複合層は、初期活性化充電の後には金属形態のリチウムとして残っていないことを特徴とする、請求項1から3の何れか一項に記載の二次電池用負極の前リチウム化方法。
- 前記負極は、シリコン酸化物を含むことを特徴とする、請求項1から4の何れか一項に記載の二次電池用負極の前リチウム化方法。
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CN113659111B (zh) | 2019-05-31 | 2023-01-06 | 宁德时代新能源科技股份有限公司 | 负极极片、电芯、锂离子电池、电子产品及电动车辆 |
CN111434609B (zh) * | 2019-12-27 | 2022-09-20 | 蜂巢能源科技有限公司 | 预锂化负极活性材料及其制备方法、负极片和锂离子电池 |
CN111244427A (zh) * | 2020-01-21 | 2020-06-05 | 浙江理工大学 | 应用于锂金属电池的无机GeO2-Li复合负极及其制备方法 |
CN111509211A (zh) * | 2020-04-29 | 2020-08-07 | 广西师范大学 | 一种LM/Li复合材料的制备方法 |
KR20220023516A (ko) * | 2020-08-21 | 2022-03-02 | 주식회사 엘지에너지솔루션 | 음극의 전리튬화 장치 및 음극의 전리튬화 방법 |
JP7523062B2 (ja) | 2020-09-17 | 2024-07-26 | 本田技研工業株式会社 | リチウム二次電池用電解質媒体及びリチウム二次電池 |
JP7353325B2 (ja) * | 2021-06-15 | 2023-09-29 | プライムプラネットエナジー&ソリューションズ株式会社 | 負極および該負極を備える非水電解質二次電池 |
CN113782744B (zh) * | 2021-08-30 | 2022-12-27 | 上海纳米技术及应用国家工程研究中心有限公司 | 锂离子修饰粘结剂用于提高高比能氧化亚硅负极性能的方法 |
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EP3570349A4 (en) | 2020-01-22 |
KR102264691B1 (ko) | 2021-06-15 |
US11316156B2 (en) | 2022-04-26 |
KR20190017417A (ko) | 2019-02-20 |
PL3570349T3 (pl) | 2021-05-17 |
EP3570349A1 (en) | 2019-11-20 |
CN110268557A (zh) | 2019-09-20 |
US20190372118A1 (en) | 2019-12-05 |
JP2020506522A (ja) | 2020-02-27 |
WO2019031732A1 (ko) | 2019-02-14 |
CN110268557B (zh) | 2022-09-13 |
EP3570349B1 (en) | 2021-01-13 |
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