JP2018530859A - リチウムイオン電池用のシリコン粒子含有アノード材料 - Google Patents
リチウムイオン電池用のシリコン粒子含有アノード材料 Download PDFInfo
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- JP2018530859A JP2018530859A JP2018506892A JP2018506892A JP2018530859A JP 2018530859 A JP2018530859 A JP 2018530859A JP 2018506892 A JP2018506892 A JP 2018506892A JP 2018506892 A JP2018506892 A JP 2018506892A JP 2018530859 A JP2018530859 A JP 2018530859A
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- anode material
- silicon particles
- lithium ion
- ion battery
- silicon
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- 229910002102 lithium manganese oxide Inorganic materials 0.000 description 1
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- ILXAVRFGLBYNEJ-UHFFFAOYSA-K lithium;manganese(2+);phosphate Chemical compound [Li+].[Mn+2].[O-]P([O-])([O-])=O ILXAVRFGLBYNEJ-UHFFFAOYSA-K 0.000 description 1
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- 238000001291 vacuum drying Methods 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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Abstract
Description
I:角張ったエッジで、空間の三方向におおよそ等しい寸法を有する形状(例:立方体形状)
II:角張ったエッジで、空間の一方向の寸法が他の二方向の寸法よりも著しく長い形状(例:角柱形状、ブレード形状)
III:角張ったエッジで、空間の一方向の寸法が他の二方向の寸法よりも著しく小さい形状(例:プレート形状、フレーク形状)
IV:丸いエッジで、空間の三方向におおよそ等しい寸法を有する形状(例:球形状)
V:丸いエッジで、空間の一方向の寸法が他の二方向の寸法よりも著しく長い形状(例:円柱形状、ロッド形状)
VI:繊維状、糸状、房状、絡まった形状
γ:Li22Si5の化学量論(4200mAh/gに相当)でのリチウムについてのシリコンの最大容量
FG:アノードコーティングの単位面積当たりの質量
ωSi:アノードコーティング中のSiの質量割合
最初に、リチウムイオン電池を、4.2Vの電圧制限に達するまで、5mA/g(C/25に相当)の定電流で、cc(定電流)法により充電することにより、電気的に充電した状態とする。ここで、アノードはリチウム化される。
電解液を、テトラヒドロフランを用いて、最初に完全に、脱リチウム化したアノードコーティング(Cu箔無し)サンプルから洗い流す。サンプルを次に、酸により消化する。この目的のために、75mgのアノードコーティングを、マイクロ波消化容器(AntonPaar社製の100mLのTFMライナー)に移し、5mLのHNO3(65%強度、AR)、0.25mLのHCl(37%強度、AR)、および1mLのHF(40%強度、超高純度)と混合する。マイクロ波消化容器を閉じて、マイクロ波装置(Multiwave 3000、AntonPaar社製)内に導入し、950Wで45分間処理する。消化した混合物を完全に50mLチューブに移し、水で50mLに調整する。この内、0.50mLを取り出し、2.50mLの4%強度のホウ酸と混合し、再び50mLに調整する(希釈:希釈係数100)。Siの質量割合、ωSiは、ICP−OES(誘導結合プラズマ発光分析)(測定機器:Optima 7300 DV、Perkin Elmer社製;サンプル導入システム:サイクロンスプレーチャンバーを備えるMeinhardアトマイザー、較正範囲:0.1〜20.0mg/LのSi、Merck社製の、Si100mg/LのSi標準原液Certipur(認証)))により測定する。
ミリングによる、非凝結、破片形状、サブミクロンシリコン粒子の製造:
物理的混合による、実施例1のシリコン粒子、グラファイトおよび結合剤を用いた本発明によるアノードの製造:
実施例2のアノードを含んでなるリチウムイオン電池:
ミリング加工による、ナノサイズ、破片形状、非凝結シリコン粒子の調製:
粉砕時間を600分とすること以外は、実施例1に記載の通りに行った。ナノサイズ、破片形状、非凝結シリコン粒子を得た。懸濁液の固体含有量は、エタノールの添加により、最大22.3質量%に調整した。
比較例4のシリコン粒子、グラファイト、導電性カーボンブラックおよび結合剤を用いた、物理的混合によるアノードの製造:
比較例4と同様に調製した、エタノール中の22.3質量%強度のSi懸濁液3.03g、および0.41gの導電性カーボンブラック(Imerys社、Super P Li)を、水中のカルボキシメチルセルロースナトリウム(株式会社ダイセル製、グレード1380)の1.4質量%強度の溶液19.35g中に、15分間4.5m/sの周速度で、さらに20℃で冷却しながら45分間17m/sの周速度で、高速混合器により分散させた。2.04gのグラファイト(Imerys社製、SFG6)を添加した後、混合物を次に、さらに30分間12m/sの周速度で攪拌した。脱気した後、懸濁液を、0.20mmの隙間高さを有する製膜フレーム(Erichsen社、モデル360)により、0.030mmの厚さを有する銅箔(Schlenk Metalldolein社、SE−Cu58)へ塗布した。この方法により調製したアノードコーティングを、その後、80℃、1barの空気圧で60分間乾燥させた。乾燥アノードコーティングの単位面積当たりの平均質量は、2.18mg/cm2であった。
比較例5のアノードを備えるリチウムイオン電池:
比較例5からの破片形状ナノサイズシリコン粒子を含んでなるアノードを、実施例3に記載のように試験した。
比較例5の形成のために、リチウムイオン電池を、最大リチウム化で操作した。
二峰性粒径分布を有する、ナノサイズ、凝結シリコン粒子:
比較例7のナノサイズ、凝結シリコン粒子を含むアノード材料を含んでなるリチウムイオン電池:
最初に、シリコン粒子として比較例7の粒子を使用する以外は、実施例2と同様の方法によりアノードを製造した。
リチウムイオン電池を、この方法により得たアノードから製造し、実施例3に記載したように試験した。
比較例8のリチウムイオン電池は、第二サイクルにおいて、1.82mAh/m2の可逆的な初期容量を有し、わずか32回の充電/放電サイクルの後に、その元も容量の80%の容量しか有していない。比較例8のリチウムイオン電池は、したがって、実施例3のパフォーマンス特性よりもはるかに遅れを取っている。
実施例3のリチウムイオン電池は、驚くべきことに、比較例6および8のリチウムイオン電池と比較して、第一サイクルにおける容量の低い不可逆的損失(=高い初期容量)およびその後のサイクルにおけるより安定的な電気化学的挙動を示す。
Claims (12)
- シリコン粒子、一または複数の結合剤、所望によりグラファイト、所望により一または複数の追加の導電性成分および所望により一または複数の添加剤に基づく、リチウムイオン電池のためのアノード材料であって、
前記シリコン粒子は非凝結であり、直径パーセンタイルはd10≧0.2μmとd90≦20.0μmの間であり、幅d90−d10≦15μmの体積加重粒径分布を有することを特徴とする、アノード材料。 - 前記シリコン粒子は、直径パーセンタイルがd10≦10μmの体積加重粒径分布を有する、請求項1に記載のアノード材料。
- 前記シリコン粒子は、直径パーセンタイルがd90≧0.5μmの体積加重粒径分布を有する、請求項1または2に記載のアノード材料。
- 前記シリコン粒子は、幅d90−d10≧0.6μmの体積加重粒径分布を有する、請求項1〜3のいずれか一項に記載のアノード材料。
- 前記シリコン粒子は、0.5〜10.0μmの直径パーセンタイルd50の体積加重粒径分布を有する、請求項1〜4のいずれか一項に記載のアノード材料。
- 前記シリコン粒子は、0.3≦Ψ≦0.9の球形度を有する、請求項1〜5のいずれか一項に記載のアノード材料。
- 前記シリコン粒子は、ミリング加工により得られる、請求項1〜6のいずれか一項に記載のアノード材料。
- リチウムイオン電池を製造するための、請求項1〜7のいずれか一項に記載のアノード材料の使用。
- 請求項1〜7のいずれか一項に記載のアノード材料に基づく、アノードを含んでなる、リチウムイオン電池。
- 前記リチウムイオン電池は、前記アノード材料がフル充電された電池において部分的にのみリチウム化されるように操作される、請求項9に記載のリチウムイオン電池。
- 前記フル充電された電池の部分的にリチウム化されたアノード材料中のリチウム原子対シリコン原子の比は≦2.2である、請求項10に記載のリチウムイオン電池。
- 前記リチウムイオン電池の前記アノード材料のシリコンの容量は、シリコン1g当たり4200mAhの最大容量に基づいて、≦50%の程度まで利用される、請求項10に記載のリチウムイオン電池。
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CN107925072B (zh) | 2021-05-07 |
US10777807B2 (en) | 2020-09-15 |
CN107925072A (zh) | 2018-04-17 |
JP6790070B2 (ja) | 2020-11-25 |
KR20180035915A (ko) | 2018-04-06 |
KR102200190B1 (ko) | 2021-01-11 |
WO2017025346A1 (de) | 2017-02-16 |
EP3335262B1 (de) | 2019-06-26 |
US20180212234A1 (en) | 2018-07-26 |
EP3335262A1 (de) | 2018-06-20 |
DE102015215415A1 (de) | 2017-02-16 |
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