TWI389374B - 以具有高矽含量之非晶形合金為主之電極組合物 - Google Patents

以具有高矽含量之非晶形合金為主之電極組合物 Download PDF

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TWI389374B
TWI389374B TW095144459A TW95144459A TWI389374B TW I389374 B TWI389374 B TW I389374B TW 095144459 A TW095144459 A TW 095144459A TW 95144459 A TW95144459 A TW 95144459A TW I389374 B TWI389374 B TW I389374B
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ion battery
lithium ion
electrode composition
amorphous alloy
metals
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Leif Christensen
Mark Nikolas Obrovac
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3M Innovative Properties Co
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Description

以具有高矽含量之非晶形合金為主之電極組合物
本發明係關於用於鋰離子電池組之電極組合物。
已提議將含有矽、鋁及各種過渡金屬元素之熔融紡絲合金(Melt－spun alloy)用作鋰離子電池組之電極。該等合金具有可增強循環壽命且因此增強整個電池組效能之非晶形微結構。然而，隨著矽含量之增加，愈來愈難以產生具有非晶形微結構之組合物。針對此問題所提議之一種解決方法係需要使用與矽及鋁組合之相對高劑量(就原子百分數而言)及/或數量之過渡金屬元素。然而，此種經提議之解決方法具有使該等材料無電化學活性之風險。
本發明描述一種用於鋰離子電池組之電極組合物，其包括具有式Six My Alz 之非晶形合金，其中x、y及z表示原子百分數值，且(a)x＋y＋z＝100；(b)x55；(c)y<22；(d)z>0；及(e)M為一或多種選自由以下各金屬組成之群的金屬：錳、鉬、鈮、鎢、鉭、鐵、銅、鈦、釩、鉻、鎳、鈷、鋯、釔及其組合。非晶形合金可為單一相之形式。"非晶形合金"為缺乏長程原子規則(long range atomic order)且x射線繞射圖案缺乏尖形、良好界定之峰的合金。
x之值可選擇成x60之值。y之值可選擇成y20之值。
M較佳僅表示兩種金屬。尤其有用之金屬之特定實例包括鐵、鈦、鋯及其組合。
電極組合物可用作亦包括陰極及電解質之鋰離子電池組之陽極。電解質可包括碳酸氟伸乙酯。陽極較佳係以包括電極組合物與黏合劑(例如，聚醯亞胺)及導電稀釋劑(例如，碳黑)之組合之複合物的形式。
電極組合物展現高容量及良好之循環壽命，同時亦將金屬M含量降至最低。將金屬M降至最低之能力產生可用作鋰離子電池組之電極的電化學活性材料。
在附圖及下文描述中闡述本發明之一或多個實施例的細節。本發明之其他特徵、目標及優勢將由描述及附圖及申請專利範圍而顯而易見。
已描述尤其可用作鋰離子電池組之陽極之電極組合物。該等電極組合物之特徵為具有式Six My Alz 之非晶形合金，其中x、y及z表示原子百分數值，且(a)x＋y＋z＝100；(b)x55；(c)y<22；(d)z>0；及(e)M為一或多種選自由以下各金屬組成之群的金屬：錳、鉬、鈮、鎢、鉭、鐵、銅、鈦、釩、鉻、鎳、鈷、鋯、釔及其組合。尤其有用之組合物為x60、y20且M表示不超過兩種之金屬的彼等組合物。
較佳藉由冷硬試件熔融紡絲法(chill block melt spinning process)製備電極組合物。例如，該等方法通常描述於"Amorphous Metallic Alloys",F.E.Luborsky編輯，第2章，Butter worth & Co.,Ltd.(London),1983中。根據該方法，在射頻場中熔融含有矽及金屬元素之鑄錠且隨後經由一噴嘴將其噴射於旋轉金屬輪(rotating metal wheel)(例如，銅或銅合金輪)之表面上。因為輪表面之溫度大體低於熔融物之溫度，所以與輪表面接觸會驟冷該熔融物。驟冷防止形成對電極效能有害之大微晶。藉由使用大於40 m/s之輪表面速度及具有小於0.5 mm之直徑的噴嘴，可製備非晶形組合物。
電極組合物尤其可用作鋰離子電池組之陽極。陽極較佳為電極組合物與黏合劑及導電稀釋劑組合之複合物。合適黏合劑之實例包括聚醯亞胺及聚偏二氟乙烯。合適導電稀釋劑之實例包括碳黑。
為製備電池組，將陽極與電解質及陰極(對立電極)組合。電解質可為液體、固體或凝膠形式。固體電解質之實例包括聚合電解質，諸如聚氧化乙烯、含氟聚合物及共聚物(例如，聚四氟乙烯)及其組合。液體電解質之實例包括碳酸乙烯酯、碳酸二乙酯、碳酸丙烯酯、碳酸氟乙烯酯(FEC)及其組合。電解質具有鋰電解鹽。合適鹽之實例包括LiPF6 、LiBF4 、雙草酸硼酸鋰(lithium bis(oxalato)borate)、LiN(CF3 SO2 )2 、LiN(C2 F5 SO2 )2 、LiAsF6 、LiC(CF3 SO2 )3 及LiClO4 。合適陰極組合物之實例包括LiCoO2 、LiCo0 . 2 Ni0 . 8 O2 及LiMn2 O4 。其他實例包括描述於下列文獻中之陰極組合物：(1)Lu等人，美國公開專利申請案第2004/0121234號；(2)Dahn等人，美國公開專利申請案第2003/0108793號；(3)Eberman等人，美國公開專利申請案第2005/0112054號；(4)Dahn等人，美國公開專利申請案第2004/0179993號；(5)Lu等人，美國專利第6,964,828號；(6)Lu等人，美國專利第7,078,128號；(7)Obrovac等人，美國專利第6,680,145號；及(8)Dahn等人，美國專利第5,900,385號。
實例 實例1
在稱盤中稱取13.93 g鋁、49.960 g矽、25.637 g鐵及10.469 g鋯(皆具有99.8%或更佳之純度)且隨後將其置於ARC爐(自Advanced Vacuum Systems,Ayer,MA購得)中。在氬氣氛圍中熔融該混合物以得到具有Si6 2 Al1 8 Fe1 6 Zr4 之組成之鑄錠，其中所有量皆為原子百分數。
使用濕鑽石鋸刀(diamond blade wet saw)將鑄錠切成條帶以形成用於熔融紡絲之20 g條帶。熔融紡絲設備係由具有圓柱形石英玻璃坩堝之真空室組成。該坩堝具有16 mm之內徑、140 mm之長度及0.28 mm之噴嘴。將坩堝定位於具有10 mm厚度及203 mm直徑的旋轉冷卻輪(含有0.45重量% Cr、2.4重量% Ni、0.6重量% Si且其餘為銅之Ni－Si－Cr－Cu C18000合金)上。操作前，使用摩擦化合物(rubbing compound)(以IMPERIAL MICROFINISHING自3M,St.Paul,MN購得)拋光輪之邊緣表面，隨後以礦物油擦拭而留下薄膜。
對熔融紡絲而言，將20 g鑄錠條帶置放於坩堝中，此後將系統抽空至80毫托(mTorr)且隨後以氦氣將其填充至200毫托之壓力。使用RF感應熔融鑄錠。當溫度達到1275℃時，將400毫托之氦壓力施加於熔融合金之表面以經由噴嘴擠壓出合金且達至以5,031 rpm(53 m/s)旋轉的紡絲輪上。製造出1毫米寬及10微米厚之帶狀條帶。使用裝備有銅靶x射線管及繞射光束單色儀之Siemens Model Kristalloflex 805 D500繞射計來收集代表性條帶之x射線繞射圖。結果展示於表1中。尖狀峰不存在表示非晶形組合物。
將1.70 g熔融紡絲條帶、150 mg Super P碳(導電稀釋劑)、0.750 g聚醯亞胺塗層溶液(自HD Microsystems,Parlink NJ購得，PYRALIN PI2555，20%於N－甲基吡咯啶酮(NMP)中)及3.75 g NMP添加至含有10 mm直徑及10.3 mm直徑碳化鎢球之40 ml碳化鎢研磨容器中。將容器置於行星研磨器(自Fritsch GmbH,Idon－Oberstein,Germany購得之PULVERISETTE 7)中且於8之設定值下研磨一小時。
研磨後，將溶液轉移至凹口塗佈棒中且以25 mm寬、125微米厚之條帶將其塗佈於15微米厚之Cu箔上。在真空中於150℃下固化該塗層2.5小時以形成電極。隨後使用該電極以藉由將其與金屬鋰陽極、兩層平面薄片狀聚丙烯膜分離器(自Celgard Inc.,Charlotte,NC購得之CELGARD 2400)及作為電解質之1：2碳酸乙烯酯與碳酸二乙酯之混合物中的1 M LiPF6 組合來建構2225硬幣型電池(coin cell)。使用電池組循環器(battery cycler)(自Maccor,Tulsa,OK購得之MACCOR,Model 4000)在下列條件下循環電池：第一循環係在0.9 V與0.005 V之間0.125 mA之恆定電流下，而所有其他循環係在0.9 V與0.005 V之間0.5 mA之恆定電流下。結果展示於表2中。如圖所示，電池展現出良好之循環效能。
實例2
根據於實例1中描述之程序製備熔融紡絲鑄錠。合金組成為Si5 5 Al2 9 . 3 Fe1 5 . 7 ，其中所有量為原子百分數。圖3中所示之x射線繞射結果揭示缺乏尖形峰，說明組合物為非晶形。
使用高剪切混合機將0.8 g熔融紡絲條帶、4.16 g 3重量% Super P碳(導電稀釋劑)之分散液、3重量%聚偏二氟乙烯、94% N－甲基吡咯啶酮(NMP)及1 g NMP混合在一起15分鐘。
混合後，將漿料轉移至凹口塗佈棒且以25 mm寬、125微米厚之條帶將其塗佈於15微米厚之Cu箔上。在真空中於150℃下固化塗層2.5小時以形成電極。隨後，使用該電極藉由將其與金屬鋰陽極、兩層CELGARD 2400作為分離器及作為電解質之1：2碳酸乙烯酯與碳酸二乙酯之混合物中的1 M LiPF6 組合來建構2225硬幣型電池。根據表1中所述之方案使用MACCOR循環器循環該電池。結果展示於圖4中。如圖所示，電池展現出良好循環效能。
實例3及4
根據實例1描述之程序製備具有表2中所述之組成的樣本。X射線繞射資料揭示在兩種情況下均缺乏尖形峰，說明該等組合物為非晶形。表2中亦闡述使用各組成製備之電化學電池的循環容量。結果說明各電池展現出良好之循環能力。
已描述本發明之諸多實施例。然而，應瞭解在不悖離本發明之精神及範疇之情況下，可進行各種修改。因此，其他實施例亦在下述申請專利範圍之範疇內。
圖1為實例1所述之熔融紡絲合金之x射線繞射概況。
圖2說明併入實例1所述之熔融紡絲合金之電化學電池的循環效能。
圖3為實例2所述之熔融紡絲合金之x射線繞射概況。
圖4說明併入實例2所述之熔融紡絲合金之電化學電池的循環效能。

Claims (18)

  1. 一種用於一鋰離子電池組之電極組合物，其包含一具有式Six My Alz 之非晶形合金，其中x、y及z表示原子百分數值，且：(a)x＋y＋z＝100； (c)y<22；(d)z>0；及(e)M為一或多種選自由以下各金屬組成之群的金屬：錳、鉬、鈮、鎢、鉭、鐵、銅、鈦、釩、鉻、鎳、鈷、鋯、釔及其組合。
  2. 如請求項1之電極組合物，其中x60。
  3. 如請求項1之電極組合物，其中y20。
  4. 如請求項1之電極組合物，其中M為不超過兩種金屬。
  5. 如請求項1之電極組合物，其中M係選自由以下各金屬組成之群：鐵、鈦、鋯及其組合。
  6. 如請求項1之電極組合物，其中x60、y20且M為不超過兩種金屬。
  7. 如請求項1之電極組合物，其中該非晶形合金係呈單一相之形式。
  8. 一種鋰離子電池組，其包含：(a)一陽極；(b)一陰極；及(c)一電解質，其中該陽極包含一具有該式Six My Alz 之非晶形合金，其中x、y及z表示原子百分數值，且：(i)x＋y＋z＝100； (iii)y<22；(iv)z>0；及(v)M為一或多種選自由以下各金屬組成之群的金屬：錳、鉬、鈮、鎢、鉭、鐵、銅、鈦、釩、鉻、鎳、鈷、鋯、釔及其組合。
  9. 如請求項8之鋰離子電池組，其中x60。
  10. 如請求項8之鋰離子電池組，其中y20。
  11. 如請求項8之鋰離子電池組，其中M為不超過兩種金屬。
  12. 如請求項8之鋰離子電池組，其中M係選自由以下各金屬組成之群：鐵、鈦、鋯及其組合。
  13. 如請求項8之鋰離子電池組，其中x60、y20且M為不超過兩種金屬。
  14. 如請求項8之鋰離子電池組，其中該非晶形合金係呈單一相之形式。
  15. 如請求項8之鋰離子電池組，其中該陽極另外包含黏合劑及導電稀釋劑。
  16. 如請求項15之鋰離子電池組，其中該黏合劑包含聚醯亞胺。
  17. 如請求項15之鋰離子電池組，其中該導電稀釋劑包含碳黑。
  18. 如請求項8之鋰離子電池組，其中該電解質包含碳酸氟乙烯酯。
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EP1955393A4 (en) 2010-01-20
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US7732095B2 (en) 2010-06-08
US20100167126A1 (en) 2010-07-01
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EP1955393A1 (en) 2008-08-13

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