TWI397206B - 適用於鋰離子電池之電極的含矽合金 - Google Patents

適用於鋰離子電池之電極的含矽合金 Download PDF

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TWI397206B
TWI397206B TW095148650A TW95148650A TWI397206B TW I397206 B TWI397206 B TW I397206B TW 095148650 A TW095148650 A TW 095148650A TW 95148650 A TW95148650 A TW 95148650A TW I397206 B TWI397206 B TW I397206B
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ion battery
electrode composition
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cobalt
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Dinh Ba Le
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Description

適用於鋰離子電池之電極的含矽合金
本發明係關於適用於鋰離子電池之電極組合物、製備此等組合物之方法及包括此等組合物之電池。
已建議金屬合金作為用於鋰離子電池之陽極。此等合金類型之陽極通常相對於諸如石墨之夾層類型陽極展現較高容量。然而，此等合金之一個問題為由於在與合金中之組成變化相關之膨脹及收縮期間合金顆粒破碎，因此其通常展現相對不良循環壽命及不良庫侖效率(coulombic efficiency)。
本發明描述一種用於鋰離子電池之具有式Six Snq My Cz 之電極組合物，其中q、x、y及z表示原子百分數值且(a)(q＋x)>2y＋z；(b)x>0，(c)q及z各自獨立地為0；且(d)M為一或多種選自由錳、鉬、鈮、鎢、鉭、鐵、銅、鈦、釩、鉻、鎳、鈷、鋯、釔或其組合組成之群的金屬。Si、Sn、M及C元素係以多相微結構之形式配置，該多相微結構包含：(a)包含矽之非晶相；(b)包含金屬矽化物之奈米晶相；及(c)當z>0時，包含碳化矽之相；及(d)當q>0時，包含Sn之非晶相。
"非晶相"為缺乏長程原子有序性且其x射線繞射圖案缺乏銳化、明確之峰值之相。
"奈米晶相"為具有不大於約50奈米之微晶，展現長程原子有序性且具有以銳化、明確峰值為特徵之x射線繞射圖案的相。
在一些實施例中，可能選擇x值以使得x60且可能選擇z值以使得z>0、z10或z15。例如，在一實施例中，x60、x70或甚至更高，z>0或z10且M為一或多種選自由鈷、鎳、鐵、鈦、鉬及其組合組成之群的金屬。在另一實施例中，M包括Co，x60且z>0。
電極組合物可用作供一亦包括一陰極及一電解質之鋰離子電池用之陽極。該電解質可包括任何已知電解質，例如，碳酸氟乙二酯。較佳地，陽極係為包括與黏合劑(任何已知黏合劑，例如聚醯亞胺)及導電稀釋劑(任何已知導電稀釋劑，例如，碳黑)組合之電極組合物之複合物的形式。
當併入鋰離子電池中時，該等電極展現良好循環壽命及庫侖效率。
本發明之一或多個實施例之細節在以下附圖及說明書中闡明。本發明之其他特徵、目標及優勢將自實施方式及申請專利範圍而顯而易見。
所有數值在本文中假定由術語"約"修飾。由端點列舉之數值範圍包括所有歸入彼範圍中之數值(例如，1至5包括1、1.5、2、2.75、3、3.80、4及5)。
描述尤其適用於鋰離子電池之陽極的電極組合物。電極組合物以用於鋰離子電池之具有式Six Snq My Cz 之電極組合物為特徵，其中q、x、y及z表示原子百分數值且(a)(q＋X)>2y＋z；(b)q0，(c)z0；且(d)M為一或多種選自由錳、鉬、鈮、鎢、鉭、鐵、銅、鈦、釩、鉻、鎳、鈷、鋯、釔或其組合組成之群的金屬。Si、Sn、M及C元素係以多相微結構之形式配置，該多相微結構包含：(a)一包含矽之非晶相(因此x>0)；(b)一包含金屬矽化物之奈米晶相；及(c)當z>0時，一包含碳化矽之相；及(d)當q>0時，一包含Sn之非晶相。較佳地，電極組合物係藉由在高剪切力及高衝擊下球磨研磨矽、金屬及(在使用碳之實施例中)碳源(例如，石墨)歷時適當之時期而製備。亦可使用在該項技術中已知之球磨機，諸如垂直球磨機(ATTRITOR,Union Process Inc.,Akron,OH)、SPEXMILL(Spex CertiPrep,Metuchen,NJ)、水平旋轉球磨機(SIMOLOYER,Zoz GmbH,Werden,Germany)或其他球磨機。
電極組合物尤其適用於鋰離子電池之陽極。陽極較佳為其中電極組合物與黏合劑及導電稀釋劑組合之複合物。適當黏合劑之實例包括聚醯亞胺及聚偏二氟乙烯。適當導電稀釋劑之實例包括碳黑。
為製備電池，將陽極與電解質及陰極(反電極)組合。電解質可為液體、固體或凝膠之形式。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二酯、碳酸二乙酯、碳酸丙二酯、碳酸氟乙二酯(FEC)及其組合。電解質具備鋰電解質鹽。適當鹽之實例包括LiPF6 、LiBF4 、雙(草酸根基)硼酸鋰、(lithium bis(oxalato)borate)、LiN(CF3 SO2 )2 、LiN(C2 F5 SO2 )2 、LiAsF6 、LiC(CF3 SO2 )3 及LiClO4 。適當陰極組合物之實例包括LiCoO2 、LiCo0 . 2 Ni0 . 8 O2 及LiMn2 O4 。額外實例包括在以下文獻中描述之陰極組合物：(1)Lu等人，美國專利第6,964,828號；(2)Lu等人，美國專利第7,078,128號；(3)Le，美國公開專利申請案第2004/0121234號；(4)Dahn等人，美國公開專利申請案第2003/0108793號；(5)Eberman等人，美國公開專利申請案第2005/0112054號；(6)Dahn等人，美國公開專利申請案第2004/0179993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
矽、鐵、鎳、鈦、鈷及錫係得自Milwaukee,WI之Ward Hill,MA,Aldrich Chemical Company之Alfa Aesar或Berkeley,CA之Alcan Metal Powders。
X射線繞射圖案係使用配備有銅靶x射線管及繞射光束單色器之Siemens Model Kristalloflex 805 D500繞射計收集。存在於表1A及表1B之標記為"自X射線資料觀察到之相"之行中的資料係基於對於所列出合金樣品之每一者所獲得之峰值特徵圖案的存在或不存在。例如，當X射線繞射圖案缺少或缺乏銳化、明確之峰值時，認為相為非晶形。結晶相之晶粒尺寸係由斯凱瑞方程式(Scherer equation)確定。當計算晶粒尺寸小於50奈米時，認為該相為奈米晶體。
藉由在氬氣氛中，使用SPEX MILL(8000－D型，Spex CertiPrep,Metuchen,NJ)，用28個碳化鎢磨球(每一者為5/16吋，大約108公克)，在45毫升碳化鎢容器中，研磨所記錄量之矽晶片(Alfa Aesar，目錄號00311)、金屬及石墨粉末(MCMB－1028，MMM Carob,Belgium)4小時而製備在表1A中列出之樣品1－14。接著，打開容器，破碎大塊結塊粉末且在氬氣氛中，繼續再研磨一小時。藉由空氣冷卻，將碳化鎢容器之溫度維持在約30℃下。
在表1A中列出之實例15－16由與實例1－14相同之通用程序，在具有以下差異之情況下製備。使用矽粉末(325篩目；Alfa Aesar，目錄號35662)、錫粉末(<10微米，Aldrich，目錄號520373)及金屬粉末(鈷，1.6微米；Alfa Aesar，目錄號10455C Alfa Aesar；鎳，Alcan Metal Powder，123型)。在氬氣氛下，在SPEX MILL中，用14個碳化鎢磨球(0.415毫米直徑；大約54公克總重量)將實例15及實例16研磨16小時。藉由空氣冷卻，將碳化鎢容器之溫度維持在約30℃下。
將表1A中列出之實例1－16中之每一者形成為電極且在具有鋰金屬反電極之電化學電池中表徵。電極係由以下程序製備。使用四個碳化鎢磨球(12.75 mm直徑)，在45毫升不銹鋼容器中，將量為1.8 g之研磨材料、0.06 g之導電碳(來自MMM Carbon,Belgium之SUPER P)及0.70 g之PI2555(PYRALIN PI2555，來自HD Microsystems,Cheesequake Road,Parlin,NJ之於N－甲基－2－吡咯啶酮中之20重量%溶液)混合。在設定為3之速度下，在行星微型研磨機中(來自Fritsch GmbH,Idon－Oberstein，Germany之PULVERISETTE7)進行混合2小時。隨後，使用具有0.0075吋(76.2微米)間隙之凹口棒體塗覆沖模，將所得溶液塗覆於13微米厚之銅箔上。將塗層在150℃下，在真空烘箱中乾燥2小時，且隨後用以建構由380微米厚之金屬鋰箔反電極、兩層平板聚丙烯薄膜隔離物(來自CELGARD Inc.,Charlotte,NC之CELGARD 2400)及於電解質(來自SynQuest Laboratories of Alachua,Florida之含有90份1：2體積之碳酸乙二酯及碳酸二乙酯之混合物及10份碳酸氟乙二酯之混合物)中之1 M LiPF6 組成的2325紐扣電池(coin cell)。使用前，將此混合物經分子篩(3A型)乾燥12 h。2325紐扣電池硬體在A.M.Wilson及J.R.Dahn,J.Electrochem.Soc ,142,326－332(1995)中描述。
使用電池測定器(Maccor Inc.,Tulsa OK)，將自實例1－16製備之電化學電池在0.9 V與5 mV之間進行循環。在下次充電週期前，在下限電壓下，使得200毫安/公克電流衰減至10毫安/公克。所量測之充電效率及庫侖效率值記錄於表2中。
藉由將65.461公克矽塊(Alfa Aesar/99.999%，目錄號39101)、18.596公克鐵片(AlfaAesar/99.97%，目錄號10454)及15.943公克海綿鈦(Alfa Asear/99.7%，目錄號10582)在ARC爐中熔融而製備實例17。將合金錠(Si7 0 Fe1 0 Ti1 0 )分裂成小塊且在錘磨機中處理以產生150微米尺寸之粉末。在SPEX MILL中，將Si7 0 Fe1 0 Ti1 0 合金粉末(3.8462 g)及石墨(0.1528 g，SFG44/Tim Rex)連同28個碳化鎢磨球(每一者為10.5毫米，總重量為108公克)在充滿氬之45毫升碳化鎢容器(8001型，Spex CertiPrep,Metuchen,NJ)中研磨1小時。在研磨期間，將該容器用空氣射流冷卻。容器溫度在研磨期間為約30℃。
如在實例17中，藉由將3.9409公克由實例17之程序製備之Si7 0 Fe1 0 Ti1 0 合金粉末及0.0591公克石墨在SPEX MILL中研磨而製備實例18。
除使用64.605 g矽塊、27.528 g鐵片及7.867 g海綿鈦製備Si7 0 Fe1 5 Ti5 合金粉末外，由與在實例17中相同之程序製備實例19。隨後，如在實例17中，將3.8481 g之Si7 0 Fe1 5 Ti5 合金粉末及0.1519 g之石墨在SPEX MILL中研磨。
如在實例17中，藉由將3.9417 g由實例19之程序製備之Si7 0 Fe1 5 Ti5 合金粉末及0.0583 g石墨在SPEX MILL中研磨而製備實例20。
將實例17－20中之每一者形成為電極且在具有鋰反電極之電化學電池中表徵。含有實例17－20之電極係由以下程序製備。在設定為1之速度下，在行星微型研磨機中，使用四個碳化鎢磨球(每一者為12.5毫米)，將研磨材料(1.84 g)、導電碳(0.024 g，Ketjen Black,Akzo Nobel)及NMP(2 g)之樣品在45 mL不銹鋼容器中混合30分鐘，隨後添加PYRALIN PI2555(0.68 g，於NMP中之20重量%PI2555固體)且在設定為2之速度下混合1小時。使用安置有125微米間隙之凹口棒體塗覆沖模，將所得溶液塗覆於13微米厚之銅箔上。將塗覆樣品在真空烘箱中，在150℃下乾燥2小時。圓盤(16 mm直徑)係自塗層衝壓。
將自實例17－20製備之塗層在以與實例1相同之方式裝配之2325紐扣電池中測試。除使用250毫安/公克合金之電流密度且在每一半週期之結束，在開路下，使用15分鐘之時期外，將用實例17－20製備之紐扣電池如實例1進行循環。所量測之充電效率及庫侖效率值記錄於表2中。
藉由在550 rpm下，在高衝擊水平研磨機(Simoloyer,CM20－Solm,Zoz.GmbH)中，用25 kg鉻鋼球(5 mm，100Cr6鋼)將903.602 g矽粉末(－100＋325篩目，Globe Metallurgical Inc.,Beverly,OH)、406.307 g鈷(純度99.8%，1.6 μm顆粒，來自Alfa Aesar，目錄號為10455C)、134.885 g鎳粉末(純度99.9%，2－3 μm顆粒，Alfa Aesar，目錄號10255)及55.206 g石墨粉末(Timrex SFG44，TimCal Ltd.,Bodio,Switzerland)研磨45秒且隨後在300 rpm下以重複循環15秒。將實例21研磨共計三小時。除研磨時間分別為5 h及7.5 h外，由與實例21相同之程序製備實例22及23。
將實例21－23中之每一者形成為電極且如在實例17中，在電化學電池中表徵且將該等電池由與實例17相同之程序進行循環。此等實例中之每一者包括包含矽之非晶相。30個循環之後，此等材料中之每一者之比容量(mAh/g)為：實例21為1220；實例22為1050；且實例23為920。
已描述本發明之許多實施例。然而，應瞭解，可進行各種修改而不悖離本發明之精神及範疇。因此，其他實施例係在以下申請專利範圍之範疇內。

Claims (28)

  1. 一種用於鋰離子電池之具有式Six Snq My Cz 之電極組合物，其中q、x、y及z表示原子百分數值且(a)(q+x)>2y+z；(b)x大於0，且x大於或等於z；(c)q及z中之每一者獨立地大於或等於0；且(d)M為一或多種選自錳、鉬、鈮、鎢、鉭、鐵、銅、鈦、釩、鉻、鎳、鈷、鋯、釔或其組合之金屬，其中，Si、Sn、M及C元素係以多相微結構之形式配置，該多相微結構包含：(i)包含矽之非晶相；(ii)包含金屬矽化物之奈米晶相；(iii)當z>0時，包含碳化矽之相；及(iv)當q>0時，包含Sn之非晶相。
  2. 如請求項1之電極組合物，其中M為一或多種選自鈷、鎳、鐵、鈦、鉬、鎢或其組合之金屬。
  3. 如請求項1之電極組合物，其中x60。
  4. 如請求項1之電極組合物，其中z>0。
  5. 如請求項1之電極組合物，其中z10。
  6. 如請求項1之電極組合物，其中z15。
  7. 如請求項1之電極組合物，其中x60且M為一或多種選自鈷、鎳、鐵、鈦、鉬或其組合之金屬。
  8. 如請求項7之電極組合物，其中z>0。
  9. 如請求項7之電極組合物，其中z10。
  10. 如請求項1之電極組合物，其中M包含Co。
  11. 如請求項10之電極組合物，其中z>0。
  12. 如請求項10之電極組合物，其中x60。
  13. 一種鋰離子電池，其包含：一陽極；一陰極；及一電解質，其中該陽極包含具有式Six Snq My Cz 之組合物，其中q、x、y及z表示原子百分數值且(a)(q+x)>2y+z；(b)q大於或等於0；(c)z大於或等於0；(d)M為一或多種選自錳、鉬、鈮、鎢、鉭、鐵、銅、鈦、釩、鉻、鎳、鈷、鋯、釔或其組合之金屬，且(e)x大於0，且x大於或等於z；其中Si、Sn、M及C元素係以多相微結構之形式配置，該多相微結構包含：(i)包含矽之非晶相；(ii)包含金屬矽化物之奈米晶相；(iii)當z>0時，包含碳化矽之相；及(iv)當q>0時，包含Sn之非晶相。
  14. 如請求項13之鋰離子電池，其中M為一或多種選自鈷、鎳、鐵、鈦、鉬、鎢或其組合之金屬。
  15. 如請求項13之鋰離子電池，其中x60。
  16. 如請求項13之鋰離子電池，其中z>0。
  17. 如請求項13之鋰離子電池，其中z10。
  18. 如請求項13之鋰離子電池，其中z15。
  19. 如請求項13之鋰離子電池，其中x60且M為一或多種選自鈷、鎳、鐵、鈦、鉬或其組合之金屬。
  20. 如請求項19之鋰離子電池，其中z>0。
  21. 如請求項19之鋰離子電池，其中z10。
  22. 如請求項13之鋰離子電池，其中M包含Co。
  23. 如請求項22之鋰離子電池，其中z>0。
  24. 如請求項22之鋰離子電池，其中x60。
  25. 如請求項13之鋰離子電池，其中該陽極進一步包含黏合劑及導電稀釋劑。
  26. 如請求項25之鋰離子電池，其中該黏合劑包含聚醯亞胺。
  27. 如請求項25之鋰離子電池，其中該導電稀釋劑包含碳黑。
  28. 如請求項13之鋰離子電池，其中該電解質包含碳酸氟乙二酯(fluoroethylene carbonate)。
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