TWI513083B - 矽或矽基材料組成之纖維的製法及其於鋰充電電池的用途 - Google Patents

矽或矽基材料組成之纖維的製法及其於鋰充電電池的用途 Download PDF

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TWI513083B
TWI513083B TW102115234A TW102115234A TWI513083B TW I513083 B TWI513083 B TW I513083B TW 102115234 A TW102115234 A TW 102115234A TW 102115234 A TW102115234 A TW 102115234A TW I513083 B TWI513083 B TW I513083B
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Mino Green
Feng-Ming Liu
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Description

矽或矽基材料組成之纖維的製法及其於鋰充電電池的用途
本發明乃關於矽或矽基材料組成之纖維的製法，以及關於其做為鋰充電電池之陽極活性材料的用途。
吾人熟知可以使用矽做為可充電之鋰離子電化學電池的活性陽極材料(舉例而言，參見「鋰充電電池的插入電極材料」，M.Winter、J.O.Besenhard、M.E.Spahr、P.Novak發表於Adv.Mater. 1998年10月，第10期)。傳統鋰離子充電電池的基本組成乃顯示於圖1，其包括基於石墨的陽極電極，而這是打算要以矽基陽極所取代的元件。雖然充電電池包含單一電池，但是也可以包含多於一個的電池。
電池一般包括用於陽極10的銅電流收集器以及用於陰極12的鋁電流收集器，它們可以對外連接於負載或充電電源(若適合的話)。石墨基複合陽極層14覆蓋著電流收集器10，而含鋰的金屬氧化物基複合陰極層16覆蓋著電流收集器12。多孔性塑膠間隔物或分隔物20則提供於石墨基複合陽極層14和含鋰的金屬氧化物基複合陰極層16之間，並且液態電解質材料乃分散於多孔性塑膠間隔物或分隔物20、複合陽極層14、複合陰極層16 裡。在某些情況下，多孔性塑膠間隔物或分隔物20可以由聚合性電解質材料所取代；在此情況下，聚合性電解質材料同時存在於複合陽極層14和複合陰極層16裡。
當充電電池是完全充電時，鋰便已經從含鋰的金屬氧化物經 由電解質而輸送到基於石墨的該層裡，在此鋰與石墨反應而產生LiC6 化合物。石墨是複合陽極層裡的電化學活性材料，其最大容量為每公克372毫安培小時。將會注意到：使用「陽極」和「陰極」二詞意味著充電電池乃跨接於負載。
一般相信當使用矽做為鋰離子充電電池的活性陽極材料 時，矽所提供的容量顯著高於目前使用石墨所提供的容量。當矽在電化學電池中與鋰反應而轉換成化合物Li21 Si5 時，其容量為每公克4,200毫安培小時。
現有做法乃使用矽或矽基活性陽極材料於鋰離子電化學電 池中，但其於所需的充電/放電循環次數下無法展現持久的容量，因此商業上並不可行。
一種做法乃使用呈粉末形式的矽，在某些情形中，其與可選 用的電子添加劑做成複合物，以及包含適合的黏結劑(例如聚偏二氟乙烯(PVDF))，再披覆於銅電流收集器上。然而，此電極接受充電/放電循環時無法展現持久的容量。相信此容量損失可歸咎於矽粉末質量發生部分的機械隔離，而這是起因於鋰插入/抽出矽主體所附帶的體積膨脹/收縮。此轉而導致粉末質量聚結成電隔離的「島」。
於Ohara等人在Journal of Power Sources 第136期(2004年)第 303-306頁所述的另一種做法，矽是蒸鍍於鎳箔電流收集器上成為薄膜，然後使用此結構來形成鋰離子電池的陽極。然而，雖然此做法的容量持久性不錯，但是這僅適用於非常薄的膜，因此這些結構的每單位面積所能產生的容量並不實用；若增加膜的厚度以使每單位面積所能產生的容量變得實用，則又喪失了原有不錯的容量持久性。
於美國專利公開案第2004/0126659號所述的另一種做法，矽 是蒸鍍於鎳纖維上，然後使用此纖維來形成鋰電池的陽極。然而，發現此做法在鎳纖維上提供的矽分布不均勻，因而顯著影響其操作。
於美國專利第6,887,511號所述的另一種做法，矽是蒸鍍於 粗糙的銅基材上，以產生高達10微米的中等厚度膜。在起始的鋰離子插入過程期間，矽膜會被打破而形成矽柱狀物。這些柱狀物然後可以可逆地與鋰離子反應，並且達成了良好的容量持久性。然而，此方法對於較厚的膜則表現不佳，並且產生中等厚度膜是昂貴的過程。再者，打破膜所造成的柱狀結構並沒有固有的多孔性，以致長期的容量持久性可能會發生問題。
本發明乃列示於申請專利範圍。因為陽極電極結構使用矽或 矽基材料的纖維，所以克服了這些矽或矽基纖維與鋰可逆反應的問題。尤其是將纖維安排於複合結構中，其係纖維、聚合性黏結劑、電子添加劑的混合物，因而充電/放電過程變成可逆、可重複的，並且達成了良好的容量保持性。此外，纖維佈置的方式可以提供許多優點。藉由提供不規則、非編織的纖維墊，則引入了完全可逆、可重複的充電能力，而無顯著機械隔離的風險。舉例而言，纖維可以沉積成為毛氈或類似毛氈的結構。在複 合結構的情況下，此可帶有額外的元件，或者毛氈可以帶有單純的黏結劑，或者結構上若適合的話亦可為鬆散的。
再者，亦提供一種纖維的簡化製法，其包括：蝕刻基材以產生柱狀物，以及分離此柱狀物；此者提供穩健和高產率的做法。
10‧‧‧陽極(電流收集器)
12‧‧‧陰極(電流收集器)
14‧‧‧石墨基複合陽極層
16‧‧‧含鋰的金屬氧化物基複合陰極層
20‧‧‧多孔性塑膠間隔物或分隔物
圖1是顯示電池元件的示意圖；圖2是根據本發明之電極的放大照片；圖3顯示矽纖維/PVDF/超級P複合電極的第一循環電壓圖。
現在將參考圖式，以舉例的方式來描述本發明的具體態樣。
概括而言，本發明可以產生矽或矽基材料的纖維或細絲，並且可以使用這些纖維來產生複合陽極結構(其帶有聚合性黏結劑、電子添加劑(若需要的話)、金屬箔電流收集器)和類似毛氈的電極結構。尤其相信構成複合物之矽元件的結構克服了充電/放電容量喪失的問題。
藉由將纖維佈置於複合物或毛氈或類似毛氈的結構(其係多個伸長的或長薄形纖維，它們交叉著而提供許多交錯)，舉例而言，是以隨機或不規則或事實上規則的方式所佈置，因而減輕了充電/放電容量喪失的問題。
典型而言，纖維的長度對直徑的比例為大約100：1，因此在陽極層(例如複合陽極層)中，每個纖維沿著其長度會接觸其他纖維許多次，造成的情形是由於破斷的矽接觸所引發之機械隔離的機會可以忽略。 同時，鋰插入和移出於纖維雖然會造成體積膨脹和體積收縮，但是不會破壞纖維，因此保有了纖維內的電子傳導度。
纖維可以從基材分離出柱狀物來製造。此外，製造柱狀物的方式可以由簡單、可重複的化學過程所提供。
一種可以製作柱狀物的方式是乾式蝕刻，例如深度反應性離子蝕刻，舉例而言，其係描述於美國專利申請案第10/049736號，此案與本案為相同申請人，其併入此以為參考。熟於此技術者將會熟悉該方法，所以在此就不須要詳細敘述。但是簡言之，是將披覆了原有氧化物的矽基材加以蝕刻和清洗，以得到親水性表面。氯化銫(CsCl)乃蒸鍍於表面上，而披覆的基材再於乾燥的情形下轉移到具有固定水蒸氣壓的腔室。CsCl薄膜會發展成為半球體的島狀陣列，此半球體的尺寸特徵則取決於起始厚度、水蒸氣壓、發展時間。島狀陣列提供了有效的遮罩，而在此之後例如以反應性離子蝕刻來進行蝕刻，因此留下了對應於半球形島的柱狀物陣列。CsCl阻障層極易溶於水，所以能夠輕易地沖洗掉。
或者是說，柱狀物可以溼式蝕刻/使用化學電流交換方法來製作，舉例而言，其係描述於同樣是本申請人之申請中的英國專利申請案第0601318.9號，標題為「蝕刻矽基材料的方法」，其併入此以為參考。也可以使用的相關方法則描述於Peng K-Q、Yan Y-J、Gao S-P、Zhu J.發表於Adv.Materials 第14期(2004年)第1164-1167頁(“Peng”)；K.Peng等人發表於Angew.Chem.Int.Ed. 第44期第2737-2742頁；以及K.Peng等人發表於Adv.Funct.Mater. 第16期(2006年)第387-394頁。
於較佳的具體態樣中，舉例而言，是從矽基材上製出長度 100微米、直徑0.2微米的柱狀物。更概括來說，可以使用之柱狀物的長度範圍在20到300微米，直徑或最大橫向尺寸範圍在0.08到0.5微米，以提供此纖維。根據本方法，矽基材可以是n型或p型；並且根據化學做法，可以蝕刻於任何暴露的(100)或(110)晶面。由於蝕刻是沿著晶面而前進，故得到的纖維是單晶。因為此結構上的特色，纖維實質上是直的，而有助於使長度對直徑的比例為大約100：1；而當位於複合陽極層中時，則允許每根纖維沿著其長度接觸其他纖維許多次。蝕刻過程也可以進行於超大型積體電路(very large scale integration，VLSI)的電子級晶圓或此類被排拒掉的樣品(單晶晶圓)上。就比較便宜的替代選擇來說，也可以使用光伏特級的多晶材料，如太陽能面板所使用的。
為了分離柱狀物以獲得纖維，附著有柱狀物的基材乃置於燒杯或任何適當的容器裡，而以鈍性液體(例如乙醇)加以淹蓋，然後接受超音波攪動。發現在幾分鐘以內就可看到液體變得混濁，並且以電子顯微鏡檢查可以看到柱狀物在此階段便已從矽基材上移除了。
也將體會出「收割」柱狀物的其他可選擇方法包括了擦刮基材表面以分離之，或採化學方式分離。一種適合n型矽材料的化學做法包括在矽晶圓背面照光的情況下於HF溶液中蝕刻基材。
一旦矽柱狀物已分離出來，它們可以用於鋰離子電化學電池而做為複合陽極的活性材料。為了製造複合陽極，收割的矽從溶液過濾出來，並且可以與聚偏二氟乙烯混合，並與鑄造溶劑(例如n-甲基比咯酮(NMP))形成漿液。此漿液然後可以施加或塗覆於金屬板或金屬箔或其他導電基材上，舉例而言，實體上是以刮刀或任何其他適合的方式來為之，以產出所 需厚度的披覆膜；然後使用合適的乾燥系統(其可以採用溫度範圍在50℃到140℃的高溫)，把鑄造溶劑從此膜蒸發掉，而使複合膜沒有或實質上沒有鑄造溶劑。所得的墊或複合膜具有多孔的和/或類似毛氈的結構，其中矽纖維的質量典型是在70%到95%之間。複合膜的孔洞體積百分率為10到30%，最好是大約20%。
上述方法所得到之複合電極結構的SEM照片乃顯示於圖2。或者是說，毛氈或類似毛氈的結構可以製成片狀材料(未必是在電流收集器上)，而自己做為電流收集器。
之後可以任何適當的方式來製造鋰離子充電電池，舉例而言，依照圖1所示的一般結構，不過是用矽或矽基的活性陽極材料而非石墨的活性陽極材料。舉例來說，矽纖維基複合陽極層是以多孔性間隔物20所覆蓋，電解質則加入最後的結構裡，而充滿著所有可用的孔洞體積。電解質的添加是在電極置於適合的箱殼後才進行，並且可以包含真空填充此陽極，以確保孔洞體積填滿了液態電解質。
請參見以下範例：稱出重0.140公克的矽纖維放入2平方公分的Eppendorf離心管裡，並且加入0.0167公克的超級P導電碳。然後把N-甲基比咯酮(NMP)藉由移液管倒入離心管裡，直到所有的材料都分散為止(0.92公克)。事先已將PVDF溶解於NMP，PVDF佔7.8重量%。將此溶液加入管中，其包含0.0074公克的PVDF。混合組成物因此是Si：PVDF：超級P=85.3：4.5：10.1重量%。
管子置於超音波浴中一小時，以使混合物均勻，然後再攪拌 一小時。接著使用刮刀間隙為0.8毫米的刮刀，把漿液披覆於14微米的銅箔上。披覆物然後在100℃的烤箱中乾燥一小時以蒸發NMP溶劑。乾燥之後，披覆層的厚度為30到40微米。圖2顯示類似混合物和披覆的SEM照片，而沒有超級P碳。
披覆物經過輕微地滾壓，然後切出直徑12毫米的電極碟。 它們在充滿氬氣的手套箱中組裝於電化學電池裡。反電極和參考電極都是鋰金屬。電解質是LiPF6 溶於有機碳酸鹽混合物。電池是在VMP3裝置上測試。三十分鐘浸泡之後，電池維持在-0.1毫安培達一小時，然後維持在-0.2毫安培直到達到了所需的鋰化容量。電極然後在+0.2毫安培下脫鋰，最高達到1.0伏特的電壓(相對於Li/Li+ )。圖3顯示在此第一循環期間的電池電壓。
此處所述做法的一項特別優點就是可以製作大片的矽基陽極，如果須要的話再加以滾壓，然後切成長條或打印出來，就如同目前鋰離子電池之石墨基陽極的做法；這意味著此處所述的做法可以相容於既有的製造能力。
在此所述排列的進一步優點在於結構的強度事實上會隨著每次充電操作而增強。這是因為發現纖維乃彼此「焊接」在一起，而這是由於破裂的結晶結構在纖維連接處產生非晶形結構的結果。此轉而降低了多次循環後喪失容量的風險，因為一旦纖維以上述方式變成連接在一起，則纖維發生機械隔離的風險就比較少。
當然將體會可以採取任何適當的做法，以便達到上述的目的和裝置。舉例而言，分離柱狀物的作業可以包括搖晃、擦刮、化學或其他 操作其中的任一種，只要柱狀物從基材移開以產生纖維即可。若適合的話，參考矽基材料的材料也包括矽。纖維可以具有任何適當的尺寸，並且例如可以是純矽或摻雜的矽或其他矽基材料，譬如矽鍺混合物或任何其他適合的混合物。產生柱狀物的基材可以是n型或p型，範圍從100到0.001歐姆公分，或者它可以是適合的矽合金，譬如Six Ge1-x 。纖維可以用於任何適當的目的，例如製造一般包括陰極在內的電極。陰極材料可以是任何適當的材料，典型則為鋰基金屬氧化物或磷酸鹽材料，例如LiCoO2 、LiMnx Nix Co1-2x O2 或LiFePO4 。若適合的話，不同具體態樣的特色可以交換或並存，並且方法的步驟可以任何適當的次序來進行。

Claims (17)

  1. 一種用於鋰充電電池的電極結構，該電極結構包含：多個伸長的含矽纖維，其中該含矽纖維交叉著而提供許多交錯；以及黏結劑和電子添加劑中之至少一者，其中該伸長的含矽纖維以及黏結劑和電子添加劑中之至少一者共同定義多孔性複合電極層。
  2. 如請求項1之電極結構，其中該纖維係以隨機或不規則的方式所安排。
  3. 如請求項1或2之電極結構，其中安排該結構以在充電和放電期間保有纖維內的電子傳導度。
  4. 如請求項1或2之電極結構，其中該結構使得由於破斷的纖維接觸所引發之機械隔離的機會可以忽略。
  5. 如請求項1或2之電極結構，其中該交錯包含破裂的結晶結構，可選擇地，其中該破裂的結晶結構包含非晶形結構。
  6. 如請求項1或2之電極結構，其中該纖維是結晶的。
  7. 如請求項1或2之電極結構，其中該纖維實質上是直的。
  8. 如請求項1或2之電極結構，其中該結構係毛氈或類似毛氈的結構。
  9. 如請求項8之電極結構，其中該毛氈或類似毛氈的結構係片狀材料。
  10. 如請求項1或2之電極結構，其中該纖維係經蝕刻纖維。
  11. 如請求項第8之電極結構，其中該結構係進一步作為自己本身的電流收集器。
  12. 如請求項9之電極結構，其中該結構係進一步作為自己本身的電流 收集器。
  13. 如請求項1或2之電極結構，其中該纖維具有範圍在0.08到0.5微米的橫向尺寸。
  14. 如請求項1或2之電極結構，其中該纖維具有範圍在20到300微米的長度。
  15. 如請求項1或2之電極結構，其中該纖維包含n型或p型摻雜的矽。
  16. 一種電化學電池或鋰電池，其包含請求項1至15中任一項之電極結構。
  17. 一種電池電極的製法，其包含沉積包含矽基纖維的漿液，以形成一層矽基纖維。
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