TWI458157B - 製造包括矽或以矽為主材料之結構化粒子之方法或其在鋰充電電池之用途 - Google Patents
製造包括矽或以矽為主材料之結構化粒子之方法或其在鋰充電電池之用途 Download PDFInfo
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- TWI458157B TWI458157B TW097127137A TW97127137A TWI458157B TW I458157 B TWI458157 B TW I458157B TW 097127137 A TW097127137 A TW 097127137A TW 97127137 A TW97127137 A TW 97127137A TW I458157 B TWI458157 B TW I458157B
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- particles
- particle
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- ruthenium
- lithium
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- 239000002245 particle Substances 0.000 title claims abstract description 131
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims description 34
- 229910052744 lithium Inorganic materials 0.000 title claims description 34
- 238000004519 manufacturing process Methods 0.000 title claims description 13
- 239000002210 silicon-based material Substances 0.000 title abstract description 4
- 229910052710 silicon Inorganic materials 0.000 title abstract 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title 1
- 239000010703 silicon Substances 0.000 title 1
- 239000002131 composite material Substances 0.000 claims abstract description 33
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims description 44
- 229910052707 ruthenium Inorganic materials 0.000 claims description 44
- 238000000034 method Methods 0.000 claims description 34
- 238000005530 etching Methods 0.000 claims description 27
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims description 15
- 229910001416 lithium ion Inorganic materials 0.000 claims description 15
- 239000010949 copper Substances 0.000 claims description 11
- 239000000835 fiber Substances 0.000 claims description 11
- 239000011149 active material Substances 0.000 claims description 10
- 239000013078 crystal Substances 0.000 claims description 10
- 229910052802 copper Inorganic materials 0.000 claims description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 7
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- 229910052684 Cerium Inorganic materials 0.000 claims description 6
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
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- 150000001875 compounds Chemical class 0.000 claims description 5
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- 239000010452 phosphate Substances 0.000 claims description 3
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- 238000001704 evaporation Methods 0.000 claims description 2
- 239000011855 lithium-based material Substances 0.000 claims description 2
- BFZPBUKRYWOWDV-UHFFFAOYSA-N lithium;oxido(oxo)cobalt Chemical compound [Li+].[O-][Co]=O BFZPBUKRYWOWDV-UHFFFAOYSA-N 0.000 claims description 2
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- 229910052782 aluminium Inorganic materials 0.000 description 3
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- 101710134784 Agnoprotein Proteins 0.000 description 2
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- 241001674044 Blattodea Species 0.000 description 1
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- 101100136092 Drosophila melanogaster peng gene Proteins 0.000 description 1
- 229910052693 Europium Inorganic materials 0.000 description 1
- 229910016703 F—Si—F Inorganic materials 0.000 description 1
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Classifications
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Description
本發明係關於包含矽之粒子、製造粒子之方法、包含粒子作為其活性材料之電極、電化學電池、鋰充電電池陽極、電池、藉電池供給電力之裝置、製造複合電極之方法、製造鋰充電電池之方法及製造包含矽的纖維之方法。
可攜式電子裝置(如,行動電話和筆記型電腦)之使用日增及顯現之充電電池用於混合電子載具的趨勢已創造出對於提供電力至前述和其他電池電力裝置之較小、較輕、較持久的充電電池之需求。1990年代的期間內,鋰充電電池,特別是鋰離子電池,變得被廣為使用且,以銷售單位來看,目前主宰可攜式電子市場並開始被用於新穎、價格敏感的應用上。然而,隨著越來越多需要電力需求的功能加諸於前述裝置(如,行動電話上的相機),需要每單位質量和每單位體積儲存更多電力之經改良和減低成本的電池。
熟知矽可作為充電式鋰離子電化學電池之活性陽極材料(請參考,例如,Insertion Electrode Materials for Rechargeable Lithium Batteries, M. Winter, J.O. Besenhard, M. E. Spahe, and P. Novak, Adv. Mater. 1998, 10, No.10)。慣用之鋰離子充電電池組電池之基本元件示於圖1,其包括以石墨為基礎的陽極,此元件被以矽為基礎的陽極所替代。此電池組電池包括單一電池,但亦可包括超過一個電
池。
此電池組電池通常包含用於陰極的銅電流收集器10和用於陰極的鋁電流收集器12(適當時,其外部可連接至承載或充電電源)。以石墨為基礎的複合陽極層14覆蓋電流收集器10且以含鋰的金屬氧化物為基礎的複合陰極層16覆蓋電流收集器12。使多孔塑膠間隔物或分隔物20介於以石墨為基礎的複合陽極層14和以含鋰的金屬氧化物為基礎的複合陰極層16之間且液態電解質材料分散於多孔塑膠間隔物或分隔物20、複合陽極層14和複合陰極層16之內。一些例子中,此多孔塑膠間隔物或分隔物20可被聚合物電解質材料所替代且在此情況下,聚合物電解質材料存在於複合陽極層14和複合陰極層16二者之內。
當電池組電池完全充電,鋰自含鋰的金屬氧化物經由電解質運送至以石墨為基礎的層,於此處與石墨反應而製造化合物LiC6
。此石墨,係複合陽極層中的電化學活性材料,具有最大容量為372毫安培小時/克。將注意到此處所謂的”陽極”和”陰極”以橫跨承載物的方式放置。
一般相信矽在作為鋰離子充電電池的活性陽極材料時,相較於目前所用的石墨,提供明顯較高容量。矽藉由與電化學電池中的鋰反應而轉化成化合物Li21
Si5
時,具有最大容量為4,200毫安培小時/克,明顯高於石墨的最大容量。因此,如果鋰充電電池中的石墨可以矽代替,則可達到提高所欲之每單位質量及每單位體積的儲存電力。
在鋰離子電化學電池中使用矽或以矽為基礎的陽極材
料之已有的發展無法在所需的充電/放電循環次數展現持續的容量並因此而無法用於商業上。
此技術所揭示的一個研究使用粉末形式的矽(直徑約10微米的粒子或球狀元件),在一些例子中,使用或未使用電子添加劑及含有適當黏合劑(如,塗佈在銅電流收集器上的聚偏二氟乙烯(polyvinylidene difluoride))地製成複合材料。然而,當用於重覆充電/放電循環時,此電極系統無法展現持續的容量。咸信此容量耗損係與鋰自主體矽嵌入/脫出(insertion/extraction)有關的體積膨脹/收縮而造成矽粉末物質的部分機械分離所致。此亦導致矽元件與銅電流收集器和它們本身二者電隔絕。此外,體積膨脹/收縮造成球狀元件破裂,導致球狀元件本身內部的電接觸損耗。
此技術中已知的另一研究設定為處理連續循環期間內的大體積改變之問題,其使得構成矽粉末的矽元件非常小,即,使用直徑在1-10奈米範圍內的球狀粒子。此策略假設奈米尺寸的元件可驅動與鋰嵌入/脫出有關之大的體積膨脹/收縮但不會破裂或受損。但此研究的問題在於其須要處理可能具有健康和安全風險之非常細、奈米尺寸的粉末且因為矽粉末驅動與鋰嵌入/脫出有關的體積膨脹/收縮,所以其無法防止球狀元件與銅電流收集器和本身之電隔離。重要地,奈米尺寸元件的大表面積會製造含鋰的表面膜,此導致大的不可逆容量進入鋰離子電池組電池。此外,大量的小矽粒子製造指定量的矽之大量的粒子
一粒子接觸且此等每一者具有接觸阻力並會因此而造成矽物質的電阻過高。前述問題使得矽粒子無法成為鋰充電電池(特別是鋰離子電池)中的石墨之商業上可利用的替代品。
Ohara等人於Journal of Power Sources 136 (2004)303-306中所描述的另一研究中,矽在鎳箔電流收集器上蒸發成薄膜且此結構於之後用以形成鋰離子電池的陽極。然而,雖然此研究提供良好的容量保持率,此僅為非常薄的膜(約50奈米)之情況且因此,這些電極結構未提供每單位面積有用的容量。提高膜厚度(約>250奈米)造成良好的容量保持率消失。本發明者認為此等薄膜之良好的容量保持率與薄膜吸收與主體矽之鋰嵌入/脫出有關的體積膨脹/收縮且膜不會破裂或受損之能力有關。此外,薄膜的表面積比對等質量之奈米尺寸的粒子小得多,因此,因為形成含鋰的表面膜而造成之不可逆容量降低。因此,前述問題使得金屬箔片電流收集器上的矽薄膜無法在商業上取代鋰充電電池(特別是鋰離子電池)中的石墨。
另一研究描述於US2004/0126659中,矽蒸發於鎳纖維上,其於之後用以形成鋰電池的陽極。
然而,發現矽於鎳纖維上之分佈不均並因此而明顯影響操作。此外,這些結構具有高的鎳電流收集器質量/活性矽質量比並因此而無法提供每單位面積或每單位質量之有用量的容量。
用於鋰離子二次電池之以奈米和整體矽為基礎的嵌入
陽極之回顧由Kasavajjula等人提出(J. Power Sources (2006), doi:10.1016/jpowsour.2006.09.84),茲將其以引用方式納入本文中。
UK專利申請案GB2395059A中描述的另一研究使用矽電極,其包含在矽基板上製造之矽導柱的規則或不規則陣列。在施以重覆充電/放電循環時,這些結構化的矽電極展現良好的容量保持率,且本發明者認為此良好的容量保持率源自於矽導柱吸收與主體矽之鋰嵌入/脫出有關的體積膨脹/收縮且膜不會破裂或受損之能力有關。然而,前述申請案中所描述之此結構化的矽電極係藉由使用高純度的單晶矽晶圓製造,因此,電極之製造具有潛在的高成本。
本發明的第一方面提供一種包含矽之粒子,該粒子具有粒子核和自彼延伸之包含矽的導柱陣列。
此導柱可為規則的或不規則。本發明之導柱的一維為0.08至0.70微米,以0.1至0.5微米為佳,0.2至0.4微米更佳,且0.3微米或較高最佳。第二維中,此導柱為4至100微米,以10至80微米為佳,30微米或較高更佳。藉此,此導柱的縱橫比大於20:1。此導柱可以具有實質上圓形的截面或實質上非圓形的截面。
此導柱粒子可包含未經摻雜的矽、經摻雜的矽或混合物,如,矽-鍺混合物。特別地,此粒子可具有矽純度為90.00至99.95質量%,以90.0至99.5%為佳。此矽可摻有
任何材料,例如,磷、鋁、銀、硼和/或鋅。此粒子可為相當低純度之冶金等級的矽。
此粒子之截面可為規則或不規則且直徑可由10微米至1毫米,以20微米至150微米為佳,25微米至75微米更佳。
本發明的第二方面提供一種製造第一方面之粒子之方法,其步驟包含蝕刻包含矽的粒子。特別地,此導柱可藉化學反應蝕刻或電流交換蝕刻而製造。
本發明的第三方面提供一種複合電極,其含有本發明的第一方面中所定義之粒子作為其活性材料之一。特別地,此第三方面提供使用銅作為電流收集器的複合電極。第三方面的特徵中,此電極係陽極。
因此,此第三方面進一步提供一種電化學電池,其含有前述定義之電極。特別地,提供一種電化學電池,其中陰極包含能夠釋出和再吸收鋰離子作為其活性材料之含鋰的化合物。特別地,提供一種電化學電池,其中陰極包含以鋰為基礎的金屬氧化物、硫化物或磷酸鹽作為其活性材料,以LiCoO2
或LiMnx
Nix
Co1-2x
O2
或LiFePO4
為佳。
本發明進一步提供一種鋰充電電池陽極,其包含第一方面的粒子。特別地,提供一種陽極,其中的粒子為複合材料的一部分。
第三方面進一步提供一種包含陽極和陰極的電池,其中陰極以包含以鋰為基礎的材料為佳,二氧化鋰鈷更佳。
進一步提供一種裝置,其由前述電池提供電力。
本發明的第四方面提供一種製造複合電極之方法,其步驟包含製造含有導柱粒子之以溶劑為基礎的漿料,將此漿料塗佈在電流收集器上及蒸發此溶劑以製造複合膜。
本發明進一步提供製造鋰充電電池之方法,其步驟包含製造前述定義之陽極和添加陰極和電解質。特別地,此方法進一步包含在陰極和陽極之間增添分隔器。可以提供套管環繞電池。
亦提供一種製造包含矽之纖維之方法,其中導柱與第一方面之粒子藉刮擦、攪動或化學蝕刻中之一或多者分離。
使用本發明之結構化的粒子製造陽極電極結構進一步克服了矽與鋰之可逆性反應之問題。特別地,藉由將粒子置於複合結構中,粒子、聚合物黏合劑和導電性添加劑之混合物或結構化的粒子直接結合至電流收集器,此充電/放電方法成為可逆方法並可得到重覆及良好的容量保持率。本發明者認為此良好的可逆性與形成一部分結構化的矽粒子之矽導柱吸收與主體矽之鋰嵌入/脫出有關的體積膨脹/收縮且導柱不會破裂或受損之能力有關。重要地,本發明中所描述的矽電極係藉由使用低純度、冶金等級的矽製造並因此而以潛在低成本製造電極。
現將藉由實例及參考圖示地描述本發明之具體體例,圖示中:圖1為顯示電池組電池的之元件之圖示;
圖2為根據本發明之具體實例之導柱粒子的電子顯微照片;圖3所示者為總電流交換蝕刻機構;和圖4所示者為電流交換蝕刻法中之部分電流形式的假設動力曲線。
總而言之,本發明得以製造矽或含矽材料之導柱粒子及使用這些粒子製造具有聚合物黏合劑、導電性添加劑(若須要)和金屬箔片電流收集器之複合陽極結構,和電極結構二者。特別地,咸信構成複合材料之粒子結構克服了充電/放電容量損耗的問題。藉由提供具有多個拉長或長薄導柱之粒子,減少充電/放電容量損耗的問題。
基本上,此導柱將具有長與直徑比約20:1。鋰嵌入導柱或自導柱脫出,雖然會造成體積膨脹和體積收縮,但不會使得導柱被破壞,並因此而得以保留纖維內的導電性。
藉濕蝕刻/使用化學電流交換法(例如,述於相同受讓人之同在申請中的申請案GB 0601318.9,其標題為"Method of etching a silicon-based material",茲將該案以引用方式納入本文中),可以在粒子上形成此導柱。可使用之相關的方法揭示於Peng K-Q, Yan, Y-J Gao S-P, Zhu J., Adv. Materials, 14 (2004), 1164-1167 ("Peng");K. Peng等人,Angew. Chem. Int. Ed., 44 2737-2742;和K. Peng等人,Adv. Funct. Mater., 16 (2006), 387-394;K. Peng, Z. Huang and J. Zhu, Adv. Mater., 16 (2004), 127-132;及T. Qui, L.
Wu, X. Yang, G. S. Huang and Z. Y. Zhang, Appl. Phys. Lett., 84 (2004), 3867-3869.。前述方法用以自高純度矽晶圓製造導柱。
在本發明的較佳具體實例中,於相當低純度的矽(如,冶金等級的矽)的晶狀粒子上製造導柱。此方法包含五個步驟:研磨和過篩;清洗;成核;蝕刻;和銀移除,其僅以實例於下文中解釋。根據本發明製造之導柱粒子的電子顯微照片示於圖2。
任何適當的研磨方法(如,電力研磨或球磨)適用。嫻於此項技術者將瞭解最小粒子尺寸係低於此值時,導柱無法於表面上蝕刻而是粒子會被均勻地蝕去。直徑低於0.5微米的粒子可能過小。
更均勻的導柱陣列,以密度和高度而言,係在蝕刻之前的成核中製得。此步驟製造銀核/島之均勻分佈(核合併並形成銀島,此銀島為導柱生長之處)。
銀島劃出形成導柱之輪廓並以電流氟蝕刻{100}平面:參考圖3。參考圖3,顯示矽表面301具有導柱307。電子305自氟離子303轉移至矽表面301。氟與矽301和氟離子303之反應形成氟矽酸鹽離子305。此為陽極蝕刻法。此陰極法釋放銀離子309而製得金屬銀311。
以蝕刻法中的基本步驟形成矽-氟鍵結為前提地解釋此結構。進一步地,結構為Si-F(單氟化物)則安定而F-Si-F(二氟化物)和Si[-F]3
(三氟化物)則不安定。此因最鄰近的基團的Si表面上之立體干擾之故。以{111}平面為例,單
氟化物表面安定但在邊緣處,無可避免地成為三氟化物表面並因此而不安定。{110}表面係Si之唯一安定的主要晶體平面,其僅具有單氟化物鍵結,因此其安定性和蝕刻率比[蝕刻率<100>]:[蝕刻率<110>]約3倍。因此,導柱側將在{110}平面上終止。
導柱表面密度可用以定義導柱在粒子表面上之密度。此處,定義為F=P/[R+P],其中:F為導柱表面密度;P為導柱所佔據的粒子總表面積;而R是導柱未佔據的粒子總表面積。
導柱表面密度越大,每單位面積矽粒子電極的鋰容量越大且可獲取之可用以製造纖維的導柱的量越大。
例如,使用前述得自挪威Elken之蝕刻前尺寸為400 x 300 x 200微米的矽粉末,在全表面上製得的導柱之導柱高度約25至30微米,直徑約200至500奈米和導柱表面密度,F,為10-50%,更常是30%。
例如,發現蝕刻前尺寸約63-80 x 50 x 35微米的粒子製得高度約10至15微米的導柱,覆蓋率約30%且直徑約200至500奈米。
在一較佳的具體實例中,長度100微米且直徑0.2微米的導柱在含矽的粒子上自含矽的粒子製得。更通常地,長度在4至100微米範圍內和直徑或截面尺寸在0.08至0.70微米範圍內的導柱自初尺寸為10至1000微米的粒子製得。
根據此方法,此矽粒子可以主要為n-或p-型且,根據
化學研究,並可在任何外露的(100)、(111)或(110)晶體面上蝕刻。由於蝕刻延著晶體平面進行,所以所得的導柱為單晶。因為此結構特徵,此導柱實質上筆直,有利於使得長度與直徑比大於20:1。
如下文所述者,導柱粒子可於之後用以形成複合電極。或者,此導柱可與粒子分離並用以形成以纖維為基礎的電極。此經分離的導柱亦可以纖維描述。
本發明包括導柱與粒子之分離。可將此附有導柱的粒子置於燒杯或任何適當的容器中,以惰性液體(如,乙醇或水)覆蓋並施以超音波振盪。發現在數分鐘之內,液體呈現混濁且可於此階段藉電子顯微鏡檢視導柱是否已自粒子分離。
一具體實例中,在二階段法中,導柱自粒子移出。第一階段中,粒子在水中清洗數次並,若需要,在低真空系統中乾燥以移除水。在第二階段中,粒子在超音波浴中攪動以與導柱分離。這些懸浮於水中並於之後使用不同的眾多濾紙尺寸過濾以收集矽纖維。
應瞭解的是用於”獲取”導柱之替代方法包括刮擦粒子表面以使其分離或以化學方式使其分離。一適用於n-型矽材料之化學方法包含在背側照明存在時,在HF溶液中蝕刻此粒子。
一旦製得導柱粒子,它們可被用來作為鋰離子電化學電池用之複合陽極的活性材料。欲製造複合陽極,此導柱粒子與聚偏二氟乙烯混合並與澆鑄溶劑(如,正-甲基吡咯
啉酮)製成漿料。之後可將此漿料施用或塗覆於金屬板或金屬箔片或其他傳導基板上(例如,以物理方式以刮刀或以任何其他適當的方式),以得到具所須厚度之經塗佈的膜,之後使用適當的乾燥系統(其可使用在50℃至140℃之提高的溫度範圍)自此膜蒸發澆鑄溶劑,以留下無或實質上無澆鑄溶劑的複合膜。所得的複合膜具有多孔結構,其中,以矽為基礎的導柱粒子的量基本上介於70%和95%之間。此複合膜的孔隙體積百分比將為10-30%,以約20%為佳。
之後,可以任何適當的方式(例如,依循圖1中所示的一般結構,但使用含矽的活性陽極材料而非石墨活性陽極材料)製造鋰離子電池組電池。例如,此以矽粒子為基礎的複合陽極層以多孔間隔物18覆蓋,電解質加至最終結構,飽和所有可資利用的孔隙體積。此電解質之添加係於將電極置於適當套管中之後進行且可包括陽極之真空充填,以確保孔隙體積被液態電解質所填滿。
一些具體實例提供含有大量導柱矽粒子作為其活性材料之電極。因為導柱矽結構得以因應與鋰的嵌入/脫出有關的體積膨脹,所以使得容量保持率獲得改良。有利地,此導柱粒子可藉由蝕刻低純度矽塊(冶金等級的矽),使得矽核仍被直徑介於0.08微米和0.5微米之間且長度介於4微米和150微米之間的導柱所覆蓋的方式製得。
此處所描述之研究的一個特別的優點在於可製得大片之以矽為基礎的陽極且於之後滾軋或於之後壓印,此如同目前之用於鋰離子電池組電池之以石墨為基礎的陽極之情
況,此意謂此處所述之研究可更新已有的製造性。
現將藉由參考下列非限制例之一或多者地說明本發明:
第一階段中,易取得的冶金等級矽,如,挪威Elkem的"Silgrain",經研磨和過篩以製得在10至1000微米範圍內,以30至300微米為佳且50至100微米更佳的粒子。
第二階段包含在水中清洗經研磨和過篩的粒子以移除黏在大粒子上的任何細微粒子。之後,經清洗的粒子在經稀釋的HNO3
(1莫耳‧升)或H2
SO4
/H2
O2
(體積比1:2)或H2
O2
/NH3
H2
O/H2
O2
(體積比1:1:1)中處理10分鐘,以去除可能的有機或金屬雜質。
在第三階段中,在17.5毫升HF (40%)+20毫升AgNO3
(0.06莫耳/升)+2.5毫升EtOH (97.5%)+10毫升H2
O的溶液中,使用0.1克尺寸約400 x 300 x 200微米的矽粒子,於室溫(~23℃)進行為時7~10分鐘之成核反應。用於相同重量的矽,較小的矽粒子因為表面積與體積比提高,所以需要較大的溶液體積。
乙醇於室溫之影響係減緩化學程序,此使得銀島之分佈較為均勻。時間(特別是於上限值)足以消耗明顯量的銀溶液。
第四個階段包含蝕刻。此蝕刻反應於室溫(~23℃)使用17.5毫升HF (40%)+12.5毫升Fe(NO3
)3
(0.06莫耳‧升)+2毫升AgNO3
(0.06莫耳‧升)+18毫升H2
O達1~1.5小時,其使用0.1克尺寸約400 x 300 x 200微米的矽粒子。用於相同重量的矽,較小的矽粒子因為表面積與體積比提高,所以需要較大的溶液體積。此外,隨著粒子尺寸降低,較小矽粒子所須時間較短,例如,30分鐘用於100~120微米(篩尺寸)樣品而20分鐘用於63~80微米樣品。
進一步的修飾中,由於釋出氫,所以攪拌可能提高蝕刻速率。此處,氟矽酸鹽離子的向外擴散限制了速率。
嫻於此技術者將瞭解Ag+
以外的氧化劑亦適用。例如:K2
PtCl6
;Cu(NO3
)2
;Ni(NO3
)2
;Mn(NO3
)2
;Fe(NO3
)3
;Co(NO3
)2
;Cr(NO3
)2
;Mg(NO3
)2
。包含Cu和Pt之化合物,具有高於氫的潛能,使得金屬沉積(Cu和Pt),但其他者(Ni除外)則不具此潛能。
可以使用圖3和4說明總電流交換蝕刻機構。圖3中,陽極法,Si+6F-
=SiF6 2-
+4e-
(-1.24伏特)
為矽之局部蝕刻。移除電子伴隨釋出銀離子係陰極法Ag+
+e-
=Ag (+0.8伏特)
用於標準條件,總電池電位是2.04伏特。感興趣的其他陰極對偶為Cu/Cu2+
(+0.35伏特);PtCl6 2-
/PtCl4 2-
(+0.74伏特);Fe3+
/Fe2+
(+0.77伏特),此由於它們相對於氫皆為正之故。比H+
/H2
為負的對偶會與氫競爭且大多無效。圖
4所示者為部分電極反應之變化圖。
方法的最終階段包含移除留在來自第三和第四階段之經蝕刻的矽粒子上的銀。使用15% HNO3
溶液達5~10分鐘以移除(並儲存)此銀。
當然,應瞭解的是,可以採用任何適當的方式以完成前述研究或裝置。例如,導柱分離操作可包含振盪、刮擦、化學或其他操作中之任何者,只要可自粒子移除導柱即可。此粒子可以具有任何適當的尺寸且除了含矽的材料(如,矽-鍺混合物或任何其他適當的混合物)以外,可為,例如,純淨的矽或經摻雜的矽。用以製造導柱的粒子可為n-或p-型,範圍由100至0.001歐姆公分,或其可為適當的矽合金,例如,Six
Ge1-x
。此粒子可為冶金等級的矽。
此粒子和/或經分離的導柱可用於任何適當目的,如,製造電極,此通常包括陰極。此陰極材料可為任何適當材料,基本上是以鋰為基礎的金屬氧化物或磷酸鹽材料,如,LiCoO2
、LiMnx
Nix
Co1-2x
O2
或LiFePO4
。不同具體實例之特徵可適當地互換或並列且此方法之步驟可以任何適當的順序進行。
雖然相對高純度的矽單晶晶圓可經蝕刻而製造所欲參數的導柱,此晶圓本身由於其高純度而非常昂貴。此外,難以將導柱晶圓置於電極幾何形狀中。本發明之具體實例因為冶金等級的矽相當便宜且導柱粒子本身可摻於複合電極中且無須進一步加工而有利。此外,導柱粒子為矽纖維
的良好來源且本身可以作為電池電極中之”活性”元件。
用於蝕刻的粒子可為晶狀,例如,單晶或多晶,其晶粒尺寸等於或大於所須的導柱高度。此多晶粒子可包含任何數目(二或更多)的晶體。
有利地,冶金等級的矽因為缺陷密度相當高(相較於半導體工業中使用的矽晶圓),所以特別適合作為電池電極。此導致低電阻和因此而導致高導電性。
如嫻於此技術者將瞭解者,n-型和p-型矽二者可經蝕刻且只要材料不會明顯變質,任何電荷密度的電荷載體皆適用。
10‧‧‧陽極銅電流收集器
12‧‧‧陰極鋁電流收集器
14‧‧‧以石墨為基礎之複合陽極層
16‧‧‧以含鋰金屬氧化物為基礎之複合陰極層
20‧‧‧多孔塑膠間隔物或分隔物
301‧‧‧矽表面
303‧‧‧氟離子
305‧‧‧電子
307‧‧‧導柱
309‧‧‧銀離子
311‧‧‧金屬銀
圖1為顯示電池組電池的之元件之圖示;圖2為根據本發明之具體實例之導柱粒子的電子顯微照片;圖3所示者為總電流交換蝕刻機構;和圖4所示者為電流交換蝕刻法中之部分電流形式的假設動力曲線。
Claims (47)
- 一種包含矽之粒子,該粒子具有粒子核和自彼延伸之包含矽的導柱陣列,其中每一個導柱的第一端直接接附於粒子核表面且實質上由此徑向延伸。
- 根據申請專利範圍第1項之粒子,其中陣列係規則的。
- 根據申請專利範圍第1項之粒子,其中陣列係不規則的。
- 根據申請專利範圍第1至3項中任一項之粒子,其中導柱具有第一維小於0.70微米。
- 根據申請專利範圍第1至3項中任一項之粒子,其中導柱具有第一維在0.08至0.70微米的範圍內。
- 根據申請專利範圍第1至3項中任一項之粒子,其中導柱具有第二維小於100微米。
- 根據申請專利範圍第1至3項中任一項之粒子,其中導柱具有第二維在4至100微米的範圍內。
- 根據申請專利範圍第1至3項中任一項之粒子,其中導柱的縱橫比大於6:1。
- 根據申請專利範圍第1至3項中任一項之粒子,其中導柱的縱橫比大於20:1。
- 根據申請專利範圍第1至3項中任一項之粒子,其中導柱具有實質上圓形的截面。
- 根據申請專利範圍第1至3項中任一項之粒子,其中導柱具有實質上非圓形的截面。
- 根據申請專利範圍第1至3項中任一項之粒子,其中粒子和/或導柱包含未經摻雜的矽、經摻雜的矽或矽鍺混合物。
- 根據申請專利範圍第1至3項中任一項之粒子,其中矽含量為90.00至99.95質量%,以90.0至99.5%為佳。
- 根據申請專利範圍第1至3項中任一項之粒子,其中粒子為冶金等級的矽。
- 根據申請專利範圍第1至3項中任一項之粒子,其具有規則的截面。
- 根據申請專利範圍第1至3項中任一項之粒子,其具有不規則的截面。
- 根據申請專利範圍第1至3項中任一項之粒子,其具有第一維為10微米至1毫米,以20微米至150微米為佳,25微米至75微米更佳。
- 根據申請專利範圍第1至3項中任一項之粒子,其中粒子核為晶體或多晶體。
- 根據申請專利範圍第1至3項中任一項之粒子,其中粒子核被導柱所佔據的表面積分率小於0.50。
- 根據申請專利範圍第1至3項中任一項之粒子,其中粒子核被導柱所佔據的表面積分率為0.10至0.50,以0.20至0.40為佳且以0.25至0.35更佳。
- 根據申請專利範圍第1至3項中任一項之粒子,其中陣列中的導柱延伸至粒子核一或多個晶體面。
- 根據申請專利範圍第1至3項中任一項之粒子,其 中陣列中的導柱塗佈粒子一或多個表面。
- 根據申請專利範圍第1至3項中任一項之粒子,其中導柱延伸至粒子核所有表面。
- 根據申請專利範圍第1至3項中任一項之粒子,其中導柱係實質上筆直。
- 根據申請專利範圍第1至3項中任一項之粒子,其中粒子具有電阻為0.001至100歐姆公分。
- 根據申請專利範圍第1至3項中任一項之粒子,其中核包含矽且具有{100}、{111}或{110}晶體表面。
- 根據申請專利範圍第1至3項中任一項之粒子,其中導柱側具有{110}表面。
- 一種製造根據申請專利範圍第1至27項中任一項之粒子之方法,其包含蝕刻包含矽的粒子的步驟。
- 根據申請專利範圍第28項之方法,其中導柱係藉化學反應蝕刻而製造。
- 根據申請專利範圍第28項之方法,其中導柱係藉電流交換蝕刻而製造。
- 一種電極,其含有根據申請專利範圍第1至27項中任一項定義之粒子作為其活性材料之一。
- 根據申請專利範圍第31項之電極,其中使用銅作為電流收集器。
- 根據申請專利範圍第31項之電極,其中電極係陽極。
- 一種電化學電池,其含有根據申請專利範圍第31至 33項中任一項之電極。
- 根據申請專利範圍第34項之電化學電池,其中陰極包含能夠釋出和再吸收鋰離子作為其活性材料之含鋰的化合物。
- 根據申請專利範圍第35項之電化學電池,其中陰極包含以鋰為基礎的金屬氧化物、硫化物或磷酸鹽作為其活性材料。
- 一種鋰充電電池陽極,其包含根據申請專利範圍第1至27項中任一項定義之粒子作為活性材料。
- 根據申請專利範圍第37項之陽極,其中粒子為複合膜的一部分。
- 一種電池,其包含根據申請專利範圍第37或38中任一者之陽極和陰極。
- 根據申請專利範圍第39項之電池,其中陰極包含以鋰為基礎的材料。
- 根據申請專利範圍第40項之電池,其中陰極包含二氧化鋰鈷。
- 一種裝置,其藉申請專利範圍第34至36項及39至41項中任一項之電池或申請專利範圍第37或38項之陽極供給電力。
- 一種製造複合電極之方法,其步驟包含製造含有根據申請專利範圍第1至27項中任一項之粒子之以溶劑為基礎的漿料,將此漿料塗佈在電流收集器上及蒸發此溶劑以製造複合膜。
- 一種製造鋰充電電池之方法,其步驟包含製造申請專利範圍第37或38項中任一者之陽極及添加陰極和電解質。
- 根據申請專利範圍第44項之方法,其中進一步包含在陰極和陽極之間增添分隔器。
- 根據申請專利範圍第44或45項之方法,其中進一步包含提供套管環繞電池。
- 一種製造包含矽之纖維之方法,其中導柱與申請專利範圍第1至27項中任一項定義之粒子藉刮擦、攪動或化學蝕刻中之一或多者分離。
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