TWI796295B - 於電極與電解質層間具有中間層之能量儲存元件 - Google Patents

於電極與電解質層間具有中間層之能量儲存元件 Download PDF

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TWI796295B
TWI796295B TW106112526A TW106112526A TWI796295B TW I796295 B TWI796295 B TW I796295B TW 106112526 A TW106112526 A TW 106112526A TW 106112526 A TW106112526 A TW 106112526A TW I796295 B TWI796295 B TW I796295B
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anode
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吉貝克 朴
炳松 郭
立中 孫
迪米崔歐斯 阿吉里斯
圭日 曹
苗君 王
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美商應用材料股份有限公司
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Abstract

本文的手段提供例如電池組保護元件的元件，包括在基板頂上提供的陰極集電器與陽極集電器、在陰極集電器頂上提供的陰極以及覆在陰極上提供的電解質層。中間層覆在電解質層上形成，中間層例如下列一種或更多種層：矽、銻、鎂、鈦、鎂鋰及/或銀鋰。接著提供覆在中間層上的陽極接觸層，陽極接觸層例如陽極或陽極集電器。藉由在陽極接觸層沉積之前在電解質層頂上提供中間層，來自陰極側的鋰與中間層合金，因此提供更等向或單軸的陽極接觸層剝離。

Description

於電極與電解質層間具有中間層之能量儲存元件
本申請案主張2016年4月14日提出申請，發明名稱為「體積變化適應TFE材料(Volume Change Accommodating TFE Materials)」之美國臨時專利申請案第62/322,415號的優先權權益，優先權案之內容全文引用併入本文中。本案的實施例是關於固態能量儲存元件，並且更確切而言是關於具有在電極與電解質層之間的中間層的能量儲存元件。
對許多應用而言，例如薄膜電池組的固態電池組正迅速發展中。各自對應至每單位體積的電池組能量容量與每單位重量的電池組能量容量的電池組能量密度與電池組比能量為值得注意的效能量測。通常，固態與薄膜電池組能提供比起含液態電池組更高的能量密度與比能量。在小尺寸中，固態電池組經常以微電子處理技術製造，並且可被使用於例如，舉例而言，可攜式電子裝置、醫療裝置以及太空系統的應用中。在大尺寸中，電池組可使用於電力電動車或家中或輸電網路中的儲存電力。
基本上，可藉由沉積金屬鋰(Li)，藉由在元件的陽極側上建立電荷載體貯槽(例如Li)來形成固態電池組。在其他案例中，由於元件先行依賴陰極中的電荷載體，故電荷載體貯槽不分別建立。在此類案例中，Li陽極層可用金屬層取代，以提供陽極區來完成電化學元件佈局。材料中的部分可包括例如Cu的過度金屬以及能與下方電解質層形成複雜介面的合金材料。
缺乏分別沉積的陽極/負電極層所形成的習知固態電池組觀察到某些問題。例如，來自陰極側(例如：LiCoO2 )的嵌出Li (deintercalated Li)可在電解質-陽極/Cu介面迫使結構非等向，由於Li的體積而由介面拆離Cu，因此導致金屬陽極層斷裂/碎裂所誘發的應力。此類碎裂會導致氧化劑的指向路徑，導致限制的電荷載體損失，亦就是電池組電容的損失。該應力起因於下列事實：來自陰極側的Li不嵌入陽極材料或非Li金屬陽極(集電器)或不易與陽極材料或非Li金屬陽極(集電器)合金。此碎裂的其他後果為來自增加的電性及電化學接觸電阻(非連續介面)的整體元件阻抗增加，以及源自反應的/氧化的電荷載體(例如：LiOH、Li2 CO3 等等形式)的阻抗，導致元件效能劣化。因此，對應習知元件的介面工程是必須的。
鑒於前述需求，本文的手段提供中間層來分開薄膜元件的陽極層與電解質層。中間層可形成在電解質層頂上，並且由下列的一種或更多種層形成：矽、銻、鋁、鎂、鈦、鎂鋰及/或銀鋰。藉由在陽極或陽極集電器層沉積之前在電解質層頂上提供此類中間層，來自陰極側的鋰能與中間層合金，由於Li在元件初始充電的期間鍍覆至陽極或陽極集電器上，因此提供更等向或單軸的陽極或陽極集電器剝離。
依據本案揭示內容的範例元件可包括：在基板頂上提供的陰極集電器；在陰極集電器頂上提供的陰極；覆在陰極上提供的電解質層；覆在電解質層上提供的中間層；以及覆在中間層上提供的陽極接觸層。
依據本案揭示內容的範例薄膜元件可包括：在基板頂上形成的陰極集電器與第一陽極集電器；在陰極集電器頂上形成的陰極；覆在陰極上形成的電解質層；覆在電解質層上形成的中間層；以及直接在中間層頂上形成的陽極或第二陽極集電器中的至少一者。
依據本案揭示內容形成元件的範例方法可包括：在基板頂上形成陰極集電器以及第一陽極集電器；在陰極集電器頂上形成陰極；形成覆在陰極上的電解質層；形成覆在電解質層上的中間層；以及在中間層頂上形成陽極接觸層。
現將參考圖示出元件及方法的實施例的附圖，於後文更全面地說明依據本案揭示內容的一種或更多種手段。手段以許多不同的形式體現，並且不被解釋為本文列舉出的實施例的限制。相反地，提供這些實施例，因而此揭示內容對於本技術領域中具有通常知識者將更徹底與完整，並且將充分表達元件與方法的範圍。
由於便利性與明確性的緣故，本文將使用例如「頂部」、「底部」、「上部」、「下部」、「垂直的」、「水平的」、「橫向的(lateral)」及「縱向的(longitudinal)」的用語來說明這些組件與其構成部件相對的佈置與方位，有關能量儲存元件的幾何與方位的每一組件及構件如圖中所示。術語將包括特定提到的用字、前述用字的衍生字以及類似含義的用字。
如本文所使用的，以單數(singular)記載以及接續用字「一(a)」或「一(an)」的零件與操作被理解為包含複數個零件或操作，除非有明確記載此類排除事項。再者，參考本案揭示內容的「一個實施例」並不用來作為限制。額外實施例亦可併入所記載的特徵。
如本文進一步所說明的，揭示內容的手段提供例如電池組保護元件的元件，包含在基板頂上形成的陰極集電器與陽極集電器、在陰極集電器頂上形成的陰極以及覆在陰極上形成的電解質層。提供例如矽、銻、鋁、鎂、鈦、鎂鋰及/或銀鋰中一層或更多層的中間層覆在電解質層上。隨後提供例如陽極及/或陽極集電器的陽極接觸層覆在中間層上。藉由在金屬陽極接觸層沉積之前，在電解質層頂上提供中間層，來自陰極側的Li與中間層合金，因此提供更等向或單軸的金屬陽極剝離。
如本文中所使用的，用語陰極用來表示正電極，以及使用用語陽極來表示負電極。本技術領域中具有通常知識者將意識到，取決於元件是否正在充電或放電，正電極可以是陰極(例如在還原以及電子獲得的案例中)或正電極可以是陽極(例如在氧化以及電子損失的案例中)。相似地，取決於元件的狀態，負電極可以是陰極或陽極。
現在回到圖 1A ～ 1B ，將更加詳細地說明依據揭示內容的各種實施例，例如固態元件(例如薄膜電池組)的元件100的截面視圖。如圖所示，元件100包括在基板110頂上形成的陰極集電器104與陽極集電器108。可在陰極集電器104頂上提供陰極112(例如正電極)，以及可提供電解質層120覆在陰極112上。可提供例如矽、銻、鋁、鎂、鈦、鎂鋰及/或銀鋰中一層或更多層的中間層124覆在電解質層120上。隨後提供陽極接觸層130覆在中間層124上。在實施例中顯示出，陽極接觸層130可包括陽極132，其特徵為電化學活性層。元件100各層的薄膜可藉由薄膜製造製程所形成，例如，舉例而言，物理或化學氣相沉積方法(PVD或CVD)、氧化、氮化或電鍍。
在一些實施例中，元件100的基板110作為電池組的支撐件，並且由環境要素適度不滲透的材料所製成。基板可在上方具有相對光滑的處理表面，用於在其上形成薄膜，以及基板亦具有適當的機械強度以在製造溫度與在電池組操作溫度支撐沉積的薄膜。舉例而言，取決於外部表面所想要的電性特徵，基板110可為絕緣體、半導體或導體。更具體而言，取決於應用，基板110可由陶瓷、金屬或玻璃(例如，舉例而言，釔安定氧化鋯、氧化鋁、矽酸鹽玻璃或甚至是鋁或鋼)所製成。在一個實施例中，基板110包含雲母以及KAl3 Si3 O10 (OH)2 的化學計量，雲母包括具有白雲母結構的層狀矽酸鹽。雲母具有六側平面單斜晶結晶結構與沿著大平坦表面方向的良好解理特性。由於雲母的晶形結構，基板110可沿著其基底的橫向解理平面被拆分成薄的箔片以提供具有比大部分化學或機械研磨表面更光滑之表面的薄基板。
在一些實施例中，元件100包括複數個安置在電解質層120相對側上的集電器。更具體而言，如圖 1B 所示，陽極接觸層130可包括具有表面135的陽極集電器134，舉例而言，來自陰極側帶電的Li「鍍覆」至表面135以一配置形成陽極/負電極，該配置中陽極接觸層130不包括分別沉積的陽極。因此，與此Li合金的中間層124容許更光滑的鍍覆與合金，以維持陽極集電器134的整體性。在一些實施例中，分別形成的電化學活性層，例如圖 1A 所示的陽極132，並不存在於圖 1B 的陽極接觸層130中，因為陽極集電器134當作陽極集電器以及陽極本身來用。舉例而言，可僅提供陽極集電器134覆在中間層124上，因為陽極在電池的第一充電循環期間在陽極集電器134下方形成。在範例實施例中，陽極集電器134可包括例如銀、金、鉑或鋁及/或鈦的非反應性金屬，其中鈦作為鉑與金的黏著層。
如所示，在陽極接觸層130與陰極112之間提供電解質層120。在一些實施例中，電解質層120舉例而言可以是非晶形鋰磷氧氮化物膜，稱之為LiPON膜。在一個非限制性實施例中，LiPON膜為具有厚度在大約0.1微米至大約5微米之間的Lix POy Nz 形式。電解質厚度適度地大以提供適當的保護，避免陰極112與陽極接觸層130短路，以及電解質厚度適度地小以減少離子通路以最小化電阻並減少應力。
在一些實施例中，陰極112可包括例如非晶形五氧化二釩V2 O5 的電化學活性材料或例如TiS2 、LiMnO2 、LiMn2 O2 、LiMn2 O4 、LiCoO2 以及LiNiO2 的數種結晶化合物中的一種。在一個非限制性實施例中，陽極接觸層130由Li製成，以及陰極112由LiCoO2 製成。陽極接觸層130或陰極112的適當厚度可自大約0.1微米至大約50微米。
陽極集電器108以及陰極集電器104為來自電極的電子耗散或收集提供傳導表面。陽極集電器108以及陰極集電器104經成形與定尺寸以為電極增加電子傳導性或增加來自電極的電子傳導性，以及陽極集電器108以及陰極集電器104在電極的上方或下方形成，以電性耦接至電極。陽極集電器108以及陰極集電器104可為包括含金屬材料的導電層，含金屬材料為例如，舉例而言，金屬、非反應性金屬、金屬合金、金屬矽化物、導體金屬氧化物或前述的混合物。
在一個非限制性實施例中，陽極集電器108以及陰極集電器104各包括例如銀、金、鉑或鋁的非反應性金屬。這些材料(但不含與元件100的其他成分反應的陽極集電器108以及陰極集電器104材料)容許在形成陽極集電器108以及陰極集電器104之後，以相對高溫處理元件100。陽極集電器108以及陰極集電器104可具有經選擇以提供適當導電性的厚度。舉例而言，在一個實施例中，陽極集電器108以及陰極集電器104可具有大約0.05微米至大約5微米的厚度。在另一個實施例中，陽極集電器108由銅製成，以及陰極集電器104由鉑製成。
儘管並未圖示出，元件100亦可包括沉積在基板110或元件100其他層的任何層表面上的一層或更多層黏著層，以改善重疊層的黏著性。黏著層可包含例如，舉例而言，鈦、鈷、鋁或其他金屬的金屬。在一些非限制性實施例中，黏著層可為AlOx 或SiNx 。
在範例實施例中，提供中間層124覆在電解質層120上，以及提供中間層124在陽極接觸層130下方，以及中間層124通常與電解質層120的形狀一致。中間層124的區段126延伸超過電解質層120的邊緣128，並且直接與陽極集電器108連結。在一些實施例中，中間層124可包括「中間層1」124-A以及一個或更多個額外的中間層，舉例而言，如所示的「中間層2」124-B。中間層124-A及124-B的材料包括Si、Sb、Al、Mg或Ti以及例如MgLi以及AgLi的合金材料。藉由在金屬陽極接觸層130沉積之前在電解質層120頂上提供中間層124，來自陰極112的鋰與中間層124的材料合金以提供更等向或單軸的金屬陽極接觸層130的剝離，因而在介面處減少碎裂或空隙形成。
現在回到圖 2 ，元件100可進一步包括配置覆在陽極接觸層130上的封裝層140。如所示，在一些實施例中，可提供封裝層140覆在陽極接觸層130、中間層124、電解質層120、陰極集電器104以及基板110的所有暴露表面上。封裝層140可為柔軟且韌曲的物理體積適應層，其能夠適應元件100的層體積改變。在各種實施例中，封裝層140可將其厚度由第一厚度改變成第二厚度以適應擴充區中不同材料的體積或厚度上的改變。舉例而言，在元件100為薄膜電池組的案例中，其中陽極接觸層130或陽極接觸層130的部分可構成選擇性擴充區，封裝層140可在厚度上延伸或收縮以適應陽極厚度的增加或減少。這使元件100的層產生較少應力、較少機械失效以及較佳保護。
現在回到圖 3 ～ 7 ，圖 3 ～ 7 顯示出依據揭示內容的各種實施例，用於形成元件200(例如：薄膜電池組)的方法的一系列截面視圖。圖 3 描繪形成在基板210的頂表面209上的陰極集電器204以及陽極集電器208。在一些實施例中，陽極集電器208以及陰極集電器204以基板210的頂表面209與陽極集電器208以及陰極集電器204的各者之間的黏著膜(未圖示出)形成在基板210上。
圖4描繪形成在陰極集電器204頂上的陰極212。在一個實施例中，為了元件200的良好效能，可退火214例如LiCoO2 的陰極212以達成LCO所欲之相/組成。舉例而言，可在大約700℃退火LiCoO2 的非晶形或微晶膜以獲得結晶LiCoO2 陰極膜。圖 5 描繪覆在陰極212上形成的電解質層220。如所示，電解質完全包住陰極212，並且沿著基板210延伸以部分覆蓋陽極集電器208。
如圖 6 所示，隨後形成覆在電解質層220上的中間層224。在一些實施例中，可藉由薄膜製造製程形成中間層224，例如，舉例而言，物理或化學氣相沉積(PVD或CVD)、氧化、氮化或電鍍。如所示，中間層224部分覆蓋電解質層220，並且沿著基板210延伸以環繞包覆電解質層220的邊緣228。如所示，中間層224可直接與陽極集電器208連結。
如圖 7 所示，隨後形成覆在中間層224上的陽極接觸層230，其中陽極接觸層230可包括陽極以及陽極集電器中的一者或更多者。陽極接觸層230沿著中間層224的頂表面延伸並且通常與中間層224的頂表面一致。在一些實施例中，陽極接觸層230包含直接沉積在中間層224上的傳導膜，舉例而言，由金屬膜(例如銅)製成。在一個實施例中，亦可沉積陽極接觸層230以與陽極集電器208的部分重疊。用來製造陽極接觸層230的材料可與用來製造陰極212的材料相同或不同。隨後可形成覆在陽極接觸層230上的封裝層，以產生圖 2 描繪的元件100的結構。
鑒於前述內容，本文所揭示的實施例達成至少下列的優點。揭示內容的第一優點包括歸因於來自陰極的Li與形成在電解質與陽極或陽極集電器之間的中間層的合金，消除或減少應力誘發的碎裂以及所產生的元件降解。揭示內容的第二優點包括來自電接觸電阻減少的整體元件阻抗減少，因而產生元件效能改善。揭示內容的第三優點包括將中間層應用至所有固態能量元件的通用性，其中，舉例而言，當電解質為固態時，不存在電荷載體貯槽，或者陽極材料不嵌入電荷載體或不易與電荷載體合金。揭示內容的第四優點為在電化學活性陽極層沉積在中間層頂上的案例中，伴隨進入的Li的較高熔化組成分的調節力。舉例而言，可藉由適當厚的中間層來緩和由電化學活性陽極層合金(對比陽極集電器的純Li)所引起的操作溫度範圍增加。
儘管本文已說明揭示內容的某些實施例，但揭示內容並不作為其限制，因為揭示內容概括的範圍如技術內容所容許並且可依照說明書所理解。因此，上述說明不被解釋為限制。相反地，上述說明僅作為特殊實施例的範例。本技術領域中具有通常知識者在本文附加的申請專利範圍的範圍及精神內將能預想到其他變化。
100‧‧‧元件104‧‧‧陰極集電器108‧‧‧陽極集電器110‧‧‧基板112‧‧‧陰極120‧‧‧電解質層124‧‧‧中間層124-A‧‧‧中間層1124-B‧‧‧中間層2126‧‧‧區段128‧‧‧邊緣130‧‧‧陽極接觸層132‧‧‧陽極134‧‧‧陽極集電器135‧‧‧表面140‧‧‧封裝層200‧‧‧元件204‧‧‧陰極集電器208‧‧‧陽極集電器209‧‧‧頂表面210‧‧‧基板212‧‧‧陰極214‧‧‧退火220‧‧‧電解質層224‧‧‧中間層228‧‧‧邊緣230‧‧‧陽極接觸層
附圖圖解所揭示實施例的範例手段，所揭示實施例在一定程度內為其原則的實施應用而設計，以及其中：
圖1A描繪依據本案揭示內容範例實施例的元件側面截面視圖；
圖1B描繪依據本案揭示內容範例實施例的元件側面截面視圖；
圖2描繪依據本案揭示內容範例實施例的元件側面截面視圖；
圖3描繪依據本案揭示內容範例實施例，形成覆在基板上的陰極集電器及陽極集電器之方法的側面截面視圖；
圖4描繪依據本案揭示內容範例實施例，形成覆在陰極集電器及陽極集電器上的陰極之方法的側面截面視圖；
圖5描繪依據本案揭示內容範例實施例，形成覆在陰極上的電解質之方法的側面截面視圖；
圖6描繪依據本案揭示內容範例實施例，形成覆在電解質上的中間層之方法的側面截面視圖；以及
圖7描繪依據本案揭示內容範例實施例，形成覆在中間層上的陽極接觸層之方法的側面截面視圖。
圖式無須依照比例尺。圖式僅為揭示內容的表現，並不用來描述特定的參數。圖式用來描繪揭示內容的範例實施例，因此不被考慮作為範圍上的限制。在圖式中，類似的編號表示類似的零件。
並且，為了說明的明確性，一些圖中的某些元件可被忽略，或者不依比例尺繪製。為了說明的明確性，截面視圖可為「切片」或「近視」截面視圖的形式，忽略原本在「真」截面視圖中可見的某些背景線條。並且，為了明確性，在某些圖式中一些參考編號可被忽略。
國內寄存資訊 (請依寄存機構、日期、號碼順序註記) 無
國外寄存資訊 (請依寄存國家、機構、日期、號碼順序註記) 無
100‧‧‧元件
104‧‧‧陰極集電器
108‧‧‧陽極集電器
110‧‧‧基板
112‧‧‧陰極
120‧‧‧電解質層
124‧‧‧中間層
124-A‧‧‧中間層1
124-B‧‧‧中間層2
126‧‧‧區段
128‧‧‧邊緣
130‧‧‧陽極接觸層
132‧‧‧陽極

Claims (12)

  1. 一種薄膜元件，包含：一陰極集電器以及一第一陽極集電器，形成在一基板頂上；一陰極，形成在該陰極集電器頂上；一電解質層，形成覆在該陰極上，其中該電解質層係直接提供在該陰極集電器頂上且直接提供在該第一陽極集電器頂上；一中間層，形成覆在該電解質層上，其中該中間層直接接觸該第一陽極集電器，以及其中該中間層為下列至少一者：矽、銻、鋁、鎂、鈦、鎂鋰以及銀鋰；以及一陽極接觸層，形成覆在該中間層上。
  2. 如請求項1所述之元件，其中該陽極接觸層包含一陽極，以及其中該陽極為一電化學活性層。
  3. 如請求項1所述之元件，其中該陽極接觸層包含一第二陽極集電器。
  4. 如請求項1所述之元件，更包含一封裝層，形成覆在該陽極接觸層上。
  5. 一種薄膜元件，包含：一陰極集電器以及一第一陽極集電器，形成在一基板頂上； 一陰極，形成在該陰極集電器頂上；一電解質層，形成覆在該陰極上，其中該電解質層係直接提供在該陰極集電器頂上且直接提供在該第一陽極集電器頂上；一中間層，形成覆在該電解質層上且直接形成在一部分的該第一陽極集電器頂上，以及其中該中間層為下列至少一者：矽、銻、鎂、鈦、鎂鋰以及銀鋰；以及下列至少一者：一陽極，配置覆在該中間層上；以及一第二陽極集電器，配置覆在該中間層上。
  6. 如請求項5所述之薄膜元件，其中該陽極為一電化學活性層。
  7. 如請求項5所述之薄膜元件，其中該中間層連結至該第一陽極集電器。
  8. 如請求項5所述之薄膜元件，更包含一封裝層，形成覆在該陽極或該第二陽極集電器上。
  9. 一種形成一薄膜元件的方法，包含以下步驟：提供一陰極集電器以及一第一陽極集電器在一基板頂上；提供一陰極在該陰極集電器頂上；形成一電解質層覆在該陰極上，其中該電解質層係直接提供在該陰極集電器頂上且直接提供在該第一陽 極集電器頂上；形成一中間層覆在該電解質層上且直接形成在一部分的該第一陽極集電器頂上，以及其中該中間層為下列至少一者：矽、銻、鎂、鈦、鎂鋰以及銀鋰；以及形成一陽極接觸層在該中間層頂上。
  10. 如請求項9所述之方法，更包含以下步驟：形成該電解質層覆在該第一陽極集電器上。
  11. 如請求項9所述之方法，其中該陽極接觸層包含下列至少一者：一陽極；以及一第二陽極集電器。
  12. 如請求項9所述之方法，更包含以下步驟：形成一封裝層覆在該陽極接觸層上。
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