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/ 博客文章 / 電池知識 / 磷酸鐵鋰電池為什麼會失效? 1、生產過程中的故障
生產過程中,人員、設備、原料、方法、環境是影響產品品質的主要因素。 在磷酸鋰鐵動力電池的生產過程中,人員和設備都屬於管理範圍,因此我們主要討論後三個影響因素。
活性電極材料中的雜質導致電池失效。
LiFePO4合成過程中會產生少量Fe2O3、Fe等雜質。 這些雜質會在負極表面還原,並可能刺穿隔膜並造成內部短路。 當LiFePO4長時間暴露在空氣中時,水分會使電池劣化。 時效初期,材料表面形成無定形磷酸鐵。 其局部成分和結構與LiFePO4(OH)相似; 隨著OH的插入,LiFePO4不斷被消耗,表現為體積增加; 隨後緩慢重結晶形成LiFePO4(OH)。 LiFePO3 中的 Li4PO4 雜質具有電化學惰性。 石墨負極的雜質含量越高,不可逆容量損失越大。
化成方法所引起的電池失效
活性鋰離子的不可逆損失首先體現在形成固體電解質界面膜時消耗的鋰離子。 研究發現,提高化成溫度會導致鋰離子更不可逆的流失。 當成膜溫度升高時,SEI膜中無機成分的比例會增加。 有機部分ROCO2Li向無機部分Li2CO3轉變過程中釋放的氣體會在SEI膜中造成更多缺陷。 這些缺陷溶劑化的大量鋰離子會嵌入負極石墨電極中。
形成過程中,小電流充電形成的SEI膜成分和厚度均勻,但耗時; 大電流充電會導致更多的副反應發生,導致不可逆的鋰離子損失增加,負極界面阻抗也會增加,但節省了時間。 時間; 目前使用較多的是小電流恆流-大電流恆流+恆壓的形成方式,這樣可以兼顧兩者的優點。
生產環境潮濕導致電池失效
在實際生產中,電池不可避免地會與空氣接觸,因為正負極材料多為微米或奈米尺寸的顆粒,且電解液中的溶劑分子具有較大的電負性羰基和亞穩態碳碳雙鍵。 都容易吸收空氣中的水分。
水分子與電解液中的鋰鹽(特別是LiPF6)反應,分解消耗電解液(分解形成PF5)並產生酸性物質HF。 PF5和HF都會破壞SEI膜,HF也會促進LiFePO4活性材料的腐蝕。 水分子也會使嵌鋰石墨負極脫鋰,在SEI膜底部形成氫氧化鋰。 另外,溶解在電解液中的O2也會加速電池的老化。 磷酸鐵鋰電池.
在生產過程中,除了生產過程影響電池性能外,導致LiFePO4動力電池失效的主要因素還包括原料(包括水)中的雜質和化成工藝,因此磷酸鐵鋰的純度材料、環境濕度的控制、成型方法等因素至關重要。
2、上架失敗
動力電池在使用壽命期間,大部分時間都處於擱置狀態。 一般擱置時間較長後,電池效能會下降,通常表現為內阻增加、電壓下降、放電容量下降。 許多因素導致電池性能下降,其中溫度、荷電狀態和時間是最明顯的影響因素。
卡西姆等人。 分析了LiFePO4動力電池在不同儲存條件下的老化。 他們認為老化機制主要是正負極的副反應。 電解液(相對於正極的副反應,負極石墨電極的副反應較重,主要是溶劑的分解、SEI膜的生長)消耗活性鋰離子。 同時,電池的總阻抗增加,活性鋰離子的損失導致電池閒置時的老化。 LiFePO4動力電池的容量損失隨著儲存溫度的增加而增加。 相反,隨著儲存荷電狀態的增加,容量損失更小。
格羅洛等人。 也得出了同樣的結論:儲存溫度對LiFePO4動力電池的老化影響較為顯著,其次是儲存荷電狀態,並提出了簡單的模型。 它可以根據與儲存時間相關的因素(溫度和荷電狀態)來預測LiFePO4動力電池的容量損失。 在特定的SOC狀態下,隨著擱置時間的增加,石墨中的鋰會向邊緣擴散,與電解質和電子形成複雜的化合物,導致不可逆鋰離子比例增加,SEI增厚,和電導率。 降低(無機成分增加,有的還有機會重新溶解)引起的阻抗增加和電極表面活性的降低共同導致電池的老化。
無論充電狀態或放電狀態,差示掃描量熱法在室溫至4℃的溫度範圍內均未發現LiFePO4與不同電解液(電解液為LiBF6、LiAsF6或LiPF85)有任何反應。 然而,當LiFePO4長時間浸泡在LiPF6的電解液中時,它仍然會表現出特定的反應活性。 由於形成界面的反應時間較長,因此浸泡4個月後,LiFePOXNUMX表面仍沒有形成阻止與電解液進一步反應的鈍化膜。
在擱置狀態下,不良的儲存條件(高溫、高荷電狀態)會增加LiFePO4動力電池的自放電程度,使電池老化更加明顯。
3.回收失敗
電池在使用過程中一般會發熱,因此溫度的影響很大。 另外,路況、使用情況、環境溫度都會產生不同的影響。
活性鋰離子的損失通常會導致LiFePO4動力電池在循環過程中容量損失。 杜巴里等人。 研究表明,LiFePO4動力電池在循環過程中的老化主要是由於複雜的生長過程消耗了功能性鋰離子SEI膜。 在此過程中,活性鋰離子的損失直接降低了電池容量的保留率; SEI膜的持續生長,一方面導致電池極化電阻的增加。 同時,SEI膜厚度過厚,也會影響石墨負極的電化學性質。 它將部分地停用該活動。
在高溫循環過程中,LiFePO2中的Fe4+會發生一定程度的溶解。 雖然Fe2+溶解量對正極容量沒有明顯影響,但Fe2+的溶解以及負極石墨電極上Fe的沉澱會對SEI膜的生長起到催化作用。 。 Tan定量分析了活性鋰離子流失的位置和位置,發現活性鋰離子的流失大部分發生在負極石墨電極表面,特別是在高溫循環過程中,即高溫循環容量損失速度較快,總結了SEI膜的三種不同的損傷和修復機制:
- 石墨負極中的電子穿過SEI膜還原鋰離子。
- SEI膜某些成分的溶解和再生。
- 由於石墨陽極的體積變化,導致SEI膜破裂。
除了活性鋰離子的損失之外,正極材料和負極材料在回收過程中都會發生劣化。 LiFePO4電極在回收過程中出現裂紋,會導致電極極化增大,活性物質與導電劑或集流體之間的電導率下降。 Nagpure利用掃描擴展電阻顯微鏡(SSRM)半定量研究了LiFePO4老化後的變化,發現LiFePO4奈米顆粒的粗化和特定化學反應產生的表面沉積物共同導致了LiFePO4正極的阻抗增加。 此外,活性石墨材料損失導致的活性表面減少和石墨電極剝落也被認為是電池老化的原因。 石墨負極的不穩定性會造成SEI膜的不穩定,促進活性鋰離子的消耗。
電池的高倍率放電可以為電動車提供顯著的動力; 即動力電池的倍率性能越好,電動車的加速性能越好。 Kim 等人的研究結果。 結果表明,LiFePO4正極和石墨負極的老化機制不同:隨著放電倍率的增加,正極的容量損失增加幅度大於負極。 低倍率循環時電池容量的損失主要是由於負極活性鋰離子的消耗。 相較之下,電池在高倍率循環過程中的功率損失是由於正極阻抗的增加所造成的。
動力電池在使用中的放電深度雖然不會影響容量損失,但卻會影響其電量損失:電量損失的速度隨著放電深度的增加而增加。 這是由於SEI膜的阻抗上升以及整個電池的阻抗上升所致。 這是直接相關的。 雖然相對於活性鋰離子的損失,充電電壓上限對電池失效沒有明顯影響,但充電電壓上限過低或過高都會增加LiFePO4電極的界面阻抗:過低的上限限制電壓將無法很好地工作。 接地上形成鈍化膜,過高的電壓上限會造成電解液的氧化分解。 它將在 LiFePO4 電極表面形成低電導率的產品。
當溫度降低時,LiFePO4動力電池的放電容量會迅速下降,這主要是由於離子電導率的降低和界面阻抗的增加。 Li分別研究了LiFePO4正極和石墨負極,發現限制負極和負極低溫性能的主控因素不同。 LiFePO4正極離子電導率的下降占主導地位,石墨負極界面阻抗的增加是主要原因。
在使用過程中,LiFePO4電極和石墨負極的降解以及SEI膜的不斷生長都會造成電池不同程度的失效。 此外,除了路況、環境溫度等不可控因素外,電池的定期使用也至關重要,包括適當的充電電壓、適當的放電深度等。
4.充放電時故障
電池在使用過程中常常不可避免地會出現過度充電的情況。 過放電較少。 過度充電或過度放電時釋放的熱量很可能會累積在電池內部,進一步升高電池溫度。 它會影響電池的使用壽命並增加風暴起火或爆炸的可能性。 即使在常規充放電條件下,隨著循環次數的增加,電池系統中單體電池的容量不一致也會增加。 容量最低的電池會經歷充電和過度放電的過程。
儘管LiFePO4在不同充電條件下相比其他正極材料具有最佳的熱穩定性,但過度充電也會帶來LiFePO4動力電池使用的不安全風險。 在過充電狀態下,有機電解液中的溶劑更容易發生氧化分解。 在常用的有機溶劑中,碳酸亞乙酯(EC)會優先在正極表面發生氧化分解。 由於石墨負極的嵌鋰電位(相對於鋰電位)較淺,因此石墨負極中極有可能析出鋰。
過充情況下電池失效的主要原因之一是鋰晶枝刺穿隔膜造成內部短路。 盧等人。 分析了過充電引起的石墨對電極表面鍍鋰失效機制。 結果表明,負極石墨電極的整體結構沒有改變,但存在鋰晶枝和表面薄膜。 鋰與電解液的反應使表面薄膜不斷增大,消耗更多的活性鋰,導致鋰擴散到石墨中。 負極變得更加複雜,這將進一步促進負極表面的鋰沉積,導致容量和庫倫效率進一步下降。
此外,金屬雜質(特別是Fe)通常被認為是電池過充失效的主要原因之一。 徐等人。 系統研究了LiFePO4動力電池在過充條件下的失效機制。 結果表明,過充/放電循環過程中Fe的氧化還原在理論上是可能的,並給出了反應機制。 發生過充電時,Fe先被氧化為Fe2+,Fe2+進一步劣化為Fe3+,然後Fe2+和Fe3+從正極脫出。 一側向負極側擴散,Fe3+最終還原為Fe2+,Fe2+進一步還原形成Fe; 當過充/過放循環時,正負極同時開始出現Fe晶枝,刺穿隔膜形成Fe橋,導致電池微短路,伴隨電池微短路的明顯現像是連續的過度充電後溫度升高。
過充電時,負極電位會迅速上升。 電位的升高會破壞負極表面的SEI膜(SEI膜中富含無機化合物的部分更容易被氧化),這會造成電解液的額外分解,導致容量損失。 更重要的是,負極集流體銅箔會被氧化。 在負極的SEI膜中,Yang等人。 檢測出Cu2O,是銅箔的氧化產物,它會增加電池的內阻,導致暴容量損失。
他等人。 詳細研究了LiFePO4動力電池的過放電過程。 結果表明,過放電時負極集流體銅箔會被氧化成Cu+,Cu+進一步氧化成Cu2+,然後擴散到正極。 正極可發生還原反應。 這樣,就會在正極側形成晶枝,刺穿隔膜,造成電池內部微短路。 另外,由於過度放電,電池溫度也會不斷升高。
LiFePO4動力電池過度充電可能會導致電解液氧化分解、析鋰、形成Fe晶枝; 過度放電可能會導致SEI損壞,導致容量下降、銅箔氧化,甚至出現銅晶枝。
5.其他故障
由於LiFePO4固有的低電導率,材料本身的形貌和尺寸以及導電劑和黏結劑的影響很容易顯現出來。 加伯謝克等。 討論了尺寸和碳塗層這兩個相互矛盾的因素,發現LiFePO4的電極阻抗僅與平均粒徑有關。 LiFePO4中的反位點缺陷(Fe佔據Li位點)會對電池的性能產生特別的影響:因為LiFePO4內部鋰離子的傳輸是一維的,這種缺陷會阻礙鋰離子的傳輸; 由於引入高價態而產生額外的靜電斥力,這種缺陷也會導致LiFePO4結構的不穩定。
LiFePO4的大顆粒在充電結束時不能完全令人滿意; 奈米結構的LiFePO4可以減少反轉缺陷,但其高表面能會導致自放電。 PVDF是目前最常使用的黏結劑,存在高溫反應、在非水電解液中溶解、柔韌性不足等缺點。 它對LiFePO4的容量損失和循環壽命有特別的影響。 此外,集流體、隔膜、電解液成分、生產過程、人為因素、外部振動、衝擊等,都會不同程度地影響電池的性能。
參考文獻:苗孟等. 「磷酸鐵鋰動力電池失效研究進展」。