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/ 博客文章 / ESM:用於實用高能鋰電池的全氟電解質的內置超共形界面 ESM:用於實用高能鋰電池的全氟電解質的內置超共形界面 研究背景 在鋰離子電池中,為了實現350 Wh Kg-1的目標,正極材料採用富鎳層狀氧化物(LiNixMnyCozO2,x+y+z=1,稱為NMCxyz)。 隨著能量密度的增加,鋰離子電池熱失控的危險引起了人們的注意。 從材料角度來看,富鎳正極有嚴重的安全問題。 此外,其他電池組件(例如有機液體和負極)的氧化/串擾也會引發熱失控,這被認為是安全問題的主要原因。 原位可控形成穩定的電極-電解質界面是新一代高能量密度鋰基電池的主要策略。 具體來說,具有較高熱穩定性無機成分的固體緻密陰極電解質界面相(CEI)可以透過抑制氧氣的釋放來解決安全問題。 目前,關於CEI正極改質材料和電池級安全性的研究仍較為缺乏。
成績展示 近日,清華大學馮緒寧、王莉、歐陽明高在儲能材料領域發表了題為「In-Built Ultraconformal Interphases Enable High-Safety Practical Lithium Batteries」的研究論文。 作者評估了實用化的NMC811/Gr軟包全電池的安全性能以及相應CEI正極的熱穩定性。 全面研究了材料與軟包電池之間的熱失控抑制機制。 使用不可燃的全氟化電解質,製備了NMC811/Gr袋型全電池。 原位形成的富含無機LiF的CEI保護層提高了NMC811的熱穩定性。 LiF的CEI可以有效緩解相變引起的氧氣釋放,並抑制令人高興的NMC811和氟化電解質之間的放熱反應。
圖文指南 圖1 使用全氟電解液和常規電解液的實用NMC811/Gr袋型全電池的熱失控特性比較。 傳統 (a) EC/EMC 和 (b) 全氟化 FEC/FEMC/HFE 電解質袋型全電池循環一次後。 (c) 傳統的 EC/EMC 電解和 (d) 全氟化 FEC/FEMC/HFE 電解質袋型全電池在 100 次循環後老化。
對於採用傳統電解液的 NMC811/Gr 電池,在一次循環後(圖 1a),T2 為 202.5°C。 當開路電壓下降時出現 T2。 然而,使用全氟化電解液的電池的T2達到220.2℃(圖1b),這表明全氟化電解液由於其較高的熱穩定性,可以在一定程度上提高電池的固有熱安全性。 隨著電池老化,傳統電解質電池的T2值下降至195.2℃(圖1c)。 然而,老化過程不會影響使用全氟電解質的電池的T2(圖1d)。 此外,使用傳統電解液的電池在TR過程中的最大dT/dt值高達113°C s-1,而使用全氟電解液的電池僅為32°C s-1。 老化電池的 T2 差異可歸因於令人高興的 NMC811 固有的熱穩定性,其在傳統電解液下會降低,但在全氟化電解液下可以有效保持。
圖2 脫鋰NMC811正極和NMC811/Gr電池混合物的熱穩定性。 (A,b) C-NMC811和F-NMC811同步加速器高能量XRD等值線圖及對應的(003)衍射峰變化。 (c) C-NMC811和F-NMC811正極的加熱和釋氧行為。 (d)高興的正極、鋰化負極和電解質的樣品混合物的DSC曲線。
圖2a和b顯示了在傳統電解質存在下,從室溫到81°C期間,具有不同CEI層的令人高興的NMC600的HEXRD曲線。 結果清楚地表明,在電解質存在的情況下,堅固的CEI層有利於鋰沉積正極的熱穩定性。 如圖2c所示,單一F-NMC811在233.8°C處顯示較慢的放熱峰,而C-NMC811的放熱峰出現在227.3°C處。 此外,C-NMC811相變引起的氧釋放強度和速率比F-NMC811更嚴重,進一步證實強大的CEI提高了F-NMC811固有的熱穩定性。 圖 2d 對令人高興的 NMC811 和其他相應電池組件的混合物進行了 DSC 測試。 對於傳統電解質,1次和100次循環的樣品放熱峰顯示傳統界面的老化會降低熱穩定性。 相較之下,對於全氟化電解質,1 次和 100 次循環後的插圖顯示出寬且溫和的放熱峰,與 TR 觸發溫度 (T2) 一致。 結果(圖1)是一致的,顯示強CEI可以有效提高老化和高興的NMC811和其他電池組件的熱穩定性。
圖 3 全氟化電解質中 NMC811 正極的特性。 (ab) 老化的 F-NMC811 正極的橫截面 SEM 圖像和相應的 EDS 圖。 (ch) 元素分佈。 (ij) 老化的 F-NMC811 正極在虛擬 xy 上的橫截面 SEM 圖像。 (km) 3D FIB-SEM 結構重建和 F 元素的空間分佈。
為了證實氟化CEI的可控形成,透過FIB-SEM對實際軟包電池中回收的老化NMC811正極的橫截面形貌和元素分佈進行了表徵(圖3ah)。 在全氟化電解液中,F-NMC811表面形成均勻的氟化CEI層。 相反,傳統電解液中的C-NMC811缺乏F並形成不均勻的CEI層。 F-NMC811截面上的F元素含量(圖3h)高於C-NMC811,這進一步證明無機氟化中間相的原位形成是維持令人高興的NMC811穩定性的關鍵。 借助FIB-SEM和EDS繪圖,如圖3m所示,在F-NMC3表面的811D模型中觀察到了許多F元素。
圖 4a) 原始 NMC811 正極表面的元素深度分佈。 (ac) FIB-TOF-SIMS濺鍍NMC811正極中F、O和Li元素的分佈。 (df) NMC811的F、O和Li元素的表面形貌和深度分佈。
FIB-TOF-SEM進一步揭示了NMC811正極表面元素的深度分佈(圖4)。 與原始樣品和C-NMC811樣品相比,在F-NMC811的頂表面層發現F訊號顯著增加(圖4a)。 此外,表面上的弱 O 和高 Li 訊號顯示形成了富含 F 和 Li 的 CEI 層(圖 4b、c)。 這些結果都證實了F-NMC811具有富含LiF的CEI層。 與C-NMC811的CEI相比,F-NMC811的CEI層含有更多的F和Li元素。 另外,如圖4、圖811所示。 如圖811d-f所示,從離子蝕刻深度的角度來看,原始NMC811的結構比令人高興的NMC811的結構更加堅固。 老化後的F-NMC811的蝕刻深度小於C-NMCXNUMX,這意味著F-NMCXNUMX具有優異的結構穩定性。
圖5 NMC811正極表面的CEI化學成分。 (a) NMC811正極CEI的XPS譜。 (bc) 原始且令人高興的 NMC1 正極 CEI 的 XPS C1s 和 F811s 光譜。 (d) 冷凍透射電子顯微鏡:F-NMC811 的元素分佈。 (e) 在 F-NMC81 上形成的 CEI 冷凍 TEM 影像。 (fg) C-NMC811 的 STEM-HAADF 和 STEM-ABF 影像。 (hi) F-NMC811 的 STEM-HAADF 和 STEM-ABF 影像。
他們使用 XPS 來表徵 NMC811 中 CEI 的化學成分(圖 5)。 與原始 C-NMC811 不同,F-NMC811 的 CEI 包含較大的 F 和 Li,但包含較小的 C(圖 5a)。 C物質的減少顯示富含LiF的CEI可以透過減少與電解質的持續副反應來保護F-NMC811(圖5b)。 此外,較少量的CO和C=O顯示F-NMC811的溶劑分解作用是有限的。 在 XPS 的 F1s 譜中(圖 5c),F-NMC811 顯示出強大的 LiF 訊號,證實 CEI 含有大量源自氟化溶劑的 LiF。 F-NMC811顆粒上局部區域的F、O、Ni、Co和Mn元素的映射顯示,細節整體均勻分佈(圖5d)。 圖5e的低溫TEM影像顯示CEI可以作為保護層均勻覆蓋NMC811正極。 為了進一步證實界面的結構演化,進行了高角度圓形暗場掃描透射電子顯微鏡(HAADF-STEM)和圓形明場掃描透射電子顯微鏡(ABF-STEM)實驗。對於碳酸鹽電解質(C -NMC811 ),循環正極表面發生了嚴重的相變,正極表面累積了無序的岩鹽相(圖5f)。對於全氟電解液,F-NMC811的表面正極保持層狀結構(圖5h),顯示有害相得到有效抑制。此外,在F-NMC811表面觀察到均勻的CEI層(圖5i-g),這些結果進一步證明了正極的均勻性。全氟電解液中 NMC811 正極表面的 CEI 層。
圖6a) NMC811正極表面相間相的TOF-SIMS譜。 (ac)對NMC811正極上特定第二離子碎片的深入分析。 (df) 在原始 C-NMC180 和 F-NMC811 上濺射 811 秒後第二個離子碎片的 TOF-SIMS 化學光譜。
C2F-碎片通常被認為是CEI的有機物質,而LiF2-和PO2-碎片通常被認為是無機物質。 實驗中獲得了LiF2-和PO2-的顯著增強訊號(圖6a,b),顯示F-NMC811的CEI層含有大量無機物。 相反,F-NMC2 的 C811F 訊號比 C-NMC811 弱(圖 6c),這意味著 F-NMC811 的 CEI 層含有較少的脆弱有機物質。 進一步研究發現(圖6d-f)F-NMC811的CEI中無機物較多,而C-NMC811中無機物較少。 所有這些結果都表明在全氟化電解質中形成了富含無機物的固體 CEI 層。 與使用傳統電解液的NMC811/Gr軟包電池相比,使用全氟化電解液的軟包電池的安全性提高可歸因於:首先,原位形成富含無機LiF的CEI層是有益的。 令人高興的NMC811正極固有的熱穩定性減少了相變引起的晶格氧的釋放; 其次,固體無機CEI保護層進一步阻止了高反應活性的脫鋰NMC811與電解液的接觸,減少了放熱副反應。 第三,全氟電解液在高溫下有較高的熱穩定性。
結論與展望 該工作報告了使用全氟化電解質開發出實用的 Gr/NMC811 袋型全電池,顯著提高了其安全性能。 固有的熱穩定性。 深入研究TR抑制機制以及材料與電池等級的相關性。 老化過程不影響全氟電解液電池在整個風暴過程中的TR觸發溫度(T2),與使用傳統電解液的老化電池相比具有明顯優勢。 此外,放熱峰與TR結果一致,顯示強CEI有利於無鋰正極和其他電池組件的熱穩定性。 這些結果表明,穩定CEI層的原位控制設計對於更安全的高能量鋰電池的實際應用具有重要的指導意義。
文獻資料 內建超共形介面實現高安全性實用鋰電池,儲能材料,2021。