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主页 / 博客 / ESM:用于实用高能锂电池的全氟电解液的内置超共形界面 ESM:用于实用高能锂电池的全氟电解液的内置超共形界面 研究背景 在锂离子电池中,为实现350 Wh Kg-1的目标,正极材料采用富镍层状氧化物(LiNixMnyCozO2,x+y+z=1,称为NMCxyz)。 随着能量密度的提高,LIBs热失控的危险性引起了人们的关注。 从材料上看,富镍正极存在严重的安全问题。 此外,其他电池组件(如有机液体和负极)的氧化/串扰也会引发热失控,这被认为是安全问题的主要原因。 稳定的电极-电解质界面的原位可控形成是下一代高能量密度锂基电池的主要策略。 具体而言,具有更高热稳定性无机组分的固体致密阴极-电解质界面(CEI)可以通过抑制氧气的释放来解决安全问题。 迄今为止,缺乏对CEI正极改性材料和电池级安全性的研究。
成绩展示 近日,清华大学冯旭宁、王莉、欧阳明高在储能材料上发表了题为“In-Built Ultraconformal Interphases Enable High-Safety Practical Lithium Batteries”的研究论文。 笔者评估了实用的NMC811/Gr软包全电池的安全性能和对应的CEI正极的热稳定性。 全面研究了材料与软包电池之间的热失控抑制机理。 使用不易燃的全氟电解液,制备了 NMC811/Gr 袋型全电池。 NMC811的热稳定性通过原位形成的富含无机LiF的CEI保护层得到改善。 LiF的CEI可以有效缓解相变引起的氧气释放,抑制NMC811与氟化电解质之间的放热反应。
图形指南 图1 使用全氟电解液和常规电解液的实用NMC811/Gr袋型全电池热失控特性比较。 传统 (a) EC/EMC 和 (b) 全氟 FEC/FEMC/HFE 电解质袋型全电池循环一个循环后。 (c) 常规 EC/EMC 电解和 (d) 全氟 FEC/FEMC/HFE 电解质袋型全电池,循环 100 次后老化。
对于使用传统电解液的 NMC811/Gr 电池在一个循环后(图 1a),T2 为 202.5°C。 T2 发生在开路电压下降时。 然而,使用全氟电解液的电池的T2达到220.2℃(图1b),这表明全氟电解液由于其较高的热稳定性能在一定程度上提高电池的固有热安全性。 随着电池老化,传统电解质电池的 T2 值下降到 195.2 °C(图 1c)。 然而,老化过程不会影响使用全氟化电解质的电池的 T2(图 1d)。 此外,使用传统电解液的电池在TR期间的最大dT/dt值高达113°C s-1,而使用全氟电解液的电池仅为32°C s-1。 老化电池的 T2 差异可归因于悦纳 NMC811 固有的热稳定性,在常规电解质下会降低,但在全氟电解质下可以有效保持。
图 2 脱锂 NMC811 正极和 NMC811/Gr 电池混合物的热稳定性。 (A,b) C-NMC811 和 F-NMC811 同步加速器高能 XRD 的等高线图和相应的 (003) 衍射峰变化。 (c) C-NMC811和F-NMC811正极的加热和释氧行为。 (d) 正极、锂化负极和电解液样品混合物的 DSC 曲线。
图 2a 和 b 显示了在常规电解质存在下和从室温到 81°C 期间,具有不同 CEI 层的高兴 NMC600 的 HEXRD 曲线。 结果清楚地表明,在存在电解质的情况下,强 CEI 层有利于锂沉积正极的热稳定性。 如图 2c 所示,单个 F-NMC811 在 233.8°C 处显示较慢的放热峰,而 C-NMC811 放热峰出现在 227.3°C 处。 此外,由 C-NMC811 的相变引起的氧释放强度和速率比 F-NMC811 更严重,进一步证实稳健的 CEI 提高了 F-NMC811 的固有热稳定性。 图 2d 对 NMC811 和其他相应电池组件的混合物进行了 DSC 测试。 对于常规电解质,1 次和 100 次循环样品的放热峰表明传统界面的老化会降低热稳定性。 相比之下,对于全氟化电解质,1 次和 100 次循环后的图示显示出宽而温和的放热峰,与 TR 触发温度 (T2) 一致。 结果(图1)是一致的,表明强CEI可以有效提高老化和高兴的NMC811和其他电池组件的热稳定性。
图 3 全氟电解液中 NMC811 正极的表征。 (ab) 老化的 F-NMC811 正极的横截面 SEM 图像和相应的 EDS 映射。 (ch) 元素分布。 (ij) 老化的 F-NMC811 正极在虚拟 xy 上的横截面 SEM 图像。 (km) 3D FIB-SEM 结构的重建和 F 元素的空间分布。
为了确认氟化CEI的可控形成,在实际软包电池中回收的老化NMC811正极的横截面形貌和元素分布通过FIB-SEM表征(图3ah)。 在全氟电解液中,在 F-NMC811 表面形成了均匀的氟化 CEI 层。 相反,传统电解液中的C-NMC811缺乏F,形成不均匀的CEI层。 F-NMC811(图3h)截面上的F元素含量高于C-NMC811,进一步证明无机氟化中间相的原位形成是保持欣喜NMC811稳定性的关键. 借助 FIB-SEM 和 EDS 映射,如图 3m 所示,在 F-NMC3 表面的 811D 模型中观察到许多 F 元素。
图 4a) 原始和高兴 NMC811 正极表面的元素深度分布。 (ac) FIB-TOF-SIMS 溅射 NMC811 正极中 F、O 和 Li 元素的分布。 (df) NMC811的F、O和Li元素的表面形貌和深度分布。
FIB-TOF-SEM进一步揭示了NMC811正极表面元素的深度分布(图4)。 与原始样品和 C-NMC811 样品相比,在 F-NMC811 的顶表层发现 F 信号显着增加(图 4a)。 此外,表面上的弱 O 和高 Li 信号表明形成了富含 F 和 Li 的 CEI 层(图 4b,c)。 这些结果都证实了 F-NMC811 具有富含 LiF 的 CEI 层。 与 C-NMC811 的 CEI 相比,F-NMC811 的 CEI 层包含更多的 F 和 Li 元素。 另外,如图所示。 如图4d-f,从离子刻蚀深度来看,原NMC811的结构比欣欣向荣的NMC811更坚固。 老化后的 F-NMC811 的蚀刻深度小于 C-NMC811,这意味着 F-NMC811 具有出色的结构稳定性。
图5 NMC811正极表面的CEI化学成分。 (a) NMC811正极CEI的XPS光谱。 (bc) 原始和令人愉悦的 NMC1 正极 CEI 的 XPS C1s 和 F811s 光谱。 (d) 低温透射电子显微镜:F-NMC811 的元素分布。 (e) 在 F-NMC81 上形成的 CEI 的冷冻 TEM 图像。 (fg) C-NMC811 的 STEM-HAADF 和 STEM-ABF 图像。 (hi) F-NMC811 的 STEM-HAADF 和 STEM-ABF 图像。
他们使用 XPS 来表征 NMC811 中 CEI 的化学成分(图 5)。 与原来的 C-NMC811 不同,F-NMC811 的 CEI 包含一个大的 F 和 Li 但较小的 C(图 5a)。 C 物种的减少表明富含 LiF 的 CEI 可以通过减少与电解质的持续副反应来保护 F-NMC811(图 5b)。 此外,较少量的 CO 和 C=O 表明 F-NMC811 的溶剂分解是有限的。 在 XPS 的 F1s 光谱中(图 5c),F-NMC811 显示出强大的 LiF 信号,证实 CEI 含有大量源自氟化溶剂的 LiF。 F-NMC811 颗粒局部区域的 F、O、Ni、Co 和 Mn 元素的映射表明细节整体均匀分布(图 5d)。 图 5e 中的低温 TEM 图像显示 CEI 可以作为保护层均匀地覆盖 NMC811 正极。 为了进一步证实界面的结构演变,进行了高角度圆形暗场扫描透射电子显微镜(HAADF-STEM)和圆形明场扫描透射电子显微镜(ABF-STEM)实验。对于碳酸盐电解质(C -NMC811),循环正极表面发生了剧烈的相变,正极表面堆积了无序的岩盐相(图5f)。对于全氟电解液,F-NMC811的表面正极保持层状结构(图5h),表明有害相得到有效抑制。此外,在F-NMC811表面观察到均匀的CEI层(图5i-g)。这些结果进一步证明了该相的均匀性。 NMC811在全氟电解液中正极表面的CEI层。
图 6a) NMC811 正极表面相间相的 TOF-SIMS 光谱。 (ac) 深入分析 NMC811 正极上的特定第二离子碎片。 (df) 在原始 C-NMC180 和 F-NMC811 上溅射 811 秒后第二个离子碎片的 TOF-SIMS 化学光谱。
C2F-碎片通常被认为是CEI的有机物,而LiF2-和PO2-碎片通常被认为是无机物。 实验中获得了明显增强的 LiF2- 和 PO2- 信号(图 6a,b),表明 F-NMC811 的 CEI 层含有大量无机物种。 相反,F-NMC2 的 C811F 信号比 C-NMC811 弱(图 6c),这意味着 F-NMC811 的 CEI 层包含的脆弱有机物种较少。 进一步研究发现(图 6d-f)F-NMC811 的 CEI 中无机物种较多,而 C-NMC811 中的无机物种较少。 所有这些结果都表明在全氟化电解质中形成了富含固体无机物的 CEI 层。 与使用传统电解液的 NMC811/Gr 软包电池相比,使用全氟电解液的软包电池的安全性提高可归因于:首先,原位形成富含无机 LiF 的 CEI 层是有利的。 欣喜NMC811正极固有的热稳定性减少了相变引起的晶格氧的释放; 其次,固体无机CEI保护层进一步防止高反应性脱锂NMC811与电解液接触,减少放热副反应; 第三,全氟电解液在高温下具有很高的热稳定性。
结论与展望 这项工作报道了一种使用全氟电解质的实用 Gr/NMC811 袋型全电池的开发,显着提高了其安全性能。 内在热稳定性。 深入研究TR抑制机制以及材料与电池水平之间的相关性。 老化过程不影响全氟电解液电池在整个风暴过程中的TR触发温度(T2),与使用传统电解液的老化电池相比具有明显优势。 此外,放热峰与TR结果一致,表明强CEI有利于无锂正极和其他电池组件的热稳定性。 这些结果表明,稳定CEI层的原位控制设计对于更安全的高能锂电池的实际应用具有重要的指导意义。
文献资料 内置超共形界面可实现高安全实用锂电池,储能材料,2021 年。