A Review of Electric Performance and SOH Research for Li4Ti5O12 Based Batteries

WANG Chu, LIU Ze-hui, SUN Yao-hong, GAO Ying-hui, YAN Ping

Advances in New and Renewable Energy ›› 2022, Vol. 10 ›› Issue (4) : 316-324.

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Advances in New and Renewable Energy ›› 2022, Vol. 10 ›› Issue (4) : 316-324. DOI: 10.3969/j.issn.2095-560X.2022.04.004

A Review of Electric Performance and SOH Research for Li4Ti5O12 Based Batteries

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Abstract

The high-power density and high energy density are the two features which make Li-ion batteries an important choice of electric vehicle power and energy storage power station of new energy grid. The two challenges of Li-ion batteries are their high-power performance and safety performance. Spinel Li4Ti5O12 is considered as one of the most promising substitutes of graphite as anode material, due to its structural stability, safety, long cycle life, high-power feature and discharging ability at high and low temperature. In this paper, the development of Li4Ti5O12 based batteries was reviewed, the structure, electrochemical feature, preparation methods of Li4Ti5O12 material and its problems as anode of Li-ion batteries were introduced, and the electric performance and state of health (SOH) research of full cell based on Li4Ti5O12 material were mainly introduced.

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Li4Ti5O12 / Li-ion battery / state of health / anode material / high-power discharging

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Chu WANG, Ze-hui LIU, Yao-hong SUN, et al. A Review of Electric Performance and SOH Research for Li4Ti5O12 Based Batteries[J]. Advances in New and Renewable Energy, 2022, 10(4): 316-324 https://doi.org/10.3969/j.issn.2095-560X.2022.04.004

0 引言

随着太阳能和风能等清洁能源和电动汽车的发展,锂离子电池由于功率密度和能量密度大、循环寿命长等特性,是化石能源之外重要的储能方式,受到广泛的关注。锂离子电池的研究涉及物理、化学、材料、电子等众多学科,其中活性材料作为直接影响电池安全性、容量、工作电压和寿命的因素,是锂电池研究方向中最重要的一支。
传统的锂电池负极材料多由焦炭或石墨制成。石墨负极具有良好的层状结构,充电时锂离子嵌入石墨层状结构中形成LiC6,理论容量为372 mA∙h/g,锂嵌入电势低于0.1 V（相对Li/Li+）,与锂电镀电势接近[1]。由于较低的锂离子嵌入/脱嵌电位,碳负极电池对过充和大倍率放电非常敏感,极易形成锂枝晶,从而导致局部短路。此外,碳负极表面在初次充电过程中生成的固体电解质界面（solid electrolyte interface, SEI）膜热稳定度较低,导致电池产气甚至爆炸。为解决类似问题,除了通过物理、化学手段对石墨负极进行改性处理外,开发非碳负极材料体系也成为了当今的一个热门研究方向。
钛酸锂（Li4Ti5O12, LTO）是一种尖晶石钛锂氧化物,具有大约1.55 V的锂嵌入/脱嵌电压[2,3],远高于形成SEI膜和锂枝晶的电势,因此大大提升了安全性。除此之外,钛酸锂材料在锂嵌入/脱嵌过程中的体积变化很小,拥有零应变特性。钛酸锂在高功率放电、循环寿命[4]、高低温稳定性[5]上也有着优秀的表现,被认为是最有前景的石墨电极替代方案之一。表1展示了石墨和钛酸锂材料的电化学性能和机械性能的对比[6,7,8]。不难发现,除上述优点外,钛酸锂负极材料的主要问题在于较低的理论比容量、电子电导率和锂扩散系数。虽然较高的对锂电位避免了SEI膜和锂枝晶的生成,但同时也影响了这一材料体系的理论比容量。低电导率和锂扩散系数导致了更大的极化损失,特别是在较高的电流下。近年来,这一问题通过制备纳米级别的钛酸锂颗粒、表面涂层（如碳包覆）和掺杂等方法已经得到了显著改善[8],大大提升了钛酸锂材料的倍率性能。本文主要介绍近年来以钛酸锂为负极材料的锂离子电池在电性能和健康状态方面的研究进展。
Table 1 Performance comparison of spinel Li4Ti5O12 and graphite

表1 尖晶石钛酸锂材料与石墨的性能比较

材料 理论比容量 / (mA∙h/g) 对Li/Li+电位 / V 电子电导率 / (S/cm) 锂扩散系数 / (cm/s) 体积膨胀率 / %
石墨 372 0.10 1 × 10-4 1 × 10-11 ~ 1 × 10-7 10.0
Li4Ti5O12 175 1.55 1 × 10-13 ~ 1 × 10-8 1 × 10-16 ~ 1 × 10-8 0.2

1 钛酸锂基锂离子电池

1.1 钛酸锂材料

尖晶石钛酸锂材料于1956年被JONKER等[9]首次报道。这一材料曾作为锂离子正极材料被研究,但因其电位较低,导致放电容量不足。然而,和一些高电位的正极材料,如LiMn2O4（LMO）搭配时,它可用于电池的负极材料[10],且显示出良好的寿命性能和安全性。钛酸锂材料在负极材料方面的应用首先由FERG等[11]提出,确认了钛酸锂负极可以与LMO、LiCoO2（LCO）等正极材料配合使用。
1.1.1 基本结构
尖晶石钛酸锂的晶体结构首次报道于1971年[12],如图1所示。Li4Ti5O12呈面心立方结构,所有的八面体32e位点都由O2- 占据,四面体8a位点由Li+ 占据,八面体16d位点由Li+ 离子和Ti4+ 离子随机占据,比例为1/5[13]。尖晶石钛酸锂材料被认为是一种零应变材料,在锂离子的嵌入/脱嵌过程中晶格参数的整体变化小于0.1%,这一特性由OHZUKU等[2]首次报道。一般认为这是由于晶格中的八面体Ti—O共价键键能远大于Li—O离子键[14,15,16],使得尖晶石钛酸锂在充放电过程中相当稳定。
Fig. 1 Crystal structure of spinel Li4Ti5O12[12]

图1 尖晶石钛酸锂材料的晶体结构[12]

Full size|PPT slide

图2显示了Li4Ti5O12在1.0 ~ 3.0 V电位范围内的典型恒电流充放电曲线[17]。如图所示,尖晶石钛酸锂在充、放电开始和结束阶段有着迅速的电压变化[3],而在中段保持稳定的1.55 V电位。一般认为,这和Li4Ti5O12的两相机制有关[3,19,20]。根据OHZUKU等[2]的报道,Li4Ti5O12的理论容量为175 mA∙h/g。
Fig. 2 Potential curve of spinel Li4Ti5O12[17]

图2 尖晶石钛酸锂材料的电势曲线[17]

Full size|PPT slide

1.1.2 优劣势与改进
虽然钛酸锂材料在寿命性能和安全性上具有突出的优势,但其面临的问题同样较多。首先是较低的理论比容量,导致了钛酸锂材料无法作为商业化电动汽车的主流方案,主要用于要求高稳定性、高功率、高安全性和长循环寿命,并对能量密度要求不高的场合,如电子设备的薄膜电池[20]、混合动力汽车的主电源和启停电源[21,22]、电网系统的调频电站[23]等。其次是较低的电子电导率（1 ×10-13 ~ 1 × 10-8 S/cm）[24]和锂扩散系数（1 ×10-16 ~ 1 ×10-8）[25]导致较大的极化损失。钛酸锂材料的电导率和锂扩散系数都对温度较为敏感[26,27],在低温下会带来更高的倍率性能损失。对钛酸锂材料的改进也主要集中在这一方向。目前主要的改进方法包括：使用溶胶-凝胶法[28,29]、微乳液法[30]、溶剂热法[31]、快速燃烧法[32]等合成方法,避免在高温下进行长时间煅烧,以生成纳米级别的钛酸锂颗粒;通过改变电极结构的方式增大比表面积,如多孔电极[33]、纳米微球电极[34,35,36]、薄膜电极[37]等;给钛酸锂颗粒包覆碳涂层[38,39]、金属涂层[40]或在不同气氛下对钛酸锂颗粒进行表面处理[41,42],以增加表面电导率;掺杂Nb5+、Cr3+、Zr4+、Al3+、Cu2+ 等元素以进行改性[43,44,45,46,47,48];与石墨烯[49]、TiO2[50,51]等材料共同制备复合电极等。通过上述对钛酸锂材料的改进方法,已经大大提升了钛酸锂负极材料的倍率性能。由于其同时具有高安全性,被认为比碳负极更加适合用于高功率放电。

1.2 钛酸锂负极电池研究进展

钛酸锂负极对多种正极材料都具有良好的适应性。JANSEN等[21]使用LiCoO2作为正极材料制备了在2.0 ~ 2.7 V间循环的电池,循环过程包括9 s脉冲、18 s搁置、10 s充电脉冲和23 s低电流充电,这些电池在117 000次循环后仍保持充放电性能。MAJIMA等[52]制作的LTO/LCO电池得到了4 000次以上的循环寿命,远高于石墨负极电池的2 800次。GUO等[53]制备了Li4Ti5O12-石墨烯复合材料,呈现出良好的倍率性能和低温放电性能,用镍钴锰酸锂（LiNixCoyMn1-x-yO2, NMC）材料作为正极组装全电池,能够在8 C放电倍率下保留82%的容量。LI等[54]使用石墨烯泡沫作为基材制备了Li4Ti5O12/LiFePO4柔性全电池,其正极材料获得了200C的超高充放电倍率,并能在200 C下保持135 mA∙h/g的比容量,相当于1 C倍率下的80%;全电池在10 C倍率下能够保持1 C倍率的88%容量,并在此倍率下循环了100次,容量仅损失4%。
尖晶石LiMn2O4是另一种常用的和钛酸锂配合的正极材料。XI等[55]使用LiMn2O4正极和单晶Li4Ti5O12纳米棒制备了全电池,在10 C下能保持0.5 C倍率的84.8%,20 C下能够保持77.3%,且在10 C下循环1 000次后容量能够保持60%。YAN等[56]制备了尖晶石钛酸锂材料,并研究了不同正极-负极质量比的Li4Ti5O12/LiMn2O4全电池的电化学性能,得到的全电池能够在55℃下循环100次,容量保持率为88.9%。一些研究为了提高电池的工作电压,使用Ni部分取代Mn,制备了Li4Ti5O12/LiNi0.5Mn1.5O4全电池[57]。PANG等[58]使用中子粉末衍射研究了Li4Ti5O12/LiNi0.5Mn1.5O4全电池在充放电循环中的结构演变。REALE等[59]报道了以LiMn2O4和LiNi0.5Mn1.5O4为正极材料的两种钛酸锂负极全电池,工作电压分别为2.5 V和3.0 V,能够在2.5 C下运行,在0.2 C下循环100次后容量衰减率小于10%。ARIYOSHI等[60]组装的Li4Ti5O12/LiNi0.5Mn1.5O4全电池放电平台电压达到3.2 V,具有良好的循环稳定性,循环1 100次后容量保持率为83%。ARIYOSHI等认为,此种材料体系的锂离子电池的功率密度可达0.67 kW/kg或2.6 kW/L,能量密度为250 W∙h/kg或1 kW∙h/L。XIANG等[61]研究Li4Ti5O12/LiNi0.5Mn1.5O4电池中正负极容量匹配对循环性能、电解质选择、过充耐受性的影响,并建议在此种材料体系的电池中增加正极材料的容量,使总容量受制于钛酸锂负极的容量。
其他被用于和钛酸锂负极匹配的正极材料还包括高压阴极材料Li2MxMn(4-x)O8（Li2Co0.4Fe0.4Mn3.2O8等）[62]、LiCoPO4[63,64]、锂化的V2O5[65]等。但这些材料各自面临着诸如电解质选择、循环性能等问题,使这些材料体系在商业上价值不高。目前应用较广的钛酸锂负极电池和正极材料的选择仍以LiCoO2或NMC材料、LiMn2O4或LiNi0.5Mn1.5O4为主。

1.3 钛酸锂负极电池健康状态与老化研究

对比现行主流的石墨负极,钛酸锂作为负极材料在安全性、循环寿命、倍率性能、对过充/过放的容忍性和低温放电上都具有一定的优势,但其过高的对Li/Li+ 电势导致使用其做成的全电池相比使用同种正极材料的石墨负极电池工作电压降低1.4 V左右,且其理论比容量也比石墨负极低。因此在现今较重视电池能量密度的新能源汽车等商业应用方面,钛酸锂负极电池的发展较为受限,对其寿命性能的研究也较少,且往往集中于其倍率性能、低温放电等方面。
HANG等[66]对Li4Ti5O12/LiCoO2全电池在不同放电深度（depth of discharge, DOD）和温度下进行电化学阻抗谱（electrochemical impedance spectroscopy, EIS）分析,并建立了等效电路模型来解释测量到的交流阻抗。这项工作将该款电池的容量衰减归因于界面电阻的增加和正极容量的降低,并认为钛酸锂负极显著提高了电池的循环性能。这项工作同时报告了钛酸锂负极电池的两级衰减现象,即随着循环次数的增加,容量衰减速度先慢后快,在1 500次循环后突然增速,但没有给出解释。HAN等[67]对包括LTO/NMC在内的5款不同材料体系的商用锂离子电池使用容量增量（incremental capacity, IC）、差分电压（differential voltage, DV）曲线分析了老化机理。LTO/NMC电池在45℃/5℃下以1/3 C充电,1.5 C放电,循环1 020次后只能观察到轻微的总容量减少,电池内阻也没有增加,电池内部几乎没有钛酸锂活性物质的损失,但IC和DV曲线显示正极材料有所损失。与之相比,碳-磷酸铁锂（C/LFP）电池的容量损失主要归因于锂的损失和负极活性材料的损失,C/LMO电池的老化来自电阻增加和活性物质的损失。在HAN等[68]的进一步研究中,将3支钛酸锂负极电池在55℃下以3 C充电,2 C放电进行循环,均观察到HANG等[66]提到过的两级衰减现象,第二阶段的衰减速度达到第一阶段的2 ~ 3倍。HAN等将这种现象归因于在电池的制造过程中,相对于负极材料加入了更多的正极材料,且正极材料的容量衰减率更高。第一阶段电池容量损失主要由负极材料损失导致,容量损失率较低;而第二阶段容量损失由正极材料损失导致,衰减率显著上升。
FARMANN等[69]测试了包含LTO/NMC电池在内的多种锂电池的开路电压（open circuit voltage, OCV）特性和弛豫行为受老化程度和温度的影响,并建立了考虑温度修正项和电池老化状态的OCV模型。该工作提到,相比石墨负极电池,钛酸锂负极电池的OCV梯度受温度的影响更为明显,在60%荷电状态（state of charge, SOC）下这种影响达到最大。
DUBARRY等[70]对夏威夷岛电网使用的基于LTO/(LCO+LiNixCoyAl1-x-yO2) 电池的1 MW/250 kW∙h储能系统三年来的运行数据进行了调查,并提供了系统容量退化的初步估计。在接下来的工作中,DUBARRY等[71]使用该项数据评估多个因素对钛酸锂电池老化的影响,包括充放电速率、SOC摆动范围和温度等,试图将钛酸锂电池在电网储能中的实际应用表现和实验室测试联系起来。在这项工作中,他们发现温度对电池退化的影响最大,其次是倍率和SOC。研究涉及的电池在保持低于35℃时不会显著老化,但会因暴露在45℃以上的温度而老化,这种老化在SOC非常低的情况下尤其显著。此外,电池在低SOC下的放置和小SOC波动下的循环也会导致更快的容量流失,前者和石墨负极的锂电池恰恰相反。在此基础上,BAURE等[72]使用容量增量法分析了更详细的老化过程。结果表明,此种电芯的衰减情况高度依赖于使用情况,负极材料的损失、正极材料的损失和锂损失在24个测试条件下呈现高度的独立性。IC分析显示,由此产生的全电池容量损失由负极材料损失主导,但随着老化过程的发展,正极LiNixCoyAl1-x-yO2材料的损失会成为主要的失效模式。BAURE等还对两个在2016年部署的电网储能系统进行了研究[73],这些储能系统使用LTO/NMC电池,对这些电池的电化学特性进行了研究以探寻所谓的“静默老化”过程。在450多天的循环中,电池仅损失了容量的0.6%。电化学分析显示,正极材料的损失遵循幂指数增加,锂损失维持线性趋势,而负极材料的损失不显著。在日历老化中则没有观察到明显的损失。BAURE等据此推测,在电网储能应用中,LTO/NMC电池寿命可以达到20年;如果温度维持在35℃以下,容量损失还可以更小。
BANK等[74]的工作同样证实了钛酸锂负极电池的日历老化在很大程度上依赖于环境温度和SOC。他们在60℃和80℃下对10 A∙h LTO/NMC电池进行了不同SOC下的日历老化[75]。结果表明,在60℃下几乎没有发生任何不可逆的老化,而在80℃下发生了明显的锂损失和正极活性物质损失,在高SOC下尤甚。值得注意的是,这与BAURE等[72]观察到的现象有所差异,这可能是正极材料和电池充放电行为的不同导致。
STROE等[76]对LTO/NMC电池进行了不同温度、倍率和SOC下的大功率加速循环老化试验,将两枚电池分别在42.5℃和50℃下以50% DOD进行循环。结果显示,当电池容量衰减至40%后,电池的功率性能呈指数级下降;在老化的末期,观察到了迅速的内阻增长,最终可达到初始的4倍;对于老化后的LTO/NMC电池,能量效率仍然可以达到80% ~ 90%,和初始的90%以上效率差距不大。
LIU等[77]对NMC材料为正极、钛酸锂材料为负极的10 A∙h电池在室温下分别以5 C和10 C的充放电倍率进行了老化循环试验。结果表明,正极材料的损失是电池容量损失的主要原因,而锂损失主要发生在循环电流较低的老化过程中。同时,当循环电流较低时,较高的DOD导致了更快的老化过程。除此之外,还有一些关于钛酸锂负极电池滥用的研究。如DEVIE等[78,79]的工作观察到过充电导致了更大的容量衰减,并将其归咎于负极活性材料的损失,提出并验证了过充导致的电解质分解产气阻塞局部离子通路的假设。发现过充电后对电池进行物理按摩可以恢复最多60%因过充导致的容量损失。WANG等[80]测试了钛酸锂负极电池在低温下的过充耐受性,并提出了用过充来补偿低温下的容量损失的方法,但代价是电池性能会下降。LIU等[81]研究了LTO/NMC电池在不同阶段的产气行为,并提出了可能的气体产生机制。HARDING等[82]对比了用于医疗植入的石墨基和钛酸锂基的锂电池在0 V状态下的储存情况,钛酸锂基电池表现出了明显的稳定性,被认为在37℃下具有出色的长期性能（5年以上）。
由于钛酸锂负极电池的商业应用较少,与之相关的老化模型工作也处于起步阶段。CHAOUI等[83] 2017年的一项工作在使用钛酸锂负极电池的电动汽车上进行了在线SOC和健康状态（state of health, SOH）估计的测试,使用电池的端电压、充放电电流和温度等参数来同时估计电池的SOC和SOH。ZHANG等[84]用反向传播神经网络（back-propagation neural network, BPNN）分析从钛酸锂负极电池的EIS谱中提取的直流内阻和极化内阻对电池老化造成的影响,提供了一个较准确的SOH估计;HASHEMI等[85]针对混合动力飞机上使用的钛酸锂负极电池提出了一种在线参数估计方法和自适应SOH估计方法,在不同的工作温度下得到了小于1.3%的SOH估计误差。目前基于钛酸锂负极电池进行的数据驱动老化模型普遍没有较强的针对性,基本属于对碳负极锂电池建模工作的移植。对钛酸锂负极电池的电化学建模工作则更为稀少。SADABADI等[86]对LTO/NMC电池建立了一个增强型单粒子模型（enhanced single particle model, eSPM）用于跟踪电池的老化机制,这是首次将这方面的工具应用于此种材料体系的电池。
在作者课题组之前的工作中[87],将容量为18 A∙h、设计倍率为50 C的LTO/LMO电池在66 C下进行循环,观察到了快速而平滑的衰减过程,电池在66 C下的可用容量在10次循环内即衰减到初始值的80%以下,而在10 C以下的常规倍率下的容量没有发生显著变化。图3展示了这一结果,在66 C循环过程中,每隔10次循环进行一次不同倍率下的放电容量标定试验。结果显示,只有在高倍率的放电下电池容量迅速衰减,而在常规倍率下的放电几乎没有受到影响。
Fig. 3 Discharging curves of LTO/LMO batteries at different current during high-rate discharging cycles[87]

图3 随着高倍率循环进行,LTO/LMO电池在不同电流下的放电曲线[87]

Full size|PPT slide

图4展示了LTO/LMO电池在高倍率循环过程中的IC曲线。结果显示,电池中参与反应的活性物质随着循环进行而增加,但相变程度随着循环进行而降低,推测这种现象的成因是由于离子扩散速度的降低;循环试验前后的IC分析显示,电池在传统IC分析使用的低倍率充电电流下响应几乎没有变化,而在较高的充电电流（2 C）下产生了峰位置的右移,峰高度和面积几乎不变。这表明加速的极化过程导致了电池电压的迅速降低,从而影响了电池在高倍率下的可用容量,而非活性物质或锂本身的损失。在对电芯实验前后的电子计算机断层摄影（computer tomography, CT）扫描中,观测到尺寸为52.97 μm × 1 125.28 μm缝隙,这可能是局部过放电导致的产气造成的。
Fig. 4 Charging response of LTO/LMO batteries during high-rate discharging cycles[87]

图4 LTO/LMO电池高倍率循环过程中的充电响应曲线[87]

Full size|PPT slide

2 结论

钛酸锂材料作为锂离子电池的负极材料,具有结构稳定、安全性高、循环寿命优异、低温放电能力强等优点,在电网储能和电动汽车动力电池等方面具有广阔的应用前景。钛酸锂材料由于较高的对锂电位,降低了全电池的开路电压,从而在能量密度上有一定劣势,在现今的商业化电动汽车方面没有得到推广,但其较好的倍率性能使其在电动大巴、高功率调频电站等领域得到了一定应用。目前对钛酸锂电池的放电性能和寿命的研究仍然较少,且多集中于高功率放电、低温放电等特种应用领域。常规倍率（10 C及以下）下的钛酸锂电池展现出了非常优异的寿命性能,活性材料损失和锂损失的速度都较慢。而在更高倍率的放电中,电池的极化作用和电压跌落成为影响电池容量的主要因素。在常温储存方面,钛酸锂材料展现出了较优异的性能,仅在高温、高SOC下表现出了不可逆的容量损失。

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