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Article(id=1241081042644300505, tenantId=1146029695717560320, journalId=1235980550691926019, issueId=1241081025531540408, articleNumber=null, orderNo=null, doi=10.3969/j.issn.0253-6099.2024.04.002, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1713801600000, receivedDateStr=2024-04-23, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1773826378737, onlineDateStr=2026-03-18, pubDate=1722441600000, pubDateStr=2024-08-01, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1773826378737, onlineIssueDateStr=2026-03-18, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1773826378737, creator=13701087609, updateTime=1773826378737, updator=13701087609, issue=Issue{id=1241081025531540408, tenantId=1146029695717560320, journalId=1235980550691926019, year='2024', volume='44', issue='4', pageStart='1', pageEnd='258', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1773826374657, creator=13701087609, updateTime=1773827517159, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1241085817590960730, tenantId=1146029695717560320, journalId=1235980550691926019, issueId=1241081025531540408, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1241085817590960731, tenantId=1146029695717560320, journalId=1235980550691926019, issueId=1241081025531540408, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=8, endPage=12, ext={EN=ArticleExt(id=1241081043994866421, articleId=1241081042644300505, tenantId=1146029695717560320, journalId=1235980550691926019, language=EN, title=Mechanism for Influence of Atomic Layer Deposition of Al2O3 on Spinel LiNi0.5Mn1.5O4 Cathode Material, columnId=1241081026567533498, journalTitle=Mining and Metallurgical Engineering, columnName=SPECIAL ISSUE: BATTERY MATERIALS, runingTitle=null, highlight=null, articleAbstract=

To improve the interfacial stability of spinel phase LiNi0.5Mn1.5O4 cathode material in deeply charged state, a nanoscale Al2O3 film was deposited on the surface of single-crystal LiNi0.5Mn1.5O4 by atomic layer deposition in a controlled manner. The modified cathode material exhibits excellent long-cycle performance and corrosion resistance (with capacity retention rate up to 94.7% after 500 cycles at 1C). The surface and interface analysis shows that the nanoscale Al2O3 coating deposited by atomic layer deposition technology can significantly inhibit the corrosion reaction between material and electrolyte, and also constrain the irreversible dissolution and precipitation of transition metal ions. In addition, AlF3 produced by HF surface etching can enhance corrosion resistance of LiNi0.5Mn1.5O4 cathode material, which can thus improve its long-cycle performance and the service performance at high voltage.

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为提升尖晶石相LiNi0.5Mn1.5O4正极材料在深度荷电状态下的界面稳定性，采用原子层沉积法在单晶LiNi0.5Mn1.5O4正极材料表面可控沉积了纳米级Al2O3层。改性后的LiNi0.5Mn1.5O4正极材料表现出优异的长循环耐腐蚀性能（1C电流密度下循环500次的容量保持率高达94.7%）。进一步的表界面解析结果表明：原子层沉积技术构建的纳米级Al2O3包覆层能够明显抑制材料本体与电解液的腐蚀反应，降低过渡金属离子的不可逆溶解与析出；另外，基于HF表面刻蚀产生的AlF3具有增强的耐刻蚀性能，可显著提升LiNi0.5Mn1.5O4正极材料在长循环及高电压下的服役性能。

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李倩（1986—），女，宁夏海原人，博士，副教授，主要从事储能电池材料研究。E-mail：

, authorsList=李倩, 赵妍, 崔雅茹, 王硕然, 黄娜, 李常林, 王文培, 马红周, 杜金晶, 何喜红, 翁雅青)}, authors=[Author(id=1241081049606844539, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241081042644300505, orderNo=0, firstName=null, middleName=null, lastName=null, nameCn=null, orcid=null, stid=null, country=null, authorPic=null, dead=0, email=lq@xauat.edu.cn, emailSecond=null, emailThird=null, correspondingAuthor=0, authorType=1, ext={EN=AuthorExt(id=1241081049707507844, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241081042644300505, authorId=1241081049606844539, language=EN, stringName=Qian LI, firstName=Qian, middleName=null, lastName=LI, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=1, address=1.School of Metallurgical Engineering, Xi'an University of Architecture and Technology, Xi'an 710055, Shaanxi, China, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null), CN=AuthorExt(id=1241081049812365452, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241081042644300505, authorId=1241081049606844539, language=CN, stringName=李倩, firstName=null, middleName=null, lastName=null, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=1, address=1.西安建筑科技大学 冶金工程学院，陕西 西安 710055, bio={"content":"

李倩（1986—），女，宁夏海原人，博士，副教授，主要从事储能电池材料研究。E-mail：

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李倩（1986—），女，宁夏海原人，博士，副教授，主要从事储能电池材料研究。E-mail：

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（a）LNMO-P；（b）LNMO-ALD

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（a）LNMO-P；（b）LNMO-ALD

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（a）LNMO-P；（b）LNMO-ALD

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原子层沉积Al2O3对尖晶石LiNi0.5Mn1.5O4正极材料的影响机理
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李倩 1 , 赵妍 1 , 崔雅茹 1 , 王硕然 1 , 黄娜 1 , 李常林 1 , 王文培 1 , 马红周 1 , 杜金晶 1 , 何喜红 1 , 翁雅青 2
矿冶工程杂志 | 电池材料专题 2024,44(4): 8-12
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矿冶工程杂志 | 电池材料专题 2024, 44(4): 8-12
原子层沉积Al2O3对尖晶石LiNi0.5Mn1.5O4正极材料的影响机理
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李倩1 , 赵妍1, 崔雅茹1, 王硕然1, 黄娜1, 李常林1, 王文培1, 马红周1, 杜金晶1, 何喜红1, 翁雅青2
作者信息
  • 1.西安建筑科技大学 冶金工程学院，陕西 西安 710055
  • 2.江西省科学院 应用化学研究所，江西 南昌 330012

    • 李倩（1986—），女，宁夏海原人，博士，副教授，主要从事储能电池材料研究。E-mail：

Mechanism for Influence of Atomic Layer Deposition of Al2O3 on Spinel LiNi0.5Mn1.5O4 Cathode Material
Qian LI1 , Yan ZHAO1, Yaru CUI1, Shuoran WANG1, Na HUANG1, Changlin LI1, Wenpei WANG1, Hongzhou MA1, Jinjing DU1, Xihong HE1, Yaqing WENG2
Affiliations
  • 1.School of Metallurgical Engineering, Xi'an University of Architecture and Technology, Xi'an 710055, Shaanxi, China
  • 2.Institute of Applied Chemistry, Jiangxi Academy of Sciences, Nanchang 330012, Jiangxi, China
出版时间: 2024-08-01 doi: 10.3969/j.issn.0253-6099.2024.04.002
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摘要
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为提升尖晶石相LiNi0.5Mn1.5O4正极材料在深度荷电状态下的界面稳定性，采用原子层沉积法在单晶LiNi0.5Mn1.5O4正极材料表面可控沉积了纳米级Al2O3层。改性后的LiNi0.5Mn1.5O4正极材料表现出优异的长循环耐腐蚀性能（1C电流密度下循环500次的容量保持率高达94.7%）。进一步的表界面解析结果表明：原子层沉积技术构建的纳米级Al2O3包覆层能够明显抑制材料本体与电解液的腐蚀反应，降低过渡金属离子的不可逆溶解与析出；另外，基于HF表面刻蚀产生的AlF3具有增强的耐刻蚀性能，可显著提升LiNi0.5Mn1.5O4正极材料在长循环及高电压下的服役性能。

锂离子电池  /  LiNi0.5Mn1.5O4  /  正极材料  /  原子层沉积  /  Al2O3  /  表面改性

To improve the interfacial stability of spinel phase LiNi0.5Mn1.5O4 cathode material in deeply charged state, a nanoscale Al2O3 film was deposited on the surface of single-crystal LiNi0.5Mn1.5O4 by atomic layer deposition in a controlled manner. The modified cathode material exhibits excellent long-cycle performance and corrosion resistance (with capacity retention rate up to 94.7% after 500 cycles at 1C). The surface and interface analysis shows that the nanoscale Al2O3 coating deposited by atomic layer deposition technology can significantly inhibit the corrosion reaction between material and electrolyte, and also constrain the irreversible dissolution and precipitation of transition metal ions. In addition, AlF3 produced by HF surface etching can enhance corrosion resistance of LiNi0.5Mn1.5O4 cathode material, which can thus improve its long-cycle performance and the service performance at high voltage.

lithium-ion battery  /  LiNi0.5Mn1.5O4  /  cathode material  /  atomic layer deposition  /  Al2O3  /  surface modification
李倩, 赵妍, 崔雅茹, 王硕然, 黄娜, 李常林, 王文培, 马红周, 杜金晶, 何喜红, 翁雅青. 原子层沉积Al2O3对尖晶石LiNi0.5Mn1.5O4正极材料的影响机理. 矿冶工程杂志, 2024 , 44 (4) : 8 -12 . DOI: 10.3969/j.issn.0253-6099.2024.04.002
Qian LI, Yan ZHAO, Yaru CUI, Shuoran WANG, Na HUANG, Changlin LI, Wenpei WANG, Hongzhou MA, Jinjing DU, Xihong HE, Yaqing WENG. Mechanism for Influence of Atomic Layer Deposition of Al2O3 on Spinel LiNi0.5Mn1.5O4 Cathode Material[J]. Mining and Metallurgical Engineering, 2024 , 44 (4) : 8 -12 . DOI: 10.3969/j.issn.0253-6099.2024.04.002
正文
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随着电动汽车和规模储能电站的快速发展，行业内对锂离子电池的能量密度和储能成本提出了更高要求[1-2]。与传统正极材料相比，LiNi0.5Mn1.5O4（LNMO）正极材料具有较高的工作电位和较低的材料成本而备受关注[3-6]。然而，界面副反应以及过渡金属溶解严重制约了其商业化进程[7]。通过对正极材料进行包覆改性可以直接减少材料与电解液接触，提高该材料的循环性能[8-9]。目前，原子层沉积（atomic layer deposition，ALD）策略已被证明是显著提高电池性能和安全性的有效手段[10-11]。本文采用原子层沉积法在LiNi0.5Mn1.5O4颗粒表面沉积纳米级Al2O3层，并阐明了Al2O3层对LiNi0.5Mn1.5O4正极材料电化学性能提升的作用机理。
1 实验
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1.1 LNMO-P样品的制备
将0.010 5 mol的硝酸锂（LiNO3，99.9%，上海阿拉丁生化科技股份有限公司）和0.020 0 mol的镍锰氢氧化物前驱体（Ni0.25Mn0.75（OH）2，99.9%，陕西煤业化工技术研究院责任有限公司）研磨混合后放入马弗炉中进行两次烧结：第1次在300 ℃下烧结2 h，以去除材料中的水分；第2次在900 ℃下烧结10 h，使其均匀反应形成LNMO晶体并长大。样品取名为LNMO-P。
1.2 LNMO-ALD样品的制备
在所制备的LNMO-P粉末上进行Al2O3原子层沉积，经过10次Al2O3原子层沉积循环后得到LNMO-ALD样品。Al2O3原子层沉积的时序为t1-t2-t3-t4，其中t1=5 s和t3=3 s分别是三甲基铝（C3H9Al，2.0 mol/L，保存在甲苯中，上海阿拉丁生化科技股份有限公司）和去离子水（H2O，实验室超纯水机制备）的暴露时间，t2=60 s和t4=45 s是前体剂量之间使用的相应吹扫时间。图1为使用三甲基铝和水作为反应物的Al2O3原子层沉积示意图。
1.3 材料的表征
使用荷兰Panalytical公司生产的Xpert Pro MPD型X射线衍射仪（XRD）分析材料结构；采用美国FEI公司生产的NovaTM Nano SEM450型场发射扫描电子显微镜（SEM）和JEOL JEM F200型透射电镜（HRTEM）分析样品形貌；采用Agilent 5110电感耦合等离子体光谱仪（ICP-OES）分析电池循环后拆解出的负极锂片元素含量；采用日本PHI公司生产的PHI 5000 VersaProbe III型X射线光电子能谱仪（XPS）分析材料的表面化学状态。
1.4 材料的电化学性能测试
活性电极的制备方法：将制备好的样品与Black Carbon、PVDF按照质量比85∶10∶5混合。使用匀浆机将它们充分混合，制备出黏度适中且具有良好流动性的正极浆料。使用涂布机进行涂布，涂布厚度为150 μm。然后对其进行真空干燥（110 ℃，12 h），干燥后使用裁片机将其切成圆片（直径12 mm），即得到本实验所需的正极片。在手套箱（w（H2O）≤0.1×10-6；w（O2）≤0.1×10-6）中将其组装成CR2032扣式电池。
电化学性能测试条件为：测试电压范围3.0～4.9 V；测试温度为室温；进行循环性能测试时，电池首先在0.1C（1.0C=147 mAh/g）电流密度下活化两圈，再于1.0C电流密度下进行长循环。使用武汉蓝电电子股份有限公司生产的LANHE型测试仪进行电化学性能测试。
2 实验结果与讨论
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2.1 LNMO-P和LNMO-ALD样品的形貌和结构分析
LNMO-P和LNMO-ALD样品SEM图如图2所示。从图2可见，LNMO-P样品呈现明显的单晶状态，表面光滑平整。相对LNMO-P样品，LNMO-ALD样品的形貌未发生明显变化，表明纳米级的Al2O3原子沉积层对颗粒形貌影响不大。
为了观察Al2O3原子层沉积对本体材料物相结构的影响，分别对2个样品进行XRD表征，结果见图3。由图3可见，沉积前后2个样品的衍射峰都可以被索引为具有空间群的尖晶石结构，且无其他杂质峰；同时，2个样品均具有较好的结晶性，说明纳米级的Al2O3原子层沉积并不会影响材料的结晶度。由于Al2O3的沉积量很少，未检测到Al2O3的衍射峰。
通过HRTEM和HRTEM Mapping对LNMO-ALD样品的Al2O3沉积厚度和元素分布进行了表征，结果如图4所示。在经过10次Al2O3原子层沉积循环后，成功在LNMO颗粒表面沉积了致密的Al2O3涂层，其厚度约2 nm。同时，Al、O、Ni、Mn元素分布均匀，说明Al2O3涂层均匀分布在LNMO颗粒表面。
为了解原子层沉积后LNMO-ALD样品表面Al的化学状态，对其进行了XPS测试，结果如图5所示。结果显示，材料表面存在Al元素的痕迹，在～74.5 eV的预期位置上观察到Al2p的特征峰，其对应为Al2O3。
2.2 LNMO-P和LNMO-ALD电极的电化学性能
为了评估Al2O3原子层沉积对材料电化学性能的影响，测试了LNMO-P和LNMO-ALD制备的扣式电池在3.0～4.9 V电压区间下的电化学性能，图6为LNMO-P和LNMO-ALD电极的充放电曲线。由图6可见，2个电极的充放电平台一致，初始容量没有太大变化，其原因为Al2O3为非活性物质，并不会带来容量贡献，充放电曲线并未出现变化。
为了评估Al2O3原子层沉积对材料长循环性能的影响，将LNMO-P和LNMO-ALD电极在1C，3.0～4.9 V电压区间下进行了长期循环测试。图7为2个电极的循环性能图。由图7可见，500次循环后，LNMO-ALD正极显示出了较高的容量保持率（94.7%），而LNMO-P正极的容量保持率较低（83.0%），这说明Al2O3原子层沉积对LNMO正极材料表面有较好的保护作用，提高了LNMO正极材料的长循环容量保持率。
2.3 LNMO-P和LNMO-ALD电极的失效分析
以上研究表明，纳米级Al2O3原子层沉积有效提升了LNMO正极材料的长循环性能，但其影响机理还需进一步探究。基于此，本文对长循环500次后的电池进行拆解，对正极材料、负极锂片等进行对比分析。
LNMO-P和LNMO-ALD正极材料500次循环后SEM表征结果如图8所示。由图8可见，2个样品在经历电化学反应后，表面均出现了副产物的堆积。相较于LNMO-P样品，LNMO-ALD样品表面副产物沉积量显著减少，表面依旧平整，这说明Al2O3原子层沉积有效降低了电解液对LNMO正极材料的侵蚀，减少了电化学反应过程中副反应的发生。
在高电位下，正极材料可能进一步与电解液反应，形成电极电解质界面膜（cathode electrolyte interphase，CEI），因此可以通过CEI演变行为来判断本体材料与电解液界面的稳定程度[12]。本文通过HRTEM对长循环后正极材料表面的CEI情况进行探究，结果如图9所示。从图9可以看到，LNMO-P样品表面所生成的CEI厚且不均匀，其厚度为6～15 nm；LNMO-ALD样品CEI呈现出薄且均匀的状态，其厚度约4 nm。通过上述对比可以得知，在电化学反应过程中，LNMO-ALD样品表面生成了更加稳定的CEI，Al2O3沉积层的存在为LNMO材料本体提供了良好的保护，使其长循环性能得到了提升。
采用XPS对循环500次后的LNMO-P和LNMO-ALD电极表面的界面层进行了分析，结果分别见图10和图11。从图10～11可以看到，循环500次后，2个样品的F1s XPS光谱存在不同的特征峰，LNMO-P样品的F1s XPS光谱存在2个特征峰，LNMO-ALD样品的F1s XPS光谱存在3个特征峰（684.9 eV对应LiF，687.7 eV对应PVDF，686.6 eV对应AlF3）。LNMO-P和LNMO-ALD正极表面均有LiF的存在，LiF主要为电化学过程中电解液分解及电极电解质界面副反应产物。2个样品的不同之处为LNMO-ALD正极表面存在AlF3特征峰，其为沉积的Al2O3在电化学过程中与电解液分解产物进行反应生成的副产物。AlF3可在材料表面起到物理阻隔作用，进一步保护LNMO正极材料，这与之前关于Al2O3涂层正极材料的报道[13-14]一致。
过渡金属溶出是影响LNMO正极材料电化学性能的重要因素。过渡金属溶出后会导致活性材料损失，其会穿过隔膜在负极上还原沉积，堵塞负极的Li+通道，阻碍锂脱嵌过程中的电荷传递，降低电池的比容量。电解液中HF对LNMO颗粒的界面侵蚀是造成过渡金属溶出的直接原因。为更直观地表征电化学过程中过渡金属的溶出程度，对循环500次后LNMO-P和LNMO-ALD半电池中的锂片进行ICP-OES测试，结果如图12所示。由图12可以发现，LNMO-ALD样品过渡金属的溶出量明显小于LNMO-P样品，这表明Al2O3沉积层在电化学过程中能够有效缓解LNMO本体材料中Mn离子的溶出，进而提升LNMO的长循环性能。
3 结论
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1）通过10次Al2O3原子层沉积循环成功制备了具有纳米级（～2 nm）Al2O3沉积层的LiNi0.5Mn1.5O4正极材料。
2）Al2O3沉积后的LiNi0.5Mn1.5O4正极材料显示出优异的长循环性能，500次循环后容量保持率达94.7%，证实原子层沉积Al2O3是提升LiNi0.5Mn1.5O4正极材料长循环性能的有效手段。
3）原子层沉积Al2O3对LiNi0.5Mn1.5O4正极材料电化学性能的影响机理为：一是原子层沉积Al2O3降低了服役过程中LiNi0.5Mn1.5O4正极材料的过渡金属溶出量，二是其有效缓解了LiNi0.5Mn1.5O4正极材料在服役过程中的界面副反应，从而协同提升了LiNi0.5-Mn1.5O4正极材料的电化学性能。
基金
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  • 国家重点研发计划(2023YFC3905904)
  • 陕西省自然科学基金(2020JQ-679)
  • 陕西省自然科学基金(2019JLM-36)
  • 陕西省重点实验室项目(20JS064)
  • 陕西省区域创新能力引导计划(2022QFY10-05)
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参考文献 引证文献
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HUANG Y, DONG Y, LI S, et al. Lithium manganese spinel cathodes for lithium-ion batteries[J]. Advanced Energy Materials, 2021, 11(2): 2000997.
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LIN F, WU H, CHEN T, et al. The Cu-Y co-doping LiNi0.5Mn1.5O4 with modified morphology and enhanced electrochemical property for a 5 V lithium-ion battery[J]. Journal of Materials Science-Materials in Electronics, 2022, 33(1): 283-297.
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CHEN T, YANG J, BARROSO-LUQUE L, et al. Removing the two-phase transition in spinel LiMn2O4 through cation disorder[J]. ACS Energy Letters, 2023, 8(1): 314-319.
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2024年第44卷第4期
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doi: 10.3969/j.issn.0253-6099.2024.04.002
  • 接收时间：2024-04-23
  • 首发时间：2026-03-18
  • 出版时间：2024-08-01
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  • 收稿日期：2024-04-23
基金
国家重点研发计划(2023YFC3905904)
陕西省自然科学基金(2020JQ-679)
陕西省自然科学基金(2019JLM-36)
陕西省重点实验室项目(20JS064)
陕西省区域创新能力引导计划(2022QFY10-05)
作者信息
    1.西安建筑科技大学 冶金工程学院，陕西 西安 710055
    2.江西省科学院 应用化学研究所，江西 南昌 330012
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https://castjournals.cast.org.cn/joweb/kygczz/CN/10.3969/j.issn.0253-6099.2024.04.002
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2种不同金属材料的力学参数
科
Family		 属数
Number of
genus		 种数
Number of
species		 占总种数比例
Percentage of
total species (%)		 属
Genus		 种数
Number of
species		 占总种数比例
Percentage of total
species (%)
鹅膏菌科Amanitaceae 2 11 5.26 鹅膏菌属 Amanita 10 4.78
小菇科 Mycenaceae 2 12 5.74 丝盖伞属 Inocybe 5 2.39
多孔菌科 Polyporaceae 8 14 6.70 蜡蘑属 Laccaria 5 2.39
红菇科 Russulaceae 3 23 11.00 小皮伞属 Marasmius 6 2.87
小菇属 Mycena 11 5.26
光柄菇属 Pluteus 5 2.39
红菇属 Russula 17 8.13
栓菌属 Trametes 5 2.39
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