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Article(id=1241321982785024254, tenantId=1146029695717560320, journalId=1235980550691926019, issueId=1241321979433767757, articleNumber=null, orderNo=null, doi=10.3969/j.issn.0253-6099.2024.02.032, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1698595200000, receivedDateStr=2023-10-30, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1773883823343, onlineDateStr=2026-03-19, pubDate=1711900800000, pubDateStr=2024-04-01, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1773883823343, onlineIssueDateStr=2026-03-19, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1773883823343, creator=13701087609, updateTime=1773883823343, updator=13701087609, issue=Issue{id=1241321979433767757, tenantId=1146029695717560320, journalId=1235980550691926019, year='2024', volume='44', issue='2', pageStart='1', pageEnd='191', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1773883822544, creator=13701087609, updateTime=1773884556149, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1241325056454881881, tenantId=1146029695717560320, journalId=1235980550691926019, issueId=1241321979433767757, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1241325056454881882, tenantId=1146029695717560320, journalId=1235980550691926019, issueId=1241321979433767757, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=141, endPage=144, ext={EN=ArticleExt(id=1241321983091208449, articleId=1241321982785024254, tenantId=1146029695717560320, journalId=1235980550691926019, language=EN, title=Rb+ and Cl- Co-doped LiNi0.8Co0.1Mn0.1O2 Cathode Material for High-Performance Lithium Ion Batteries by One-Step Method, columnId=1236276108207902848, journalTitle=Mining and Metallurgical Engineering, columnName=MATERIALS, runingTitle=null, highlight=null, articleAbstract=

To solve the problem of structural instability of cathode material (LiNi0.8Co0.1Mn0.1O2)(NCM)) during cycling, a strategy of co-doping of Rb+ and Cl- was proposed for NCM materials. The synergistic effect of co-doping of Rb+ and Cl- in the NCM lattice can increase the diffusion rate of Li+ and relieve the internal strain, thus hindering the mixing of Li+/Ni2+ during high cut-off voltage cycling. Electrochemical test results show that Li0.99Rb0.01(Ni0.8Co0.1Mn0.1) O1.99Cl0.01 (RbCl-NCM) has a discharge capacity up to 176.9 mAh/g at a current density of 10C. The initial discharge capacity at 1C is 203.5 mAh/g. After 200 cycles, its capacity retention ratio is as high as 87.8%, showing an excellent cycling performance, while the capacity retention ratio of NCM material is only 57.3%.

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针对LiNi0.8Co0.1Mn0.1O2（NCM）正极材料在循环过程中结构不稳定的问题，提出了Rb+/Cl-双位点共掺杂NCM材料的策略。NCM晶格中Rb+/Cl-双位点共掺杂的协同效应提高了Li+扩散速率，缓解了内部应变，抑制了高截止电压循环时Li+/Ni2+的混排。电化学测试结果表明，Li0.99Rb0.01（Ni0.8Co0.1Mn0.1）O1.99Cl0.01（RbCl-NCM）材料在电流密度10C下放电容量高达176.9 mAh/g；RbCl-NCM材料在电流密度1C下首次放电容量203.5 mAh/g，且具有优异的循环性能，经200个循环后，容量保持率高达87.8%，而NCM材料在相同测试条件下的容量保持率仅57.3%。

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赖飞燕（1989—），女，广西玉林人，博士，副研究员，主要研究方向为新能源材料与技术。E-mail：
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杨桂芬（1984—），女，广西柳州人，硕士，工程师，主要研究方向为新能源汽车产品检测。E-mail：

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杨桂芬（1984—），女，广西柳州人，硕士，工程师，主要研究方向为新能源汽车产品检测。E-mail：

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杨桂芬（1984—），女，广西柳州人，硕士，工程师，主要研究方向为新能源汽车产品检测。E-mail：

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（a）NCM，SEM；（b）NCM，TEM；（c）NCM，HRTEM；（d）RbCl-NCM，SEM；（e）RbCl-NCM，TEM；（f）RbCl-NCM，HRTEM

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（a）Ni2p；（b）Rb3d；（c）Cl2p

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（a）电流密度0.1C下的首次充放电曲线；（b）不同倍率下的放电曲线；（c）1C电流密度下的循环曲线

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（a）NCM；（b）RbCl-NCM

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一步法实现Rb+/Cl-双位点共掺杂高性能锂离子电池正极材料LiNi0.8Co0.1Mn0.1O2
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杨桂芬 1, 2 , 杨广场 2 , 方明 2 , 杨怡诗 2 , 赖飞燕 2
矿冶工程杂志 | 材料 2024,44(2): 141-144
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矿冶工程杂志 | 材料 2024, 44(2): 141-144
一步法实现Rb+/Cl-双位点共掺杂高性能锂离子电池正极材料LiNi0.8Co0.1Mn0.1O2
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杨桂芬1, 2 , 杨广场2, 方明2, 杨怡诗2, 赖飞燕2
作者信息
  • 1.深圳市计量质量检测研究院，广东　深圳　518055
  • 2.贺州学院　广西碳酸钙资源综合利用重点实验室，广西　贺州　542899

    • 杨桂芬（1984—），女，广西柳州人，硕士，工程师，主要研究方向为新能源汽车产品检测。E-mail：

通讯作者:

赖飞燕（1989—），女，广西玉林人，博士，副研究员，主要研究方向为新能源材料与技术。E-mail：
Rb+ and Cl- Co-doped LiNi0.8Co0.1Mn0.1O2 Cathode Material for High-Performance Lithium Ion Batteries by One-Step Method
Guifen YANG1, 2 , Guangchang YANG2, Ming FANG2, Yishi YANG2, Feiyan LAI2
Affiliations
  • 1.Shenzhen Academy of Metrology and Quality Inspection, Shenzhen 518055, Guangdong, China
  • 2.Guangxi Key Laboratory of Calcium Carbonate Resources Comprehensive Utilization, Hezhou University, Hezhou 542899, Guangxi, China
出版时间: 2024-04-01 doi: 10.3969/j.issn.0253-6099.2024.02.032
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摘要
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针对LiNi0.8Co0.1Mn0.1O2（NCM）正极材料在循环过程中结构不稳定的问题，提出了Rb+/Cl-双位点共掺杂NCM材料的策略。NCM晶格中Rb+/Cl-双位点共掺杂的协同效应提高了Li+扩散速率，缓解了内部应变，抑制了高截止电压循环时Li+/Ni2+的混排。电化学测试结果表明，Li0.99Rb0.01（Ni0.8Co0.1Mn0.1）O1.99Cl0.01（RbCl-NCM）材料在电流密度10C下放电容量高达176.9 mAh/g；RbCl-NCM材料在电流密度1C下首次放电容量203.5 mAh/g，且具有优异的循环性能，经200个循环后，容量保持率高达87.8%，而NCM材料在相同测试条件下的容量保持率仅57.3%。

锂离子电池  /  三元正极材料  /  富镍层状氧化物  /  双位点掺杂  /  放电容量  /  电流密度  /  循环性能  /  容量保持率

To solve the problem of structural instability of cathode material (LiNi0.8Co0.1Mn0.1O2)(NCM)) during cycling, a strategy of co-doping of Rb+ and Cl- was proposed for NCM materials. The synergistic effect of co-doping of Rb+ and Cl- in the NCM lattice can increase the diffusion rate of Li+ and relieve the internal strain, thus hindering the mixing of Li+/Ni2+ during high cut-off voltage cycling. Electrochemical test results show that Li0.99Rb0.01(Ni0.8Co0.1Mn0.1) O1.99Cl0.01 (RbCl-NCM) has a discharge capacity up to 176.9 mAh/g at a current density of 10C. The initial discharge capacity at 1C is 203.5 mAh/g. After 200 cycles, its capacity retention ratio is as high as 87.8%, showing an excellent cycling performance, while the capacity retention ratio of NCM material is only 57.3%.

lithium-ion battery  /  ternary cathode materials  /  nickel-rich laminated oxide  /  double-site doping  /  discharge capacity  /  current density  /  cycling performance  /  capacity retention
杨桂芬, 杨广场, 方明, 杨怡诗, 赖飞燕. 一步法实现Rb+/Cl-双位点共掺杂高性能锂离子电池正极材料LiNi0.8Co0.1Mn0.1O2. 矿冶工程杂志, 2024 , 44 (2) : 141 -144 . DOI: 10.3969/j.issn.0253-6099.2024.02.032
Guifen YANG, Guangchang YANG, Ming FANG, Yishi YANG, Feiyan LAI. Rb+ and Cl- Co-doped LiNi0.8Co0.1Mn0.1O2 Cathode Material for High-Performance Lithium Ion Batteries by One-Step Method[J]. Mining and Metallurgical Engineering, 2024 , 44 (2) : 141 -144 . DOI: 10.3969/j.issn.0253-6099.2024.02.032
正文
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市场迫切需要高比能锂离子电池（大于500 Wh/kg），对正极材料的可逆容量和循环寿命提出了挑战性要求[1-3]。目前，LiNi0.8Co0.1Mn0.1O2（NCM）层状氧化物材料以其高容量、低成本和动力学性能的优势引领着正极材料的技术发展趋势[4-7]。然而，NCM材料在循环过程中存在结构不稳定和容量衰减严重的问题，这是因为NCM材料在循环中发生了严重的各向异性体积变化，晶格快速坍塌，影响了结构完整性，导致晶间裂纹的出现[8-12]。
针对上述问题，研究人员提出了许多改进方法，包括体相掺杂、表面涂覆、形貌/结构设计、表面处理等[13]。掺杂离子可取代部分过渡金属（TM）离子或占据某些特定位点，抑制TM离子迁移[14-16]。为了同时改善NCM材料的结构稳定性和倍率性能，本文提出了一步法制备Rb+/Cl-共掺杂Li0.99Rb0.01（Ni0.8Co0.1Mn0.1）O1.99Cl0.01（RbCl-NCM）材料的策略。Rb+的半径（0.133 nm）远大于Li+的半径（0.076 nm），NCM结构中Li+部分被Rb+取代可以减少Li+/Ni2+的混排和提高Li+的扩散能力。同时，Cl的共价半径和电负性远高于O，晶体结构中O2-部分被Cl-取代，可强化TM—O键，使结构更稳定，提高了循环性能。通过双位点共掺杂，NCM的循环性能和倍率性能得到了显著提高。
1　实验
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1.1　实验原料及方法
采用一步法制备Li0.99Rb0.01（Ni0.8Co0.1Mn0.1）O1.99-Cl0.01材料，具体步骤如下：将（Ni0.8Co0.1Mn0.1）（OH）2（粒度12 μm，贵州振华新材料有限公司）、RbCl（分析纯，99%）、LiOH·H2O（分析纯，99%）按照物质的量比0.99∶0.01∶1.05称量，使用斜式混料机（DSHS-6P，合肥科晶材料技术有限公司）混合后将其转移至马弗炉中，以升温速率5 ℃/min升温至480 ℃预烧5 h，于780 ℃保温15 h，最后，将样品自然冷却至150 ℃得到Li0.99Rb0.01（Ni0.8Co0.1Mn0.1）O1.99Cl0.01材料，将其标记为RbCl-NCM。在不添加RbCl条件下，按相同工艺制备Li（Ni0.8Co0.1Mn0.1）O2材料，将其标记为NCM。
1.2　电化学表征
正极片中正极材料、导电碳（SP）、伦琴黑（KS-6）、聚偏氟乙烯（PVDF）质量比为85∶5∶5∶5，正极片直径为12 mm，负载量为3.2 mg/cm2。在手套箱中组装成扣式电池，对电极为锂片，电解液由1 mol/L LiPF6溶解在碳酸二甲酯（DMC）、碳酸甲乙酯（EMC）和碳酸乙烯酯（EC）按体积比1∶1∶1混合的溶剂中构成。采用LAND-CT2001A型电池测试系统（武汉市蓝电电子股份有限公司）于室温下对材料进行测试，充放电电压区间为2.8～4.5 V，充放电电流以1.0C=200 mA/g计算；电化学阻抗谱（EIS）通过电化学工作站（CHI 660E）测试。
1.3　材料表征
采用X射线衍射仪（XRD，Rigaku，日本理学公司）分析物相结构，采用扫描电子显微镜（SEM，S-4800，日本日立公司）和透射电子显微镜（TEM，JSM-2010F，日本电子株式会社）观察材料的微观形貌，采用X射线光电子能谱分析仪（XPS，PHI QUANTERA-II SXM，日本真空公司）研究材料元素价态。
2　结果与讨论
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图1为NCM和RbCl-NCM样品的XRD图谱。所有样品均具有α-NaFeO2层状结构，R-3m空间群，且没有检测到杂质相。清晰的（006）/（102）和（108）/（110）峰分裂表明所有样品都具有有序的层状结构。NCM和RbCl-NCM材料的I（003）/I（104）强度比分别为1.62和1.80。通常认为I（003）/I（104）值大于1.2是材料具有良好层状结构的标准，I（003）/I（104）值越高，对应于晶格中Li+/Ni2+的无序化程度越低。所有样品的I（003）/I（104）值均大于1.2，表明其具有良好有序的层状结构。RbCl-NCM材料较NCM具有更高的I（003）/I（104）值，表明Rb+/Cl-共掺杂改性降低了Li+/Ni2+的混排程度。从图1中（003）晶面的扩展图谱可以看出，经Rb+/Cl-共掺杂改性后，RbCl-NCM材料的峰值向较低的角度偏移，表明NCM材料晶格参数c有所增加。上述分析表明，Rb+/Cl-成功进入NCM晶格中，使得晶胞参数c明显增加，有利于提高Li+的扩散速率，进而改善其电化学性能。
图2为NCM和RbCl-NCM样品的微观形貌。由图2可知，NCM和RbCl-NCM样品均表现出微米级椭球形形貌，表明Rb+/Cl-的掺杂不会破坏其微观形貌。NCM球表面有许多絮状沉积物，而RbCl-NCM球表面更光滑。采用高分辨率透射电镜（HRTEM）进一步研究样品的局部结构变化，发现NCM和RbCl-NCM样品均呈现良好的层状结构，且在表面和次表面区域并未发现异质相，说明Rb+/Cl-共掺杂并没有破坏NCM的层状结构。NCM晶面间距为0.496 nm，属于层状结构的（003）晶面，RbCl-NCM的（003）晶面间距为0.502 nm，比NCM略大，说明Rb+/Cl-共掺杂扩展了Li+层间距，有助于改善倍率性能。
为了研究Rb+/Cl-的掺杂对NCM材料表面元素化学态的影响，使用X射线光电子能谱技术对NCM和RbCl-NCM样品进行表面分析，结果如图3所示。RbCl-NCM的Rb3d和Cl2p高分辨谱中出现了Rb+和Cl-的特征峰，表明Rb+/Cl-成功进入NCM晶格中。此外，在对NCM和RbCl-NCM中Ni2P的高分辨图谱进行分峰处理后可知，两种样品表面的Ni均由Ni2+（854.5 eV）及Ni3+（855.6 eV）组成，经Rb+/Cl-共掺杂的NCM样品中，Ni2+相对含量较少，表明Rb+/Cl-共掺杂可以在一定程度上抑制Li+/Ni2+的无序化。
为了研究Rb+/Cl-掺杂前后材料的电化学性能，对上述两种正极材料进行了电化学性能测试，结果如图4所示。NCM和RbCl-NCM均呈现出典型的三元材料充放电特性。NCM和RbCl-NCM首次放电容量分别为217.4 mAh/g和220.2 mAh/g，初始库仑效率分别为83.9%和84.8%。掺杂Rb+/Cl-后的NCM材料在第一次嵌/脱锂离子过程中较未掺杂的NCM材料表现出更好的容量可逆性，表明Rb+/Cl-共掺杂可以维持结构稳定。
在2.8～4.5 V电位区间内，采用0.2C～10C电流密度检测样品倍率性能。随着电流密度增加，样品放电容量逐渐减小，电流密度0.2、0.5、1、2、3、5、10C下NCM的放电容量分别为217.6、210.0、200.2、189.9、182.2、172.1、154.3 mAh/g；相同条件下，RbCl-NCM的放电容量分别为216.2、213.1、205.4、198.6、193.5、186.5、176.9 mAh/g，在较大电流密度下，RbCl-NCM放电容量明显高于NCM。此外，电流密度从10C降回0.2C时，NCM容量降低了9 mAh/g，RbCl-NCM容量小幅增加。在典型的层状结构中，Li+在由a轴和b轴组成的平面内传输，而c轴的扩展可以提高Li+扩散速率。
为了评估NCM和RbCl-NCM的循环性能，将半电池在电流密度0.2C下活化3个循环，然后，在电流密度1C条件下进行200个室温循环。循环初期，NCM放电容量为204.3 mAh/g，略高于RbCl-NCM（203.5 mAh/g）。经过200个循环后，NCM放电容量衰减至117.1 mAh/g，容量保持率仅57.3%；而RbCl-NCM最终放电容量为178.6 mAh/g，容量保持率为87.8%。表明Rb+/Cl-双位点掺杂后，RbCl-NCM容量衰减得到抑制。
NCM和RbCl-NCM样品的CV曲线如图5所示。由图5可知，NCM和RbCl-NCM样品的氧化还原峰形状相似，这归因于Ni2+/Ni4+的氧化还原反应。ΔE表示氧化电位和还原电位的差值，RbCl-NCM的ΔE值为0.142 V，远小于NCM的ΔE值（0.295 V），表明RbCl-NCM中Li+嵌/脱过程的可逆性较好，这与NCM和RbCl-NCM首次充放电曲线的结果一致。此外，Rb+/Cl-双位点掺杂抑制了循环过程中的容量衰减。综上，Rb+/Cl-双位点掺杂可以减弱电极极化，提高电化学性能。
3　结论
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1）Rb+占据了部分Li+位点，稳定了NCM的晶体结构，增强了Li+的扩散动力学。
2）Li0.99Rb0.01（Ni0.8Co0.1Mn0.1）O1.99Cl0.01在10C电流密度下具有176.9 mAh/g的高容量；室温1C电流密度下首次放电容量为203.5 mAh/g，200个循环后，容量保持率高达87.8%。
基金
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  • 汽车标准化公益性开放课题(CATARC-Z-2022-01353)
  • 国家自然科学基金(51964013)
  • 广西自然科学基金(2024GXNSFAA010515; 2022GXNSFAA035610; 桂科AD23026038; 2020GXNSFBA297152)
文献
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2024年第44卷第2期
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doi: 10.3969/j.issn.0253-6099.2024.02.032
  • 接收时间：2023-10-30
  • 首发时间：2026-03-19
  • 出版时间：2024-04-01
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  • 收稿日期：2023-10-30
基金
汽车标准化公益性开放课题(CATARC-Z-2022-01353)
国家自然科学基金(51964013)
广西自然科学基金(2024GXNSFAA010515; 2022GXNSFAA035610; 桂科AD23026038; 2020GXNSFBA297152)
作者信息
    1.深圳市计量质量检测研究院，广东　深圳　518055
    2.贺州学院　广西碳酸钙资源综合利用重点实验室，广西　贺州　542899

通讯作者:

赖飞燕（1989—），女，广西玉林人，博士，副研究员，主要研究方向为新能源材料与技术。E-mail：
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https://castjournals.cast.org.cn/joweb/kygczz/CN/10.3969/j.issn.0253-6099.2024.02.032
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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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