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Article(id=1320107544404673145, tenantId=1146029695717560320, journalId=1263187385517883426, issueId=1320107530261479891, articleNumber=null, orderNo=null, doi=10.14062/j.issn.0454-5648.20250532, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1751904000000, receivedDateStr=2025-07-08, revisedDate=1754150400000, revisedDateStr=2025-08-03, acceptedDate=null, acceptedDateStr=null, onlineDate=1792667764998, onlineDateStr=2026-10-22, pubDate=1775664000000, pubDateStr=2026-04-09, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1792667764998, onlineIssueDateStr=2026-10-22, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1792667764998, creator=13701087609, updateTime=1792667764998, updator=13701087609, issue=Issue{id=1320107530261479891, tenantId=1146029695717560320, journalId=1263187385517883426, year='2026', volume='54', issue='7', pageStart='2171', pageEnd='2576', issueExtLink='null', onlineDate='null', pubDate='1784476800000', pubDateStr='2026-07-20', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1792667761625, creator='13701087609', updateTime=1792720444956, updator='13701087609', preIssue=null, nextIssue=null, articleTotal=null, ext={EN=IssueExt(id=1320328500238725499, tenantId=1146029695717560320, journalId=1263187385517883426, issueId=1320107530261479891, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1320328500238725500, tenantId=1146029695717560320, journalId=1263187385517883426, issueId=1320107530261479891, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null, downloadFileDto=null}, startPage=2431, endPage=2444, ext={EN=ArticleExt(id=1320107544694080122, articleId=1320107544404673145, tenantId=1146029695717560320, journalId=1263187385517883426, language=EN, title=Stable Single-Crystal LiNi0.9Mn0.1O2 Cathode Material: Enhanced Phase Transition Reversibility via Mg/Nb/Ti Multi-Regulation Strategy, columnId=1263922769897599102, journalTitle=Journal of the Chinese Ceramic Society, columnName=Research Articles, runingTitle=null, highlight=null, articleAbstract=
Introduction

Commercial ternary cathode materials have their theoretical performance limits. Consequently, enhancing energy density, reducing costs, and improving cycling stability without compromising safety are critical challenges for both academia and industry. Among the existing candidates, LiNi0.9Mn0.1O2(NM91) offers a significant potential due to its high specific capacity, cost-effectiveness, and low-cobalt (or cobalt-free) nature. However, ahigh nickel content induces severe structural instability. Elevated Ni levels exacerbate Li+/Ni2+ cation disordering, thus disrupting the α-NaFeO2-type layered structure and impeding lithium-ion de/intercalation kinetics, which degrades a rate capability. Furthermore, during high-voltage cycling (>4.3 V), detrimental interfacial reactions occur, i.e., electrolyte decomposition, transition metal dissolution, and the formation of Ni-rich rock-salt or amorphous phases. These degradation mechanisms destabilize the electrode-electrolyte interface, accelerate capacity fade, exacerbate electrode polarization, and severely compromise cycling longevity and battery safety. To address these challenges, this study was to propose an innovative Mg/Nb/Ti co-modification strategy to enhance the structural stability and electrochemical performance of single-crystal LiNi0.9Mn0.1O2 cathodes.

Methods

The Ni0.9Mn0.1(OH)2 precursor was first homogeneously blended with LiOH·H2O and flux under strictly controlled stoichiometric conditions (i.e., at a Li : (Ni+Mn) molar ratio of 1.05∶1.00 and a (LiCl+KCl) ∶ (Ni+Mn) mass ratio of 0.3 ∶ 1.0). The mixture was then calcined in a flowing oxygen atmosphere, heated to 550 ℃ at 3 ℃/min (300 min hold), ramped to 900 ℃ at the same rate for 60 min, cooled controllably at 5 ℃/min to 820 ℃ for 840 min, and finally cooled to ambient temperature, yielding a phase-pure single-crystal LiNi0.9Mn0.1O2 (designated SC-NM91).

For the doped samples, Ni0.9Mn0.1(OH)2 precursor was homogenized with LiOH·H2O, Mg(NO3)2, and C10H5NbO20·xH2O in anhydrous ethanol under vigorous agitation. C16H36O4Ti was added in dropwise, followed by continuous stirring and drying at 60 ℃ until complete solvent evaporation. The resultant mixture had a controlled stoichiometry of Li ∶ (Ni+Mn) ∶ Mg ∶ Nb ∶ Ti = 1.05 : (1-x-y-z) ∶ x ∶ y ∶ z (x=0.005, 0.010, 0.020; y=0.002 5, 0.005 0, 0.010 0; z=0.01).

The identical solid-state sintering protocol used for SC-NM91 was applied to synthesize Mg/Nb/Ti tri-doped LiNi0.9-x-y-zMn0.1MgxNbyTizO2 cathodes with controlled dopant gradients. The compositions of SC-NM91-0.5Mg@0.25Nb@1Ti, SC-NM91-1Mg@0.5Nb@1Ti, and SC-NM91-2Mg@1Nb@1Ti were produced via unified thermal processing.

Results and Discussion

Among the modified cathodes, SC-NM91-0.5Mg@0.25Nb@1Ti demonstrates significantly enhanced cycling stability and superior overall electrochemical performance, compared to SC-NM91-1Mg@0.5Nb@1Ti and SC-NM91-2Mg@1Nb@1Ti.

The XRD patterns reveal a systematic peak shift toward lower angles in the modified samples relative to SC-NM91, indicating a lattice expansion along the c-axis induced by elemental doping. SC-NM91-0.5Mg@0.25Nb@1Ti exhibits enhanced cationic ordering with an R-factor of 1.749 0 versus 1.641 8 for pristine SC-NM91, demonstrating that optimized Mg/Nb/Ti co-doping effectively mitigates cationic disordering and stabilizes the layered structure. The SEM images indicate that SC-NM91 comprises irregular particles (the diameter of ~1 µm) with a non-uniform distribution and a broad size range, including oversized particulates. Increasing Mg/Nb/Ti doping concentration yields a significant morphological evolution. The particle distribution becomes more homogeneous, particle size gradually decreases, and the EDS mapping confirms spatially uniform elemental dispersion, verifying an effective dopant incorporation. The XPS analysis reveals that Mg/Nb/Ti doping effectively modulates the material surface electronic structure and valence state distribution, enhances structural stability, increases the Ni3+ proportion, consequently improving the electrochemical performance.

SC-NM91-0.5Mg@0.25Nb@1Ti has a superior rate capability across multiple current densities, significantly outperforming other specimens. This indicates that optimal doping enhances a structural stability, while maintaining high lithium-ion transport kinetics. When cycled at 1 C under different cut-off voltages (i.e., 4.3 V and 4.4 V), SC-NM91-0.5Mg@0.25Nb@1Ti electrode exhibits the maximum capacity retention rate, showing a remarkable improvement over counterparts. These results verify that multi-element doping combined with surface modification effectively enhances electrochemical properties. Furthermore, its differential capacity curves exhibit more symmetric phase transition peaks, significantly reduced voltage hysteresis, and compact/stable peak profiles, indicating enhanced phase transition reversibility and substantially improved structural stability. The electrochemical impedance spectroscopy (EIS) primarily reveal two key parameters, i.e., series resistance (Rs) and charge transfer resistance (Rct), reflecting intrinsic material resistance and the electron transfer barrier at the electrode-electrolyte interface, respectively. After 100 cycles, SC-NM91-0.5Mg@0.25Nb@1Ti exhibits significantly lower resistance values rather than pristine SC-NM91. This demonstrates that Mg/Nb/Ti co-modification effectively mitigates electrolyte corrosion, stabilizes the interfacial structure, and facilitates the formation of arobust cathode electrolyte interphase film. Consequently, the modified electrode maintains efficient charge transfer kinetics during prolonged cycling, while retarding Rct degradation. Finally, the cyclic voltammetry (CV) analysis reveals that the modified sample has a distinct hysteretic shift in the oxidation peak and reduces peak intensities, compared to the unmodified sample. Nevertheless, the high degree of peak overlap across cycles indicates that the synergistic doping-coating modification significantly suppresses electrochemical polarization and enhances interfacial reaction kinetics, thereby contributing to superior electrochemical performance.

Conclusions

This study systematically explored a synergistic co-modification strategy combining Mg/Nb bulk doping and Ti surface coating for SC-NM91 high-nickel cathodes. The optimally designed SC-NM91-0.5Mg@0.25Nb@1Ti sample that was fabricated via high-temperature solid-state synthesis could exhibit the superior structural stability and electrochemical performance. It demonstrated a capacity retention of 89.2% at 4.3 V after 100 cycles, significantly exceeding the unmodified counterpart (i.e., 73.3%), while maintaining a retention of 66.5% at 4.4 V, indicating the exceptional high-voltage stability. The mechanistic investigations revealed that Mg doping primarily suppressed Li/Ni cation mixing and inhibited the H1→M phase transition at low voltages, while Nb doping stabilized oxygen frameworks, mitigated oxygen release under high-voltage conditions, and enhanced H2→H3 phase transition reversibility. Ti4+doping reinforced transition metal layer stability and suppressed Ni4+-induced lattice oxygen release at high voltages, extending cycle life. The concomitant formation of TiO2/LiTi2O4 coating layers during thermal processing effectively blocked parasitic reactions and boosted electronic conductivity, collectively improving interfacial integrity and rate capability. The electrochemical characterization confirmed reduced Rct post-cycling and diminished redox peak potential separation in CV, evidencing enhanced reaction kinetics and suppressed polarization. This co-modification approach could elevate the comprehensive performance of SC-NM91 cathodes, establishing an effective paradigm for developing high-energy-density lithium-ion battery cathodes with a robust stability.

, authors=Ruijian HUANG, Jianyao MA, Xin HUANG, Bin HUANG, Yanwei LI, Shunhua XIAO, authorsList=Ruijian HUANG, Jianyao MA, Xin HUANG, Bin HUANG, Yanwei LI, Shunhua XIAO, authorCompany=null, correspAuthors=Shunhua XIAO, authorNote=

HUANG Ruijian (2001-), male, Master candidate. E-mail:

, correspAuthorsNote=
{XIAO} Shunhua (1969-), male, Professor. E-mail:
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高镍正极材料因其高能量密度而备受关注，但存在高电压下结构不稳定、容量衰减快等问题。为提升其综合性能，本工作以LiNi0.9Mn0.1O2为基础，提出Mg/Nb/Ti协同掺杂与表面包覆的多重调控策略，并采用高温固相法合成系列样品。结果表明，样品SC-NM91-0.5Mg/0.25Nb@1Ti在4.3 V下循环100圈后容量保持率达89.2%，较未改性样品（73.3%）提升15.9%，在4.4 V下仍保持66.5%的容量，展现优异的高压稳定性。Mg掺杂可抑制Li+/Ni+混排，提升低压区结构稳定性；Nb掺杂能提升电导率，促进Li+扩散动力学；Ti则稳定结构并抑制晶格氧释放，形成的TiO2/LiTi2O4包覆层可改善界面与电子传导性能。电化学测试显示改性样品具有更低的电荷转移阻抗和极化，反应动力学更优。综上，所提出的协同掺杂-包覆策略可显著提升样品如SC-NM91-0.5Mg/0.25Nb@1Ti等SC-NM91材料的结构稳定性与电化学性能，为高性能锂离子电池正极材料设计提供有效路径。

, authors=黄睿健, 马健尧, 黄信, 黄斌, 李延伟, 肖顺华, authorsList=黄睿健, 马健尧, 黄信, 黄斌, 李延伟, 肖顺华, authorCompany=null, correspAuthors=肖顺华, authorNote=

黄睿健（2001—），男，硕士研究生。

, correspAuthorsNote=
肖顺华（1969—），男，教授。
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HUANG Ruijian (2001-), male, Master candidate. E-mail:

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优越稳定性单晶LiNi0.9Mn0.1O2正极材料：Mg/Nb/Ti多重调控增强相变可逆性
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黄睿健 , 马健尧 , 黄信 , 黄斌 , 李延伟 , 肖顺华
硅酸盐学报 | 研究论文 2026,54(7): 2431-2444
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硅酸盐学报 |研究论文 2026 , 54 (7) : 2431 -2444
优越稳定性单晶LiNi0.9Mn0.1O2正极材料：Mg/Nb/Ti多重调控增强相变可逆性
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黄睿健 , 马健尧, 黄信, 黄斌, 李延伟, 肖顺华
作者信息
  • 桂林理工大学化学与生物工程学院，广西高校表面与界面电化学重点实验室，广西电磁化学功能物质重点实验室，桂林 541006
通讯作者:
肖顺华（1969—），男，教授。
作者简介:

黄睿健（2001—），男，硕士研究生。

Stable Single-Crystal LiNi0.9Mn0.1O2 Cathode Material: Enhanced Phase Transition Reversibility via Mg/Nb/Ti Multi-Regulation Strategy
Ruijian HUANG , Jianyao MA, Xin HUANG, Bin HUANG, Yanwei LI, Shunhua XIAO
Affiliations
  • Guangxi Colleges and Universities Key Laboratory of Surface and Interface Electrochemistry, Guangxi Key Laboratory of Electrochemical and Magnetochemical Functional Materials, College of Chemistry and Bioengineering, Guilin University of Technology, Guilin 541004, Guangxi, China
    • Corresponding Author:
    {XIAO} Shunhua (1969-), male, Professor. E-mail:

    HUANG Ruijian (2001-), male, Master candidate. E-mail:

出版时间: 2026-04-09 doi: 10.14062/j.issn.0454-5648.20250532
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高镍正极材料因其高能量密度而备受关注，但存在高电压下结构不稳定、容量衰减快等问题。为提升其综合性能，本工作以LiNi0.9Mn0.1O2为基础，提出Mg/Nb/Ti协同掺杂与表面包覆的多重调控策略，并采用高温固相法合成系列样品。结果表明，样品SC-NM91-0.5Mg/0.25Nb@1Ti在4.3 V下循环100圈后容量保持率达89.2%，较未改性样品（73.3%）提升15.9%，在4.4 V下仍保持66.5%的容量，展现优异的高压稳定性。Mg掺杂可抑制Li+/Ni+混排，提升低压区结构稳定性；Nb掺杂能提升电导率，促进Li+扩散动力学；Ti则稳定结构并抑制晶格氧释放，形成的TiO2/LiTi2O4包覆层可改善界面与电子传导性能。电化学测试显示改性样品具有更低的电荷转移阻抗和极化，反应动力学更优。综上，所提出的协同掺杂-包覆策略可显著提升样品如SC-NM91-0.5Mg/0.25Nb@1Ti等SC-NM91材料的结构稳定性与电化学性能，为高性能锂离子电池正极材料设计提供有效路径。

高镍层状氧化物  /  表面包覆  /  镁/铌/钛掺杂  /  高截止电压  /  单晶
Introduction

Commercial ternary cathode materials have their theoretical performance limits. Consequently, enhancing energy density, reducing costs, and improving cycling stability without compromising safety are critical challenges for both academia and industry. Among the existing candidates, LiNi0.9Mn0.1O2(NM91) offers a significant potential due to its high specific capacity, cost-effectiveness, and low-cobalt (or cobalt-free) nature. However, ahigh nickel content induces severe structural instability. Elevated Ni levels exacerbate Li+/Ni2+ cation disordering, thus disrupting the α-NaFeO2-type layered structure and impeding lithium-ion de/intercalation kinetics, which degrades a rate capability. Furthermore, during high-voltage cycling (>4.3 V), detrimental interfacial reactions occur, i.e., electrolyte decomposition, transition metal dissolution, and the formation of Ni-rich rock-salt or amorphous phases. These degradation mechanisms destabilize the electrode-electrolyte interface, accelerate capacity fade, exacerbate electrode polarization, and severely compromise cycling longevity and battery safety. To address these challenges, this study was to propose an innovative Mg/Nb/Ti co-modification strategy to enhance the structural stability and electrochemical performance of single-crystal LiNi0.9Mn0.1O2 cathodes.

Methods

The Ni0.9Mn0.1(OH)2 precursor was first homogeneously blended with LiOH·H2O and flux under strictly controlled stoichiometric conditions (i.e., at a Li : (Ni+Mn) molar ratio of 1.05∶1.00 and a (LiCl+KCl) ∶ (Ni+Mn) mass ratio of 0.3 ∶ 1.0). The mixture was then calcined in a flowing oxygen atmosphere, heated to 550 ℃ at 3 ℃/min (300 min hold), ramped to 900 ℃ at the same rate for 60 min, cooled controllably at 5 ℃/min to 820 ℃ for 840 min, and finally cooled to ambient temperature, yielding a phase-pure single-crystal LiNi0.9Mn0.1O2 (designated SC-NM91).

For the doped samples, Ni0.9Mn0.1(OH)2 precursor was homogenized with LiOH·H2O, Mg(NO3)2, and C10H5NbO20·xH2O in anhydrous ethanol under vigorous agitation. C16H36O4Ti was added in dropwise, followed by continuous stirring and drying at 60 ℃ until complete solvent evaporation. The resultant mixture had a controlled stoichiometry of Li ∶ (Ni+Mn) ∶ Mg ∶ Nb ∶ Ti = 1.05 : (1-x-y-z) ∶ x ∶ y ∶ z (x=0.005, 0.010, 0.020; y=0.002 5, 0.005 0, 0.010 0; z=0.01).

The identical solid-state sintering protocol used for SC-NM91 was applied to synthesize Mg/Nb/Ti tri-doped LiNi0.9-x-y-zMn0.1MgxNbyTizO2 cathodes with controlled dopant gradients. The compositions of SC-NM91-0.5Mg@0.25Nb@1Ti, SC-NM91-1Mg@0.5Nb@1Ti, and SC-NM91-2Mg@1Nb@1Ti were produced via unified thermal processing.

Results and Discussion

Among the modified cathodes, SC-NM91-0.5Mg@0.25Nb@1Ti demonstrates significantly enhanced cycling stability and superior overall electrochemical performance, compared to SC-NM91-1Mg@0.5Nb@1Ti and SC-NM91-2Mg@1Nb@1Ti.

The XRD patterns reveal a systematic peak shift toward lower angles in the modified samples relative to SC-NM91, indicating a lattice expansion along the c-axis induced by elemental doping. SC-NM91-0.5Mg@0.25Nb@1Ti exhibits enhanced cationic ordering with an R-factor of 1.749 0 versus 1.641 8 for pristine SC-NM91, demonstrating that optimized Mg/Nb/Ti co-doping effectively mitigates cationic disordering and stabilizes the layered structure. The SEM images indicate that SC-NM91 comprises irregular particles (the diameter of ~1 µm) with a non-uniform distribution and a broad size range, including oversized particulates. Increasing Mg/Nb/Ti doping concentration yields a significant morphological evolution. The particle distribution becomes more homogeneous, particle size gradually decreases, and the EDS mapping confirms spatially uniform elemental dispersion, verifying an effective dopant incorporation. The XPS analysis reveals that Mg/Nb/Ti doping effectively modulates the material surface electronic structure and valence state distribution, enhances structural stability, increases the Ni3+ proportion, consequently improving the electrochemical performance.

SC-NM91-0.5Mg@0.25Nb@1Ti has a superior rate capability across multiple current densities, significantly outperforming other specimens. This indicates that optimal doping enhances a structural stability, while maintaining high lithium-ion transport kinetics. When cycled at 1 C under different cut-off voltages (i.e., 4.3 V and 4.4 V), SC-NM91-0.5Mg@0.25Nb@1Ti electrode exhibits the maximum capacity retention rate, showing a remarkable improvement over counterparts. These results verify that multi-element doping combined with surface modification effectively enhances electrochemical properties. Furthermore, its differential capacity curves exhibit more symmetric phase transition peaks, significantly reduced voltage hysteresis, and compact/stable peak profiles, indicating enhanced phase transition reversibility and substantially improved structural stability. The electrochemical impedance spectroscopy (EIS) primarily reveal two key parameters, i.e., series resistance (Rs) and charge transfer resistance (Rct), reflecting intrinsic material resistance and the electron transfer barrier at the electrode-electrolyte interface, respectively. After 100 cycles, SC-NM91-0.5Mg@0.25Nb@1Ti exhibits significantly lower resistance values rather than pristine SC-NM91. This demonstrates that Mg/Nb/Ti co-modification effectively mitigates electrolyte corrosion, stabilizes the interfacial structure, and facilitates the formation of arobust cathode electrolyte interphase film. Consequently, the modified electrode maintains efficient charge transfer kinetics during prolonged cycling, while retarding Rct degradation. Finally, the cyclic voltammetry (CV) analysis reveals that the modified sample has a distinct hysteretic shift in the oxidation peak and reduces peak intensities, compared to the unmodified sample. Nevertheless, the high degree of peak overlap across cycles indicates that the synergistic doping-coating modification significantly suppresses electrochemical polarization and enhances interfacial reaction kinetics, thereby contributing to superior electrochemical performance.

Conclusions

This study systematically explored a synergistic co-modification strategy combining Mg/Nb bulk doping and Ti surface coating for SC-NM91 high-nickel cathodes. The optimally designed SC-NM91-0.5Mg@0.25Nb@1Ti sample that was fabricated via high-temperature solid-state synthesis could exhibit the superior structural stability and electrochemical performance. It demonstrated a capacity retention of 89.2% at 4.3 V after 100 cycles, significantly exceeding the unmodified counterpart (i.e., 73.3%), while maintaining a retention of 66.5% at 4.4 V, indicating the exceptional high-voltage stability. The mechanistic investigations revealed that Mg doping primarily suppressed Li/Ni cation mixing and inhibited the H1→M phase transition at low voltages, while Nb doping stabilized oxygen frameworks, mitigated oxygen release under high-voltage conditions, and enhanced H2→H3 phase transition reversibility. Ti4+doping reinforced transition metal layer stability and suppressed Ni4+-induced lattice oxygen release at high voltages, extending cycle life. The concomitant formation of TiO2/LiTi2O4 coating layers during thermal processing effectively blocked parasitic reactions and boosted electronic conductivity, collectively improving interfacial integrity and rate capability. The electrochemical characterization confirmed reduced Rct post-cycling and diminished redox peak potential separation in CV, evidencing enhanced reaction kinetics and suppressed polarization. This co-modification approach could elevate the comprehensive performance of SC-NM91 cathodes, establishing an effective paradigm for developing high-energy-density lithium-ion battery cathodes with a robust stability.

high-nickel layered oxides  /  surface coating  /  magnesium/niobium/titanium doping  /  high cutoff voltage  /  single crystal
黄睿健, 马健尧, 黄信, 黄斌, 李延伟, 肖顺华. 优越稳定性单晶LiNi0.9Mn0.1O2正极材料：Mg/Nb/Ti多重调控增强相变可逆性. 硅酸盐学报, 2026 , 54 (7) : 2431 -2444 . DOI: 10.14062/j.issn.0454-5648.20250532
Ruijian HUANG, Jianyao MA, Xin HUANG, Bin HUANG, Yanwei LI, Shunhua XIAO. Stable Single-Crystal LiNi0.9Mn0.1O2 Cathode Material: Enhanced Phase Transition Reversibility via Mg/Nb/Ti Multi-Regulation Strategy[J]. Journal of the Chinese Ceramic Society, 2026 , 54 (7) : 2431 -2444 . DOI: 10.14062/j.issn.0454-5648.20250532
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doi: 10.14062/j.issn.0454-5648.20250532
  • 接收时间：2025-07-08
  • 首发时间：2026-10-22
  • 出版时间：2026-04-09
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  • 收稿日期：2025-07-08
  • 修回日期：2025-08-03
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国家自然科学基金(22362011; 22169007)
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    桂林理工大学化学与生物工程学院，广西高校表面与界面电化学重点实验室，广西电磁化学功能物质重点实验室，桂林 541006

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肖顺华（1969—），男，教授。
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