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Article(id=1240631880043787228, tenantId=1146029695717560320, journalId=1235980550691926019, issueId=1240631872800215183, articleNumber=null, orderNo=null, doi=10.3969/j.issn.0253-6099.2025.01.025, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1725465600000, receivedDateStr=2024-09-05, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1773719290028, onlineDateStr=2026-03-17, pubDate=1738339200000, pubDateStr=2025-02-01, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1773719290028, onlineIssueDateStr=2026-03-17, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1773719290028, creator=13701087609, updateTime=1773719290028, updator=13701087609, issue=Issue{id=1240631872800215183, tenantId=1146029695717560320, journalId=1235980550691926019, year='2025', volume='45', issue='1', pageStart='1', pageEnd='187', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1773719288300, creator=13701087609, updateTime=1773724138257, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1240652215052989235, tenantId=1146029695717560320, journalId=1235980550691926019, issueId=1240631872800215183, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1240652215052989236, tenantId=1146029695717560320, journalId=1235980550691926019, issueId=1240631872800215183, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=133, endPage=137, ext={EN=ArticleExt(id=1240631882380013617, articleId=1240631880043787228, tenantId=1146029695717560320, journalId=1235980550691926019, language=EN, title=Influence of Precursor Synthesis Process on Nickel-Rich NCM Cathodes, columnId=1236276108207902848, journalTitle=Mining and Metallurgical Engineering, columnName=MATERIALS, runingTitle=null, highlight=null, articleAbstract=

The effects of continuous and semi-continuous synthesis processes of precursor on the structure and performance of precursor materials and nickel-rich NCM cathode materials were explored. The results show that primary particles of the precursors synthesized by these two processes are quite different in morphology, leading to the difference in structure of primary/secondary particles and electrochemical property of the correspondingly synthesized cathode materials. These two cathode materials present little different performance in a button half cell, but significant difference in a soft pack battery. The nickel-rich cathode synthesized by the semi-continuous process has a lower impedance at a low state of charge, and retains 87.61% of its capacity after 750 cycles at 45 ℃, much higher than the retention rate (77.65%) of the nickel-rich cathode synthesized by the continuous process. It is concluded that the semi-continuous synthesis process for precursor is superior in the production of nickel-rich cathode materials.

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研究了连续法和半连续法前驱体合成工艺对前驱体材料和高镍三元正极材料结构与性能的影响。结果表明，2种工艺合成的前驱体一次颗粒形貌存在显著差异，导致合成的正极材料一/二次颗粒结构及其电化学性能有所不同。2种前驱体制备的正极材料在扣式半电池中的性能差异较小，但在软包电池中却呈现出显著差异：采用半连续法制备的高镍正极在低荷电状态下具有较低的阻抗，45 ℃下循环750次后容量保持率为87.61%，显著优于连续法制备的高镍正极的容量保持率（77.65%）。半连续前驱体合成工艺在高镍正极材料生产中具备更大优势。

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杨立山（1983—），男，湖南岳阳人，博士，副教授，硕士研究生导师，主要研究方向为新能源材料与器件。E-mail：
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白立雄（1987—），男，新疆伊宁人，博士，高级工程师，主要研究方向为三元正极材料制备与性能优化。E-mail：

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白立雄（1987—），男，新疆伊宁人，博士，高级工程师，主要研究方向为三元正极材料制备与性能优化。E-mail：

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白立雄（1987—），男，新疆伊宁人，博士，高级工程师，主要研究方向为三元正极材料制备与性能优化。E-mail：

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（a）半连续法，前驱体SEM；（b）半连续法，切面SEM；（b）连续法，前驱体SEM；（d）连续法，切面SEM

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（a）半连续法，正极材料SEM；（b）半连续法，切面SEM（b）连续法，正极材料SEM；（d）连续法，切面SEM

, figureFileSmall=jd35vpsHrlhgjaC/Zz2n5A==, figureFileBig=yZAFu/YlcWkpBuPMdQO5lQ==, tableContent=null), ArticleFig(id=1240651354193056293, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1240631880043787228, language=EN, label=Fig.7, caption=The first Coulomb efficiency of button batteries with two cathode materials at different C-rate, figureFileSmall=xdA0lOOSb0BwLMoHTJjoUQ==, figureFileBig=ZvCpUaSGuNTrVgJjLNt2hA==, tableContent=null), ArticleFig(id=1240651354310496810, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1240631880043787228, language=CN, label=图7, caption=2种正极材料纽扣电池不同倍率下的首次库仑效率, figureFileSmall=xdA0lOOSb0BwLMoHTJjoUQ==, figureFileBig=ZvCpUaSGuNTrVgJjLNt2hA==, tableContent=null), ArticleFig(id=1240651354444714549, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1240631880043787228, language=EN, label=Fig.8, caption=Impedance of soft pack battery under different charging conditions, figureFileSmall=eWRAFntkUxHarjwt2Ajbkg==, figureFileBig=0m/uNr3U2JvzdAYtwjSmVA==, tableContent=null), ArticleFig(id=1240651354566349374, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1240631880043787228, language=CN, label=图8, caption=不同荷电状态下软包电池的阻抗, figureFileSmall=eWRAFntkUxHarjwt2Ajbkg==, figureFileBig=0m/uNr3U2JvzdAYtwjSmVA==, tableContent=null), ArticleFig(id=1240651354662818377, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1240631880043787228, language=EN, label=Fig.9, caption=Cycle curves of soft pack batteries at normal temperature and high temperature, figureFileSmall=djvKrL3dDKnbb/JRZdCNuA==, figureFileBig=tDhHhWjjcp4Z093dWBm9mQ==, tableContent=null), ArticleFig(id=1240651354759287374, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1240631880043787228, language=CN, label=图9, caption=2种软包电池的常温和高温循环曲线

（a）25 ℃；（b）45 ℃

, figureFileSmall=djvKrL3dDKnbb/JRZdCNuA==, figureFileBig=tDhHhWjjcp4Z093dWBm9mQ==, tableContent=null), ArticleFig(id=1240651354851562071, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1240631880043787228, language=EN, label=Fig.10, caption=SEM images of sections of materials after 50 cycles at 45 ℃, figureFileSmall=Lmo9Cb1LgtIwMUsuvILarw==, figureFileBig=6Hblq9pXPSsAtnfxZyHqOQ==, tableContent=null), ArticleFig(id=1240651354977391209, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1240631880043787228, language=CN, label=图10, caption=2种材料45 ℃循环50次后的切面SEM图

（a）半连续法；（b）连续法

, figureFileSmall=Lmo9Cb1LgtIwMUsuvILarw==, figureFileBig=6Hblq9pXPSsAtnfxZyHqOQ==, tableContent=null), ArticleFig(id=1240651355073860208, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1240631880043787228, language=EN, label=Table 1, caption=

Physical properties of product prepared by different synthesis processes

, figureFileSmall=null, figureFileBig=null, tableContent=
合成工艺Ni物质的量比/%振实密度/（g·cm-3）比表面积/（m2·g-1）粒度d50/μm
半连续法≥802.18.710.3
连续法≥802.26.010.7
), ArticleFig(id=1240651355237438075, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1240631880043787228, language=CN, label=表1, caption=

2种前驱体合成工艺所得产品基础物性结果

, figureFileSmall=null, figureFileBig=null, tableContent=
合成工艺Ni物质的量比/%振实密度/（g·cm-3）比表面积/（m2·g-1）粒度d50/μm
半连续法≥802.18.710.3
连续法≥802.26.010.7
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前驱体合成工艺对高镍三元正极材料性能的影响
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白立雄 1 , 贡浩天 2 , 甘柏瑶 2 , 周春仙 1 , 朱健 1 , 周友元 1 , 杨亚辉 2 , 杨立山 2
矿冶工程杂志 | 材料 2025,45(1): 133-137
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矿冶工程杂志 | 材料 2025, 45(1): 133-137
前驱体合成工艺对高镍三元正极材料性能的影响
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白立雄1 , 贡浩天2, 甘柏瑶2, 周春仙1, 朱健1, 周友元1, 杨亚辉2, 杨立山2
作者信息
  • 1.五矿新能源材料（湖南）股份有限公司，湖南　长沙　410205
  • 2.湖南师范大学　化学化工学院，湖南　长沙　410081

    • 白立雄（1987—），男，新疆伊宁人，博士，高级工程师，主要研究方向为三元正极材料制备与性能优化。E-mail：

通讯作者:

杨立山（1983—），男，湖南岳阳人，博士，副教授，硕士研究生导师，主要研究方向为新能源材料与器件。E-mail：
Influence of Precursor Synthesis Process on Nickel-Rich NCM Cathodes
Lixiong BAI1 , Haotian GONG2, Boyao GAN2, Chunxian ZHOU1, Jian ZHU1, Youyuan ZHOU1, Yahui YANG2, Lishan YANG2
Affiliations
  • 1.Minmetals New Energy Materials (Hunan) Co., Ltd., Changsha 410205, Hunan, China
  • 2.School of Chemistry and Chemical Engineering, Hunan Normal University, Changsha 410081, Hunan, China
出版时间: 2025-02-01 doi: 10.3969/j.issn.0253-6099.2025.01.025
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摘要
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研究了连续法和半连续法前驱体合成工艺对前驱体材料和高镍三元正极材料结构与性能的影响。结果表明，2种工艺合成的前驱体一次颗粒形貌存在显著差异，导致合成的正极材料一/二次颗粒结构及其电化学性能有所不同。2种前驱体制备的正极材料在扣式半电池中的性能差异较小，但在软包电池中却呈现出显著差异：采用半连续法制备的高镍正极在低荷电状态下具有较低的阻抗，45 ℃下循环750次后容量保持率为87.61%，显著优于连续法制备的高镍正极的容量保持率（77.65%）。半连续前驱体合成工艺在高镍正极材料生产中具备更大优势。

锂离子电池  /  前驱体  /  正极材料  /  循环稳定性  /  高镍三元正极  /  连续法  /  半连续法

The effects of continuous and semi-continuous synthesis processes of precursor on the structure and performance of precursor materials and nickel-rich NCM cathode materials were explored. The results show that primary particles of the precursors synthesized by these two processes are quite different in morphology, leading to the difference in structure of primary/secondary particles and electrochemical property of the correspondingly synthesized cathode materials. These two cathode materials present little different performance in a button half cell, but significant difference in a soft pack battery. The nickel-rich cathode synthesized by the semi-continuous process has a lower impedance at a low state of charge, and retains 87.61% of its capacity after 750 cycles at 45 ℃, much higher than the retention rate (77.65%) of the nickel-rich cathode synthesized by the continuous process. It is concluded that the semi-continuous synthesis process for precursor is superior in the production of nickel-rich cathode materials.

lithium-ion battery  /  precursor  /  cathode material  /  cycle stability  /  nickel-rich NCM cathode  /  continuous processing  /  semi-continuous processing
白立雄, 贡浩天, 甘柏瑶, 周春仙, 朱健, 周友元, 杨亚辉, 杨立山. 前驱体合成工艺对高镍三元正极材料性能的影响. 矿冶工程杂志, 2025 , 45 (1) : 133 -137 . DOI: 10.3969/j.issn.0253-6099.2025.01.025
Lixiong BAI, Haotian GONG, Boyao GAN, Chunxian ZHOU, Jian ZHU, Youyuan ZHOU, Yahui YANG, Lishan YANG. Influence of Precursor Synthesis Process on Nickel-Rich NCM Cathodes[J]. Mining and Metallurgical Engineering, 2025 , 45 (1) : 133 -137 . DOI: 10.3969/j.issn.0253-6099.2025.01.025
正文
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电网储能和电动车续航[1-2]对电池能量密度[3]有着很高要求，合理调控前驱体结构可以充分发挥材料容量[4-5]。三元材料前驱体[6-7]形貌和粒径对正极材料性能影响较大，合理设计正极材料二次颗粒的结构[8]能够有效提升材料结构稳定性并充分释放材料潜力[9]。通过调控前驱体球形度和表面结构[10]，可以改善材料循环性能、热稳定性能[11]等。大量研究表明，前驱体结构在一定程度上决定了高镍正极材料[12]的性能。
受设备限制，实验室往往采用间歇法[8,13-14]生产前驱体，即在同一反应釜中形成晶核→控制粒径长大→陈化→出料。但间歇法生产周期长，对设备产能影响较大，实际生产往往采取连续法或连续-间歇法（即半连续法）进行大规模生产[15]。本文对比分析了连续法和半连续法2种合成工艺生产的前驱体的优缺点以及对应正极材料的电化学性能，可为工业大规模生产提供技术参考。
1　实验
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1.1　实验原料及方法
实验所用前驱体为金驰能源材料有限公司提供的半连续法前驱体（M308m1）和连续法前驱体（M308m2），化学式均为Ni0.8Co0.1Mn0.1（OH）2。通过Ni、Co、Mn等金属硫酸盐溶液与氨水、氢氧化钠等络合剂、沉淀剂进行沉淀反应，再经脱水、干燥等过程，得到前驱体。
使用2种不同合成方法所得前驱体与电池级LiOH[雅化锂业（雅安）有限公司]按照化学式LiNi0.8Co0.1-Mn0.1O2中的物质的量比称取原料，且LiOH过量3%，在行星球磨机中乙醇湿法球磨6 h，转速300 r/min，然后鼓风60 ℃烘干，转移到氧化铝瓷舟，在氧气气流下830 ℃煅烧12 h，冷却后通过研磨粉碎，过400目（38 μm）筛网收集备用。
1.2　材料表征
使用SU8010发射扫描电镜（SEM）分析材料微观形貌；使用SmartLab X射线衍射仪（XRD）观察材料结构、晶型；使用PerkinElmer 8300电感耦合等离子体发射光谱分析仪（ICP）测试元素含量；使用Malvern Mastersizer 2000激光粒度仪测量材料粒径。
1.3　电化学表征
纽扣电池制备：按照正极材料∶炭黑∶PVDF质量比90∶5∶5进行混料，制备半电池正极浆料，涂布厚度为200 μm。极片在105 ℃真空干燥箱中干燥12 h，并在手套箱中组装成2032纽扣电池，进行电化学性能测试（标称容量1C=185 mAh/g）。
软包电池制备：按照正极材料∶炭黑∶碳纳米管∶PVDF质量比93∶2∶2∶3进行正极材料涂布，涂布厚度500 μm；负极使用人造石墨。正负极质量比控制在1.05[16]左右，极片烘干温度110 ℃，裁片，制备容量0.8 Ah软包电池。
纽扣电池及软包电池使用常规电解液（1 mol/L 99.9%LiPF6，溶于碳酸亚乙酯∶碳酸二甲酯体积比1∶1的溶液）。
2　结果与讨论
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2.1　前驱体差异分析
2种前驱体合成工艺示意图如图1所示。连续法指原料进入反应釜后直接进行沉淀，操作简单，生产效率高，但得到的产品粒度分布窄。半连续法原料进料后先在第1个反应釜中合成粒度分布较窄、粒径较小的一次颗粒浆料[17]，再流入第2个反应釜让浆料继续结晶长大并聚集成二次颗粒[18]，直至二次颗粒粒度分布达到要求，即通过控制成核反应和生长实现粒度分布优化。
表1为2种前驱体合成工艺所得产品的基础物性结果。无论半连续法还是连续法前驱体，其Ni物质的量比、振实密度、比表面积、粒度等数据均处于合理范围内。其中连续法前驱体在单反应釜中反应，产生的一次颗粒粒度较小且连接紧密，导致二次颗粒振实密度大、比表面低。前驱体表面致密不利于后续混锂火法制备正极材料时锂的扩散[18]。
高镍三元正极材料晶体结构与前驱体结构具有一定继承性[19]，前驱体会影响锂离子有效脱嵌通道数量，从而影响合成正极材料的倍率、阻抗等电化学性能。连续法和半连续法前驱体的XRD图谱见图2。与Ni（OH）2标准卡片（PDF#74-2075）对比，2种前驱体XRD图谱无杂峰，说明结晶较好、样品较纯。整体而言，半连续法前驱体峰值更强，特别是（001）晶面更尖锐，代表半连续法制备的前驱体结晶性更好。
采用Scherrer公式D=Kλ/（βcosθ）对图2所示的2种前驱体的3个晶面的半峰宽数据进行计算，结果如图3所示。
2种前驱体样品的二次颗粒及切面SEM图见图4。2种前驱体合成工艺所用设备及合成过程连续性有一定差异，所得前驱体呈现不同形貌。半连续法制备的前驱体一次颗粒较长且粗，整体结合呈现团簇状，二次颗粒表面空隙较大；二次颗粒截面形貌呈放射状，且截面具有一定孔隙分布，这些孔隙有利于高温状态下氢氧化锂由外向内扩散，合成的正极材料结构更加完整。连续法制备的前驱体一次颗粒均匀，内部截面同样呈现放射状，一次颗粒之间结合较致密，未见明显孔隙分布。前驱体一次颗粒大小、分布、外延方向在一定程度上会影响合成的高镍正极材料的性能。正极材料充放电过程中，随着锂离子的嵌入与脱出，材料晶胞结构会发生一定变化，导致正极颗粒发生不可逆的相变，进而导致材料内部发生龟裂，产生新的界面，使得电化学性能下降。因此，具有优良结构的前驱体对合成高性能镍正极材料至关重要。
2.2　正极材料成品理化差异分析
前驱体经过火法烧结、水洗烘干后制备成正极材料备用。图5为连续法和半连续法前驱体制备正极材料的XRD图谱。I（003）/I（104）均大于1.4，证明锂镍混排较小，半连续法前驱体对应的正极材料（003）峰峰强更高，证明其结晶性较好，因为一次颗粒间隙较大，有利于锂源在烧结中的迁移。
图6为2种前驱体烧结后正极材料二次颗粒及切面SEM图。连续法前驱体一次颗粒较密，烧结中会影响锂源的渗透，且烧结成材料后一次颗粒更加紧密，会阻碍Li+的迁移。半连续法前驱体一次颗粒较大，其离子传输空隙较大，更容易传输Li+，可以进一步发挥材料的循环倍率性能。
2.3　电化学性能分析
图7为2种前驱体材料制备成的纽扣电池不同倍率下的首次库仑效率。随着倍率从0.2C/0.33C增加到0.2C/2C，半连续法产品的倍率性能优势逐渐体现出来。
在0.2C倍率下，半连续法前驱体对应纽扣电池的放电比容量为207.8 mAh/g，首次库仑效率为92.0%；连续法前驱体对应纽扣电池的放电比容量为205.7 mAh/g，首次库仑效率为91.1%。半连续法前驱体制备成品容量和首次库仑效率高的原因主要是其前驱体形貌属于离散多孔结构，高温烧结过程氢氧化锂更容易扩散至颗粒内部，整体反应较均匀；同时，在相同烧结温度条件下，材料结晶度相同，半连续法前驱体一次颗粒明显小于连续法，离子扩散能力较强[20]，容量和首次库仑效率能够发挥优势。
软包电池是评估正极材料综合电化学性能的有效方式，本实验将不同前驱体制备的正极材料组装成0.8 Ah软包电池，负极采用商用石墨负极。
图8为不同前驱体制备的正极材料在不同荷电状态（SOC）下的测试结果。直流阻抗主要分为欧姆阻抗、电荷转移阻抗和离子扩散阻抗。充电过程中，欧姆阻抗基本不变，电荷转移阻抗和离子扩散阻抗呈先减小后稳定再增大的趋势，与测试结果相符。低充电荷度下半连续法前驱体内部疏松孔隙结构能更好地浸润电解液，有利于锂离子的迁移，因此离子扩散阻抗较小。半连续法前驱体制备的正极材料在0.33C倍率下的放电比容量为200.7 mAh/g（首次库仑效率90.9%），高于连续法前驱体制备成品在0.33C倍率下的放电比容量198.0 mAh/g（首次库仑效率89.6%），与纽扣电池容量结果一致。
2种软包电池的常温和高温循环曲线如图9所示，2种材料45 ℃循环50次后的切面SEM图见图10。正极材料容量差异与前驱体结构差异相关。常温下，半连续法前驱体对应的正极循环性能没有明显优势是因为一次颗粒间隙大，与电解液副反应增多，导致微裂缝不断累积，但连续法前驱体对应的正极一次颗粒紧密，不利于锂离子的脱嵌，因此初始放电容量较低。高温下，半连续法前驱体制备的正极材料循环性能优于连续法前驱体制备的正极材料，是因为在高温下电解液浸润更快，离子迁移率高，但蓬松的二次颗粒更容易减小充放电过程中离子迁移的剪应力，减少了晶格收缩的微裂纹[21]。切面SEM图显示，连续法的二次颗粒中间破裂现象明显。
3　结论
收起
聚焦半连续法与连续法这2种前驱体合成工艺路线，对其制备的前驱体及对应高镍正极产品性能差异展开研究。XRD测试结果显示，2种前驱体物相相近，但半连续法制备的前驱体内部形貌更疏松多孔，较大一次颗粒间隔利于后续嵌锂与氧化反应，所得正极产品层状结构更优、孔隙率更大、低荷电状态下阻抗更低、放电比容量及首次库仑效率更高。面对45 ℃高温循环检测，半连续法前驱体制备的正极因二次颗粒孔隙结构可缓冲充放电时晶体体积膨胀应力，循环性能更佳，材料不易碎裂。基于当前工艺水平，半连续法生产的前驱体制备的高镍正极产品更具市场竞争力。
基金
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  • 国家自然科学基金重点项目(52234001)
  • 湖南省教育厅科学重点研究项目(22A0045)
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2025年第45卷第1期
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doi: 10.3969/j.issn.0253-6099.2025.01.025
  • 接收时间：2024-09-05
  • 首发时间：2026-03-17
  • 出版时间：2025-02-01
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  • 收稿日期：2024-09-05
基金
国家自然科学基金重点项目(52234001)
湖南省教育厅科学重点研究项目(22A0045)
作者信息
    1.五矿新能源材料（湖南）股份有限公司，湖南　长沙　410205
    2.湖南师范大学　化学化工学院，湖南　长沙　410081

通讯作者:

杨立山（1983—），男，湖南岳阳人，博士，副教授，硕士研究生导师，主要研究方向为新能源材料与器件。E-mail：
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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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