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Article(id=1241081041398592138, tenantId=1146029695717560320, journalId=1235980550691926019, issueId=1241081025531540408, articleNumber=null, orderNo=null, doi=10.3969/j.issn.0253-6099.2024.04.011, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1717257600000, receivedDateStr=2024-06-02, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1773826378440, onlineDateStr=2026-03-18, pubDate=1722441600000, pubDateStr=2024-08-01, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1773826378440, onlineIssueDateStr=2026-03-18, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1773826378440, creator=13701087609, updateTime=1773826378440, 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=61, endPage=66, ext={EN=ArticleExt(id=1241081043042759387, articleId=1241081041398592138, tenantId=1146029695717560320, journalId=1235980550691926019, language=EN, title=Synthesis of Sn-Sb-Cu-Fe-Zn High-Etropy Alloy/Carbon Nanofiber Composite Anode Material by Electrospinning, columnId=1241081026567533498, journalTitle=Mining and Metallurgical Engineering, columnName=SPECIAL ISSUE: BATTERY MATERIALS, runingTitle=null, highlight=null, articleAbstract=

Sn-Sb-Cu-Fe-Zn high-entropy alloy nanoparticles were uniformly anchored on conductive interconnected carbon nanofibers by electrospinning in combination with calcination process, and a composite anode material of SnSbCuFeZn@CNFs for lithium-ion batteries was successfully synthesized. Research shows that calcination temperature has an important influence on the phase composition and morphology characteristics of the synthesized material, and directly affects the crystal phase, size and distribution of Sn-Sb-Cu-Fe-Zn high-entropy alloy nanoparticles, also determines the electrochemical performance of SnSbCuFeZn@CNFs electrode. In the studied samples, the SnSbCuFeZn@CNFs-900 electrode can present excellent comprehensive performance: it delivers an initial specific discharge capacity of 1 232.8 mA/g at 0.1 A/g, and has reversible specific discharge capacity retaining at 786.0 mA/g after 200 cycles; it delivers a specific discharge capacity of 433.8 mA/g after 500 cycles at 1.0 A/g; it is found that the pseudo-capacitance accounts for as high as 93.37% at a scanning speed of 2.0 mV/s.

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采用静电纺丝技术，结合煅烧工艺，将SnSbCuFeZn高熵合金纳米颗粒均匀地锚定在导电互联的碳纳米纤维中，成功制备了SnSbCuFeZn@CNFs锂离子电池复合负极材料。结果表明，煅烧温度对材料的物相组成和形貌特征有重要影响，且直接影响SnSbCuFeZn高熵合金纳米颗粒的晶相、尺寸和分布，决定SnSbCuFeZn@CNFs电极的电化学性能。其中SnSbCuFeZn@CNFs-900电极展现出优良综合性能：0.1 A/g时，初始放电比容量达1 232.8 mA/g，循环200次后可逆放电比容量保持在786.0 mA/g；1.0 A/g时，循环500次后放电比容量仍有433.8 mA/g；2.0 mV/s扫描速度下，赝电容贡献率高达93.37%。

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肖围（1985—），男，湖北荆州人，博士，教授，主要研究方向为资源化工、新能源材料。E-mail：
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辛玉（1999—），女，河南信阳人，博士研究生，主要研究方向为新能源材料。E-mail：

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辛玉（1999—），女，河南信阳人，博士研究生，主要研究方向为新能源材料。E-mail：

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Advanced Materials, 2021, 33(37): 2100808., articleTitle=Increasing accessible subsurface to improving rate capability and cycling stability of sodium-ion batteries, refAbstract=null)], funds=[Fund(id=1241081057869623743, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241081041398592138, awardId=52274292, language=CN, fundingSource=国家自然科学基金(52274292), fundOrder=null, country=null), Fund(id=1241081057945121218, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241081041398592138, awardId=2020CFA090, language=CN, fundingSource=湖北省自然科学基金杰青项目(2020CFA090), fundOrder=null, country=null), Fund(id=1241081058024812998, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241081041398592138, awardId=2023EC37, language=CN, fundingSource=荆州市科技计划项目(2023EC37), fundOrder=null, country=null)], companyList=[AuthorCompany(id=1241081050047246497, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241081041398592138, xref=null, ext=[AuthorCompanyExt(id=1241081050051440802, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241081041398592138, companyId=1241081050047246497, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=College of Chemistry and Environmental Engineering, Yangtze University, Jingzhou 434023, Hubei, China), AuthorCompanyExt(id=1241081050059829411, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241081041398592138, companyId=1241081050047246497, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=长江大学 化学与环境工程学院，湖北 荆州 434023)])], figs=[ArticleFig(id=1241081054530957672, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241081041398592138, language=EN, label=null, caption=null, figureFileSmall=bR53BlTYuugokMLWSGfwBg==, figureFileBig=JYPLBTaBQ1zfX3O0dRQGYw==, tableContent=null), ArticleFig(id=1241081054669369712, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241081041398592138, language=CN, label=图1, caption=不同煅烧温度下材料XRD图谱, figureFileSmall=bR53BlTYuugokMLWSGfwBg==, figureFileBig=JYPLBTaBQ1zfX3O0dRQGYw==, tableContent=null), ArticleFig(id=1241081054908445051, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241081041398592138, language=EN, label=null, caption=null, figureFileSmall=woqduEHorbnbhAtk+XFk3g==, figureFileBig=OI8NIEzlyffFRb4ek9Ma5A==, tableContent=null), ArticleFig(id=1241081055025885568, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241081041398592138, language=CN, label=图2, caption=不同煅烧温度下复合材料SEM及EDS图

（a）600 ℃，SEM；（b）700 ℃，SEM；（c）800 ℃，SEM；（d）900 ℃，SEM；（e）1 000 ℃，SEM；（f）900 ℃，EDS

, figureFileSmall=woqduEHorbnbhAtk+XFk3g==, figureFileBig=OI8NIEzlyffFRb4ek9Ma5A==, tableContent=null), ArticleFig(id=1241081055139131782, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241081041398592138, language=EN, label=null, caption=null, figureFileSmall=zmQI/LfyxfSj1N8Cq0U8+A==, figureFileBig=msWEvvG6AjJtFg10ijFQpg==, tableContent=null), ArticleFig(id=1241081055260766605, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241081041398592138, language=CN, label=图3, caption=电极循环性能测试结果

（a）0.1 A/g下循环性能曲线；（b）不同电流密度下倍率性能曲线；（c）SnSbCuFeZn@CNFs-900电极1.0 A/g下长循环性能曲线

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（a）0.2～2.0 mV/s扫描速度下的CV曲线；（b）lgi-lgv曲线；（c）0.2 mV/s扫描速度下的赝电容贡献；（d）各扫描速度下的赝电容贡献

, figureFileSmall=f6YXwHyeCBXJcK7YS158cw==, figureFileBig=kvGWNX8Wmg14JrN4kevQ1Q==, tableContent=null), ArticleFig(id=1241081057215312295, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241081041398592138, language=EN, label=null, caption=null, figureFileSmall=u7/e+Pair0eeZJvIhHyc2A==, figureFileBig=UtKnyZk9tYtMc2Fl+NK9Zw==, tableContent=null), ArticleFig(id=1241081057332752813, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241081041398592138, language=CN, label=图6, caption=SnSbCuFeZn@CNFs-900电极循环200次后SEM及EDS图, figureFileSmall=u7/e+Pair0eeZJvIhHyc2A==, figureFileBig=UtKnyZk9tYtMc2Fl+NK9Zw==, tableContent=null), ArticleFig(id=1241081057462776242, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241081041398592138, language=EN, label=null, caption=null, figureFileSmall=NXpqX6TrtorJ3v5WTughVw==, figureFileBig=W5rk1BNLZAbPaQPzbOkyEg==, tableContent=null), ArticleFig(id=1241081057542468021, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241081041398592138, language=CN, label=图7, caption=SnSbCuFeZn@CNFs-900电极Nyquist图及低频区Z′与ω-1/2的拟合图, figureFileSmall=NXpqX6TrtorJ3v5WTughVw==, figureFileBig=W5rk1BNLZAbPaQPzbOkyEg==, tableContent=null), ArticleFig(id=1241081057622159800, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241081041398592138, language=EN, label=null, caption=null, figureFileSmall=null, figureFileBig=null, tableContent=
样品状态Rct/Ωσ/（Ω·cm2·s-1/2）D（Li+）/（cm2·s-1）
循环前140.5332.05.2×10-16
循环后45.5222.41.2×10-15
), ArticleFig(id=1241081057722823099, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241081041398592138, language=CN, label=表1, caption=

等效电路拟合样品的相关参数

, figureFileSmall=null, figureFileBig=null, tableContent=
样品状态Rct/Ωσ/（Ω·cm2·s-1/2）D（Li+）/（cm2·s-1）
循环前140.5332.05.2×10-16
循环后45.5222.41.2×10-15
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静电纺丝法制备SnSbCuFeZn高熵合金/碳纳米纤维复合负极材料
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辛玉 , 潘石 , 聂淑晴 , 缪畅 , 肖围
矿冶工程杂志 | 电池材料专题 2024,44(4): 61-66
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矿冶工程杂志 | 电池材料专题 2024, 44(4): 61-66
静电纺丝法制备SnSbCuFeZn高熵合金/碳纳米纤维复合负极材料
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辛玉 , 潘石, 聂淑晴, 缪畅, 肖围
作者信息
  • 长江大学 化学与环境工程学院，湖北 荆州 434023

    • 辛玉（1999—），女，河南信阳人，博士研究生，主要研究方向为新能源材料。E-mail：

通讯作者:

肖围（1985—），男，湖北荆州人，博士，教授，主要研究方向为资源化工、新能源材料。E-mail：
Synthesis of Sn-Sb-Cu-Fe-Zn High-Etropy Alloy/Carbon Nanofiber Composite Anode Material by Electrospinning
Yu XIN , Shi PAN, Shuqing NIE, Chang MIAO, Wei XIAO
Affiliations
  • College of Chemistry and Environmental Engineering, Yangtze University, Jingzhou 434023, Hubei, China
出版时间: 2024-08-01 doi: 10.3969/j.issn.0253-6099.2024.04.011
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摘要
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采用静电纺丝技术，结合煅烧工艺，将SnSbCuFeZn高熵合金纳米颗粒均匀地锚定在导电互联的碳纳米纤维中，成功制备了SnSbCuFeZn@CNFs锂离子电池复合负极材料。结果表明，煅烧温度对材料的物相组成和形貌特征有重要影响，且直接影响SnSbCuFeZn高熵合金纳米颗粒的晶相、尺寸和分布，决定SnSbCuFeZn@CNFs电极的电化学性能。其中SnSbCuFeZn@CNFs-900电极展现出优良综合性能：0.1 A/g时，初始放电比容量达1 232.8 mA/g，循环200次后可逆放电比容量保持在786.0 mA/g；1.0 A/g时，循环500次后放电比容量仍有433.8 mA/g；2.0 mV/s扫描速度下，赝电容贡献率高达93.37%。

静电纺丝法  /  SnSbCuFeZn高熵合金  /  碳纳米纤维  /  负极材料  /  锂离子电池

Sn-Sb-Cu-Fe-Zn high-entropy alloy nanoparticles were uniformly anchored on conductive interconnected carbon nanofibers by electrospinning in combination with calcination process, and a composite anode material of SnSbCuFeZn@CNFs for lithium-ion batteries was successfully synthesized. Research shows that calcination temperature has an important influence on the phase composition and morphology characteristics of the synthesized material, and directly affects the crystal phase, size and distribution of Sn-Sb-Cu-Fe-Zn high-entropy alloy nanoparticles, also determines the electrochemical performance of SnSbCuFeZn@CNFs electrode. In the studied samples, the SnSbCuFeZn@CNFs-900 electrode can present excellent comprehensive performance: it delivers an initial specific discharge capacity of 1 232.8 mA/g at 0.1 A/g, and has reversible specific discharge capacity retaining at 786.0 mA/g after 200 cycles; it delivers a specific discharge capacity of 433.8 mA/g after 500 cycles at 1.0 A/g; it is found that the pseudo-capacitance accounts for as high as 93.37% at a scanning speed of 2.0 mV/s.

electrospinning  /  Sn-Sb-Cu-Fe-Zn high-entropy alloy  /  carbon nanofiber  /  anode material  /  lithium-ion battery
辛玉, 潘石, 聂淑晴, 缪畅, 肖围. 静电纺丝法制备SnSbCuFeZn高熵合金/碳纳米纤维复合负极材料. 矿冶工程杂志, 2024 , 44 (4) : 61 -66 . DOI: 10.3969/j.issn.0253-6099.2024.04.011
Yu XIN, Shi PAN, Shuqing NIE, Chang MIAO, Wei XIAO. Synthesis of Sn-Sb-Cu-Fe-Zn High-Etropy Alloy/Carbon Nanofiber Composite Anode Material by Electrospinning[J]. Mining and Metallurgical Engineering, 2024 , 44 (4) : 61 -66 . DOI: 10.3969/j.issn.0253-6099.2024.04.011
正文
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便携式电子设备和新能源汽车的蓬勃发展大力推动了可靠、经济、环保储能设备的开发[1-2]。锂离子电池具有零排放、便携性好、工作电压高、循环寿命长等优点，被认为是满足未来设计要求极具前景的代表[3-4]。然而，理论容量仅372 mAh/g的石墨负极限制了下一代锂离子电池的功率和能量密度[5-6]。因此，设计和开发具有高放电比容量的新型负极材料尤为重要，例如硅基材料、锡基材料、过渡金属氧化物[7-8]等。
高熵合金是金属合金领域一个新兴概念，区别于传统合金材料，它将5种及以上金属元素结合在一起，各元素原子随机分布在晶格位置上，热力学上表现出高熵效应[9-10]。凭借特有的熵稳定效应和多主元协同效应，高熵合金作为锂离子电池负极材料表现出优异的储锂容量[11-12]。然而，合金负极固有的体积膨胀制约了其发展，因此研究者常采用调控形貌等手段来改善高熵合金的本征缺陷。采用静电纺丝技术构筑一维碳纳米纤维（CNFs）是当前应用广泛的一种方法，不仅构建了独特的纳米纤维网络，还能显著缩短Li+的扩散路径[13]。此外，原位生成的致密碳基质层能较好地缓冲离子脱/嵌过程中的体积变化[14-15]。基于此，本文通过静电纺丝法和控温煅烧处理，成功将SnSbCuFeZn高熵合金纳米颗粒均匀地封装在导电碳纳米纤维中，深入研究了煅烧温度对样品形貌和物相组成的影响。
1 实验部分
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1.1 实验原料
实验原料主要包括二水合氯化亚锡（SnCl2·2H2O）、氯化锑（SbCl3）、一水合醋酸铜（Cu（CH3COO）2·H2O）、六水合氯化铁（FeCl3·6H2O）、硝酸锌（Zn（NO3）2）、柠檬酸（C6H8O7）、N，N-二甲基甲酰胺（DMF）、聚丙烯腈（PAN，分子质量150 000）和聚乙烯吡咯烷酮（PVP，分子质量1 300 000），均为分析纯，购自上海麦克林生化科技股份有限公司。
1.2 材料制备
前驱体溶液的制备：称取0.400 0 g PAN和0.200 0 g PVP粉末溶于6.00 mL DMF溶液中，60 ℃下持续搅拌12 h。随后，依次加入等摩尔（1 mmol）柠檬酸、SnCl2·2H2O、SbCl3、Cu（CH3COO）2·H2O、FeCl3·6H2O和Zn（NO3）2，60 ℃继续搅拌4 h，获得前驱体溶液，待用。
纳米纤维薄膜的制备：将上述溶液吸入10 mL塑料针管中，选用静电纺丝专用22号针头，铝箔收集，正电压和接收距离分别设定为20 kV和12 cm。纺丝结束后，将纺丝薄膜置于60 ℃干燥12 h，获得纳米纤维薄膜，待用。
SnSbCuFeZn@CNFs复合材料的制备：将上述纺丝薄膜置于空气条件下、280 ℃恒温烧结2 h；再置于氮气条件下，控制煅烧温度分别为600、700、800、900和1 000 ℃，恒温烧结3 h；两步烧结的升温速率均为2 ℃/min。待自然冷却至室温，制得复合材料SnSbCuFeZn@CNFs-x（x=600，700，800，900，1 000，代表对应煅烧温度下的样品）。
1.3 材料表征
采用Bruker D8衍射仪测试样品晶体结构和物相组成；采用日立S-4800场发射扫描电子显微镜（SEM）对样品形貌进行表征；利用牛津X-Max能谱仪确定样品的元素分布情况。
1.4 性能测试
采用传统浆料涂覆工艺，按质量比将80%活性物质、10%乙炔黑和10%聚偏氟乙烯组成的浆料均匀涂覆在铜箔上，干燥后冲片即可制得工作电极，活性物质在铜箔上的负载量为1.0 mg/cm2。选取金属锂片为对电极，电解液溶质为1 mol/L LiPF6，电解液溶剂为碳酸乙烯酯、碳酸二甲酯和碳酸二乙酯（体积比1∶1∶1），聚丙烯膜为隔膜，组装成2025扣式电池。在CT-2001A蓝电测试系统上、0.01～3.00 V范围内进行恒流充放电测试，CHI660E电化学工作站上记录循环伏安（CV）曲线和电化学阻抗谱（EIS）曲线。
2 实验结果与讨论
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2.1 煅烧温度对材料物相和形貌的影响
图1为SnSbCuFeZn@CNFs复合材料的XRD图谱。煅烧温度600、700 ℃时，复合材料存在氧化物杂峰，制备的SnSbCuFeZn高熵合金物相不纯。氮气气氛下，PAN和PVP热解碳具有还原性，但较低的温度下还原能力较弱，使得5种金属组分之间的合金化反应不完全，导致复合材料物相不纯[16]。SnSbCuFeZn@CNFs-x（x=800，900，1 000）复合材料的特征衍射峰十分明显，表明高熵合金材料结晶度高；且与Cu6Sn5标准卡片（JCPDS-45-1488）匹配度高，属于单斜晶系。30.09°、43.27°和44.78°处的尖峰分别对应Cu6Sn5的、和（024）晶面。样品只存在Cu6Sn5相的特征信号，这是由于相似的原子半径，Sb原子部分取代Sn原子，Fe和Zn原子部分取代Cu原子随机分布在晶胞中。因此，煅烧温度高于800 ℃是成功制备SnSbCuFeZn高熵合金材料的一个关键条件。
SnSbCuFeZn@CNFs复合材料SEM及EDS结果如图2所示。结果表明，所有样品均由连续且相互缠绕的纳米纤维构成，成功搭建了独特的3D网络结构，这有利于缩短Li+扩散路径，加快Li+传输速率。需要注意的是，煅烧温度不同，复合纳米纤维负载的纳米颗粒数量和分布状态也存在明显差异。煅烧温度600 ℃和700 ℃所得复合材料外表面负载纳米颗粒较少，这是由于弱的碳热还原反应有利于生成的氧化物和少量的高熵合金纳米颗粒嵌入碳纤维骨架中。煅烧温度800～1 000 ℃时，复合材料中SnSbCuFeZn高熵合金纳米颗粒可以被清楚地观察到。同时，随着煅烧温度升高，纤维表面黏附的高熵合金纳米颗粒数量不断增加，说明晶粒聚集现象加重，最终将诱导合金颗粒向外扩散[17]。900 ℃复合材料的EDS图再次证明了Sn、Sb、Cu、Fe和Zn元素均匀地分布在整个纤维网络。
图1和图2证实已成功定制了连续导电的碳纳米纤维框架、均匀封装了SnSbCuFeZn高熵合金纳米颗粒。
2.2 煅烧温度对电极循环性能的影响
SnSbCuFeZn@CNFs-x（x=800，900，1 000）电极循环性能测试结果见图3。图3显示，SnSbCuFeZn@CNFs-x（x=800，900，1 000）电极在0.1 A/g下的初始放电比容量分别为1 336.0、1 232.8、1 018.6 mAh/g；循环200次后，可逆放电比容量分别为658.6、786.0、655.2 mAh/g。SnSbCuFeZn@CNFs-1 000电极的比容量较低，说明过高温易引起碳基质结构严重破坏，明显降低材料储锂能力。SnSbCuFeZn@CNFs-x（x=800，900，1 000）电极在2.0 A/g电流密度下的放电比容量分别是351.4、366.8、267.2 mAh/g；当电流密度恢复到0.1 A/g时，电极的比容量分别可达到575.8、688.6、522.8 mAh/g。循环和倍率性能测试表明：SnSbCuFeZn @CNFs-900电极表现出优异的放电比容量和稳定的循环性能。此外，长循环性能曲线也证实了SnSbCuFeZn@CNFs-900电极的耐久性，1.0 A/g下循环500次，电极放电比容量仍有433.8 mA/g，库仑效率高达99.73%。可以得出结论：900 ℃下烧结制备的SnSbCuFeZn@CNFs电极表现出极佳的电化学储锂性能。
2.3 SnSbCuFeZn@CNFs-900电极储锂机制分析
图4（a）为SnSbCuFeZn@CNFs-900电极在0.01～3.00 V电压范围、0.1 mV/s扫描速度下的CV曲线。首次锂化/去锂化过程中，1.15 V处的还原宽峰与中间产物Li3SnSbZn合金相的形成有关（式（1）），同时生成稳定致密的固体电解质界面（solid electrolyte interphase，SEI）膜[18]。随着Li+不断嵌入，Li3SnSbZn合金相结合Li+生成LixM（M=Sn，Sb，Zn）合金相，因此在0.45 V处存在明显且尖锐的阴极还原峰（式（2））。同样地，位于0.63～1.03 V范围内多个阳极氧化峰代表LixM多元合金相的逐步去合金化反应（式（1）与式（2）逆反应）。此外，后续的CV曲线基本重合，证明了SnSbCuFeZn@CNFs-900电极具有高度电化学可逆性。SnSbCuFeZn@CNFs-900电极在0.1 A/g下前4圈恒流充放电曲线如图4（b）所示。电极在1.0和0.3 V附近表现出延长的放电电压平台，在1.1 V附近表现出倾斜的充电电压平台，这分别与CV曲线中的还原峰和氧化峰相对应，反映SnSbCuFeZn@CNFs-900电极发生的电化学氧化还原反应过程[19]。
图5为SnSbCuFeZn@CNFs-900电极赝电容性能测试结果，可以进一步揭示电极内在的电荷存储机制。如图5（a）所示，即使在2.0 mV/s扫描速度下，CV曲线形状仍被很好保持，这是由SnSbCuFeZn@CNFs-900电极高度可逆性决定的。一般来说，复合电极总电荷存储行为分为扩散控制行为和表面电容控制行为，可根据式（3）中b值的大小来判断。式（3）中a和b值可以通过对峰值电流i（mA）与扫描速度v（mV/s）间对数曲线（lgi-lgv曲线）的截距和斜率分别进行拟合得到，它们是变化的可调参数。如图5（b）所示，阴极、阳极峰的b值分别为0.85与0.80，均接近1.0，这意味着SnSbCuFeZn@CNFs-900电极赝电容行为占主导地位，从而表现出快速的电化学反应动力学[20-21]。此外，各扫描速度下的赝电容贡献率可以依据式（4）进一步量化。图5（c）显示SnSbCuFeZn@CNFs-900电极在0.2 mV/s时的赝电容贡献率为64.70%。从图5（d）可看出，扫描速度从0.2 mV/s增加到2.0 mV/s时，赝电容贡献比从64.70%逐渐上升到93.37%。需要指出的是，增强的赝电容储锂机制是SnSbCuFeZn@CNFs-900电极保持高放电比容量和优异循环性能的重要原因。
式中：i（V）为电压V下的电流，mA；k1v为赝电容贡献的电流，mA；k2v1/2为扩散控制过程的反应电流，mA。特定电压下k1和k2为常数。
2.4 SnSbCuFeZn@CNFs-900电极性能优异原因分析
图6为SnSbCuFeZn@CNFs-900电极在0.1 A/g下循环200次后的SEM及EDS图。如图6（a）所示，电极表面没有出现任何裂纹和破损；在遭受反复Li+脱嵌过程后，可以很好地缓解合金化反应引起的体积膨胀效应，展现出完整稳定的电极结构，有利于所装配电池提升的储锂性能。从图6（b）～（c）可以明显看出，复合纳米纤维外表面由于致密SEI膜的产生而变得相对粗糙。此外，纳米纤维不仅可以维持初始连续的3D纤维网络特征，并且没有任何团聚趋势。图6（d）的EDS结果表明C、Sn、Sb、Cu、Fe和Zn元素在循环后的SnSbCuFeZn@CNFs-900电极中是均匀分布的，说明碳纳米纤维骨架可以很好地阻止SnSbCuFeZn高熵合金纳米颗粒发生团聚。
通过EIS测试对SnSbCuFeZn@CNFs-900电极在200次循环前后的动力学性能进行了评价。图7（a）是电极在开路电压下的Nyquist图，其中插图为等效电路图，相应的拟合结果如表1所示。经过200次循环后，由于液体电解质的充分渗透，SnSbCuFeZn@CNFs-900电极电荷转移阻抗（Rct）从140.5 Ω明显降到45.5 Ω。为了进一步研究Li+在电极材料中的扩散能力，根据式（5）～（6）计算了电极循环前后的D（Li+）值，如图7（b）所示，SnSbCuFeZn@CNFs-900电极循环前后D（Li+）值分别为5.2×10-16 cm2/s和1.2×10-15 cm2/s，呈现出一个数量级的增长；这部分得益于导电碳纳米纤维基体增强了材料电子导电性，部分归因于互连纤维网络结构提供了丰富的离子转移通道，进而提升Li+在电极材料中的扩散能力。上述结果进一步证实了SnSbCuFeZn@CNFs-900电极在循环过程中突出的储锂能力。
式中：Z′为实部电阻，Ω；Rs为欧姆阻抗，Ω；σ为韦伯因子，Ω·cm2/s1/2；ω为角频率，s-1；D（Li+）为Li+扩散系数，cm2/s；R为气体常数，8.314 J/（K·mol）；T为开尔文温度，K；A为电极面积，cm2；n为电子转移数；F为法拉第常数，96 486 C/mol；C为Li+浓度，mol/cm3。
3 结论
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1）利用静电纺丝工艺，成功将SnSbCuFeZn高熵合金纳米颗粒均匀集成在连续导电的碳纳米纤维中，构建了具有良好机械稳定性的纳米纤维网络结构。
2）控温烧结下，成功制备SnSbCuFeZn高熵合金相的关键条件是煅烧温度高于800 ℃，此时合成的SnSbCuFeZn@CNFs复合材料具有单一Cu6Sn5晶相结构。
3）SnSbCuFeZn高熵合金纳米颗粒的熵稳定效应和导电碳纤维基质的缓冲作用协同提升了SnSbCuFeZn@CNFs-900电极的电化学性能，即使在1.0 A/g下循环500次后，该电极放电比容量仍可达433.8 mA/g。
基金
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  • 国家自然科学基金(52274292)
  • 湖北省自然科学基金杰青项目(2020CFA090)
  • 荆州市科技计划项目(2023EC37)
文献
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2024年第44卷第4期
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doi: 10.3969/j.issn.0253-6099.2024.04.011
  • 接收时间：2024-06-02
  • 首发时间：2026-03-18
  • 出版时间：2024-08-01
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  • 收稿日期：2024-06-02
基金
国家自然科学基金(52274292)
湖北省自然科学基金杰青项目(2020CFA090)
荆州市科技计划项目(2023EC37)
作者信息
    长江大学 化学与环境工程学院，湖北 荆州 434023

通讯作者:

肖围（1985—），男，湖北荆州人，博士，教授，主要研究方向为资源化工、新能源材料。E-mail：
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2种不同金属材料的力学参数
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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
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