现代化工

现代化工 ›› 2025, Vol. 45 ›› Issue (1) : 112-115. DOI: 10.16606/j.cnki.issn0253-4320.2025.01.021

科研与开发

NbTe₂/MXene超结构钾离子电池负极的制备及其性能研究

董臻 ¹ ,
吴邦军 ¹ ,
王重权 ¹ ,
许冠南 ² ,
刘争 ¹ ,
张业龙 ¹^,^*

作者信息 +

Preparation and property of NbTe₂/MXene superstructure anode for potassium ion battery

Author information +

文章历史 +

Received		Published
2024-03-11		2025-01-20
Issue Date	Revised Date
2025-01-17	2024-03-11

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摘要

针对较大尺寸的钾离子在钾离子电池充放电过程中导致负极扩散动力学缓慢并伴随着剧烈的体积变化问题,制备了NbTe₂纳米针垂直生长在MXene纳米片上的三维超结构NbTe₂/MXene。结果表明,该三维超结构具有优异的循环稳定性和倍率性能,在0.2 A/g的电流密度下循环150圈后,可逆比容量仍达到306.8 mAh/g,容量保持率为68.4%,平均每圈容量损耗率仅为0.21%。即使在20 A/g的大电流密度下仍展现出139.8 mAh/g的可逆容量。该超结构具有比表面积大、良好的电子导电性和多活性位点等诸多优势,能够提高钾离子电池的性能,为高性能负极材料的开发提供参考。

Abstract

The relatively large size of potassium ions can lead to slow diffusion kinetics and accompany dramatic volume changes for anodes during the charge-discharge process of potassium-ion battery.In order to solve these problems,NbTe₂/MXene with three-dimensional superstructure is prepared through NbTe₂ nanoneedles vertically growing on MXene nanosheets,which exhibits excellent cycling stability and rate performance.After it has been circled over 150 cycles at a current density of 0.2 A·g^-1,its reversible specific capacity still reaches 306.8 mAh·g^-1 with a capacity retention of 68.4% and an average capacity loss of only 0.21% per cycle.Even at a high current density of 20 A·g^-1,it still achieves a reversible capacity of 139.8 mAh·g^-1.This superstructure possesses numerous advantages such as a large specific surface area,good electronic conductivity,and multiple active sites,which can improve the performance of potassium ion batteries and provide valuable references for the development of high-performance anode materials.

Graphical abstract

关键词

钾离子电池 / NbTe₂ / MXene / 负极材料

Key words

potassium ion battery / NbTe₂ / MXene / anode material

Author summay

董臻(1997-),女,硕士生,研究方向为钾离子电池,dzz1362355@163.com。

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School of Applied Physics and Materials, Wuyi University, Jiangmen 529020, China), AuthorCompanyExt(id=1241353038603973085, tenantId=1226480274814496768, journalId=1226484258170171394, articleId=1240719913624498922, companyId=1241353038595584475, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1.五邑大学应用物理与材料学院,广东江门 529020)])])] 董臻,吴邦军,王重权,许冠南,刘争,张业龙. NbTe₂/MXene超结构钾离子电池负极的制备及其性能研究[J]. 现代化工, 2025, 45(1): 112-115 DOI:10.16606/j.cnki.issn0253-4320.2025.01.021

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钾离子电池(PIBs)作为能源储存系统中锂离子电池的潜在替代品,具有资源丰富、氧化还原电位接近于锂、离子导电性优越^[1⇓-3]。然而,钾离子本身较大的尺寸通常导致其扩散动力学缓慢,并伴随着充放电过程中严重的体积变化,从而导致电池倍率性能和循环性能不令人满意^[4⇓-6]。因此,负极材料是决定全电池性能的重要因素,合理设计高性能负极材料对于提升钾离子电池性能至关重要。

到目前为止,用于电池负极的材料主要有碳基材料^[7-8]、钛基材料^[9-10]、合金材料^[11⇓-13]、磷基材料^[14-15]、有机化合物^[16]和过渡金属二硫化物(TMDs)^[17-18]材料。过渡金属硫化物/硒化物由于其独特的结构特征和高理论比容量,在能源存储领域引起了广泛关注。与过渡金属硫化物和硒化物相比,过渡金属碲化物通常展示出更高的导电性^[19-20]。在各种碲化物中,六方相NbTe₂(H-NbTe₂)由于其出色的电导率而成为一种有潜力的PIBs负极材料^[21]。然而,类似于其他TMDs材料,NbTe₂的性能仍受限于巨大的体积变化和缓慢的离子扩散动力学。MXene作为一类过渡金属碳化物/氮化物,具有高稳定性的二维结构和出色的导电性,在PIBs中广泛应用^[22⇓-24]。

笔者通过溶剂热法将NbTe₂纳米针垂直生长在MXene纳米片上(NbTe₂/MXene)。并考察了垂直生长的NbTe₂纳米的循环性能及倍率性能。

1 实验材料与方法

1.1 药品

MAX粉末(Ti₃AlC₂,纯度99.0%),先丰纳米生产;氢氟酸溶液(HF,AR,48%)、无水乙醇(C₂H₄O₂,AR)、草酸铌(C₁₀H₅NbO₂₀)、十六烷基三甲基溴化铵(CTAB)、Te粉、N,N-二甲基甲酰胺(DMF)、聚偏二氟乙烯(PVDF,99.9%)、N-甲基吡咯烷酮(NMP)、KPF₆[V(EC)∶V(DEC)=1∶1],阿拉丁生产。电池隔膜采用Whatman的GF/F。

1.2 分析测试仪器

德国ZEISS生产的GEMINISEM 300扫描电子显微镜(SEM);德国Bruker生产的D8 Advance X射线衍射能谱仪(XRD);上海Micromeritics Instrument Corp生产的ASAP2460比表面积测试仪(BET);美国Thermo Fisher Scientific Inc生产的Escalab250Xi X射线光电子能谱仪(XPS);武汉CT2001A蓝电测试仪。

1.3 MXene材料的制备

MXene制备:将2 g MAX缓慢浸入40% HF溶液(30 mL)中,在室温下磁力搅拌24 h。所得产物在3 000 r/min的转速下离心5 min,用去离子水洗涤数次。最后在60℃真空烘箱中干燥12 h,得到MXene粉末。

1.4 NbTe₂/MXene及纯NbTe₂的制备

NbTe₂/MXene及纯NbTe₂制备:将0.04 g MXene、0.538 g C₁₀H₅NbO₂₀和0.02 g CTAB加入 20 mL超纯水中,再将0.255 g Te粉加入20 mL DMF中,室温搅拌10 h。将以上溶液倒入50 mL反应釜中,在200℃保持24 h。冷却后用离子水和乙醇进行多次洗涤,并在60℃真空干燥10 h。若不添加MXene则合成为纯NbTe₂。

1.5 电池组装和电化学性能测试

电池组装:以7∶2∶1的质量比将活性物质、碳黑和聚偏氟乙烯(PVDF)混合,随后滴入适量NMP搅拌12 h。将所得混合物作为浆料涂覆在铜箔上,后真空烘干得到极片。在充满氩气的手套箱中进行电池组装,将金属钾片作为对电极,Whatman的GF/F玻璃纤维作为隔膜,0.8 mol/L KPF₆[V(EC)∶V(DEC)=1∶1]作为电解液组装成CR2032型电池。

电化学测试:在蓝电电池测试平台进行恒电流充放电测试,电压为0.01~2.6 V。电化学阻抗谱(EIS)使用电化学工作站(VMP3,Bio-Logic SAS)进行测试。

2 结果与讨论

2.1 材料的形貌和结构分析

2.1.1 SEM、SAED和EDS表征

NbTe₂/MXene和MXene的SEM、SAED和EDS图如图1所示。从图1(a)中可以看出,MXene呈现出三维分层的“手风琴”结构。从图1(b)中可以看出,NbTe₂纳米针成功垂直生长于MXene表面,形成NbTe₂/MXene超结构。从图1(c)中可以看出,利用选区衍射(SEAD)发现,NbTe₂/MXene中存在属于NbTe₂的衍射环,对应(-310)、(600)和(-913)晶面^[25]。从图1(d)中可以看出,EDS证实Nb、Ti和Te元素在NbTe₂/MXene中均匀分布。

2.1.2 XRD、BET和XPS分析

NbTe₂/MXene和对照组的XRD、BET和XPS测试结果如图2所示。从图2(a)中可以看出,NbTe₂/MXene的衍射峰来自于NbTe₂(PDF 21-0605-1111)的(001)、(002)、(100)和(011)晶面,分别位于13.4、27.28、31.1°和39.2°。MXene的(002)向较低角度明显移动^[26-27]。从图2(b)中可以看出,NbTe₂/MXene的比表面积相较于NbTe₂和MXene有一定的增大,表明NbTe₂纳米针的负载一定程度上增大了MXene层间距,有助于容纳体积膨胀。计算得出NbTe₂/MXene、NbTe₂和MXene比表面积分别为72.5、49.9 m²/g和36.5 m²/g。通过NbTe₂纳米针均匀覆盖MXene,该超结构暴露出更多的活性位点,并有利于电极液浸润^[28]。从图2(b)中可以看出,NbTe₂/MXene内存在Nb、Te和Ti元素。

从图2(c)中可以清晰地看到2个明显的分裂峰,分别位于207.1 eV和209.8 eV,对应于Nb 3d核心峰,归属于Nb 3d_5/2和

Nb 3d 3 / 2

^[29]。从图2(d)中可以看出,572.7 eV和583.1 eV处为Nb—Te键的峰,576.4 eV处的峰为Te 3d_5/2,586.8 eV处的峰为

Te 3d 3 / 2

^[30]。值得注意的是,在574.1 eV和584.7 eV处观察到2个属于Ti—Te键的峰,证实了MXene和NbTe₂之间通过化学键连接。综上所述,XRD、BET和XPS的结果表明,材料成功合成且具有较大的比表面积和丰富的化学键。

2.2 电化学性能分析

NbTe₂/MXene基钾离子电池电化学性能测试结果如图3所示。从图3(a)中可以看出,NbTe₂/MXene在0.2 A/g电流密度下,第1、2、10和100圈循环时的充电比容量分别为457.8、387.9、362.2 mAh/g和345.5 mAh/g。从图3(b)中可以看出,即使经过150圈循环之后,NbTe₂/MXene的可逆容量为306.8 mAh/g,明显大于NbTe₂(158.9 mAh/g)和MXene(81.4 mAh/g)。在前150圈循环中,NbTe₂/MXene显示了68.4%的容量保持率,平均每圈损耗约0.21%。

从图3(c)中可以看出,NbTe₂/MXene电极在电流密度为0.2、0.5、1、2、5、10 A/g和20 A/g的可逆容量分别为412.96、318.72、266.04、239.04、215.28、172.2 mAh/g和139.8 mAh/g,明显大于NbTe₂和MXene材料。当电流密度恢复到10 A/g时,可逆容量与之前10 A/g时没有明显变化,展现出优异的倍率性能和电化学稳定性。

从图3(d)中可以看出,NbTe₂/MXene负极的电子转移电阻(R_ct)为1 212.4 Ω,明显小于与NbTe₂(1 674.3 Ω)和MXene(2 275.7 Ω),该结果证明NbTe₂/MXene具有最快的电子转移动力学^[31]。

根据Nb基硫族化物在锂离子电池和钠离子电池的充放电机理,结合测得的NbTe₂/MXene电化学性能,推测NbTe₂/MXene的钾储存机制为:

(1)

(2)

(3)

3 结论

利用水热法合成了NbTe₂/MXene超结构钾离子电池负极。该超结构具有优异的循环稳定性和出色的倍率性能,在0.2 A/g的电流密度下循环150圈后,保持可逆容量为306.8 mAh/g,当电流密度达到20 A/g时,其可逆容量仍保持139.8 mAh/g。该超结构钾离子电池负极的优点在于大的比表面积、良好的导电性和丰富的活性位点。该研究将为高性能钾离子电池负极的设计提供新的思路。

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