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2023 , Vol. 51 >Issue 4: 87 - 96

DOI: https://doi.org/10.15983/j.cnki.jsnu.2023314

Shape modulation of three-dimensional porous Ni3S2 electrodes for enhanced sodium storage performance

  • FAN Xiaoyong , * ,
  • ZHANG Lulu ,
  • SUN Ruibo
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  • School of Materials Science and Engineering, Chang’an University, Xi’an 710061, Shaanxi, China

Received date: 2023-02-20

  Online published: 2023-07-24

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Abstract

Ni3S2 anode of sodium-ion batteries suffers severe volume changes and materials pulverization during cycling, resulting in poor cycle stability. This work selects three-dimensional porous nickel as the substrate and simultaneously controls the hydrothermal time to regulate the morphology of the Ni3S2 electrode. The results show that the three-dimensional porous Ni3S2 electrode tends to generate nanosheet arrays in a short hydrothermal time. With the increase of hydrothermal time, the nanosheet arrays partially transformed into nanotube arrays and eventually completely transformed into nanotube arrays. Due to the high stability of nanotube structure during cycling, three-dimensional porous Ni3S2 nanotube array electrode shows the best long cycle performance and rate performance. It delivers a specific capacity of 279.1 mA·h/g after 200 cycles at a current density of 100 mA/g with a retention of 53.7%, which was much higher than that of the three-dimensional porous Ni3S2 nanosheet array electrode (26.6%) and the Ni3S2 electrode with three-dimensional porous nanosheet/nanotube structure (38.7%). Even at a high current density of 1.6 A/g, the three-dimensional porous Ni3S2 nanotube array electrode still provides a specific capacity of 291.1 mA·h/g.

Key words： sodium-ion battery; three-dimensional porous; nickel sulfide; nanosheet; nanotube

Cite this article

FAN Xiaoyong , ZHANG Lulu , SUN Ruibo . Shape modulation of three-dimensional porous Ni3S2 electrodes for enhanced sodium storage performance[J]. Journal of Shaanxi Normal University(Natural Science Edition), 2023 , 51(4) : 87 -96 . DOI: 10.15983/j.cnki.jsnu.2023314

近年来,随着电动汽车产业和手机等通信类产业的快速发展,对储能器件提出了更高的要求[1⇓-3]。锂离子电池(lithium-ion batteries)由于其能量密度高和循环寿命长等特点,目前已经成为便携式电子器件的主要电源。然而,锂资源的匮乏和价格的上涨限制了锂离子电池在大型储能等领域中的应用[4⇓-6]。金属钠在地壳中含量丰富,同时钠离子电池(sodium-ion batteries)的电化学反应机理与锂离子电池相似,可替代锂离子电池作为新一代的储能电源[7⇓⇓⇓⇓⇓-13]。然而,Na+ 在循环过程中结构应变和体积变化较大,以及离子传输和反应动力学等不佳,导致循环寿命有限,高倍率容量低,阻碍了其大规模商业化。因此,寻求具有合适孔结构和电子转移通道的电极材料以有效地存储和传输较大的Na+,适应反复的体积变化被认为是增强钠离子电池电化学性能的关键途径。Ni3S2具有理论比容量高、原材料成本低、合成方法简单且容易制备等优点,被认为是钠离子电池理想负极选择之一。然而,其作为钠离子电池负极在循环过程中存在体积变化大和材料粉化等问题,导致其循环稳定性差[14⇓⇓⇓⇓⇓⇓⇓-22]。
迄今为止,已采用许多策略来增强转换型电极的Na+储存性能:(1)合成阵列电极以通过缩短离子/电子传输路径并提供丰富的空隙来缓解循环过程中较大的体积变化和释放机械应力来增强其电化学性能[23⇓-25];(2)设计和构筑三维集流体以支撑电极材料,可适应活性材料的体积变化,缓解活性物质和集流体之间的应力以保证电极完整性,并在循环过程中为Na+离子提供快速的传输通道[26⇓-28]。目前,用于锂离子电池或钠离子电池的传统三维多孔金属集流体主要包括通过自组装模板牺牲法制备的三维有序多孔金属[29]、通过脱合金法制备的纳米多孔金属[30]、以电沉积方法通过氢气泡模板法作为自组装模板制备的大孔金属[31]。然而,这些三维集流体仍然存在诸多问题,例如:合成方法复杂、耗时较长、孔结构不稳定、在负载活性材料或循环过程中容易损坏、难以适应电极材料的体积变化等。本研究组开发了一种工艺简单、易规模化的化学镀方法,以制备结构稳定、孔径约几微米的三维多孔集流体,并成功地提高了Li+和Na+的存储性能[15,31⇓⇓ -34]。
构筑不同微观形貌的电极,借助形貌调控改善电极材料的电子/离子传输动力学,也被认为是一种缓解材料应力、提升电池循环寿命的有效手段[32,35⇓⇓⇓⇓-40]。目前,已有多种形貌被设计出来,主要有:纳米片[41⇓-43]、纳米管[44-45]、纳米棒[25,46]和纳米线[47-48]等。Fan等[33]通过阳极氧化法在多孔铜表面制备Cu(OH)2纳米线阵列,继而在氩气气氛下热处理,得到三维多孔铜纳米线阵列,然后恒电流电沉积锑,获得三维 Cu@Sb 纳米线阵列(nanowire arrays)。相互贯穿的三维多孔结构和纳米线之间的大量空隙可极大地缓解材料在循环过程中的体积膨胀,改善其电化学性能,在330 mA/g的电流密度下,经过200次循环后,三维Cu@Sb NWAs电极的比容量为561.1 mA·h/g,保持率高达92.7%。Liang等[49]通过水热法在碳纤维上构筑了自支撑的MoS2纳米片阵列,作为钠离子电池的负极材料时,CFC/MoS2纳米片阵列在0.5 A/g下可以提供413 mA·h/g的比容量,这种良好的性能主要归因于碳纤维的网状结构和独特纳米片阵列结构,纳米片可以作为离子的定向传输通道,纳米片之间的空隙可以适应循环过程中的体积变化,改善材料的循环性能。
本工作以三维多孔镍为集流体,利用水热法合成三维多孔硫化镍纳米材料,通过控制水热过程的时间,设计了3种具有不同形貌的Ni3S2负极材料。如图1所示,水热时间为1 h时得到三维多孔Ni3S2纳米片阵列,水热时间变为4 h时得到纳米片和纳米管复合形貌的三维多孔Ni3S2,当水热时间进一步延长为10 h时得到三维多孔Ni3S2纳米管阵列,依次记为3D Ni3S2-Ⅰ,3D Ni3S2-Ⅱ,3D Ni3S2-Ⅲ。探索了时间变化对三维多孔硫化镍形貌的影响并分析形貌变化中电化学性能的演变。
图1 三维多孔Ni3S2电极的形貌调控示意图

注:网络版为彩图。

Fig.1 Schematic diagram of morphological regulation of three-dimensional porous Ni3S2 electrode

1 实验

1.1 不同形貌的三维多孔硫化镍制备

以自制的三维多孔镍为基底[15],采用水热法制备不同形貌的三维多孔Ni3S2电极。首先将三维多孔镍(质量为m1)加入0.000 625 mol/L的硫代硫酸钠溶液中,并抽负压以保证硫代硫酸钠溶液与三维多孔镍集流体充分接触;然后将其取出放入含有15 mL硫代硫酸钠液的聚四氟乙烯水热反应釜中,以 2 ℃/min升温至130 ℃,分别保温1、4、10 h。水热过程发生的反应:3Ni+2Na2S2O3→Ni3S2+2Na2SO3。水热反应完成后,用水和乙醇清洗反应产物Ni3S23次,将其放入真空干燥箱中,在80 ℃下真空烘干12 h,待其冷却至室温便可取出反应产物,得到三维多孔Ni3S2,记为3D Ni3S2-Ⅰ,3D Ni3S2-Ⅱ 和3D Ni3S2-Ⅲ,并且称量其质量,记为m2,活性物质Ni3S2的质量记为m3=Δm×240.1/64,其中Δm=m2-m1。3D Ni3S2-Ⅰ,3D Ni3S2-Ⅱ,3D Ni3S2-Ⅲ的负载量分别为2.0、2.3、2.9 mg/cm2。本实验中所使用的药品均为国药购买,无需进一步加工。

1.2 电池的组装

以三维多孔Ni3S2电极为正极,钠片为负极,将NaClO4以1 mol/L的浓度溶解于碳酸丙烯酯和5%氟代碳酸亚乙酯混合而成的溶剂中,制备成电解液。玻璃纤维(Whatman GF/D)为隔膜,在含有高纯氩气的手套箱中组装成2025型纽扣电池。

1.3 材料表征与电化学测试

本文选用德国布鲁克公司生产的D8 ADVANCE的X射线衍射仪进行物相分析,辐射源为Cu靶所产生的λ=0.154 18 nm的Kα射线,测试角度2θ选择10°到80°。采用 Hitachi S-4800型场发射扫描电子显微镜(SEM, 日立公司)对样品表面形貌进行观察。恒电流长循环和倍率性能测试在新威测试仪上进行,电压窗口0.01~3 V,恒电流长循环测试的电流密度为0.1 A/g,倍率性能测试分别以0.1、0.2、0.4、0.8、1.6 A/g的电流密度循环5次,最后再以0.1 A/g的电流密度进行循环。采用新威测试仪进行恒电流间歇滴定测试,电池经过24 h的静置后首先以100 mA/g的电流密度循环5次以达到稳定状态,测试期间,弛豫时间为2 h,恒电流过程是在46 mA/g的电流密度下进行充电或放电30 min。

2 结果与讨论

2.1 形貌分析

图2给出不同水热时间制备的三维多孔Ni3S2的SEM图。由图2a~c可以发现,当水热时间为1 h时,Ni3S2呈现纳米片状的阵列结构,附着在三维多孔镍的孔壁上;图2d~f是水热时间为4 h时三维多孔Ni3S2的形貌,此时纳米管开始出现,Ni3S2呈现纳米片和纳米管的混合形貌。进一步对纳米管的出现区域进行了高分辨分析(见图2a和2d),在红色虚线区域内发现纳米片通过卷绕的方式向纳米管进行转化。可以推测:水热过程中首先生成纳米片阵列,随着水热时间的增长,纳米片逐渐卷绕,转化为纳米管。为了得到更多的纳米管形貌,将水热时间延长为10 h,所得到的形貌如图2g~i所示,可见数根纳米管交错排列形成纳米管阵列,纳米管的直径大约为50 nm,已经观察不到纳米片的存在。综上所述,在较短的水热时间内,三维多孔Ni3S2形貌趋向于纳米片状结构,随着水热时间的延长,形貌会从纳米片逐渐卷曲成纳米管的结构。
图2 水热时间分别为1 h(a~c),4 h(d~f),10 h(g~i)时得到的三维多孔Ni3S2的SEM图

注:网络版为彩图。

Fig.2 SEM images of 3D Ni3S2 obtained for 1 h (a~c), 4 h (d~f), and 10 h (g~i)

2.2 X射线衍射分析

图3给出了Ni3S2-Ⅲ 的XRD结果,其中44.5°、51.8°、76.4° 出现3个衍射峰,分别对应基底三维多孔镍 (PDF#87-0712) 的 (111)、(200)、(220) 晶面。此外, 21.8°、31.1°、37.8°、49.7°、50.1° 的特征峰对应六方晶型Ni3S2 (PDF#44-1418) 的 (101)、(110)、(003)、(113)和(211)晶面,表明成功制备出三维多孔Ni3S2纳米片阵列。
图3 3D Ni3S2-Ⅲ 的XRD图谱

注:网络版为彩图。

Fig.3 XRD pattern of 3D Ni3S2-Ⅲ

2.3 电化学性能测试

不同的微观形貌会影响材料的电化学性能,为研究形貌对材料性能的影响,对三维多孔Ni3S2-Ⅰ、Ni3S2-Ⅱ和Ni3S2-Ⅲ 分别进行充放电测试,如图4和图5所示。由图4a和图5a可见,3种电极在0.6 V和0.7 V之间分别出现2个放电平台,对应Ni3S2向Ni和Na2S的转换反应(Ni3S2+4Na++4e-→3Ni+2Na2S),即Ni3S2的嵌钠过程。经过2次循环,3种电极的充放电平台几乎相同,其中放电平台在0.91 V左右,充电平台在1.53 V左右(见图4b和5b)。50次循环后(图4c和5c),三维多孔Ni3S2-Ⅰ电极的充放电电压差为0.66 V,大于3D Ni3S2-Ⅱ和3D Ni3S2-Ⅲ的充放电电压差(0.58 V),说明随着循环的进行,三维多孔Ni3S2-Ⅰ电极出现更大的极化,导致其容量降低。经过100次循环后(图4d和5d)三维多孔Ni3S2-Ⅰ电极和三维多孔Ni3S2-Ⅱ电极的充放电电压差分别增大至0.67 V和0.61 V,而三维多孔Ni3S2-Ⅲ的充放电电压差仍为0.58 V,说明三维多孔Ni3S2-Ⅲ电极极化更小,具有优秀的循环性能,其可能的原因是纳米管结构在充放电过程中稳定性更好,而纳米片结构经过循环后结构逐渐塌陷造成极化增大。
图4 三维多孔Ni3S2-Ⅰ、Ni3S2-Ⅱ和Ni3S2-Ⅲ的首圈(a)、第2圈(b)、第50圈(c)、第100圈(d)充放电曲线和对应的长循环性能对比(e)

注:网络版为彩图。

Fig.4 The charge/discharge curves in the first (a), second (b), 50th (c) and 100th (d) cycle of 3D Ni3S2-Ⅰ,3D Ni3S2-Ⅱ and 3D Ni3S2-Ⅲ, and their corresponding long-cycle performance profiles (e)

图5 三维多孔Ni3S2-Ⅰ,三维多孔Ni3S2-Ⅱ和三维多孔Ni3S2-Ⅲ 的首圈(a),第2圈(b),第50圈(c)和第100圈(d) 的微分电容曲线

注:网络版为彩图。

Fig.5 Differential capacitance curves for the first (a), second (b), 50th (c) and 100th (d) cycle of 3D Ni3S2-Ⅰ, 3D Ni3S2-Ⅱ and 3D Ni3S2-Ⅲ

图4e给出了3种电极在100 mA/g下的长循环对比图。三维多孔Ni3S2-Ⅲ电极具有最高的首次可逆比容量,为520.2 mA·h/g,而三维多孔Ni3S2-Ⅰ和三维多孔Ni3S2-Ⅱ 分别为419.9 mA·h/g和420.2 mA·h/g。三维多孔Ni3S2-Ⅰ 的容量持续缓慢衰减,经过200次循环后,比容量仅保持111.5 mA·h/g,保持率为26.6%;而三维多孔Ni3S2-Ⅱ和三维多孔Ni3S2-Ⅲ电极的比容量保持162.5 mA·h/g和279.1 mA·h/g,容量保持率分别为38.7%和53.7%。三维多孔Ni3S2-Ⅲ电极的首次库伦效率高达83.1%,高于三维多孔Ni3S2-Ⅰ(78.9%)和三维多孔Ni3S2-Ⅱ(80.7%)电极的首次库伦效率,说明纳米管结构有利于提高首次库伦效率。
由图6a可观察到,随着电流密度的增大,三维多孔Ni3S2-Ⅰ的充放电电压平台差异明显;当形貌开始从纳米片向纳米管转换时(图6b),三维多孔Ni3S2-Ⅱ的充放电电压平台差异减小;当表面形貌全部为纳米管时(图6c),三维多孔Ni3S2-Ⅲ 表现最小的充放电电压平台差异,此时极化效应最小。图6d为3种电极的倍率性能对比图,可观察到三维多孔Ni3S2-Ⅲ电极拥有最好的倍率性能,在0.1、0.2、0.4、0.8 A/g的电流密度下其可逆比容量分别为400.2、340.8、322.4、308.4 mA·h/g,即使在1.6 A/g的大电流密度下,仍可以提供291.1 mA·h/g的比容量,容量保持率高达72.7%。三维多孔Ni3S2-Ⅱ电极在1.6 A/g时可以提供229.9 mA·h/g的比容量,相比之下,三维多孔Ni3S2-Ⅰ电极仅能提供102.7 mA·h/g,这说明纳米管的结构有利于改善材料的倍率性能。
图6 三维多孔Ni3S2-Ⅰ(a)、Ni3S2-Ⅱ(b)和Ni3S2-Ⅲ(c)的充放电曲线和对应的循环性能曲线(d)

注:网络版为彩图;图中数据为不同的电流密度,单位为A/g。

Fig.6 Charge-discharge curves of 3D Ni3S2-Ⅰ (a), 3D Ni3S2-Ⅱ (b) and 3D Ni3S2-Ⅲ (c),and their corresponding cyclability profiles (d)

为了研究不同形貌对Ni3S2电极循环过程中Na+扩散系数的影响,分别对Ni3S2-Ⅰ、Ni3S2-Ⅱ和Ni3S2-Ⅲ进行恒电流间歇滴定测试,结果如图7所示。恒电流间歇滴定测试是由脉冲、弛豫和恒电流3部分组成,通过记录脉冲和恒电流期间的电压变化,结合弛豫时间,利用如下公式可计算扩散系数
D= 4 π τ m B V M S M B 2 Δ E s Δ E τ 2。
图7 三维多孔Ni3S2-Ⅰ(a)、Ni3S2-Ⅱ(b)和Ni3S2-Ⅲ(c)电极的GITT曲线;三维多孔Ni3S2-Ⅲ电极在GITT测试过程中的单次滴定曲线(d);充电(e)和放电(f)过程的Na+扩散系数

注:网络版为彩图。

Fig.7 The GITT profiles of the 3D Ni3S2-Ⅰ (a), 3D Ni3S2-Ⅱ (b), 3D Ni3S2-Ⅲ (c) electrodes; the single titration profiles of 3D Ni3S2-Ⅲ electrode during the GITT test(d); calculated diffusion coefficients during charging (e) and discharging (f)

其中:τ为弛豫时间,本实验中为120 min;mB为活性物质Ni3S2的质量;MB为Ni3S2的摩尔质量;VM为活性物质Ni3S2的摩尔体积,为41.42 cm3/mol;ΔEs是平衡电位变化;ΔEτ是恒电流极化电位变化。图7d给出了三维多孔Ni3S2-Ⅲ电极在测试过程中的单次滴定曲线,其中:弛豫时间为120 min,恒电流过程是在46 mA/g的电流密度下进行的,时间为30 min。
在Ni3S2储钠过程中Na+的扩散系数的计算结果如图7e、f所示。三维多孔Ni3S2纳米管阵列电极在充电和放电过程中Na+的扩散系数均大于三维多孔Ni3S2纳米片阵列,这说明三维多孔Ni3S2纳米管可以提升电化学反应的动力学,提高Na+的扩散系数,这也进一步解释了比容量和倍率性能提升的原因。

3 结论

以自制的三维多孔镍为集流体,水热生长获得三维多孔Ni3S2,并通过控制水热反应的时间,获得不同微观形貌。结果显示,水热1 h得到纳米片阵列结构,水热4 h得到纳米片和纳米管的混合结构,水热10 h得到纳米管阵列结构,说明随着水热时间的延长,纳米片趋向卷曲成纳米管。三维多孔镍作为集流体可为Na+提供快速传输通道,并为Na+存储期间的体积变化提供自由空间,从而确保电极完整性和活性材料与集流体之间的良好电接触,可有效避免电化学极化的增加和容量衰减。纳米管可以提高活性物质的利用率,中空的纳米管可以更快速地传输电子和离子,同时更好保持其结构不被破坏,改善循环性能。电化学测试显示,三维多孔Ni3S2纳米管阵列(三维多孔Ni3S2-Ⅲ)具有最佳的电化学性能,首次可逆比容量为520.2 mA·h/g,首次库伦效率高达83.1%,循环200次后保持279.1 mA·h/g,容量保持率53.7%,远高于三维多孔Ni3S2纳米片阵列电极(26.6%)和三维多孔纳米片和纳米管复合形貌的Ni3S2电极(38.7%);即使在1.6 A/g下,仍可保持291.1 mA·h/g的高比容量,容量保持率达72.7%。这说明所制备的三维多孔硫化镍纳米管阵列电极在实际电池或其他相关储能应用中有广阔前景。

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