多孔纳米Ni3S2的制备及其电化学性能研究

通过两步液相法合成了生长在泡沫镍上的具有多孔结构的纳米Ni3S2,分别用XRD,SEM对材料进行了物相和微观形貌表征,并利用电化学工作站测试了其电化学性能.实验结果表明,利用(NH4)2S2O8氧化泡沫镍时反应温度应在70℃以上,反应时间在3 h以上,合成的电极材料表面呈多孔薄层的三维结构,孔径大小分布广,并且薄层之间没有互相重叠的现象.循环伏安曲线及恒流充放电曲线显示,Ni3S2电极材料具有良好的可逆性,明显的电池电容特点.当电流密度增大10倍时,比电容只下降了35.5%,具有良好的倍率性能.由交流阻抗谱图可知,高频区电阻率为0.91Ω,低频区直线斜率大,表明材料具有良好的导电性.当电极材料充放电次数从0增加到1 000次时,比电容由1 015.4 F g^-1增加到1 222.7 F g^-1,增加了20.4%,表明制备的Ni3S2具有良好的循环稳定性.

Ni3S2/SiC复合电极的制备及光电催化性能研究

采用电沉积法在碳化硅纳米线薄膜上沉积镍硫合金,制备碳化硅纳米线/镍硫合金薄膜复合电极,采用 场发射扫描电子显微镜（ FESEM）、 X射线衍射（ XRD）、阴极极化曲线（LSV）等分析测试方法对该薄膜的形貌、结构 和电化学性能进行了表征.结果表明：镍硫合金沉积层主要以Ni3S2 结晶态的形式覆盖在碳化硅纳米线薄膜表面,纳米线沉积合金前直径约80 nm ,沉积后增大到100nm左右.重点研究了Ni3S2/SiC 电极在光照前后的光电性能, 在1MKOH 溶液中的LSV曲线测试表明： Ni3S2/SiC 电极的起始电压比SiC 电极减小约200mV ;在光照下Ni3S2/ SiC电极起始电压比无光照下降低约400mV （电流密度为9 mA·cm^-2）,计时电位曲线测试表明电极具有很好的稳定性.

Ni3S2@碳纳米管复合材料的制备及其储钠性能

采用一步固相煅烧工艺制备了碳纳米管原位封装Ni3S2纳米颗粒(Ni3S2@CNT),并研究了其作为钠离子电池(SIBs)负极材料的电化学性能.通过X射线衍射(XRD)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)、循环伏安测试、恒流充放电以及交流阻抗等研究了Ni3S2@CNT的物相结构、形貌特征以及电化学性能.电化学测试表明,材料在100 mA·g^(-1)电流密度下,放电容量可以达到541.6 m Ah·g^(-1),甚至在2000 mA·g^(-1)的大电流密度下其放电比容量也可以维持在274.5 m Ah·g^(-1).另外,材料在100 mA·g^(-1)电流密度下,经过120周充放电循环后其放电和充电比容量仍然可以保持在374.5 m Ah·g^(-1)和359.3 m Ah·g^(-1),说明其具有良好倍率性能和循环稳定性能.良好的电化学性能归因于这种独特的碳纳米管原位封装Ni3S2纳米颗粒结构.碳纳米管不但可以提高复合材料的导电性,也可以缓冲Ni3S2纳米颗粒在反复充放电过程中产生的体积膨胀效应,明显改善了Ni3S2@CNT负极复合材料的电化学性能.

Graphene-immobilized flower-like Ni3S2 nanoflakes as a stable binder-free anode material for sodium-ion batteries

A binder-free Ni3S2 electrode was prepared directly on a graphene-coated Ni foam （G/Ni） substrate through surface sulfiding of substrate using thiourea as the sulfur source in this work. The Ni3S2 showed a flower-like morphology and was uniformly distributed on the G/Ni surface. The flower-like Ni3S2 was composed of cross-arrayed nanoflakes with a diameter and a thickness of 1-2 μm and -50 nm, re- spectively. The free space in the flowers and the thin feature of Ni3S2 buffered the volume changes and relieved mechanical strain during re- peated cycling. The intimate contact with the Ni substrate and the fixing effect of graphene maintained the structural stability of the Ni3S2 electrode during cycling. The G/Ni-supported Ni3S2 maintained a reversible capacity of 250 mAh·g^-1 after 100 cycles at 50 mA·g^-1, demon- strating the good cycling stability as a result of the unique microstructure of this electrode material.

Ni3S2微纳米结构超疏水表面的制备及耐蚀性能

随着表面科学和仿生学的迅速发展,超疏水材料的制备和研究已成为当下研究的热点,其性能优异,具有十分广阔的应用前景。本工作采用水热反应法在泡沫镍基体上直接生长Ni3S2微纳米复合结构,经过十四酸修饰后获得性能优良的超疏水表面。实验探究了水热反应温度和反应时间对水滴在超疏水表面接触角的影响。研究发现,水热反应温度为180℃、反应时间为6 h的条件下获得的水热反应层表面的水滴接触角达到最大值160.28°。采用扫描电子显微镜观察超疏水试样表面的微观结构,发现在基体表面生长了一层交错排列的锥状结构。利用X射线衍射仪和能谱仪对水热反应层表面进行物相及表面化学成分分析发现,与泡沫镍基体相比,水热反应层表面除了存在Ni相外还形成了新的Ni3S2相。对获得的超疏水试样进行性能测试,发现利用该方法制备的超疏水材料具有良好的耐酸碱性和耐电化学腐蚀特性。

一步水热法制备Ni3S2纳米空心球及其在超级电容器中的应用

将四水合醋酸镍和L-半胱氨酸分别作为镍源和硫源,采用一步水热法成功制备出了Ni3S2纳米空心球材料.分别利用X射线衍射仪、X射线光电子能谱仪、扫描电子显微镜以及透射电子显微镜等仪器分析材料的形貌、组分和物相结构.结果表明:制备出的Ni3S2为尺寸均一的空心球,直径约300 nm,且具有良好的分散性.将制备出的Ni3S2压在泡沫镍上制成电极,研究其超级电容器的性能,结果显示:Ni3S2纳米空心球具有优良的倍率性能和循环性能,这归因于材料优异的稳定性和特定的空心球状结构,不仅为电极反应提供了丰富的活性位点,还有效缩短了电子以及离子的扩散路径.

Ni3S2 nanorods growing directly on Ni foam for all-solid-state asymmetric supercapacitor and efficient overall water splitting

Transition metal compounds are attractive for their significant applications in supercapacitors and as non-noble metal catalysts for electrochemical water splitting.Herein,we develop Ni3 S2 nanorods growing directly on Ni foam,which act as multifunctional additive-free Ni3 S2@Ni electrode for supercapacitor and overall water splitting.Based on PVA-KOH gel electrolyte,the assembled all-solid-state Ni3 S2@Ni//AC asymmetric supercapacitor delivers a high areal energy density of 0.52 mWh cm^-2 at an areal power density of 9.02 MW cm^-2,and exhibits an excellent cycling stability with a capacitance retention ratio of 89%after 10000 GCD cycles at a current density of 30 mA cm^-2.For hydrogen evolution reaction and oxygen evolution reaction in 1 M KOH,Ni3 S2@Ni electrode achieves a benchmark of 10 mA cm^-2at overpotentials of 82 mV and 310 mV,respectively.Furthermore,the assembled Ni3 S2@Ni‖Ni3 S2@Ni electrolyzer for overall water splitting attains a current density of 10 mA cm^-2 at 1.61 V.The in-situ synthesis of Ni3 S2@Ni electrode enriches the applications of additive-free transition metal compounds in high-performance energy storage devices and efficient electrocatalysis.

溶剂热技术制备Ni3S2纳米粉体

以硝酸镍和硫脲作镍源及硫源，以乙二醇作溶剂，采用溶剂热技术成功地制备了Ni3S2纳米粉体。用X射线粉末衍射（XRD）和透射电镜（TEM）对Ni3S2粉体的结构及形貌进行表征，结果表明反应温度和物料配比是影响Ni3S2粉体的结构和形貌的重要因素。

Correction to:High‑Index‑Faceted Ni3S2 Branch Arrays as Bifunctional Electrocatalysts for Efficient Water Splitting

In the original publication,Figure S4 is an ancillary image to compare the specific surface areas of TiO2/Ni3S2 and Ni3S2 samples and it was incorrectly published.To better serve our readers,the correct figure is provided in this correction.The BET values are correct and unaffected.The corresponding figure caption,data analysis and conclusions are not affected and thus not to be changed.The authors would like to apologize for any inconvenience caused.

Facile synthesis of Co and Ce dual-doped Ni3S2 nanosheets on Ni foam for enhanced oxygen evolution reaction

Nano Research volume 13,pages2130–2135(2020)Cite this article 376 Accesses 2 Citations Metrics details Abstract Developing efficient and stable oxygen evolution reaction(OER)electrocatalysts via doping strategy has well-documented for electrochemical water splitting.Herein,a homogeneous structure(denoted as Co/Ce-Ni3S2/NF)composed of Co and Ce dual doped Ni3S2 nanosheets on nickel foam was synthesized by a facile one-step hydrothermal method.Co and Ce dopants are distributed inside the host sulfide,thereby raising the active sites and the electrical conductivity.Besides,the CeOx nanoparticles generated by part of the Ce dopants as a cocatalyst further improve the catalytic activity by adding defective sites and enhancing the electron transfer.As a consequence,the obtained Co/Ce-Ni3S2/NF electrode exhibits better electrocatalytic activity than single Co or Ce doped Ni3S2 and pure Ni3S2,with low overpotential(286 mV)at 20 mA-cm^−2,a small Tafel slope and excellent long-term durability in strong alkaline solution.These results presented here not only offer a novel platform for designing transition metal and lanthanide dual-doped catalysts,but also supply some guidelines for constructing catalysts in other catalytic applications.

Graphene as an intermediary for enhancing the electron transfer rate： A free-standing Ni3S2@graphene@CogSs electrocatalytic electrode for oxygen evolution reaction

A highly active and stable oxygen evolution reaction （OER） electrocatalyst is critical for hydrogen production from water splitting. Herein, three-dimensional Ni3Sa@graphene@Co9S8 （Ni3S2@G@Co9S8）, a sandwich- structured OER electro-catalyst, was grown in situ on nickel foam; it afforded an enhanced catalytic performance when highly conductive graphene is introduced as an intermediary for enhancing the electron transfer rate and stability. Serving as a free-standing electrocatalytic electrode, Ni3S2@G@Co9S8 presents excellent electrocatalytic activities for OER： A low onset overpotential （2 mA·cm^-2 at 174 mV）, large anode current density （10 mA·cm^-2 at an overpotential of 210 mV）, low Tafel slope （66 mV·dec^-1）, and predominant durability of over 96 h （releasing a current density of N 14 mA·cm^-2 with a low and constant overpotential of 215 mV） in a 1 M KOH solution. This work provides a promising, cost-efficient electrocatalyst and sheds new light on improving the electrochemical performance of composites through enhancing the electron transfer rate and stability by introducing graphene as an intermediary.

Sulfur-deficient Co9S8/Ni3S2 nanoflakes anchored on N-doped graphene nanotubes as high-performance electrode materials for asymmetric supercapacitors

In this paper,Co9S8/Ni3S2 nanoflakes(NFs)with sulfur deficiencies were grown in-situ on N-doped graphene nanotubes(NGNTs).They were successfully prepared through electrodeposition followed by hydrogenation treatment,which is able to act as a self-supported electrode for asymmetric supercapacitors(ASCs).Combining the defect-rich active materials with highly conductive skeletons,the hybrid electrode N-GNTs@sd-Co9S8/Ni3S2NFs show ultrahigh specific capacity of^304 mA hg^-1 and prominent rate capability(capacity retention ratio of^85%even at 100 Ag^-1),and deliver a long cycling lifespan of^1.9%capacitance loss after 10000 cycles.In addition,an ASC was constructed using the as-synthesized composite electrode as the positive electrode and active carbon(AC)as the negative electrode.The fabricated device shows a high energy density of^45.1 Wh kg^-1 at^3.4 kW kg^-1 and superior cycling stability.This work substantiates a smart strategy to fabricate novel composite electrode materials for next-generation supercapacitors by incorporating riched deficiencies into nanostructures.

High performance hybrid supercapacitor based on hierarchical MoS2/Ni3S2 metal chalcogenide

Recently,because of excellent electrical conductivities and many active sites,transition metal sulfides have been utilized as efficient electrodes for supercapacitors.Herein,we synthesize hierarchical MoS2/Ni3S2 structures grown on nickel foam by a facile one-pot hydrothermal process.The as-fabricated asymmetric hybrid capacitor based on hierarchical MoS2/Ni3S2 electrode exhibit a specific capacitance of^1.033 C/cm2 at1 mA/cm2.Furthermore,the hybrid capacitor unveils an energy density of 35.93 m W h/cm3 at a power density of 1064.76 mW/cm3.The observed results clearly revealed that the synthesized MoS2/Ni3S2 structure might be used as potential electrode material for future energy storage devices.

Fe-doped and sulfur-enriched Ni3S2 nanowires with enhanced reaction kinetics for boosting water oxidation

Exploring cost-effective and highly-active oxygen evolution reaction(OER)electrocatalysts is a pressing task to propel water electrolysis for green hydrogen production.Herein,we constructed a class of Fe-doped and Senriched Ni_(3)S_(2)nanowires electrocatalysts for optimizing the target intermediates adsorption to decrease the OER overpotentials at various current densities.The optimal Ni_(3)S_(2)-1.4%Fe electrocatalyst possesses the most active sites and exhibits an ultralow overpotential of 190 mV at 10 mA cm^(-2) with an excellent stability of>60 h,exceeding the majority of recently-reported Ni_(3)S_(2)-based electrocatalysts.The trivalence Fe-doping not only reduces the electron density of the Ni center,but also enables the sulfur enrichment on the Ni_(3)S_(2) surface,which greatly improves the intrinsic activity and the number of target intermediates(*OOH).A novel methanol-assisted electrochemical evaluation further reveals that the Ni_(3)S_(2)-1.4%Fe electrocatalyst demonstrates a weaker binding ability to*OH with the rapid generation of*OOH species,and thus gives a lower apparent activation energy compared with the surface sulfur reduced ones.This work provides a new perspective for regulating the adsorption of intermediates through doping strategy.

硫化镍试金扣成分探讨(英文)

实验对比了熔剂中硫和镍的质量(mS和mNiO)变化对镍扣质量(mbutton)的影响,结果表明:mbutton主要受mNiO的控制,mS的变化对其影响则较小。采用X射线衍射(XRD)分析了6个不同mS、mNiO的熔剂所制备镍扣的矿物成分,结果显示:镍扣矿物成分单一,以Ni3S2为主,含少量NixS6,不含NiS、Ni3S4和NiS2等矿物。改变所加入的mS和mNiO,镍扣的矿物组成并不改变,仅是Ni3S2和NixS6相对含量发生变化。

溶剂热技术制备硫化镍纳米粉体

分别以硝酸镍和硫脲作镍源及硫源、以乙二醇作溶剂,采用溶剂热技术成功地制备了Ni3S2,α-NiS和NiS2粉体。研究结果显示原料的配比及反应温度能够影响产物的物相组成及形貌。

纳米多孔Ni、Ni_(3)S_(2)/Ni复合电极的制备及其电催化析氢性能

采用脱合金化和水热合成的方法制备纳米多孔Ni和纳米多孔Ni_(3)S_(2)/Ni复合电极。通过N2吸附-脱附测试、XRD、SEM、TEM等方法表征电极的孔径分布、物相和微观结构。在1 mol·L^(-1)的NaOH溶液中,运用线性扫描伏安(LSV)曲线、交流阻抗(EIS)谱图、恒电流电解法等测试电极的电催化析氢性能。结果表明:在电流密度为50 mA·cm^(-2)时,与纳米多孔Ni相比,Ni_(3)S_(2)/Ni合金具有更低的析氢过电位以及更高的析氢活性,同时纳米多孔Ni_(3)S_(2)/Ni复合电极具有更低表观活化能和电子转移阻抗,进一步明确了过渡金属硫化物对电催化析氢性能的特殊贡献。

不同浓度不溶性镍化物与人肺癌A549细胞内Cap43、HIF-1α关系的研究

目的探讨不同浓度不溶性镍化物对人肺癌A549细胞内钙激活蛋白43(Cap43)、缺氧诱导因子1α(HIF-1α)的影响。方法用不同浓度的水不溶性二硫化三镍(Ni3S2)处理人肺癌A549细胞,24h后用间接免疫荧光法观察染毒后细胞内Cap43与HIF-1α蛋白表达的变化。结果通过细胞免疫荧光法发现,随着处理物浓度的增加,细胞内Cap43、HIF-1α蛋白含量均增加。结论不溶性镍化物可以诱导人肺癌A549细胞内Cap43、HIF-1α蛋白含量的增加。

含氯离子电解质体系Ni_3S_2阳极溶解热效应

本文首次报导了用电化学量热方法测定的Ｎｉ３Ｓ２在含氯离子电解质体系中阳极溶解过程热效应，并据此推测了阳极溶解过程中可能发生的化学反应，所得结果与文献中报导的现代物理检测结果相符合。

锂硫电池正极材料Ni_3S_2/C/S的制备及电化学性能

以配合物为模板和镍源,蔗糖为碳源,通过一步高温法获得片状硫化镍/炭(Ni_3S_2/C)材料。采用XRD,SEM,FT-IR,XPS对制备的材料进行表征。以此材料作为锂硫电池正极活性物质的载体并进行充放电等测试,结果表明,在0.2C的倍率下,硫电极首次放电容量为1392.7mAh/g,循环100次后的放电容量仍然保持有1009mAh/g,表现出较高的放电比容量和良好的循环稳定性。进一步研究表明Ni_3S_2在改善硫电极性能和抑制穿梭效应发挥重要作用。