Template Synthesis of Shape-Tailorable NiS

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Template Synthesis of Shape-Tailorable NiS2 Hollow Prisms as High-performance Supercapacitor Materials Ziyang Dai, Xiaoxian Zang, Jun Yang, Chencheng Sun, Weili Si, Wei Huang, and Xiao-Chen Dong ACS Appl. Mater. Interfaces, Just Accepted Manuscript • Publication Date (Web): 26 Oct 2015 Downloaded from http://pubs.acs.org on October 27, 2015

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ACS Applied Materials & Interfaces

Template Synthesis of Shape-Tailorable NiS2 Hollow Prisms as High-performance Supercapacitor Materials Ziyang Dai, Xiaoxian Zang, Jun Yang, Chencheng Sun, Weili Si, Wei Huang*, Xiaochen Dong*

Key Laboratory of Flexible Electronics (KLOFE) & Institute of Advanced Materials (IAM), Jiangsu National Synergistic Innovation Center for Advanced Materials (SICAM), Nanjing Tech University (NanjingTech), 30 South Puzhu Road, Nanjing 211816, China.

ABSTRACT: Uniform NiS2 hollow nanoprisms have been controllably synthesized by a facial sacrificial template method including two-step refluxed reactions. The morphology of the hollow NiS2 prisms can be easily tailored by the low cost nickel complex template. With unique hollow structure, efficient electron and ion transport pathway as well as single crystal structure, the NiS2 hollow prisms electrode exhibits excellent pseudocapacitive performance in LiOH electrolyte. It can deliver a specific capacitance of 1725 F g-1 at a current density of 5 A g-1 and 1193 F g-1 even at a current density of 40 A g-1. Further more, the materials also present an amazing cycling stability, that is, the specific capacitance can increase from 1367 F g-1 to 1680 F g-1 after 10000 cycles of charge-discharge at the current density of 20 A g-1.

KEYWORDS: nickel disulfide; supercapacitor; hollow structure; shape-tailorable; prism

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1. INTRODUCTION Electrochemical capacitors, as known as supercapacitors, have attracted much more attention due to its potential advantages, such as high power density, fast charge-discharge capability, long cycle lifetime, and so on.1,2 Based on the type of electrochemical response, supercapacitors generally can be classified into two categories, electrical double layer capacitors (EDLCs) and pseudocapacitors.2-5 The electrode materials of EDLCs mainly use carbon-based materials, while the pseudocapacitors electrodes are usually made by transition metal oxides and conducting polymers. Among the two types of capacitors, the pseudocapacitors often have a higher specific capacitance than that of EDLCs because of the superior energy storage mechanism and the combination of the advantages of both mechanisms6-8. In the past decades, considerable efforts have been focused on the development of new electrode materials and various transition metal oxides have been studied, such as RuO29, 10, MnO211, 12, V2O513-16, Co3O417, 18, NiO19, 20, NiCo2O421-25, and so on. But except RuO2, most materials show poor conductivity, which limits their application on Pseudocapacitors. Although RuO2 can provide excellent conductivity and high capacitance, the high cost, rareness, and toxic nature restrict its wide application in supercapacitors26. Besides the above mentioned materials, silicon, metal hydroxide, metal nitride and metal phosphide are also developed as electrode materials for supercapacitors27-30. More recently, transition metal sulfides, especially nickel sulfides, cobalt sulfides and nickel cobalt sulfides have become most attractive class of supercapacitor electrode

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materials31-36 because of its high intrinsic electrical conductivity and theoretic capacitance37, 38. For example, Zhang et al.39 synthesized a tube-like NiCo2S4. Serving as supercapacitor electrode, its specific capacitance can reach 1048 F g-1 at the current density of 3.0 A g-1. But the cycling stability of NiCo2S4 still need to be enhanced (after 5000 cycles of charge-discharge at 10 A g-1, only 75.9% of the initial capacitance maintained). Pang et al.40 prepared the NiS2 nanocubes using microwave-assisted method, which presented excellent cycling stability (maintaining 93.4% of initial specific capacitance after 3000 cycles). However, the specific capacitance of the NiS2 nanocubes is poor (695 F g-1 at 1.25 A g-1). According to the reported literatures, it still is a challenge to meet the requirements of both specific capacitance and cycling stability for transition metal sulfides. To overcome this problem, the synthesis of porous materials with hollow architecture is one of the most effective approaches. The hollow nanostructure has relatively high specific area, which can lead to sufficient contact between electrode materials and the electrolyte to enhance the electrochemical performance. Zhang et al.41 obtained Co3O4 hollow structures by the calcinations of metal-organic frameworks (MOFs) ZIF-67 in air. The resulting hollow Co3O4 exhibits a specific capacitance of 1110 F g-1 at 1.25 A g-1. Jiang et al.42 reported a facial ion-exchange method to transfer ZIF-67 to Ni-Co LDH hollow structure with specific capacitance of 1203 F g-1 at 1 A g-1. However, the high cost and rare resource of metal elements for the synthesis of MOFs nanocrystals greatly limits its application. Here, a facile sacrificial template method is proposed to synthesize the shape-tailorable

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NiS2 hollow prisms with nickel acetate hydroxide complex as template43. And the NiS2 prisms with hollow structure are prepared according to the Kirkendall effect during the refluxed reactions. The supercapacitor electrode based on NiS2 hollow prisms presents high specific capacitance (1725 F g-1 at a current density of 5 A g-1 and 1193 F g-1 even at 40 A g-1) and outstanding cycling stability in LiOH electrolyte. 2. EXPERIMENTAL SECTION 2.1 Synthesis of sacrificial templates The nickel complex sacrificial template was synthesized by a reflux method. Its morphology was controlled by the concentration of Ni(NO3)2·6H2O. In a typical experiment, 0.75 g Ni(OAc)2·4H2O and 2.0 g PVP (K30) were added into 100 mL ethanol and refluxed for 4 hour under stirring36. After the reaction, the mixture from a clear green solution changed to a green turbid liquid. The precipitate was centrifuged and washed with ethanol for several times to obtain a green nickel complex powder (signed as NC-0). The number 0 refers to the amount (mmol) of Ni(NO3)2·6H2O added into the reaction solution. NC-0.2, NC-0.3 and NC-0.5 were synthesized by the addition of corresponding quantity of Ni(NO3)2·6H2O into the mixture under same procedure. 2.2 Synthesis of NiS2 hollow prisms With the nickel complex as sacrificial templates, the NiS2 hollow prisms were synthesized by the reflux reaction. Typically, 80 mg nickel complex templates and 0.11 g thioacetamide were dispersed into 100 ml ethylene glycol by sonification. Then, the mixture was transferred into a flask and reflux 1 hour at 200 oC. After cooling down to room temperature, the product was centrifuged and washed with ethanol for several

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times to obtain a black NiS2 powder. The corresponding NiS2 hollow prisms with different templates were signed as NS-0, NS-0.2, NS-0.3 and NS-0.5, respectively. 2.3 Characterization The morphology of the nickel complex templates and NiS2 hollow prisms were characterized by Field emission scanning electron microscopy (FESEM; Hitachi, S-4800, Japan) and transmission electron microscopy (TEM; JEOL, JSM-2100F). X-ray diffraction (XRD, Bruker D8 Advance) were determined by a powder XRD system (Bruker, AXS D8). The specific surface areas of the NiS2 hollow prisms were measured using a surface area analyzer (Tri-star 3020) and calculated by the Brunauer-Emmett-Teller (BET) method. 2.4 Electrochemical characterization All the electrochemical characterizations were carried out using a three-electrode system in 2 M aqueous LiOH electrolyte with a Ag/AgCl electrode as the reference electrode and Pt wire as the counter electrode. The NiS2 prisms working electrodes were prepared according to the reported literature44. The mass loading of the NiS2 prisms was about 1.0 mg cm-2. Cyclic voltammetry (CV), galvanostatic charge–discharge and electrochemical impedance spectroscopy (EIS, 1–100000 Hz) tests were carried out by a CHI 660D electrochemical workstation. The specific capacitance of the electrode was calculated from the charge-discharge curve based on the following equation: Cs = It / (m×∆V) Where Cs, I, t, m and ∆V refer to the specific capacitance (F g-1), discharge current

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density (A g-1), discharge time (s), mass of active materials and discharge potential range (V), respectively. 3. RESULTS AND DISCUSSION The morphologies of the nickel complex templates synthesized in different conditions were firstly examined by FESEM. As shown in Figure 1, all the samples have a prism morphology with different size and smooth surface. NC-0 (Figure 1a) presents a gather of short prisms (length/diameter ratio about 1.0) with uneven size distribution. With the increase of Ni(NO3)2·6H2O concentration, the size of the prisms becomes uniform and the length/diameter ratio increases obviously, as shown in Figure 1b-d. When the amount of Ni(NO3)2·6H2O increases to 0.5 mmol (NC-0.5), the sample has a length of about 800 nm and a width of about 350 nm (length/diameter ratio about 2.2, Figure 1d). XRD patterns (Figure S1) demonstrate that all the complexes have same crystal structure and good crystallinity.

Figure 1 FESEM images of nickel complex. (a) NC-0, (b) NC-0.2, (c) NC-0.3, and (d) 6


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NC-0.5. It is well known that the nickel acetate hydroxide can be synthesized by hydrolysis of salt in the solution along with the generation of OH- and H+. Then, the coordinate of OH- and CH3COO- with Ni2+ forms complex and the combination of H+ and CH3COOobtains CH3COOH. The reaction can be described by the following equation43: 5Ni(CH3COO)2 + 4H2O → Ni5(OH)2(CH3COO)8·2H2O + 2CH3COOH In the reaction system, PVP serves as the assistant for the formation of nanosized crystals with high quality. With the increase of Ni(NO3)2·6H2O, it produces more H+, which can greatly affect the formation and growth of the complex. And the growth speed towards the symmetric crystal orientation with rectangular pyramid ended is faster than the other four orientations. However, too high concentration of Ni(NO3)2·6H2O, for example, 0.8 mmol, could not lead to the formation of nickel complex due to the strong acidic condition. It can be concluded that the concentration of Ni(NO3)2·6H2O is very important for the growth of uniform nickel complex crystals.

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Figure 2 FESEM images of NiS2 hollow prisms. (a) NS-0, (b) NS-0.2, (c) NS-0.3, and (d) NS-0.5. Figure 2 shows the FESEM images of the NiS2 hollow prisms synthesized with different morphological nickel complex as sacrificial templates, named as NS-0, NS-0.2, NS-0.3 and NS-0.5, respectively). As expected, all the resulting materials present the similar morphologies with the corresponding nickel complex templates and the surface becomes much rougher compared to that of the templates, suggesting that the nickel complexes have reacted with the thioacetamide to form NiS2 nanoparticles. More importantly, the prisms became hollow structures due to the Kirkendall effect happened in the reaction45, 46. The nanoparticles stack tightly to form the outer shell and complete hollow structure.

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Figure 3 TEM images of NiS2 hollow prisms. (a) NS-0, (b) NS-0.2, (c) NS-0.3 and (d) NS-0.5. The inset of (d) shows the HR-TEM of NS-0.5. To get further insight into the hollow interior of the prisms, transmission electron microscope (TEM) images are shown in Figure 3. The TEM images further indicate that the prisms have hollow structure and the shell is composed by many irregular NiS2 nano-particles. The thicknesses of all the shells are about 40 nm, which is independent on the morphologies of the nickel complex templates. The high-resolution TEM (HR-TEM) image (the inset of Figure 3d) shows that the lattice spacing of the material is about 0.284 nm, which is well corresponding to the (200) plane of NiS2.

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Figure 4 (a) XRD patterns of different morphological NiS2 hollow prisms. (b) N2 adsorption–desorption isotherms of NiS2 hollow prisms (NS-0.5). Figure 4a shows the X-ray diffraction (XRD) patterns of the NiS2 hollow prisms synthesized using different Ni(NO3)2·6H2O concentration. All the products display relatively smooth lines and sharp characteristic peaks at 27.2o, 31.5o, 35.3o, 38.8o, 45.1o and 53.5o, corresponding to (111), (200), (210), (211), (220) and (311) plane, respectively. All the peaks in the XRD patterns can be well indexed to NiS2 (JCPDS no. 65-3325). The relative peak intensities of the materials also indicate that the crystal structure is independent on the morphology of nickel complex template. Figure 4b displays the nitrogen adsorption-desorption isotherm of NS-0.5. The shape of the adsorption-desorption curves indicates that the NiS2 hollow prisms are not mesoporous material. The calculated BET surface area is about 24.2 m2 g-1. The formation of the non-mesoporous structure may be ascribed to the good crystallization of the materials, which lead to the formation of a compact solid.

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Figure 5 Electrochemical characterizations of the NS-0.5 hollow prisms. (a) CV curves of NS-0.5 hollow prisms at different scan rates. (b) Charge-discharge curves of NS-0.5 hollow prisms at different current densities. (c) Comparison of specific capacitances versus different current densities for NS-0.5 hollow prisms. (d) Cycling stability of NS-0.5 hollow prisms at a current density of 20 A g-1. The inset shows the charge-discharge curve at current density of 20 A g-1. The electrochemical performance the NiS2 hollow prisms is measured by cyclic voltammogram (CV) and galvanostatic charge-discharge measurements in 2.0 M aqueous LiOH electrolyte. Due to the similar electrochemical performance of the NiS2 hollow prisms with different morphologies, here we present the electrochemical performance of NS-0.5. Figure 5a shows the CV curves of NS-0.5 hollow prisms at different scan rate with the potential window from -0.4 to 0.8 V. A pair of redox peaks

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attributed to the reversible Faradaic reactions of the electrode materials can be observed clearly. Due to the efficient ions diffusion from the electrolyte to the electrode material at low scan rate, the potential of the redox peaks is lower at a low scan rate. The same area of the anodic and cathodic curve also indicates a quasi-reversible reaction happened in the electrode. Figure 5b presents the charge-discharge curves evaluated at different current densities. The calculated results indicate the specific capacitances of the material are 1725, 1584, 1489, 1411, 1293, and 1193 F g-1 at current densities of 5, 10, 15, 20, 30, 40 A g-1, respectively, which is better than that of NiS2 reported elsewhere.40, 47, 48 The large specific capacitance can be attributed to unique hollow structure. Figure 5c shows the comparison of the specific capacitances versus different current densities for NS-0.5 hollow prism. It indicates that the specific capacitance decreases with the increase of current density. But about 70% of the specific capacitance of NiS2 hollow prism is still retained when the current density increases from 5 to 40 A g-1, suggesting efficient surface redox reactions can take place on the NiS2 hollow prisms. Figure 5d shows the cycling stability of the NS-0.5 hollow prism examined at a constant current density of 20 A g-1. After 10000 cycles charge-discharge measurements, the specific capacitance increases gradually from 1367 F g-1 to 1680 F g-1 (growth about 22.9%). And the highest specific capacitance is 1716 F g-1 at the 6600th cycle. This phenomenon may come from the fact that the original activation process makes the intercalation and de-intercalation of electrochemical species more complete49. When the activation process goes, the electrolyte may permeate into the inner of the hollow structure gradually. More additional area would be utilized to form

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materials-electrolyte interfaces. It indicates that the NiS2 hollow prism possesses excellent cycling stability, making it potential electrode materials for long-life supercapacitors.

Figure 6 (a) CV curves at scan rate 20 mV s-1, and (b) Nyquist plots of the NS-0.5 electrode before and after 10000 charge-discharge cycles. Figure 6a shows the CV curves of NS-0.5 hollow prisms electrode before and after 10000 charge-discharge cycles. It can be seen obviously that the CV curves before and after 10000 cycles are similar, demonstrating the excellent cycling stability of the hollow structured materials. Figure 6b presents the Nyquist plots before and after 10000 charge-discharge cycles, indicating a good conductivity of the electrode with an equivalent series resistance of 0.61 and 0.69 Ω, respectively. No obvious semicircles appearance at high frequency range demonstrates very small charge-transfer resistance of the electrode50. The small change of the equivalent series resistance further confirms the excellent stability of the NiS2 hollow prisms and highly reversible redox reaction. 4. CONCLUSIONS In conclusion, morphology tailorable NiS2 hollow prisms are synthesized with the nickel complex as sacrificial templates. The resulting NiS2 can deliver a specific 13



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capacitance of 1725 F g-1 at a current density of 5 A g-1 and 1193 F g-1 even at 40 A g-1. Due to its unique hollow interior and high conductivity, the NiS2 hollow prisms also present an excellent cycling stability, 22.9% increase is achieved after 10000 cycles. These make the NiS2 hollow prism is a promising candidate for high performance and long cycle life supercapacitors. ASSOCIATED CONTENT Supporting Information Available: XRD patterns of Nickel complexes with different morphologies, pore size distribution of NiS2 hollow prisms, comparison of specific capacitances versus different current densities for the hollow prisms and another 10000 times cycling stability of NS-0.5 hollow prisms at a current density of 20 A g-1. AUTHOR INFORMATION Corresponding Author E-mail: [email protected]; [email protected]. Notes The authors declare no competing financial interest. ACKNOWLEDGEMENTS The project was supported by Key University Science Research Project of Jiangsu Province (15KJA430006), Jiangsu Provincial Founds for Distinguished Young Scholars (BK20130046), the NNSF of China (21275076, 61328401), Program for New Century Excellent Talents in University (NCET-13-0853), Qing Lan Project, Synergetic Innovation Center for Organic Electronics and Information Displays, the Priority Academic Program Development of Jiangsu Higher Education Institutions

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(PAPD).

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Hierarchitectures:

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to

Achieve

Nickel

Phosphide

Nanoparticles

with

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Template Synthesis of Shape-Tailorable NiS

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