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1 Supporting Information Hierarchical Mesoporous Zinc-Nickel-Cobalt Ternary Oxide Nanowire Arrays on Nickel Foam as High Performance Electrodes for Supercapacitors Chun Wu a, Junjie Cai a, Qiaobao Zhang a, Xiang Zhou a, Ying Zhu a, Pei Kang Shen b, *, Kaili Zhang a, * a Department of Mechanical and Biomedical Engineering, City University of Hong Kong, 83 Tat Chee Avenue, Hong Kong b Department of Physics and Engineering, Sun Yat-sen University, Guangzhou, , China * Corresponding authors, address: kaizhang@cityu.edu.hk and stsspk@mail.sysu.edu.cn Figure S1, Figure S2, Figure S3, Figure S4, Figure S5, Figure S6, Figure S7, Figure S8, Figure S9 Table S1 References S-1

2 Figure S1 Schematic illustration of the as-fabricated ZNCO//AC asymmetric supercapacitor in 6 M KOH electrolyte S-2

3 (a) (b) 5 µm 3 µm (c) (d) 5 µm 3 µm (e) (f) 5 µm 3 µm Figure S2 Low and high-magnification SEM images of various ZNCO nanostructures on different substrates: (a) and (b) Si wafer, (c) and (d) Cu foam, (e) and (f) carbon cloth S-3

4 (a) (b) 50 µm 10 µm (c) (d) 50 µm 10 µm (e) (f) 50 µm 10 µm Figure S3 Low and high-magnification SEM images of ZNCO nanostructures prepared from different salts with the same ratios between Co, Ni and Zn at 130 o C for 5 h. (a) and (b) chlorates, (c) and (d) acetates, (e) and (f) sulfates. S-4

5 s s Figure S4 (a) Co 2p, (b) Ni 2p, (c) Zn 2p and (d) O 1s XPS spectra of ZNCO electrode material XPS analyses provide a careful investigation of the compositions of the ZNCO electrode materials. Obviously, the Co 2p spectrum in Fig. S4(a) presents two prominent peaks at ev for Co 2p 3/2 and ev for Co 2p 1/2, indicating the presence of Co 3+ oxidation state. 1 While a very intense, characteristic satellite at ~787.0 ev can be observed, the approximate position of which is indicated by the arrow of Fig. S4(a), demonstrating the existence of Co Moreover, the Ni 2p spectrum in Fig. S4(b) shows two obvious peaks at and ev, which is the Ni 2p 3/2 and 2p 1/2 binding energies, respectively. 2 The Ni 2p spectrum also can be fitted by considering two spin-orbit doublets and two shake-up satellites, in which the nickel 2p 3/2 spectra can be assigned to two distinct peaks, indicating the presence of S-5

6 both Ni 2+ and Ni 3+. 3,4 And the peak with binding energy value at in Fig. S4(c) is ascribed to Zn 2p 3/2, indicating the Zn 2+ oxidation state. 5,6 Furthermore, the high-resolution spectrum for the O 1s region (Fig. S4(d)) shows four oxygen contributions. The fitting peak of O 1 at ev and peak of O 2 at ev are attributed to the metal-oxygen bonds. 7 The well-resolved O 3 component corresponds to a high number of defect sites with low oxygen coordination in the material with small particle size. 8 Furthermore, the component O 4 at ev can be attributed to hydroxide oxygen in Co-O-OH, which is agreement with the peak at ev of Co 2p 3/2 binding energy. 9 From above results, the binding energy values at and ev of Co and ev of Ni can be assigned to CoOOH and NiOOH, 10,11 indicating that the energy storage mechanism of the ZNCO electrode originated mainly from Faradic redox reactions assigned to the M-O/M-O-OH, where M represents both Ni and Co ions. 12 Based on the Faradic redox reactions, the theoretical specific capacitance can be calculated as follows: The required amount of power used for electrolysis is of 1 mol active material is 1 F which is equal to C. For ZNCO electrode material, its molar mass is g mol -1 according to the EDX measurement (ZnNi 1.6 Co 3.5 O 7.5 ), however, the element taking part in the Faradic redox reactions are Co and Ni (Zn would not to be covered), molar mass is g mol -1, so theoretical faradaic capacitance is calculated as follows: C = Q U = ( )/404.2 U Where U is the voltage window, Q is electrical energy per 1 gram. When U is 0.5V in charge/discharge measurement, the theoretical faradaic capacitance is about F S-6

7 g -1, which is lower than that of the charge/discharge measurement, the reason may be that the obtained capacitance is the contribution of faradaic capacitance from redox reaction at interfaces and EDLC from high surface area of the porous electrode material. S-7

8 Figure S5 Capacitance retention and coulombic efficiency of the ZNCO electrode at a current density of 10 A g -1 S-8

9 Figure S6 Electrochemical performance of the ZNCO electrode: (a) and (c) CV curves of the ZNCO-3 and ZNCO-7 at different scan rates, (b) and (d) charge/discharge curves of the ZNCO-3 and ZNCO-7 under different current densities, (e) and (f) Comparisons of CV and charge/discharge curves among ZNCO-3, ZNCO and ZNCO-7 (With the temperature during the hydrothermal process were 3, 5 and 7 h, the samples were marked with ZNCO-3, ZNCO and ZNCO-7, respectively) S-9

10 (a) (b) 5 µm 5 µm Figure S7 SEM images of (a) ZNCO-3 and (b) ZNCO-7 S-10

11 Figure S8 (a) CV curves of AC electrode under different scan rates, (b) charge/discharge curves of AC electrode at different current densities, (c) specific capacitance of AC electrode at different current densities and (d) the Nyquist plots (the inset shows the expanded high-frequency region of the plot) of the AC electrode As presented in Fig. S8(a), a good double layer capacitive behavior in aqueous system on AC electrode is obtained. The charge/discharge curves of the AC electrode (Fig. S8(b)) are almost symmetrical isosceles lines, demonstrating that the AC material possesses stable electrochemical properties. The electrode delivers a specific capacitance of 247.9, 231.1, 219.3, and F g -1 at the current density of 1, 2, 3, 4 and 5 A g -1, respectively. The ac impedance spectrum depicted in Fig. S8(d) indicates a good capacitive behavior of the AC electrode. S-11

12 Figure S9 Capacitance retention and coulombic efficiency at more than 3000 charge/discharge cycle of the ZNCO//AC ASC device at a current density of 3 A g -1 S-12

13 Table S1 Comparison of specific capacitance of ZNCO electrode with different metal oxide electrodes reported in literature Electrode material Current Specific Ref. density capacitance ZnCo 2 O 4 /MnO 2 nanocones 1 A g F g NiCo 2 O 4 /MnO 2 nanoflakes 1 A g F g ZnCo 2 O 4 nanorods/nickel foam 1 A g F g NiCo 2 O nanoarrays 1 A g F g CoMn 2 O 4 nanowire 1 A g F g Mn-Ni-Co nanowires 1 A g F g Mn-Ni-Co composites 1 A g F g ZNCO nanowires 1 A g F g -1 This work References (1) Zhong J. H.; Wang A. L.; Li G. R.; Wang J. W.; Ou Y. N.; Tong Y. X. Co 3 O 4 /Ni(OH) 2 Composite Mesoporous Nanosheet Networks as a Promising Electrode for Supercapacitor Applications. J. Mater. Chem. 2012, 22, (2) Kim J. G.; Pugmire D. L.; Battaglia D.; Langell M. A. Analysis of the NiCo 2 O 4 Spinel Surface with Auger and X-ray Photoelectron Spectroscopy. Appl. Surf. Sci. 2000, 165, S-13

14 (3) Kamath P. V.; Therese G. H. A.; Gopalakrishnan J. On the Existence of Hydrotalcite-like Phases in the Absence of Trivalent Cations. J. Solid State Chem. 1997, 128, (4) Natile M. M.; Glisenti A. Surface Reactivity of NiO: Interaction with Methanol. Chem. Mater. 2002, 14, (5) Grohmann I.; Peplinski B.; Unger W. New Entries in the XPS Fingerprint Database for the Characterization of Precipitated Cu-Zn-Al Oxide Catalysts. Surf. Interface Anal. 1992, 19, (6) Long H.; Shi T.; Jiang S.; Xi S.; Chen R.; Liu S.; Liao G.; Tang Z. Synthesis of a Nanowire Self-assembled Hierarchical ZnCo 2 O 4 Shell/Ni Current Collector Core as Binder-free Anodes for High-performance Li-ion Batteries. J. Mater. Chem. A 2014, 2, (7) Choudhury T.; Saied S. O.; Sullivan J. L.; Abbot A. M. Reduction of Oxides of Iron, Cobalt, Titanium and Niobium by Low-energy Ion Bombardment. J. Phys. D: Appl. Phys. 1989, 22, (8) Jimenez V. M.; Fernandez A.; Espinos J. P.; Gonzalez-Elipe A. R. The State of the Oxygen at the Surface of Polycrystalline Cobalt Oxide. J. Electron Spectrosc. Relat. Phenom. 1995, 71, (9) Barr T. L. An ESCA Study of the Termination of the Passivation of Elemental Metals. J Phys. Chem. 1978, 82, S-14

15 (10) Biesinger M. C.; Payne B. P.; Grosvenor A. P.; Lau L. W. M.; Gerson A. R.; Smart R. S. C. Resolving Surface Chemical States in XPS Analysis of First Row Transition Metals, Oxides and Hydroxides: Cr, Mn, Fe, Co and Ni. Appl. Surf. Sci. 2011, 257, (11) Mansour A. N.; Melendres C. A. Characterization of Electrochemically Prepared γ-niooh by XPS. Surf. Sci. Spectra 1994, 3, (12) Wang H.; Gao Q.; Jiang L. Facile Approach to Prepare Nickel Cobaltite Nanowire Materials for Supercapacitors. Small 2011, 7, (13) Qiu K.; Lu Y.; Zhang D.; Cheng J.; Yan H.; Xu J.; Liu X.; Kim J. K.; Luo Y. Mesoporous, Hierarchical Core/shell Structured ZnCo 2 O 4 /MnO 2 Nanocone Forests for High-performance Supercapacitors. Nano Energy 2015, 11, (14) Li G.; Li W.; Xu K.; Zou R. J.; Chen Z. G.; Hu J. Q. Sponge-like NiCo 2 O 4 /MnO 2 Ultrathin Nanoflakes for Supercapacitor with High-rate Performance and Ultra-long Cycle Life. J. Mater. Chem. A 2014, 2, (15) Liu B.; Liu B.; Wang Q.; Wang X.; Xiang Q.; Chen D.; Shen G. New Energy Storage Option: Toward ZnCo 2 O 4 Nanorods/Nickel Foam Architectures for High-Performance Supercapacitors. ACS Appl. Mater. Interfaces 2013, 5, (16) Zhou W.; Kong D.; Jia X.; Ding C.; Cheng C.; Wen G. NiCo 2 O 4 Nanosheet Supported Hierarchical Core-shell Arrays for High-performance Supercapacitors. J. Mater. Chem. A 2014, 2, (17) Xu Y.; Wang X.; An C.; Wang Y.; Jiao L.; Yuan H. Facile Synthesis Route of Porous MnCo 2 O 4 and CoMn 2 O 4 Nanowires and Their Excellent Electrochemical Properties in Supercapacitors. J. Mater. Chem. A 2014, 2, S-15

16 (18) Li L.; Zhang Y.; Shi F.; Zhang Y.; Zhang J.; Gu C.; Wang X.; Tu J. Spinel Manganese-Nickel-Cobalt Ternary Oxide Nanowire Array for High-Performance Electrochemical Capacitor Applications. ACS Appl. Mater. Interfaces 2014, 6, (19) Luo J. M.; Gao B.; Zhang X. G. High Capacitive Performance of Nanostructured Mn-Ni-Co Oxide Composites for Supercapacitor. Mater. Res. Bull. 2008, 43, S-16

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