Dominating Role of Aligned MoS 2 /Ni 3 S 2. Nanoarrays Supported on 3D Ni Foam with. Hydrophilic Interface for Highly Enhanced
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1 Supporting Information Dominating Role of Aligned MoS 2 /Ni 3 S 2 Nanoarrays Supported on 3D Ni Foam with Hydrophilic Interface for Highly Enhanced Hydrogen Evolution Reaction Jiamu Cao a, Jing Zhou a, Yufeng Zhang a,b,*, Yuxi Wang a, Xiaowei Liu a,b a MEMS Center, Harbin Institute of Technology, , China. b Key Laboratory of Micro-systems and Micro-Structures Manufacturing, Ministry of Education, , China. Corresponding author address: yufeng_zhang@hit.edu.cn S-1
2 Table S1. Comparison of the HER performances of representative non-platinum electrocatalysts in alkaline solution. Electrocatalyst (morphology) η onset (mv) η 10 (mv) η 20 (mv) Tafel slope (mv/dec) Electrolyte Ref. 3D MoS 2 /Ni 3 S 2 /Ni composite M KOH This work Ni 3 S 2 /CNTs M KOH (21) MoS 2 /graphene/ni foam 25 > M KOH (30) NiSe 2 nanosheets M KOH (31) NiCo 2 S 4 /Ni foam M KOH (32) NiSe nanowires/ni foam M KOH (33) Ni 3 S 2 nanosheet arrays/ni foam V-doped Ni 3 S 2 nanowire arrays M KOH (34) M KOH (23) MoS 2 /Ni 3 S 2 heterostructures M KOH (37) NiO nanotube hybrids carbon M KOH (38) NiCo 2 S 4 nanowire arrays/ni foam M KOH (39) Ni-Co-P hollow nanocubes ~ M KOH (35) Ni-Fe/nanocarbon M KOH (36) S-2
3 Figure S1. Photographs of Ni foam without and with the MoS 2 /Ni 3 S 2 coating. Figure S1 presents photographs of the Ni foam surface before and after MoS 2 /Ni 3 S 2 growth by the hydrothermal method. Once the MoS 2 /Ni 3 S 2 nanoarrays had grown on the Ni foam, the foam surface became totally black. This suggests the uniform and complete coverage of MoS 2 /Ni 3 S 2 on the Ni foam with no exposed Ni surface. S-3
4 Figure S2. Photograph of the 3D MoS 2 /Ni 3 S 2 /Ni after ultrasonication in solution for 10 min. The robust mechanical adhesion of the nanostructure is confirmed by an ultrasonication test. Figure S2 shows that no material loss occurred after ultrasonication in solution for 10 min. S-4
5 Figure S3. Photographs of the electrode surfaces of Ni foam and Ni3S2/Ni. Figure S4. Low-magnification (a) and high-magnification (b) SEM images of Ni3S2/Ni. S-5
6 Figure S5. XPS spectra of (a) Ni 2p and (b) S 2p of Ni 3 S 2 /Ni. XPS spectra were performed to analyze the surface elements and their valence state of the 3D Ni 3 S 2 /Ni composite, as shown in Figure S5. The binding energy at ev in Ni 2p 3/2 and ev in Ni 2p 1/2 corresponds to the spin-orbit characteristics of Ni 2+, and the binding S-6
7 energy at ev in Ni 2p 3/2 and ev in Ni 2p 1/2 agree with the characteristics of Ni 3+, accompanied by satellite peaks in the Figure S5 (a). S1 The peak at ev is the characteristic peak of Ni 3 S 2. In Figure S5 (b), the peaks at ev (S 2p 1/2 ) and ev (S 2p 3/2 ) are associated with the typical metal-sulfur bonds. S2 Figure S6. Photograph of the Ni 3 S 2 /Ni after ultrasonication in solution for 10 min. S-7
8 Figure S7. Polarization curves of the Ni foam, MoS 2 /Ni, Ni 3 S 2 /Ni, and 3D MoS 2 /Ni 3 S 2 /Ni composite. S-8
9 Figure S8. Durable operation of the 3D MoS 2 /Ni 3 S 2 /Ni and Pt foil at 10 ma cm -2 in an alkaline electrolyzer (1 M KOH solution). Figure S9. Photos of the Pt foil (a) and 3D MoS 2 /Ni 3 S 2 /Ni (b) during the durable operation at 10 ma cm -2 in an alkaline electrolyzer (1 M KOH solution). S-9
10 Figure S10. The long-term stability test result at 20 ma cm -2 in 1 M KOH. Figure S11. Time-dependent current density curves of 3D MoS 2 /Ni 3 S 2 /Ni at a static potential of 76mV versus RHE for 24 h in 1 M KOH. S-10
11 Figure S12. The low-magnification (a) and high-magnification (b) SEM images of 3D MoS 2 /Ni 3 S 2 /Ni after a long-term test. It depicted that the original morphology of the composite was well preserved. Figure S13. The Nyquist plots of bare Ni foam, Ni 3 S 2 /Ni, and 3D MoS 2 /Ni 3 S 2 /Ni electrodes. The inset is an equivalent circuit. S-11
12 The inset of Figure S13 gives the equivalent circuit, which is applied to a circuit model to fit the impedance data. This equivalent circuit is composed of the solution resistance (Rs), constant phase element (CPE), and charge transfer resistance (Rct). S3 Figure S14. Contact angle photograph of surface modified 3D MoS 2 /Ni 3 S 2 /Ni composite. The contact angle of the surface modified 3D MoS 2 /Ni 3 S 2 /Ni composite was 152 Figure S15. Potentiodynamic polarization curves for Ni foam, 3D MoS 2 /Ni 3 S 2 /Ni composite and surface modified 3D MoS 2 /Ni 3 S 2 /Ni composite in 3.5 wt.% NaCl solution. S-12
13 The 3D MoS 2 /Ni 3 S 2 /Ni composite was immersed in 0.5 wt.% fluoroalkyl silane (FAS) ethanol solution for 1 h at room temperature, then heated at 120 for 1 h to obtain a superhydrophobic surface (Figure S14). As shown in Figure S15, the potentiodynamic polarization curves are tested after the as-prepared samples were immersed in 3.5 wt.% NaCl aqueous solution for 2 h. The corrosion current density of untreated 3D MoS 2 /Ni 3 S 2 /Ni composite and Ni foam are A/cm 2 and A/cm 2. Compared with Ni foam, the larger corrosion current density of 3D MoS 2 /Ni 3 S 2 /Ni composite may be on account of its unique structure which has a very large specific surface area. After the surface modification, the surface modified 3D MoS 2 /Ni 3 S 2 /Ni composite (SM MoS 2 /Ni 3 S 2 /Ni) formation of the superhydrophobic interface on the composite surface, the corrosion current density decreases to A/cm 2, indicating that the superhydrophobic interface which in the surface modified unique structured 3D MoS 2 /Ni 3 S 2 /Ni composite reduces the S4, S5 corrosion rate. S-13
14 SUPPLEMENTARY REFERENCES (S1) Chang Y.; Sui Y.; Qi J.; Jiang L.; He Y.; Wei F.; Meng Q.; Jin Y. Facile Synthesis of Ni 3 S 2 and Co 9 S 8 Double-size Nanoparticles Decorated on rgo for High-performance Supercapacitor Electrode Materials. Electrochim. Acta. 2017, 226, (S2) Wang J.; Liu J.; Yang H.; Chao D.; Yan Jia.; Savilove S. V.; Lin J.; Shen Z. MoS 2 Nanosheets Decorated Ni 3 S 2 Coaxial Nanofibers: Constructing an Ideal Heterostructure for Enhanced Na-ion Storage. Nano Energy 2016, 20, (S3) Zhuang M.; Ou X.; Dou Y.; Zhang L.; Zhang Q.; Wu R.; Ding Y.; Shao M.; Luo Z. Polymer-Embedded Fabrication of Co 2 P Nanoparticles Encapsulated in N,P-Doped Graphene for Hydrogen Generation. Nano Lett. 2016, 16, (S4) Wang P.; Zhang D.; Lu Z. Advantage of Super-hydrophobic Surface as a Barrier Against Atmospheric Corrosion Induced by Salt Deliquescence. Corros. Sci. 2015, 90, (S5) Xie Z. H.; Li D.; Skeete Z.; Sharma A.; Zhong C. J. Nanocontainer-Enhanced Self-Healing for Corrosion-Resistant Ni Coating on Mg Alloy. ACS Appl. Mater. Interfaces 2017, 9, S-14
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