Formation of Hierarchical Structure Composed of (Co/Ni)Mn-LDH Nanosheets on MWCNT Backbones for Efficient Electrocatalytic Water Oxidation

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1 Supporting Information Formation of Hierarchical Structure Composed of (Co/Ni)Mn-LDH Nanosheets on MWCNT Backbones for Efficient Electrocatalytic Water Oxidation Gan Jia, Yingfei Hu, Qinfeng Qian, Yingfang Yao, Shiying Zhang, Zhaosheng Li, *, Zhigang Zou Collaborative Innovation Center of Advanced Microstructures, National Laboratory of Solid State Microstructures, College of Engineering and Applied Sciences, 22 Hankou Road, Nanjing , People's Republic of China, Hunan Key Laboratory of Applied Environmental Photocatalysis, Changsha University, Changsha, People s Republic of China *Corresponding author: Prof. Zhaosheng Li zsli@nju.edu.cn S-1

2 Figure S1. Typical FESEM images of Co 2 Mn-LDH/MWCNT (A), Co 3 Mn-LDH/MWCNT (B), Co 5 Mn-LDH/MWCNT (C) and Co 7 Mn-LDH/MWCNT (D). S-2

3 Figure S2. Typical FESEM images of Ni 2 Mn-LDH/MWCNT (A), Ni 3 Mn-LDH/MWCNT (B), Ni 5 Mn-LDH/MWCNT (C) and Ni 7 Mn-LDH/MWCNT (D). S-3

4 Table S1. EDS analysis results for the Co/Mn and Ni/Mn atomic ratios in CoMn-LDH/MWCNT and NiMn-LDH/MWCNT, respectively. Co 2 Mn-LDH/ MWCNT Co 3 Mn-LDH/ MWCNT Co 5 Mn-LDH/ MWCNT Co 7 Mn-LDH/ MWCNT Starting materials atomic ratios (Co : Mn) 2 : 1 3 : 1 5 : 1 7 : 1 EDS atomic ratios (Co : Mn) 2.54 : : : : 1 Ni 2 Mn-LDH/ MWCNT Ni 3 Mn-LDH/ MWCNT Ni 5 Mn-LDH/ MWCNT Ni 7 Mn-LDH/ MWCNT Starting materials atomic ratios (Ni : Mn) 2 : 1 3 : 1 5 : 1 7 : 1 EDS atomic ratios (Ni : Mn) 2.12 : : : : 1 S-4

5 Table S2 Co/Mn and Ni/Mn atomic ratios determined by ICP-AES Co 5 Mn-LDH/MWCNT (Co : Mn) Ni 5 Mn-LDH/MWCNT (Ni : Mn) Starting materials atomic ratios 5 : 1 5 : 1 As-prepared materials atomic ratios : : 1 S-5

6 Figure S3. TEM image of the hybrids in a relatively sparse fraction (red circle: MWCNT; blue circle: LDH nanoplates). S-6

7 Figure S4. TEM image of the Co 5 Mn-LDH nanoplatelets. S-7

8 Figure S5 HRTEM image of an individual Co 5 Mn-LDH nanocrystal. S-8

9 Figure S6. HRTEM image of an individual Ni 5 Mn-LDH nanocrystal. S-9

10 Figure S7. XRD patterns of the CoMn-LDH/MWCNT hybrids with different Co/Mn ratios. S-10

11 Figure S8. XRD patterns of the NiMn-LDH/MWCNT hybrids with different Ni/Mn ratios. S-11

12 Figure S9. Linear slope is equivalent to twice the double-layer capacitance (C dl ). Charging current density differences ( J = J a J c ) plotted as a function of the scan rate. The corresponding cyclic voltammograms obtained with CoMn-LDH/MWCNT hybrids loaded on RDEs in a capacitance current range of 0.25~0.35 vs. Hg/HgO at scan rates of 20, 40, 80, 120, 160 and 200 mv s -1. S-12

13 Figure S10. Linear slope is equivalent to twice of the double-layer capacitance (C dl ). Charging current density differences ( J = J a J c ) plotted as a function of the scan rate. The corresponding cyclic voltammograms obtained with NiMn-LDH/MWCNT hybrids loaded on RDEs in a capacitance current range of 0.25~0.35 vs. Hg/HgO at scan rates of 20, 40, 80, 120, 160 and 200 mv s -1. S-13

14 Table S3 Comparison of electrocatalytic performance of Co 5 Mn-LDH/MWCNT and Ni 5 Mn-LDH/MWCNT as well as some similar previously reported materials. Catalyst Material 10 ma cm -2 Ref. Co 3 O 4 /2.7Co 2 MnO 4 ~ 540 mv 1 MnCo 2 O 4 ~ 510 mv 2 CoMn 2 O 4 /N-rGO ~ 430 mv 3 dp-mnco 2 O 4 /CNT ~ 470 mv 4 CoMn-LDH ~ 325 mv 5 Co 3 O 4 /CNT ~ 380 mv 6 MCC-5-V72 ~ 420 mv 7 Ni 6 MnO 8 Not Reach 8 NiO/CNT ~ 360 mv 6 MnNiCoO 4 /N-MWCNT ~ 395 mv 9 h-co@ mv 10 Ni@[Ni( 2+/3+ )Co 2 (OH) 6 7 ] x 350 mv 11 NiCo 2 O 4 /CNTs 320 mv 12 MWCNTs/Ni(OH) mv 13 Co 5 Mn-LDH/MWCNT ~ 300 mv This Work Ni 5 Mn-LDH/MWCNT ~ 350 mv This Work S-14

15 The TOF value of Co 5 Mn-LDH/MWCNT and Ni 5 Mn-LDH/MWCNT was calculated according to the following equation: TOF = j A /(4 F m), where j is the current density obtained at a fixed overpotential in A cm -2, A is the surface area of the GC electrode (~ 0.07 cm -2 ), F is the Faraday efficiency (96485 C mol -1 ) and m is the number of moles of the electro-active elements in the electrocatalysts modified on the GC electrode. We calculated a TOF of ~ s 1, which was associated with Co 5 Mn-LDH/MWCNT at an overpotential of 350 mv in 1 M KOH, assuming that all the Co and Mn were involved in the electrochemical reaction. In addition, the TOF associated with Ni 5 Mn-LDH/MWCNT at an overpotential of 350 mv was ~ s -1. The table below shows the TOF value compared to those previously reported. Table S4 Comparison of TOF value of Co 5 Mn-LDH/MWCNT and Ni 5 Mn-LDH/MWCNT to some similar previously reported data. Catalyst TOF Ref. Co 5 Mn-LDH/MWCNT 350 mv ~ s -1 This work Ni 5 Mn-LDH/MWCNT 350 mv ~ s -1 This work NiFe/NF 400 mv ~ s NiFe/CNT 300 mv ~ s 1 15 NiCo 2.7 (OH) x 350 mv ~ s 1 16 Zn Co LDH 410 mv s 1 17 NG-CoSe mv ~ s α-ni(oh) mv ~ s S-15

16 References (1) Wang, D.; Chen, X.; Evans, D. G.; Yang, W. Well-Dispersed Co 3 O 4 /Co 2 MnO 4 Nanocomposites as a Synergistic Bifunctional Catalyst for Oxygen Reduction and Oxygen Evolution Reactions. Nanoscale, 2013, 5, (2) Menezes, P. W.; Indra, A.; Sahraie, N. R.; Bergmann, A.; Strasser, P.; Driess, M. Cobalt-Manganese-Based Spinels as Multifunctional Materials that Unify Catalytic Water Oxidation and Oxygen Reduction Reactions. ChemSusChem 2015, 8, (3) Prabu, M.; Ramakrishnan, P.; Shanmugam, S. CoMn 2 O 4 Nanoparticles Anchored on Nitrogen-Doped Graphene Nanosheets as Bifunctional Electrocatalyst for Rechargeable Zinc-Air Battery. Electrochem. Commun. 2014, 41, (4) Ge, X.; Liu, Y.; Goh, F. W. T.; Hor, T. S. A.; Zong, Y.; Xiao, P.; Zhang, Z.; Lim, S. H.; Li, B.; Wang, X.; Liu, Z. Dual-Phase Spinel MnCo 2 O 4 and Spinel MnCo 2 O 4 /Nanocarbon Hybrids for Electrocatalytic Oxygen Reduction and Evolution. ACS Appl. Mater. Interface 2014, 6, (5) Song, F.; Hu, X. Ultrathin Cobalt-Manganese Layered Double Hydroxide is an Efficient Oxygen Evolution Catalyst. J. Am. Chem. Soc. 2014, 136, (6) Andersen, N. I.; Serov, A.; Atanassov, P. Metal Oxides/CNT Nano-Composite Catalysts for Oxygen Reduction/Oxygen Evolution in Alkaline Media. Appl. Catal., B 2015, 163, (7) Xie, K.; Masa, J.; Madej, E.; Yang, F.; Weide, P.; Dong, W.; Muhler, M.; Schuhmann, W.; Xia, W. Co 3 O 4 -MnO 2 -CNT Hybrids Synthesized by HNO 3 Vapor Oxidation of Catalytically Grown CNTs as OER Electrocatalysts. ChemCatChem 2015, 7, (8) Menezes, P. W.; Indra, A.; Levy, O.; Kailasam, K.; Gutkin, V.; Pfrommer, J.; Driess, M. Using Nickel Manganese Oxide Catalysts for Efficient Water Oxidation. Chem. Commun. 2015, 51, (9) Yu, X.; Manthiram, A. MnNiCoO 4 /N-MWCNT Nanocomposite Catalyst with High Selectivity in Membraneless Direct Formate Fuel Cells and Bifunctional Activity for Oxygen Electrochemistry. Catal. Sci. Technol. 2015, 5, S-16

17 (10) Zhao, J.; Zou, Y.; Zou, X.; Bai, T.; Liu, Y.; Gao, R.; Wang, D.; Li, G. Self-Template Construction of Hollow Co 3 O 4 Microspheres from Porous Ultrathin Nanosheets and Efficient Noble Metal-Free Water Oxidation Catalysts. Nanoscale 2014, 6, (11) Zhao, Z.; Wu, H.; He, H.; Xu, X.; Jin, Y. A High-Performance Binary Ni-Co Hydroxide-Based Water Oxidation Electrode with Three-Dimensional Coaxial Nanotube Array Structure. Adv. Funct. Mater. 2014, 24, (12) Cheng, H.; Su, Y.; Kuang, P.; Chen, Z.; Liu, Z. Hierarchical NiCo 2 O 4 Nanosheet-Decorated Carbon Nanotubes towards Highly Efficient Electrocatalyst for Water Oxidation. J. Mater. Chem. A 2015, 3, (13) Zhou, X.; Xia, Z.; Zhang, Z.; Ma, Y.; Qu, Y. One-Step Synthesis of Multi-Walled Carbon Nanotubes/Ultra-Thin Ni(OH) 2 Nanoplate Composite as Efficient Catalysts for Water Oxidation. J. Mater. Chem. A 2014, 2, (14) Lu X.; Zhao C. Electrodeposition of Hierarchically Structured Three-Dimensional Nickel-Iron Electrodes for Efficient Oxygen Evolution at High Current Densities. Nat. Commun. 2015, 6, (15) Gong M.; Li Y.; Wang H.; Liang Y.; Wu J.; Zhou J.; Wang J.; Regier T.; Wei F.; Dai H. An Advanced Ni-Fe Layered Double Hydroxide Electrocatalyst for Water Oxidation. J. Am. Chem. Soc. 2013, 135, (16) Nai J.; Yin H.; You T.; Zheng L.; Zhang J.; Wang P.; Jin Z.; Tian Y.; Liu J.; Tang Z.; Guo L. Efficient Electrocatalytic Water Oxidation by Using Amorphous Ni-Co Double Hydroxides Nanocages. Adv. Energy Mater. 2015, 5, (17) Zou X.; Goswami A.; Asefa T. Efficient Noble Metal-Free (Electro) Catalysis of Water and Alcohol Oxidations by Zinc-Cobalt Layered Double Hydroxide. J. Am. Chem. Soc. 2013, 135, (18) Gao M.; Cao X.; Gao Q.; Xu Y.; Zheng Y.; Jiang J.; Yu S. Nitrogen-Doped Graphene Supported CoSe 2 Nanobelt Composite Catalyst for Efficient Water Oxidation. ACS Nano 2014, 8, (19) Gao M.; Sheng W.; Zhuang Z.; Fang Q.; Gu S.; Jiang J.; Yan Y. Efficient Water S-17

18 Oxidation using Nanostructured α-nickel-hydroxide as an Electrocatalyst. J. Am. Chem. Soc. 2014, 136, S-18

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