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1 Supporting Information Nest-like NiCoP for Highly Efficient Overall Water Splitting Cheng Du, a Lan Yang, a Fulin Yang, a Gongzhen Cheng a and Wei Luo a,b* a College of Chemistry and Molecular Sciences, Wuhan University, Wuhan, Hubei , P. R. China, Tel.: *Corresponding author. addresses: wluo@whu.edu.cn. b Key laboratory of Advanced Energy Materials Chemistry (Ministry of Education), Nankai University, Tianjin , P. R. China Scheme S1. Schematic illustration of the nest-like NiCoP/CC fabrication process. S1
2 Figure S1. SEM images for NiCo2O4/CC Figure S2. EDS elemental mapping images of nest-like NiCoP/CC. S2
3 Figure S3. (a) and (b) XRD patterns for metal oxides and metal phosphides. Figure S4. N 2 adsorption-desorption isotherms of (a) nest-like NiCoP/CC, (b) Ni 2 P/CC, and (c) CoP/CC. Figure S5. EDX spectrum of nest-like NiCoP/CC. S3
4 Figure S6. SEM images for NiCoP/CC with different amounts of urea. (a, d) 5 mmol, (b, e) 10 mmol, (c, f) 20 mmol. Figure S7. SEM images for Ni0.33Co0.67P/CC (a, c) and Ni0.67Co0.33P/CC (b, d). S4
5 Figure S8. XRD patterns for NiCoP/CC, Ni 33 Co 67 P/CC and Ni 67 Co 33 P/CC. Figure S9. XPS survey scans for the nest-like NiCoP (a); High-resolution XPS spectra of (b) Co(2p), (c) Ni(2p), (d) P(2p), (e) O(1s) and (f) C(1s) peaks for the nest-like NiCoP/CC. S5
6 Figure S10. The current density per geometric surface area (black), and specific current densities per BET surface area (red) at 0.1 V overpotential for HER (a) and 0.27 V overpotential for OER (b) in 1 M KOH. Figure S11. (a) The HER polarization curves in 0.5 M H 2 SO 4 and (b) the OER polarization curves in 1 M KOH of 3D nest-like NiCoP/CC and NiCoP/CC nanoarray. The mass loading for electrodes was controlled to be ~1.3 mg cm -2. S6
7 Figure S12. High-resolution XPS spectra of (a) Co(2p), (b) Ni(2p), (c) P(2p) and (d) O(1s) peaks for the nest-like NiCoP/CC after OER test. Figure S13. Nyquist plots of nest-like NiCoP/CC, CoP/CC and Ni 2 P/CC recorded at (a) η = 60 mv in 0.5 M H 2 SO 4 solution, (b) η = 237 mv in 1 M KOH solution. S7
8 Figure S14. Cyclic voltammetries for (a) nest-like NiCoP/CC, (c) Ni 2 P/CC, and (e) CoP/CC. The capacitive currents at 0.10 V as a function of scan rate for (b) nest-like NiCoP/CC, (d) Ni 2 P/CC, and (f) CoP/CC in 0.5 M H 2 SO 4. S8
9 Figure S15. Cyclic voltammetries for (a) nest-like NiCoP/CC, (c) Ni 2 P/CC, and (e) CoP/CC. The capacitive currents at 0.96 V as a function of scan rate for (b) nest-like NiCoP/CC, (d) Ni 2 P/CC, and (f) CoP/CC in 1 M KOH. S9
10 Figure S16. Current-time slopes of chronoamperometric tests for HER in acid (a) and basic (b) solution; the voltage-time slopes of chronopotentiometric test for OER (c) and water (d). Figure S17. Faraday efficiency of H 2 and O 2 production. S10
11 Table S1 Comparison of the catalytic activity toward the HER in 0.5 M H 2 SO 4 of the nest-like NiCoP/CC with other reported high performance HER catalysts. Materials η10 (mv) Tafel slop Ref. (mv dec -1 ) Ni-P nanoplates/gc Ni-P/carbon fiber paper NiCoP /Ti CoP/rGO u-cop/ti NiCoP/rGO Ni5P4 films/ Ni foam Ni2P nanorods arrays/ni foam Ni5P4-Ni2P nanosheets array Ni2P/carbon nanospheres Ni12P5 nanoparticles/ti CoP/CNT CoP/CC CoP/Ti N2P nanoparticles/ti Ni2P hollow NPs/Ti CoP/NCNTs NiP2 NS/CC Ni2P/NRGO NiCoP /CC This work Table S2 Comparison of representative Co-based and Ni-based water- catalysts in alkaline electrolyte. Mass Materials loading (mg cm -2 ) Ni5P4 films/ NiOOH NiCoP/Ni foam 1.6 Ni-P/carbon fiber paper 25.8 Water electrolysis test (in 1.0 M KOH) η10 Tafel Energy slop consumption of (mv) (mv the cells dec -1 ) (kwh (kgh2) -1 ) Mass activity at the overpotential of 0.3 V (ma g -1 ) HER OER >470 - > HER OER HER OER Fe-Co/carbon 1.2 HER fiber papers 2 OER Ref S11
12 HER > OER NiFe@NC HER OER CoP/rGO HER OER Co-P film >400 - > HER CoP N-doped OER carbon >470 - > Ni-Co nanowire 0.3 OER Ni Co P HER C@NiCoP 0.65 HER HER OER CoP2/RGO u-cop/ti 6.32 HER HER NiCoP/rGO 0.15 NiCoP/Ni foam ~5 Ni0.51Co0.49P film OER HER OER 133 (η 50) 308 (η 50) 540 (η 50) HER OER HER OER Ni@C-400 NSs ~ HER OER Ni/NiP HER OER CoP NS/C HER OER CoP-MNA S
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