Nickel Sulfides Freestanding Holey Films as Air-Breathing Electrodes for. Flexible Zn-Air Batteries

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1 Nickel Sulfides Freestanding Holey Films as Air-Breathing Electrodes for Flexible Zn-Air Batteries Kyle Marcus, 1,# Kun Liang, 1,# Wenhan Niu, 1,# Yang Yang 1,* 1 NanoScience Technology Center, Department of Materials Science and Engineering, University of Central Florida, Orlando, FL 32826, USA * Corresponding author: Yang.Yang@ucf.edu # These authors contributed equally to this work. S-1

2 Experimental Section Fabrication of NiS x flexible holey film (FHF): First, a nickel thin film was fabricated by electrodeposition, where stainless steel was used as the working electrode and nickel foil as the counter electrode. Typical electrolyte composition consisted of 0.9 M NiSO 4, 0.13 M NiCl 2, and 0.5 M H 3 BO 4, dissolved in deionized water (18.1 MΩ cm) and stirred for 1 hr. The constant current density of 20 ma cm -2 was applied for 7 mins to deposit an approximate 2 µm thick nickel layer onto the stainless steel foil substrate (0.1 mm thick, MTI Corp.). Samples were subsequently rinsed with deionized (DI) water, then air dried. The nickel deposit layer was peeled from the stainless steel foil substrate, leaving a freestanding Ni thin film. It should be noted that the stainless steel foil substrate can be reused for multiple deposit cycles. Holey structures were created by electrochemical etching of the nickel deposit layer by using the same electrolyte employed for electrodeposition. The thin film nickel deposit layer replaced the nickel foil as the counter electrode and stainless steel foil remained as the working electrode. The current density was left at 20 ma cm -2 for 30 s. Samples were rinsed with DI water, then air dried. Lastly, sulfuration was carried out in a two-heating zone chemical vapor deposition (CVD) system (MTI Corporation), using nitrogen as the carrying gas at 110 sccm. The sulfur powder was placed in the upstream heating zone at 150 o C and the holey nickel deposit layer was placed in the downstream heating zone at 250 o C for a reaction time of 30 minutes at target temperatures. After sulfuration, the films were cooled in a nitrogen atmosphere. It should be noted that a typical, ready to use, freestanding NiS x FHF can be fabricated in under one hour. S-2

3 Characterization: Structure and morphology were evaluated by a scanning electron microscope (SEM, Zeiss Ultra 55) and high-resolution transmission electron microscope (HRTEM, FEI Tenchi F30). X-ray diffraction (XRD) measurements were taken using a Panalytical Empyrean Diffractometer (Panalytical) with Cu Kα radiation. Raman spectroscopy was obtained with a Renishaw Raman RE01 (Renishaw, Inc.) using 532 nm excitation argon laser. The material chemical composition was evaluated by X-ray photoelectron spectroscopy (XPS, Physical Electronics). All XPS spectrums were calibrated according to C 1s of ev. Electrochemical measurements: All electrochemical testing was performed in a three-electrode configuration using a CHI 760E electrochemical workstation (CH Instruments) in O 2 saturated 0.1 M KOH solution. Linear sweep voltammograms (LSV) were used for evaluation of ORR/OER activity by using a Pine Research Instrumentation (USA) MSR rotator at a scan rate of 5 mv s -1. A GC based rotating disk electrode (RDE) with a disk area of cm -2 and a rotating-ring disk electrode (RRDE) with a disk area of cm -2, Pt ring area of cm -2, and collection efficiency of 37% (Pine Research Instrumentation). Freestanding NiS x FHF was punched to match the GC areal dimension and attached by conductive silver paint (SPI Supplies). OER performance was observed at a rotation speed of 1600 rpm in the potential range of 1.0 to 1.6 V vs. RHE and was subjected to ir-correction. A Tafel plot was obtained according to the following Tafel equation: = log + (1) where η is the overpotential (η = E (V vs. RHE) V), b is the Tafel slope, j geo is current S-3

4 density (ma cm -2 ). LSV for ORR were obtained by adjusting the RDE rotation speed in the range of rpm in O 2 -saturated 0.1 M KOH solution at a scan rate of 5 mv s -1. Cyclic voltammograms (CV) for ORR were attained at a scan rate of 50 mv s -1 in saturated N 2 and O M KOH solutions. Electron transfer number (n) and peroxide yield (H 2 O 2 %) values for ORR were extracted from an RRDE LSV curve obtained at 2500 rpm and a scan rate of 5 mv s -1. Calculations are based on the following equations: [3] = H 2 O 2 % = 200 N N + (2) (3) where I Disk is the disk current, I Ring is the Pt ring current, N is the RRDE collection efficiency (37%). Electrochemical impedance spectroscopy (EIS) measurements were taken from open circuit potential (OCP) in the frequency range of to 0.01 Hz. Rechargeable ZAB galvanostatic charge/discharge (GDC) assessments were performed with a Land CT2001A battery testing system (Wuhan Land Electronic Company). ZAB configuration consisted of the freestanding NiS x FHF acting as the air-breathing cathode, zinc plate (2 cm x 4 cm x 1 mm) as an anode, a separator of Whatman Grade GF/D fiberglass. Koutecky-Levich plots derived from LSV tested by RDE technology were used to determine the electron-transfer number as following: = + = + / B=0.62 / / (S1) (S2) where is the angular speed of the rotating electrode, j D is the disk current density, j d is the S-4

5 diffusion controlled current density, j k is the kinetically controlled current density, F is the Faraday constant, D 0 and C 0 is are the diffusion coefficient and bulk concentration of O 2 in the electrolyte. Electrochemically active surface area (EASA) was acquired by CV at scan rates ranging from 10 mv s -1 to 100 mv s -1 in the non-faradaic potential range of to V vs RHE. Each scan rate sample interval underwent 10 complete cycles before final evaluation. Double layer capacitance (C DL ) was calculated based on averages from positive and negative slopes obtained from CV values at V vs RHE for different scan rates. The C DL can be calculated based on equation S3: C DL = i v (S3) where i is the double layer current from CV. The EASA can be calculated from the equation S4: EASA= C DL C s (S4) where C s is the capacitance of an atomically smooth planar surface of the material per unit area. An average value of C s = 40 µf cm -2 is used in this work. 1 S-5

6 Figure S1. Top view SEM images of NiS x FHF with different magnifications. The scale bars in (a-c) denote 10 µm, 10 µm, and 2 µm, respectively. Figure S2. Cross-sectional TEM image of a partially formed pore within the NiS x FHF. Red boxes 1 and 2 show EDX elemental identification of Ni and S present in the active layer region. S-6

7 Figure S3. XPS survey of NiS x FHF. Figure S4. The ORR performance of Pt/C electrode. S-7

8 Figure S5. (a) RDE LSV curves for ORR at rotation speeds from rpm in 0.1 M KOH with a scan rate of 5 mv s-1. (b) K-L plots. Figure S6. (a) CVs at different scan rates of 10, 20, 40, 60, 80, and 100 mv s -1 for evaluating the NiS x FHF electrochemically active surface area (ECSA) in a potential window of V vs RHE. Central dotted line indicates V vs RHE. (b) Slopes used in the calculation of C DL. S-8

9 Figure S7. SEM image and EDS elemental mapping of NiS x HTF after 400 min of rechargeable Zn-air coin cell battery testing. The current density of 2 ma cm -2 at 100 min cycle -1. Scale bar is 20 µm. Figure S8. XRD curves before and after cycling test. S-9

10 Table S1. Comparison of electrocatalytic performance of NiS x FHF with the state-of-the-art catalysts. Reference 1. Gao, M.; Sheng, W.; Zhuang, Z.; Fang, Q.; Gu, S.; Jiang, J.; Yan, Y. Efficient water oxidation using nanostructured α-nickel-hydroxide as an electrocatalyst. J. Am. Chem. Soc. 2014, 136, S-10

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