Ecsalab 250

The ¹H nuclear magnetic resonance (NMR) was performed on a 400 MHz NMR spectrometer (Bruker AMX 400 system) to confirm the chemical structures of EDOT‐MeCl and EDOT‐CQH₂ monomer. Ex situ FT‐IR spectra (BRUKER VECTOR 22 Spectrometer) were used to characterize the structure changes of anodes and cathodes during different charged/discharged stages. Raman spectra (Renishaw's InVia Raman Microscopes) and XPS (Thermo ECSALAB 250) were also used to clarify the reaction mechanism of the cathode, accompanied by C1s peak calibration (284.8 eV). Crystal structures of PUQ powder and anode were characterized using Rigaku wide‐angle X‐ray diffractometer (XRD, D/max rA, using Cu Kα radiation, λ = 1.5406 Å). Morphology was observed using field‐emission SEM (FEI Nova Nano SEM 450) before and after long‐term cycles.

Microstructure characterizations and chemical component analysis of nanoporous electrocatalyst electrodes were performed on a field-emission scanning electron microscope (JSM-6700F, JEOL, 7 keV) equipped with X-ray energy-dispersive spectroscopy (EDS), and a field-emission transition electron microscope (JEM-ARM300F, JEOL) equipped with double spherical-aberration correctors for both condenser and objective lens, respectively. XRD measurements of nanoporous electrocatalyst electrodes were conducted on a D/max2500pc diffractometer with a monochromated Cu K_α radiation. Chemical states and distribution of surface elements were analyzed using XPS and LEIS on a Thermo ECSALAB 250 with an Al anode. Charging effects were compensated by shifting binding energies according to the C 1 s peak (284.8 eV). Inductively coupled plasma optical emission spectrometry (ICP-OES, Thermo electron) analysis was conducted to determine the concentrations of metal ions. Raman spectra were measured on a micro-Raman spectrometer (Renishaw) equipped with 532 nm-wavelength laser at a power of 0.5 mW.

The microstructural and chemical features of nanoporous Zn, Cu/Zn and Zn_xCu_y/Zn sheets were characterized by a field-emission scanning electron microscope equipped with an X-ray energy-dispersive spectroscopy (SEM–EDS, JEOL, JSM-7900F, 15 kV) and a field-emission transition electron microscope (TEM, JEOL, JEM-2100F, 200 kV). X-ray diffraction (XRD) measurements of all specimens were taken on a D/max2500pc diffractometer with a Cu Kα radiation. Raman spectra were measured on a micro-Raman spectrometer (Renishaw) with a 532-nm-wavelength laser at the power of 0.5 mW. X-ray photoelectron spectroscopy (XPS) analysis was conducted on a Thermo ECSALAB 250 with an Al anode. Charging effects were compensated by shifting binding energies based on the adventitious C 1 s peak (284.8 eV). Ion concentrations in electrolytes were analyzed by inductively coupled plasma optical emission spectrometer (ICP-OES, Thermo electron).

The microstructures of NP c-V₂O₃, c-V₂O₃/r-VO_2−x and r-VO₂ were investigated using a field-emission scanning microscope (JEOL JSM-6700F, 15 keV) and a field-emission transmission electron microscope (JEOL JEM-2100F, 200 keV). HR-STEM characterization was performed on a field-emission transition electron microscope (JEM-ARM200F, 200 kV) equipped with double spherical aberration correctors for the condenser lens and objective lens. The chemical composition was characterized by X-ray photoelectron spectroscopy on Thermo ECSALAB 250 with an Al anode. Binding energies were calibrated using containment carbon (C 1s = 284.6 eV). Nitrogen adsorption/desorption isotherms at 77 K were measured on a micromeritics ASAP 2020 system to evaluate the specific surface area by the BET method, as well as the pore volume and the pore size by the Barrett–Joyner–Halenda (BJH) method. X-ray diffraction measurements were performed on a D/max2500pc diffractometer using Cu Kα radiation. Raman spectra were collected using a micro-Raman spectrometer (Renishaw) with a laser of 532 nm wavelength at 0.2 mW. Temperature dependence of resistivity was collected on Hall Effect measurement system (HMS-5000).

Field-emission scanning electron microscope (JSM-6700F, JEOL, 15 keV) equipped with X-ray energy-dispersive spectroscopy (EDS) was employed to characterize microstructure and chemical composition of nanoporous catalysts. High-resolution transmission electron microscopy (HRTEM) and scanning transmission electron microscopy (STEM) characterizations were performed on a field-emission transmission electron microscope (JEM-2100F, JEOL, 200 keV) and a field-emission transition electron microscope (JEM-ARM200CF, JEOL) operated at 200 keV and equipped with double spherical-aberration correctors for both condenser and objective lens, respectively. X-ray diffraction patterns of all nanoporous catalyst electrodes were collected from a D/max2500pc diffractometer with a monochromated Cu K_α radiation. X-ray photoelectron spectroscopy (XPS) analysis was conducted on a Thermo ECSALAB 250 with an Al anode. Charging effects were compensated by shifting binding energies based on the adventitious C 1s peak (284.8 eV). Atomic ratio of elements was analyzed using ICP-MS (Thermo electron). N₂ adsorption/desorption isotherms were collected at 77 K by a Micromeritics (ASAP 2020 Plus) system.

The metallographic microstructure of Zn_xAl_100−x alloy sheets was investigated by using a confocal laser scanning microscope (OLS3000, Olympus) after conventional grinding and mechanical polishing, followed by chemical etching in acetic picric solution (5 ml HNO₃ and 5 ml HF, 90 ml ultrapure water). The electron micrographic structures were characterized by using a field-emission scanning electron microscope (JEOL, JSM-6700F, 15 kV) equipped with an X-ray energy-dispersive microscopy, and a field-emission transmission electron microscope (JEOL, JEM-2100F, 200 kV). XRD measurements were conducted on a D/max2500pc diffractometer using Cu Kα radiation. Ion concentrations in electrolytes were analyzed by inductively coupled plasma optical emission spectrometer (ICP-OES, Thermo electron). XPS analysis was conducted on a Thermo ECSALAB 250 with an Al anode. Charging effects were compensated by shifting binding energies based on the adventitious C 1s peak (284.8 eV).