1：Experimental Design and Method Selection:

The study employed potentiostatic pulse electrodeposition to synthesize InSb films, focusing on varying pulse duration times (1 ms, 10 ms, 100 ms) while keeping duty cycle and total process time constant. The rationale was to explore how pulse frequency affects film properties through competitive reactions like ion reduction and hydrogen evolution.

2：Sample Selection and Data Sources:

InSb films were electrodeposited on copper foil substrates pre-treated with electropolishing and etching, followed by sputtering a 30 nm Au layer. Electrolyte composition was fixed with citrate bath containing In3? and Sb3? ions.

3：List of Experimental Equipment and Materials:

Equipment included a BioLogic SP300 potentiostat for electrodeposition, FEI VERSA 3D SEM for morphology, Panalytical Empyrean diffractometer for XRD, DektakXT Bruker profilometer and Agilent 5500 ILM AFM for thickness/roughness, PHI VersaProbeII XPS for surface composition, LabRam HR Raman microscope for crystallinity, Bode 100 analyzer for electrical measurements, Nicolet 8700 FT-IR Spectrometer for optical properties, and Kelvin probe-based SPV spectrometer for photovoltage. Materials included InCl?, SbCl?, citric acid, sodium citrate from Alfa Aesar and Sigma Aldrich.

4：Experimental Procedures and Operational Workflow:

Electrodeposition was performed in a three-electrode cell at room temperature with fixed E_on and E_off potentials. Post-deposition, films were characterized using SEM, XRD, AFM, XPS, Raman, FTIR, electrical resistance, and SPV measurements under controlled conditions (e.g., temperature 21°C).

5：Data Analysis Methods:

Data analysis involved calculating Faraday efficiency, coherent domain size from XRD using LaB? standard, roughness via Gwyddion software, band gap from Tauc plots, resistivity from two-point measurements, and photovoltage parameters using capacitor charging equation fits.