Effects of heating rate and deposition cycle on the structural, optical, and photoelectrocatalytic properties of electrodeposited hematite films

Abstract

In this research, electrodeposited hematite films were prepared at voltammetry deposition cycles of 60 and calcined at 550 °C in a furnace after ramping the temperature at the rates of 2 °C/min, 10 °C/min, 35 °C/min, and rapid heating of about 100 °C/min. Additional samples were fabricated at deposition cycles of 15, 30, and 80, and also calcined at 550⁰C at a heating rate of 10⁰C/min. The impact of heating rate and deposition cycle number variations on the structural, optical, and photoelectrocatalytic (PEC) properties of the hematite films were assessed. All the films' X-ray diffraction (XRD) measurements showed strong peaks at the lattice planes (104) and (110), verifying hematite's rhombohedral crystal structure. The films prepared at the heating rate of 10⁰C/min boosted the crystallization of the films by 47.2 % relative to the ones prepared at 2⁰C/min. An increase in the deposition cycle number resulted in increasing film thickness and the sample’s crystallization. An indirect bandgap of 1.94–2.1 eV was estimated for the samples, with the least value obtained for the films treated at the heating rate of 10⁰/min and deposition cycles of 60. The same samples also yielded the largest photocurrent density of 26.2 μA/cm2 at 1.23 V vs. reversible hydrogen electrode (RHE), while the photoanodes fabricated at 2 °C/min exhibited the lowest photo-activity. The enhanced photocurrent observed for the films has been associated with high crystallinity, improved photon absorption, reduced flatband potential, and increased charge separation at the film’s surface. This research underscores the importance of optimizing both the heating rate and deposition cycle numbers in the fabrication of electrodeposited photoelectrodes for PEC applications.