Design, Synthesis, Characterization, and Surface Texture Investigation of a Novel Nickel-Supported Magnetic Nanocatalyst (Hierarchical Layered) for Efficient Hydrogen Production (Hydrolysis/Alcoholysis)

Abstract

In this study, Fe3O4@TROMETHAMINE-Ni magnetic nanocatalysts (MNCs) were synthesized for the first time. Various characterization techniques, including fourier transform infrared spectroscopy (FTIR), x-ray diffractometer (XRD), scanning electron microscopy (SEM), pulsed sample magnetometer, electron paramagnetic resonance (EPR), and surface area measurement (BET), have been used to elucidate the structure and morphology of Fe3O4@TROMETHAMINE-Ni MNCs. The average particle size, surface area, and saturation magnetization value of Fe3O4@TROMETHAMINE-Ni MNCs have been measured as 7.97 nm, 60.11 m2/g, and 43.49 emu/g, respectively. The Fe3O4@TROMETHAMINE-Ni MNCs were determined to be superparamagnetic. EPR analysis was used to calculate the g-factor values before and after sodium borohydride (NaBH4) hydrolysis of Fe3O4@TROMETHAMINE-Ni MNCs, which were found to be 4.81 and 4.95, respectively. This value indicates that the electrons surrounding the oxygen vacancies formed on the catalyst surface can enhance transport efficiency and improve catalytic activity. It was optimized by many parameters in hydrogen production with hydrolysis/alcoholysis of NaBH4 using Fe3O4@TROMETHAMINE-Ni MNCs. For hydrogen production by NaBH4 hydrolysis of Fe3O4@TROMETHAMINE-Ni MNCs, it has been carried out using 265 mM NaBH4, 75 mg Fe3O4@TROMETHAMINE-Ni MNCs, and 20 mL of pure water/methanol at room temperature. The amount of hydrogen produced under optimum conditions has been measured as 1533 mL/min·gcat. It was determined that the reusability performance of Fe3O4@TROMETHAMINE-Ni MNCs showed a minor decrease of 8.42 % compared to the initial usage after the sixth cycle. These results show that Fe3O4@TROMETHAMINE-Ni MNCs are a promising material with advantages such as high efficiency in hydrogen production and the ability to be used repeatedly. © 2025 Elsevier B.V.