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Gadolinium hydroxide (Gd(OH)₃) was synthesized via a microwave-assisted synthesis method. Nickel ion (Ni²⁺) was doped into Gd(OH)₃, in which 4–12% Ni-Gd(OH)₃ was synthesized, to study the effect of doping. The structural, optical, and morphological properties of the synthesized materials were analyzed. The crystallite sizes of the hexagonal structure of Gd(OH)₃ and Ni-Gd(OH)₃, which were 17–30 nm, were obtained from x-ray diffraction analysis. The vibrational modes of Gd(OH)₃ and Ni-Gd(OH)₃ were confirmed using Raman and Fourier-transform infrared spectroscopies. The band gap energy was greatly influenced by Ni-doping, in which a reduction of the band gap energy from 5.00 to 3.03 eV was observed. Transmission electron microscopy images showed nanorods of Gd(OH)₃ and Ni-Gd(OH)₃ and the particle size increased upon doping with Ni²⁺. Photocatalytic degradations of brilliant green (BG …