This review presents an introduction to the synthesis of metallic nanoparticles by radiation-induced method, especially gamma irradiation. This method offers some benefits over the conventional methods because it provides fully reduced and highly pure nanoparticles free from by-products or chemical reducing agents, and is capable of controlling the particle size and structure. The nucleation and growth mechanism of metallic nanoparticles are also discussed. The competition between nucleation and growth process in the formation of nanoparticles can determine the size of nanoparticles which is influenced by certain parameters such as the choice of solvents and stabilizer, the precursor to stabilizer ratio, pH during synthesis, and absorbed dose.

This paper focuses on the recent advances on radiolysis-assisted shape-controlled synthesis of noble metal nanostructures. The techniques and protocols for producing desirable shapes of noble metal nanoparticles are discussed through introducing the critical parameters which can influence the nucleation and growth mechanisms. Nucleation rate plays a vital role on the crystallinity of seeds while growth rate of different seeds’ facets determines the final shape of resultant nanoparticles. Nucleation and growth rate both can be altered with factors such as absorbed dose, capping agents, and experimental environment condition to control the final shape. Remarkable physical and chemical properties of synthesized noble metal nanoparticles by controlled morphology have been systematically evaluated to fully explore their applications.

Colloidal Fe₃O₄ nanoparticles were synthesized using a gamma-radiolysis method in an aqueous solution containing iron chloride in presence of polyvinyl alcohol and isopropanol as colloidal stabilizer and hydroxyl radical scavenger, respectively. Gamma irradiation was carried out in a ⁶⁰Co gamma source chamber at different absorbed doses. Increasing the radiation dose above a certain critical dose (100 kGy) leads to particle agglomeration enhancement, and this can influence the structure and crystallinity, and consequently the magnetic properties of the resultant particles. The optimal condition for formation of Fe₃O₄ nanoparticles with a uniform and narrow size distribution occurred at a dose of 100 kGy, as confirmed by X-ray diffractometry and transmission electron microscopy. A vibrating sample magnetometry study showed that, when radiation dose increased, the saturation and remanence magnetization decreased, whereas the coercivity and the remanence ratio increased. This magnetic behavior results from variations in crystallinity, surface effects, and particle size effects, which are all dependent on the radiation dose. In addition, Fourier transform infrared spectroscopy was performed to investigate the nature of the bonds formed between the polymer chains and the metal surface at different radiation doses.

Colloidal Cu@CuAlO₂-Al₂O₃ bimetallic nanoparticles were prepared by a gamma irradiation method in an aqueous system in the presence of polyvinyl pyrrolidone (PVP) and isopropanol respectively as a colloidal stabilizer and scavenger of hydrogen and hydroxyl radicals. The gamma irradiation was carried out in a ⁶⁰Co gamma source chamber with different doses up to 120 kGy. The formation of Cu@CuAlO₂-Al₂O₃ nanoparticles was observed initially by the change in color of the colloidal samples from colorless to brown. Fourier transform infrared spectroscopy (FTIR) confirmed the presence of bonds between polymer chains and the metal surface at all radiation doses. Results of transmission electron microscopy (TEM), energy dispersive X-ray spectrometry (EDX), and X-ray diffraction (XRD) showed that Cu@CuAlO₂-Al₂O₃ nanoparticles are in a core-shell structure. By controlling the absorbed dose and precursor concentration, nanoclusters with different particle sizes were obtained. The average particle diameter increased with increased precursor concentration and decreased with increased dose. This is due to the competition between nucleation, growth, and aggregation processes in the formation of nanoclusters during irradiation.

The thermal treatment method was employed to prepare nickel-cobalt oxide (NiO/Co₃O₄) nanoparticles. This method was attempted to achieve the higher homogeneity of the final product. Specimens of nickel-cobalt oxide were characterized by various experimental techniques, including X-ray diffraction (XRD), transmission electron microscopy (TEM) and Fourier transform infrared spectroscopy (FTIR). X-ray diffraction results showed that there was no crystallinity in the predecessor, and it still had the amorphous phase. The formations of the crystalline phases of the nickel-cobalt oxide nanoparticles started from 350–500 °C, and the final products had different crystallite sizes ranging from 11–35 nm. Furthermore, the variation of DC conductivity (σ_dc), impedance, tangent loss (tgδ) and dielectric constant (ε′) of the calcined specimens with frequency in the range of 10²–10⁶ Hz was investigated. σ_dc showed a value of 1.9 × 10⁻⁶ S/m, 1.3 × 10⁻⁶ S/m and 1.6 × 10⁻⁶ S/m for the specimens calcined at 350, 400 and 450 °C, respectively. Additionally, a decrease in tgδ values with an increase in temperature was observed. Finally, the formed nanoparticles exhibited ferromagnetic behaviors, which were confirmed by using a vibrating sample magnetometer (VSM).