The structural, optical, magnetic, and photocatalytic properties of NiO/SiO2(x) nanoparticles with different SiO2 concentration (x) = 0%, 30%, 50%, 60%, and 70% have been investigated. XRD confirmed that the phase formation of NiO nanoparticles and the average crystallite size decreased with increasing SiO2 concentration. FTIR spectra confirmed the presence of Ni—O and Si—O—Si symmetric and asymmetric bands at 440, 800, and 1050 cm−1, respectively. The one-phonon (1P) optical mode in Raman spectra revealed the presence of interstitial oxygen defects, whereas the two-magnon (2M) peak indicates antiferromagnetic (AFM) ordering in x = 0% and 30% nanoparticles due to the large average crystallite size. The 2M peak at 1472 cm−1 diminished for x = 50%, 60%, and 70% nanoparticles, which confirmed the magnetic transition from AFM to a superparamagnetic (SPM) state. The magnetic data also confirmed the AFM to SPM transition in these nanoparticles. It is clear from diffuse reflectance spectra that x = 70% nanoparticles showed higher and wide absorbance spectra due to the presence of a large amount of fused SiO2. The HRTEM images showed that the crystalline NiO nanoparticles are well dispersed in a fused amorphous SiO2 matrix, which served as the UV wave guiding medium to activate NiO nanoparticles as a photocatalyst. The photocatalytic activity of x = 70% nanoparticles was found maximum due to their ability to absorb a wide range of UV/Vis light, and this is attributed to a higher concentration of SiO2 and oxygen defects at the surface of the nanoparticles. Therefore, a higher SiO2 concentration is beneficial for enhancing the photocatalytic performance and achieving SPM in NiO nanoparticles.
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