This paper describes the synthesis of Na_1/2Bi_1/2Cu₃Ti₄O₁₂ (BNCTO) with different morphologies like nanoparticles, micro cubic, and micro sheet structure prepared by modify sol–gel method, using different surfactants (SDS, CTAB, PVP, and PVA). This study aimed to investigate the effects of different surfactant such as SDS, CTAB, PVP, and PVA and chelating agent on the morphology and particle size of final products. It was found that the size and morphology of the products could be greatly influenced by the aforementioned parameters. To our knowledge, this is the first report on the synthesis of Na_1/2Bi_1/2Cu₃Ti₄O₁₂ nanostructure with different morphologies in the presence of salicylic acid as a chelating agent. The as-synthesized products were characterized by powder X-ray diffraction, scanning electronic microscopy, ultraviolet–visible, and energy dispersive spectrometry analysis of X-ray techniques.