Low-Temperature Synthesis of Bi₂S₃ Hierarchical Microstructures via Co-Precipitation and Digestive Process in Aqueous Medium

Bismuth sulfide (Bi2S3) nanostructures have gained significant attention in the fields of catalysis, optoelectronics, and biomedicine due to their unique physicochemical properties. This paper introduces a simple and cost-effective method for producing Bi2S3 microstructures at low temperatures (25 and 70 °C). These microstructures are formed by the hierarchical self-assembly of Bi2S3 nanoparticles, which are typically 15–40 nm in size. The nanoparticles are synthesized by the co-precipitation of thioglycolic acid, thioacetamide, and bismuth nitrate in water. The study delves into the phase composition and morphological evolution of the microstructures, concerning the chemical composition of the solution and the synthesis temperature. X-ray analysis has confirmed the formation of single-phase bismuthinite Bi2S3. The synthesis process generates primary building blocks in the form of 15–40 nm Bi2S3 nanocrystals, which then go through a hierarchical self-assembly process to produce a range of micrometer-sized structures. A scanning electron microscopy examination revealed that the primary nanoparticles self-assemble into quasi-1D worm-like nanostructures, which then self-assemble to create sponge-shaped microstructures. These structures subsequently self-organize and refine into either flower- or dandelion-like microstructures, mostly depending on the synthesis temperature and the chemistry of the digestion medium.