Controlled Synthesis and Formation Mechanism of Uniformly Sized Spherical CeO2 Nanoparticles

As the core abrasive in chemical mechanical polishing (CMP) processes, the morphology, size uniformity, and chemical reactivity of CeO2 nanoparticles (NPs) are crucial factors determining the surface precision and yield of devices. In this work, a KNO3–LiNO3 eutectic molten salt was used as the reaction medium. By systematically adjusting key processing parameters (such as the type of cerium source, the species and dosage of surfactants, and calcination conditions), the regulatory effects of these factors on particle growth mechanisms were clarified. This adjustment enabled the controlled synthesis of spherical CeO2 NPs with customized morphology, particle size, and surface defect states. The multi-stage reaction process of the precursor during calcination was identified by applying thermal analysis techniques, including TG-DSC and TG-FTIR. This process includes dehydration, ion exchange, and thermal decomposition. Microstructural analysis shows that the type and dosage of the cerium source and template agent significantly affect the uniformity of particle size and spherical morphology. Moreover, by using an optimized process with a heating rate of 6 °C/min and maintaining at 400 °C for 3 h, spherical CeO2 NPs with an average particle size of 60 nm, uniform size distribution, and high sphericity were successfully synthesized via a single-step calcination process. Based on these findings, a further proposal was put forward regarding a crystal growth mechanism mediated by micelle-directed assembly and oriented attachment. This method only requires a single calcination step, has mild reaction conditions, and involves a simple process without the need for specialized equipment—features that show great potential for scalable production. It provides both a theoretical basis and experimental support for the controlled preparation of high-performance CeO2 abrasives.