Monodispersed, Micron-Sized Supermicroporous Silica Particles by Cetyltrimethylammonium Bromide-Mediated Preparation

In this study, we present a novel modified Stöber method utilizing cetyltrimethylammonium bromide (CTAB) as a mediator for the preparation of monodispersed, micron-sized supermicroporous silica particles. Observed results show prepared silica particles ranging in size from 0.64 to 1.36 μm with an increase in CTAB concentration from 1.0 to 5.0 mM. The particles exhibited low polydispersity (<5%), a high Brunauer–Emmett–Teller surface area (570 to 1064 m²/g), and pore volumes ranging from 0.22 to 0.39 cm³/g. The pore size, determined using the Barrett–Joyner–Halenda method from the adsorption branches of the isotherms, was approximately 1.9 nm, specifically 1.83, 1.85, and 1.90 nm, as the CTAB concentration increased from 1.0 to 2.5 and 5.0 mM, respectively. The resulting particles displayed a narrow distribution of pore diameters. In addition, to obtain an in-depth understanding of the role of CTAB on the preparation of silica particles, a possible mechanism is also investigated using conductivity, dynamic light scattering (DLS), zeta potential, FT-IR spectra, and transmission electron microscopy. Our findings demonstrate that CTAB plays multiple roles in the hydrolysis/condensation of TEOS (tetraethyl orthosilicate) and subsequent nucleation and growth of silica particles. CTAB acts as a template for superporosity, a stabilizer for colloids, and an accelerator for nucleation and growth, leading to formation of monodispersed micrometer silica particles. Further characterization through FT-IR and ²⁹Si solid NMR spectra revealed that the micron silica particles were obtained with inhomogeneity in the condensation degree, allowing for selective etching through hot incubation to form micron-sized hollow silica spheres.