Qualification of an ultrasonic instrument for real-time monitoring of size and concentration of nanoparticles during liquid phase bottom-up synthesis

Abstract

Both in design and production of nanoparticles and nanocomposites it is of vital importance to have information about their size and concentration. During the formation of nanoparticles, real-time monitoring of particle size and concentration during bottom-up synthesis in liquids allows for a detailed study of nucleation and growth. This provides valuable insights into the formation of nanoparticles that can be used for process optimization and scale up. In the production of nanoparticles, real-time monitoring enables intervention to minimize the number of off-spec batches. In this paper we will qualify an ultrasound nanoparticle sizer (UNPS) as a real-time monitor for the growth of nanoparticles (or sub-micro particles) in the 100 nm-1 μm range. Nanoparticles affect the speed and attenuation of ultrasonic waves in the dispersion. The size of the change depends, amongst other things, on the size and concentration of the nanoparticles. This dependency is used in the UNPS method. The qualification of the UNPS was undertaken in two successful experiments. The first experiment consisted of static measurements on commercially available silica particles, and the second experiment was real-time monitoring of the size and concentration during the growth of silica nanoparticles in Stöber synthesis in a water-alcohol mixture starting from the molecular precursor tetraethyl orthosilicate. The results of the UNPS were verified by measurements of a dynamic light scattering device and a transmission electron microscope.