A small angle X-ray scattering study on high pH silica precipitations

Abstract

Silica prcipitations were carried out at high pH (7–10) and elevated temperatures (60–90°C) by means of simultaneous dosing of diluted water glass and sulphuric acid into a stirred thermostatted reaction vessel. In order to investigate the development of the vulnerable silica structures during the processes, every 5–10 min small samples were taken from the reaction mixture and analysed using small angle X-ray scattering. It was found that a narrow particle size distribution was maintained throughout the entire preparation procedure (or at least from about 1 h until the end of the process), despite the fact that the primary silica particles were growing continuously. In addition, a continuous decrease in the total number of primary particles was observed, indicating that the primary particles were involved in clustering and aging processes, and that (except for the initial reaction stages) newly dosed silica does not form new particles but is deposited onto the already existing particles. Ostwald ripening, which is regarded as the most important aging mechanism, probably proceeds relatively rapidly under the applied process conditions, leading to a persistent high degree of monodispersity.