Raman spectroscopy in investigation of rheometric processes

Studies of application of Raman spectroscopy in measurement of important parameters of rheometric process, including profile of oil film thickness and composition of oil/paste system, were carried out. The films of silicone oil AK106 (Wacker) extracted from ceramic paste AlOOH were subjects of investigations presented in this paper. Boundary between oil film and extruded paste is not regular and ambiguous during the extrusion process of ceramic paste in capillary rheometer. Moreover, the pastes are scattering materials, what makes determination of the film thickness by conventional optical methods difficult. Preliminary Raman measurements were made separately for oil and paste samples in range extending from 50 to 3500 cm-1. Determination of main Raman bands assigned to oil, ceramics and glass showed that Raman spectroscopy enables discernment of these materials. During the next step, studies were conducted for a model sample of the oil spread on the paste, using Raman microscope. This device was equipped with long-working-distance objective which should enable remote measurements through a borosilicate, view-port-window in the wall of capillary rheometry die. Two methods of Raman determination of the thickness were compared. Results of analysis and experimental works suggest that one of them can be applied for in-situ monitoring of the extrusion process.