Influence of an Ultrasonic Treatment on the Structure and Flow Behaviour of Oxide Ceramic Masses

Abstract

Abstract Oxide ceramic masses are used for catalysts and catalyst carriers. For a reliable processing hydrocolloids (e. g. cellulose) are usually added in order to decelerate demixing phenomena. Oxide ceramic masses react to simple shearing with hardening (peptisation: increase of the shear stress with the shear deformation) [1]. The present study analyses, if an ultrasonic treatment has also an impact on the structure, the shelf-life (in the green state), the correlated flow behaviour of oxide ceramic masses and presumably (not tested) the mechanical properties in the hardened, sintered state. The idea of using ultrasonic treatment is to change the microstructure (see below) and, therefore, to minimise or even give up the standard addition of stabilizers to minimize demixing in aqueous oxide ceramic suspensions. Besides the additional costs of an extra process unit, stabilisers cause often deteriorated mechanical properties (porosity, crack behaviour) of the ceramics in the hardened state after the sintering. Therefore, pump experiments (apparent viscosity), oscillatory (G´ and G´´) and steady shear experiments (h), particle-size analysis (particle-size distribution, agglomerate strength), light microscopy, decanting experiments and pH-determinations have been performed. The obtained results show, that the hardening of the apparent viscosity (derived from the flow) during pump experiments with simultaneous ultrasonic treatment in a flow cell is combined with an increase of the fine fraction, the formation of enlarged, but smoother agglomerates, the change of the pH-value and the evolution of a three-dimensional network (gelling). All these processes increase both the amount of bound/immobilised (chemically or physically bound by or onto the solid-surfaces) and of retained water (interior of agglomerates and/or the pores of the flowand ultrasonic-induced network). This means that the volume fraction of the rheologically "free" water decreases and simultaneously the effective solid volume fraction increases. With respect to the concept of the rheologically effective solid fraction this is combined with an increasing viscosity. At the same time the tendency of demixing decreases significantly. Thus, by an appropriate combination of shear flow and ultrasonic treatment, the aqueous oxide ceramic suspensions are stabilised and a reliable processing of the initially problematic solid/fluid mixtures can be realised without stabilisers (eluding their negative consequences with respect to the quality of the sintered state).