Cementitious pastes are multiphase suspensions that are rheologically characterized by viscosity and yield stress. They tend to flocculate during rest due to attractive interparticle forces, and desagglomerate when shear is induced. The shear history, e.g., mixing energy and time, determines the apparent state of flocculation and accordingly the particle size distribution of the cement in the suspension, which itself affects suspension's plastic viscosity and yield stress. Thus, it is crucial to understand the effect of the mixing procedure of cementitious suspensions before starting rheological measurements. However, the measurement of the in-situ particle agglomeration status is difficult, due to rapidly changing particle network structuration. The focused beam reflectance measurement (FBRM) technique offers an opportunity for the in-situ investigation of the chord length distribution. This enables to detect the state of flocculation of the particles during shear. Cementitious pastes differing in their solid fraction and superplasticizer content were analyzed after various pre-shear histories, i.e., mixing times. Yield stress and viscosity were measured in a parallel-plate-rheometer and related to in-situ measurements of the chord length distribution with the FBRM-probe to characterize the agglomeration status. With increasing mixing time agglomerates were increasingly broken up in dependence of pre-shear: After 300 s of pre-shear the agglomerate sizes decreased by 10 µm to 15 µm compared to a 30 s pre-shear. At the same time dynamic yield stress and viscosity decreased up to 30% until a state of equilibrium was almost reached. The investigations show a correlation between mean chord length and the corresponding rheological parameters affected by the duration of pre-shear.
Keywords: FBRM; flocculation; pre-shear; rheology; state of flocculation.