The destabilization of kaolinite suspension by anionic flocculant addition occurs in three zones: free settling, hindered settling and compression which usually includes a final bed raking process in mineral processing practice. This paper reports changes in the kaolinite aggregate and Hoc structures in the different settling and raking zones by cryo-vitrification/cryo-SEM techniques with image analysis combining micro- and macro-flocs. Cryo-SEM images indicate that, even during free settling. fine clay particles are bridged predominantly in edge-edge (E-E) with some face-face (F-F) configurations forming single, small flocs and some chain structures. When these small flocs and chains settle into the hindered settling zone. the collision between flocs and chains results in "honeycomb" network structures formed with lateral chain-like extension. The settled bed consists of these honeycomb structures with both inter-aggregate and intra-aggregate trapped water and has relatively low bed density (e.g. <12 wt.% for a 2 wt.% slurry). The effect of the raking process in dramatically improving thickener underflow solids has been extensively studied but the structural changes ill flocs and aggregates in this process are less well defined. Raking the compression zone for 1 h at 3 rpm can release some of the trapped water in the "honeycomb" structure and the bed density for 2 wt.% slurry improves dramatically to more than 36 wt.%. Cryo-SEM illustrates the extensive restructuring of flocs from predominantly E-E to predominantly F-F in many areas. The STructural IMage ANalysis (STIMAN) software is used to combine a series of images at magnifications from 1000x to 8000x. including both macro- and micro-flocs. This structural analysis comparing the un-raked and raked bed samples gives increases in total particle area of 30% and in relative particle area of 6%. The relatively low energy rake action of the shear stress results in the disruption of the E-E chains and the honeycomb structure. partly releasing the trapped water and inducing some E-E to F-F aggregate restructuring are clearly illustrated in these results. (C) 2009 Elsevier B.V. All rights reserved.