Study of the geopolymer restructuration by impulse rheology

The aim of the study is to describe the evolution of the microstructure during the setting process of the geo-polymer using an original rheological method named Optimal Fourier Rheology (OFR). The alkali activation of meta-kaolin enables physicochemical transformation from a fresh paste to a hard meso-porous matrix. Classically, oscillatory rheology technique provides viscoelastic moduli spectrum and enables to determine rheological comportment of the material under investigation. However the duration to perform a complete spectrum (more than 2.5 h) makes useless this technique in the case of changing material. The OFR technique decreases the measurement duration under 10 minutes and enables to perform several snapshots of the evolving rheological behaviour. Contrary to monochromatic iterations, here the applied stress takes the form of a chirp function which contains the full usable bandwidth. Interpretations of spectrums provide efficient access to structural evolution along the setting. Results show that the number of oligomers increases into the solution due to the dissolution of the meta-kaolin leading to a constant increase of the viscoelastic parameters until the gradual appearance of the percolating networks. The gelling time was rigorously assessed by using the Winter and Chambon criterion. A fractal percolating network is formed inside the material after a reaction time depending on the formulation parameters; corresponding fractal dimensions were established. After the gel point, the viscoelastic moduli grow rapidly until geo-polymers reach a classic viscoelastic state. Structural unit size were determined using moduli curves crossover and equalled to 2.1 nm in the case of Na geo-polymer; this value fits extremely well with value previously obtained by SAXS. Finally, the elasticity becomes constant in a large frequency range and the viscous parameter strongly decreases which means that the solid porous network is under formation. In conclusion, this rheological approach gives an efficient tool to accurate the mechanisms occurring during the geo-polymerization. (authors)