Search Results (3)

Alkaline sodium hydroxide/sodium silicate-activating high-purity metakaolin geopolymerization is described in terms of metakaolin deconstruction in tetrahedral hydrate silicate [O[Si(OH)₃]]⁻ and aluminate [Al(OH)₄]⁻ ionic precursors followed by their reassembling in linear and branched sialates monomers that randomly copolymerize into an irregular crosslinked aluminosilicate network. The novelty of the approach resides in the concurrent thermo-calorimetric (differential scanning calorimetry, DSC) and rheological (dynamic mechanical analysis, DMA) characterizations of the liquid slurry during the transformation into a gel and a structural glassy solid. Tests were run either in temperature scan (1 °C/min) or isothermal (20 °C, 30 °C, 40 °C) cure conditions. A Gaussian functions deconvolution method has been applied to the DSC multi-peak thermograms to separate the kinetic contributions of the oligomer’s concurrent reactions. DSC thermograms of all tested materials are well-fitted by a combination of three overlapping Gaussian curves that are associated with the initial linear low-molecular-weight (Mw) oligomers (P1) formation, oligomers branching into alumina-rich and silica-rich gels (P2), and inter- and intra-molecular crosslinking (P3). The loss factor has been used to define viscoelastic behavioral zones for each DMA rheo-thermogram operated in the same DSC thermal conditions. Macromolecular evolution and viscoelastic properties have been obtained by pairing the deconvoluted DSC thermograms with the viscoelastic behavioral zones of the DMA rheo-thermograms. Two main chemorheological behaviors have been identified relative to pre- and post-gelation separation of the viscoelastic liquid from the viscoelastic solid. Each comprises three behavioral zones, accounting for the concurrently occurring linear and branching oligomerization, aluminate-rich and silica-rich gel nucleations, crosslinking, and vitrification. A “rubbery plateau” in the loss factor path, observed for all the testing conditions, identifies a large behavioral transition zone dividing the incipient gelling liquid slurry from the material hard setting and vitrification. Full article

Kaolin is an industrial mineral used in a wide variety of applications due to its crystalline structure, mineral and elemental composition. After kaolin undergoes heat treatment in a specific temperature range, metakaolin, which exhibits a strong pozzolanic reaction, is formed. This paper examines the effects of different kaolin qualities on the thermal activation process of metakaolin production. The qualities of kaolin depend on the impurities they contain, such as mica, feldspar and quartz. In this study, four different samples of kaolin are investigated. Each sample was heat treated in a lab-scale rotary kiln in order to study the chemical, structural and morphological changes that occurred and their influence on pozzolanic activity. The parameters being considered in the experimental process were the temperature and the duration of the treatment. Thus, the calcination process for each of the four kaolin types was carried out at 600, 650 and 700 °C for 3 h. The occurred changes were monitored using XRD, FTIR and DTA analysis. Additionally, the reactivity of all thermally treated samples was evaluated based on the Chapelle test. The results showed that the fewer the impurities, the easier the transformation of the material to metakaolin. The optimum result was the metakaolin, which originated from the purest quality of kaolin and was comparable to the commercial product. Finally, the pozzolanic activity of the thermally activated samples also depended on the purity of the kaolin. Full article

This paper investigates alkali leaching from geopolymers under various concentrations of acetic acid solutions. The effects of the raw metakaolin purity as well as fly ash-based geopolymer mortars and pastes are considered. A new methodology for (acetic) acid attack is proposed, adapting standard approaches, where the concentration of the leached alkali in the exposure solution is measured over time. The applicability of a simple diffusion-based mathematical model to determine the apparent diffusion coefficient (D_app) for geopolymer pastes and mortars was validated. At the end of the paste tests, microstructural alterations of the specimens’ cross-sections were analyzed microscopically, revealing occurrence of degradation across the outermost surface parts and, especially under acid attack, the formation of long cracks that connect the surface with the intact inner zone. Drastically different D_app are discussed in terms of the differences in the mix designs, principally resulting in different alkali-binding capacities of the geopolymers, while the acid promoted dissolution and increased porosity. As a result of this interpretation, it was concluded that D_app is governed mainly by the chemistry of the alkali release from the gel, as it overruled the effects of porosity and cracks. Full article