4.7 Article

Curing process and pore structure of metakaolin-based geopolymers: Liquid-state 1H NMR investigation

Journal

CEMENT AND CONCRETE RESEARCH
Volume 143, Issue -, Pages -

Publisher

PERGAMON-ELSEVIER SCIENCE LTD
DOI: 10.1016/j.cemconres.2021.106394

Keywords

Metakaolin-based geopolymers; NMR relaxometry; Cryoporometry; Curing; Pore structure

Funding

  1. University of Oulu Kvantum Institute under Emerging projects-program (Zero-CO2 cement concept via phaseseparated nano-glass)
  2. Academy of Finland [321701, 322085, 329477, 326291, 289649, 294027, 319216]
  3. European Research Council (ERC) under Horizon 2020 (H2020/2018-2022/ERC) [772110]
  4. COST Action (EURELAX) [CA15209]
  5. Academy of Finland (AKA) [321701, 321701] Funding Source: Academy of Finland (AKA)

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Geopolymers based on metakaolin with a water-to-solid ratio of 0.59-0.66 were studied during the curing process. Monitoring of the curing process and pore structures was done using NMR relaxometry and cryoporometry, showing changes in relaxation times and pore sizes as the geopolymers matured during curing.
Geopolymers are emerging construction materials with lower carbon dioxide emissions compared to the conventional cementitious materials. The knowledge of the curing process and the related pore structures are important for optimizing the properties of these materials for different applications. The curing process and final pore structure are sensitive to the amount of used water, however the specifics are unclear. The curing process and pore structures of metakaolin-based geopolymers with a narrow water-to-solid (w/s) ratio (0.59-0.66) were monitored by nuclear magnetic resonance (NMR) relaxometry and cryopommetry. The 14-day curing process was investigated by monitoring the change of T-2 and T-1 relaxation times and water signal intensity. After the curing, the pore structures were characterized by 2D T-1-T-2 correlation and T-2-T-2 exchange measurements of absorbed water. The pore size distributions (PSDs) were measured with NMR cryoporometry and compared to nitrogen physisorption and mercury intrusion pomsimetry (MIP) results. We found that the relaxation times decreased as the pore structure of the geopolymers matured during the curing while the dissolution and the condensation periods of the curing were distinguished by the changes in signal amplitude reflecting the proton density. After the curing, three distinct pore sizes and connectivity between pores were identified from T-1-T-2 and T-2-T-2 spectra. Their PSDs were measured, and they were found to correspond to two different pore sizes originating from the arrangement of clusters and defective pores. In the narrow w/s ratio (0.59-0.66), the curing times were the same for all samples when cured at 24 degrees C while the pore sizes were observed to increase as a function of the w/s ratio.

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