In this paper, raw natural metakaolin (MK, Serbia) clay was used as a starting material for the synthesis of geopolymers for thermal treatment. Metakaolin was obtained by calcination of kaolin at 750 °C for 1 h while geopolymer samples were calcined at 900 °C, which is the key transition temperature. Metakaolin was activated by a solution of NaOH of various concentrations and sodium silicate. During the controlled heat treatment, the geopolymer samples began to melt slightly and coagulate locally. The high-temperature exposure of geopolymer samples (900 °C) caused a significant reduction in oxygen, and even more sodium, which led to the formation of a complex porous structure. As the concentration of NaOH (6 mol dm−3 and 8 mol dm−3) increased, new semi-crystalline phases of nepheline and sanidine were formed. Thermal properties were increasingly used to better understand and improve the properties of geopolymers at high temperatures. Temperature changes were monitored by simultaneous use of thermogravimetric analysis (TGA) and differential thermal analysis (DTA). The loss of mass of the investigated samples at 900 °C was in the range of 8–16%. Thermal treatment of geopolymers at 900 °C did not have much effect on the change in compressive strength of investigated samples. The results of thermal treatment of geopolymers at 900 °C showed that this is approximately the temperature at which the structure of the geopolymer turns into a ceramic-like structure. All investigated properties of the geopolymers are closely connected to the precursors and the constituents of the geopolymers.

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The aim of the presented research was to investigate the application possibility of wood ash and metakaolin to obtain alkali-activated materials as relatively new materials in the building industry. Thus, in order to assess the adequate use of these waste materials, structural and radiological characteristics should be considered. Until now, the focus has been on ash from thermal power plants produced by burning coal, but a large part of households in our country have individual fireplaces in which wood is used as the basic raw material; thus, it is very interesting to measure the activity concentration of radionuclide in wood ash as well as the possibility of reusing that ash for other purposes. All materials were studied, in terms of physical and chemical characteristics, by methods such as X-ray diffraction (XRD), Fourier transform infra-red (FTIR) spectroscopy, and scanning electron microscopy and energy-dispersive X-ray spectroscopy (SEM/EDS). XRD measurements of wood ash samples showed that it consists of calcite and larnite. FTIR spectroscopy revealed a polymeric Si–O–Al framework in alkali-activated materials and Si–O bonding bands corresponding to silicon dioxide. Determination of radionuclide content was performed by means of gamma-ray spectrometry. Results showed that the alkaline activation process led to the decrease in the activity concentration of radionuclides detected in the measured samples. External radiation hazard index (Hex) for wood ash was reduced by more than 50% after alkali activation. The results of activity concentration measurements in alkali-activated materials indicate potential for their safe application in building construction.