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.

The objective of this study was to demonstrate the potential utilization of fly ash (FA), wood ash (WA), and metakaolin (MK) in developing new alkali-activated materials (AAMs) for the removal of cadmium ions from waste water. The synthesis of AAMs involved the dissolution of solid precursors, FA, WA, and MK, by a liquid activator (Na₂SiO₃ and NaOH). In concentrated solutions of the activator, the formation of an aluminosilicate gel structure occurred. DRIFT spectroscopy of the AAMs indicated main vibration bands between 1036 cm⁻¹ and 996 cm⁻¹, corresponding to Si-O-Si/Si-O-Al bands. Shifting vibration bands were seen at 1028 cm⁻¹ to 1021 cm⁻¹, indicating that the Si-O-Si/Si-O-Al bond is elongating, and the bond angle is decreasing. Based on the X-ray diffraction results, alkali-activated samples consist of an amorphous phase and residual mineral phases. The characteristic “hump” of an amorphous phase in the range from 20 to 40° 2θ was observed in FA and in all AWAFA samples. By the XRD patterns of the AAMs obtained by the activation of a solid three-component system, a new crystalline phase, gehlenite, was identified. The efficiency of AAMs in removing cadmium ions from aqueous solutions was tested under various conditions. The highest values of adsorption capacity, 64.76 mg/g (AWAFA₆), 67.02 mg/g (AWAFAMK₆), and 72.84 mg/g mg/g (AWAMK₆), were obtained for materials activated with a 6 M NaOH solution in the alkali activator. The Langmuir adsorption isotherm and pseudo-second kinetic order provided the best fit for all investigated AAMs.

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 (H_ex) 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.

The formation of an aluminosilicate gel structure made of alkali-activated materials (AAMs) was conducted through an alkali-activation reaction of the solid precursors (fly ash, metakaolin, and wood ash). Fly and wood ash are by-products of the burning process of coal and wood, respectively. Alkali-activated materials of aluminosilicate origin, made from the different ashes, fly and wood, are very attractive research targets and can be applied in various technological fields due to their thermal stability, resistance to thermal shock, high porosity, high sustainability, and finally, low energy loss during production. In this paper, we evaluate physico-chemical properties, microstructure, and radiological environmental impacts when wastes that contain elevated levels of naturally occurring radionuclides (NORs) such as fly ash and wood ash are made into “green cements” such as AAMs. The determination of radionuclide content was performed by means of gamma-ray spectrometry. Results showed that the AAMs have a lower value in the activity concentration of radionuclides than raw materials. The external absorbed gamma dose rate was 74.7–107.3 nGy/h, and the external radiation hazard index values were in range of 0.445–0.628 Bq/kg. The results of the activity concentration measurements for alkali-activated materials indicate the potential of their safe application in building construction. In terms of the structural characterizations, the obtained alkali-activated materials were examined using XRD, DRIFT, FESEM, and TEM analyses.

This study investigates the gel characteristics of alkali-activated materials (AAMs) synthesized using wood ash (WA), and metakaolin (MK) as solid precursors. The research explores the influence of precursor type and sodium hydroxide (NaOH) concentrations in the alkali activator solution on the resulting physicochemical, microstructural, mechanical, and radiological properties of gels. The alkaline activators were prepared by mixing sodium hydroxide solutions (6 M and 12 M) with a sodium silicate (water glass) solution at a volume ratio of 1.5. The physicochemical characteristics of raw materials and AAMs were thoroughly analyzed using X-ray fluorescence (XRF), Diffuse Reflectance Infrared Fourier Transform (DRIFT) spectroscopy, X-ray diffraction (XRD), and scanning electron microscopy (SEM) with EDS elemental mapping. FTIR analysis confirmed the formation of an amorphous gels geopolymer network. XRD revealed the presence of characteristic crystalline phases (quartz, calcite) within an amorphous matrix. Mechanical properties, such as compressive strength, depended on precursor type and alkali molarity: metakaolin (12 M) reached ~14 MPa, while wood ash showed ~4 MPa (6 M) and ~0.5 MPa (12 M) due to high CaO, low Si and Al, and unfavorable SiO₂/Al₂O₃ (5.71) and Na₂O/Al₂O₃ (3.19) ratios. Furthermore, this research estimates radiological doses by quantifying radionuclide content via gamma-spectrometry. Alkali activation significantly reduced radiological hazard parameters, with radium equivalent activity (Ra_eq) decreasing to 238.0 Bq/kg and the external hazard index (H_ex) to 0.643 for A₁₂MK, while the annual effective dose rate for A₁₂WA was only 0.265 nSv/y-all values remaining well below the recommended safety limit of 370 Bq/kg (≤1 mSv/y). The decrease in activity concentration index (I_γ), Ra_eq, and H_ex with increasing NaOH concentration indicates effective radionuclide immobilization within the geopolymer matrix, confirming the suitability of these alkali-activated materials for safe use in construction from a radiation protection perspective.

A promising approach for the removal of Cs⁺ ions from aqueous solutions and their long-term immobilization was investigated, as the safe containment of radioactive cesium is essential due to its long half-life and environmental hazards. The approach involves ion exchange using zeolite, geopolymerization, and subsequent heat treatment of the geopolymer/zeolite composite. Cs⁺ ions were removed from water by ion exchange using Na-13X zeolite, in which Cs⁺ ions replaced Na⁺ ions within the zeolite framework. The resulting Cs-13X zeolite was subsequently combined with kaolinite to prepare geopolymer/Cs-13X zeolite composites containing 10–50 wt% Cs-13X zeolite. During geopolymerization, a portion of the Cs was released from Cs-13X zeolite and incorporated into the geopolymer matrix, while the remaining Cs remained immobilized within the zeolite structure. Heat treatment of the geopolymer/Cs-13X zeolite composites at 950 °C induced crystallization of two stable Cs-bearing phases. The Cs incorporated into the geopolymer matrix crystallized as the CAS phase, whereas the Cs retained in the Cs-13X zeolite crystallized as pollucite. The crystalline phase content in the heat-treated composite samples increased with Cs-13X zeolite loading, resulting in improved density and compressive strength. The highest values of crystallinity (72%), bulk density (2.42 g/cm³), and compressive strength (~53 MPa) were measured for samples containing 50 wt% Cs-13X zeolite. This level of compressive strength is sufficient to ensure safe handling and long-term containment of the immobilized Cs⁺ ions.