The continuous development of urban areas around the world led to an increase in construction material use and demand, with concrete seeing significant market uptake. Although significant progress has been made to reduce the environmental impact of concrete, there is still a stringent need for improvement. One of the most widely used methods to reduce the environmental impact of the cement industry and the construction industry alike is the replacement of ordinary Portland cement (OPC) by supplementary cementitious materials (SCM). Aside from by-products of industry, SCMs could also come from natural sources. Taking into account the porous structure of zeolites and their contribution to the improvement of the mechanical and durability properties of cement-based materials, the analysis of pore structure in cement pastes incorporating micronized natural zeolite is deemed necessary. In this research, the OPC was replaced by zeolite in three different percentages: 10%, 20%, and 30% by mass. The evolution of pore structure was investigated by means of nuclear magnetic resonance relaxometry at the curing ages of 1, 7, and 28 days. The microstructure of cement pastes was assessed by scanning electron microscopy investigations at 1, 7, 14, 21, and 28 days. The obtained results show that smaller pore sizes are present in cement pastes containing zeolites during the first 7 days. However, at the age of 28 days, the reference mix exhibits a similar pore structure to the mix containing 10% micronized zeolite due to the presence of larger amounts of hydration products. Increasing the replacement percentage to 30% results in larger pores, as indicated by larger values of the relaxation time.

Developing highly efficient Au/TiO₂/WO₃ heterostructures with applications in heterogeneous photocatalysis (photocatalytic degradation) and surface-enhanced Raman spectroscopy (dye detection) is currently of paramount significance. Au/TiO₂/WO₃ heterostructures were obtained via heat or time-assisted synthesis routes developed by slightly modifying the Turkevich–Frens synthesis methods and were investigated by TEM, SEM, XRD, Raman spectroscopy, XPS, photoluminescence, and UV–vis DRS techniques. Structural features, such as WO₃ crystalline phases, TiO₂ surface defects, as well as the WO₃ (220) to TiO₂-A (101) ratio, were the key parameters needed to obtain heterostructures with enhanced photocatalytic activity for removing oxalic acid, phenol, methyl orange, and aspirin. Photodegradation efficiencies of 95.9 and 96.9% for oxalic acid; above 96% (except one composite) for phenol; 90.1 and 97.9% for methyl orange; and 81.6 and 82.1% for aspirin were obtained. By employing the SERS technique, the detection limit of crystal violet dye, depending on the heterostructure, was found to be between 10⁻⁷–10⁻⁸ M. The most promising composite was Au/TiO₂/WO₃-HW-TA it yielded conversion rates of 82.1, 95.9 and 96.8% for aspirin, oxalic acid, and phenol, respectively, and its detection limit for crystal violet was 10⁻⁸ M. Au/TiO₂/WO₃-NWH-HA achieved 90.1, 96.6 and 99.0% degradation efficiency for methyl orange, oxalic acid, and phenol, respectively, whereas its limit of detection was 10⁻⁷ M. The Au/TiO₂/WO₃ heterojunctions exhibited excellent stability as SERS substrates, yielding strong-intensity Raman signals of the pollutant molecules even after a long period of time.

The hydration process of Portland cement is still not completely understood. For instance, it is not clear what produces the induction period, which follows the initial period of fast reaction, and is characterized by a reduced reactivity. To contribute to such understanding, we compare here the hydration process of two cement samples, the simple cement paste and the cement paste containing calcium nitrate as an accelerator. The hydration of these samples is monitored during the induction period using two different low-field nuclear magnetic resonance (NMR) relaxometry techniques. The transverse relaxation measurements of the ¹H nuclei at 20 MHz resonance frequency show that the capillary pore water is not consumed during the induction period and that this stage is shortened in the presence of calcium nitrate. The longitudinal relaxation measurements, performed at variable Larmor frequency of the ¹H nuclei, reveal a continuous increase in the surface-to-volume ratio of the capillary pores, even during the induction period, and this increase is faster in the presence of calcium nitrate. The desorption time of water molecules from the surface was also evaluated, and it increases in the presence of calcium nitrate.

Multifunctional materials based on carbon xerogel (CX) with embedded bismuth (Bi) and iron (Fe) nanoparticles are tested for ultrasensitive amperometric detection of lead cation (Pb²⁺) and hydrogen peroxide (H₂O₂). The prepared CXBiFe-T nanocomposites were annealed at different pyrolysis temperatures (T, between 600 and 1050 °C) and characterized by X-ray diffraction (XRD), Raman spectroscopy, N₂ adsorption, dynamic light scattering (DLS), and electron microscopies (SEM/EDX and TEM). Electrochemical impedance spectroscopy (EIS) and square wave anodic stripping voltammetry (SWV) performed at glassy carbon (GC) electrodes modified with chitosan (Chi)-CXBiFe-T evidenced that GC/Chi-CXBiFe-1050 electrodes exhibit excellent analytical behavior for Pb²⁺ and H₂O₂ amperometric detection: high sensitivity for Pb²⁺ (9.2·10⁵ µA/µM) and outstanding limits of detection (97 fM, signal-to-noise ratio 3) for Pb²⁺, and remarkable for H₂O₂ (2.51 µM). The notable improvements were found to be favored by the increase in pyrolysis temperature. Multi-scale parameters such as (i) graphitization, densification of carbon support, and oxide nanoparticle reduction and purification were considered key aspects in the correlation between material properties and electrochemical response, followed by other effects such as (ii) average nanoparticle and Voronoi domain dimensions and (iii) average CXBiFe-T aggregate dimension.

Multifunctional Bi- and Fe-modified carbon xerogel composites (CXBiFe), with different Fe concentrations, were obtained by a resorcinol–formaldehyde sol–gel method, followed by drying in ambient conditions and pyrolysis treatment. The morphological and structural characterization performed by X-ray diffraction (XRD), Raman spectroscopy, N₂ adsorption/desorption porosimetry, scanning electron microscopy (SEM) and scanning/transmission electron microscopy (STEM) analyses, indicates the formation of carbon-based nanocomposites with integrated Bi and Fe oxide nanoparticles. At higher Fe concentrations, Bi-Fe-O interactions lead to the formation of hybrid nanostructures and off-stoichiometric Bi₂Fe₄O₉ mullite-like structures together with an excess of iron oxide nanoparticles. To examine the effect of the Fe content on the electrochemical performance of the CXBiFe composites, the obtained powders were initially dispersed in a chitosan solution and applied on the surface of glassy carbon electrodes. Then, the multifunctional character of the CXBiFe systems is assessed by involving the obtained modified electrodes for the detection of different analytes, such as biomarkers (hydrogen peroxide) and heavy metal ions (i.e., Pb²⁺). The achieved results indicate a drop in the detection limit for H₂O₂ as Fe content increases. Even though the current results suggest that the surface modifications of the Bi phase with Fe and O impurities lower Pb²⁺ detection efficiencies, Pb²⁺ sensing well below the admitted concentrations for drinkable water is also noticed.

In this study, bismuth- and iron-embedded carbon xerogels (XG) were obtained using a modified resorcinol formaldehyde sol–gel synthesis method followed by additional enrichment with iron content. Pyrolysis treatment was performed at elevated temperatures under Ar or N₂ atmosphere to obtain nanocomposites with different reduction yields (XGAr or XGN). The interest was focused on investigating the extent to which changes in the pyrolysis atmosphere of these nanocomposites impact the structure, morphology, and electrical properties of the material and consequently affect the electroanalytical performance. The structural and morphological particularities derived from X-ray diffraction (XRD), Raman spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), and X-ray photoelectron spectroscopy (XPS) measurements revealed the formation of the nanocomposite phases, mostly metal/oxide components. The achieved performances for the two modified electrodes based on XG treated under Ar or N₂ atmosphere clearly differ, as evidenced by the electroanalytical parameters determined from the detection of heavy metal cations (Pb²⁺) or the use of the square wave voltammetry (SWV) technique, biomarkers (H₂O₂), or amperometry. By correlating the differences obtained from electroanalytical measurements with those derived from morphological, structural, and surface data, a few utmost important aspects were identified. Pyrolysis under Ar atmosphere favors a significant increase in the α-Fe₂O₃ amount and H₂O₂ detection performance (sensitivity of 0.9 A/M and limit of detection of 0.17 μM) in comparison with pyrolysis under N₂ (sensitivity of 0.5 A/M and limit of detection of 0.36 μM), while pyrolysis under N₂ atmosphere leads to an increase in the metallic Bi amount and Pb²⁺ detection performance (sensitivity of 8.44 × 10³ A/M and limit of detection of 33.05 pM) in comparison with pyrolysis under Ar (sensitivity of 6.47·10³ A/M and limit of detection of 46.37 pM).