ZnO nanospheres were synthesised and then deposited by both single- and double-fire fast processes on as-prepared ceramic substrates. The photocatalytic degradation of resazurin ink was tested under UV light. The single-fired samples did not show any evidence of photocatalytic activity because the nanoparticles melted during sintering at 1210°C. The double-fire ZnO spray-coating method successfully produced glazed materials with an active ZnO surface layer despite the high sintering temperature. The influence of experimental parameters, including the ZnO nanoparticle loading (0.03 to 1 mg/cm2) and firing temperature (650 to 800°C), were also investigated. Samples with a ZnO loading of 1 g/cm2 fired at 650°C showed the best photocatalytic activity. Increasing the temperature to 700 and 800°C led to the coalescence of ZnO nanoparticles, which reduced the photocatalytic activity.

The increasing need for sustainable construction materials has prompted research into alternatives to Ordinary Portland Cement (OPC), a major contributor to global CO₂ emissions. Geopolymers, synthesized via alkali activation of aluminosilicate precursors such as metakaolin and fly ash, are a promising alternative, reducing up to 80% of carbon emissions. However, their long-term durability in aggressive chemical environments, particularly when up against organic acids, remains insufficient. While mineral and inorganic acid resistance have been studied, the impact of naturally occurring organic acids like oxalic acid (Ox)—commonly found in soils and organic-rich sediments—has received limited attention. Ox is known to chelate metal ions and alter mineral phases, potentially affecting the integrity of geopolymer matrices. This study investigates the degradation behavior of geopolymers under continuous exposure to Ox (0.2, 0.4, and 0.6 M) at 25 °C using a flow-through reactor. Mass loss over time was monitored to determine reaction kinetics, while SEM, FT-IR, XRD, and EDS analyses were conducted to evaluate microstructural and chemical changes. The results revealed significant alterations in the geopolymers’ structures due to Ox exposure, providing key insights into their vulnerability to organic acid attack. These findings indicate the importance of considering organic acid interactions in long-term performance assessments of geopolymers.