Gallium-doped zinc oxide (GZO) has demonstrated significant potential in gas-sensing applications due to its enhanced electrical and chemical properties. This study focuses on the synthesis, characterization, and gas-sensing performance of GZO nanoparticles (NPs), specifically targeting CO₂ detection, which is crucial for environmental monitoring and industrial safety. The GZO samples were synthesized using a sol–gel method, and their crystal structure was determined through X-ray diffraction (XRD), confirming the successful incorporation of gallium into the ZnO lattice. X-ray photoelectron spectroscopy (XPS) was employed to analyze the samples’ elemental composition and chemical state, revealing the presence of Ga in the ZnO matrix and providing insights into the doping effects. Transmission electron microscopy (TEM) combined with energy-dispersive X-ray spectroscopy (EDS) was used to confirm the purity and elemental distribution of the synthesized samples, ensuring the homogeneity of the Ga doping. In-situ TEM measurements were also conducted on one of the three samples, with the smallest size. The experiment involved exposing the sample to argon (Ar) as a reference gas and carbon dioxide (CO₂) as the target gas to evaluate the sensor’s response under real-time conditions. The in-situ TEM provided nanoscale observation of changes in the crystal structure parameters, particularly the d-spacing, which exhibited significant alterations exceeding 3.2% when exposed to CO₂ and Ar gases. Furthermore, electron paramagnetic resonance (EPR) and optical joint density of states (OJDS) analyses were performed to examine the presence of paramagnetic defects and to comprehensively understand the electronic structure within the GZO sample, respectively.
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