Catalina Gabriela Mihalcea

The tuning sensitivity towards CO₂ detection under in-field-like conditions was investigated using SnO₂-sensitive material deposited onto Al₂O₃ substrates provided with platinum electrodes with interdigital gaps of 100 µm and 30 µm. X-ray diffraction, low-magnification and high-resolution transmission electron microscopy, and electrical and contact potential difference investigations were employed to understand the sensing mechanism involved in CO₂ detection. The morpho-structural analysis revealed that the SnO₂ nanoparticles exhibit well-defined facets along the (110) and (101) crystallographic planes. Complex phenomenological investigations showed that moisture significantly affects the gas sensing performance. The experimental results corroborated the literature evidence, highlighting the importance of Pt within the interdigital electrodes subsequently reflected in the increase in the CO₂ sensing performance with the decrease in the interdigital gap. The catalytic efficiency is explained by the distribution of platinum at the gas-Pt-SnO₂ three-phase boundary, which is critical for enhancing the sensor performance.

This study investigates the influence of synthesis methods and electrode geometry on the physico-chemical properties of 5%Gd-doped SnO₂. Two distinct synthesis routes, co-precipitation and hydrothermal growth, were employed, resulting in powders denoted as SnO₂: Gd 5%-CP and SnO₂: Gd 5%-HT. Morpho-structural and textural analyses reveal a uniform morphology consisting of quasi-spherical nanoparticles with dimensions of ~6 nm and mesoporosity for CP and a non-uniform morphology with larger nanoparticles of ~42 nm, with irregular shapes and macroporosity for the HT sample, respectively. The powders were deposited onto alumina substrates equipped with platinum interdigital electrodes with alternative gaps of 200 μm and 100 μm. The back-side heater allows for variation in the temperature of the layer. Sensing properties assessed under in-field-like atmospheres simulated by a computer-controlled Gas Mixing System reveal higher sensitivity to methane compared to carbon dioxide. Although the sensor signals did not differ quantitatively, they exhibited distinct saturation tendencies with an increasing methane concentration, attributed to the morpho-structure and porosity induced by the synthesis method. Differentiation was achieved by varying the interdigital gap of the electrodes, highlighting different sensor signals and conduction mechanisms, determined by the specific size of the crystallites.

Titanium dioxide nanobelts were prepared via the alkali-hydrothermal method for application in chemical gas sensing. The formation process of TiO₂-(B) nanobelts and their sensing properties were investigated in detail. FE-SEM was used to study the surface of the obtained structures. The TEM and XRD analyses show that the prepared TiO₂ nanobelts are in the monoclinic phase. Furthermore, TEM shows the formation of porous-like morphology due to crystal defects in the TiO₂-(B) nanobelts. The gas-sensing performance of the structure toward various concentrations of hydrogen, ethanol, acetone, nitrogen dioxide, and methane gases was studied at a temperature range between 100 and 500 °C. The fabricated sensor shows a high response toward acetone at a relatively low working temperature (150 °C), which is important for the development of low-power-consumption functional devices. Moreover, the obtained results indicate that monoclinic TiO₂-B is a promising material for applications in chemo-resistive gas detectors.

The aim of this paper is to provide a simple and efficient photoassisted approach to synthesize silver nanoparticles, and to elucidate the role of the key factors (synthesis parameters, such as the concentration of TSC, irradiation time, and UV intensity) that play a major role in the photochemical synthesis of silver nanoparticles using TSC, both as a reducing and stabilizing agent. Concomitantly, we aim to provide an easy way to evaluate the particle size based on Mie theory. One of the key advantages of this method is that the synthesis can be “activated” whenever or wherever silver nanoparticles are needed, by premixing the reactants and irradiating the final solution with UV radiation. UV irradiance was determined by using Keitz’s theory. This argument has been verified by premixing the reagents and deposited them in an enclosed space (away from sunlight) at 25 °C, then checking them for three days. Nothing happened, unless the sample was directly irradiated by UV light. Further, obtained materials were monitored for 390 days and characterized using scanning electron microscopy, UV-VIS, and transmission electron microscopy.

In this study, two alternative synthesis routes have been used in obtaining gas-sensitive NiO materials. The structural and morphological aspects were systematically investigated by X-ray diffraction (XRD) and transmission electron microscopy (TEM), revealing significant differences further mirrored in their sensing performances. Simultaneous electrical resistance and contact potential differences have been involved aiming to decouple the energetic contributions: work function (ΔΦ), surface band bending (qΔVs) and electron affinity (Δχ). Two sensing mechanism scenarios explained the enhancement and downgrading in the sensor response to carbon monoxide (CO) concerning the synthesis strategies. The role of relative humidity (RH) was considered throughout the electrical operando (in-field) investigations.

Special attention has recently been paid to surface-defective titanium dioxide and black TiO₂ with advanced optical, electrical, and photocatalytic properties. Synthesis of these materials for photodegradation and mineralization of persistent organic pollutants in water, especially under visible radiation, presents interest from scientific and application points of view. Chemical reduction by heating a TiO₂ and NaBH₄ mixture at 350 °C successfully introduced Ti³⁺ defects and oxygen vacancies at the surface of TiO₂, with an increase in the photocatalytic degradation of amoxicillin—an antibiotic that is present in wastewater due to its intense use in human and animal medicine. Three TiO₂ samples were prepared at different annealing temperatures to control the ratio between anatase and rutile and were subjected to chemical reduction. Electron paramagnetic resonance investigations showed that the formation of surface Ti³⁺ defects in a high concentration occurred mainly in the anatase sample annealed at 400 °C, contributing to the bandgap reduction from 3.32 eV to 2.92 eV. The reduced band gap enhances visible light absorption and the efficiency of photocatalysis. The nanoparticles of ~90 m²/g specific surface area and 12 nm average size exhibit ~100% efficiency in the degradation of amoxicillin under simulated solar irradiation compared with pristine TiO₂. Mineralization of amoxicillin and by-products was over 75% after 48 h irradiation for the anatase sample, where the Ti³⁺ defects were present in a higher concentration at the catalyst’s surface.

The aim of this experimental work was to investigate the influence of the ion beam charge state on damage production in nanomaterials. To achieve this, we employed Raman spectroscopy, atomic force microscopy, and transmission electron microscopy to investigate nanomaterials irradiated by a 23 MeV I beam. We found a significant influence of the ion charge state on damage production in monolayer graphene, but found no evidence of this effect in bilayer and trilayer graphene, nor in graphite. Furthermore, we found no evidence of this effect in CaF₂ and SiO₂ nanocrystals irradiated with the same ion beam.

NiO-sensitive materials have been synthesized via the hydrothermal synthesis route and calcined in air at 400 °C and, alternatively, at 500 °C. Structural, morphological, and spectroscopic investigations were involved. As such, the XRD patterns showed a higher crystallinity degree for the NiO calcined at 500 °C. Such an aspect is in line with the XPS data indicating a lower surface hydroxylation relative to NiO calcined at 400 °C. An HRTEM microstructural investigation revealed that the two samples differ essentially at the morphological level, having different sizes of the crystalline nanoparticles, different density of the surface defects, and preferential faceting according to the main crystallographic planes. In order to identify their specific gas-sensing mechanism towards CO exposure under the in-field atmosphere, the simultaneous evaluation of the electrical resistance and contact potential difference was carried out. The results allowed the decoupling of the water physisorption from the chemisorption of the ambient oxygen species. Thus, the specific CO interaction mechanism induced by the calcination temperature of NiO has been highlighted.

Polycrystalline NiO thick film-based gas sensors have been exposed to different test gas atmospheres at 250 °C and measured via simultaneous electrical resistance and work function investigations. Accordingly, we decoupled different features manifested toward the potential changes, i.e., work function, band-bending, and electron affinity. The experimental results have shown that the presence of moisture induces an unusual behavior toward carbon monoxide (CO) detection by considering different surface adsorption sites. On this basis, we derived an appropriate detection mechanism capable of explaining the lack of moisture influence over the CO detection with NiO-sensitive materials. As such, CO might have both chemical and dipolar interactions with pre-adsorbed or lattice oxygen species, thus canceling out the effect of moisture. Additionally, morphology, structure, and surface chemistry were addressed, and the results have been linked to the sensing properties envisaging the role played by the porous quasispherical–hollow structures and surface hydration.

Cation-substituted hydroxyapatite (HA), standalone or as a composite (blended with polymers or metals), is currently regarded as a noteworthy candidate material for bone repair/regeneration either in the form of powders, porous scaffolds or coatings for endo-osseous dental and orthopaedic implants. As a response to the numerous contradictions reported in literature, this work presents, in one study, the physico-chemical properties and the cytocompatibility response of single cation-doped (Ce, Mg, Sr or Zn) HA nanopowders in a wide concentration range (0.5–5 at.%). The modification of composition, morphology, and structure was multiparametrically monitored via energy dispersive X-ray, X-ray photoelectron, Fourier-transform infrared and micro-Raman spectroscopy methods, as well as by transmission electron microscopy and X-ray diffraction. From a compositional point of view, Ce and Sr were well-incorporated in HA, while slight and pronounced deviations were observed for Mg and Zn, respectively. The change of the lattice parameters, crystallite size, and substituting cation occupation factors either in the Ca(I) or Ca(II) sites were further determined. Sr produced the most important HA structural changes. The in vitro biological performance was evaluated by the (i) determination of leached therapeutic cations (by inductively coupled plasma mass spectrometry) and (ii) assessment of cell behaviour by both conventional assays (e.g., proliferation—3-(4,5-dimethyl thiazol-2-yl) 5-(3-carboxymethoxyphenyl)-2-(4-sulfophenyl)-2H-tetrazolium assay; cytotoxicity—lactate dehydrogenase release assay) and, for the first time, real-time cell analysis (RTCA). Three cell lines were employed: fibroblast, osteoblast, and endothelial. When monophasic, the substituted HA supported the cells’ viability and proliferation without signs of toxicity. The RTCA results indicate the excellent adherence of cells. The study strived to offer a perspective on the behaviour of Ce-, Mg-, Sr-, or Zn-substituted HAs and to deliver a well-encompassing viewpoint on their effects. This can be highly important for the future development of such bioceramics, paving the road toward the identification of candidates with highly promising therapeutic effects.