National Institute Of Materials Physics - Romania

TiO2 nanoparticles (NPs) doped with W (W:TiO2), double-doped with W and V (W&V:TiO2), and loaded with noble metals (W:TiO2 @Pt/Pd/Ag and W&V:TiO2@Pt/Pd/Ag) were synthesized by laser pyrolysis followed by chemical impregnation and reduction. Due to its exceptional properties, TiO2 is considered a key material being used in a wide range of applications. To improve its detection activity, the increase in the specific surface of the material, and the presence of defects in its structure play a decisive role. Doped and double-doped TiO2 nanoparticles with dimensions in the range of 25-30 nm presented a mixture of phases corresponding to titania, with the anatase phase accounting for the majority (95%). By loading these nanoparticles with small particles of noble metals, a significant increase in the specific surface area by three or even five times the original values was achieved. Sensitive thin films for surface acoustic wave (SAW) sensors were made with the NPs, embedded in polyethyleneimine (PEI) polymer and deposited by spin-coating. Each sensor was tested at CH4 concentrations between 0.4 and 2%, at room temperature, and the best results were obtained by the sensor with NPs doped with V and decorated with Pd, with a limit of detection (LOD) of 17 ppm, due to the strong catalytic effect of Pd.

In view of their potential applicability in technology fields where magnets are required to operate at higher temperatures, the class of nanocomposite magnets with little or no rare earth (RE) content has been widely researched in the last two decades. Among these nanocomposite magnets, the subclass of magnetic binary systems exhibiting the formation of L10 tetragonal phases is the most illustrious. Some of the most interesting systems are represented by the Mn-based alloys, with addition of Al, Bi, Ga, Ge. Such alloys are interesting as they are less costly than RE magnets and they show promising magnetic properties. The paper tackles the case of MnGa binary alloys with various compositions around the Mn3Ga stoichiometry. Four MnGa magnetic alloys, with Mn content ranging from 70 at% to 75 at% were produced using rapid solidification to form the melt. By combining structural information arising from X-ray diffractometry and transmission electron microscopy with magnetic properties determined by vibrating sample magnetometry, we are able to document the nature and properties of the structural phases formed in the alloys in their as-cast state and upon annealing, the evolution of the phase structure after annealing and its influence on the magnetic behavior of the MnGa alloys. After annealing at 400 degrees C and 500 degrees C, MnGa alloys are showing a multiple-phase microstructure, consisting of co-existing crystallites of L10 and D022 tetragonal phase. As a consequence of these structurally and magnetically different phases, co-existing within the microstructure, promising magnetic features are obtained, with both coercive fields and saturation magnetization exceeding values previously reported for both alloys and layers of MnGa.

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 similar to 6 nm and mesoporosity for CP and a non-uniform morphology with larger nanoparticles of similar to 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 mu m and 100 mu m. 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.

Magnesium doped hydroxyapatite nanoparticles in dextran matrix (7MgHApDx) with average size diameter of 18.2 +/- 0.5 nm are synthesized by co-precipitation. The surface morphology and shape of 7MgHApDx particles are established by scanning electron microscopy (SEM). The stability that is evaluated by ultrasound measurements and zeta potential reveals a good stability. More than that, the functional groups present in the studied samples are identified by Fourier transform infrared spectroscopy studies. The antimicrobial properties of 7MgHApDx suspensions are determined against Staphylococcus aureus ATCC 25923, Escherichia coli ATCC 25922, and Candida albicans ATCC 10231 microbial strains.

The aim of this study is to develop a new nanobiocomposite based on silver doped hydroxyapatite (AgHAp)/chitosan (CH), AgHAp-CH (x(Ag) = 0.15) by an adapted method. The obtained nanobiocomposites are studied by scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FTIR) studies. The good stability of AgHAp-CH suspension is established by ultrasound and zeta potential measurements. More than that, the antimicrobial activity of AgHAp-CH nanobiocomposites against Staphylococcus aureus ATCC 25923, Escherichia coli ATCC 25922, and Candida albicans ATCC 10231 microbial strains is evaluated. AgHAp-CH nanobiocomposites demonstrate an effective antibacterial effect against the studied microbial strains. Considering the facile method involved in the development of these nanobiomaterials and their excellent properties, it is suggested that they can be suitable candidates for applications in the biomedical field.

The hydroxyapatite and copper-doped hydroxyapatite coatings (Ca10-xCux(PO4)6(OH)2; xCu = 0, 0.03; HAp and 3CuHAp) were obtained by the vacuum deposition technique. Then, both coatings were analyzed by the X-ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectroscopy (FTIR) and water contact angle techniques. Information regarding the in vitro antibacterial activity and biological evaluation were obtained. The XRD studies confirmed that the obtained thin films consist of a single phase associated with hydroxyapatite (HAp). The obtained 2D and 3D SEM images did not show cracks or other types of surface defects. The FTIR studies' results proved the presence of vibrational bands characteristic of the hydroxyapatite structure in the studied coating. Moreover, information regarding the HAp and 3CuHAp surface wettability was obtained by water contact angle measurements. The biocompatibility of the HAp and 3CuHAp coatings was evaluated using the HeLa and MG63 cell lines. The cytotoxicity evaluation of the coatings was performed by assessing the cell viability through the MTT assay after incubation with the HAp and 3CuHAp coatings for 24, 48, and 72 h. The results proved that the 3CuHAp coatings exhibited good biocompatible activity for all the tested intervals. The ability of Pseudomonas aeruginosa 27853 ATCC (P. aeruginosa) cells to adhere to and develop on the surface of the HAp and 3CuHAp coatings was investigated using AFM studies. The AFM studies revealed that the 3CuHAp coatings inhibited the formation of P. aeruginosa biofilms. The AFM data indicated that P. aeruginosa's attachment and development on the 3CuHAp coatings were significantly inhibited within the first 24 h. Both the 2D and 3D topographies showed a rapid decrease in attached bacterial cells over time, with a significant reduction observed after 72 h of exposure. Our studies suggest that 3CuHAp coatings could be suitable candidates for biomedical uses such as the development of new antimicrobial agents.

The development of kesterite (Cu2ZnSn(S,Se)4, CZTSSe) thin films for photovoltaic applications is highly necessary, given their composition of Earth-abundant, environmentally friendly elements and their compatibility with established photovoltaic technologies. This study presents a novel synthesis approach for CZTSSe films with varied S/(S+Se) ratios, ranging from 0.83 to 0.44, by a two-step magnetron sputtering deposition/annealing process. The first step consists in an initial deposition of stacked Mo/SnS2/Cu layers, which, upon thermal treatment in a sulfur atmosphere, were transformed into Cu2SnS3 (CTS) films. In the second step, further deposition of ZnSe and subsequent annealing in a tin and selenium atmosphere resulted in the formation of a CZTSSe phase. These processes were optimized to fabricate high-quality and single-phase CZTSSe films, thereby mitigating the formation of secondary phases. Characterization techniques, including scanning electron microscopy, demonstrated a clear correlation between decreased S/(S+Se) ratios and enhanced film densification and grain size. Moreover, grazing incidence X-ray diffraction and Raman spectroscopy confirmed a compositional and structural transition from close to CZTS to nearly a CZTSe phase as the S/(S+Se) ratios decreased. This study advances kesterite-based solar cell technology by enhancing the structural properties and crystallinity of the absorber layer, necessary for improving photovoltaic performance.

The compounds KBa 1-x Sr x Cr 2 (PO 4 ) 3 (with x = 0.00; 0.25; 0.50; 0.75; 1.00) were synthesized by a solid-state reaction, and they were thoroughly characterized by different spectroscopic and microscopic techniques. Their structures were indexed in a cubic system with a P2 1 3 space group forming a 3D framework built on CrO 6 octahedra and PO 4 tetrahedra sharing vertices leading to identical Cr 2 P 3 O 18 (U) units. The interconnection between the tetrahedral and octahedral groups leads to the formation of two large closed cavities (K, M II )(1) and (K, M II )(2), statistically occupied by K + and M 2+ (M = Ba, Sr) atoms. Electron paramagnetic resonance spectroscopy confirmed the presence of paramagnetic Cr 3+ ions, showing the effects of substituting the Ba 2+ ions with smaller Sr 2+ ions on the dipolar coupling between the Cr 3+ centers. The obtained materials and active carbon were used as electrode materials in hybrid SC devices. At the same time, their electrochemical properties were assessed by potentiostatic electrochemical impedance spectroscopy, cyclic voltammetry, and galvanostatic charge-discharge measurements, showing promising results with a maximal specific capacitance (3.86 F/g), energy density (343 mWh/kg), and power density (30.9 kW/kg) in the case of KBa 0.5 Sr 0.5 Cr 2 (PO 4 ) 3 , proving them as good candidates for positive and/or negative electrode materials for energy storage applications.

Quaternary multicomponent Cu2BaSnS4 (CBTS) has emerged as a potential absorber material due to its abundant and nontoxic constituents, high absorption coefficient (10-4 cm-1) and suitable bandgap (1.5-2.0 eV) for the solar photovoltaic application. In this study, polycrystalline CBTS thin layers have been deposited by a typical spray pyrolysis technique on glass substrates using different substrate temperatures (Ts = 200, 250, 300 and 350 degrees C) followed by annealing in a sulfur-rich atmosphere at 550 degrees C under an argon flow. The (micro-)structural, compositional, and optical properties of both types of films have been studied. Analysis of x-ray diffractogram (XRD) patterns for all acquired films showed the presence of polycrystalline CBTS alongside various secondary phases, including Cu2SnS3 being predominant. Nonetheless, the XRD of the films deposited at 250 degrees C and annealed at 550 degrees C showed only the CBTS phase. Raman spectroscopy confirm the formation of the trigonal phase of CBTS. The presence of Cu, Ba, Sn and S in CBTS thin films was confirmed by X-ray photoelectron spectroscopy and Energy-dispersive X-ray spectroscopy. Scanning electron micrographs show a smooth and dense structure with enhanced crystallinity and improved uniformity. Overall, the physical properties of CBTS thin films were found to be spray deposition temperature dependent. An appropriate optical band gap of 1.6 to 1.8 eV and a compact structure indicate their prospective for solar cell applications.

This work presents the synthesis of tungsten nanoparticles (W NPs) using a cluster source based on magnetron sputtering combined with gas aggregation (MSGA), operated with up to 81% H-2 in the hydrogen/argon mixture used as a working gas. The results show that, with up to 41% H-2 in discharge, the synthesis rate increases by more than 60 times, rapidly decreasing for over 50% H-2 in discharge. The W dust is still produced for H-2-dominated discharges (81%), and its deposition rate is small but not negligible (0.02 mg/h). The obtained W NPs are isolated, with the diameter decreasing from 50 nm to 15 nm when the amount of H-2 in discharge is smaller than 41%. Over this value, the particles tend to agglomerate, forming structures similar to film-like deposits. Also, the diameter of the dust spots deposited on substrates depends on the H-2 content of the discharge. This allows the efficient coating of substrates up to 26 mm wide by translating them in front of the MSGA cluster source exit aperture. Additionally, for 41% H-2 in discharge, the influence of synthetic air leaks (0%-8.2%) in discharge was investigated. The deposition rate decreases rapidly (ceasing for around 6% air in discharge), and the obtained nanoparticles tend to agglomerate on the substrate (at 3.3% air content, the dust deposit has the aspect of a near-continuous film). Chemical composition investigations show a pronounced tendency for oxidation, nitridation, and oxynitride formation in the presence of air leaks.