National Institute Of Materials Physics - Romania

In the literature, a comprehensive assessment of the combined impacts of chemical and mechanical parameters on the properties of thin films grown by SILAR is missing. In this work, ZnO film formation is investigated under variable precursor concentration, pH, withdrawal speed and number of cycles. Interestingly, the produced ZnO films displayed remarkable aspect ratio and morphological variability, ranging from the commonly obtained nanograins shape towards hexagonal nanorods, flowerlike rods and nanoneedles, which to our knowledge have not yet been achieved by using single step SILAR process. More particularly, low concentration and intermediate pH and withdrawal rates were favorable for nanorods formation. In addition, increasing the withdrawal speed from 26 to 30 cmmin(-1 )resulted in a thinner film with improved rod uniformity and reduced crystallite size. This is the first study on the impact of substrate withdrawal speed on SILAR films. Among all studied parameters, the number of cycles was particularly useful for tuning film thickness, while preserving its target shape. In addition, the films grown under a higher number of cycles showed improved film crystallinity and rod orientation with reduced dislocation density, microstrain and bandgap energy. In our conditions, the most suitable combination of parameters required for exhibiting optimized nanorod-shaped coating are: a concentration of 0.07 M, pH of 10.5, speed of 30 cmmin(-1 ) and 40 cycles. In this case, XRD, XPS, Raman and FTIR spectra displayed typical features of hexagonal Wurtzite structure of ZnO with no impurities within the film surface, whereas AFM measured a thickness of 1.4 mu m with 243 nm surface roughness.

Cu2ZnSnSe4 thin films have been synthesized by employing two magnetron-sputtering depositions, interlaced with two sequential post-deposition heat treatments in low vacuum, Sn+Se and Se-rich atmospheres at 550 degrees C. By employing successive structural analysis methods, namely Grazing Incidence X-Ray Diffraction (GIXRD) and Raman Spectroscopy, secondary phases such as ZnSe coexisting with the main kesterite phase have been identified. SEM peered into the surface morphology of the samples, detecting structural defects and grain profiles, while EDS experiments showed off-stoichiometric elemental composition. The optical bandgaps in our samples were calculated by a widely used extrapolation method from recorded transmission spectra, holding values from 1.42 to 2.01 eV. Understanding the processes behind the appearance of secondary phases and occurring structural defects accompanied by finding ways to mitigate their impact on the solar cells' properties is the prime goal of the research beforehand.

Dielectric spectroscopy is a well-known method to characterize different liquid or solid (nano) materials such as liquid crystals, polymers, composites, ceramics etc. More the material structure is complex, more the molecular dynamics are put in evidence with difficulty. In many such cases, the analysis of the spectra with the classic Havriliak-Negami (H-N) functions is hard to apply or even fails. Therefore, we propose a simple numerical approach (with two different procedures) for the deconvolution of complex spectra in dielectric spectroscopy (DS). The final goal is to obtain the frequency of maximum loss (fmax) depending on the temperatures, Arrhenius diagram, and the activation energy/energies. The developed procedures have as their starting point the "logarithmic derivative of the permittivity". To our knowledge, these procedures have not yet been presented in the literature. The proposed first numerical processing allows a better separation of the different relaxation processes, a decrease in the contribution of the electrical conductivity and a better localization of the frequencies where the dielectric loss has maximum values. The second of the procedures is applied in certain particular situations, and the other procedure is more general. Where the former can be applied, it is equivalent to using the classical H-N functions in terms of obtaining the fmax, but it is simpler to apply. The first procedure uses an "artificial" and simpler H-N function, in which the fewer fitting parameters have no physical meaning, but allow a good localization of the frequency of maximum dielectric loss. The proposed procedure was applied on experimental data of dielectric spectroscopy obtained on pristine materials (nematic mixture E7 and ZnO) and composites E7-ZnO, obtained by a "green technology". The complicated spectra of the dielectric permittivity presented by these samples represent the suitable test to highlight the advantages but also the limitations of our approach. Comparing the values of the activation energy obtained for the two procedures is the criterion for verifying their correctness. The volume of processed experimental data is large, for this reason we present only the results obtained based on numerical approaches. The differences between the results obtained with the two procedures are small. The procedures can be considered as alternatives to the application of fitting with H-N functions. One procedure replaces H-N by eliminating the use of functions with complex variables and the method of least squares and has the advantage that it can apply non-specialized software like Origin. The other allows a better analysis of spectra being an improved-modified H-N approach. Proposed procedures are

One of the new materials for next-generation thin film solar cells is Cu2ZnSnSe4 (CZTSe). However, achieving a single-phase CZTSe compound remains a challenge. This study describes the development of Cu2ZnSnSe4 thin films through the sequential deposition of stacked films of non-stoichiometric Cu2SnSe3 (CTSe) and ZnSe by magnetron sputtering. The structural, morphological, and electrical properties as well as the surface chemistry of the films were investigated and compared depending on the growth sequence of the thin films. By using Raman spectroscopy and grazing incidence X-ray diffraction, the tetragonal CZTSe structure was confirmed. Scanning electron microscopy and energy-dispersive spectroscopy measurements of the morphological and compositional properties indicated large grains and dense surfaces with an elemental composition close to the desired stoichiometry in SLG\SnSe2\Cu\ZnSe and SLG\SnSe2\Cu2Se\ZnSe stacks. To ascertain the surface chemistry and unique characteristics of the produced films, additional X-ray photoemission spectroscopy experiments were carried out. The optimal band gap values for the absorber layers were found using conventional spectroscopy, and they ranged from 0.88 to 1.47 eV. According to the electrical measurements, all the films were p-type and have high carrier concentrations between 1016 and 1020 cm-3. Our findings demonstrate that employing a sequential deposition approach and annealing in different atmospheres can yield CZTSe absorber layers with desirable properties, overcoming the challenge of non-stoichiometric CTSe precursors.

This study aimed to exploit two invasive plant species to develop a novel, multifunctional, bioactive wound dressing based on a microporous cellulosic sponge (CS) from Gleditsia triacanthos pods and functionalizing them with Phytolacca americana fruit extract. The CS was functionalized, lyophilized, and characterized by Attenuated total reflectance-Fourier transform infrared spectroscopy, X-ray diffraction, scanning electron microscopy, contact angle, water absorption, and retention capacity. In addition, two parameters were evaluated in temporal dynamics: controlled release of phenolic compounds and antioxidant activities. The hemolytic index, blood clotting kinetics, lactate dehydrogenase release, and wound scratch assays proved their hemo- and bio-compatibility, as well as their ability to promote cell proliferation and migration promoting-activity and to inhibit microbial growth. Furthermore, the obtained spongious material exhibited an anti-inflammatory effect by modulating the macrophages' secretion profile of IL-6 and IL-10. In conclusion, the microporous cellulosic sponge obtained from G. triacanthos could be used as a vehicle to ensure the controlled release of bioactive principles with pro-wound healing activities extracted from invasive plants. [GRAPHICS] .

The aim of this work is to highlight the influence of UV light on the hydrolysis reaction of nifedipine (NIF) in the presence of alkaline solutions. In this context, the photodegradation of NIF in the absence of alkaline solutions caused (a) a change in the ratio between the absorbances of three bands in the UV-VIS spectra localized at 224-240 nm, 272-276 nm and 310-340 nm, assigned to the electronic transitions of -COOCH3 groups, -NO2 groups and a heterocycle with six atoms; (b) a red-shift of the photoluminescence (PL) band from 458 nm to 477 nm, simultaneous with an increase in its intensity; (c) a decrease in the ratio of the Raman line intensities, which peaked at 1224 cm-1 and 1649 cm-1, associated with the vibrational modes of -C-C-O in the ester group and C=C stretching; and (d) a decrease in the ratio between the absorbances of the IR bands, which peaked at 1493 cm-1 and 1223 cm-1, associated with the vibrational modes of the -NO2 group and C-N stretching. These changes were explained considering the NIF photodegradation reaction, which leads to the generation of the compound 4-(2-nitrosophenyl)-2.6-dimethyl-3.5-dimethoxy carbonyl pyridine. The interaction of NIF with NaOH in the absence of UV light was demonstrated to induce changes in the vibrational mode of the -C-C-O bond in the ester group. The photodegradation of NIF after its reaction with NaOH induces significant changes highlighted in its (a) UV-VIS spectra, by the shift of the absorption band at 238 nm; (b) PL spectra, by the supraunitary value of the ratio between the emission band intensities at 394-396 nm and 450 nm; (c) Raman spectra, by the change in the ratio between the intensities of the lines that peaked at 1224 cm-1 and 1649 cm-1 from 0.61 to 0.49; and (d) FTIR spectra, by the lowered absorbance of the IR band at 1493 cm-1 assigned to the vibrational mode of the -NO2 group as a result of the generation of the nitroso compound. These changes were explained considering the hydrolysis reaction products of NIF, as the nitroso compound is converted to a lactam-type compound. The photodegradation reaction rate constants of NIF and NIF after interaction with NaOH were also reported. The decrease in thermal stability of NIF samples after interaction with NaOH, as well as of NIF after exposure to UV light compared to NIF prior to exposure to UV light, was demonstrated by thermogravimetry, and the key fragments were confirmed by mass spectrometry.

A critical brief review of the evolution of the ideas describing the matter, with emphasis on concepts relevant to the journal's goals: surfaces, interfaces, and interphases is presented. The complex relationship between interphase and interface, including the role of the submicron confinement on the physical and chemical properties of matter are analyzed from both theoretical and experimental standpoints. The most important consequences triggered by the recognition of interphases are briefly discussed. Most matter (at a macroscopic scale) is dominated by bulk behavior. The rapid advances in materials and especially the accelerated progress in the synthesis and characterization of submicron materials and associated technologies, labeled as the "nano revolution", revived the research on interfaces and interphases at atomic and molecular scales. It is suggested that interphase ignites a new kind of material, whose "bulk physical features" have been distorted by the submicron confinement. Such an "interphase surface" (for example a drop of gold with a diameter smaller than a few nanometers, or a few layers of graphene), may exist free standing and be stable. These materials, which no more exhibit the bulk properties will be tentatively referred to as "Sutter" ("Sutter" defines an abbreviation that involves both surface and matter concepts). Sutter is characterized by the fact that its physical and chemical properties are controlled by the interphase. It is concluded that Sutter is essentially a submicron phase of the matter, that exhibits size-dependent features. Sutter materials may be embedded in various materials (such as polymers, metals, and alloys) as nanocomposites, thus projecting specific features at the macroscopic scale. Most free standing interphases may be considered as Sutter materials or phases. The interface does not qualify as a Sutter material.

In this work, applications of nanohybrid composites based on titanium dioxide (TiO2) with anatase crystallin phase and single-walled carbon nanohorns (SWCNHs) as promising catalysts for the photodegradation of amoxicillin (AMOX) are reported. In this order, TiO2/SWCNH composites were prepared by the solid-state interaction of the two chemical compounds. The increase in the SWCNH concentration in the TiO2/SWCNH composite mass, from 1 wt.% to 5 wt.% and 10 wt.% induces (i) a change in the relative intensity ratio of the Raman lines located at 145 and 1595 cm(-1), which are attributed to the E-g(1) vibrational mode of TiO2 and the graphitic structure of SWCNHs; and (ii) a gradual increase in the IR band absorbance at 1735 cm(-1) because of the formation of new carboxylic groups on the SWCNHs' surface. The best photocatalytic properties were obtained for the TiO2/SWCNH composite with a SWCNH concentration of 5 wt.%, when approx. 92.4% of AMOX removal was achieved after 90 min of UV irradiation. The TiO2/SWCNH composite is a more efficient catalyst in AMOX photodegradation than TiO2 as a consequence of the SWCNHs' presence, which acts as a capture agent for the photogenerated electrons of TiO2 hindering the electron-hole recombination. The high stability of the TiO2/SWCNH composite with a SWCNH concentration of 5 wt.% is proved by the reusing of the catalyst in six photodegradation cycles of the 98.5 mu M AMOX solution, when the efficiency decreases from 92.4% up to 78%.

Thick tungsten oxide layers were prepared electrophoretically in order to be used as photoanodes in photoelectrochemical water oxidation applications. The highest photocurrent density was obtained for a WO3 layer with thickness of similar to 900 nm. Additionally, WO3/BiVO4 and WO3/BiVO4/MIL-101(Fe) heterojunctions have been fabricated using WO3 layer as substrate. WO3/BiVO4 shows an increased value of the electrochemical active surface area indicating that more sites of this photoanode are activated through the formation of the heterojunction. The small V5+ signals observed in the V 2p XPS spectra of these heterojunctions were attributed to the substitution of V5+ atoms with W6+ atoms on the surface of BiVO4. Excessive W doping of the BiVO4 film determined the decrease of the photoelectrochemical performance of WO3/BiVO4 photoanode. The significant improvement of the photoconversion efficiency of the sample decorated with MIL-101(Fe) indicated that this cocatalyst provides sites more efficiently in the photoelectrochemical process. This performance was correlated with the reduced value of the charge transfer resistance at electrode/electrolyte interface obtained from electrochemical impedance spectroscopy investigation.

We report a novel approach in producing and characterizing enriched isotopic selenium-82 (82Se) thin films with trigonal hexagonal crystal structure (t-82Se), the most thermodynamically stable form of the element. The ob-tained t-82Se thin films are used as targets in accelerator based nuclear structure experiments. Several 82Se thin films with thicknesses around 5 mg/cm2 (10.4 & mu;m) were deposited on 5 mg/cm2 (3 & mu;m) tantalum (Ta) foils by vacuum evaporation-condensation method. The condensed 82Se films exhibit unstable amorphous structure (a-82Se), therefore were converted to t-82Se by means of an appropriate vacuum heat treatment developed in the target laboratory of IFIN-HH. After the thermal treatment, the microstructure, morphology and composition of the 82Se films were evaluated before and after the vacuum thermal treatment using Fourier Transform Raman Spectroscopy (FT-Raman), X-Ray Diffraction (XRD), Atomic Force Microscopy (AFM), Scanning Electron Mi-croscopy (SEM) and Energy-Dispersive X-Ray Spectroscopy (EDX) techniques. Furthermore, an in-beam & gamma;-spectroscopy experiment performed at the 9-MV tandem accelerator of IFIN-HH confirmed that the ther-mally treated t-82Se films possess high durability and high purity with no detectable contamination and no mass loss.