National Institute Of Materials Physics - Romania

A quaternary Fe-Pt-Nb-B alloy has been fabricated by the melt spinning method with the purpose of the formation of crystallographically coherent multiple magnetic phases, emerging from the same metastable precursor, as well as to investigate the phase interactions and the influence of their coupling on magnetic performances. For this purpose, extended structural and magnetic investigations were undertaken by making use of X-ray diffraction, transmission electron microscopy, and Fe-57 Mossbauer spectroscopy, as well as magnetic measurements using SQUID magnetometry. It was documented that intermediate metastable phases formed during primary crystallization, in intermediate stages of annealing, and a growth-dominated mode was encountered for the secondary crystallization stage upon annealing at 700 degrees C and 800 degrees C where fcc Fe3Pt and fct Fe2B polycrystalline were formed. The Mossbauer investigations have documented rigorously the hyperfine parameters of each of the observed phases. The fcc A1 FePt phase was shown to exhibit a peculiar ferromagnetic transition, and this transition has been proven to occur gradually between 300 K and 77 K. The magnetic measurements allowed us to identify the annealing at 700 degrees C as optimal for obtaining good magnetic features. Coercive field dependence shows similarities to the random anisotropy model for samples annealed at 500 degrees C to 700 degrees C which are nanocrystalline. These results show good perspectives for use in applications where different magnetic states are required at different operating temperatures.

High density (94-98% of the theoretical density) MgB2 samples added with C6H10Ge2O7 and cubic BN with compositions (MgB2)(1-x)(Ge2C6H10O7)(0.0028)(cBN)(x) (x = 0.003, 0.005, 0.007, 0.01) and (MgB2)(1-y)(Ge2C6H10O7)(y)(cBN)(0.005) (y = 0.0014, 0.0028, 0.005, 0.0075) were obtained by spark plasma sintering technique. For optimum doped samples with x = 0.005-0.007 and y = 0.0028-0.005, a weak enhancement of zero-field critical current density J(c0), irreversibility field H-irr, and volume pinning force F-p,F-max was determined. This behavior is very different from similar samples added with a single additive for which H-irr has a large enhancement. Consequently, it suggests the presence of opposite structural and microstructural effects induced by the additives. These effects, on the one hand, are discussed to decrease the sensitivity of MgB2 superconducting properties in the co-added samples comparative to samples added with C6H10Ge2O7, and, on the other hand, they contribute to anomalies that were found when assessing the pinning force-related parameters by the universal scaling law.

The microcrystallization effects induced by the real-time laser annealing in Cr-Al-C ion-sputtered films with an off-stoichiometric composition are studied. The laser annealing has been performed during Raman experiments with tunable laser power densities. Morphostructural changes induced during laser annealing were investigated by scanning electron microscopy. It has been proven that real-time laser annealing in the high-laser-power-density mode promotes quite clearly the formation of nanograins through surface microcrystallization. Detailed Raman analysis allowed for the observation of the optical modes that unequivocally identifies the low-symmetry 211 MAX phase in both low- and high-power-density modes. Such findings confirming the microcrystallization as well as the stabilization of the grain boundaries by carbon nanoclustering are confirmed by X-ray diffraction results, where the single-phase hexagonal 211 was unequivocally proven to form in the high-laser-power-density mode. The microcrystallization via laser annealing was also found to be beneficial for the elastic behavior, as the hardness values between 16 and 26 GPa were found after laser annealing, accompanied by a significantly high Young's bulk modulus. Such large values, larger than those in bulk compounds, are explicable by the nanometric grain sizes accompanied by the increase of the grain boundary regions.

The structural properties of VO2 thin films, grown on either LSAT or Si substrates by pulsed laser deposition (PLD), are elucidated by means of transmission electron microscopy (TEM) methods. The TEM observations confirmed the successful growth of VO2 by PLD in variable thicknesses, by optimizing the O-2 partial pressure and growth temperature. The films adopt a columnar polycrystalline morphology with narrow columns, up to the film thickness height. Four VO2 polymorphs have been detected by electron diffraction and high-resolution TEM (HRTEM) analysis, with M1 being by far the most abundant phase. Post-experimental strain measurements in HRTEM images have revealed that the actual residual strain is minimized due to the columnar morphology of the VO2 grains, as well as intrinsic oxide layers in the VO2/Si epitaxy. The TEM outcomes confirmed the complementary electrical and magnetic measurements in the films, where a transition from a monoclinic M1 to a rutile VO2 R phase has been identified, influenced by the initial percentage of phases in thick VO2 films.

We have investigated the pinning potential of high-quality single crystals of superconducting material CaKFe4As4 having high critical current density and very high upper critical field using both magnetization relaxation measurements and frequency-dependent AC susceptibility. Preliminary studies of the superconducting transition and of the isothermal magnetization loops confirmed the high quality of the samples, while temperature dependence of the AC susceptibility in high magnetic fields show absolutely no dependence on the cooling conditions, hence, no magnetic history. From magnetization relaxation measurements were extracted the values of the normalized pinning potential U*, which reveals a clear crossover between elastic creep and plastic creep. The extremely high values of U*, up to 1200 K around the temperature of 20 K lead to a nearly zero value of the probability of thermally-activated flux jumps at temperatures of interest for high-field applications. The values of the creep exponents in the two creep regimes resulted from the analysis of the magnetization relaxation data are in complete agreement with theoretical models. Pinning potentials were also estimated, near the critical temperature, from AC susceptibility measurements, their values being close to those resulted (at the same temperature and DC field) from the magnetization relaxation data.

The chemical precipitation was used to obtain carbon fibers (CF) with surface modified by magnetite particles (Fe3O4). Processing was carried out by employing up to three subsequent coating stages of ultrasonic treatments. After each sonication stage, the coating was 17, 33, and 47 wt. % of the total weight of the modified fibers. Raman spectroscopy indicates the presence in the coating of a mixture of iron II and III states. As-decorated fibers were used to fabricate composites with an epoxy resin (ED-20) matrix cured with PEPA. The quantity of the carbon fiber filler was of 1, 3, and 6 wt %. At room temperature, the saturation magnetization of the soft magnetic samples was 0.37, 0.83, and 1.72 emu/g for the indicated compositions. Carbon fiber reinforced polymer materials with extra functions such as magnetic in this case, are expected to be useful in applications from the power and energy industries.

Polycrystalline MgB2 bulk samples were produced by ex-situ spark plasma sintering (SPS) using the oxygen-free preceramic polymer additive poly(dimethylsilane) as a source for carbon doping and as a sintering aid. Two major effects were identified. One is the significant enhancement of the densification kinetics during sintering for all tested compositions. The second one is the improvement of the high field critical current density for a certain level of the poly(dimethylsilane) addition.

In the present work, stannite Cu2CoSnS4 (CCTS) films were elaborated using spray pyrolysis method on soda-lime glass, at different deposition temperatures (T-d = 250, 300, and 350 degrees C), followed by different chosen sulfurization temperatures (T-s = 450, 500, and 550 degrees C). X-ray diffraction (XRD) revealed the nearly single-phase formation of CCTS films at 300 degrees C deposition temperature. After sulfurization in argon flow, the XRD lines become narrower, the average crystallite size expanding above 70 nm. The Raman spectroscopy analysis confirmed the stannite structure formation, as well as the presence CoS2 secondary phases, which reduces at higher sulfurization temperature (550 degrees C). The energy dispersive spectroscopy results indicated atomic ratios of Cu/Co/Sn/S close to the ideal stoichiometric ratio 2:1:1:4. The room temperature photoluminescence emission is recorded with maximum in the 1.35-1.40 eV range. Thermoelectric properties are measured up to 130 degrees C, the films show poor power factor as a result of small positive Seebeck coefficients 10-45 Of K -1 and low electrical conductivity despite of having relatively high carrier concentration (similar to 10(20) cm(-3)).

This work explores the possibility of involving aluminothermy in processing donor-doped zinc oxide-based thermoelectrics by relying on local, strong exothermic effects developed during sintering, with a potential positive impact on the electrical and thermal transport properties. The strategy was exemplified by using aluminium as a dopant, due to its recognized ability to generate additional, available charge carriers in ZnO, and by using two different metallic Al powders and conventional Al2O3 as precursors. Nanosized aluminium powder was involved in order to evaluate the possible desirable effects of the particles size, as compared to aluminium micropowder. A significant enhancement of the electrical and thermoelectric performance of the samples prepared via metallic Al precursors was observed and discussed in terms of the potential impacts provided by the aluminothermic reaction on the microstructure, charge carrier concentration and mobility during sintering. Although the presented results are the first to show evidence of how aluminothermic reactions can be used for boosting the thermoelectric performance of zinc oxide materials, the detailed mechanisms behind the observed enhancements are yet to be understood.

Two unreacted commercially available Nb3Sn precursor wires with different architecture were subject to a two-temperature heat treatment in vacuum at 650 degrees C for 72 h and at 700 degrees C for 168 h. Evolution of wires towards formation of the superconducting phase was assessed by the non-invasive X-ray computed microtomography (micro XRT) with a spatial resolution of similar to 2 mu m on the samples before and after the heat treatments. Statistical image analysis quantified the defects and quantitatively revealed the deviation of the geometrical perfection of the wire components comparative to designed parameters depending on the wire architecture and heat treatment conditions. Our results position XRT as a tool to evaluate the quality of Nb3Sn, also promoting it as a method capable for providing new insights that could be used in the optimization processes of Nb3Sn wires design, technology, and during operation.