National Institute Of Materials Physics - Romania

Preparation under non-identical conditions involving the reduction of sol-gel-derived precursors of various Zn:Fe atomic ratios (0.97:0.03, 0.8:0.2 and 0.4:0.6) in a hydrogen-containing atmosphere was used to obtain composites of nanosized ferromagnetic (FM) alpha-Fe and antiferromagnetic (AFM) FeO in different concentrations and of the desired magnetic responses. ZnO nanoparticles, developed in all preparation stages, served primarily as a matrix for the separation of Fe (and FeO) nanoparticles, preventing their agglomeration and coarsening. The average crystallite/particle size is about 5-32 nm, 10-75 nm and 21-31 nm for FeO, Fe and ZnO, respectively. Magnetisation investigations of FeO-Fe-ZnO nanocomposites revealed a coexistence of ferromagnetic and superparamagnetic behaviours ascribed to the Fe nanoparticles in different magnetic states. All samples exhibit the exchange bias effect, EB. Values up to 375 Oe for coercivity at 300 K, 600 Oe for coercivity, 223 for coercivity enhancement and 243 Oe for EB field at 5 K were measured. The magnitude of EB depends on the processing conditions - the EB field and coercivity enhancement are larger for samples processed under conditions of a higher degree of non-equilibrium. The presence of FeO appears crucial for the occurrence of EB, irrespective of its quantity. The EB is ascribed primarily to the exchange coupling between the AFM and FM spins at the FeO/Fe interfaces of nanostructures after field-cooling from above the TN of FeO and below the Curie temperature of Fe. An approach based on magnetically disordered AFM/FM interfaces featuring like spin-glass systems was adopted to explain the EB effects. An aspect of practical relevance is the suppression of room temperature coercivity in apparent correlation with the training of the EB; an attempt has been made to understand the origin of this suppression.

In the quest for advanced materials suitable for next-generation electronic and optoelectronic applications, tungsten disulfide (WS2) ultrathin films have emerged as promising candidates due to their unique properties. However, obtaining WS2 directly on the desired substrate, eliminating the need for transfer, which produces additional defects, poses many challenges. This paper aims to explore the synthesis of WS2 ultrathin films via physical vapor deposition (PVD) followed by sulfurization in a confined space, addressing the challenge of film formation for practical applications. Precursor layers of tungsten and WS2 were deposited by RF magnetron sputtering. Subsequent sulfurization treatments were conducted in a small, closed, graphite box to produce WS2 films. The physical and chemical properties of these precursor and sulfurized layers were thoroughly characterized using techniques such as X-ray reflectometry (XRR), X-ray diffraction (XRD), Raman spectroscopy, scanning electron microscopy (SEM), and X-ray photoelectron spectroscopy (XPS). The findings reveal notable distinctions in film thickness, structural orientation, and chemical composition, attributable to the different precursor used. Particularly, the sulfurized layers from the tungsten precursor exhibited a preferred orientation of WS2 crystallites with their (00L) planes parallel to the substrate surface, along with a deviation from parallelism in a small angular range. This study highlights the necessity of precise control over deposition and sulfurization parameters to tailor the properties of WS2 films for specific technological applications.

The corrosion protection property of three Brij-type surfactants, namely, Brij 35, Brij 56 and Brij 58P, was considered on OLC 45 carbon steel in a 0.5 M H2SO4 medium. The efficacy for these organic compounds was examined using potentiodynamic polarization and electrochemical impedance spectroscopy (EIS) methods, scanning electron microscopy (SEM) procedures, and Fourier transform infrared (FT-IR) spectroscopy. We hypothesized that these surfactants hinder the corrosion for OLC 45 samples through a protecting mechanism owing to the adsorption of organic molecules that form an inhibitive film or through the formation of complex oxides. These surfactants exhibited an appreciable protective effect against OLC 45 corrosion, operating as mixed inhibitors, as could be demonstrated by their influence on the electrochemical characteristics of the metallic substrates. The adsorption of surfactants over the substrates zone conformed to the representation of the Langmuir isotherm. The effect of temperature on the electrochemical comportment of the OLC 45 specimens in H2SO4 without and with Brij at 800 ppm was examined in the temperature interval of 293 to 333 K. The negative estimate of thermodynamic attributed as Gibbs free energy of adsorption presented the spontaneity of the adsorption activity. The investigation with FT-IR and SEM established the adsorption of Brij and the constitution of the corrosive components on the OLC 45 surface. Electrochemical determinations of these surfactants indicated its anticorrosion inhibition performance and the highest inhibition of 96% was reached when the Brij 35 concentration was at 800 or 1000 ppm, while for Brij 56 and Brij 58P, the highest inhibition was obtained when their concentrations were 500, 800, or 1000 ppm.

When a severe plastic deformation (SPD) process is performed at high temperatures, it becomes more versatile. Designed originally for the bulk nanoconstruction of hard-to-deform alloys, high-speed high-pressure torsion (HSHPT) is an SPD method used in this research for assembling multiple layers of shape memory nanocomposites. Three hard-to-deform magnetic alloys in the cast state were used. Soft magnetic shape memory alloys, NiFeGa and FePdMn, and a potentially hard magnetic alloy, CoZr, were assembled in various composites. Both grain refinement and strong layer bonding were achieved in ZrCo/FePdMn and ZrCo/NiFeGa composites in seconds. The very short SPD time is specific to HSHPT because of the intense friction that occurs under high pressures, which generates huge amounts of heat. After SPD, the temperature rises in bulk material like a pulse, being dissipated mostly through heat conduction. The SPD parameters were carefully controlled with an advanced automation system using a programmable logic controller. Nevertheless, the major drawbacks of high-pressure torsion were overcome, and large SPD discs were obtained. Various investigation techniques (optical microscopy, scanning electron microscopy, energy dispersive spectroscopy and atomic force microscopy) show well-defined interfaces as well as a fine and ultrafine structure.

In the present work, single phase CoSb3 skutterudite nanomaterials were prepared via a ball milling method, and their thermoelectric characteristics were compared with the samples synthesized by the solvo-hydrothermal method. Thermoelectric transport properties were recorded in the temperature regime of 300-830 K. Both samples exhibit p-type conduction behavior with a positive sign of Seebeck coefficient. CoSb3 ball mill sample exhibit higher resistivity of 127 x 10(-5)Omega.m at 300 K as compared to CoSb3 solvo-hydrothermal sample with 4.85 x 10(-5)Omega.m. However, CoSb3 ball mill sample show enhanced Seebeck coefficient of 183 mu V/K at 473 K where CoSb3 solvo-hydrothermal sample depict 98 mu V/K at 650 K. Furthermore, the total thermal conductivity of sintered CoSb3 ball mill and CoSb3 solvo-hydrothermal samples was found to be 3.02 Wm(-1)K(-1) and 3.23 W m(-1)K(-1) at room temperature and reaches a significantly lower value of 2.47 W m(-1)K(-1) and 2.46 W m(-1)K(-1) at 580 and 670 K, respectively. The dimensionless figure of merit ZT values of CoSb3 ball mill and CoSb3 solvo-hydrothermal obtained are 0.053 and 0.060 at 650 and 700 K, respectively. A systematic tuning of processing parameters by ball milling method can lead to better thermoelectric efficiency.

The thermodynamic and kinetic simulations based on the re-assessment of the thermodynamic and kinetic database of the Ni-Ti-Cu system were employed to predict the phenomena of mechanical alloying, spark plasma sintering and thermal properties of the intriguing Ni-Ti-Cu system. Thermodynamic calculations are presented for the stable and unstable phases of NiTiCu materials and support a correlation with the evolving microstructure during the technological process. Also, the thermal conductivity, the thermal diffusivity and the specific heat of spark plasma sintered and aged Cu-alloyed NiTi-based shape memory alloys (NiTiCu) with two compositions, Ni45Ti50Cu5 and Ni40Ti50Cu10, are evaluated and the influence of mechanical alloying and precipitates on thermal properties is discussed. Measurements of these thermal properties were carried out from 25 degrees C up to 175 degrees C using the laser flash method, as well as differential scanning calorimetry. The thermal hysteresis of the 20 mm diameter samples was between 8.8 and 24.5 degrees C. The observed T0 temperatures from DSC experimental transformation features are in reasonable accordance with the thermodynamic predictions. The determined k values are between 20.04 and 26.87 W/m K and in agreement with the literature results. Moreover, this paper can provide some suggestions for the preparation of NiTiCu shape memory alloys and their applications.

Novel biocompatible composite hydrogels with good elastic and antimicrobial properties have been fabricated by e-beam cross-linking using chitosan and water-soluble polymers mixed with commercial silver nanoparticles (AgNP). Hydrogels having different formulations were characterized by rheological, swelling, FTIR, SEM, and biodegradation measurements. The network structure, biocompatibility, and antimicrobial properties were evaluated as well. The composite hydrogels showed higher stability and absorb large amounts of fluids specific to an infected wound without losing structural integrity. The rheological, SEM, and network structure results demonstrate that at above 0.1 mg/mL AgNP, hydrogels with high cross-linking density are obtained. The in vitro response of fibroblasts proved the high biocompatibility of the hydrogel's composites. The antimicrobial activity is directly influenced by the amount of AgNP and cross-linking degree of the hydrogel. Significant antimicrobial activity was recorded against Gram-negative bacteria, while for the Gram-positive ones, the growth inhibition seems to require a decrease of the cross-linking degree.

Selective growth of 2D MoS2 layers on patterned substrates is highly desired for easy fabrication of devices. Selectively grown 2D MoS2 on Mo patterned substrates for the formation of intimate metallic contact was obtained by a Mo-CVD method in which MoO2 from an oxidized Mo pattern and S powder are the growth precursors. Mo films were deposited by magnetron sputtering on SiO2(300 nm)/c-Si substrates and patterned by photolithography techniques for obtaining Mo strips and finger contact structures, with the gap between the strips and finger varied from 5 to 20 mu m. The filling of the gap by selectively grown atomically thin MoS2 plates of 1-2 monolayers (MLs) was demonstrated by scanning electron microscopy and atomic force microscopy imaging. Field effect devices for the characterization of the photosensitivity of selectively grown MoS2 have been fabricated from finger contact structures. The dark current is drastically reduced from 10(-9) to 10(-13)-10(-14) A by varying the gate voltage from +7 to -7 V, showing the n-type semiconductor behavior of the selectively grown 2D MoS2. High photosensitivity of 10(5) (%) was obtained for 4.5 x 10(-4) mW/cm(2) at 650 nm wavelength illumination. The spectral responsivity reaches values of 15-25 A/W at 600 nm wavelength and shows an energy onset of 1.72-1.77 eV corresponding to about 2 ML MoS2. The carrier-trapping effect responsible for the slow part of the device response can be caused by structural defects and also by adsorbed molecules like in gas sensors.

Bioactive glasses (BGs) are known for their selective ability to (i) form a mechanically strong interfacial bond with hard (bone) or soft tissues (gingivae or cartilages) (i.e., silica-, silica-phosphate-, phosphate-, boratephosphate-, or silica-phosphate-borate-based BGs); or (ii) serve as reservoirs for fast-release of therapeutic (osteogenic, angiogenic, anticarcinogenic, or antimicrobial) ions (i.e., phosphate-based BGs and mesoporous BGs). The strength of the bone bond yielded by the osteoproductive-capable BGs is generally equivalent to, or higher than the bone strength. The resorbability of phosphate-based BG is dependent on the content of network formers and cross-linkers. All BGs elicit excellent biochemical compatibility. However, their fracture toughness is typically less than and the elastic modulus is greater than those of bone, indicating that most BGs have suboptimal biomechanical compatibility when used in load-bearing applications. One promising approach to overcome this problem is the development of BGs in coating form, applied to the surface of load-bearing endosseous implants. This work critically assesses BG thin-layers fabricated by the radio-frequency magnetron sputtering method, an industry-ready large-scale physical vapour deposition technology. It is demonstrated that, despite the relative lack of attention paid to this technology, it enables the development of unique BG coatings with efficacious therapeutic capabilities. Here, we present an overview of the most relevant developments achieved thus far, along with the remarkable advantages, drawbacks to overcome, and future perspectives with the intention of highlighting the vast possibilities of this specific field of research.