National Institute Of Materials Physics - Romania

In this paper, we report studies on Al2O3/Ge/Al2O3 trilayer memory structures deposited by magnetron sputtering at room temperature on p-Si substrates coated with 3 nm SiO2. The changes of the structure, morphology and memory properties induced by rapid thermal annealing (RTA) in a broad temperature range 550-900 degrees C have been carefully investigated. High resolution transmission electron microscopy (HRTEM) revealed the existence of distinct RTA effects for different temperature ranges, in correlation with memory properties measured on Al/Al2O3/Ge/Al2O3/SiO2/p-Si/Al devices. Thus, at temperatures smaller than 650 degrees C, Ge diffuses into adjacent Al2O3, the layers remaining amorphous. The memory window increases from as-deposited samples to those annealed at 600 degrees C reaching the maximum of 5.4 V. After RTA at 700 degrees C, Ge nanocrystals (NCs) in intermediate Ge layer and Ge-rich amorphous nanoparticles in Al2O3 tunnel oxide are formed. Increasing RTA temperature to 800 and 900 degrees C, Ge NCs are no longer formed due to Ge strong diffusion. Instead, Ge-rich mixed GeAl oxide NCs of unknown crystalline structure are evidenced by HRTEM. The memory window continuously decreases with annealing temperature in the range 650-900 degrees C. The ON (OFF) charge loss of only 11% (9.8%) was found by extrapolation to 10 years.

An analysis of the field dependence of the pinning force in different, high density sintered samples of MgB2 is presented. The samples were chosen to be representative for pure MgB2, MgB2 with additives, and partially oriented massive samples. In some cases, the curves of pinning force versus magnetic field of the selected samples present peculiar profiles and application of the typical scaling procedures fails. Based on the percolation model, we show that most features of the field dependence of the critical force that generate dissipation comply with the Dew-Hughes scaling law predictions within the grain boundary pinning mechanism if a connecting factor related to the superconducting connection of the grains is used. The field dependence of the connecting function, which is dependent on the superconducting anisotropy, is the main factor that controls the boundary between dissipative and non-dissipative current transport in high magnetic field. Experimental data indicate that the connecting function is also dependent on the particular properties (e.g., the presence of slightly non-stoichiometric phases, defects, homogeneity, and others) of each sample and it has the form of a single or double peaked function in all investigated samples.

Eu, Er, Yb-Er, and Dy-doped phosphate glasses were prepared by a wet-route processing of chemical precursors followed by melt-quenching and annealing. XRD measurements highlighted the amorphous nature of the investigated glasses. UV-Vis absorption spectra revealed peaks specific to f-f electronic transitions of the doping ions whereas FTIR and Raman spectroscopy proved the vitreous network forming role of phosphorous pentoxide. Luminescence spectra in the Vis domain, at RT, showed emission bands characteristic to the ion transitions from the excited states to the ground state. The luminescence spectra collected in the 25-160 degrees C range exhibited a decrease of the emission intensity with temperature rise. In the case of Eu and Dy-doped glasses a relatively small decrease of the emission intensity with temperature is observed by comparison with Er and, respectively, Yb-Er-doped glass where a significant change of the emission intensity is noticed, which recommends the latter as promising candidate for sensing devices.

In the present study, the synthesis of titanium nitride (TiN) by carbothermal reduction nitridation (CRN) reaction using nanocomposites made of mesoporous TiO2/acrylonitrile with different content of inorganic phase were explored. The choice of hybrid nanocomposite as precursor for the synthesis of TiN was made due to the possibility of having an intimate interface between the organic and inorganic phases in the mixture that can favours CRN reaction. Subsequently, the hybrid composites have been subjected to four-step thermal treatments at 290 degrees C, 550 degrees C, 1000 degrees C and 1400 degrees C under nitrogen atmosphere. The XRD results after thermal treatment at 1000 degrees C under nitrogen flow show the coexistence of two crystalline phases of TiO2, i.e. anatase and rutile, as well as TiN phase, together with the detection of amorphous carbon that proved the initiation of CRN reaction. Furthermore, the observations based on XRD patterns of samples thermally treated at 1400 degrees C in nitrogen atmosphere were in agreement with SEM analysis, that shows the formation of TiN by CRN reaction via hybrid nanocomposites mesoporous TiO2/acrylonitrile.

Currently, there is a considerable time-lag in the industrialisation of innovative technological solutions for the functionalization of osseous implants, with ever-demanding healthcare requirements (e.g., controlled release of therapeutic ions, match of biomaterial degradation - bone growth rates, antimicrobial efficiency). As third-generation biomaterials, phosphate bio-glasses (PBGs) have demonstrated an ability to stimulate specific biological responses from tissue to molecular level, by successfully coupling bioactive and resorbable material properties. Here, radio-frequency magnetron sputtered (RF-MS) PBGs were explored as sacrificial resorbable layers for prospective biomedical implant designs. A PBG powder with a 50-P2O5, 35-CaO, 10-Na2O and 5-Fe2O3 composition (mol%) was used as source (target) material. The influence of the argon working pressure (0.2-1 Pa) - one of the most prominent RF-MS variables - on the morphology, structure, uniformity, composition, degradation rate and cytocompatibility of PBG films was investigated. The engineered modification of physical-chemical and biological features of the PBG sputtered films was multi-parametrically surveyed by AFM, EDXS, spectroscopic ellipsometry, GIXRD, FTIR spectroscopy measurements and in vitro assays. Results suggested that the film thickness, composition, density and structure were preserved over a uniformity region having a diameter of similar to 30 mm, irrespective of sputtering pressure. The network connectivity and the surface porosity of the films were found to have antagonistic roles with respect to the in vitro degradation performance. The possibility of fine tuning the composition, structure and thereby biological interaction of the PBG films by conveniently modifying the sputtering pressure was shown (i.e., permitting their complete controlled degradation, without cytotoxic effects). This work is the first to show in vitro cytocompatibility outcomes of sputtered PBG films and their cross-area uniformity, and thus, it could prove to be an important technological step in their future biomedical application and suggest implications for future industrial scale-up.

Cu-Fe-Sn-S films were obtained on indium tin oxide / glass substrates by a low-cost electrodeposition using an aqueous solution of CuSO4, FeSO4, SnSO4, and Na2S2O3 at room temperature followed by high-temperature sulfurization (500 degrees C) in argon flow. A range of cathodic potentials have been used for electrodeposition, those being chosen after a preliminary cyclic voltammetry study. The coatings were characterized using X-ray diffraction, Raman spectroscopy, scanning electron microscopy, energy dispersive spectroscopy, X-ray Photoelectron Spectroscopy and conventional spectroscopy (diffuse reflectance and specular transmission). The results are discussed with respect to the used applied potential.

We report a novel strategy to enhance the dielectric breakdown strength and the energy storage performance of lead-free relaxor ferroelectric ceramics through the fabrication of semiconductor/relaxor 0-3 type composites based on 0.6Ba(Zr0.2Ti0.8)O-3-0.4(Ba0.7Ca0.3)TiO3 [BZCT] and ZnO. X-ray diffraction (XRD), Raman spectroscopy, and scanning electron microscopy (SEM) measurements confirm the formation of semiconductor/relaxor 0-3 type composites, in which ZnO particles are randomly distributed at the grain boundaries of BZCT. Further, the XRD analysis suggests a structural phase change from a tetragonal to a pseudocubic phase as the ZnO content increases from 0 to 5 wt. % in BZCT/ZnO composites. The pseudocubic phase favors the relaxor behavior of the composites as is evident from dielectric studies. The polarization-electric field (P-E) loops reveal the ferroelectric nature of the BZCT/ZnO composites. The energy storage properties of BZCT/ZnO composite ceramics as a function of different wt. % of ZnO are found to be optimum at 1 wt. % with a recoverable energy density of 2.61 J/cm(3) and an efficiency of 74.2%, at an electric field of 282 kV/cm. Besides, an enhancement of 166% in the electric breakdown and 220% in the recoverable energy density was achieved compared to the BZCT ceramics due to the improved density and the large value of Delta P = P-m - P-r (25.55 mu C/cm(2)). Therefore, this work evidences that the formation of the semiconductor/relaxor 0-3 type composites can be an effective way to significantly improve the energy storage performance of lead-free relaxor ferroelectric ceramics. (C) 2020 The Authors. Publishing services by Elsevier B.V. on behalf of Vietnam National University, Hanoi.

The bone remodeling field has shifted focus towards the delineation of products with two main critical attributes: internal architectures capable to promote fast cell colonization and good mechanical performance. In this paper, Luffa-fibers and graphene nanoplatelets were proposed as porogen template and mechanical reinforcing agent, respectively, in view of framing 3D products by a one-stage polymer-free process. The ceramic matrix was prepared through a reproducible technology, developed for the conversion of marble resources into calcium phosphates (CaP) powders. After the graphene incorporation (by mechanical and ultrasonication mixing) into the CaP matrix, and Luffa-fibers addition, the samples were evaluated in both as-admixed and thermally-treated form (compact/porous products) by complementary structural, morphological, and compositional techniques. The results confirmed the benefits of the two agents' addition upon the compact products' micro-porosity and the global mechanical features, inferred by compressive strength and elastic modulus determinations. For the porous products, overall optimal results were obtained at a graphene amount of <1 wt.%. Further, no influence of graphene on fibers' ability to generate at high temperatures internal interconnected-channels-arrays was depicted. Moreover, its incorporation led to a general preservation of structural composition and stability for both the as-admixed and thermally-treated products. The developed CaP-reinforced structures sustain the premises for prospective non- and load-bearing biomedical applications.

A simple dynamic method was developed to evaluate the components in the equivalent circuit of a ferroelectric capacitor. The method is based on the application of short trapezoidal voltage pulses of variable amplitude and the analysis of the resulting current by considering the ferroelectric capacitor as a parallel R-p-C-p equivalent circuit. The values of R-p and C-p components are obtained in relation to different stages of polarization switching as the amplitude of the applied pulses increases. The most important result obtained by applying the present method is the evidence of an abrupt decrease of the R-p value (about 2 orders of magnitude) at the coercive voltage, while the equivalent C-p does not present a dramatic variation during polarization switching. This is interpreted in the context of negative capacitance obtained for ferroelectrics when polarization passes through zero value. The results obtained by using the proposed dynamic characterization method that will be referred to as "dynamic dielectric characterization", are in good agreement with those obtained by classic capacitance-voltage measurements. A method to stabilize the negative capacitance for longer periods of time is also presented by adding an external resistance in series with the ferroelectric capacitor.

The thermal behavior of Cu-doped TiO2 gels obtained by the sol-gel method was investigated by thermogravimetric and differential thermal analysis (TG/DTG/DTA) and differential scanning calorimetry (DSC) measurements. The comparative investigation of the structure and morphology of the as-prepared gels and of the nanopowders obtained by annealing them was realized by transmission electron microscopy (TEM), Fourier transmission infrared spectroscopy (FTIR), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). Significant differences were noticed depending on the amount of dopant (0.5 or 2.0 mol % CuO). A higher dopant concentration resulted in a more complex decomposition of the sample. This behavior was associated with the formation of various molecular species in the sol-gel solutions before gelation, determined by the different amount of the dopant used.