When used as the active layers-either as a light absorber in photovoltaic devices or as an electroluminescent material in light-emitting devices-lead-free perovskites significantly impact the performance of optoelectronic devices. This study focuses on antimony-based perovskites, which are promising for lighting applications. These types of perovskites enable the formation of self-trapped excitons (STEs) with higher dissociation energy than lead-based perovskites, which generate excitons with lower dissociation energy. The (CH3NH3)3Sb2I9 crystals are synthesized using two methods, resulting in distinct spatial configurations - dimer and dimer/layered mixtures, each exhibiting unique structural and spectroscopic properties, as revealed by comprehensive multi-parametric complementary analyses. Their emissive properties underscore the efficiency of the STE photoluminescence, driven by electron-phonon interactions and influenced by Sb-Sb distances in (CH3NH3)3Sb2I9 powder, whether dispersed in polymethyl-methacrylate or solution. The phase transition from monoclinic to hexagonal (dimer) and trigonal (layered) structures enabled the tuning of the optical properties in direct correlation with the structural and electrical features. The photoluminescence behavior of the STEs, analyzed in conjunction with the Raman spectroscopy, elucidates the dynamic process of the electron-phonon coupling effects in the dimer (face-capping Sb-I octahedra) and layered (corner-sharing Sb-I octahedra) crystallographic structures.

In this work a method in two steps for the preparation of the composites based on poly(ortho-toluidine) (POT) and the MoS2 and WS2 sheets was reported. In the first step, by ball-milling of mixtures of MoS2 and WS2 particles, the sheets of MoS2 and WS2 (MoS2: WS2) with weight ratio equal to 3:1, 1:1 and 1:3 were prepared. In the second step, the interaction in solid-state of the MoS2: WS2 samples with POT in emeraldine-base (POT-EB) and emeraldine-salt (POT-ES) was used to obtain composites of the type MoS2: WS2/POT-EB and MoS2: WS2/ POT-ES. Using X-ray diffraction (XRD), FTIR spectroscopy, Raman scattering and X-ray photoelectron spectroscopy (XPS), we demonstrate that: i) the ball-milling method can allow the preparation of the MoS2 and WS2 sheets with different stacking order, ii) the interaction of POT-EB with the MoS2: WS2 samples involves the transformation of some repeating units of the type EB into ES; and iii) the interaction of POT-ES with the MoS2: WS2 samples leads to the appearance of new positive charges onto macromolecular chains which are compensated by S2- ions. According to thermogravimetric analysis (TG) and differential scanning calorimetry (DSC), all samples are demonstrated to be stable up to 230 degrees C. Dielectric spectroscopy data reveal a complex dependence of DC electrical conductivity on frequency, temperature, and composite concentration. We use the apparent activation energy, defined as the derivative of the logarithm of conductivity with respect to the inverse temperature. The obtained results indicate that apparent activation energy is influenced by system composition via filling factors. The electrical properties of these heterogeneous materials are described using Lichtenecker's mixing laws. For components with similar electrical properties, the effective conductivity and apparent activation energy were determined as linear combinations of the individual conductivities and activation energies, respectively, weighted by the component concentrations. Our findings align with experimental data, offering a framework for understanding conductivity and activation energy in multi-component systems.

The precise control of the magnetic compensation temperature (theta c) in ferrimagnetic garnets is essential for the development of cutting-edge ultrafast customizable spintronic devices. In this work we demonstrate how fine variation in stoichiometry and cation distribution in iron gadolinium garnets significanty influences theta c. Two samples of Gd3Fe5O112 garnets synthesized via a new hydrothermal method and a conventional solid-state reaction, respectively, were considered. The complex study was carried out using a complex approach combining X-ray diffraction, magnetometry, and M & ouml;ssbauer spectroscopy. Atomic-scale analysis revealed with unprecedent accuracy a cationic inversion between Fe3+ ang Gd3+ at octahedral and dodecahedral sites in both samples, and their chemical compositions were determined as Gd2.70Fe4.76O11.9 and Gd2.96Fe4.68O11.5, respectively. These local rearrangements have been shown to have a consistent influence on theta c (290 K and 317 K, respectively) around room temperature, emphasizing the high sensitivity of exchange interactions to internal atomic order. Results clearly illustrate the strong correlation between the processing, atomic configuration and macroscopic magnetic behavior, establishing a new paradigm for the design of garnet-based materials with tunable theta c. The strategy for the accurate determination of cation inversion illustrated in this work exhibits great potential in guiding material innovations for next-generation spintronics.

The Ni49+xMn32-2xGa19+x (x = 0; 2) Heusler ferromagnetic shape memory alloys were prepared using spark plasma sintering using raw flake-type powders obtained by soft grinding melt-spun ribbons. Samples were characterized using x-ray diffraction, electron microscopy, thermal analysis, and bending tests. Although the properties of ribbons and corresponding powders show similar properties' tendencies, they are opposite in the bulk sintered alloys when compared with precursor powders. Namely, Ni49Mn32Ga19 bulk shows a higher enthalpy (5.8 J g-1), an increased martensitic transformation (MT) temperature (by 9 K), and a reduced hysteresis span (5 K). Conversely, for the Ni51Mn28Ga21 sintered sample, a lower enthalpy (2 J g-1), a significant decrease (by 40 K) in the MT starting temperature, and a broadening of the hysteresis range (26 K) were observed. This difference is analyzed versus specific features of the microstructure. Moreover, the activation energy and the pre-exponential factor of the MT, extracted through kinetic analysis within two non-isothermal models, Kissinger and Friedman, complement and sustain these findings. Fractography details of the sintered samples are discussed in relation to the stress-strain curves from the bending tests. The Ni49Mn32Ga19 bulk sample exhibits a higher bending strength (260 MPa) and a lower strain (0.55%) than the Ni51Mn28Ga21 sample (177 MPa and 0.61%). The observed dependence of functional characteristics on preparation enables the possibility of property control required for various applications and suggests that the proposed route is promising in this regard for further investigations.

The crystallization mechanism of Yb/Er-doped GdF3 nanocrystals in silica nano-glass ceramics was analyzed using model-free and model-fitting methods and thermal analysis data in correlation with structural data. The formation of GdF3 nanocrystals occurs at around 300 degrees C, and their size is temperature dependent, ranging from 14 to 40 nm, depending on the processing temperature. A similar trend is observed for cell volume, where a contraction of up to approximate to 2.3% (at 600 degrees C) was assigned to the gradual incorporation of Li and Yb,Er dopants. Model-free analysis showed an increase in activation energy (Ea) and the preexponential factor (log A) up to 175 kJ mol-1 and 14.8 s-1, respectively, until the completion of crystallization. Model-fitting analysis indicated a crystallization process controlled by an autocatalytic-type reaction where a second metastable phase (LiF) acts as a catalyst and facilitates a rapid and self-accelerated crystallization of the main GdF3 nanocrystalline phase. The ceramization process boosted UC luminescence up to values comparable to those of NaYF4:18Yb/2Er.

Fabrication and extensive characterization of hard-soft nanocomposites composed of hard magnetic low-temperature phase LTP-MnBi and amorphous Fe70Si10B20 soft magnetic phase for bulk magnets are reported. Samples with compositions Mn55Bi45 + x center dot(Fe70Si10B20) (x = 0, 3, 5, 10, 20 wt.%) were prepared by spark plasma sintering of powder mixtures. Characterization has been performed by X-ray diffraction, scanning and transmission electron microscopy, magnetometry and Fe-57 Mossbauer spectroscopy. It was shown that samples contain crystallized and nanometric LTP-MnBi phases with various elemental compositions depending on the degree of Bi clustering. Complex correlations between starting compositions, processes during fabrication, and functional magnetic characteristics were observed. Unexpected special situations of the relation between microstructure and magnetic coupling mechanisms are discovered. Exchange spring effects of different strengths occur, being very sensitive to morpho-structural and compositional features, which in turn are controlled by processing conditions. An in-depth analysis of related microscopic characteristics is provided. Results of this work suggest that fabrication by powder metallurgy routes, such as spark plasma sintering of hard and soft magnetic powder mixtures, of MnBi-based composites with exchange spring phenomena have a high potential in designing and optimization of suitable materials with tunable magnetic properties towards rare-earth-free permanent magnet applications.

Rare-earth doped GdF3 nanocrystals embedded in silica glassy matrix have been prepared by controlled crystallization of the xerogel; the influence of rare-earth ion (Pr, Sm, Eu, Tb, Dy, Er, Yb) and additional Li-codopant on structural and optical properties was discussed. The precipitation of RE-doped GdF3 nanocrystalline phase is the result of Gd-trifluoracetate thermolysis revealed as a strong exothermic peak at around 300 degrees C. Structural analysis of RE-doped SiO2-GdF3 glass-ceramic sample calcined at 525 degrees C showed the occurrence of GdF3 nanocrystals of about 25 nm size, showing hexagonal or orthorombic structure depending on the RE-ion. Under UV-light excitation at 273 nm of Gd3+ ions (S-8(7/2) -> I-6(13/2,15/2) transition), photoluminescence spectra showed characteristic RE3+ luminescence due to the non-radiative energy transfer between the excited Gd3+ and acceptor RE ions; the highest energy transfer (congruent to 80 %) was observed for Tb3+ and lowest (congruent to 21 %) for Sm3+.

Glassy nanocomposites containing Yb3+/Er3+-doped GdF3 and LiGdF4 nanocrystals have been prepared by controlled crystallization of the xerogel and the structural, up-conversion luminescence, and magnetic properties were analyzed and discussed. Structural and morphological analysis showed uniform distribution of both GdF3 and LiGdF4 nanocrystals (tens of nm size), embedded in silica glass matrix as the result of thermal decomposition of the trifluoracetates, revealed as a strong exothermic peak at about 300 degrees C; the Li-ions co-doping showed a strong influence on the GdF3 and LiGdF4 nanocrystalline fraction. The energy dispersive spectrometry mapping showed Gd, F and Yb, Er within the nanocrystals but not in the silica glass matrix. X-ray diffraction pattern analysis indicated the crystalline lattice distortion consistent with the Yb/Er incorporation in both fluoride nanocrystals. The "green" ((H-2(11/2), S-4(3/2)) -> I-4(15/2)) and "red" (F-4(9/2)-> I-4(15/2)) up-conversion luminescences at 525, 545, and 660 nm observed under 980 nm laser light pumping were assigned to the Er3+ ions deexcitation through a two-photon process. The magnetic properties of the nanocomposite are strongly temperature dependent. The magnetization hysteresis loops show a ferromagnetic behavior at low temperatures (5K) related to the rare-earth ions contribution and the saturation magnetization of 39 emu/g. At 300 K a paramagnetic behavior was observed that was ascribed to the non-interacting localized nature of the magnetic moment of the rare-earth ions. Hence, such novel, multifunctional magnetic and optical materials can allow the intertwining between magnetism and photonics and might offer new opportunities for new magneto-optical device development.

In this study, a sol-gel film based on lead sulfide (PbS) quantum dots incorporated into a host network was synthesized as a special nanostructured composite material with potential applications in temperature sensor systems. This work dealt with the optical, structural, and morphological properties of a representative PbS quantum dot (QD)-containing thin film belonging to the Al2O3-SiO2-P2O5 system. The film was prepared using the sol-gel method combined with the spin coating technique, starting from a precursor solution containing a suspension of PbS QDs in toluene with a narrow size distribution and coated on a glass substrate in a multilayer process, followed by annealing of each deposited layer. The size (approximately 10 nm) of the lead sulfide nanocrystallites was validated by XRD and by the quantum confinement effect based on the band gap value and by TEM results. The photoluminescence peak of 1505 nm was very close to that of the precursor PbS QD solution, which demonstrated that the synthesis route of the film preserved the optical emission characteristic of the PbS QDs. The photoluminescence of the lead sulfide QD-containing film in the near infrared domain demonstrates that this material is a promising candidate for future sensing applications in temperature monitoring.

In our work, the kinetics of martensitic transformations and the influence of thermal treatments on martensitic transformations, as well as the related magnetic properties of the Ni49Mn32Ga19 ferromagnetic shape memory melt-spun ribbons, have been investigated. Thermal treatments at 673 K for 1, 4 and 8 h can be considered an instrument for fine-tuning the performance parameters of alloys. One-hour thermal treatments promote an improvement in the crystallinity of these otherwise highly textured ribbons, reducing internal defects and stress induced by the melt-spinning technique. Longer thermal treatments induce an important magnetization rise concomitantly with a slight and continuous increase in martensitic temperatures and transformation enthalpy. The activation energy, evaluated from differential scanning calorimeter experimental data with a Friedman model, significantly increases after thermal treatments as a result of the multi-phase coexistence and stabilization of the non-modulated martensitic phase, which increases the reverse martensitic transformation hindrance.

This study explored a new green approach of the wet ferritization method to obtain magnetic cobalt ferrite (CoFe2O4) by using eucalyptus leaves aqueous extract as a reducing/chelating/capping agent. The spinel single cubic phases of prepared samples were proved by powder X-ray diffraction (XRD), Fourier-Transform Infrared (FTIR) and Raman spectroscopy. The average crystallite size is in the range between 3 and 20 nm. The presence of the functional groups coating the obtained material is confirmed from FTIR and thermal analysis. The scanning electron microscopy (SEM) analysis showed a morphology consisting of nanoparticle aggregates. Raman spectroscopy detects the characteristic bands of spinel-type CoFe2O4. Magnetic investigations reveal the formation of ferromagnetic compounds with cubic magnetic anisotropy and a blocking temperature around 140 K, specific for this type of material. The biosynthesized CoFe2O4 could be an attractive candidate for biomedical applications, exhibiting promising antimicrobial and antibiofilm activity, particularly against Gram-negative bacteria and fungal strains.

A convenient and low-cost sol-gel approach for the one-step synthesis of ZnO-P2O5-rGO nanostructures with tuned bandgap and fluorescence was investigated. The obtained hybrid nanostructures exploit the properties of zinc oxide, graphene oxide and phosphorous oxide as promising candidates for a wide range of optoelectronic applications. A predominant amorphous structure, ZnO-P2O5-rGO, containing ZnO nanorods was evidenced by X-ray diffraction analysis (XRD) and scanning electron microscopy (SEM). The estimated size of the ZnO nanorods in nanostructures with P2O5 was noticed to decrease when the P2O5/ZnO ratio was increased. The presence of ZnO, P2O5 and rGO was confirmed by Fourier-transform infrared spectroscopy (FTIR) and Raman investigation. P2O5 was noticed to tune the bandgap and the fluorescence emissions of the nanostructured films, as estimated by UV-Vis-NIR and fluorescence spectroscopy, respectively. The electrical measurements performed at room temperature showed that the main influence on the film's resistivity does not come from the 1% rGO doping but from the P2O5/ZnO ratio. It was found that a 10/90 molar ratio of P2O5/ZnO decreases the resistivity almost seven-fold compared with rGO-doped ZnO films.

Complex physico-chemical investigations have been performed on white inlaid substance used in the orna-mentation of prehistoric clay artefacts from southern Romania ceramics from the Early Chalcolithic, up to the Middle/Late Bronze Age. Structural and morphological investigations of the white pigments have showed hundreds of nm up to microns size particles with calcite and hydroxyapatite (ash bone) as dominant components. The calcite was found on Early Chalcolithic pigment vessels while those where hydroxyapatite was dominant from the Middle/Late Bronze Age. FTIR spectra revealed the biogenic source of the hydroxyapatite (i.e. cremated animal bone) and the crystallinity degree values agrees with the expected temperatures of firing of the ancient furnaces; the calcite-based pigments were supposed to be filled post firing. The EPR was not able to able to provide a clear assignment of the cremated animal bones but thermoluminescence showed various sources of calcite.

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.

Sesquipedalian mud and burnt bricks (second to third century AD) were excavated from the Roman city of Romula located in the Lower Danube Region (Olt county, Romania). Along with local soils, bricks are investigated by petrographic analysis, X-ray fluorescence (XRF), X-ray diffraction (XRD), Fourier transformed infrared spectroscopy (FT-IR), electron microscopy (SEM/EDX), X-ray microtomography (XRT), thermal analysis (DTA-TG), M.ssbauer spectroscopy, magnetometry, colorimetry, and mechanical properties assessment. The results correlate well with each other, being useful for conservation/restoration purposes and as reference data for other ceramic materials. Remarkably, our analysis and comparison with literature data indicate possible control and wise optimization by the ancient brickmakers through the recipe, design (size, shape, and micro/ macrostructure), and technology of the desired physical-chemical-mechanical properties. We discuss the Roman bricks as materials that can adapt to external factors, similar, to some extent, to modern "smart" or "intelligent" materials. These features can explain their outstanding durability to changes of weather/climate and mechanical load.

Nanosized CoFe1.8RE0.2O4 (RE3+ = Tb3+, Er3+) ferrites were obtained through wet ferritization method. These ferrites were characterized by X-ray diffraction (XRD), scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM/HR-TEM), Fourier transform infrared spectroscopy (FTIR), Mossbauer spectroscopy and magnetic measurements. The XRD results revealed that the average crystallite size is 5.77 nm for CoFe1.8Tb0.2O4 and 6.42 nm for CoFe1.8Er0.2O4. Distribution of metal cations in the spinel structure estimated from X-ray diffraction data showed that the Tb3+ and Er3+ ions occupy the octahedral sites. TEM images indicated the presence of polyhedral particles with average size 5.91 nm for CoFe1.8Tb0.2O4 and 6.80 nm for CoFe1.8Er0.2O4. Room temperature Mossbauer spectra exhibit typical nanoscaled cobalt ferrite spectra in good agreement with XRD and TEM data. The saturation magnetization value (M-s) is 60 emu/g for CoFe1.8Tb0.2O4 and 80 emu/g for CoFe1.8Er0.2O4. CoFe1.8RE0.2O4 nanoparticles showed similar antimicrobial efficacy against the five tested microbial strains, both in planktonic and biofilm state. The results highlight the promising potential of these types of nanoparticles for the development of novel anti-biofilm agents and materials.

Luminescent nanocrystals embedded into silica microspheres were shown to be useful for silica labeling for biological applications, ensuring mechanical and chemical stability, nontoxicity, biocompatibility and optical properties. We used sol-gel technology to prepare silica nanospheres embedded with fluorescent and magnetic Eu3+(1 mol%)-doped CeO2 nanocrystals. The X-ray diffraction pattern analysis and transmission electron microscopy investigations showed CeO2:Eu3+(1 mol%) nanocrystals of about 9 nm size and Ce3+ ions substitution by the Eu3+ ions; the nanocrystals dispersed inside the nanosized silica spheres of about 400 nm diameters. The photoluminescence spectra recorded under UV-light excitation showed Eu3+ ions luminescence peaks (D-5(0)-F-7(J), J = 0-4) accompanied by a weaker 425 nm luminescence due to the silica matrix; the quantum yield was 0.14. The weak hysteresis loop and magnetization curves recorded up to 20,000 Oe showed dominantly paramagnetic behavior associated with the silica matrix; a slight opening of the hysteresis loop to a very small magnetic field (about 0.005 Oe) was due to the presence of the two rare earth ions. The photonic crystal properties of SiO2-CeO2:Eu3+(1 mol%) silica nanospheres deposited as films on quartz plates were revealed by the two weak attenuation peaks at 420 and 500 nm and were associated with the reflection from different planes. The SiO2-CeO2:Eu3+(1 mol%) nanospheres are attractive potential candidates for photonics-related applications or for multifunctional bio-labels by combining the luminescence and magnetic properties of the nanocrystals.

The incorporation of therapeutic-capable ions into bioactive glasses (BGs), either based on silica (SBGs) or phosphate (PBGs), is currently envisaged as a proficient path for facilitating bone regeneration. In conjunction with this view, the single and complementary structural and bio-functional roles of CuO and Ga2O3 (in the 2-5 mol% range) were assessed, by deriving a series of SBG and PBG formulations starting from the parent glass systems, FastOs (R) BG -38.5SiO2-36.1CaO-5.6P2O5-19.2MgO-0.6CaF2, and 50.0P2O5-35.0CaO-10.0Na2O-5.0 Fe2O3 (mol%), respectively, using the process of melt-quenching. The inter-linked physico-chemistry -biological response of BGs was assessed in search of bio-functional triggers. Further light was shed on the structural role -as network former or modifier -of Cu and Ga, immersed in SBG and PBG matrices. The preliminary biological performance was surveyed in vitro by quantification of Cu and Ga ion release under homeostatic conditions, cytocompatibility assays (in fibroblast cell cultures) and antibacterial tests (against Staphylococcus aureus). The similar (Cu) and dissimilar (Ga) structural roles in the SBG and PBG vitreous networks governed their release. Namely, Cu ions were leached in similar concentrations (ranging from 10-35 ppm and 50-110 ppm at BG doses of 5 and 50 mg/mL, respectively) for both type of BGs, while the release of Ga ions was 1-2 orders of magnitude lower in the case of SBGs (i.e., 0.2-6 ppm) compared to PBGs (i.e., 9-135 ppm). This was attributed to the network modifier role of Cu in both types of BGs, and conversely, to the network former (SBGs) and network modifier (PBGs) roles of Ga. All glasses were cytocompatible at a dose of 5 mg/mL, while at the same concentration the antimicrobial efficiency was found to be accentuated by the coupled release of Cu and Ga ions from SBG. By collective assessment, the most prominent candidate material for the further development of implant coatings and bone graft substitutes was delineated as the 38.5SiO2-34.1CaO-5.6P2O5-16.2MgO-0.6CaF2-2.0CuO-3.0Ga2O3 (mol%) SBG system, which yiel-ded moderate Cu and Ga ion release, excellent cytocompatibility and marked antibacterial efficacy. (c) 2021 The Chinese Ceramic Society. Production and hosting by Elsevier B.V. This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).

The effect of sodium thiosulfate (ST) on the photodegradation of azathioprine (AZA) was analyzed by UV-VIS spectroscopy, photoluminescence (PL), FTIR spectroscopy, Raman scattering, X-ray photoelectron (XPS) spectroscopy, thermogravimetry (TG) and mass spectrometry (MS). The PL studies highlighted that as the ST concentration increased from 25 wt.% to 75 wt.% in the AZA:ST mixture, the emission band of AZA gradual downshifted to 553, 542 and 530 nm. The photodegradation process of AZA:ST induced: (i) the emergence of a new band in the 320-400 nm range in the UV-VIS spectra of AZA and (ii) a change in the intensity ratio of the photoluminescence excitation (PLE) bands in the 280-335 and 335-430 nm spectral ranges. These changes suggest the emergence of new compounds during the photo-oxidation reaction of AZA with ST. The invoked photodegradation compounds were confirmed by studies of the Raman scattering, the FTIR spectroscopy and XPS spectroscopy through: (i) the downshift of the IR band of AZA from 1336 cm(-1) to 1331 cm(-1), attributed to N-C-N deformation in the purine ring; (ii) the change in the intensity ratio of the Raman lines peaking at 1305 cm(-1) and 1330 cm(-1) from 3.45 to 4.57, as the weight of ST in the AZA:ST mixture mass increased; and (iii) the emergence of a new band in the XPS O1s spectrum peaking at 531 eV, which was associated with the C=O bond. Through correlated studies of TG-MS, the main key fragments of ST-reacted AZA are reported.

IV-VI semiconductor quantum dots embedded into an inorganic matrix represent nanostructured composite materials with potential application in temperature sensor systems. This study explores the optical, structural, and morphological properties of a novel PbS quantum dots (QDs)-doped inorganic thin film belonging to the Al2O3-SiO2-P2O5 system. The film was synthesized by the sol-gel method, spin coating technique, starting from a precursor solution deposited on a glass substrate in a multilayer process, followed by drying of each deposited layer. Crystalline PbS QDs embedded in the inorganic vitreous host matrix formed a nanocomposite material. Specific investigations such as X-ray diffraction (XRD), optical absorbance in the ultraviolet (UV)-visible (Vis)-near infrared (NIR) domain, NIR luminescence, Raman spectroscopy, scanning electron microscopy-energy dispersive X-ray (SEM-EDX), and atomic force microscopy (AFM) were used to obtain a comprehensive characterization of the deposited film. The dimensions of the PbS nanocrystallite phase were corroborated by XRD, SEM-EDX, and AFM results. The luminescence band from 1400 nm follows the luminescence peak of the precursor solution and that of the dopant solution. The emission of the PbS-doped film in the NIR domain is a premise for potential application in temperature sensing systems.

The current study aims to present and discuss the results obtained by complementary archaeometric methods applied for the first time on white pigments inlaid on excised pottery of the Boian-Vidra tradition (Early Chalcolithic, c. 4900-4600 BCE). The samples came from three settlements located in Southern Romania (Sultana-Ghetarie, Vidra, and Vladiceasca). They were selected considering that the pottery was produced in approximately contemporary sites, located relatively close to each other in the same geographical region, namely the Romanian Plain. The experimental part included the analysis of local samples of carbonate concretions and prehistoric animal bone ash as reference materials. Archaeometric investigations consisted in applying "in-air" PIXE and EDX methods for the chemical composition, XRD and FTIR for mineralogical data, SEM for microstructure observation, and EPR for the characterisation of the paramagnetic centres. Calcite, bone ash, and silica rich sediments were identified as the primary decorating pigments. The mixtures of calcite and bone-ash observed in 13 samples were specific to the sites at Vidra and Vladiceasca. Silica-rich sediments from distant sources were the main whitening materials in two samples from Vladiceasca, while for the samples from Sultana-Ghetarie, calcite was the only whitening mineral. The results show with a high degree of confidence the use of both local (i.e., carbonate neo-formations and bone ash) and exotic (silica-rich sediments) raw materials to obtain the white pigment applied to Boian-Vidra pottery. Thus, the current data show the adaptability of the potters with respect to the surrounding resources and also provide new evidence for a vast trade network of raw materials and/or finished products in the Lower Danube area during the Early Chalcolithic. The deliberate mixing of two whitening materials from different sources could be a technological choice and may highlight complex symbolic behaviours.

In this work, new optical evidences concerning the changes induced of the UV light on pantoprazole sodium (PS), in solid state and as aqueous solution, are reported by UV-VIS spectroscopy, photoluminescence (PL), Raman scattering and FTIR spectroscopy. New evidences concerning the products of the PS photodegradation pathways are reported by the correlated studies of thermogravimetry and mass spectrometry. The influence of the excipients and alkaline medium on the PS photodegradation is also studied. New aspects regarding the chemical mechanism of the PS photodegradation in the presence of the water vapor and oxygen form air and the alkaline medium are shown. Our results confirm that the PS photodegradation induced of the water vapors and oxygen from air leads to the generation of 5-difluoromethoxy-3H-benzimidazole-2-thione sodium, 5-difluoromethoxy-3H-benzimidazole sodium, 2-thiol methyl-3, 4-dimethoxypyridine and 2-hydroxymethyl-3, 4-dimethoxypyridine, while in the alkaline medium, compounds of the type of the 2-oxymethyl-3,4-dimethoxypyridine sodium salts are resulted.

Rare-earth doped oxyfluoride glass ceramics represent a new generation of tailorable optical materials with high potential for optical-related applications such as optical amplifiers, optical waveguides, and white LEDs. Their key features are related to the high transparency and remarkable luminescence properties, while keeping the thermal and chemical advantages of oxide glasses. Sol-gel chemistry offers a flexible synthesis approach with several advantages, such as lower processing temperature, the ability to control the purity and homogeneity of the final materials on a molecular level, and the large compositional flexibility. The review will be focused on optical properties of sol-gel derived nano-glass ceramics related to the RE-doped luminescent nanocrystals (fluorides, chlorides, oxychlorides, etc.) such as photoluminescence, up-conversion luminescence, thermoluminescence and how these properties are influenced by their specific processing, mostly focusing on the findings from our group and similar ones in the literature, along with a discussion of perspectives, potential challenges, and future development directions.

This paper describes for the first time two processing routes-the precursor method and the two-step wet chemical process-for the synthesis of magnetic cobalt ferrite using the Tamarindus indica fruit extract. These green approaches are eco-friendly, safe and efficient alternatives to classical chemical methods. The aqueous extract from tamarind fruit contains numerous metabolites (organic acids, aminoacids). All these bioactive components are able to chelate metal ions leading to the formation of the multimetallic complex (precursor of cobalt ferrite). The obtained precursor was characterized by Fourier transform infrared spectroscopy (FTIR), thermal analysis, X-ray diffraction analysis (XRD) and magnetic measurements. The structure, morphology and magnetic behavior of the cobalt ferrite samples prepared through both synthesis routes were investigated by various characterization techniques: FTIR, XRD, scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDS), Mossbauer spectroscopy and magnetic measurements. XRD data confirmed that a cubic spinel structure was obtained for both ferrite powders with average crystallite size of 13 and 5 nm, respectively. The microstructure study by SEM revealed the formation of nanocrystallites assemblies using the precursor method and carbon-rich particles forming granulated micron-sized agglomerates, embedding ferrite nanocrystallites obtained through the two-step wet chemical process. Mossbauer spectroscopy results evidenced relaxation processes in the CoFe2O4 samples at room temperature, and the main characteristics of the involved sublattices were derived. The magnetic investigation revealed a typical magnetic behavior for a spinel, with CoFe2O4 nanoparticles ferrimagnetic at low temperature and superparamagnetic at room temperature.

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.

Melt spun ribbons of Mn53Al45C2 and Mn52Al46C2 have been synthesized by rapid quenching of the melt with the purpose of monitoring the epsilon-tau phase transformation to show technologically feasible ways to increase magnetic parameters and to illustrate the viability of these alloys as the next generation of rare earth (RE)-free magnets. By differential scanning calorimetry (DSC), activation energies and temperatures of onset of the epsilon-tau phase transformation were obtained. Structural analysis was performed using X-ray diffraction (XRD) and the resulting XRD patterns were quantitatively assessed using full profile Rietveld-type analysis. Appropriate annealing was performed in order to enable the epsilon-tau phase transformation. While hcp epsilon-phase was found to be predominant in the as-cast samples, after appropriate annealing, the tetragonal tau-phase, the one that furnishes the relevant magnetic response, was found to be predominant with an abundance of about 90%. The data suggested a mechanism of hcp epsilon-phase decomposition controlled by the segregation towards the interfacial regions, having the rate of transformation governed by antiphase boundary diffusion processes. Magnetic measurements of annealed sample Mn53Al45C2, consisting of predominant tetragonal tau-phase, showed high values of magnetization and increased coercivity, consistent with an energy product of about 10 MGOe, similar with previously reported magnetization measurements, providing further insight into the realization of future class of RE-free low-cost permanent magnets.

In this work, new films containing composite materials based on blends of thermoplastic polymers of the polyurethane (TPU) and polyolefin (TPO) type, in the absence and presence of BaTiO3 nanoparticles (NPs) with the size smaller 100 nm, were prepared. The vibrational properties of the free films depending on the weight ratio of the two thermoplastic polymers were studied. Our results demonstrate that these films are optically active, with strong, broad, and adjustable photoluminescence by varying the amount of TPU. The crystalline structure of BaTiO3 and the influence of thermoplastic polymers on the crystallization process of these inorganic NPs were determined by X-ray diffraction (XRD) studies. The vibrational changes induced in the thermoplastic polymer's matrix of the BaTiO3 NPs were showcased by Raman scattering and FTIR spectroscopy. The incorporation of BaTiO3 NPs in the matrix of thermoplastic elastomers revealed the shift dependence of the photoluminescence (PL) band depending on the BaTiO3 NP concentration, which was capable of covering a wide visible spectral range. The dependencies of the dielectric relaxation phenomena with the weight of BaTiO3 NPs in thermoplastic polymers blends were also demonstrated.

Pottery vessels made of kaolin clay from the Roman Period (2nd, 3rd centuries CE) found in Romula (Re?ca village, Olt County, Romania) from Dacia Inferior (Malvensis) were investigated by petrographic, X-ray diffraction, X-ray fluorescence, thermal analysis, electron microscopy, and mechanical tests. Our results are compared with available data on kaolin clays and pottery vessels from other sites located along the lower course of Danube river and near the Black Sea, namely in Moesia Superior, Moesia Inferior, and Thracia. Archeological and geographical contexts are addressed. Results of our analysis suggest a local production of ceramics in Romula, by using raw materials from the north of Lower Danube, in opposition to the idea that kaolin ware was imported from the provinces south of the Danube.

Phosphate-tellurite crystalline materials containing titanium and aluminum oxide as well as a tellurite crystalline material containing lithium, barium and aluminum oxide were synthesized and investigated by X-ray diffraction (XRD) and Fourier Transform Infrared (FTIR) spectroscopy. XRD analysis shows peaks specific to the crystalline phases Al(PO3)(3) and TiP2O7. FTIR analysis revealed absorption bands specific to the bending and stretching vibration modes of the phosphate and tellurite crystalline networks.

A composite material with applications in optoelectronics has been investigated. Pulsed laser deposition CdSe-doped glass film was prepared by the combinatorial deposition from two targets, namely pure CdSe and glass belonging to the 20Li(2)O-10Al(2)O(3)-7BaO-2La(2)O(3)-2ZnO-59P(2)O(5)system. Exciton peaks in the Vis domain, related to electron-hole pairs transitions from the valence band to the conduction band, were revealed in the optical absorption spectra of the CdSe-doped film. CdSe quantum dots (QDs) band gap energy depends on the CdSe quantum confinement effect. CdSe-doped film photoluminescence exhibits peaks in the red domain assigned to CdSe transitions from the excited state to the ground state. The size of CdSe nanoclusters, determined from x-ray diffraction is correlated with scanning electron microscopy-energy dispersive x-ray spectroscopy and atomic force microscopy results. Vibration modes specific both to CdSe QDs and to the vitreous network have been evidenced by Fourier transform infrared and Raman spectroscopy.

This work investigates the structural, magnetic and magneto-optical properties of a new zinc phosphate-tellurite glass belonging to the 45ZnO-10Al(2)O(3)-40P(2)O(5)-5TeO(2)system. The glass was prepared by a wet method of processing the starting reagents followed by suitable melting-stirring-quenching-annealing steps. Specific parameters such as density, average molecular mass, molar volume, oxygen packaging density, refractive index, molar refractivity, electronic polarizability, reflection loss, optical transmission, band gap and optical basicity have been reported together with thermal, magnetic and magneto-optical characteristics. Absorption bands appear in the blue and red visible region, while over 600 nm the glass becomes more transparent. FTIR and Raman spectra evidenced phosphate-tellurite vibration modes proving the P(2)O(5)and TeO(2)network forming role. Magnetic measurements reveal the diamagnetic character of the Te-doped glass with an additional weak ferromagnetic signal, specific to diluted ferromagnetic oxides. Positive Faraday rotation angle with monotonous decreasing value at increasing wavelength was evidenced from magneto-optical measurements. The final product is a composite material comprising of a non-crystalline vitreous phase and Te-based nanoclusters accompanied by oxygen vacancies. The metallic-like Te colloids are responsible for the dark reddish color of the glass whereas the accompanying oxygen vacancies might be responsible for the weak ferromagnetic signal persisting up to room temperature.

In this study, we report on the structural, magnetic, and optical properties of Tb3+-doped CeF(3)nanocrystals prepared via a polyol-assisted route, followed by calcination. X-ray diffraction analysis and electron microscopy investigations have shown the formation of a dominant Ce(0.75)F(3)nanocrystalline phase (of about 99%), with a relatively uniform distribution of nanocrystals about 15 nm in size. Magnetization curves showed typical paramagnetic properties related to the presence of Ce(3+)and Tb(3+)ions. The magnetic susceptibility showed a weak inflexion at about 150 K, assigned to the cerium ions' crystal field splitting. Under UV light excitation of the Ce(3+)ions, we observed Tb(3+)green luminescence with a quantum yield of about 20%.

A new composite base on reduced graphene oxide (RGO) and poly(5-amino-1-naphthol) (P5A1N) was synthesized by the electrochemical polymerization of 5-amino-1-naphthol (5A1N) in the presence of HClO(4)and H(4)SiW(12)O(40)onto the surface of Au electrode covered with the RGO sheets. The linear dependence of the current densities of the anodic and cathodic peaks with the scan rate of the potential range (0; 0.8) V vs. SCE, reported during electropolymerization of 5A1N, indicates an electron transfer that is controlled by diffusion. A covalent functionalization of the RGO sheets with P5A1N is argued by: (i) the simultaneous disappearance of the IR band at 1584 cm(-1)and the appearance of the new IR bands at 812, 976 and 3744 cm(-1), and (ii) the appearance of two Raman lines at 738 and 1428 cm(-1). An application of the RGO sheets covalently functionalized with P5A1N is demonstrated to support 1,4-phenylene diisothiocyanate (PDITC), a compound used as a cross-linking agent for various biological applications. The chemical adsorption of PDITC onto the RGO sheets covalently functionalized with P5A1N, which involves the appearance of new functional groups of the type thiourea, was proven by Raman scattering and IR spectroscopy.

A study on clay mineral polymer nanocomposites (CPN), namely polyaniline/montmorillonite-cetyltrimethylammonium bromide (PANI/Mt-CTAB), poly o-anisidine/montmorillonite-cetyltrimethylammonium bromide (poly(o-ANIS)/Mt-CTAB) and poly o-anisidine-co-aniline/montmorillonite-cetyltrimethylammonium bromide (poly(o-ANIS-co-ANI)/Mt-CTAB), synthesized by oxidative chemical polymerization method is presented. The nanocomposites have been characterized by Fourier transform infrared spectroscopy, UV-vis spectroscopy, and cyclic voltammetry, X-ray diffraction, scanning electron microscopy, transmission electron microscopy, cyclic voltammetry and thermogravimetry and differential scanning calorimetry analysis. By UV-vis measurements different electronic transitions for the CPNs were pointed out. The voltammograms indicate that the synthetized materials are electroactive. The FTIR analysis reveals the characteristic bands of the polymers and of the Mt-CTAB. The shift of the bands to higher/lower wavenumbers demonstrate the interaction between the pristine polymers macromolecular chains and the montmorillonite (Mt). The intercalation of the polymers inside the mineral clay was confirmed by the increased interlayer distance connected with the position of the 011 diffraction plane of the Mt., and the intercalation and exfoliation states were highlighted in the scanning and transmission electron microscopy images. The obtained results are encouraging in respect with the purpose to use them in the field of photovoltaic applications.

Polycrystalline In2S3 thin films have been grown on SnO2/glass substrates by chemical bath deposition technique and irradiated at different high gamma doses 3, 7, 15 and 40 kGy. X-ray diffraction, Scanning Electron Microscope (SEM), Energy Dispersive Spectroscopy (EDS), Spectrophotometer, Photoluminescence and Thermoluminescence were used to investigate physical properties of In2S3 thin films induced by gamma irradiation. After being irradiated, structural properties of In2S3 thin films have shown that preferred orientation has been moved from (4 0 0) plan at 2 theta(1)=33.42 degrees to a new created orientation at 2 theta(2)=38.06 degrees for 40 kGy gamma dose. EDS analysis has shown that atomic percentage (S/In) has been strongly varied for 40 kGy which indicate significant changes in stoichiometry. Thermoluminescence of irradiated In2S3 thin films has revealed a good sensitivity toward absorbed gamma dose. After irradiation, optical transmittance of In2S3 thin films has been increased from 50% to a maximum value of 70% in the visible range for 15 kGy dose. Band gap energy E-g has been slightly decreased. Other optical parameters such absorption and extinction coefficients, refractive index and permittivity have been determined. These experimental results show that gamma radiations can be used for tuning physical properties of In2S3 thin films for photovoltaic applications.

The influence of the Gd3+ co-dopant on the structure, morphology and up-conversion luminescence/magnetic properties of the LiYF4:Gd3+/Yb3+/Er3+ nanocrystals was investigated and compared to those of Gd-free samples. Electron microscopy has indicated an inhibiting effect of the agglomeration and collapsing process of the nanocrystals compared to the Gd-free powder samples. The surface analysis of nanocrystals have not shown oxygen-metal bonds related to the metal oxidation within the surface nanometric layer. The paramagnetic properties are related to the magnetic moment of the Gd3+ ions. The up-conversion luminescence of the LiYF4:Gd3+/Yb3+/Er3+ nanocrystals is about six times stronger than in LiYF4:Yb3+/Er3+ nanocrystals; the enhancement effect is most probably due to the lattice distortion induced by the Gd co-doping.

In this work, we report on the synthesis and characterization of BNT-BT0.08/CoFe2O4 biphasic composite with core-shell structure. This artificial core (BNT-BT0.08/shell (CoFe2O4) heterostructure was prepared by sol-gel method and the resulting composite was characterized in term of microstructure, dielectric, piezoelectric and magnetic properties. BNT-BT0.08/CoFe2O4 sintered ceramic shows high permittivity (epsilon' >= 30) and high dielectric losses (tan delta >= 10) in the low frequency range (nu <= 10(4) Hz), remnant polarization (Pr) of similar to 7.7 mu C/cm(2) and, remanent magnetization (Mr) of 24 emu/g at 5 K and of 14 emu/g, at room temperature. The present study reveals that the ferroelectric, piezoelectric and magnetic properties of this new architectured composite depend on the amount of each component and, can be tailored by adjusting their synthesis conditions. BNT-BT0.08/CoFe2O4 core-shell material investigated in this work provides a novel way to exploit new applications for the multifunctional composite, such as piezoelectric sensor, magnetoelectronic sensors and data storage devices.

This research work is dedicated to study structural, morphological, optical and photoluminescence properties of samarium doped calcium sulfate (CaSO4) thin films after exposure to high gamma radiations. Polycrystalline doped CaSO4 thin films have been grown on glass substrates by spray pyrolysis technique and irradiated at different high gamma doses 3, 7, 15 and 40 kGy. Physical characterization of irradiated thin films has been made by X-ray diffraction, Spectrophotometer, Scanning Electron Microscope, Energy Dispersive Spectroscopy, Fluorescence Spectrometer and Thermoluminescence. The most remarkable result, as shown by structural analysis, is the increase of grain size from 52 to a maximum value of 93 nm for 15 kGy gamma dose which indicates a clear enhancement in crystal structure by gamma irradiation. Moreover, the preferred orientation has been immediately changed from (102) plan to (100) just after the first 3 kGy gamma dose. SEM micrographs of irradiated thin layers show deep modifications in surface morphology. Optical transmission spectra have shown a sharp and intense peak at 350 nm wavelength. Band gap energy has been slightly decreased from 3.9 eV before irradiation to 3.6 eV for 40 kGy. A new and strong energy level noted E r , has been emerged and created due to high gamma irradiations in addition to the principal one relative to band gap energy. Other parameters like absorption and extinction coefficients and refractive index have been determined. Thermoluminescence data show a high sensibility to gamma radiations doses which offer opportunities for dosimetry applications. These experimental results suggest the use of irradiated samarium doped calcium sulfate as optical window for space photovoltaic devices where gamma rays are abundant. These results are also helpful for researchers using CaSO4 thin films near nuclear apparatus (nuclear reactors and particle accelerators) or those interested in studying interaction between radiations and condensed matter.

Hybrid ferromagnetic/piezoelectric core-shell nanoparticles and ceramics have potential for a wide range of applications due to their tunability, electronic and magnetic properties. In this study, we designed a core-shell-type nanostructure of composition CoFe2O4/BNT-BT0.08, where BNT-BT0.08 is the abbreviation of bismuth, sodium titanate (Bi0.5Na0.5TiO3, BNT) doped with 8 mol% barium titanate (BaTiO3, BT). This multiferroic composite was prepared by covering CoFe2O4 nanoparticles with a shell of BNT-BT0.08 using the sol-gel technique. Scanning and transmission electron microscopy confirmed formation of a core-shell structure. The results of microstructure, dielectric, piezoelectric and magnetic investigations demonstrated that this heterostructure shows simultaneously electrical and magnetic behavior, at room temperature. XRD pattern of core-shell composite CoFe2O4/BNT-BT0.08 powder reveals only cubic CoFe2O4 and rhombohedral Bi0.5Na0.5TiO3 phases. CoFe2O4/BNT-BT0.08 core-shell nanostructure sample shows high values of permittivity (epsilon >= 600) together with high dielectric losses (tan delta >= 1) in the low-frequency range (nu <= 10(4) Hz). PFM and polarization hysteresis indicated a ferroelectric domains structure and remnant polarization of similar to 2.6 A mu C/cm(2) for the ceramics pellets samples of CoFe2O4/BNT-BT0.08. The present study reveals the possibility of coating nanoparticles onto nanometer-sized core particles, using controlled sol-gel process, in order to prepare multifunctional core-shell composites for piezoelectric and magnetoelectronic sensors.

Silico-phosphate films doped with CdS/ZnS quantum dots (QDs) for luminescence temperature sensing devices, were deposited on silicon substrate by sol-gel method, spin coating technique. Optical absorption and photoluminescence emission of CdS/ZnS-doped silico-phosphate films were investigated. CdS/ZnS nano-crystalline particles were put into evidence by X-Ray Diffraction (XRD) spectroscopy. The specific vibration modes of the constituents were evidenced by structural analysis carried out by Raman and Fourier Transform Infrared spectroscopy (FTIR). The characteristic fluorescence emission of CdS/ZnS nanoparticles was noticed in the visible domain. The morphology of the films was investigated by Scanning Electron Microscopy (SEM), Atomic Force Microscopy (AFM) and Transmission Electron Microscopy (TEM). Clusters of hexagonal crystalline CdS/ZnS QDs were put into evidence.

A novel class of quaternary intermetallic alloys based on CoPt is investigated in view of their interesting magnetic properties induced by the presence of hard magnetic L1(0) phase. A Co48Pt28Ag6B18 alloy has been prepared by rapid solidification from the melt and subjected to various isothermal annealing procedures. The structure and magnetism of both as-cast and annealed samples as well as the phase evolution with temperature are investigated by means of thermal analysis, X-ray, and selected area electron diffraction, scanning and high-resolution electron microscopy, and magnetic measurements. The X-ray diffraction (XRD) analysis shows that both the as-cast alloy and the sample annealed at 400 degrees C (673 K) have a nanocrystalline structure where fcc CoPt phase predominates. Annealing at 473 degrees C promotes the formation of L1(0) phase triggered by the disorder-order phase transformation as documented in the differential scanning calorimetry results. The sample annealed at 670 degrees C (943 K) shows full formation of L1(0) CoPt as revealed by XRD. Magnetic measurements showed coercivity values ten times increased compared to the as-cast state. This confirms the full formation of L1(0) CoPt in the annealed samples. Moreover, detailed atomic resolution HREM images and SAED patterns show the occurrence of the rarely seen (003) superlattice peaks, which translated into a high ordering of the L1(0) CoPt superlattice. Such results spur more interest in finding novel classes of nanocomposite magnets based on L1(0) phase.

We have undertaken a temperature-dependent, investigation of the thermodynamics, structure, morphology and magnetism of two MnAl nanocomposite alloys (Mn60Al40 and Mn55Al45). Differential scanning calorimetry (DSC) studies allowed the determination of the exo-effects occurring in the structural phase transformation of MnAI, while by using temperature-dependent X-ray diffraction of synchrotron radiation we were able to monitor the phase transformation effects and the evolution with temperature of various structural phases occurring in the samples. We have shown that slight changes in stoichiometry (5 at.%) give rise to different phase structure in the as-cast state. While in Mn60Al40 only hcp epsilon phase can be found, in Mn55Al45 as-cast alloy, there is a quite complex phase structure with a mixture of gamma(2) (Al8Mn5) and epsilon as well as ferromagnetic MnAI T-phase. Activation energies of about 165 kJ/mol and 290 kJ/mol have been calculated from the Ozawa-Flynn-Wall analysis of DSC experimental data. These findings are in good agreement with the results obtained from XRD. For the Mn55Al45 as cast alloy, we have confirmed by temperature-dependent synchrotron XRD that the hcp e phase decomposes through the migration of interphase interfaces with the transformation rate controlled by boundary diffusion processes. High-resolution transmission electron microscopy have confirmed the phase structure obtained by XRD, while magnetic properties, obtained for the as-cast alloys are consistent with the multiphase character of the samples and in good agreement with previously reported results. The magnetization does not saturate for the maximum applied field of about 4 x 10(6) A/m and a marked coercivity of about 160 kA/m is obtained for the Mn55Al45 as-cast alloy.

Local atomic configuration, phase composition and atomic intermixing in Fe-rich Fe1-xCrx and Fe1-xMox ribbons (x = 0.05, 0.10, 0.15), of potential interest for high-temperature applications and nuclear devices, are investigated in this study in relation to specific processing and annealing routes. The Fe-based thin ribbons have been prepared by induction melting, followed by melt spinning and further annealed in He at temperatures up to 1250 degrees C. The complex structural, compositional and atomic configuration characterisation has been performed by means of X-ray diffraction (XRD), transmission Mossbauer spectroscopy and differential scanning calorimetry (TG-DSC). The XRD analysis indicates the formation of the desired solid solutions with body-centred cubic (bcc) structure in the as-quenched state. The Mossbauer spectroscopy results have been analysed in terms of the two-shell model. The distribution of Cr/Mo atoms in the first two coordination spheres is not homogeneous, especially after annealing, as supported by the short-range order parameters. In addition, high-temperature annealing treatments give rise to oxidation of Fe (to haematite, maghemite and magnetite) at the surface of the ribbons. Fe1-xCrx alloys are structurally more stable than the Mo counterpart under annealing at 700 degrees C. Annealing at 1250 degrees C in He enhances drastically the Cr clustering around Fe nuclei.

We investigated in this paper a novel bilayer composite obtained by sol-gel and spin coating of the ferroelectric 0.92Na(0.5)Bi(0.5)TiO(3)-0.08BaTiO(3) (abbreviated as BNT-BT0.08) and ferromagnetic CoFe2O4 phases, for miniature low-frequency magnetic sensors and piezoelectric sensors. This heterostructure, deposited on Si-Pt substrate (Si-Pt/CoFe2O4/BNT-BT0.08), was characterized using selected method such as: X-ray diffraction, dielectric spectroscopy, piezoelectric force microscopy, SQUID magnetometry, atomic force microscopy/magnetic force microscopy, and advanced methods of transmission electron microscopy. CoFe2O4/BNT-BT0.08 ferromagnetic-piezoelectric thin films show good magnetization, dielectric constant and piezoelectric response. The results of analyses and measurements reveal that this heterostructure can have applications in high-performance magnetoelectric devices at room temperature.

One of the most promising ways for the realization of multi-functional materials is the integration of oxides with different properties in artificial heterostructures. In this paper, a novel piezoelectric-ferromagnetic heterostructure consisting of 0.92Na(0.5)Bi(0.5)TiO(3)-0.08BaTiO(3) (abbreviated as BNT-BT0.08) and CoFe2O4 layers is fabricated on Si-Pt substrate, by sol-gel method coupled with spin-coating technique. The composite thin film shows only perovskite Bi0.5Na0.5TiO3-like rhombohedral phase and CoFe2O4 cubic phase. The thickness of CoFe2O4 and BNT-BT0.08 layers is similar to 280 and similar to 400 nm, respectively. BNT-BT0.08/CoFe2O4 heterostructure thin film shows a saturation magnetization of 0.11 emu/g at 5 K and 0.07 emu/g at 295 K, dielectric constant of 235 at 1 kHz and tunability of 70% at 1 kHz and an electric field E = 110 kV/cm. The results reveal that the investigated hybrid piezoelectric/ferromagnetic structure shows piezoelectric behavior, good ferroelectric and ferromagnetic properties. This bilayer composite can be used in miniature low-frequency magnetic sensor and piezoelectric sensor for biomedical domain.

The crystallization mechanism of sol-gel-derived NaYF4:(Yb, Er) up-converting phosphors has been studied by differential scanning calorimetry analysis using both model-free and model fitting approaches. Structural and optical data have shown that the hexagonal NaYF4:(Yb, Er) phase crystallization process occurs at around 315 degrees C as a result of the thermal decomposition of the metal trifluoroacetates. As the annealing temperature increases, sphere-like microcrystals of about 1-2 mu m size (at 300 degrees C) break up into smaller ones (400-500 nm size) and finally collapse at higher temperatures (600 degrees C); the up-conversion luminescence signal intensity increases due to the crystallinity improvement and dehydration process. The crystallization process can be described as an autocatalytic-type reaction where the accompanying cubic NaYF4 phase played a catalytic role by reducing the energy barrier against the crystallization of the hexagonal NaYF4 phase, causing its fast self-accelerated crystallization. The energy resulting from the disintegration process of the initial NaYF4 microcrystals contributed to the growth and agglomeration processes and finally the collapse of the crystalline fragments with increasing temperature.

In the present work, optical, structural and morphological properties of CdS-doped phosphate films obtained by pulsed laser deposition (PLD) method were investigated. In the deposition process, a target based on a mixture composed of Li2O-Al2O3-BaO-La2O3-ZnO-P2O5 glass and CdS powder as dopant was used. The phosphate glass target was obtained by non-conventional wet route of raw reagents processing followed by melt-quenching technique. The complex oxide composition of the glass as well as the final PLD target consisting in a mixture of glass and CdS powder followed by pressing and heat treatment represents the novelty of the work. CdS dopant particles were highlighted by X-ray diffraction analysis as well as by Raman spectroscopy. Thus, cubic CdS particles having less than 10 nm size corroborated with specific LO (longitudinal optical phonons) and 2LO CdS Raman peaks from 300 and 600 cm(-1), respectively, certified the presence of the dopant in the deposited films. Specific vibration modes for the vitreous phosphate matrix were revealed by fourier transform infrared spectroscopy, and spherulitic units characteristic to PLD technique were found by scanning electron microscopy and atomic force microscopy analyses. A relative large luminescence band located around 430 nm was provided by UV excitation, representative for CdS nanoparticles having about 9-10 nm size.

The crystallization process of Yb3+/Er3+ codoped LiYF4 nanoparticles obtained by sol-gel method was studied using differential scanning calorimetry and X-ray diffraction. Thermal data obtained from differential scanning calorimetry measurements under non-isothermal conditions at different heating rates were examined using both model-free and model fitting approaches. It was shown that LiYF4 phase crystallization occurs at around 383 degrees C as a result of the thermal decomposition of trifluoracetates and is shifted to higher temperatures as the heating rate increases. Both Friedman and Ozawa-Flynn-Wall analyses have indicated that the activation energy and pre-exponential factor decrease slightly as the crystallization proceeds. According to the model-fitting approach (by using extended Prout-Tompkins nth-order, ath autocatalysis reaction), LiYF4 nanocrystalline phase is the result of an autocatalytic process where a second metastable phase YF3 acts as a catalyst that accelerates the crystallization process of the LiYF4 phase. (C) 2016 Elsevier Ltd and Techna Group S.r.l. All rights reserved.

The double-perovskite Sr2FeMoO6 has been obtained by solid state method at low temperature (1060 degrees C) and a very short time of synthesis (up to 4h). Both, X-ray diffraction and scanning electron microscopy (SEM) confirmed the formation of Sr2FeMoO6 oxide with grain sizes around 160 mm, and a small amount of SrMoO4 as an impurity. Mossbauer spectroscopy revealed a mixed site population with Fe and Mo ions generating a structure type with population inversion. This structure has a critical influence on the magnetic properties, as confirmed by the magnetization and TC values, i.e 3.56 mu(B)/f.u and 415 K, respectively. The Sr2FeMoO6 behavior was interpreted in terms of ferrimagnetic couplings generated by the various distributions of local interactions between Fe and Mo neighbors while comparing the ideal structure should show antiferromagnetic coupling between the two sublattices.

A quantitative treatment of the effects of magnetic mutual interactions on the specific absorption rate of a superparamagnetic system of iron oxide nanoparticles coated with oleic acid is reported. The nanoparticle concentration of the considered ferrofluid samples varied from a very low (0.005) to a medium (0.16) value of the volume fraction, whereas the amplitude of the exciting AC magnetic field ranged from 14-35 kA m(-1). It was proved that a direct effect of the interparticle interactions resides in the regime of the modified superparamagnetism, dealing, besides the usual increase in the anisotropy energy barrier per nanoparticle, with the decrease in the specific time constant tau(0) of the relaxation law, usually considered as a material constant. Consequently, the increase in the specific absorption rate versus the volume fraction is significantly diminished in the presence of the interparticle interactions compared to the case of non-interacting superparamagnetic nanoparticles, with direct influence on the magnetic hyperthermia efficiency.

This paper presents the synthesis and characterization of hydroxyapatite (HAp) and hydroxyapatite embedded in a collagen matrix (C-HAp6). The aim of this study was to investigate the influence of collagen on the structure and morphology of hydroxyapatite. According to the XRD patterns, the samples have the structure characteristic to hydroxyapatite. The FTIR and Raman spectra proved the successfully embedding of hydroxyapatite in the collagen matrix. Morphologically, the collagen increases the porosity of HAp. The collagen influences the structure and morphology of the hydroxyapatite causing a decrease of the mean particle size and/or a decrease of crystallinity while increasing the porosity.

Glassy nanocomposites containing Eu3+-doped LaOCl nanocrystals of about tens of nm size embedded in a silica matrix have been prepared by using sol-gel route followed by controlled crystallization of the xerogel. Crystallization behavior of LaOCl nanocristalline phase was discussed on the basis of thermal analysis, X-ray diffraction and photoluminescence measurements. LaOCl nanocrystalline phase precipitation is the result of lanthanum chloride hydrolytic and oxidative reactions. As the annealing temperature increases nanocrystallites size grows up to tens of nm; Eu3+-ions are gradually incorporated during the nanocrystals growth. Structural changes were studied using the Eu3+ as probe ion and the luminescence properties were analysed by using Judd-Ofelt theory. (C) 2015 Elsevier Ltd. All rights reserved.

The synthesis routes for polycrystalline bulk Sr2FeMoO6 (SFMO), offer various possibilities, but in all the cases it is difficult to obtain a single phase of this compound. A new challenge in the field is to achieve mono-crystals using different growing routes and the Bridgman method represents one of them. In order to establish the optimal conditions of mono-crystals growing process, a complex thermal investigation of bulk double perovskite has been performed. Differential thermal analysis investigation in argon inert atmosphere, starting from room temperature up to 1650 degrees C provided information about melting and re-crystallization temperature range. Both, the activation energy of Sr2FeMoO6 re-crystallization process and the re-crystallization mechanism were comparatively analyzed by two free-model estimations (Friedman and Ozawa-Flynn-Wall analysis). The resulted data are very important in order to set up the heating program of Bridgman furnace.

The goal of this study was to obtain at low temperature a functional nano-composite with characteristics similar to the natural bone by using a cost effective method. The structure and morphology of collagen coated zinc doped hydroxyapatite bio-composites (Zn:HAp-CBc) were examined by X-Ray diffraction (XRD) and Scanning Electron Microscopy (SEM). XRD analysis revealed that the unique hexagonal Ca-10(PO4)(6)(OH)(2) in P-63m space group was observed in the obtained nanocomposites Zn: HAp-CBc. The cytotoxicity of the Zn: HAp-CBc was studied on HeLa cell lines. Cell cycle distribution after treatment was examined by flow cytometry analysis. Our preliminary in vitro studies revealed that the obtained composites based on Zn doped HAp embedded in collagen matrix have excellent biocompatibility and support their further characterization by in vivo approaches and development as a biomaterial used in bone regeneration.

Chromium substituted cobalt ferrites (CoFe2-xCrxO4, 0 <= x <= 2) were synthesized through solution combustion method using glycine as fuel, named glycine-nitrates process (GNP). As evidenced by X-ray diffraction data (XRD), single cubic spinel phase was formed for all CoFe2-xCrxO4 (0 <= x <= 2) series. The cubic lattice parameter (a) decreases with increasing chromium content. Room temperature Fe-57 Mossbauer spectra revealed the Fe3+ and Cr3+ site occupancy, the local hyperfine magnetic fields and the substitution of Fe3+ by Cr3+ in the lattice. Scanning electron microscopy (SEM) showed a refinement of particle size with the increase of Cr3+ content. Magnetic measurements from 5 K to 120 K have shown a dropping in the saturation magnetization as the chromium content increases. This behaviour has been explained in terms of substitution of Fe3+ by Cr3+ in the cubic lattice of cobalt ferrite.

Sol-gel route using metal alkoxides precursor and trifluoroacetic acid as in situ fluorination reagent has been used to prepare Eu3+ -doped silicate xerogel, followed by thermal annealing to obtain oxyfluoride glass ceramic containing Eu3+ -doped BaF2 nanocrystals. We have used Eu3+ as probe ion and we analyzed its characteristic features (photoluminescence, optical absorption and magnetic circular dichroism) to get information about the local environment around the ion during thermally activated evolution of the sol to xerogel and then glass ceramic. As the drying and annealing proceeds silica network is formed accompanied by precipitation of the nanofluoride crystalline phase; Eu3+ coordination changes gradually from a random and assymetric CF3COO- one (in the sol) to a symmetric one (in the BaF2 nanocrystals) given by the fluorine ions. Glass ceramization is based on a homogenous crystallization mechanism with BaF2 nucleation centres resulted from thermal decomposition of Ba-trifluoacetate at around 300 degrees C followed by subsequent growth into BaF2 nanocrystals above 600 degrees C; Eu3+-ions are incorporated during the nanocrystals growth. (C) 2013 Elsevier B.V. All rights reserved.

Lead-free piezoelectric (Bi0.5Na0.5)(0.92)Ba0.08TiO3, doped with 5 mol %BiFeO3 (BNT-BT-BFO) nanowires was prepared from its corresponding precursor sol. A polycarbonate membrane with the thickness of 30 mu m and the pore diameter of 100 nm was used as template. Nanowires with average diameter of similar to 80 nm and different lengths of a few microns were prepared from BNT-BT-BFO precursor sol with similar to 0.03 M concentration. Ferroelectric and piezoelectric characterizations of BNT-BT-BFO nanowires were performed using AFM-PFM equipment. The HR-TEM micrograph of nanocrystals, SAED patterns, and XRD pattern indicated that BNT-BT-BFO nanowires crystallized on the lattice of rhombohedral (Na0.5Bi0.5TiO3) phase. The BNT-BT-BFO nanowires showed a significant piezoelectric response, suggesting a good piezoelectric behavior. The saturation magnetization of the nanowires, measured at room temperature and at 5 kOe magnetic field, was Ms = 0.061 emu/g. A saturated ferromagnetic hysteresis loop has been also obtained.

With the aim of synthesizing the mixed nanoparticle system xIn(2)O(3)-(1-x)SnO2 over all molar concentration range 0 <= x <= 1, Delta x = 0.1, we performed hydrothermal supercritical experiments on indium-tin hydrogel resulted from InCl3-SnCl4 water solution. Nanophases isostructural with InOOH and SnO2 were obtained by hydrothermal reaction at 400 degrees C, in the molar concentration range of 0.1 <= x <= 0.7; at x = 0.8 and x = 0.9 only one phase, isostructural with InOOH, was observed. Samples calcined at 500 degrees C with x in the range of 0.2 <= x <= 0.7 contain a nanoscaled phase isostructural with rhombohedral In2O3 and a second one isostructural with tetrahedral SnO2. At x = 0.8 and x = 0.9 only one phase isostructural with rhombohedral In2O3 appears: rhombohedral ITO phase. The determined band gap energies could recommend the rhombohedral ITO structure for visible light photocatalytic applications. The phase dynamics together with the concentration range for existence of the solid solutions in the InOOH-SnO2 and In2O3-SnO2 composite semiconducting nanoparticle systems have been evidenced and discussed. (C) 2013 Elsevier B.V. All rights reserved.

A kinetic analysis under non-isothermal conditions has been performed on europium-doped phosphate glasses with molar composition 20.42 Li2O-10.25 Al2O3-58.49 P2O5-7.23 BaO-1.44 La2O3-2.16 Eu2O3 and particle size 50 mu m. Differential scanning calorimetry measurements at four heating rates, from room temperature up to 900 degrees C using synthetic air have revealed that no significant mass change occurs during the heat treatment, as normally expected for glass samples. The step changes in heat flow signals are associated with the presence of three important effects: the first one, that occurs as a slope corresponds to the glass transition effect (T-g) is followed by two exothermic peaks, first of them more pronounced, associated with the first crystallization process (T-p1), while, the second one, lower in intensity corresponds to the second crystallization (T-p2) process. As expected, all peaks (T-g, T-p1 and T-p2) increase with the increasing of the heating rate. Both the activation energy of crystallization process and the crystallization mechanism were comparatively analyzed by two free-model estimations and using the formal theory of transformations for heterogeneous nucleation. (C) 2014 Elsevier Ltd and Techna Group S.r.l. All rights reserved.

Cobalt chromites (CoCr2O4) powders have been synthesized via thermal decomposition of oxalate precursor compounds (NH4)(4)[CoCr2(C2O4)(4)(OH)(4)]center dot 7H(2)O (I) and (Na-4)(12)[CoCr2(C2O4)(8)(OH)(4)]center dot(NH4)(2)C2O4 center dot 12H(2)O (II). The oxalate precursors have been characterized by infrared (IR) and ultraviolet visible spectroscopy (UV-vis), X-ray diffraction (XRD), scanning electron microscopy (SEM) and thermal analysis. The structure, morphology and magnetic properties of CoCr2O4 powders have been investigated by XRD, SEM, IR and Raman spectroscopy (RS), UV-vis and magnetic measurements. XRD patterns confirmed the formation of spinel-type cobalt chromite, with average crystallite sizes calculated from XRD patterns of 38 nm and 58 nm, for spinel chromites from precursors I and II, respectively. SEM micrographs revealed particle sizes between 30 and 130 nm, with a low degree of aggregation of primary nanocrystallites. Both CoCr2O4 powders presented ferrimagnetic ordering below the Currie temperature (T-c) and a phase transition at T-s similar to 20 K attributed to the onset of long-range spiral magnetic order. (C) 2014 Elsevier Ltd and Techna Group S.r.l. All rights reserved.

Tetragonal Sr2FeMoO6 powders were prepared by the sol gel and solid-state reaction methods. The structure, microstructure and magnetic characteristics of the double perovskite Sr2FeMoO6 in the form of as-prepared powders and classical sintered ceramics were analyzed and compared. Moreover, the magnetic properties of Sr2FeMoO6 ceramics obtained by sol gel and solid state reaction methods and sintered by the classical method were compared with those of Sr2FeMoO6 ceramics obtained by the same two methods, but sintered by the spark plasma sintering technique. The morphology of the powders obtained from the gel precursor and oxides mixture was characterized by homogeneity, as well as the grains shape and size. The powder prepared by the sol gel method was finer (particle average size of 0.6 mu m) than those obtained from oxides mixture (particle average size of 0.9 mu m). Sintered ceramics with tetragonal Sr2FeMoO6 phase were prepared from the two mentioned powders by classical sintering at 1200 degrees C, 2 h in 5%H-2/Ar. The pellets obtained from the gel powder exhibited higher magnetic characteristics than those derived from the oxides mixture. The saturation magnetization and the total magnetic moment of the samples prepared by the sol-gel method were M-sat=41.18 emu/g and mu(exp)/f.u.=3.26, respectively, while for the samples derived from the oxides mixture were M-sat=40.77 emu/g and mu(exp)/f.u=3.10. Also, Sr2FeMoO6 pellets sintered by the conventional method showed higher saturation magnetization values than those sintered by spark plasma sintering technique. (C) 2014 Elsevier Ltd and Techna Group S.r.l. All rights reserved.

Multivalence Ce and Sn oxide doped materials are of critical importance in many renewable energy applications, especially in a porous form. Of special interest is the understanding of the basic properties of Ce-Sn-O nanoparticles and the effect of doping with different trivalent (Fe3+, Yb3+, Gd3+) elements, as well as developing Ce-Sn-O materials in the form of homogeneous and heterogeneous multilayers with unique properties at high temperature. We discuss various applications of nanosize metal-oxide sensors and energy conservation through improved energy efficiency such as renewable sources and fuel cells. In addition, ceria and ceria-based materials are studied for their electronic, magnetic, optical, and catalytic properties, which are important in applications such as gas sensors, heterogeneous catalysis, solid electrolyte fuel cells (SOFC), and UV-shielding application. Additionally, at the nanoscale, the surface area of metal oxide particles is dramatically increased, which not only increases oxygen exchange but also makes it easy for redox reactions.

Ferrofluid samples consisting of magnetite nanoparticles (NPs) coated with oleic acid and dispersed in a non-polar organic solvent have been synthesized by chemical routes. Different volume fractions, phi, of magnetic NPs were considered. The overall structural characterization of NPs has been performed by x-ray diffractometry, with lattice parameters and average coherence lengths evaluated via Rietveld refinements. The magnetic properties of different samples have been analysed by SQUID magnetometry and temperature-dependent Mossbauer spectroscopy and finally explained by adequate magnetic relaxation mechanisms. Zero field cooling-field cooling protocols provided useful information about specific volume fraction dependent magnetic relaxation and de-freezing processes, the lack of the Verwey transition and stronger dipolar interactions at higher volume fractions. Anisotropy energies as obtained by both temperature dependent Mossbauer spectroscopy and magnetometry data are compared and a new procedure for a quantitative characterization of the dipolar interactions is proposed.

Trace amounts of substitutional Mn2+ ions and shallow donors magnetic centers were identified by electron paramagnetic resonance (EPR) in crystalline Zn(OH)(2) prepared by precipitation of a Zn-nitrate solution with NaOH. Strong changes in the Mn2+ ions spectrum, as well as a sharp increase in the concentration of the shallow donor centers were observed by EPR in the 110-140 degrees C temperature range, during pulse annealing experiments in air up to 240 degrees C. They reflect the decomposition of the crystalline Zn(OH)(2) host lattice into nanocrystalline ZnO, confirmed by X-ray diffraction and thermal analysis measurements. Accurate spin Hamiltonian parameters of the observed paramagnetic centers were determined by lineshape simulation and fitting of the EPR spectra, to be used as reference data in further studies of nanocrystalline systems involving Zn(OH)(2). (C) 2012 Elsevier B.V. All rights reserved.

The paper reports on magnetite successfully functionalized with two new molecules. The investigations, involving chemical and physical methods, provided relevant features involving cell parameters and grain sizes, or the intermingling ratio between magnetite and functionalizing molecules, as deduced from magnetic measurements. A large amount of interesting data concerning various surface and local interaction mechanisms was supplied by detailed Mossbauer measurements. The new outputs are explained in terms of material processing and intimate mixing of the involved molecules.

Double perovskite Sr2FeMoO6 was prepared by two ways consisting in sol gel technique and solid-state reaction method. The resulting powders from gel and mixed oxides precursors showed microstructures consisting of very fine grains (0.5-0.8 mu m) and a crystalline perovskite structure. The structural and microstructural properties of the double perovskite Sr2FeMoO6 powders as-prepared and ceramics were compared. Tetragonal Sr2FeMoO6 pellets were prepared from the two powders by spark plasma sintering at: 1000, 1100 and 1200 degrees C and then annealing at 1200 degrees C, 2 h in 5%H-2/Ar. The pellets presented different magnetic characteristics. The saturation magnetization of the samples prepared by sol-gel is close to those prepared by conventional synthesis method. (C) 2013 Elsevier Ltd. All rights reserved.

Sol-gel chemistry within the pores of a polycarbonate template membrane was used for the preparation of Eosin Y-SiO2 hybrid nano- and microrods, using tetraethylorthosilicate [TEOS, Si(OC2H5)(4)] as the precursor in the presence of trifluoroacetic acid (TFA) catalyst. The ethanolic solution of Eosin-Y was added to the silica sal to trap dye molecules inside the SiO2 gel network during the gelation. Structural and morphological characterization using scanning electron microscopy (SEM) and luminescence microscopy have shown the formation of rods with 200 nm and 1.2 mu m diameter and about 30 mu m length, exhibiting luminescence properties. Spectroscopic characterization has shown that the luminescence is due to Eosin-Y molecule in the xerogel porous network, surrounded by a solvation shell given mainly by the water. (C) 2013 Elsevier B.V. All rights reserved.

Oxalates containing various 3d transitional elements and positive NH(4) or negative OH groups were newly synthesized. Each above-mentioned component has directly influenced the structure, the electronic or interaction properties, while some unexpected behaviors were revealed by various magnetic and Mossbauer measurements. The main magnetic parameters, the long-range anti-ferromagnetic couplings observed at very low temperature and, particularly the uncompensated moment are discussed in detail. The induced lower spin states for bivalent ions and especially the anti-parallel arrangement of the spins belonging to trivalent and bivalent iron inside the molecule are also emphasized. (C) 2010 Elsevier B.V. All rights reserved.

BaTi0.87Sn0.13O3 (BTS13) nanopowder was prepared by low-temperature aqueous synthesis (LTAS) method. The evolution of the structure and microstructure of the precursor precipitate, heated at temperatures up to 1000 degrees C was studied by TGA, FT-IR, SEM and XRD techniques. The dried precipitate showed a microstructure consisting of nano-sized grains (similar to 40 nm) with great tendency to agglomeration. BaTi0.87Sn0.13O3 single phase was obtained at 800 degrees C. The ceramics prepared from as-obtained BTS13 powders (60-70 nm) show good dielectric and ferroelectric characteristics. The dielectric constant was about 4800 and the dielectric loss (tan delta) was 0.229 at 1 kHz and at the Curie temperature (31 degrees C). The remanent polarization (P-r) and the coercive field (E-C) of Ba0.97Ho0.03TiO3 ceramics, at 1 kHz, were P-r = 13 mu C/cm(2) and E-C = 0.89 kV/cm. The ferroelectric parameters E-C and P-r decrease with increasing frequency in the domain 100 Hz to 10 kHz. (C) 2011 Elsevier B.V. All rights reserved.

Doped ceria powders, Ce-0.8 Ln(0.2)O(2-x) (Ln = Gd3+, Sm3+ and Yb3+) were sintered to nearly full density by Spark Plasma Sintering at 1100 and 1200 degrees C. The starting powders were obtained via a sol-gel method and had nanometric dimensions: 26.4 nm (Gd), 19.3 nm (Sm) and 31.4 nm (Yb). Samples characterization was performed by SEM, TEM and XRD to determine their structural and microstructural characteristics. The ionic conductivities of the sintered samples were determined by impedance measurements. The influence of the chemical composition, sintering temperature and microstructural characteristics on the total ionic conductivity were evaluated and discussed.

The article reports the preparation and complex characterization of iron-containing phosphate glasses considered to be ecological materials, as they contain nontoxic compounds related to environment. The oxide system Li2O-MgO-(CaO)-Al2O3-P2O5-(FeO/Fe2O3) was investigated in respect to its structural changes caused by MgO replacement with CaO and by the iron addition. UV-vis-NIR (ultraviolet-visible-near infrared) spectroscopy as well as thermo-gravimetric (TG) measurements, differential thermo-analysis (DTA), X-ray diffraction (XRD) analysis, electronic paramagnetic resonance (EPR), and Mossbauer (nuclear gamma resonance) spectroscopy have been used to investigate redox states and coordination symmetry of iron, together with vitreous network changes during the heat treatment up to 1000 degrees C. UV-vis-NIR transmission spectroscopy revealed no structural modifications when MgO was substituted by CaO, but noteworthy absorption bands attributed to Fe2+/Fe3+ species. TG analysis made in the 20-1000 degrees C range shows low weight loss accompanied by several thermal effects, as evidenced by DTA. XRD patterns for the glass samples heat treated at about 700 degrees C revealed the presence of different phosphate crystalline phases containing Mg, Al, and Fe ions. EPR spectroscopy revealed the presence of paramagnetic Fe3+ ions and the change of the first coordination symmetry, when the samples are heated below the vitreous transition temperature. Mossbauer spectroscopy has evidenced two paramagnetic species, Fe2+ and Fe3+, both in octahedral coordination symmetry and a clustering process supported by only Fe3+ ions.

In this work, we synthesized the properties of bioactive nanocrystalline hydroxyapatite (HAp), Ca-10(PO4)(6)(OH)(2) ceramic powder and nanocrystalline HAp doped with europium (III). The europium doped hydroxyapatite with an atomic ratio Eu/(Eu +Ca) between 2% and 20% were synthesized. The structure, morphology and optical properties were characterized by Xray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), and Fourier transform infrared spectroscopy (FT-IR). The XRD results reveal that the obtained Eu: HAp shows the characteristic peaks of hydroxyapatite in a hexagonal lattice structure. The results indicated that Eu3+ has been successfully doped into the framework of HAp.

Double perovskite Sr2FeMoO6 type compounds show special properties, such as magnetoresistance response at relatively small-applied fields and at rather high temperatures (ca. 400 K). Perovskite precursors were obtained unconventionally, in liquid phase, using oxalic acid as complexing agent, in the presence of ethylene glycol as polymerization agent. Ordering control concerning the magnetic properties is predictable to be strongly influenced by the synthesis route. The thermal stability of the precursors and the phase transitions of the oxide samples were analyzed by thermal analysis method, IR spectroscopy, Mossbauer spectroscopy, X-ray diffraction method and magnetic measurements. The experimental data for the perovskite compounds prepared by using oxalic acid as complexing agent revealed a double perovskite structure of analyzed samples, convenient magnetorezistive response (3.51 mu(B)/f.u), in good agreement with the Mossbauer spectra. Moreover, Mossbauer spectreoscopy allows the distinction between the ordered and the disordered phases of the perovskite structure and put in evidence the strong dependence of the structural and magnetic characteristics of the double perovskites on the synthesis route.

In present work, complex mixtures were designed based on fused SiO2, beta-SiC and different oxide additives. The addition of Al2O3 and mulite - 3Al(2)O(3) 2SiO(2) influence was investigated in order to obtain high temperature strength, thermal shock resistant and corrosion resistant composites. Thermal treatment was conducted in conventionally electric furnace in air and in argon respectively, in the 800-1250 degrees C temperature range. Sintered composites were characterised by bulk density, open porosity, and thermal shock resistance and thermal expansion measurements. The crystalline phase evolution in conjunction with each heat curing procedure was analysed by X-ray diffraction and FTIR spectrometry. Microstructure investigation of sintered samples was carried using scanning and transmission electron microscopy. The relationship between the FTIR spectra and structure of the powders and sintered composites was explained.

Small particles of iron - based magnetic spinel oxide are technologically interesting because of their magnetic properties. The synthesis from solution, generally achieved by coprecipitation, offers some advantages: simple and rapid preparation, control of particle size and composition, various possibilities to modify the particle surface state allowing to make homogeneous and stable dispersion in liquid or solid media. This work reports the thermal studies of magnetic iron spinel oxide nanoparticles. For this study, the Fe2+-Fe3+ mixture (Fe2+/Fe3+=0.5) was introduced in an alkaline solutions of which the pH was kept constant. The influence of the particles sizes on the Y -> aFe(2)O(3) transformation is analyzed.

The iron oxide-based nanomaterials have a great importance because of their impact on a wide number of industries. They have many properties and applications in domains as: environmental protection, biomedical, catalysis, information displays and electronics. In order to avoid the tendency of nanoparticles to aggregate, they are often included in sol-gel derived silica matrices, thus being also ensured a homogeneous dispersion of the ultra-fine metal oxide particles in the host matrix. The reasons of the attempt are both an economic and a non-pollutant one, tacking into account the fact that it is well known that aqueous silica sol is cheaper and less toxic than TEOS. The Fe3O4 was introduced in the reaction mixture as aqueous suspension. A final iron content related to SiO2 of 3% wt. was chosen for the prepared nanocomposite. Thermal analysis, IR spectroscopy, XRD and TEM methods have been used for the structural characterisation,. Some experiments of water depollution (from As) have been proceeded using the prepared Fe3O4-SiO2 nanocomposite.

Sr2FeMoO6 was synthesizes by soft chemistry route using citric and/or oxalic acid as complexing agents. This method provides good compositional control with promising results as a base for further improvements. The material shows complex temperature- and field(magnitude and orientation) dependent electro-magnetic behavior as probed by magnetic and transport measurements. The zero-field cooling curves of magnetization versus temperature taken at different magnetic fields, show two temperature regions separated by a transition temperature T-cups(ZFC). When H increases, T-cups(ZFC) values decrease. At 5 K and 5 T the saturation moment is 3.55 JIB per formula unit, and the coercitive force is 0.021 T. The relative value of the magnetoresistive effect (i.e. 100 (rho(H)-rho(0))/rho(H), %, with rho being resistivity) at 5 K is 68% and 36% when applied field H is parallel and perpendicular the measuring current I, respectively. The results are discussed in relation to magnetic sublattices and the interaction that produces anti-site defects and spin-dependent electron anisotropy. (C) 2006 Elsevier B.V. All rights reserved.

TiO2 anatase doped with 0.5 at%Fe powders were prepared by sol-gel technique. Titanium (IV) butoxide and iron (III) acetylacetonate were used as starting precursors, n-butanol as solvent, acetylacetone is added as a chelating agent and acetic acid to decrease the kinetics of the hydrolysis and condensation of Ti(O-Bu-n)(4). The evolution of the network bonds and the structural characterization of the gel were studied by thermogravimetric analysis (TG), differential thermal analysis (DTA), differential thermogravimetric analysis (DTG), Fourier transform infrared spectroscopy(FTIR) scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X-ray diffraction (XRD) techniques, respectively. A gelprecusor nanopowder with the mean grain size of about 15-20 nm was obtained. In order to prepare a Fe-cloped TiO2 material with the structure of the anatase, a thermal treatment at 450 degrees C, 3 h in air, was fund enough.

Recently, a double perovskite oxide, Sr2FeMoO6, has been reported to show a very sharp magnetoresistance (MR) response at relatively small-applied fields and at high temperatures. The half-metallic state of this compound ensures a theoretical magnetic moment of 4 mu(B) per formula unit. Ordering control is expected to be influenced by the synthesis route. In this regard, in this article, perovskite samples were obtained from the liquid phase, using oxalic acid as complexing agent. Application of a field above 0.08 T increases the zero-field-cooled (ZFC) magnetization. Below this field, for the ZFC-curves measured from 2 K up to 400 K, magnetization increases, reaching a peak at T-cups(ZFC), before decreasing cups gradually to a paramagnetic state. Saturation moment is relatively low (2.1-2.2 mu(B)), probably due to anti-site defects, as suggested in the literature.

A composite material with applications in optoelectronics has been investigated. Pulsed laser deposition CdSe-doped glass film was prepared by the combinatorial deposition from two targets, namely pure CdSe and glass belonging to the 20Li(2)O-10Al(2)O(3)-7BaO-2La(2)O(3)-2ZnO-59P(2)O(5)system. Exciton peaks in the Vis domain, related to electron-hole pairs transitions from the valence band to the conduction band, were revealed in the optical absorption spectra of the CdSe-doped film. CdSe quantum dots (QDs) band gap energy depends on the CdSe quantum confinement effect. CdSe-doped film photoluminescence exhibits peaks in the red domain assigned to CdSe transitions from the excited state to the ground state. The size of CdSe nanoclusters, determined from x-ray diffraction is correlated with scanning electron microscopy-energy dispersive x-ray spectroscopy and atomic force microscopy results. Vibration modes specific both to CdSe QDs and to the vitreous network have been evidenced by Fourier transform infrared and Raman spectroscopy.