Characterization of Pr-Doped LaF3 Nanoparticles Synthesized by Different Variations of Coprecipitation Method

A set of Pr3+:LaF3 nanoparticles (NPs) were synthesized via coprecipitation method at three stoichiometric proportions of La(NO3)3, Pr(NO3)3, and NaF (1 : 0.8, 1 : 1, and 1 : 6, respectively). Two ways of mixing of the La(NO3)3, Pr(NO3)3, and NaF solutions (dropwise and swift addition) were used. One sample was subjected to microwave (MW) treatment for 30, 90, and 180 min. All the samples were characterized by transmission electron microscopy (TEM) and X-ray diffraction (XRD). For all the samples, optical spectroscopy experiments were carried out. The XRD data were analyzed via the Debye-Scherrer and Williamson-Hall methods. It was revealed that the way of mixing of the La(NO3)3, Pr(NO3)3, and NaF solutions strongly affects the shape of the NPs. The slow dropwise addition of the NaF solution leads to the plate-like NP (PLNP) formation; otherwise, the swift addition of the NaF solution leads to the formation of more sphere-like NPs (SLNPs). The size and regularity in shape of the NP increase with the increasing stoichiometric proportion of La(NO3)3, Pr(NO3)3, and NaF from 1 : 0.8 to 1 : 6. The size and regularity in shape of the SLNPs increase with the increasing time of MW treatment. The Debye-Scherrer and Williamson-Hall methods confirmed the anisotropic shape of the PLNPs. The Williamson-Hall method showed that the values of strain are almost similar for all the samples (around 14∗10-4). Optical spectroscopy experiments revealed that although all the samples have an equal chemical composition, the luminescence lifetimes for different samples differ between each other. The luminescence lifetime of the PLNPs is less than that of the SLNPs having an equal stoichiometric proportion of La(NO3)3, Pr(NO3)3, and NaF. The luminescence lifetime of the 1 : 1 SLNPs increases with the increasing time of MW treatment.

Kinetic properties and structural analysis of LaCrO3 nanoparticles

LaCrO3 perovskite nanopowders were successfully prepared via a sol-gel method using stoichiometric proportion of materials containing lanthanum and chromium in stearic acid complexing agent. Structural analysis of LaCrO3 indicated an octahedral framework in its XRD pattern bearing crystallite size in the range of 28 nm. The particle sizes were confirmed by morphological scanning of the sample. The optical properties of LaCrO3 nanopowders clearly indicated an interesting optical activity of LaCrO3 in the UV and visible ranges. The degradation activation energy (Ed) was calculated from the output of a moderate thermal programming profile at about 207.97 kJ·mol-1 using Kissinger equation. Capacity, impedance and AC resistance of the perovskites was obtained at 2.970 nF, 2.522 MΩ and 16.19 MΩ, respectively.

Structure and Inverse Magnetocaloric Effect of Mn1.2Co0.8Si0.2P0.8 Compound Prepared by SPS

The single-phase Mn1.2Co0.8Si0.2P0.8 compound was fabricated by the spark plasma sintering (SPS) technology followed by vacuum annealing. The microstructure, Néel temperature (TN) and “inverse” magnetocaloric effect of this compound were investigated. The results show that the structure of Mn1.2Co0.8Si0.2P0.8 compound prepared by SPS is a single phase with precise stoichiometric proportion. Increasing the magnetic field from 0.05 T to 1 T, the TN of the material reduces gradually from 110 k to 45 k, and a splitting of TN appears. The splitting of the antiferro-to-ferromagnetic transition is an intrinsic feature rather than the secondary phase. Though the maxima entropy changes is about 0.6 Jkg-1K-1 at B=5T, the Mn1.2Co0.8Si0.2P0.8 phase synthesized by SPS is more favorable, more overall magnetic moment. In addition to the magnetic refrigeration applications, this compound may be used in thermomagnetic generators.

Synthesis of AlN-SiC Ceramics by Hot Pressing

AlN-SiC ceramics were prepared at 1950°C by hot pressing (HP) of AlN/SiC powders in stoichiometric proportion. The sintered product was characterized using X-ray diffraction (XRD). Scanning electron microscopy (SEM) with energy-dispersive spectroscopy (EDS) were utilized to investigate the morphology characteristics. The results show that AlN-SiC phase is well-developed with a close and lamellar structure. The grains are plate-like with the size of 1-3μm, the thickness of 3-5μm and elongated dimension. The results showed that the products had the density of 99 percent of the theoretical, bending strength of 550-800 MPa and fracture toughness of 5-6 MPa·m1/2. The distribution of AlN-SiC grains is relatively uniform.

The Study of Theoretic Coated Carbon Amount and Excess Lithium in LiFePO4/C Synthesis by Means of Carbon Thermal Reduction Route

LiFePO4/C(LFP/C) composite cathode material was synthesized by carbon thermal reduction route with the sucrose as reducing agent and characterized by X-ray diffraction (XRD) and scanning electron microscope (SEM). Some parameters were optimized by means of determining the amount of sucrose and Li2CO3. The electrochemical performances were also tested through assembling batteries. The experimental results demonstrated that the proper theoretic coated carbon amount was 11.4% and 4.21% respectively, and the proper lithium usage is the normal stoichiometric proportion, namely, the lithium amount is not excess.

Variation of Tungsten Oxide Reduction Mode Using Different High Energy Milling Conditions

High energy ball milling has been used like alternative route for processing of materials. In the present paper, the reduction of tungsten oxide by aluminum in order to obtain metallic tungsten was studied using a SPEX type high energy mill. A powdered mixture of WO3and metallic aluminum, weighed according to the stoichiometric proportion with an excess 10% Al, was processed with hardened steel utensils using a 1:6 powder-to-ball ratio. The processing was carried out with milling jar temperature measurement in order to detect the reaction type. The temperature evaluation indicated the self-propagating reaction occurrence by fast increase of the jar temperature after a short milling time. The tungsten oxide reduction was verified by X-Ray Diffraction (XRD) analysis and the milling products were characterized by Scanning Electron Microscopy (SEM). The results were slightly different from the literature due to the mill type and milling parameters used in the work.

Influence of the Urea Content in the Combustion Synthesis for Preparation of NiAl2O4 Support Catalytic to Steam Reforming of Methane

The aim of this work is to evaluate the catalytic performance in steam reforming of methane of the NiAl2O4catalysts prepared by combustion reaction with different urea levels. The catalysts were prepared with urea in the stoichiometric proportion, and with excess of 10% and 20%. The samples were characterized by DRX, textural analysis by nitrogen adsorption, SEM, TPR, and then, catalytically evaluated in the methane reforming reaction. The results showed the presence of NiAl2O4and traces of NiO for all the samples. The increase of the urea content caused an increase in the particle size and a reduction in the surface area, from 171 to 35 m2/g. All the samples presented irregular morphology. The TPR curves showed peaks of reduction of the NiO species, and reduction of nickel present in the NiAl2O4. Regarding the conversion of methane to synthesis gas, it was observed that the increase of the urea content allowed obtaining higher conversion. However, it was also observed a rapid deactivation of these catalysts due to high coke deposition on the active phases surfaces.

Influence of Fuel in the Synthesis of ZnAl2O4 Catalytic Supports by Combustion Reaction

The aim of this work is to evaluate the influence of fuel in the synthesis of ZnAl2O4 catalytic supports by combustion reaction. For this, it was used the fuels: urea, carbohidrazide, glycine and aniline. The total amount of reagents was calculated according to the theory of propellants and explosive using urea in the stoichiometric proportion (Φe = 1). The structural and morphological characteristics of the powders were evaluated by XRD, FTIR, TEM, SEM and particle size distribution. The results from XRD showed the formation of the normal cubic spinel structure. The powders presented nanosized particles with narrow agglomerates size distribution. The powders prepared with urea showed better value of surface area and smaller crystallite size.

Morphologic and Structural Characterization of the CoFe2O4 Synthesized by Combustion Reaction

CoFe2O4 powders were synthesized by combustion reaction using glycine as fuel, aiming obtaining nanosized and monophase powders. Thus, different conditions of external heating during the synthesis were investigated. The powders were prepared according to the propellants and explosives theory, using glycine as fuel in the stoichiometric proportion (Φe = 1). During the synthesis the flame temperature and time were measured. The resulting powders were characterized by X-rays diffraction and scanning electronic microscopy (SEM). The results show that the condition in which the synthesis was done it influences in the combustion flame temperature and time and contributes for the obtainment of powders with majority phase without secondary phases. Crystallite size varied of 33 to 50 nm. All powders presented morphology constituted by soft agglomerated formed by nanoparticles.

Structure determination and Rietveld refinement of Y0.8Ca0.2Ba1.8La0.2Cu3Oy

The structure of the new Y0.8Ca0.2Ba1.8La0.2Cu3Oy (YBLCO) compound was obtained at 298 K from X-ray powder diffraction data and refined by the Rietveld technique. YBLCO has a structure isotypical with YBa2Cu3Oy (YBCO) at room temperature. The crystal data are: Y0.81Ca0.19Ba1.8La0.2Cu3O7.08, Mw=657.69, orthorhombic system, space group Pmmm, a=3.8731(1) Å, b=3.8249(1) Å, c=11.6602(3) Å, V=172.740(13) Å3, Z=1, dx=6.325 g/cm3; the structure was refined with 37 parameters to Rwp=7.66%, Rp=5.86%, and Rexp=5.11% for 2001 data points. Moreover, the proportions of Ca and La were refined to be 0.19 and 0.2, in agreement with the stoichiometric proportion of 0.2.