Application of the Potentiometric Stripping Analysis with Constant Current for the Determination of Lithium Ions Using a Spinel-Type Manganese (IV) Oxide-Modified Carbon Paste Electrode

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Study of the potentiometric response of the doped spinel Li1.05Al0.02Mn1.98O4 for the optimization of a selective lithium ion sensor

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Electrochemical evaluation of the a carbon-paste electrode modified with spinel manganese(IV) oxide under flow conditions for amperometric determination of lithium

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Columnar microstructure of nanocrystalline Ga1-xMnxN films deposited by reactive sputtering

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Resonant excitation of Mn local vibrational modes in the higher order Raman spectra of nanocrystalline Ga(1-x)Mn(x)N films

The effect of manganese on the vibrational properties of Ga(1-x)Mn(x)N (0 <= x <= 0.18) films has been investigated by Raman scattering using 488.0 and 632.8 nm photon excitations. The first-order transverse and longitudinal optical GaN vibrational bands were observed in the whole composition range using both excitations, while the corresponding overtones, as well as a prominent peak located in 1238 cm(-1) (153.5 meV) were only observed in the Mn-containing films under 488.0 nm excitation. We propose that the peak observed at 1238 cm(-1) is due to resonant Mn local vibrational modes, the excitation process being related to electronic transitions involving the Mn acceptor band.

Disorder effects produced by the Mn and H incorporations on the optical absorption edge of Ga1-xMnxAs:H nanocrystalline films

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

The optical absorption edge of nanocrystalline Ga(1-x)Mn(x)N films deposited by reactive sputtering

We have focused on the optical absorption edge of nanocrystalline Ga(1-x)Mn(x)N (0.00 <= x <= 0.18) films deposited by reactive RF magnetron sputtering. The films obtained are nanocrystalline with grain sizes of about 25 nm, having wurtzite structure and strong orientation texture in the c-axis direction. The optical characterizations of the absorption edges were obtained in the 190-2600 nm spectral range. The increase of the Mn content causes an increase of the absorption coefficient which can be clearly noticed at low energies, and a quasi-linear decrease of the optical gap. Broad absorption bands observed around similar to 1.3 and similar to 2.2 eV were associated with transitions between the Mn acceptor level and the valence and conduction bands, respectively. The observed changes in the optical properties due to the Mn incorporation observed in these nanocrystalline films are similar to those reported for ferromagnetic GaMnN single-crystal films.

Structural Characterization of Nanocrystalline Sb-Doped SnO2 Xerogels by Multiedge X-ray Absorption Spectroscopy

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Síntese, sinterização e caracterização de ferritas à base de Ni-Zn

Were synthesized different ferrites NixZn1-xFe2O4 (0,4 ≤ x ≤ 0,6) compositions by using citrate precursor method. Initially, the precursors citrates of iron, nickel and zinc were mixed and homogenized. The stoichiometric compositions were calcined at 350°C without atmosphere control and the calcined powders were pressed in pellets and toroids. The pressed material was sintered from 1100º up to 1200ºC in argon atmosphere. The calcined powders were characterized by XRD, TGA/DTG, FTIR, SEM and vibrating sample magnetometer (VSM). All sintered samples were characterized using XRD, SEM, VSM and measurements of magnetic permeability and loss factor were obtained. It was formed pure ferromagnetic phase at all used temperatures. The Rietveld analyses allowed to calculate the cations level occupation and the crystallite size. The analyses obtained nanometric crystals (12-20 nm) to the calcined powder. By SEM, the sintered samples shows grains sizes from 1 to 10 μm. Sintered densities (ρ) were measured by the Archimedes method and with increasing Zn content, the bulk density decrease. The better magnetization results (105-110 emu/g) were obtained for x=0,6 at all sintering temperatures. The hysteresis shows characteristics of soft magnetic material. Two magnetization processes were considered, superparamagnetism at low temperature and the magnetic domains formation at high temperatures. The sintered toroids presents relative magnetic permeability (μr) from 7 to 32 and loss factor (tanδ) of about 1. The frequency response of toroids range from 0,3 kHz to 0,2 GHz. The composition x=0,5 presents both greater μr and tanδ values and x=0,6 the most broad range of frequency response. Various microstructural factors show influence on the behavior of μr and tanδ, such as: grain size, porosity across grain boundary and inside the grain, grain boundary content and domain walls movement during the process of magnetization at high frequency studies (0,3kKz 0,2 GHz)

Síntese análise das propriedades magnéticas da ferrita de NiMg e características de absorção de radiação

It was synthesized different Ni1-xMgxFe2O4 (0,2 ≤ x ≤ 0,7) compositions by use of citrate precursor method. Initially, the precursory citrates of iron, nickel and magnesium were mixed and homogenized. The stoichiometric compositions were calcined from 350°C to 1200°C at ambient atmosphere or in argon atmosphere. The calcined powders were characterized by XRD, TGA/DTG, FTIR, magnetic measures and reflectivity using the wave guide method. I was observed pure magnetic phase formation between 350°C and 500°C, with formation of ferrite and hematite after 600°C at ambient atmosphere. The calcined powder at argon atmosphere formed pure ferromagnetic phase at 1100°C and 1200°C. The Rietveld analyses calculated the cations level occupation and the crystallite size. The analyses obtained nanometric crystals (11-66 nm), that at 900°C/3h presents micrometric sizes (0,45 - 0,70 Om). The better magnetization results were 54 Am2/Kg for x= 0,2 composition, calcined at 350°C/3h and 30 min, and 55,6 Am2/Kg for x= 0,2 1200°C, calcined in argon. The hysteresis shows characteristics of soft magnetic material. Two magnetization processes were considered, superparamagnetism at low temperature and the magnetic domains formation at high temperatures. The materials presented absorption less or equal the 50 % in ranges specific frequency. As for the 2,0 and 3,0 thickness (in 11,0 - 11,8 GHz), the reflectivity of the x= 0,3, 0,5 and 0,4 compositions, all calcined at 900°C/3h showed agreement with MS and O. Various factors contribute for the final radiation absortion effect, such as, the particle size, the magnetization and the polymer characteristics in the MARE composition. The samples that presented better magnetization does not obtaining high radiation absorption. It is not clear the interrelaction between the magnetization and the radiation absorption in the strip of frequencies studied (8,2 - 12,4 GHz)

Estudo das características magnéticas e absorvedoras das ferritas de nizn, niznmn, mnzn, nimg, nicuzn e nicuznmg obtidas via método do citrato precursor

Were synthesized systems Ni0,5Zn0,5Fe2O4, i0,2Zn0,5Mn0,3Fe2O4, Mn0,5Zn0,5Fe2O4, Ni0,5Mg0,5Fe2O4, Ni0,2Cu0,3Zn0,5Fe2O4 and Ni0,2Cu0,3Zn0,5Mg0,08Fe2O4, the precursors citrate method. The decomposition of the precursors was studied by thermogravimetric analysis and spectroscopy in the infrared region, the temperature of 350°C/3h. The evolution of the phases formed after calcinations at 350, 500, 900 and 1100ºC/3h was accompanied by X-ray diffraction using the Rietveld refinement to better identify the structures formed. The materials were also analyzed by scanning electron microscopy, magnetic measurements and analysis of the reflectivity of the material. The samples calcined at different temperatures showed an increase of crystallinity with increasing calcination temperature, verifying that for some compositions at temperatures above 500°C precipitates of second phase such as hematite and CuO. The compositions of manganese present in the structure diffusion processes slower due to the ionic radius of manganese is greater than for other ions substitutes, a fact that delays the stabilization of spinel structure and promotes the precipitation of second phase. The compositions presented with copper precipitation CuO phase at a temperature of 900 and 1100ºC/3h This occurs according to the literature because the concentration of copper in the structure is greater than 0.25 mol%. The magnetic measurements revealed features of a soft ferrimagnetic material, resulting in better magnetic properties for the NiZn ferrite and NiCuZnMg at high temperatures. The reflectivity measurements showed greater absorption of electromagnetic radiation in the microwave band for the samples calcined at 1100ºC/3h, which has higher crystallite size and consequently the formation of multi-domain, increasing the magnetization of the material. The results of absorption agreed with the magnetic measurements, indicating among the ferrites studied, those of NiZn and NiCuZnMg as better absorbing the incident radiation.

Síntese e caracterização de ferritas de níquel dopadas com cobalto e efeito da substituição nas suas propriedades magnéticas

The ferrite composition Ni1 - xCoxFe2O4 (0 ≤ x ≤ 0.75) were obtained by the method of microwave assisted synthesis and had their structural and magnetic properties evaluated due to the effect of the substitution of Ni by Co. The compounds were prepared: according to the concept of chemical propellants and heated in the microwave oven with power 7000kw. The synthesized material was characterized by absorption spectroscopy in the infrared (FTIR), Xray diffraction (XRD) using the Rietveld refinement, specific surface area (BET) , scanning electron microscopy (SEM) with aid of energy dispersive analysis (EDS) and magnetic measurements (MAV). The results obtained from these techniques confirmed the feasibility of the method of synthesis employed to obtain the desired spinel structure, the ferrite, nickel ferrite as for nickel doped with cobalt. The results from XRD refinement ally showed the formation of secondary phases concerning stages α - Fe2O3, FeO, (FeCo)O e Ni0. On the other hand, there is an increase in crystallite size with the increase of cobalt in systems, resulting in an increased crystallinity. The results showed that the BET systems showed a reduction in specific surface area with the increase of cobalt and from the SEM, the formation of irregular porous blocks and that the concentration of cobalt decreased the agglomerative state of the system. The magnetic ferrites studied showed different characteristics according to the amount of dopant used, ranging from a very soft magnetic material (easy magnetization and demagnetization ) - for the system without cobalt - a magnetic material with a little stiffer behavior - for systems containing cobalt. The values of the coercive field increased with the increasing growth of cobalt, and the values of saturation magnetization and remanence increased up to x = 0,25 and then reduced. The different magnetic characteristics presented by the systems according to the amount of dopant used, allows the use of these materials as intermediates magnetic

Síntese e caracterização da ferrita de MnZn obtida pelo método dos citratos precursores

It was synthesized MnZn ferrite with general formulae Mn1-xZnxFe2O4 (mol%), 0,3 ≤ x ≤ 0,7 by using the citrate precursor method. The precursors decomposition was studied by thermogravimetric analysis (TGA), differential thermogravimetric analysis (DTG), differential thermal analysis (DTA) and Fourier transform infrared (FTIR) of powder calcined at 350ºC/3,5h. X-ray diffraction pattern (XRD) of samples was done from 350 to 1200ºC/2h using various atmospheres. The power calcined at 350ºC/3,5h formed spinel phase. It is necessary atmosphere control to avoid secondary phase such as hematite. From 900 to 1200ºC was obtained 90,66 and 100% of MnZn spinel ferrite phase, respectively. Analysis by dispersive energy scanning (EDS) at 350ºC shows high Mn and Zn dispersion, indicating that the diffusion process was homogeneous. Semi-quantitative analysis by EDS verified that despite the atmosphere control during calcinations at high temperatures (< 800ºC) occurred ZnO evaporation causing stoichiometric deviation. Vibrating sample magnetometer (VSM) measures show soft ferrite material characteristics with Hc from 6,5 x 10-3 to 11,1 x 10-2 T. Saturation magnetization (Ms) and initial permeability (µi) of MnZn spinel phase obtained, respectively, from 14,3 to 83,8 Am2/kg and 14,1 to 62,7 (Am2/kg)T

Síntese, sinterização e caracterização de ferrita de níquel

In this work we obtain nickel ferrite by the combustion synthesis method whcih involves synthesising in an oven at temperatures of 750oC, 950oC and 125oC. The precursors oxidizing used were nickel nitrate, ferric as an oxidizing and reducing urea (fuel). After obtaining the mixture, the product was deagglomerated and past through a 270 mesh sieve. To assess the structure, morphology, particle size, magnetic and electrical properties of nanoparticles obtained the samples were sintered and characterized by x-ray distraction (XRD), x-ray fluorescence spectroscopy (FRX); scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), vibrating sample magnetometer (MAV ) and electrical permittivity. The results indicated the majority of phase inverse spinel ferrite and Hematite secondary phase nickel and nickel oxide. Through the intensity of the distraction, the average size of the crystallization peaks were half-height width which was calculated using the Scherrer equation. From observing the peaks of all the reflections, it appears that samples are crystal clear with the formation of nanoparticles. Morphologically, the nanoferritas sintered nickel pellet formation was observed with three systems of particle size below 100mn, which favored the formation of soft pellets. The average size of the grains in their micrometric scale. FRX and EDS showed qualitatively the presence of iron elements nickel and oxygen, where through quantitative data we can observe the presence of the secondary phase. The magnetic properties and the saturation magnetization and the coercive field are in accordance with the nickel, ferrite where the curve of hysteresis has aspects of a soft material. Dielectric constant values are below 10 and low tangent loss

The Effect of Coating Patterns with Spinel-Based Investment on the Castability and Porosity of Titanium Cast into Three Phosphate-Bonded Investments

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)