Physical characterization of K-doped 0.9PMN-0.1PT synthesized by an association of the columbite route and the polymeric precursor method

The solid solution 0.9PbMg 1/3Nb 2/3O 3-0.1PbTiO 3 is one of the most widely investigated relaxor ceramic, because of its high dielectric constant and low sintering temperatures. PMN-PT powders containing single perovskite phase were prepared by using a Timodified columbite precursor obtained by the polymeric precursor method. Such precursor reacts directly with stoichiometric amount of PbO to obtain pyrochlore-free PMN-PT powders. The structural effects of K additive included in the columbite precursor and 0.9PMN-0.1PT powders were also studied. The phase formation at each processing step was verified by XRD analysis, being these results used for the structural refinement by the Rietveld method. It was verified the addition of K in the columbite precursor promotes a slight increasing in the powder crystallinity. There was not a decrease in the amount of perovskite phase PMN-PT for 1mol% of K, and the particle and grain size were reduced, making this additive a powerful tool for grain size control.

Preparation of lanthanum doped Bi4Ti3O12 ceramics by the polymeric precursor method

Lanthanum-modified bismuth titanate, Bi4 - xLaxTi3O12 (BLT) ceramics, with x ranging from 0 to 0.75 were prepared by the polymeric precursor method. Orthorhombicity of the system is decreased with the increase of lanthanum content in the bismuth titanate (BIT) crystal lattice. No secondary phases were evident after lanthanum addition. Increasing lanthanum content causes a structural distortion in the bismuth titanate lattice. The shape of the grains is strongly influenced by the lanthanum added to the system. © 2005 Elsevier B.V. All rights reserved.

Thermoanalytical study of praziquantel-loaded PLGA nanoparticles

Polymeric nanoparticles have received great attention as potential controlled drug delivery systems. Biodegradable polymers has been extensively used in the development of these drug carriers, and the polyesters such as polylactic acid, polyglycolic acid and their copolymers as poly-lactide-co- glycolide are the most used, considering its biocompatibility and biodegradability. Thermal analysis techniques have been used for pharmaceutical substances for more than 30 years and are routine methods for screening drug-excipient interactions. The aim of this work is to use thermal analysis to characterize PLGA nanoparticles containing a hydrophobic drug, praziquantel. The results show that the drug is in an amorphous state or in disordered crystalline phase of molecular dispersion in the PLGA polymeric matrix and that the microencapsulation process did not interfere with the chemical structure of the polymer, mantaining the structural drug integrity.

Electrical devices obtained from polymeric precursors process

Nowadays, many investments have been made in the area of superconductor materials, with the aim to improve their potential technological applications. Applications on the energy transport using cables, to get high resolution images in the medicine use high magnetic fields, high speed signals use superconductor devices all of them are in crescent evidence and they are showing that the future is coming and next for this new kind of materials. Obviously that everything of this is possible due to the increasing of research with new materials, where the synthesis, characterization and applications are of the mainly objective of these researches. The production of cable for the energy transport has been in advanced stage as the bulks production is too. However, the film production that to aim at the electronic devices area is not as developed or it still need expensive investments. Thinking about that, we are developing a research where we may increase the relation of cost/benefits. Thereby, we are applying the polymeric precursors method to obtain films that will be used in the built of electronic devices. Thin films (mono and multilayers, on crystalline or metallic substrates, controlled thickness) of the BSCCO system have been obtained from dip coating deposition process with excellent results in terms of preferential orientation, controlled thickness, a large area, which may indicate future applications. Based on these results, we present an electrical circuit and their principal characteristics as superconductor transition (85K), transport current density and structure. DC four probes method, scanning electron microscopy, digital optical microscopy and X-ray diffractometry were some techniques used for the characterization of this superconductor electric device. © 2006 Materials Research Society.

Characterization of Zn0. 95Mn0.05O synthesized by polymeric precursors

This paper discusses the preparation and characterization of Zn 0.95Mn0.05O phase obtained by the polymeric precursor method for DMS applications. The as-obtained powders were calcined between 500 to 800°C and characterized by XRD, SEM and BET. The XRD analysis of the powder showed a crystalline material containing second phase. The crystallite sizes ranged from 20 to 51 nm. The micrographs showed that the powders consisted of soft and homogeneous agglomerations. The nitrogen adsorption/desorption curves of the Zn0.95Mn0.05O phases were type II curves, which is characteristic of mesoporous materials.

Structural and optical properties of Eu3+ and Mg2+ doped LiTaO3 obtained via the polymeric precursor method

This work reports on the pure lithium tantalate (LiTaO3), europium (III)-doped LiTaO3 and magnesium (II)-europium (III)-doped LiTaO3 preparared by the polymeric precursor method, using four different powered samples of Eu3+ ion concentrations 0.1 to 1at %. Structural and optical properties of powders have been studied. The different possible sites occupied by the rare earth were examined. The phase contents and lattice parameters were studied by the Rietveld method and the structural disorder in the LiTaO3 host caused by Eu3+ ions was analyzed. Results indicated LiTaO3 free of secondary phases at 650°C and the photoluminescence (PL) emission spectra showed the characteristic sharp emission bands given by Eu3+ ions when they are excited at a wavelength of 399 nm. An increase of dopants contents caused a non-homogeneous broadening and showed a slightly larger one when Mg was added. A displacement of the transition 5D0-7F0 to shorter wavelengths as function of Eu3+ concentration was also noticed.

High-density nanoparticle ceramic bodies: A study of heating rates in the sinterization of Gadolinium-doped Ceria

An investigation on the sinterization of Gd:CeO2 (Ce 0.85Gd0.15O1.9-δ ceramic system) 3-10 nm nanoparticles in pressed bodies was done. The heating rate was taken as a key parameter and two competing sinterization processes were identified, associated with different diffusional mechanisms. Using heating rates of 113 C min -1, a high-final density (98 % of the theoretical) was obtained by superposing the two aforementioned mechanisms, resulting in a homogeneous microstructure at lower temperatures. © 2012 Akadémiai Kiadó, Budapest, Hungary.

Effect of the composition on the thermal behaviour of the SrSn1-xTixO3 precursor prepared by the polymeric precursor method

Strontium stannate titanate Sr(Sn, Ti)O3 is a solid solution between strontium stannate (SrSnO3) and strontium titanate (SrTiO3). In the present study, it was synthesized at low temperature by the polymeric precursor method, derived from the Pechini process. The powders were calcined in oxygen atmosphere in order to eliminate organic matter and to decrease the amount of SrCO3 formed during the synthesis. The powders were annealed at different temperatures to crystallize the samples into perovskites-type structures. All the compositions were studied by thermogravimetry (TG) and differential thermal analysis (DTA), infrared spectroscopy (IR) and X-ray diffraction (XRD). The lattice former, Ti4+ and Sn4+, had a meaningful influence in the mass loss, without changing the profile of the TG curves. On the other hand, DTA curves were strongly modified with the Ti4+:Sn4+ proportion in the system indicating that intermediate compounds may be formed during the synthesis being eliminated at different temperature ranges, while SrCO3 elimination occurs at higher temperature as shown by XRD and IR spectra. © 2013 Akadémiai Kiadó, Budapest, Hungary.

Osteogenesis-inducing calcium phosphate nanoparticle precursors applied to titanium surfaces

This study investigated the effects of the morphology and physicochemical properties of calcium phosphate (CaP) nanoparticles on osteogenesis. Two types of CaP nanoparticles were compared, namely amorphous calcium phosphate (ACP) nano-spheres (diameter: 9-13 nm) and poorly crystalline apatite (PCA) nano-needles (30-50 nm x 2-4 nm) that closely resemble bone apatite. CaP particles were spin-coated onto titanium discs and implants; they were evaluated in cultured mouse calvarial osteoblasts, as well as after implantation in rabbit femurs. A significant dependence of CaP coatings was observed in osteoblast-related gene expression (Runx2, Col1a1 and Spp1). Specifically, the PCA group presented an up-regulation of the osteospecific genes, while the ACP group suppressed the Runx2 and Col1a1 expression when compared to blank titanium substrates. Both the ACP and PCA groups presented a more than three-fold increase of calcium deposition, as suggested by Alizarin red staining. The removal torque results implied a slight tendency in favour of the PCA group. Different forms of CaP nanostructures presented different biologic differences; the obtained information can be used to optimize surface coatings on biomaterials. © 2013 IOP Publishing Ltd.

Degradation of dipyrone via advanced oxidation processes using a cerium nanostructured electrocatalyst material

This work studied the degradation of dipyrone, via electrochemical processes and via electro-Fenton reaction using a 4% CeO2/C gas diffusion electrode (GDE) prepared via modified polymeric precursor method. This material was used to electrochemically generate H2O2 through oxygen reduction. The mean crystallite sizes estimated by the Scherrer equation for 4% CeO2/C were 4 nm for CeO2-x (0 4 4) and 5 nm for CeO2 (1 1 1) while using transmission electron microscopy (TEM) the mean nanoparticle size was 5.4 nm. X-ray photoelectron spectroscopy (XPS) measurements revealed nearly equal concentrations of Ce(III) and Ce(IV) species on carbon, which contained high oxygenated acid species like CO and OCO. Electrochemical degradation using Vulcan XC 72R carbon showed that the dipyrone was not removed during the two hour electrolysis in all applied potentials by electro-degradation. Besides, when the Fenton process was employed the degradation was much similar when using cerium catalysts but the mineralization reaches just to 50% at -1.1 V. However, using the CeO2/C GDE, in 20 min all of the dipyrone was degraded with 26% mineralization at -1.3 V and when the Fenton process was employed, all of the dipyrone was removed after 5 min with 57% mineralization at -1.1 V. Relative to Vulcan XC72R, ceria acts as an oxygen buffer leading to an increase in the local oxygen concentration, facilitating H2O2 formation and consequently improving the dipyrone degradation © 2013 Elsevier B.V. All rights reserved.

Luminescent properties of hybrid materials prepared by the polymeric precursor method

Rare earth complexes (RE) can be incorporated in silica matrixes, originating organic/inorganic hybrid materials with good thermal stability and high rare earth emission lines. In this work, the hybrid material was obtained by the polymeric precursor method and ultrasonic dispersed with spherical silica particles prepared by the Stöber Method. The Raman spectra indicated that the Eu3+ ions are involved in a polymeric structure formed as consequence of the chelation and polyesterification reactions of this ion with citric acid and ethylene glycol. After the ultrasonic stirring, 2-hydroxynicotinic ligand will also compose this polymeric rigid structure. The TGA/DTA analysis showed that this polymeric material was thermal decomposed at 300 °C. Moreover, this process allows the chelating process of the 2-hydroxynicotinic acid ligand to the Eu3+ ions. The 29Si NMR showed that the ultrasonic dispersion of the reactants was not able to promote the functionalization of the silica particles with the 2-hydroxynicotinic acid ligand. Moreover, heat treatment promotes the [Eu(HnicO2)3] complex particles incorporation into silica pores. At this temperature, the TGA curve showed that only the thermal degradation of ethylene glycol and citric acid used during the experimental procedure occurs. The silica and hybrid materials are composed by spherical and aggregated particles with particle size of approximately 450 nm, which can be influenced by the heat treatment. These materials also present an absorption band located at 337 nm. The photoluminescent study showed that when the hybrid samples were excited at 337 nm wavelength, the ligand absorbs the excitation light. Part of this energy is transferred to the Eu3+ ion, which main emission, 5D0→ 7F2, is observed in the emission spectrum at 612 nm. As the heating temperature increases to 300 C, the energy transfer is more favorable. The lifetime values showed that the Eu3+ emission is enhanced due to the energy transfer process in the powders. © 2013 Elsevier B.V. All rights reserved.

Nanoparticle characterization of Er-doped SnO2 pellets obtained with different pH of colloidal suspension

SnO2:2 at. %Er xerogel samples were obtained by sol-gel technique from colloidal suspensions with distinct pHs. The evaluation of critical regions inside the nanocrystallite is fundamental for the interpretation of the influence of pH on the emission data. In this way, the nanocrystal depletion layer thickness was obtained with the help of photoluminescence, Raman, X-ray diffraction, and field-emission gun scanning electron microscopy measurements. It was observed that acid suspensions (pH < 7) lead to high surface disorder in which a larger number of cross-linked bonds Sn-O-Sn among nanoparticles are present. For these samples, the nanoparticle depletion layer is larger as compared to samples obtained from other pH. Photoluminescence measurement in the near infrared region indicates that the emission intensity of the transition 4I13/2 → 4I15/2 is also influenced by the pH of the starting colloidal suspension, generating peaks more or less broadened, depending on location of Er3+ ions in the SnO2 lattice (high or low symmetry sites). © 2013 AIP Publishing LLC.

Influence of the preparation method and the support on H2O 2electrogeneration using cerium oxide nanoparticles

This work describes the influence of the preparation method and the carbon support using a low contentof cerium oxide nanoparticles (CeO2/C 4%) on H2O2electrogeneration via the oxygen reduction reac-tion (ORR). For this purpose, the polymeric precursor (PPM) and sol-gel (SGM) methods with Vulcan XC72R (V) and Printex L6 (P) supports were employed. The materials were characterized by X-ray diffrac-tion (XRD), X-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM). TheXRD analysis identified two phases comprising CeO2and CeO 2-x. The smallest mean crystallite size wasexhibited for the 4% CeO2/C PPM P material, which was estimated using the Debye-Scherrer equation tobe 6 nm and 4 nm for the CeO2and the CeO 2-xphases, respectively, and was determined by TEM to be5.9 nm. XPS analysis was utilized to compare the oxygen content of the 4% CeO2/C PPM P to Printex L6.The electrochemical analysis was accomplished using a rotating ring-disk electrode. The results showedthat the 4% CeO2/C specimen, prepared by PPM and supported on Printex L6, was the best electrocatalystfor H2O2production in 1 mol L -1NaOH. This material showed the highest ring current, producing 88%H2O2and transferring 2.2 electrons per O 2molecule via the ORR at the lowest onset potential. Addition-ally, the ring-current of the 4% CeO2/C PPM P material was higher than that of Vulcan XC 72R and PrintexL6, the reference materials for H2O 2production, indicating the highest electrocatalytic activity for the 4%CeO2/C PPM P material. © 2013 Elsevier Ltd. All rights reserved.

A polymeric europium complex with the ligand thiophene-2-carboxylic acid: Synthesis, structural and spectroscopic characterization

A polymeric complex [Eu(α-tpc)3(α-Htpc) 2]n and its characterization by single crystal X-ray and thermal analysis, infrared and photoluminescence spectroscopies are described. The compound crystallizes in the monoclinic Cc space group. The asymmetric unit is formed from a europium ion bonded to one carboxyl oxygen of five different thiophene carboxylic moieties. Three of these moieties are deprotonated and bridge between neighboring europium ions giving rise to an infinite polymer along the c axis. Besides the europium characteristic emission lines, the emission spectra show unambiguously the crystal size effect on the 5D0 → 7F0 transition. The complex thermal decomposition at 220 C leads to a stable luminescent complex in which the 5D0 → 7F4 transition reveals a monomeric characteristic. The Judd-Ofelt intensity parameters to the polymeric and the monomeric compound with the same ligand and coordination number were compared. © 2013 Published by Elsevier Ltd.

Chemical modification of the surface of alumina with alkaline earth metal oxides using the polymeric precursor method for catalysis application

In this study, modifications of alumina surface with of alkaline earth metal oxides were studied, using the polymeric precursor method. The modified compounds were characterized by X-ray diffraction, nitrogen adsorption-desorption and scanning electron microscopy. The catalytical properties of these new catalysts were evaluated for the transesterification reaction of babassu oil. It is observed that the transesterification reaction of babassu oil with methanol was successfully carried out using the modified alumina samples.