Advanced Powder Technology V

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Authors: Maria Isabel Brasileiro, D.H.S. Oliveira, Hélio Lucena Lira, Lisiane Navarro de Lima Santana, Gelmires Araújo Neves, A.P. Novaes, J.Marcos Sasak
Authors: Normanda Lino de Freitas, Elias Fagury-Neto, Hélio Lucena Lira, Lucianna Gama, Ruth Herta Goldsmith Aliaga Kiminami, Ana Cristina Figueiredo de Melo Costa
Abstract: Among ceramic materials, the alumina has high importance because of its characteristics of resistance and refractory. The possibility to improve the final characteristics of this material, open possibilities for new applications. The aim of this work is to synthesize (α-Al2O3) alumina powders by combustion reaction and to evaluate the effect of the urea content in the final characteristics of the α-Al2O3 powders. Three compositions were studied : a) stoichiometric, b) with 10% of urea reduction and c) with 20% of urea reduction. The initial solution composition was based on the total valence of the reagents by using chemical concepts of the propellant. This powders were characterized by X-ray diffraction (XRD), granulometric determination by laser diffraction, nitrogen adsorption by BET, scanning electron microscopy (SEM), infrared spectroscopy (IR) and helium picnometer. The results showed that the urea reduction change the temperature of the reaction from 525 to 463oC , the characteristics of the powders, and principally the reduction of the particles size.
Authors: M.A.F. Ramalho, Ana Cristina Figueiredo de Melo Costa, Lucianna Gama, Ruth Herta Goldsmith Aliaga Kiminami, E.P. Hernandez, Daniel R. Cornejo, S.M. Rezende
Abstract: Ultrafine magnetic nickel ferrite particles have a significant potential for use in many applications such as magnetic recording media, ferrofluids, microwaves, catalysis and radar-absorbing coatings [1, 2]. Nickel ferrite powders with a nominal NiFe2O4 composition were synthesized by combustion reaction and an evaluation was made of the effect of two different conditions of synthesis on the nanostructural and magnetic characteristics of the resulting powders. Two synthesization routes were studied. The first, NFB, involved the preparation of the powder using a Pyrex beaker heated directly on a hot plate at 480°C until self-ignition occurred. By the second route, NFC, the powder was obtained under the same synthesization condition as the NFB route, but a vitreous silica basin was used. The resulting powders were characterized by X-ray diffraction (XRD), nitrogen adsorption by BET and scanning electron microscopy (SEM). The first route, NFB, proved more favorable to obtain powders with high surface area and, hence, smaller crystalline sizes (5.70 nm) and a superparamagnetic behavior. The NFC route confirmed the feasibility of obtaining powders with a crystalline size of 18.00 nm and a magnetic behavior. Saturation magnetization was 33.18 emu/g and the coercivity field was 25.63 Oe for powders obtained by the NFC route.
Authors: Rubens Chiba, Reinaldo Azevedo Vargas, Marco Andreoli, Emília Satoshi Miyamaru Seo
Abstract: Nowadays, the La1-XSrXMnO3 (LSM) is one of the most common cathodic materials used in the solid oxide fuel cells (SOFCs). The dopant strontium increases the electronic conductivity of the material, besides presents an excellent electrochemical performance, relatively good chemical and thermal stability and compatibility with solid electrolyte of ZrO2/Y2O3 (YSZ). In this work, a contribution to the study of synthesis of LSM is presented with strontium concentration of 50 mol % by the citrate technique. The powders have been characterized for various techniques, as gas absorption and adsorption, X-ray fluorescence spectroscopy, laser scattering granulometry, gas helium picnometry, scanning electron microscopy (SEM), X-ray diffractometry (XRD) and calculations of theoretical density and particle average diameter. The ceramics have been characterized by SEM and XRD. The adequate characteristics of LSM have been evaluated aiming at the use in the preparation of suspensions for cathodic thin films of SOFCs.
Authors: G.C.C. da Costa, R. Muccillo
Abstract: Lanthanum beta alumina powders were obtained by the polymeric precursor technique using lanthanum nitrate, aluminum nitrate, ethylene glycol and citric acid. The transformations that occur during thermal treatment of the precursor solution were evaluated by thermogravimetric and differential thermal analysis. Fourier Transform Infrared analysis for residual carbon qualitative detection and gas adsorption analysis for evaluating specific surface area, BET method, were carried out in powder specimens heat treated at different temperatures. High calcination temperature leads to the formation of hard agglomerates. The powders calcined at 800°C for 4 h have high specific surface area, ~ 120 m2/g. All processed powders and green pellets sintered at different temperatures were analyzed by X-ray diffraction for structural phase determination. Single phase LaAl11O18 pellets have application as solid electrolytes in disposable electrochemical devices for monitoring dissolved oxygen species in molten steel at very high temperatures, > 1500 °C, during steel production.
Authors: Adriana Scoton Antonio Chinelatto, C. Lago, S.R.M. Antunes, A.C. Antunes, Osvaldo Mitsuyuki Cintho, Adilson Luiz Chinelatto
Abstract: Alumina is utilized in many areas of modern industry because of its unique mechanical, electrical and optical properties. Various methods are been employed for produce alumina for different end uses. The preparation of fine and sintering-reactive alumina powders is probably one of the most important steps for production alumina ceramics with controlled microstructure. In this work, it was studied the production of alumina powders by “Pechini” method associated to highenergy milling. For this, it was prepared the resin by Pechini method, using aluminum nitrate nonahydrate. This resin was calcined at 500oC. Then, the calcined powders were submitted a high energy milling for different times. The powders mechanically activated were characterized by x ray diffraction, FT-IR and scanning electronic microscopic. After milling, the powders were calcined at 900oC. The results showed that the alumina phase transitions and powders characteristics were modified when the step of activation mechanical was introduced.
Authors: S.T. Fonseca, Maria do Carmo de Andrade Nono, Carlos Alberto Alves Cairo
Abstract: In this work, was proposed to produce nanosized α-Al2O3 powder from precipitation reactions, in order to reduce the alumina ceramics sintering temperature. For this an addition of nanosized powder in the commercial microsized powders was done. The nano and microsized powder particle mixtures were obtained by precipitation of nanosized aluminum hydroxide in microsized Al2O3 in liquid suspension. Several compositions of nano and microsized powders were carried out. These powder compositions were based on data of simulated particle packing. The nano and microsized powder mixtures was characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD) and thermogravimetric and differential thermal analysis (TGA and DTG). The powder mixtures were compacted by uniaxial (75MPa) and isostatic (300MPa) pressing, producing cylindrical samples. The powder compacted samples were sintered at 1400oC. Sintered ceramics were characterized by XRD and SEM. The results showed that the higher density of sintered ceramic was obtained for 65% of microsized powder and 35% of nanosized powder mixture. This composition of size of particles of the powder was in agreement with the theoretical simulation.
Authors: Yu. Koldayeva, Maria do Carmo de Andrade Nono, Pedro José Castro
Abstract: In this work the BaSO4 powder was synthesized from BaCO3 powder that was attacked with HCl. Then BaCl2 was precipitated in (NH4)2 SO4, containing TiO2 powder. The influences of processing and TiO2 particles presence were investigated by X-rays diffraction and SEM. It was found that the washing of BaSO4 - TiO2 precipitated by ethanol greatly benefited the formation of smaller size particles.
Authors: L.F.G. Setz, H.P.S. Corrêa, Carlos de Oliveira Paiva-Santos, Sonia Regina Homem de Mello-Castanho
Abstract: Lanthanum chromite (LaCrO3) is one of the most adequate materials for use as interconnector in solid oxide fuel cell (SOFC) applications, due to its intrinsic properties, namely its good electrical conductivity and resistance to environment conditions in fuel cell operations. Due to difficulties in sintering, additives are usually added to help in the densification process. In this work, the influence of added cobalt and strontium, in the sintering of LaCrO3 obtained by combustion synthesis was studied. The starting materials were respectively nitrates of chromium, lanthanum, cobalt and strontium, and urea was used as fuel. The results show that by increasing the strontium and cobalt concentrations it is possible to reduce the temperature of sintering. Using both additives, the sintering processes took place in lesser times than normally used for this material, as well as greater values of density were attained.
Authors: R.H.L. Garcia, Valter Ussui, Nelson Batista de Lima, Dolores Ribeiro Ricci Lazar
Abstract: The addition of alumina in a zirconia stabilized in a tetragonal phase matrix enhances ceramic hardness and inhibits the tetragonal → monoclinic phase transformation of zirconia when exposed to an aqueous environment. These characteristics are important for applications such as bioceramics and structural materials. For these purposes, the strict control of powder synthesis and the processing conditions are vital to tailor the ceramic characteristics. This work evaluates the influence of 20 wt% alumina in a Y-TZP matrix on powder characteristics, obtained by coprecipitation route, and calcined from 600 to 1200°C for 1 and 3 hours. The powders obtained were characterized by X-ray diffraction, scanning electronic microscopy, laser diffraction and gaseous adsorption (BET). The results reveal that presence of Al3+ inhibits the crystallization of composite at lower temperatures.

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