Papers by Keyword: Rietveld

Abstract: Many synthesis methods are available to obtain a set of specific characteristics for lead zirconate titanate (PZT) piezoelectric ceramic powders. In this work, we have successfully prepared PZT powder samples through the Polymeric Precursor Method with x = 0.6, according the general formula Pb (Zr_xTi_1-x)O₃. The powders were thermally treated from 380 to 550 oC and characterized by Raman spectroscopy and X-ray diffraction (DRX) in order to evaluate the effects of thermal treatment on the phase formation and the crystallization processes. The results obtained by Raman spectroscopy were compared to refined crystal data obtained by Rietveld method, leading to coherent conclusions about the structural effects occurring along the temperature of calcination. It was possible to characterize the tetragonal perovskite phase as predominant phase occurs only after 500 oC, but its crystallinity is already determined by synthesis method. Thus, no ordering process is verified for perovskite as a function of the temperature increasing during thermal treatment, in spite of the continuous pyrochlore-to-perovskite phase transition. The pyrochlore secondary phase starts to vanish before its proper crystallization process, changing the tetragonality of previously formed perovskite phase.

Abstract: The anatase phase of titanium dioxide ceramic material plays important rule in heterogeneous photocatalysis, beside the global phase amount and powder morphology. Some of structural parameters are useful to predict several properties, including the crystallization process and mechanism of the irreversible anatase-to-rutile phase transition. The photocatalytic process is based on charge transference from electron-hole pair to material surface, starting some redox reactions in aqueous media. The stable positive defects harm the recombination event and improve the final properties of that material. Modifiers with lower oxidation state than titanium (IV) is applicable for this purpose, what idea becomes the objective of this work. The Sol-Gel method was used to prepare bare and zinc doped-titanium dioxide powder samples reaching good compositional homogeneity for both samples calcined at 500 oC for 4 hours. Rietveld refinement carried out from raw x-ray diffraction patterns was used to demonstrate the formation of solid solution between zinc and titanium oxides. Besides that result, the determination of bandgap energy and SEM images corroborated the structural changes caused by zinc insertion in anatase phase and important difference in powder morphology was observed for zinc doped powder samples in order to reduce the agglomeration degree for better performance for heterogeneous photocatalysis applications.

Abstract: Important changes in anatase crystal structure are responsible for the consequent anatase-to-rutile phase transition in titanium dioxide powders. In order to investigate several structural rearrangements occurring in anatase phase obtained by hydrolysis-based method such as Sol-Gel method the X-ray diffraction techniques followed by Rietveld method seems to better approach. Several alterations in anatase lattice parameters can occur by doping insertion and the investigation of isostructural zircon silicate can provide interesting ones. In the present paper, the monitoring of anatase structure reordering and the consequent anatase-to-rutile phase transition along the thermal treatment up to higher temperatures were monitored carrying out DSC and XRD characterizations. The insertion of 6 mol% of zircon silicate leads to the fully anatase stabilization up to 900 °C due the control of ordering process, even that a continuous increasing in anatase tetragonality is present during the entire process. We can conclude the reconstructive anatase-to-rutile phase transition is delayed to very higher temperatures can consequence of more stable cross-linked metal oxide bond in anatase phase.

Abstract: The reconstructive transformation occurring during the anatase-to-rutile phase transition can be observed through adequate techniques such as Thermal Analyses and Z-ray diffractometry followed by structural refinement. The typical photonic properties of titanium dioxide photocatalysts depend on the anatase structure and how the modifiers can provide their performance enhancement. In the present work, we investigate the structural effects caused by the simultaneous homovalent modification on the anatase structure in order to understand the mechanisms of the anatase-to-rutile phase transition in terms of the atomic coordinates and the lattice parameters. The refined structures along the calcination temperature from 500 to 900 oC suggest the oxygen bonds are strongly affected in unmodified anatase in order to destroy and rebuilt the crystal structure and lead to the rutile phase formation above 700 oC, unless some modifier pairs stabilize them.

Abstract: Pulp and paper mills have a process that generates waste with high levels of CaO and SiO₂, which can be valued as an alternative mineral source in the cement industry. In this work the lime mud, biomass ashes and WWTP sludge are used in the production of clinker. Analysis of X-ray diffraction (XRD) confirmed the crystalline phases calcite and quartz. Chemical analysis by X-ray fluorescence (XRF) identified Al₂O₃, CaO and SiO₂, providing support for the calculation of theoretical stages by applying the Bogue equations. Five formulations and three processing temperatures (1350, 1400, 1455 °C) were studied. The products obtained and an ordinary Portland cement (OPC) were characterized by XRD with quantification by the Rietveld method. The results showed that the processing conditions used produced belíticos (higher content of C₂S) and Portland (C₃S content greater) ecoclinker.

Abstract: Currently the composite two-phase Al₂O₃-YAG laser has been widely exploited by having good properties such as high abrasion resistance and deformation in harsh environments. Thus, one can predict that this material has very attractive applications such as fins of jet engines and gas turbines. In this study, five mixtures were processed Y₂O₃-Al₂O₃-Nb₂O₅, in proportions of 0, 1, 5, 15 and 35 wt% Y₂O₃ and 4% by weight of Nb2O5. These samples were sintered at 1550 to 1650 °C in air where it was detected by X-Ray Diffraction (XRD) with Rietveld refinement training YAG and also two intermediate stages, and AlNbO₄ YNbO₄. Finally they were characterized by hardness by Vickers microindentation and fracture toughness. The highest hardness and fracture toughness were 15 GPa and 5.5 MPa.m^1/2, respectively.

Abstract: The titanium dioxide phase formation is dependent on the synthesis method, temperature of calcination and modifiers insertion. By using chemical methods, such as Polymeric Precursor Method, the organic impurities or extrinsic defects caused by doping play an important rule on the formation of precursor structure before the phase crystallization above 500 oC. Some dopants can change the decomposition mechanism of the precursor, which affects the anatase-rutile phase transition. In this work, the Polymeric Precursor Method was used to synthesize titanium dioxide powder samples in order to investigate the effects of iron (III) and vanadium (V) dopants on the phase formation. Through thermal analysis of polymeric precursors and X-ray diffractometry for calcined powder samples it was possible to show the existence of antagonistic effects for both investigated dopants. While the iron doping reduces the anatase phase tetragonality and delays the rutile phase conversion, the vanadium one changes the mechanism of decomposition of polymeric precursor and leads to more amount of rutile phase.

Abstract: The production of high purity samarium doped ceria (SDC20, Sm_0.2Ce_0.8O_2-δ) nanopowders by modified sol-gel process using maltose and pectin as organic precursors. Around, 6 nm particle size can be obtained after calcination of the as synthesized (pre dried) gel at 500 °C for 2 h. Rietveld refinement of Powder X-ray diffraction (XRD) patterns confirms the cubic structure with single phase. Chemical composition of SDC20 is in good agreement with EDX measurements. TEM and XRD analysis indicate the influence of sintering temperature on particle size, which increases with increasing temperature. This modified sol-gel process is a non-toxic and environmentally friendly for large-scale production of high purity nanopowders.

Abstract: Al based intermetallic materials are commonly susceptible to hydrogen embrittlement reaction. Water vapor in the air reacts with the aluminum in the alloy and releasing hydrogen. Thus, the aid of this work is to know how much hydrogen can be released when the embrittlement reaction is induced inside the milling container. For this purpose the CuAl₂ intermetallic material was made by conventional castings methods and then subjected to high-energy ball milling in water. The samples were characterized by X-ray diffraction pattern, attenuated total reflectance spectroscopy and scanning electron microscopy (SEM). After the milling process, the amount of hydrogen released was correlated with the other reaction products obtained during the reaction. These products were primarily aluminum hydroxides. The amount of hydrogen that can be released is similar to the theoretical amount possible that can be released.

Abstract: Al₂O₃-Nb₂O₅ has been widely explored as one of the most used material for sintering mixing in the literature, due to its excellent hardness properties, used in armor. In this study, Al₂O₃-Nb₂O₅ and Y₂O₃-Nb₂O₅ powders were prepared, with 50% in mole fraction of each oxide. The mixtures were subjected to high energy milling in an eccentric ball mill for 3 h, dried and sieved in a sieve vibrator. The green bodies were compacted at 70 MPa and sintered from 1250 to 1650 °C for 3 h, at 100 °C steps. The materials were characterized by quantitative X-Ray diffraction (XRD) using Rietveld method and by mass loss. The Al₂O₃-Nb₂O₅ mixtures experienced a weight loss of 84% at sintering temperatures of 1550 and 1650 °C.