Estudo da estrutura e ordem local de particulas nanocristalinas usando tecnicas de difração, absorção e espalhamentode raios - X

AUTOR(ES)
DATA DE PUBLICAÇÃO

1996

RESUMO

MateriaIs with a nanometer-scale microstructure can have unusual physical and chemical properties. The development of methods to prepare and process these materials obtaining stable nanoscale structures suitable for scientific studies of low dimensional systems or technological applications, is today a major challenge. For this reason, it is very important to find the appropriate techniques to study the evolution of the microstructure during the crystallization and grain growth, as well as the structure and final composition of the crystallites and the grain boundary interface. In this work, three techniques of structural analysis, X-Ray diffraction (XRD), X-Ray absorption spectroscopy (EXAFS) and small angle X-Ray scattering (SAXS), have been used to study amorphous and nanocrystalline samples obtained with different growth parameters. The material studied was the metallic alloy Fe73,5CU1Nb3Si13,5B9 ( at. % ), grown as amorphous ribbons by rapid quenching from the melt. With the combined use of the aforementioned methods, the crystallization process was studied from the initial amorphous state up to its final nanocrystalline stage. X-Ray diffraction analysis was fundamental for the characterization of the crystalline structure obtained after thermal treatment. Small angle scattering experiments complemented these results through the investigation of amorphous samples produced with different quenching rates. The local order around the Fe atoms was studied using EXAFS and confirmed the information obtained by the previous methods. It must be mentioned that the use of transmission experiments is somewhat hindered in metallic alloys by high absorption and, in the case of SAXS, by the fact that these are dense systems of non-identical scatterers. In the case of the F e alloy studied, this technique led to important results, since it proved that the dimensions of the nanocrystalline particles and the high crystalline volumetric fraction in the annealed samples are directly related to a distribution of atomic aggregates already present in the initial amorphous state, which can be varied by controlling the quenching rate. The combination of analytical methods used in this work proved to be efficient in the study of structural, dimensional and compositional parameters of this nanocrystalline alloy, rendering complementary results which optimized its characterization. This is a very adequate methodology that can be successfully used to study the microstructure of low dimensional systems

ASSUNTO(S)

estrutura fina de absorção de raio x estendido (exafs) ligas de ferro vidros metalicos raios x - difração raios x - espalhamento a baixo angulo nanoparticulas

ACESSO AO ARTIGO

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