RESUMONeste trabalho a função TCHZ (Modificada por Thompson-Cox-Hastings) foi usada para a análise das larguras integrais dos perfis das linhas de difração dos raios X de caulinitas através do método de ajuste Le Bail. Este método não requer informações estruturais, exceto dos parâmetros de rede aproximados e dos parâmetros de resolução instrumental. Esta técnica de refinamento faz parte do programa FullProf onde é conhecido como "Profile Matching". O método foi aplicado para dois casos de alargamento devido aos tamanhos de cristalitos e microdeformações da rede da caulinita de depósitos brasileiros, que passaram por beneficiamentos químico e físico. As amostras apresentam teores de Fe 2 O 3 variando entre 1,55 (moderado) a 3,04% (alto). O refinamento através do método de Rietveld foi realizado com os dados de uma amostra de referência padrão do LaB 6 para obter simultaneamente os parâmetros instrumentais e como uma maneira independente de validar os resultados obtidos pelo método "Profile Matching". Foi observado que o tamanho do cristalito decresce e a deformação cresce com o aumento do conteúdo de Fe 2 O 3 (% em peso) na amostra. A forma Lorentziana dos alargamentos intrínsecos das linhas de difração é um forte indicador que são os pequenos tamanhos dos cristalitos a principal causa das imperfeições das amostras de caulinitas analisadas.Palavras chaves: Caulinita, difração de raios X, parâmetros da microestrutura. ABSTRACTIn this work, the modified Thompson-Cox-Hastings function (TCHZ) was used in the analisys of the integral breadths obtained from the broadned X ray diffraction line profiles. These set of X ray diffraction results were calculated from the "Le Bail" fitting method, which does not require any structural information, except unit cell and resolution instrumental parameters. The refinement used here is called 'Profile Matching' in the FullProf, a program for Rietveld analysis. The method was applied in two case size-strain broadening of kaolinites from Brazilian deposits that after the treatment chemical and physical still had a content ranging between 1,55 % w/w (intermediate) to amount of 3,04% w/w (high) of structural and total iron. The Rietveld refinement was first performed by using the set of data from standard reference material LaB 6 to obtain all the instrumental parameters, simultaneously. This result has been used as an independent method to validate the results obtained by the 'Profile Matching' method. It has been shown that the crystallite size decreasing and the strain increasing with Fe 2 O 3 (% w/w) contents. The Lorentzian shape of the inherent widths of the lines diffraction is a strong indication that are the small crystallite size the main cause of the analysed kaolinites samples.

The study of nickel-based alloy 625 clad (weld overlay) by X-ray diffraction (XRD) is difficult and often impossible because of its coarse and anisotropic microstructure. In this work, a sample preparation including machining, grinding, and annealing was proposed to avoid this negative effect in XRD analysis. Electron backscatter diffraction and hardness testing were used to evaluate the microstructure of the surface and the inner region of a sample during its preparation. The proposed sample preparation allowed accurate determination of the Young's modulus and the Poisson ratio through XRD. The values obtained using a small bending fixture are 212 ± 2 GPa and 0.31 ± 0.01, respectively.

In the present work, residual stresses in nickel-based (Ni 625) superalloy weld metal of a 9%Ni steel-welded joint were measured by X-ray diffraction (XRD). This technique presents some difficulties in performing measurements in coarse and preferentially oriented weld metal microstructures. It is proposed a preliminary surface treatment by rotating steel wire brushing to perform the stress analysis through XRD technique possible for this kind of material. Stress measurements with proposed XRD technique showed that the stress state in Ni 625 weld metal on the outside surface of the welded joint is characterised by tensile stresses in the transverse and longitudinal directions, while compressive transverse and tensile longitudinal residual stresses are developed in the root pass region.

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