Papers by Author: Daniel Chateigner

Abstract: We illustrate the x-ray Combined Analysis approach capabilities in characterizing silicates and phyllosilicates for samples exhibiting crystallographic textures. Two mullite composite ceramics, one elaborated under uniaxial pressure the other under centrifugation, and one uniaxially pressed montmorillonite aggregate, are studied in terms of texture, cell parameters and phase contents. Several weak texture components are present in the mullite samples, combinations of planar- and fibre-like textures. The methodology is able to take account of the amorphous silica-like matrix of the composite, and cell parameters and structure of mullite correspond to the commonly modelled used for this phase. The montmorillonite turbostratic phase is correctly reproduced with its fibre texture, eventhough minor phases are also present and modelled in the aggregate.

Abstract: We give the necessary formulas to extract pure magnetic diffraction signals from the difference spectra between two neutron texture measurements, one operated with a sample at zero-magnetic field, and the other under a magnetic field. This enables us to calculate the total-magnetic-scattering ODF, and the polarisation-magnetic-scattering ODF, of an iron sample. Using the developed approach it is shown that under some hypotheses one can describe the three dimensional orientation of the magnetic moments in the sample under a given magnetic field.

Abstract: The orientation distributions of α-Al2O3 textured ceramics are determined from neutron diffraction and SEM-EBSD. A curved position-sensitive detector coupled to a tilt angle (χ) scan allowed the whole neutron diffraction pattern treatment in the combined Rietveld-WIMV-Popa algorithm. Analyses from neutron and electron diffraction data gave similar results if EBSD data are smoothed to account for grain statistics. Four textured alumina ceramics were prepared by slipcasting under a high magnetic field and sintered at 800°C, 1300°C, 1400°C and 1600°C. The inverse pole figures and EBSD-mapping highlights the influence of the magnetic field and sintering temperature on the texture development. The inverse pole figures calculated for the fiber direction show a major (001) component for all the samples. With the increasing sintering temperature, the texture strength is enhanced and the c-axis distribution is sharper. The effectiveness of the combined approach for determining the crystallite size is also evident. As a global trend, the calculated crystallite size and observed grain size are similar and increase with the increasing sintering temperature. The mechanism of the texture development in the sintered specimens is certainly initiated from the preferred orientation of the green body after slip-casting under a high magnetic field. The basal texture is enhanced during sintering by selective anisotropic grain growth. We evidenced here the powerfulness of the Rietveld texture analysis correlated to SEM-EBSD calculation to provide a basis for the correlation of texture, microstructural parameters and anisotropic properties.

Abstract: In this study, a hot forging process is applied to Nd-Fe-V as cast alloys in order to develop both the microstructure and the crystallographic texture appropriate for permanent magnet properties. A neutron diffraction texture analysis is used to account for the extrinsic magnetic anisotropy: the stabilisation of the Nd(Fe,V)12 hard magnetic phase has been achieved during forging but its extrinsic anisotropy level remains low. Attempts to understand this phenomenon are made through a discussion on the Nd-Fe-V alloy rheological and mechanical behaviour and a comparison with Nd-Fe-B permanent magnets.

Abstract: The crystal structure of R-phase in Ti50.75.Ni47.75.Fe1.50 shape memory alloy (SMA) has been studied at a temperature of (290 ± 7) K on cooling by combined synchrotron and neutron powder diffraction using Rietveld refinement with generalized spherical harmonic (GSH) description for preferred orientation (PO). The results showed that (i) no significant improvement in the crystallographic RWP-factor was found when the inversion center was removed from the 3 P model, suggesting that the space group was indeed 3 P and not lower symmetry 3 P neither m P31 and (ii) the refined atomic parameters were converging only when the 3 P space group was used in the refinement.

Abstract: Orientation distributions of polyphased (Bi,Pb)2Sr2Ca2Cu3O10+d superconducting textured materials are determined from neutron diffraction analysis. The quantitative texture analysis of neutron data was accomplished by using the combined Rietveld-WIMV-Popa algorithms, implemented in the program package Materials Analysis Using Diffraction (MAUD). Curved position-sensitive detector and 4-circle diffractometry allow the whole diffraction pattern treatment. Transport critical current densities, measured on different samples, are strongly dependent of the calculated texture strengths, crystallite sizes and phase ratios. The results prove the interest of the combined approach for a quantitative texture analysis of complex materials. Texture to anisotropic physical properties relationship is discussed.

Abstract: A high speed hot forging process was applied to Nd-Fe-B and Nd-Fe-V as cast alloys in order to develop both the microstructure and the crystallographic texture appropriate for permanent anisotropic magnet properties. Neutron diffraction texture analyses are used to demonstrate the effect of the hot forging process on both kind of alloys. Microstructural changes are an important feature on forging in both cases. Coercivity is developed in the Nd-Fe-B alloy mainly from grain size reduction and disappearance of free iron. Stabilisation of the Nd(Fe,V)12 hard magnetic phase is achieved from the iron and Nd-rich microstructure of the starting Nd-Fe-V material. A comparison of the crystallographic textures of Nd2Fe14B and Nd(Fe,V)12 phases is done to account for the development of extrinsic magnetic anisotropy. In both cases, a nearly fibre texture is obtained in correlation with the symmetry of the deformation. However, the orientations are quite different in both alloys and the consequences on the magnetic properties are evidenced.

Abstract: The preferred crystallographic orientation (i.e. texture) and the non-transformed austenite can cause serious systematic errors in the structural study of the R-phase in 50.75at.%Ti- 47.75at.%Ni-1.50at.%Fe (hereafter referred to as Ti-Ni-Fe ternary) shape memory alloy. The crystal structure refinement of R-phase synchrotron high resolution powder diffraction (SRD) data using Rietveld refinement with generalized spherical harmonic (GSH) description for preferred orientation correction showed that the sample consists of minor cubic phase and the space group was 3 P [1]. The objective of the present paper is to study the crystallographic phase composition and crystal structure refinement of SRD data of trigonal R-phase martensite and monoclinic (B19¢) martensite in Ti-Ni-Fe ternary alloy during thermal cycling using the GSH description.