scholarly journals Neutron Diffraction Texture Analysis of Multi-Phase Systems

1989 ◽  
Vol 10 (4) ◽  
pp. 325-346 ◽  
Author(s):  
H.-G. Brokmeier

Neutron diffraction methods for texture analysis are closely parallel to well-known X-ray diffraction techniques. The chief advantage of neutron diffraction over X-ray diffraction, however, arises from the fact that the interaction of neutrons with matter is relatively weak, and consequently the penetration depth of neutrons is 102–103 times larger than that of X-rays. Hence neutron diffraction is an efficient tool for measuring textures in multi-phase systems. Based on the high transmission of a neutron beam the effect of anisotropic absorption in multi-phase materials can be neglected in most cases. Moreover, the analysis of bulk textures becomes possible, such that textures in a wide variety of multi-phase systems can be studied which are of special interest in engineering and science (metals, alloys, composites, ceramics and geological specimens).

1999 ◽  
Vol 33 (1-4) ◽  
pp. 13-33 ◽  
Author(s):  
H.-G. Brokmeier

Due to the high penetration depth of thermal neutrons for most materials, neutron diffraction is an efficient tool for bulk texture analysis. The main applications are investigations of coarse-grained materials, non-destructive pole figure measurements of identical samples at different states, detection of weak textures, measurement of unprepared samples and texture investigations of multi-phase systems. It should be pointed out that neutron texture analysis is suitable for basic research as well as for applications.


1997 ◽  
Vol 53 (1) ◽  
pp. 135-142 ◽  
Author(s):  
D. L. Corker ◽  
A. M. Glazer ◽  
J. Dec ◽  
K. Roleder ◽  
R. W. Whatmore

The crystal structure of the perovskite lead zirconate PbZrO3 has been redetermined using single-crystal X-ray diffraction (Mo Kα radiation, λ = 0.71069 Å). Single-crystal data at 100 K: space group. Pbam, a = 5.884 (1), b = 11.787 (3), c = 8.231 (2) Å, V = 570.85 Å3 with Z = 8, μ = 612.6 cm−1, D x = 8.06 Mg m−3, F(000) = 1168, final R = 0.033, wR = 0.061 over 555 reflections with I > 2σ(I). An investigation is made into previous contradicting reports of a possible disorder in the O atoms and their origin by examining the crystal pseudo-symmetry. Information distinguishing an ordered and disordered oxygen substructure is shown to reside in weak l odd reflections. Because of their extremely low intensities these reflections have not contributed sufficiently in previous X-ray structure investigations and hence, to date, conclusive evidence differentiating between ordered and disordered models has not been possible. By collecting single-crystal X-ray data at low temperature and by using exceptionally long scans on selected hkl, l odd, reflections, a new accurate structure determination is presented and discussed, showing the true ordered oxygen positions. Because of the large difference in scattering factors between lead and oxygen when using X-rays, a neutron diffraction Rietveld refinement using polycrystalline samples (D1A instrument, ILL, λ = 1.90788 Å) is also reported as further evidence to support the true ordered oxygen structure revealed by the low-temperature X-ray analysis.


2008 ◽  
Vol 41 (2) ◽  
pp. 377-385 ◽  
Author(s):  
Thomas Erbacher ◽  
Alexander Wanner ◽  
Tilmann Beck ◽  
Otmar Vöhringer

The experimental analysis of near-surface residual stresses by X-ray diffraction methods is based on measuring the spacings of lattice planes while the inclination ψ with respect to the surface plane is changed stepwise. A characteristic feature of conventional techniques is that the penetration depth of the X-rays is altered as inclination is varied. By simultaneously varying three different goniometer angles in a particular fashion, both the penetration depth and the measuring direction can be held constant while ψ is varied. Thus the normal and shear stresses can be derived from the sin2ψ plots by means of standard evaluation procedures developed for gradient-free stress states. The depth profile of residual stress is then obtainedviaLaplace transformation of the results from several stress measurements carried out at different penetration depths. In the present paper, the feasibility of this experimental approach for characterizing the strongly graded, non-equiaxed stress state existing at a machined surface is demonstrated. The results from constant-penetration-depth measurements on the ground surface of an engineering ceramic are compared with those from conventional sin2ψ measurements.


2014 ◽  
Vol 70 (a1) ◽  
pp. C1110-C1110
Author(s):  
Martin Meven ◽  
G. Gatta

Up to now minerals of the silicate family are an interesting and versatile topic of research. Different members of the epidote, lithium tourmaline and beryl groups with very different structural features were studied on the single crystal diffractometer HEIDI at the hot source of the Heinz Maier-Leibnitz Zentrum in Garching (MLZ) in the recent past. The combination of neutron and X-ray diffraction in combination with other methods revealed for each of the studied minerals valuable information about their structural details. Epidote, an important mineral for metamorphic or magmatic petrology was studied with neutrons at room temperature and at 1070 K. The results confirm the high structural stability with no dehydration and only slight thermal expansion [1]. A combined study with x-ray and neutron diffraction on the complex boro-cyclo-silicate elbaite give insight to the displacement regime and H and O order and disorder respectively [2]. Combined single crystal diffraction with x-rays at room temperature and with neutrons at 2.3 K on pezzottaite, an obverse/reverse twin of the beryl family reveals a complex displacement regime with possible partial H2O replacement [3].


Author(s):  
Kunal Kumar Jha ◽  
Barbara Gruza ◽  
Prashant Kumar ◽  
Michal Leszek Chodkiewicz ◽  
Paulina Maria Dominiak

Hydrogen is present in almost all of the molecules in living things. It is very reactive and forms bonds with most of the elements, terminating their valences and enhancing their chemistry. X-ray diffraction is the most common method for structure determination. It depends on scattering of X-rays from electron density, which means the single electron of hydrogen is difficult to detect. Generally, neutron diffraction data are used to determine the accurate position of hydrogen atoms. However, the requirement for good quality single crystals, costly maintenance and the limited number of neutron diffraction facilities means that these kind of results are rarely available. Here it is shown that the use of Transferable Aspherical Atom Model (TAAM) instead of Independent Atom Model (IAM) in routine structure refinement with X-ray data is another possible solution which largely improves the precision and accuracy of X—H bond lengths and makes them comparable to averaged neutron bond lengths. TAAM, built from a pseudoatom databank, was used to determine the X—H bond lengths on 75 data sets for organic molecule crystals. TAAM parametrizations available in the modified University of Buffalo Databank (UBDB) of pseudoatoms applied through the DiSCaMB software library were used. The averaged bond lengths determined by TAAM refinements with X-ray diffraction data of atomic resolution (d min ≤ 0.83 Å) showed very good agreement with neutron data, mostly within one single sample standard deviation, much like Hirshfeld atom refinement (HAR). Atomic displacements for both hydrogen and non-hydrogen atoms obtained from the refinements systematically differed from IAM results. Overall TAAM gave better fits to experimental data of standard resolution compared to IAM. The research was accompanied with development of software aimed at providing user-friendly tools to use aspherical atom models in refinement of organic molecules at speeds comparable to routine refinements based on spherical atom model.


2011 ◽  
Vol 681 ◽  
pp. 19-24
Author(s):  
Bob B. He

Two-dimensional x-ray diffraction is an ideal method for examining the residual stress and texture. The most dramatic development in two-dimensional x-ray diffractometry involves three critical devices, including x-ray sources, x-ray optics and detectors. The recent development in brilliant x-rays sources and high efficiency x-ray optics provided high intensity x-ray beam with the desired size and divergence. Correspondingly, the detector used in such a high performance system requires the capability to collect large two-dimensional images with high counting rate and high resolution. This paper introduces the diffraction vector approach in two-dimensional x-ray diffraction for stress and texture analysis, and an innovative large area detector based on the MikroGap™ technology.


Texture ◽  
1972 ◽  
Vol 1 (2) ◽  
pp. 125-127 ◽  
Author(s):  
J. Tobisch ◽  
H. J. Bunge

Neutron diffraction proves advantageous as compared to X-ray diffraction in texture analysis because of the lower absorption coefficient for a broad variety of materials especially metals. The spherical sample method is recommended because it yields the most reliable results and it does not require great preparational efforts. The fundamental difference between the spherical sample method in X-ray and in neutron diffraction is discussed.


Author(s):  
W. Z. Chang ◽  
D. B. Wittry

Since Du Mond and Kirkpatrick first discussed the principle of a bent crystal spectrograph in 1930, curved single crystals have been widely utilized as spectrometric monochromators as well as diffractors for focusing x rays diverging from a point. Curved crystal diffraction theory predicts that the diffraction parameters - the rocking curve width w, and the peak reflection coefficient r of curved crystals will certainly deviate from those of their flat form. Due to a lack of curved crystal parameter data in current literature and the need for optimizing the choice of diffraction geometry and crystal materials for various applications, we have continued the investigation of our technique presented at the last conference. In the present abstract, we describe a more rigorous and quantitative procedure for measuring the parameters of curved crystals.The diffraction image of a singly bent crystal under study can be obtained by using the Johann geometry with an x-ray point source.


Author(s):  
M. D. Vaudin ◽  
J. P. Cline

The study of preferred crystallographic orientation (texture) in ceramics is assuming greater importance as their anisotropic crystal properties are being used to advantage in an increasing number of applications. The quantification of texture by a reliable and rapid method is required. Analysis of backscattered electron Kikuchi patterns (BEKPs) can be used to provide the crystallographic orientation of as many grains as time and resources allow. The technique is relatively slow, particularly for noncubic materials, but the data are more accurate than any comparable technique when a sufficient number of grains are analyzed. Thus, BEKP is well-suited as a verification method for data obtained in faster ways, such as x-ray or neutron diffraction. We have compared texture data obtained using BEKP, x-ray diffraction and neutron diffraction. Alumina specimens displaying differing levels of axisymmetric (0001) texture normal to the specimen surface were investigated.BEKP patterns were obtained from about a hundred grains selected at random in each specimen.


Author(s):  
Mateus Dobecki ◽  
Alexander Poeche ◽  
Walter Reimers

AbstractDespite the ongoing success of understanding the deformation states in sheets manufactured by single-point incremental forming (SPIF), the unawareness of the spatially resolved influence of the forming mechanisms on the residual stress states of incrementally formed sheet metal parts impedes their application-optimized use. In this study, a well-founded experimental proof of the occurring forming mechanisms shear, bending and stretching is presented using spatially resolved, high-energy synchrotron x-ray diffraction-based texture analysis in transmission mode. The measuring method allows even near-surface areas to be examined without any impairment of microstructural influences due to tribological reactions. The depth-resolved texture evolution for different sets of forming parameters offers insights into the forming mechanisms acting in SPIF. Therefore, the forming mechanisms are triggered explicitly by adjusting the vertical step-down increment Δz for groove, plate and truncated cone geometries. The texture analysis reveals that the process parameters and the specimen geometries used lead to characteristic changes in the crystallites’ orientation distribution in the formed parts due to plastic deformation. These forming-induced reorientations of the crystallites could be assigned to the forming mechanisms by means of defined reference states. It was found that for groove, plate and truncated cone geometries, a decreasing magnitude of step-down increments leads to a more pronounced shear deformation, which causes an increasing work hardening especially at the tool contact area of the formed parts. Larger step-down increments, on the other hand, induce a greater bending deformation. The plastic deformation by bending leads to a complex stress field that involves alternating residual tensile stresses on the tool and residual compressive stresses on the tool-averted side incrementally formed sheets. The present study demonstrates the potential of high-energy synchrotron x-ray diffraction for the spatially resolved forming mechanism research in SPIF. Controlling the residual stress states by optimizing the process parameters necessitates knowledge of the fundamental forming mechanism action.


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