A high-energy triple-axis X-ray diffractometer for the study of the structure of bulk crystals

2004 ◽  
Vol 37 (6) ◽  
pp. 901-910 ◽  
Author(s):  
C. Seitz ◽  
M. Weisser ◽  
M. Gomm ◽  
R. Hock ◽  
A. Magerl
Keyword(s):  
High Energy ◽  
X Rays ◽  
Bulk Crystals ◽  
X Ray Diffraction ◽  
X Ray ◽  
Peak Intensity ◽  
High Penetration ◽  
Massive Sample ◽  
Laue Geometry ◽  
The Ideal

A triple-axis diffractometer for high-energy X-ray diffraction is described. A 450 kV/4.5 kW stationary tungsten X-ray tube serves as the X-ray source. Normally, 220 reflections of thermally annealed Czochralski Si are employed for the monochromator and analyser. Their integrated reflectivity is about ten times higher than the ideal crystal value. With the same material as the sample, and working with the WKα line at 60 keV in symmetric Laue geometry for all axes, the full width at half-maximum (FWHM) values for the longitudinal and transversal resolution are 2.5 × 10−3and 1.1 × 10−4for ΔQ/Q, respectively, and the peak intensity for a non-dispersive setting is 3000 counts s−1. In particular, for a double-axis mode, an energy well above 100 keV from theBremsstrahlungspectrum can be used readily. High-energy X-rays are distinguished by a high penetration power and materials of several centimetre thickness can be analysed. The feasibility of performing experiments with massive sample environments is demonstrated.

A focusing Laue diffractometer for the investigation of bulk crystals

2008 ◽  
Vol 41 (4) ◽  
pp. 754-760 ◽  
Author(s):  
Matthias Stockmeier ◽  
Andreas Magerl
Keyword(s):  
High Energy ◽  
X Rays ◽  
Bulk Crystals ◽  
Attenuation Length ◽  
X Ray ◽  
Area Detector ◽  
Massive Sample ◽  
Crystallite Structure ◽  
High Temperature Furnaces ◽  
Non Destructive

A focusing Laue diffractometer for high-energy X-rays of up to 300 keV in a laboratory environment is presented. The long attenuation length for X-ray energies above 50 keV allows for the non-destructive investigation of structural issues and bulk properties of single crystals. Furthermore, massive sample environments such as high-temperature furnaces can be used more easily. With an area detector, anisotropic mosaicities or crystallite structure become visible without any rocking movement of the sample.

Epitaxial growth of BaO and SrO with new crystal structures using mass-separated low-energy O+ beams

1993 ◽  
Vol 8 (2) ◽  
pp. 321-323 ◽  
Author(s):  
Ryusuke Kita ◽  
Takashi Hase ◽  
Hiromi Takahashi ◽  
Kenichi Kawaguchi ◽  
Tadataka Morishita
Keyword(s):  
Lattice Constant ◽  
High Energy ◽  
Low Energy ◽  
Diffraction Reflection ◽  
High Energy Electron ◽  
Bulk Crystals ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transmission Electron ◽  
Cubic Structure

The growth of BaO and SrO on SrTiO3(100) substrates using mass-separated low-energy (50 eV) O+ beams has been studied using x-ray diffraction, reflection high-energy electron diffraction, and high-resolution transmission electron microscopy. It was found that the BaO and SrO films have been epitaxially grown with new structures different from those of corresponding bulk crystals: The BaO films have a cubic structure with a lattice constant of 4.0 Å, and the SrO films have a tetragonal structure with a lattice constant of a = 3.7 Å parallel to the substrate and with c = 4.0 Å normal to the substrate.

In situ time-resolved X-ray diffraction of tobermorite formation process under hydrothermal condition: Influence of reactive al compound

2011 ◽  
Vol 26 (2) ◽  
pp. 134-137 ◽  
Author(s):  
K. Matsui ◽  
A. Ogawa ◽  
J. Kikuma ◽  
M. Tsunashima ◽  
T. Ishikawa ◽  
...  
Keyword(s):  
Hydrothermal Reaction ◽  
High Energy ◽  
Saturated Steam ◽  
Array Detector ◽  
Time Interval ◽  
X Rays ◽  
X Ray Diffraction ◽  
Formation Reaction ◽  
X Ray

Hydrothermal formation reaction of tobermorite in the autoclaved aerated concrete (AAC) process has been investigated by in situ X-ray diffraction. High-energy X-rays from a synchrotron radiation source in combination with a newly developed autoclave cell and a photon-counting pixel array detector were used. XRD measurements were conducted in a temperature range 100–190°C throughout 12 h of reaction time with a time interval of 4.25 min under a saturated steam pressure. To clarify the tobermorite formation mechanism in the AAC process, the effect of Al addition on the tobermorite formation reaction was studied. As intermediate phases, non-crystalline calcium silicate hydrate (C-S-H), hydroxylellestadite (HE), and katoite (KA) were clearly observed. Consequently, it was confirmed that there were two reaction pathways via C-S-H and KA in the tobermorite formation reaction of Al containing system. In addition, detailed information on the structural changes during the hydrothermal reaction was obtained.

IN SITU STUDIES OF EPITAXIAL GROWTH BY SYNCHROTRON X-RAY DIFFRACTION

2006 ◽  
Vol 13 (02n03) ◽  
pp. 155-166 ◽  
Author(s):  
WOLFGANG BRAUN ◽  
KLAUS H. PLOOG
Keyword(s):  
Ostwald Ripening ◽  
Crystal Surface ◽  
High Energy ◽  
Molecular Beam Epitaxy Growth ◽  
X Rays ◽  
Surface Kinetics ◽  
X Ray Diffraction ◽  
X Ray ◽  
Kinetics Of

X-rays are ideal to study the structure of crystals due to their weak interaction with matter and in most cases allow a quantitative analysis using kinematical theory. To study the incorporation of atoms during crystal growth and to analyze the kinetics on the crystal surface high primary beam intensities available at synchrotrons are required. Our studies of the molecular beam epitaxy growth of III–V semiconductors reveal that, despite their similarity in crystal structure, the surface kinetics of GaAs (001), InAs (001) and GaSb (001) differ strongly. GaAs shows an unexpectedly large coarsening exponent outside the predicted range of Ostwald ripening models during recovery. GaSb exhibits dramatically different surface morphology variations during growth and recovery. Overgrowth of GaAs by epitaxial MnAs demonstrates the ability of X-ray diffraction to follow an interface as it is buried during heteroepitaxy, which is not possible by reflection high-energy electron diffraction.

Recrystallization of AA1050 Studied by 3DXRD

2006 ◽  
Vol 519-521 ◽  
pp. 1569-1578
Author(s):  
Dorte Juul Jensen
Keyword(s):  
Single Crystals ◽  
High Energy ◽  
Nucleation And Growth ◽  
X Rays ◽  
X Ray Diffraction ◽  
Orientation Relationships ◽  
X Ray ◽  
3 Dimensional ◽  
Kinetics Of

By 3 dimensional X-ray diffraction (3DXRD) using high energy X-rays from synchrotron sources it is possible to study in-situ the nucleation and growth during recrystallization. In this paper it is described and discussed how 3DXRD can supplement EBSP measurements of nucleation and growth. Three types of studies are considered: i) orientation relationships between nuclei and parent deformed matrix, ii) recrystallization kinetics of individual bulk grains and iii) filming of growing grains in deformed single crystals.

Accurate charge densities from powder X-ray diffraction – a new version of the Aarhus vacuum imaging-plate diffractometer

2017 ◽  
Vol 73 (4) ◽  
pp. 521-530 ◽  
Author(s):  
Kasper Tolborg ◽  
Mads R. V. Jørgensen ◽  
Sebastian Christensen ◽  
Hidetaka Kasai ◽  
Jacob Becker ◽  
...  
Keyword(s):  
Electron Density ◽  
High Energy ◽  
Imaging Plate ◽  
High Symmetry ◽  
X Rays ◽  
X Ray Diffraction ◽  
Core Electron ◽  
X Ray ◽  
Peak Broadening ◽  
Structure Factors

In recent years powder X-ray diffraction has proven to be a valuable alternative to single-crystal X-ray diffraction for determining electron-density distributions in high-symmetry inorganic materials, including subtle deformation in the core electron density. This was made possible by performing diffraction measurements in vacuum using high-energy X-rays at a synchrotron-radiation facility. Here we present a new version of our custom-built in-vacuum powder diffractometer with the sample-to-detector distance increased by a factor of four. In practice this is found to give a reduction in instrumental peak broadening by approximately a factor of three and a large improvement in signal-to-background ratio compared to the previous instrument. Structure factors of silicon at room temperature are extracted using a combined multipole–Rietveld procedure and compared withab initiocalculations and the results from the previous diffractometer. Despite some remaining issues regarding peak asymmetry, the new diffractometer yields structure factors of comparable accuracy to the previous diffractometer at low angles and improved accuracy at high angles. The high quality of the structure factors is further assessed by modelling of core electron deformation with results in good agreement with previous investigations.

Impact of Sn ions on structural and electrical description of TiO2 nanoparticles

2021 ◽  
Vol 0 (0) ◽  
Author(s):  
Mutaz Salih ◽  
M. Khairy ◽  
Babiker Abdulkhair ◽  
M. G. Ghoniem ◽  
Nagwa Ibrahim ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Simple Procedure ◽  
High Energy ◽  
X Rays ◽  
X Ray Diffraction ◽  
Energy Storage Devices ◽  
X Ray ◽  
Storage Devices ◽  
Transmission Electron ◽  
High Energy Storage

Abstract In this paper, Sn-doped TiO2 nanomaterials with varying concentrations were manufactured through a simple procedure. The fabricated TiO2 and Sn loaded on TiO2 nanoparticles were studied using X-ray diffraction, scanning electron microscopy, transmission electron microscopy, energy dispersive X-rays, Fourier transform infrared spectroscopy, and resistance analyses. The benefits of dielectric constant and ac conductivity rise at high Sn loaded concentration on TiO2 nanoparticles. The enhanced electrical conductivity is seen for STO3 (3.5% Sn doped TiO2) and STO4 (5% Sn doped TiO2) specimens are apparently associated with the introduced high defect TiO2 lattice. Furthermore, the fabricated specimens’ obtained findings may be applied as possible candidates for high-energy storage devices. Moreover, proper for the manufacture of materials working at a higher frequency.

Investigations of Buried Interfaces Using High Energy X-Ray Reflectivity

2001 ◽  
Vol 678 ◽  
Author(s):  
F. Rieutord ◽  
J. Eymery ◽  
O. Plantevin ◽  
B. Bataillou ◽  
D. Buttard ◽  
...  
Keyword(s):  
Grazing Angle ◽  
High Energy ◽  
Silicon On Insulator ◽  
Nanometer Scale ◽  
X Rays ◽  
X Ray ◽  
Buried Interfaces ◽  
High Penetration ◽  
Silicon Silicon ◽  
Insulator Substrate

AbstractX-ray reflectivity using high-energy X-rays allows one to characterize interfaces between thick materials at nanometer scale. The technique combines the high penetration of X-rays allowing the crossing of the radiation through large thicknesses of material with the interface sensitivity of grazing angle techniques. In the case of a buried interface between two thick materials, the beam enters the sample through the side of one material and contributions of external surfaces are suppressed. Then, the technique is sensitive to the interface structure only. Examples are given using wafer bonding interfaces, both in the hydrophilic case (as used e.g. in Silicon-On-Insulator substrate fabrication) and in the hydrophobic case (Silicon/Silicon bonding).

scholarly journals High-resolution strain mapping in bulk samples using full-profile analysis of energy-dispersive synchrotron X-ray diffraction data

2004 ◽  
Vol 37 (6) ◽  
pp. 883-889 ◽  
Author(s):  
A. Steuwer ◽  
J. R. Santisteban ◽  
M. Turski ◽  
P. J. Withers ◽  
T. Buslaps
Keyword(s):  
Reference Data ◽  
Profile Analysis ◽  
High Energy ◽  
X Rays ◽  
X Ray Diffraction ◽  
Strain Mapping ◽  
X Ray ◽  
Full Profile ◽  
Complementary Techniques ◽  
Point To Point

The feasibility of both high spatial and strain resolution is demonstrated using high-energy X-rays between 100 and 300 keV on beamline ID15A at the ESRF. The data analysis was performed using a multiple-peak Pawley-type refinement on the recorded spectra. An asymmetric peak profile was necessary in order to obtain a point-to-point uncertainty of 10−5. The measurements have been validated with complementary techniques or reference data.

Oxford HEXameter: Laboratory High Energy X-Ray Diffractometer for Bulk Residual Stress Analysis

2006 ◽  
Vol 524-525 ◽  
pp. 743-748 ◽  
Author(s):  
Alexander M. Korsunsky ◽  
Shu Yan Zhang ◽  
Daniele Dini ◽  
Willem J.J. Vorster ◽  
Jian Liu
Keyword(s):  
Accurate Determination ◽  
High Energy ◽  
Energy Dispersive ◽  
Detector Response ◽  
X Rays ◽  
X Ray Diffraction ◽  
X Ray ◽  
New Instrument ◽  
Synchrotron Beamlines

Diffraction of penetrating radiation such as neutrons or high energy X-rays provides a powerful non-destructive method for the evaluation of residual stresses in engineering components. In particular, strain scanning using synchrotron energy-dispersive X-ray diffraction has been shown to offer a fast and highly spatially resolving measurement technique. Synchrotron beamlines provide best available instruments in terms of flux and low beam divergence, and hence spatial and measurement resolution and data collection rate. However, despite the rapidly growing number of facilities becoming available in Europe and across the world, access to synchrotron beamlines for routine industrial and research use remains regulated, comparatively slow and expensive. A laboratory high energy X-ray diffractometer for bulk residual strain evaluation (HEXameter) has been developed and built at Oxford University. It uses a twin-detector setup first proposed by one of the authors in the energy dispersive X-ray diffraction mode and allows simultaneous determination of macroscopic and microscopic strains in two mutually orthogonal directions that lie approximately within the plane normal to the incident beam. A careful procedure for detector response calibration is used in order to facilitate accurate determination of lattice parameters by pattern refinement. The results of HEXameter measurements are compared with synchrotron X-ray data for several samples e.g. made from a titanium alloy and a particulate composite with an aluminium alloy matrix. Experimental results are found to be consistent with synchrotron measurements and strain resolution close to 2×10-4 is routinely achieved by the new instrument.

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