scholarly journals Gradient of Residual Stress and Lattice Parameter in Mechanically Polished Tungsten Measured Using Classical X-rays and Synchrotron Radiation

2020 ◽  
Vol 51 (11) ◽  
pp. 5945-5957
Author(s):  
Adrian Oponowicz ◽  
Marianna Marciszko-Wiąckowska ◽  
Andrzej Baczmański ◽  
Manuela Klaus ◽  
Christoph Genzel ◽  
...  
Keyword(s):  
Stress Gradient ◽  
Diffraction Method ◽  
High Energy ◽  
Lattice Parameter ◽  
Free Lattice ◽  
Stress Profile ◽  
X Rays ◽  
X Ray Diffraction ◽  
X Ray ◽  
Subsurface Region

Abstract In this work, the stress gradient in mechanically polished tungsten sample was studied using X-ray diffraction methods. To determine in-depth stress evolution in the very shallow subsurface region (up to 10 μm), special methods based on reflection geometry were applied. The subsurface stresses (depth up to 1 μm) were measured using the multiple-reflection grazing incidence X-ray diffraction method with classical characteristic X-rays, while the deeper volumes (depth up to 10 μm) were investigated using energy-dispersive diffraction with white high energy synchrotron beam. Both complementary methods allowed for determining in-depth stress profile and the evolution of stress-free lattice parameter. It was confirmed that the crystals of tungsten are elastically isotropic, which simplifies the stress analysis and makes tungsten a suitable material for testing stress measurement methods. Furthermore, it was found that an important compressive stress of about − 1000 MPa was generated on the surface of the mechanically polished sample, and this stress decreases to zero value at the depth of about 9 μm. On the other hand, the strain-free lattice parameter does not change significantly in the examined subsurface region.

Analysis of stresses and crystal structure in the surface layer of hexagonal polycrystalline materials: a new methodology based on grazing incidence diffraction

2016 ◽  
Vol 49 (1) ◽  
pp. 85-102 ◽  
Author(s):  
Marianna Marciszko ◽  
Andrzej Baczmański ◽  
Chedly Braham ◽  
Mirosław Wróbel ◽  
Wilfrid Seiler ◽  
...  
Keyword(s):  
Synchrotron Radiation ◽  
Stress Gradient ◽  
Grazing Incidence ◽  
Lattice Parameter ◽  
Polycrystalline Materials ◽  
X Rays ◽  
X Ray Diffraction ◽  
Surface Layers ◽  
X Ray ◽  
Good Agreement

The multireflection grazing-incidence X-ray diffraction (MGIXD) method is commonly used to determine a stress gradient in thin surface layers (about 1–20 µm for metals). In this article, the development of MGIXD to enable the determination not only of stresses but also of thec/aratio and thea0strain-free lattice parameter in hexagonal polycrystalline materials is presented and tested. The new procedure was applied for the results of measurements performed using a laboratory X-ray diffractometer and synchrotron radiation. The evolution of stresses and lattice parameters with depth was determined for Ti and Ti-alloy samples subjected to different mechanical surface treatments. A very good agreement of the results obtained using three different wavelengths of synchrotron radiation as well as classical X-rays (CuKα radiation) was found.

scholarly journals Growth of sillenite Bi12FeO20 single crystals: structural, thermal, optical, photocatalytic features and first principle calculations

2020 ◽  
Vol 10 (1) ◽  
Author(s):  
Durga Sankar Vavilapalli ◽  
Ambrose A. Melvin ◽  
F. Bellarmine ◽  
Ramanjaneyulu Mannam ◽  
Srihari Velaga ◽  
...  
Keyword(s):  
Single Crystal ◽  
Single Crystals ◽  
Photoelectron Spectroscopy ◽  
Diffraction Method ◽  
Lattice Parameter ◽  
First Principle ◽  
X Ray Diffraction ◽  
X Ray ◽  
First Principle Calculations ◽  
Photodegradation Efficiency

AbstractIdeal sillenite type Bi12FeO20 (BFO) micron sized single crystals have been successfully grown via inexpensive hydrothermal method. The refined single crystal X-ray diffraction data reveals cubic Bi12FeO20 structure with single crystal parameters. Occurrence of rare Fe4+ state is identified via X-ray photoelectron spectroscopy (XPS) and X-ray absorption spectroscopy (XAS). The lattice parameter (a) and corresponding molar volume (Vm) of Bi12FeO20 have been measured in the temperature range of 30–700 °C by the X-ray diffraction method. The thermal expansion coefficient (α) 3.93 × 10–5 K−1 was calculated from the measured values of the parameters. Electronic structure and density of states are investigated by first principle calculations. Photoelectrochemical measurements on single crystals with bandgap of 2 eV reveal significant photo response. The photoactivity of as grown crystals were further investigated by degrading organic effluents such as Methylene blue (MB) and Congo red (CR) under natural sunlight. BFO showed photodegradation efficiency about 74.23% and 32.10% for degrading MB and CR respectively. Interesting morphology and microstructure of pointed spearhead like BFO crystals provide a new insight in designing and synthesizing multifunctional single crystals.

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.

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.

Influence of Surface Roughness on the Quality of Data Obtained by Pseudo-Grazing Incidence X-Ray Diffraction

2006 ◽  
Vol 514-516 ◽  
pp. 1618-1622 ◽  
Author(s):  
Maria José Marques ◽  
J.C.P. Pina ◽  
A. Morão Dias
Keyword(s):  
Residual Stress ◽  
Surface Roughness ◽  
Stress Gradient ◽  
Roughness Parameter ◽  
Diffraction Method ◽  
Grazing Incidence ◽  
Bragg Diffraction ◽  
X Ray Diffraction ◽  
Residual Surface Stress ◽  
X Ray

The conventional Bragg diffraction geometry, normally used to characterize the residual surface stress state, it is not suitable to evaluate surface treated materials and thin films. The X-ray path lengths through a surface layer or thin film are too short to produce adequate diffraction intensities in relation to the bulk or the substrate. Another limitation of the conventional technique appears when a residual stress gradient is present in the irradiated surface. The technique only enables the evaluation of the mean value of this gradient. In these cases, a recently proposed Pseudo-Grazing Incident X-ray Diffraction method would be better applicable. In this study, the Pseudo-Grazing Incidence X-ray Diffraction is applied to characterize the residual stress depth profiles of several AISI 4140 samples, which were prepared, by mechanical polishing and grinding, in order to present different surface roughness parameters, Ra. The experimental results lead to the conclusion that the surface roughness limits the application of the Pseudo-Grazing Incidence methodology to a minimum X-ray incident angle. This angle is the one that enables a mean X-ray penetration depth with the same order of magnitude of the sample surface roughness parameter, Ra.

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.

scholarly journals DLSR: a solution to the parallax artefact in X-ray diffraction computed tomography data

2020 ◽  
Vol 53 (6) ◽  
pp. 1531-1541
Author(s):  
A. Vamvakeros ◽  
A. A. Coelho ◽  
D. Matras ◽  
H. Dong ◽  
Y. Odarchenko ◽  
...  
Keyword(s):  
Computed Tomography ◽  
Tomographic Reconstruction ◽  
Scale Up ◽  
Lattice Parameter ◽  
Chemical Information ◽  
X Rays ◽  
X Ray Diffraction ◽  
Major Barrier ◽  
X Ray ◽  
Tomography Data

A new tomographic reconstruction algorithm is presented, termed direct least-squares reconstruction (DLSR), which solves the well known parallax problem in X-ray-scattering-based experiments. The parallax artefact arises from relatively large samples where X-rays, scattered from a scattering angle 2θ, arrive at multiple detector elements. This phenomenon leads to loss of physico-chemical information associated with diffraction peak shape and position (i.e. altering the calculated crystallite size and lattice parameter values, respectively) and is currently the major barrier to investigating samples and devices at the centimetre level (scale-up problem). The accuracy of the DLSR algorithm has been tested against simulated and experimental X-ray diffraction computed tomography data using the TOPAS software.

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.

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