scholarly journals Energy-dispersive X-ray micro Laue diffraction on a bent gold nanowire

2021 ◽  
Vol 54 (1) ◽  
Author(s):  
Ali AlHassan ◽  
A. Abboud ◽  
T. W. Cornelius ◽  
Z. Ren ◽  
O. Thomas ◽  
...  

This article reports on energy-dispersive micro Laue (µLaue) diffraction of an individual gold nanowire that was mechanically deformed in three-point bending geometry using an atomic force microscope. The nanowire deformation was investigated by scanning the focused polychromatic X-ray beam along the nanowire and recording µLaue diffraction patterns using an energy-sensitive pnCCD detector that permits measurement of the angular positions of the Laue spots and the energies of the diffracted X-rays simultaneously. The plastic deformation of the nanowire was shown by a bending of up to 3.0 ± 0.1°, a torsion of up to 0.3 ± 0.1° and a maximum deformation depth of 80 ± 5 nm close to the position where the mechanical load was applied. In addition, extended Laue spots in the vicinity of one of the clamping points indicated the storage of geometrically necessary dislocations with a density of 7.5 × 1013 m−2. While µLaue diffraction with a non-energy-sensitive detector only gives access to the deviatoric strain, the energy sensitivity of the employed pnCCD offers absolute strain measurements with a resolution of 1%. Here, the residual strain after complete unloading of the nanowire amounted to maximum tensile and compressive strains of the order of +1.2 and −3%, which is comparable to the actual resolution limit. The combination of white-beam µLaue diffraction using an energy-sensitive pixel detector with nano-mechanical testing opens up new possibilities for the study of mechanical behavior at the nanoscale.

Author(s):  
Marc H. Peeters ◽  
Max T. Otten

Over the past decades, the combination of energy-dispersive analysis of X-rays and scanning electron microscopy has proved to be a powerful tool for fast and reliable elemental characterization of a large variety of specimens. The technique has evolved rapidly from a purely qualitative characterization method to a reliable quantitative way of analysis. In the last 5 years, an increasing need for automation is observed, whereby energy-dispersive analysers control the beam and stage movement of the scanning electron microscope in order to collect digital X-ray images and perform unattended point analysis over multiple locations.The Philips High-speed Analysis of X-rays system (PHAX-Scan) makes use of the high performance dual-processor structure of the EDAX PV9900 analyser and the databus structure of the Philips series 500 scanning electron microscope to provide a highly automated, user-friendly and extremely fast microanalysis system. The software that runs on the hardware described above was specifically designed to provide the ultimate attainable speed on the system.


Author(s):  
Y. Sato ◽  
T. Hashimoto ◽  
M. Ichihashi ◽  
Y. Ueki ◽  
K. Hirose ◽  
...  

Analytical TEMs have two variations in x-ray detector geometry, high and low angle take off. The high take off angle is advantageous for accuracy of quantitative analysis, because the x rays are less absorbed when they go through the sample. The low take off angle geometry enables better sensitivity because of larger detector solid angle.Hitachi HF-2000 cold field emission TEM has two versions; high angle take off and low angle take off. The former allows an energy dispersive x-ray detector above the objective lens. The latter allows the detector beside the objective lens. The x-ray take off angle is 68° for the high take off angle with the specimen held at right angles to the beam, and 22° for the low angle take off. The solid angle is 0.037 sr for the high angle take off, and 0.12 sr for the low angle take off, using a 30 mm2 detector.


1999 ◽  
Vol 32 (5) ◽  
pp. 924-933 ◽  
Author(s):  
A. R. Lang ◽  
A. P. W. Makepeace ◽  
J. E. Butler

Optical microscopic and goniometric measurements were combined with microradiography, diffraction-pattern analysis and topography to study a 2 mm thick [001]-texture CVD (chemical vapour deposition) diamond film that had developed a coarse-grained structure composed of separate columnar crystallites. Individual columns were capped by large (001) facets, with widths up to 0.5 mm, and which were smooth but not flat, whereas the column sides were morphologically irregular. The refractive deviation of X-rays transmitted through the crystallites was exploited for delineating facet edges, thereby facilitating the controlled positioning of small-cross-section X-ray beams used for recording diffraction patterns from selected volumes in two representative crystallites. Their structure consisted of a [001]-axial core column surrounded by columns in twin orientation with respect to the core. The diamond volume directly below the (001) facets was free from low-angle boundaries, and no dislocation outcrops on the facets were detected. Significant elastic deformation of this volume was only present close to the facet periphery, where misorientations reached a few milliradians. Lattice imperfection was high in the twins, with ∼1° misorientations.


about chemical bonding and molecular structure. This information can be used to detect th e types of organic materials present on the surface. 4.3.2.2. Raman spectroscopy (RS) [7, 8] It is used to examine the energy levels of molecules that cannot be well character-ized via infrared spectroscopy. Th e two techniques, however, are complimentary. In the RS, a sample is irradiated with a strong monochromatic light source (usu-ally a laser). Most of the radiation will scatter or "reflect off' the sample at the same energy as the incoming laser radiation. However, a small amount will scat-ter from the sample at a wavelength slightly shifted from the original wavelength. It is possible to study the molecular structure or determine the chemical identity of the sample. It is quite straightforward to identify compounds by spectral library search. Due to extensive library spectral information, the unique spectral finger-print of every compound, and the ease with which such analyses can be per-formed, the RS is a very useful technique for various applications. An important application of the RS is the rapid, nondestructive characterization of diamond, diamond-like, and amorphous-carbon films. 4.3.2.3. Scanning electron microscopy (SEM) / energy dispersive X-ra y analysis (EDX) [7, 8] The SEM produce s detailed photographs that provide important information about the surface structure and morphology of almost any kind of sample. Image analy-sis is often the first and most important step in problem solving and failure analy-sis. With SEM, a focused beam of high-energy electrons is scanned over the sur-face of a material, causing a variety of signals, secondary electrons, X-rays, photons, etc. - each of which may be used to characterize the material with re-spect to specific properties . The signals are used to modulate the brightness on a CRT display, thereb y providing a high-resolution map of the selected material property. It is a surface imaging technique, but with Energy Dispersive X-ray (EDX) it can identify elements in the near-surface region. This technique is most useful for imaging particles. 4.3.2.4. X-ray fluorescence (XRF) [7, 8] Incident X-rays are used to excite surface atoms. The atoms relax through the emission of an X-ray with energy characteristic of the parent atoms and the inten-sity proportional to the amount of the element present. It is a bulk or "total mate-rials" characterization technique for rapid, simultaneous, and nondestructive analysis of elements having an atomic number higher than that of boron. Tradi-tional bulk analysis applications include identifying metals and alloys, detecting trace elements in liquids, and identifying residues and deposits. 4.3.2.5. Total-reflection X-ray fluorescence (TXRF) [7, 8] It is a special XRF technique that provides extremely sensitive measures of the elements present in a material's outer surface. Applications include searching for metal contamination in thin films on silicon wafers and detecting picogram-levels o f arsenic, lead, mercury and cadmium on hazardous, chemical fume hoods.

2003 ◽  
pp. 43-45

2016 ◽  
Vol 23 (5) ◽  
pp. 1210-1215 ◽  
Author(s):  
Jonathan Logan ◽  
Ross Harder ◽  
Luxi Li ◽  
Daniel Haskel ◽  
Pice Chen ◽  
...  

Recent progress in the development of dichroic Bragg coherent diffractive imaging, a new technique for simultaneous three-dimensional imaging of strain and magnetization at the nanoscale, is reported. This progress includes the installation of a diamond X-ray phase retarder at beamline 34-ID-C of the Advanced Photon Source. The performance of the phase retarder for tuning X-ray polarization is demonstrated with temperature-dependent X-ray magnetic circular dichroism measurements on a gadolinium foil in transmission and on a Gd5Si2Ge2crystal in diffraction geometry with a partially coherent, focused X-ray beam. Feasibility tests for dichroic Bragg coherent diffractive imaging are presented. These tests include (1) using conventional Bragg coherent diffractive imaging to determine whether the phase retarder introduces aberrations using a nonmagnetic gold nanocrystal as a control sample, and (2) collecting coherent diffraction patterns of a magnetic Gd5Si2Ge2nanocrystal with left- and right-circularly polarized X-rays. Future applications of dichroic Bragg coherent diffractive imaging for the correlation of strain and lattice defects with magnetic ordering and inhomogeneities are considered.


Author(s):  
Kannan M. Krishnan

X-rays diffraction is fundamental to understanding the structure and crystallography of biological, geological, or technological materials. X-rays scatter predominantly by the electrons in solids, and have an elastic (coherent, Thompson) and an inelastic (incoherent, Compton) component. The atomic scattering factor is largest (= Z) for forward scattering, and decreases with increasing scattering angle and decreasing wavelength. The amplitude of the diffracted wave is the structure factor, F hkl, and its square gives the intensity. In practice, intensities are modified by temperature (Debye-Waller), absorption, Lorentz-polarization, and the multiplicity of the lattice planes involved in diffraction. Diffraction patterns reflect the symmetry (point group) of the crystal; however, they are centrosymmetric (Friedel law) even if the crystal is not. Systematic absences of reflections in diffraction result from glide planes and screw axes. In polycrystalline materials, the diffracted beam is affected by the lattice strain or grain size (Scherrer equation). Diffraction conditions (Bragg Law) for a given lattice spacing can be satisfied by varying θ or λ — for study of single crystals θ is fixed and λ is varied (Laue), or λ is fixed and θ varied to study powders (Debye-Scherrer), polycrystalline materials (diffractometry), and thin films (reflectivity). X-ray diffraction is widely applied.


1989 ◽  
Vol 33 ◽  
pp. 389-396 ◽  
Author(s):  
Y. Yoshioka ◽  
T. Shinkai ◽  
S. Ohya

The development of linear position-sensitive detectors (PSD) has resulted in a large reduction of data acquisition times in the field of x-ray stress analysis. However, we also require two-dimensional (2-D) diffraction patterns for material evaluation. Especially, the microbeam x-ray diffraction technique gives valuable information on the structure of crystalline materials and this technique has been applied to fracture analysis by x-rays. Many kinds of 2-D PSD have been developed that have insufficient spatial resolution. So x-ray film has still been used as a 2-D detector, but it requires relatively long exposure times and then the process after exposure is very troublesome.


1981 ◽  
Vol 25 ◽  
pp. 39-44 ◽  
Author(s):  
C. A. N. Conde ◽  
L. F. Requicha Ferreira ◽  
A. J. de Campos

AbstractA review of the basic physical principles of the gas proportional scintillation counter is presented. Its performance is discussed and compared with that of other room-temperature detectors in regard to applications to portable instruments for energy-dispersive X-ray fluorescence analysis. It is concluded that the gas proportional scintillation counter is definitely superior to all other room-temperature detectors, except the mercuric iodide (HgI2) detector. For large areas or soft X-rays it is also superior to the HgI2 detector.


1963 ◽  
Vol 7 ◽  
pp. 1-13 ◽  
Author(s):  
Volkmar Gerold ◽  
Heinz Auer ◽  
Winfried Merz

AbstractThe formation of the spherical Guinier—Preston zones in an aluminum-silver alloy is governed by a metastable miscibility gap, which consists of two different sections. The lower section occurs below 170°C (η state), the higher section up to 420°C (∊ state). The zones in the two sections differ in their silver concentration and in their atomic order. To prove the change in order, a combination of X-ray small-angle scattering and electric resistivity measurements was used. As the resistivity depends on the zone size and the atomic order, the change in order can be found when the zone size is known. This size was measured by the X-ray technique. To complete the results, X-rays ingle-crystal diffraction patterns with monochromatic radiation were taken at different stages. According to these patterns, three different states must be distinguished.The η′ state exists at room temperature after quenching from 550°C. The silver atoms prefer a layered arrangement in the zones, which is not very stable. It is destroyed after short annealings above 100°C. The η state is developed during annealing below 170°C. A three-dimensional atomic order is built up with increasing zone size, which results in a marked decrease in the resistivity. For the ∊ state (above 170°C), a nearly random atomic distribution exists. Step-quenching experiments prove that the ordered η state can also be developed at room temperature.


1985 ◽  
Vol 4 (6) ◽  
pp. 637-642 ◽  
Author(s):  
T. Aoi ◽  
T. Higuchi ◽  
R. Kidokoro ◽  
R. Fukumura ◽  
A. Yagi ◽  
...  

1 Energy dispersive X-ray analysis was performed on the renal tubular cells of two patients with inorganic mercury intoxication. 2 Some lysosomes of these cells consisted of unusual matrices of aggregated electron-dense grains which were positive for mercury, selenium and sulphur. 3 Though maps of the specific X-rays of both mercury and selenium coincided exactly with these lysosomes, the molecular ratio of selenium to mercury ranged between zero and 2.9. 4 It is unlikely that the trace element of selenium and exogenous inorganic mercury are deposited in the lysosomes independent of each other, but rather their coexistence in the characteristic lysosomes strongly suggests a compound formed by binding mercury to the SeH residues of selenoprotein.


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