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At least 127 records · Page 7

Effect of Stacking Faults on the X-Ray Diffraction Profiles of Beta-SiC Powders

X-ray diffraction patterns or beta-SiC (3C or the cubic polytype or sic) powders often exhibit an additional peak at d = 0.266 nm, high background intensity around the (111) peak, and relative intensities for peaks which differ from those predicted from the crystal structure. Computer simulations were used to show that all these features are due to stacking faults in the powders and not due to the presence of other polytypes in the powders. Such simulations allow diffraction patterns to be generated for different types, frequencies, and spatial distribution or faults. Comparison of the simulation results to the XRD data indicates that the B-SiC particles consist either of heavily faulted clusters distributed irregularly between regions that have only occasional faults or twins, or the powders consist of two types of particles with different populations of faults: those with a high density of faults and those with only twins or occasional faults. Additional information is necessary to determine which description is correct. However, the simulation results can be used to rule out certain fault configurations.

Pujar, Vijay V.↗

Intrinsic self-stressing and low carbon Engineered Cementitious Composites (ECC) for improved sustainability

Highlights: • A self-stressing criterion for ECC was established and experimentally verified. • An intrinsic self-stressing ECC was developed by utilizing LC3 and CSA cement. • Initial maximum expansion and later expansion loss were successfully tailored. • Expansion mechanism was identified by XRD patterns. • Self-stressing ECC has 64% of the carbon footprint of conventional concrete. Engineered Cementitious Composites (ECC) is an emerging cementitious composite material with ultra-high ductility. However, its higher cement dosage limits its material greenness and leads to concerns with drying shrinkage. In this research, an ECC utilizing limestone calcined clay cement (LC3) and calcium sulphoaluminate cement (CSA) is investigated, focusing on minimizing the material's embodied carbon while enhancing its durability with intrinsic self-stressing functionality. A self-stressing criterion is theoretically established and experimentally verified. X-ray diffraction patterns reveal an ettringite quantity that modulates the initial expansion and later expansion-reversal of LC3-CSA-ECC to support a persistent self-stressing mechanism. LC3-CSA-ECC has a lower (64%) carbon footprint and similar embodied energy compared to conventional concrete. When combined with the durability advantage (tiny crack, high ductility of 5.5%, and self-stressing function), this low carbon self-stressing ECC holds promise as a sustainable repair material that lowers the embodied and operational carbon in civil infrastructure.

36 MATERIALS SCIENCE↗

The Convolutional Multiple Whole Profile (CMWP) Fitting Method, a Global Optimization Procedure for Microstructure Determination

The analysis of line broadening in X-ray and neutron diffraction patterns using profile functions constructed on the basis of well-established physical principles and TEM observations of lattice defects has proven to be a powerful tool for characterizing microstructures in crystalline materials. These principles are applied in the convolutional multiple-whole-profile (CMWP) procedure to determine dislocation densities, crystallite size, stacking fault and twin boundary densities, and intergranular strains. The different lattice defect contributions to line broadening are separated by considering the hkl dependence of strain anisotropy, planar defect broadening and peak shifts, and the defect dependent profile shapes. The Levenberg–Marquardt (LM) peak fitting procedure can be used successfully to determine crystal defect types and densities as long as the diffraction patterns are relatively simple. However, in more complicated cases like hexagonal materials or multiple-phase patterns, using the LM procedure alone may cause uncertainties. Here, we extended the CMWP procedure by including a Monte Carlo statistical method where the LM and a Monte Carlo algorithm were combined in an alternating manner. The updated CMWP procedure eliminated uncertainties and provided global optimized parameters of the microstructure in good correlation with electron microscopy methods.

36 MATERIALS SCIENCE↗

In Situ Transmission Electron Microscopy of High-Temperature Inconel-625 Corrosion by Molten Chloride Salts

This paper describes an approach to monitor high temperature molten chloride (MgCl 2 -NaCl-KCl) salt corrosion of Inconel-625 alloy in real time at high spatial resolution. The approach is based on a micro-environmental-cell assembly integrated into a transmission-electron-microscope goniometer to examine in situ the salt-alloy interface during corrosion, employing real time electron diffraction and imaging. It establishes procedures to minimize incorporation of H 2 O or O 2 from atmosphere in the chloride salts during sample fabrication and corrosion, which is critical to understanding the fundamental corrosion mechanisms. A clustering algorithm and a 2D Gaussian fit function are used to determine diffraction spot intensities in in situ diffraction patterns, to quantify alloy corrosion. This facilitates quantitative observation of the evolution of individual grains, in contrast to conventional macroscopic corrosion rate quantification. The isothermal corrosion rate of Inconel-625 in an anhydrous, unoxidized salt-stack is 220 ± 30 μm year -1 at 700 °C and 350 ± 20 μm year -1 at 800 °C. However, the corrosion rate at 700 °C increases five-fold to 1000 ± 170 μm year -1 when the salt stack is air-exposed, indicating the dominant effects of hydrated or oxidized impurities on corrosion acceleration. Furthermore, real time imaging of the microstructure evolution suggests that corrosion is initiated at grain boundaries.

14 SOLAR ENERGY↗

Tensile behavior of dual-phase titanium alloys under high-intensity proton beam exposure: radiation-induced omega phase transformation in Ti-6Al-4V

A high-intensity proton beam exposure with 181 MeV energy has been conducted at Brookhaven Linac Isotope Producer facility on various material specimens for accelerator targetry applications, including titanium alloys as a beam window material. The radiation damage level of the analyzed capsule was 0.25 dpa at the beam center region with an irradiation temperature around 120 oC. Tensile tests showed increased hardness and a large decrease in ductility for the dual a+ß-phase Ti-6Al-4V Grade-5 and Grade-23 extra low interstitial alloys, with the near a-phase Ti-3Al-2.5V Grade-9 alloy still exhibiting uniform elongation of a few % after irradiation. Transmission Electron Microscope analyses on Ti-6Al-4V indicated clear evidence of a high-density of defect clusters with size less than 2 nm in each a-phase grain. The ß-phase grains did not contain any visible defects such as loops or black dots, while the diffraction patterns clearly indicated ?-phase precipitation in an advanced formation stage. The radiation-induced ?-phase transformation in the ß-phase could lead to greater loss of ductility in Ti-6Al-4V alloys in comparison with Ti-3Al-2.5V alloy with less ß-phase.google scho

Tensile Test, titanium, acclerator, proton beam↗

Ultraviolet Photooxidation of Smectite-Bound Fe(II) and Implications for the Origin of Martian Nontronites

Clay minerals detected with orbital and in situ instruments in ancient Martian terrains constrain Mars' climate and aqueous alteration history. Early in its history, Mars experienced an atmospheric redox change and iron-bearing clay minerals may preserve the effects of that transition. Ferrous smectites, the thermodynamically predicted product of chemical weathering of basalts under anoxic conditions, may have undergone oxidation by exposure to chemical oxidants in the atmosphere or regolith, or by direct photooxidation at the surface. To assess these potential oxidation pathways, ferrous trioctahedral smectites of varying initial iron content were synthesized and subjected to oxidation by ultraviolet (UV) irradiation. Experimental UV irradiation under an anoxic atmosphere equivalent to approximately 7 years of flux on the Martian surface caused partial oxidation of smectite-bound Fe (Fe3+/ΣFe = 16–18%) and octahedral sheet contraction. Metal-OH vibrational bands in visible/near infrared (VNIR) reflectance spectra of oxidized smectites changed in band depth and asymmetry with higher iron content. X-ray diffraction patterns of UV irradiated samples indicate the formation of a mixed di- and trioctahedral smectite or a secondary nontronite phase, possibly on the surfaces of higher iron content smectites. These experiments suggest that UV irradiation is able to oxidize structurally bound iron in smectites without the presence of other chemical oxidants. Photooxidation may have influenced the mineralogy, both syndepositionally and postdepositionally, of Martian alteration assemblages formed near the surface and this process needs not be limited to one part of their formation history. Plain Language Summary: Martian mineral assemblages observed with orbiters and rover instruments allow us to understand the planet's past climate and aqueous activity. Hydrated minerals that contain Fe(II) are of particular interest as they would have been affected by the early atmosphere becoming more oxidizing overtime, changing the structural iron into Fe(III). In this study, we synthesized Fe(II) smectites with varying iron content and irradiated them with an ultraviolet (UV) light source to test whether they could be photooxidized. Iron in the smectite minerals was incompletely oxidized by UV radiation after being exposed for the equivalent of approximately 7 years of exposure on the early Mars surface. The smectites with higher iron content showed more changes with photooxidation in their visible/near infrared spectra as well as in their X-ray diffraction patterns, two datasets collected by instruments on currently active Martian missions. These results suggest that UV photooxidation is a plausible contributor to the mineralogy and redox state of clay mineral assemblages observed at the Martian surface.

V. B. Rivera Banuchi↗

Understanding Formation of Irradiation-Induced Defects through 4D-STEM, Electron Tomography, and WBDF-STEM

A major challenge in advancing nuclear materials for next-generation fission and proposed fusion reactors is to comprehensively understand the formation of irradiation-induced defects. Here it is essential to correlate the evolution of irradiation-induced defects and the degradation of mechanical properties, as they collectively dictate the material's lifespan and ensure nuclear safety. Scanning transmission electron microscopy (STEM) based techniques have emerged as indispensable tools for irradiation-induced defect characterization, offering high spatial resolution imaging and chemical analysis, such as electron energy loss spectroscopy (EELS) and energy dispersive X-ray spectroscopy (EDXS). These techniques have been effectively used to obtain an atomic-scale view of the defect structure. Recent advances in electron microscopy, particularly in 4D-STEM, offer detailed insight into microstructural evolution by capturing full 2D diffraction patterns at every pixel position. Using high-speed direct electron detectors, this technology generates a four-dimensional dataset, overcoming the limitations of traditional STEM imaging.

36 MATERIALS SCIENCE↗

Structure of the pellet-cladding interaction layer of a high-burnup Zr-Nb-O nuclear fuel cladding

Here, structure of the pellet/cladding-interaction (PCI) layer of a high-burnup nuclear fuel with niobium-bearing cladding was investigated using modern transmission electron microscopy (TEM) techniques. Morphology of the PCI consisted of uniform zirconia layer on the cladding side and finger-like features towards to the ceramic fuel. The PCI layer showed a complex microstructure that constitutes three distinct zirconia layers formed by two zirconia phases. From cladding to fuel, monoclinic, tetragonal, and another tetragonal phase were determined via TEM diffraction patterns and precession electron diffraction (PED) using ASTAR microscopy platform (AMP). Characterizations showed that monoclinic and tetragonal phases close to the cladding were crack-free, but the tetragonal layer adjacent to the fuel contained cracks and pores. Presence of the monoclinic layer suggested that its formation involved the gaseous diffusion of oxygen below threshold dose of fission product damage before the fuel/cladding contact occurred. Furthermore, high-resolution TEM revealed compound phase of (U,Zr)O 2 at fringes of zirconia fingers on the fuel side.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Fresnel diffraction plates are simple and inexpensive

Fresnel plate demonstrates diffraction phenomena simply and inexpensively. A large number of identical diffracting apertures are made in random orientation on photographic film. When a small source of light is viewed through the plate, the diffraction pattern typical of the diffracting aperture is readily seen.

Hoover, R. B.↗

Study of X-ray diffraction on aging alloys with different degrees of volume discrepancy between the precipitation phase and the matrix

Study of the diffraction patterns of X rays diffracted by dispersion-hardened alloys with various degrees of difference between the specific atomic volumes of their precipitation phases and matrices. Experiments were performed on aging alloys KhN77TIuR (nimonic) and KhN67VMTIuO, which have the same types of gamma solid solutions and precipitating gamma prime phases, but differ considerably with respect to the volume factor. It is found that in the decay of supersaturated solid solutions for which the difference between the specific atomic volumes of the precipitation phase and the matrix is small (alloy KhN67VMTIuO) the nature of the intensity distribution of the diffraction lines remains practically unchanged regardless of the aging, while in cases where the volume discrepancy is large (alloy KhN77TIuR) significant changes in the appearance of the diffraction lines are recorded.-

Gitgarts, M. I.↗

Radiation sensitive area detection device and method

A radiation sensitive area detection device for use in conjunction with an X ray, ultraviolet or other radiation source is provided which comprises a phosphor containing film which releases a stored diffraction pattern image in response to incoming light or other electromagnetic wave. A light source such as a helium-neon laser, an optical fiber capable of directing light from the laser source onto the phosphor film and also capable of channelling the fluoresced light from the phosphor film to an integrating sphere which directs the light to a signal processing means including a light receiving means such as a photomultiplier tube. The signal processing means allows translation of the fluoresced light in order to detect the original pattern caused by the diffraction of the radiation by the original sample. The optical fiber is retained directly in front of the phosphor screen by a thin metal holder which moves up and down across the phosphor screen and which features a replaceable pinhole which allows easy adjustment of the resolution of the light projected onto the phosphor film. The device produces near real time images with high spatial resolution and without the distortion that accompanies prior art devices employing photomultiplier tubes. A method is also provided for carrying out radiation area detection using the device of the invention.

Carter, Daniel C.↗

Apparatus and method for a light direction sensor

The present invention provides a light direction sensor for determining the direction of a light source. The system includes an image sensor; a spacer attached to the image sensor, and a pattern mask attached to said spacer. The pattern mask has a slit pattern that as light passes through the slit pattern it casts a diffraction pattern onto the image sensor. The method operates by receiving a beam of light onto a patterned mask, wherein the patterned mask as a plurality of a slit segments. Then, diffusing the beam of light onto an image sensor and determining the direction of the light source.

Leviton, Douglas B.↗

Griffith Saponite as an Analog for Clay Minerals at Yellowknife Bay in Gale Crater, Mars: A Marker for Low-temperature Hydrothermal Processes

The CheMin X-ray diffraction (XRD) instrument onboard the Mars Science Laboratory rover Curiosity in Gale Crater, Mars, discovered smectite in drill fines of the Sheepbed mudstone at Yellowknife Bay (YNB). The mudstone has a basaltic composition, and the XRD powder diffraction pattern shows smectite 02l diffraction bands peaking at 4.59 A for targets John Klein and Cumberland, consistent with tri-octahedral smectites (saponite). From thermal analysis, the saponite abundance is ~20 wt. %. Among terrestrial analogues we have studied, ferrian saponite from Griffith Park (Los Angeles, CA) gives the best match to the position of the 02l diffraction band of YNB saponites. Here we describe iron-rich saponites from a terrestrial perspective, with a focus on Griffith saponite, and discuss their implications for the mineralogy of Sheepbed saponite and its formation pathways. Iron-rich saponite: Iron-rich saponite on the Earth is recognized as a low-temperature (<100 C), authigenic alteration product of basalt [e.g., 4-16]. In the discussion that follows, we reference the position of the 02l band because it is a measure of the unit cell 'b' dimension of the octahedral layer and thus the cations (including Fe redox state) in the octahedral layer. Ordinarily, the 06l band near 1.5 A is used to determine the 'b' dimension of smectite, but this band is not accessible with MSL CheMin instrument. For reference, a ferrosaponite (i.e., Fe2+ saponite) studied by [15] has a 02l spacing of 4.72 A and Fe3+/Fe = 0.27 [15]. Samples of terrestrial ferrosaponite, however, are reported to oxidize on the timescale of days when removed from their natural environment and not protected from oxidation. The Griffith saponite is Mg-rich ferrian saponite, and sample AMNH 89172 has an 02l spacing of 4.59 A (same as the Sheepbed saponites) and Fe3+/Fe = 0.64 [3]. This similarity suggests that Sheepbed saponites are ferrian (incompletely oxidized ferrosaponite). More oxidized Griffith saponites (Fe3+/Fe > 0.90) have somewhat smaller 02l d-spacings and also show Mossbauer evidence for an XRD amorphous Fe-bearing phase (e.g., ferrihydrite, hisingerite, superparamagnetic ferric oxides, etc.). The Griffith saponite occurs as vesicle fills, as replacements of olivine, and as replacements of mesostasis (basaltic glass). Similar occurrence modes are reported elsewhere. Hisingerite has been proposed by [13] as the alteration product of ferrian saponite whose precursor by oxidation was ferrosaponite.

Morris, R.V.↗

Geometry of divergent-beam diffraction.

Divergent-beam diffraction geometry for interpretation of Kossel diffraction patterns in space group assignment lattice parameters and structure factor evaluation

CRYSTAL STRUCTURE↗

Diamonds in detonation soot

Diamonds 4 to 7 nm in diameter have been identified and partially isolated from soot formed in detonations of carbon-forming composite explosives. The morphology of the soot has been examined by transmission electron microscopy (TEM), and the identity of the diamond has been established by the electron diffraction pattern of the TEM samples and by the X-ray diffraction (XRD) pattern of the isolated solid. Graphite is also present in the form of ribbons of turbostatic structure with a thickness of 2 to 4 nm. A fraction, about 25 percent of the soot by weight, was recovered from the crude soot after oxidation of the graphite with fuming perchloric acid. This fraction showed a distinct XRD pattern of diamond and the diffuse band of amorphous carbon. The IR spectrum of these diamonds closely matches that of diamonds recovered from meteorites (Lewis et al., 1987), perhaps indicating similar surface properties after the oxidation. If these diamonds are produced in the detonation itself or during the initial expansion, they exhibit a phenomenal crystal growth rate (5 nm/0.00001 s equal 1.8 m/hr) in a medium with a very low hydrogen/carbon ratio. Because the diamonds will be carried along with the expanding gases, they will be accelerated to velocities approaching 8 km/s.

Greiner, N. Roy↗

Modeling and experimental validation of dynamical effects in Bragg coherent x-ray diffractive imaging of finite crystals

Bragg coherent diffractive imaging (BCDI) is a noninvasive microscopy technique that can visualize the shape and internal lattice deviations of crystals with nanoscale spatial resolution and picometer deformation sensitivity. Its strain imaging capability relies on Fourier transform–based iterative phase retrieval algorithms, which are mostly developed under the kinematical approximation. Such approximation prohibits the application of BCDI on larger crystals, which are commonly seen in most emerging functional materials. Understanding the dynamical effect in BCDI, as well as developing a validated method for modeling BCDI at the dynamical diffraction limit, is crucial for applying BCDI to hierarchical systems that contain micron-sized crystals and grains. Thus we report a comparative study on the impact of dynamical diffraction effects by comparing the reconstruction results from two measurements of the same crystal. Forward simulation is implemented to show subtle changes of interference fringes in the diffraction pattern due to the dynamical diffraction, and is compared directly with the experimental data.

36 MATERIALS SCIENCE↗