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At least 595 records · Page 33

Scanning transmission election microscopy observations of twisted epitaxial gold nanodiscs in twisted molybdenum disulfide bilayers

Atomic scale, scanning transmission electron microscopy (STEM) analysis of the moiré structures in twisted epitaxial gold nanodiscs encapsulated in twisted bilayer molybdenum disulfide is presented. High angle annular dark field STEM imaging reveals that the period of the moiré patterns between gold and molybdenum disulfide varies with different twist angles of the bilayer molybdenum disulfide, ranging from 1.80 nm (epitaxial alignment of gold) to 1.53 nm (twisted epitaxial alignment of gold). Additionally, bright field STEM imaging reveals a faint, larger "moiré of moiré" structure in cases where the bilayer molybdenum disulfide twist angle is small (~6°), arising from the overlapping three-layers, which is not visible in conventional transmission electron microscopy images. In conclusion, our experiments indicate that scanning transmission electron microscopy as a suitable tool for moiré analysis of twisted multilayer planar heterostructures, complementary to information provided by conventional transmission electron microscopy and diffraction.

Au↗

Noise spatial nonuniformity and the impact of statistical image reconstruction in CT myocardial perfusion imaging

Purpose: To achieve high temporal resolution in CT myocardial perfusion imaging (MPI), images are often reconstructed using filtered backprojection (FBP) algorithms from data acquired within a short-scan angular range. However, the variation in the central angle from one time frame to the next in gated short scans has been shown to create detrimental partial scan artifacts when performing quantitative MPI measurements. This study has two main purposes. (1) To demonstrate the existence of a distinct detrimental effect in short-scan FBP, i.e., the introduction of a nonuniform spatial image noise distribution; this nonuniformity can lead to unexpectedly high image noise and streaking artifacts, which may affect CT MPI quantification. (2) To demonstrate that statistical image reconstruction (SIR) algorithms can be a potential solution to address the nonuniform spatial noise distribution problem and can also lead to radiation dose reduction in the context of CT MPI. Methods: Projection datasets from a numerically simulated perfusion phantom and an in vivo animal myocardial perfusion CT scan were used in this study. In the numerical phantom, multiple realizations of Poisson noise were added to projection data at each time frame to investigate the spatial distribution of noise. Images from all datasets were reconstructed using both FBP and SIR reconstruction algorithms. To quantify the spatial distribution of noise, the mean and standard deviation were measured in several regions of interest (ROIs) and analyzed across time frames. In the in vivo study, two low-dose scans at tube currents of 25 and 50 mA were reconstructed using FBP and SIR. Quantitative perfusion metrics, namely, the normalized upslope (NUS), myocardial blood volume (MBV), and first moment transit time (FMT), were measured for two ROIs and compared to reference values obtained from a high-dose scan performed at 500 mA. Results: Images reconstructed using FBP showed a highly nonuniform spatial distribution of noise. This spatial nonuniformity led to large fluctuations in the temporal direction. In the numerical phantom study, the level of noise was shown to vary by as much as 87% within a given image, and as much as 110% between different time frames for a ROI far from isocenter. The spatially nonuniform noise pattern was shown to correlate with the source trajectory and the object structure. In contrast, images reconstructed using SIR showed a highly uniform spatial distribution of noise, leading to smaller unexpected noise fluctuations in the temporal direction when a short scan angular range was used. In the numerical phantom study, the noise varied by less than 37% within a given image, and by less than 20% between different time frames. Also, the noise standard deviation in SIR images was on average half of that of FBP images. In the in vivo studies, the deviation observed between quantitative perfusion metrics measured from low-dose scans and high-dose scans was mitigated when SIR was used instead of FBP to reconstruct images. Conclusions: (1) Images reconstructed using FBP suffered from nonuniform spatial noise levels. This nonuniformity is another manifestation of the detrimental effects caused by short-scan reconstruction in CT MPI. (2) Images reconstructed using SIR had a much lower and more uniform noise level and thus can be used as a potential solution to address the FBP nonuniformity. (3) Given the improvement in the accuracy of the perfusion metrics when using SIR, it may be desirable to use a statistical reconstruction framework to perform low-dose dynamic CT MPI.

62 RADIOLOGY AND NUCLEAR MEDICINE↗

Data-driven prediction of geometry- and toolpath sequence-dependent intra-layer process conditions variations in laser powder bed fusion

Geometrical features and toolpath sequence are two important factors that cause process condition variations, such as variations in the meltpool temperature or meltpool size, that might lead to undesired material properties in the laser powder bed fusion (LPBF) process. Due to the high dynamics and complex physics of the LPBF process, it is difficult to predict variations in process conditions with simulations alone. Advances in measurement technology and computational technologies open up new possibilities for smart manufacturing. In this paper, a data-driven method to predict intra-layer variations in the processing conditions that source from the toolpath sequence and part geometry is presented. The approach is demonstrated using two-color on-axis pyrometer measurements. Three demonstration cases are presented in which it is demonstrated (1) how the trained predictive model can be used as a filter to ease the interpretation of process variations and discover patterns related to toolpath and part geometry, and (2) how to generate predictions that can be used for feedforward control, i.e., for adjusting laser power or scanning speed along the toolpath using a meltpool temperature prediction model generated based on on-axis measurements. Results show that the developed prediction model is able to meaningfully predict process variations resulted from toolpath sequence and geometry. Predictions are aligned with the results from the related work of others and for the case of 180° laser path turnarounds in our high-speed X-ray imaging experiments. In conclusion, the potential issues related to the current maturity status of the process and measuring equipment that could in practice affect the performance of the proposed solutions are also discussed.

42 ENGINEERING↗

Microstructural study and densification analysis of hot work tool steel matrix composites reinforced with TiB{sub 2} particles

Hot work tool steels are characterized by good toughness and high hot hardness but are less wear resistant than other tooling materials, such as high speed steel. Metal matrix composites show improved tribological behavior, but not much work has been done in the field of hot work tool steels. In this paper TiB{sub 2}-reinforced hot work tool steel matrix composites were produced by spark plasma sintering (SPS). Mechanical alloying (MA) was proposed as a suited process to improve the composite microstructure. Density measurements and microstructure confirmed that MA promotes sintering and produces a fine and homogeneous dispersion of reinforcing particles. X-ray diffraction patterns of the sintered composites highlighted the formation of equilibrium Fe{sub 2}B and TiC, as predicted by thermodynamic calculations using Thermo-Calc® software. Scanning electron microscopy as well as scanning Kelvin probe force microscopy highlighted the reaction of the steel matrix with TiB{sub 2} particles, showing the formation of a reaction layer at the TiB{sub 2}-steel interface. Phase investigations pointed out that TiB{sub 2} is not chemically stable in steel matrix because of the presence of carbon even during short time SPS. - Highlights: • TiB{sub 2} reinforced steel matrix composites were produced by spark plasma sintering. • TiB{sub 2} was successfully dispersed in the steel matrix by mechanical alloying. • Steel and TiB{sub 2} react during sintering forming equilibrium Fe{sub 2}B and TiC. • The new phases were investigated by means of AFM, Volta potential and XRD analyses.

36 MATERIALS SCIENCE↗

Enhanced phase contrast transfer using ptychography combined with a pre-specimen phase plate in a scanning transmission electron microscope

We report the ability to image light elements in both crystalline and noncrystalline materials at near atomic resolution with an enhanced contrast is highly advantageous to understand the structure and properties of a wide range of beam sensitive materials including biological specimens and molecular hetero-structures. This requires the imaging system to have an efficient phase contrast transfer at both low and high spatial frequencies. Here, we introduce a new phase contrast imaging method in a scanning transmission electron microscope (STEM) using a pre-specimen phase plate in the probe forming aperture, combined with a fast pixelated detector to record diffraction patterns at every probe position, and phase reconstruction using ptychography. The phase plate significantly enhances the contrast transfer of low spatial frequency information, and ptychography maximizes the extraction of the phase information at all spatial frequencies. In addition, the STEM probe with the presence of the phase plate retains its atomic resolution, allowing simultaneous incoherent Z-contrast imaging to be obtained along with the ptychographic phase image. An experimental image of Au nanoparticles on a carbon support shows high contrast for both materials. Multislice image simulations of a DNA molecule shows the capability of imaging soft matter at low dose conditions, which implies potential applications of low dose imaging of a wide range of beam sensitive materials.

36 MATERIALS SCIENCE↗

Towards 3D mapping of BO₆ octahedron rotations at perovskite heterointerfaces, unit cell by unit cell

The rich functionalities in the ABO₃ perovskite oxides originate at least partly from the ability of the corner-connected BO₆ octahedral network to host a large variety of cations through distortions and rotations. Characterizing these rotations, which significantly affect both fundamental aspects of materials behavior and possible applications, remains a major challenge. In this work, we have developed a unique method of investigating BO₆ rotation patterns in complex oxides ABO₃ with unit cell resolution at heterointerfaces, where novel properties often emerge. Our method involves column shape analysis in annular bright field - scanning transmission electron microscope images of the ABO₃ heterointerfaces taken in specific orientations. The rotating phase of BO₆ octahedra can be identified for all three spatial dimensions without the need of case-by-case simulation. In several common rotation systems, it is now possible to quantitatively measure all three rotation angles. With this method, we examined interfaces between perovskites with distinct tilt systems as well as interfaces between tilted and untilted perovskites, identifying an unusual coupling behavior at the CaTiO₃/LSAT interface. We believe this unique method will significantly improve our knowledge of the complex oxide heterointerfaces.

36 MATERIALS SCIENCE↗

Temperature-dependent morphology of hybrid nanoflowers from elastin-like polypeptides

We report a method for creating hybrid organic-inorganic “nanoflowers” using calcium or copper ions as the inorganic component and a recombinantly expressed elastin-like polypeptide (ELP) as the organic component. Polypeptides provide binding sites for the dynamic coordination with metal ions, and then such noncovalent complexes become nucleation sites for primary crystals of metal phosphates. We have shown that the interaction between the stimuli-responsive ELP and Ca{sup 2+} or Cu{sup 2+}, in the presence of phosphate, leads to the growth of micrometer-sized particles featuring nanoscale patterns shaped like flower petals. The morphology of these flower-like composite structures is dependent upon the temperature of growth and has been characterized by scanning electron microscopy. The composition of nanoflowers has also been analyzed by energy-dispersive X-ray spectroscopy, X-ray photoelectron spectroscopy, and X-ray diffraction. The temperature-dependent morphologies of these hybrid nanostructures, which arise from the controllable phase transition of ELPs, hold potential for morphological control of biomaterials in emerging applications such as tissue engineering and biocatalysis.

36 MATERIALS SCIENCE↗

Structural and photoluminescence studies of TiO{sub 2} nanoparticles synthesized by solution combustion method

In this study titanium dioxide nanoparticle is prepared by simple solution combustion method. The powder X-ray diffraction pattern indicates the prepared titanium dioxide nanoparticles crystalline nature with tetragonal structure. Also it shows the nanoparticle is anatase and rutile mixed phase. The Field Emission Scanning Electron Microscopy image shows the nanostructure of particles in the size range about 50 nm. Room temperature photoluminescence shows intrinsic defects of oxygen vacancies.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

SU-C-213-02: Characterizing 3D Printing in the Fabrication of Variable Density Phantoms

Purpose: In this work, we present characterization, process flow, quality control and application of 3D fabricated low density phantoms for radiotherapy quality assurance. Methods: A Rostock delta 3D printer using polystyrene filament of diameter 1.75 mm was used to print geometric volumes of 2×2×1 cm{sup 3} of varying densities. The variable densities of 0.1 to 0.75 g/cm {sup 3} were created by modulating the infill. A computed tomography (CT) scan was performed to establish an infill-density calibration curve as well as characterize the quality of the print such as uniformity and the infill pattern. The time required to print these volumes was also recorded. Using the calibration, two low density cones (0.19, 0.52 g/cm{sup 3}) were printed and benchmarked against commercially available phantoms. The dosimetric validation of the low density scaling of Anisotropic Analytical Algorithm (AAA) was performed by using a 0.5 g/cm{sup 3} slab of 10×10×2.4 cm{sup 3} with EBT3 GafChromic film. The gamma analysis at 3%/3mm criteria were compared for the measured and computed dose planes. Results: Analysis of the volume of air pockets in the infill resulted in a reasonable uniformity for densities 0.4 to 0.75 g/cm{sup 3}. Printed phantoms with densities below 0.4 g/cm{sup 3} exhibited a higher ratio of air to polystyrene resulting in large non-uniformity. Compared to the commercial inserts, good agreement was observed only for the printed 0.52 g/cm{sup 3} cone. Dosimetric comparison for a printed low density volume placed in-between layers of solid water resulted in >95% gamma agreement between AAA calculated dose planes and measured EBT3 films for a 6MV 5×5 cm{sup 2} clinical beam. The comparison showed disagreement in the penumbra region. Conclusion: In conclusion, 3D printing technology opens the door to desktop fabrication of variable density phantoms at economical prices in an efficient manner for the quality assurance needs of a small clinic.

60 APPLIED LIFE SCIENCES↗

WE-D-303-02: Applications of Volumetric Images Generated with a Respiratory Motion Model Based On An External Surrogate Signal

Purpose: Respiratory motion can vary significantly over the course of simulation and treatment. Our goal is to use volumetric images generated with a respiratory motion model to improve the definition of the internal target volume (ITV) and the estimate of delivered dose. Methods: Ten irregular patient breathing patterns spanning 35 seconds each were incorporated into a digital phantom. Ten images over the first five seconds of breathing were used to emulate a 4DCT scan, build the ITV, and generate a patient-specific respiratory motion model which correlated the measured trajectories of markers placed on the patients’ chests with the motion of the internal anatomy. This model was used to generate volumetric images over the subsequent thirty seconds of breathing. The increase in the ITV taking into account the full 35 seconds of breathing was assessed with ground-truth and model-generated images. For one patient, a treatment plan based on the initial ITV was created and the delivered dose was estimated using images from the first five seconds as well as ground-truth and model-generated images from the next 30 seconds. Results: The increase in the ITV ranged from 0.2 cc to 6.9 cc for the ten patients based on ground-truth information. The model predicted this increase in the ITV with an average error of 0.8 cc. The delivered dose to the tumor (D95) changed significantly from 57 Gy to 41 Gy when estimated using 5 seconds and 30 seconds, respectively. The model captured this effect, giving an estimated D95 of 44 Gy. Conclusion: A respiratory motion model generating volumetric images of the internal patient anatomy could be useful in estimating the increase in the ITV due to irregular breathing during simulation and in assessing delivered dose during treatment. This project was supported, in part, through a Master Research Agreement with Varian Medical Systems, Inc. and Radiological Society of North America Research Scholar Grant #RSCH1206.

60 APPLIED LIFE SCIENCES↗

A phantom design for assessment of detectability in PET imaging

Purpose: The primary clinical role of positron emission tomography (PET) imaging is the detection of anomalous regions of {sup 18}F-FDG uptake, which are often indicative of malignant lesions. The goal of this work was to create a task-configurable fillable phantom for realistic measurements of detectability in PET imaging. Design goals included simplicity, adjustable feature size, realistic size and contrast levels, and inclusion of a lumpy (i.e., heterogeneous) background. Methods: The detection targets were hollow 3D-printed dodecahedral nylon features. The exostructure sphere-like features created voids in a background of small, solid non-porous plastic (acrylic) spheres inside a fillable tank. The features filled at full concentration while the background concentration was reduced due to filling only between the solid spheres. Results: Multiple iterations of feature size and phantom construction were used to determine a configuration at the limit of detectability for a PET/CT system. A full-scale design used a 20 cm uniform cylinder (head-size) filled with a fixed pattern of features at a contrast of approximately 3:1. Known signal-present and signal-absent PET sub-images were extracted from multiple scans of the same phantom and with detectability in a challenging (i.e., useful) range. These images enabled calculation and comparison of the quantitative observer detectability metrics between scanner designs and image reconstruction methods. The phantom design has several advantages including filling simplicity, wall-less contrast features, the control of the detectability range via feature size, and a clinically realistic lumpy background. Conclusions: This phantom provides a practical method for testing and comparison of lesion detectability as a function of imaging system, acquisition parameters, and image reconstruction methods and parameters.

60 APPLIED LIFE SCIENCES↗

TR-XPS Realtime Analysis Tool (ArroyoXPS) v0.1

The ALS has developed a Time-Resolved X-ray Photoelectron Spectroscopy (TR-XPS) technique, which involves applying a specific pattern of voltage curves to a sample while measuring XPS peaks. This pattern is repeated over multiple cycles, and changes in the material's response provide valuable scientific insights. Traditionally, file-based analysis workflows have been used: scans are run for a predetermined time, and after one or more scans are complete, calculations are made. ArroyoXPS changes this by offering in-experiment scan and analysis, allowing researchers to gain insights before a scan is finished. This enables them to adjust experimental parameters quickly, potentially saving valuable beamtime. ArroyoXPS includes tools for integrating with beamline control systems, performing analysis, and visualizing scan data in a web browser.

McReynolds, Dylan [Lawrence Berkeley National Labo↗

Climatology of aerosol properties at an atmospheric monitoring site on the northern California coast

Between April 2002 and June 2017, the Global Monitoring Laboratory (GML) of the National Oceanic and Atmospheric Administration (NOAA) made continuous measurements of a suite of in situ aerosol optical properties at a long-term monitoring site near Trinidad Head (THD), California. In addition to aerosol optical properties, between 2002–2006 a scanning humidograph system was operated, and inorganic ion and total aerosol mass concentrations were obtained from filter measurements. A combined analysis of these datasets demonstrates consistent patterns in aerosol climatology and highlights changes in sources throughout the year. THD is predictably dominated by sea salt aerosols; however, marine biogenic aerosols are the largest contributor to PM1 in the warmer months. Additionally, a persistent combustion source appears in the winter, likely a result of wintertime home heating. While the influences of local anthropogenic sources from vehicular and marine traffic are visible in the optical aerosol data, their influence is largely dictated by the wind direction at the site. Comparison of the THD aerosol climatology to that reported for other marine sites shows that the location is representative of clean marine measurements, even with the periodic influence of anthropogenic sources.

54 ENVIRONMENTAL SCIENCES↗

Applications of High Resolution Laser Induced Breakdown Spectroscopy for Environmental and Biological Samples

This chapter details the application of LIBS in a number of environmental areas of research such as carbon sequestration and climate change. LIBS has also been shown to be useful in other high resolution environmental applications for example, elemental mapping and detection of metals in plant materials. LIBS has also been used in phytoremediation applications. Other biological research involves a detailed understanding of wood chemistry response to precipitation variations and also to forest fires. A cross-section of Mountain pine (pinceae Pinus pungen Lamb.) was scanned using a translational stage to determine the differences in the chemical features both before and after a fire event. Consequently, by monitoring the elemental composition pattern of a tree and by looking for abrupt changes, one can reconstruct the disturbance history of a tree and a forest. Lastly we have shown that multivariate analysis of the LIBS data is necessary to standardize the analysis and correlate to other standard laboratory techniques. LIBS along with multivariate statistical analysis makes it a very powerful technology that can be transferred from laboratory to field applications with ease.

Martin, Madhavi Z↗

Copper intercalation at the interface of graphene and Ir(111) studied by scanning tunneling microscopy

We report on the intercalation of a submonolayer of copper at 775 K underneath graphene epitaxially grown on Ir(111) studied by means of low energy electron diffraction (LEED) and scanning tunneling microscopy (STM) at 77 K. Nucleation and growth dynamics of Cu below graphene have been investigated, and, most importantly, the intercalation mechanism has been identified. First, LEED patterns reveal the pseudomorphic growth of Cu on Ir under the topmost graphene layer resulting in a large Cu in-plane lattice parameter expansion of about 6% compared to Cu(111). Second, large-scale STM topographs as a function of Cu coverage show that Cu diffusion on Ir below graphene exhibits a low energy barrier resulting in Cu accumulation at Ir step edges. As a result, the graphene sheet undergoes a strong edges reshaping. Finally, atomically-resolved STM images reveal a damaged graphene sheet at the atomic scale after metal intercalation. Point defects in graphene were shown to be carbon vacancies. According to these results, a Cu penetration path beneath graphene is proposed to occur via metal aided defect formation with no or poor self healing of the graphene sheet. This work illustrates the fact that Cu intercalation is harmful for graphene grown on Ir(111) at the atomic scale.

36 MATERIALS SCIENCE↗

Characterization of morphology and hydration products of high-volume fly ash paste by monochromatic scanning x-ray micro-diffraction (μ-SXRD)

The present study focuses on identification and micro-structural characterization of the hydration products formed in high-volume fly ash (HVFA)/portland cement (PC) systems using monochromatic scanning x-ray micro-diffraction (μ-SXRD) and SEM-EDS. Pastes with up to 80% fly ash replacement were studied. Phase maps for HVFA samples using μ-SXRD patterns prove that μ-SXRD is an effective method to identify and visualize the distribution of phases in the matrix. μ-SXRD and SEM-EDS analysis shows that the C-S-H formed in HVFA system containing 50% or more of fly ash has a similar structure as C-S-H(I) with comparatively lower Ca/Si ratio than the one produced in PC system. Moreover, coexistence of C-S-H(I) and strätlingite is observed in the system containing 80% of fly ash, confirming that the amount of alumina and silicate phases provided by the fly ash is a major factor for the formation of C-S-H(I) and strätlingite in HVFA system. - Highlights: • High-volume fly ash (HVFA) paste was studied by scanning x-ray micro-diffraction. • Coexistence of C-S-H(I) and strätlingite in the HVFA system is clearly shown. • The distribution of minor phases in the HVFA system is shown. • Differences between inner and outer products of fly ash are observed by SEM-EDS.

36 MATERIALS SCIENCE↗

Structural, Morphological, Raman, and Mössbauer Studies on (La{sub 0.8}Ca{sub 0.2}){sub 1−x}Bi{sub x}FeO{sub 3} (x = 0.0, 0.1, and 0.2) Compounds

(La{sub 0.8}Ca{sub 0.2}){sub 1−x}Bi{sub x}FeO{sub 3} (x = 0.0, 0.1, and 0.2) compounds were prepared by the sol-gel method, using the citric acid route. Structural and microstructural characteristics of the samples were studied by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and Raman spectroscopy. Mössbauer spectroscopy was also used for magnetic characterization and structural confirmation of X-ray data. Refinement of XRD patterns indicated that the compounds crystallize in an orthorhombic structure, Pnma space group. The SEM measurements showed that the morphology of the samples is characterized by the existence of large agglomerates, while TEM confirmed the fine particle size. Raman spectra revealed that, when increasing temperature, the level of oxygen species adsorbed at the surface of the particles increases progressively. Room temperature Mössbauer spectroscopy data revealed the existence of two octahedral magnetic sites in the structure of the compounds, which is compatible with XRD data, and a small percentage of a paramagnetic phase in the samples, which increases with Bi-content.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

System and method for adaptive range 3D scanning

A scanner system is configured for acquiring three dimensional image information of an object. The scanner includes a projector, a camera, a graphics processing device, and a processor. The projector projects one of several pre-defined patterns upon the object. The camera captures an image from the object, which is received by the processor. The processor approximates mutual information from the object and the pattern using the graphics processing device, and selects a second pattern for projecting on the object.

Rosman, Guy↗