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At least 379 records · Page 21

Low-temperature synthesis of CuFeO{sub 2} (delafossite) at 70 °C: A new process solely by precipitation and ageing

This study presents a new low temperature synthesis method to obtain pure delafossite (Cu{sup 1+}Fe{sup 3+}O{sub 2}) at a temperature of 70 °C within 24 h. For the first time delafossite is synthesized solely by precipitation and subsequent ageing process and without usage of any additives controlling the oxidation state of copper. The synthesized material, called LT-delafossite, consists of pure Cu{sup 1+}Fe{sup 3+}O{sub 2} exclusive of any side products. Rietveld analysis confirms the presence of both 3R (space group (SG): R-3m) and 2H (SG: P6{sub 3}/mmc) polytypes in LT-delafossite. Electron microscopy images show nanometer-sized hexagonal plates with a diameter <500 nm and a thickness of <30 nm. Measurements of the magnetic susceptibility from 2 K to 350 K in zero-field show one peak ∼18.5 K, which is attributed to an AFM phase transition. Zero-field-cooled magnetization data between −14 T and +14 T at 2 K revealed an s-shape form around the origin having no remanent magnetization. - Highlights: • New process: low temperature synthesis of pure CuFeO{sub 2} nanoparticles. • Synthesis at 70 °C within 24 h solely by precipitation and ageing. • Nanoparticle characterization by XRD, FTIR, SEM, ICP–OES, TEM and Mößbauer. • Special magnetic properties of nano-sized CuFeO{sub 2} synthesized at low temperatures.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Randomly Layered Superstructure of In 2 O 3 Truncated Nano-Octahedra and Its High-Pressure Behavior

This study outlines the synthesis and characterization of a unique superlattice composed of vertex-truncated indium oxide (In 2 O 3 ) nano-octahedra, along with an exploration of its response to high-pressure conditions. Here, using a bright-field transmission electron microscope (BF-TEM), we determined an average circumradius of 15.2 nm for these octahedral building blocks. The resilience and response of the superlattice to pressure variations, peaking at 18.01 GPa, were examined by employing synchrotron-based Wide-Angle X-ray Scattering (WAXS) and Small-Angle X-ray Scattering (SAXS) techniques. The WAXS data revealed no phase transitions, reinforcing the stability of the 2D superlattice comprised of random layers in alignment with a 2D p31m symmetry. Notably, the SAXS data unveiled a pressure-induced, irreversible octahedron translation and ligand interaction occurring within the random layer. Through our examination of these pressure-sensitive behaviors, we identified a distinctive translation model inherent to octahedra and observed modulation in the superlattice cell parameter induced by pressure. This research signifies a noteworthy progression in deciphering the intricate behaviors of 2D superlattices under high-pressure conditions.

36 MATERIALS SCIENCE↗

Nature and origin of matrix in the unique type 3 chondrite, Kakangari

The characteristics of the matrix of the Kakangari type-3 chondrite were investigated using high-resolution TEM and AEM. It was found that the textural and mineralogical characteristics of the fine-grained matrix of Kakangari are different from those of the other chondrite groups. Unlike the matrix phases present in the CV3 and CO3 chondrites, the matrix mineralogy of Kakangari contains clear information regarding its possible origin and thermal history. Data obtained are most consistent with an origin of Kakangari by annealing, without melting at high temperature (possibly during a chondrule-forming thermal event), of clusters or aggregates of ultrafine-grained amorphous or crystalline phases. The precursor materials were most likely to have been a mixture of nebula and presolar dust. Chondrules in Kakangari were probably formed from identical precursors to the matrix, but reached temperatures sufficiently high to produce melting.

Brearley, Adrian J.↗

TEM Cell Testing of Cable Noise Reduction Techniques from 2 MHz to 200 MHz -- Part 2

This paper presents empirical results of cable noise reduction techniques as demonstrated in a TEM cell operating with radiated fields from 2 - 200 MHz. It is the second part of a two-paper series. The first paper discussed cable types and shield connections. In this second paper, the effects of load and source resistances and chassis connections are examined. For each topic, well established theories are compared to data from a real-world physical system. Finally, recommendations for minimizing cable susceptibility (and thus cable emissions) are presented. There are numerous papers and textbooks that present theoretical analyses of cable noise reduction techniques. However, empirical data is often targeted to low frequencies (e.g. <50 KHz) or high frequencies (>100 MHz). Additionally, a comprehensive study showing the relative effects of various noise reduction techniques is needed. These include the use of dedicated return wires, twisted wiring, cable shielding, shield connections, changing load or source impedances, and implementing load- or source-to-chassis isolation. We have created an experimental setup that emulates a real-world electrical system, while still allowing us to independently vary a host of parameters. The goal of the experiment was to determine the relative effectiveness of various noise reduction techniques when the cable is in the presence of radiated emissions from 2 MHz to 200 MHz.

Bradley, Arthur T.↗

Chemical composition, microstructure, and hygroscopic properties of aerosol particles at the Zotino Tall Tower Observatory (ZOTTO), Siberia, during a summer campaign

In this study we describe the hygroscopic properties of accumulation- and coarse-mode aerosol particles sampled at the Zotino Tall Tower Observatory (ZOTTO) in Central Siberia (61° N; 89° E) from 16 to 21 June 2013. The hygroscopic growth measurements were supplemented with chemical analyses of the samples, including inorganic ions and organic/elemental carbon. In addition, the microstructure and chemical composition of aerosol particles were analyzed by X-ray micro-spectroscopy (STXM-NEXAFS) and transmission electron microscopy (TEM). A mass closure analysis indicates that organic carbon accounted for 61 and 38% of PM in the accumulation mode and coarse mode, respectively. The water soluble fraction of organic matter was estimated to be 52 and 8% of PM in these modes. Sulfate, predominantly in the form of ammoniated sulfate, was the dominant inorganic component in both size modes: ~ 34% in the accumulation vs. ~ 47% in the coarse mode. The hygroscopic growth measurements were conducted with a filter-based differential hygroscopicity analyzer (FDHA) over the range of 5–99.4% RH in the hydration and dehydration operation modes. The FDHA study indicates that both accumulation and coarse modes exhibit pronounced water uptake approximately at the same RH, starting at ~ 70%, while efflorescence occurred at different humidities, i.e., at ~ 35% RH for submicron particles vs. ~ 50% RH for supermicron particles. This ~ 15% RH difference was attributed to higher content of organic material in the submicron particles, which suppresses water release in the dehydration experiments. The kappa mass interaction model (KIM) was applied to characterize and parameterize non-ideal solution behavior and concentration-dependent water uptake by atmospheric aerosol samples in the 5–99.4% RH range. Based on KIM, the volume-based hygroscopicity parameter, &kappa; v , was calculated. The &kappa; v, ws value related to the water soluble (ws) fraction was estimated to be ~ 0.15 for the accumulation mode and ~ 0.36 for the coarse mode, respectively. The obtained &kappa; v, ws for the accumulation mode is in good agreement with earlier data reported for remote sites in the Amazon rain forest (&kappa; v &approx; 0.15) and a Colorado boreal forest (&kappa; v &approx; 0.16). We used the Zdanovskii–Stokes–Robinson (ZSR) mixing rule to predict the chemical composition dependent hygroscopicity, &kappa; v, p . The obtained &kappa; v, p values overestimate the experimental FDHA-KIM-derived &kappa; v, ws by factors of 1.8 and 1.5 for the accumulation and coarse modes, respectively. This divergence can be partly explained by incomplete dissolution of the hygroscopic inorganic compounds resulting from kinetic limitations due to a sparingly soluble organic coating. The TEM and STXM-NEXAFS results indicate that aged submicron (>300 nm) and supermicron aerosol particles possess core-shell structures with an inorganic core, and are enriched in organic carbon at the mixed particle surface. The direct FDHA kinetic studies provide a bulk diffusion coefficient of water of ~ 10 &minus;12 cm 2 s &minus;1 indicating a semi-solid state of the organic-rich phase leading to kinetic limitations of water uptake and release during hydration and dehydration cycles. Overall the present ZOTTO data set, obtained in the growing season, has revealed a strong influence of organic carbon on the hygroscopic properties of the ambient aerosols. The sparingly soluble organic coating controls hygroscopic growth, phase transitions, and microstructural rearrangement processes. The observed kinetic limitations can strongly influence the outcome of experiments performed on multi-second time scales, such as the commonly applied HTDMA (Hygroscopicity Tandem Differential Mobility Analyzer) and CCNC (Cloud Condensation Nuclei Counter) measurements.

54 ENVIRONMENTAL SCIENCES↗

Finding simplicity: unsupervised discovery of features, patterns, and order parameters via shift-invariant variational autoencoders *

Abstract Recent advances in scanning tunneling and transmission electron microscopies (STM and STEM) have allowed routine generation of large volumes of imaging data containing information on the structure and functionality of materials. The experimental data sets contain signatures of long-range phenomena such as physical order parameter fields, polarization, and strain gradients in STEM, or standing electronic waves and carrier-mediated exchange interactions in STM, all superimposed onto scanning system distortions and gradual changes of contrast due to drift and/or mis-tilt effects. Correspondingly, while the human eye can readily identify certain patterns in the images such as lattice periodicities, repeating structural elements, or microstructures, their automatic extraction and classification are highly non-trivial and universal pathways to accomplish such analyses are absent. We pose that the most distinctive elements of the patterns observed in STM and (S)TEM images are similarity and (almost-) periodicity, behaviors stemming directly from the parsimony of elementary atomic structures, superimposed on the gradual changes reflective of order parameter distributions. However, the discovery of these elements via global Fourier methods is non-trivial due to variability and lack of ideal discrete translation symmetry. To address this problem, we explore the shift-invariant variational autoencoders (shift-VAEs) that allow disentangling characteristic repeating features in the images, their variations, and shifts that inevitably occur when randomly sampling the image space. Shift-VAEs balance the uncertainty in the position of the object of interest with the uncertainty in shape reconstruction. This approach is illustrated for model 1D data, and further extended to synthetic and experimental STM and STEM 2D data. We further introduce an approach for training shift-VAEs that allows finding the latent variables that comport to known physical behavior. In this specific case, the condition is that the latent variable maps should be smooth on the length scale of the atomic lattice (as expected for physical order parameters), but other conditions can be imposed. The opportunities and limitations of the shift VAE analysis for pattern discovery are elucidated.

97 MATHEMATICS AND COMPUTING↗

Bridging the length scales on mechanical property evaluation (Final Report)

The development of small-scale mechanical testing in combination with microstructural investigation is of great interest to the nuclear materials community for both materials development and monitoring applications. Dramatically reducing the sample sizes to reduce radioactivity and obtaining mechanical properties of irradiated samples is truly intriguing. Moreover, such studies promise a range of benefits including cost reduction, fundamental insight in structure-property relationships, increased statistics on less sample material, and reinvestigation of prior irradiated and tested reactor samples while simultaneously enabling the generation of mechanical test data on ion beam irradiated materials with limited penetration depths. Small scale materials testing on sub-sized samples has been studied for several decades, though it has only been after the development of micro-testing based on Focused Ion Beam (FIB) sample manufacturing in that orders of magnitude smaller samples could really be investigated in a quantitative manner. In recent years, small scale mechanical testing techniques at a number of length scales has been developed for both unirradiated and irradiated (ion and neutron) materials. Technological advances made in this field have enabled ex-situ and in-situ transmission electron microscopy (TEM) and scanning electron microscopy (SEM) examination, thus leading to more accurate measurements as well as additional mechanistic information. A recent review of the benefits of these techniques show that these techniques are at a stage to tackle multi-scale ranges of materials investigations and can be utilized to obtain fundamental science-based understanding of nuclear materials. Considering the tremendous advances made, one can see how small-scale mechanical testing techniques combined with modeling can enable true small scale to bulk scale mechanical property correlations. However, for the engineering community to adapt this approach fully, one needs to demonstrate that a) that these techniques can produce results with high fidelity and reproducibility, b) generate engineering stress-strain data that one can utilize to understand bulk behavior, and c) generate new insight into relevant phenomena fostering the true understanding of radiation damage and microstructure in materials for nuclear applications. It is the objective of this proposal to bridge the length scale between macro- and micro- scale mechanical testing of unirradiated and irradiated materials. This involves the development and demonstration of procedures for multi-scale mechanical testing that enable high fidelity reproducibility of data and the generation bulk property data from small-scale mechanical tests. Through this, the proposal aims to enhance the confidence in the obtained data at the smaller length scales and enhance the insight provided from these techniques for bulk scale applications on both unirradiated and irradiated materials.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

A facile approach towards synthesis, characterization, single crystal structure, and DFT study of 5-bromosalicylalcohol

5-Bromosalicylalcohol was prepared by the interaction of NaBH{sub 4} and 5-bromosalicylaldehyde. The use of sodium borohydride makes the reaction easy, facile, economic and does not require any toxic catalyst. The compound is characterized by FTIR, {sup 1}H NMR, {sup 13}C NMR, TEM and ESI-mass spectra. Crystal structure is determined by single crystal X-ray analysis. Quantum mechanical calculations of geometries, energies and thermodynamic parameters are carried out using density functional theory (DFT/B3LYP) method with 6-311G(d,p) basis set. The optimized geometrical parameters obtained by B3LYP method show good agreement with experimental data.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Feasibility study of a high spatial and time resolution beam emission spectroscopy diagnostic for localized density fluctuation measurements in Lithium Tokamak eXperiment-β (LTX-β)

Trapped electron mode (TEM) is the main source of turbulence predicted for the unique operation regime of a flat temperature profile under low-recycling conditions in the LTX-β tokamak, while ion temperature gradient driven turbulence may also occur with gas fueling from the edge. To investigate mainly TEM scale density fluctuations, a high spatial and time resolution 2D beam emission spectroscopy (BES) diagnostic is being developed. Apart from spatially localized density turbulence measurement, BES can provide turbulence flow and flow shear dynamics. This BES system will be realized using an avalanche photodiode-based camera and narrow band interference filter. The system can acquire data at 2 MHz. Simulations with the Simulation of Spectra (SOS) code indicate that a high signal to noise ratio can be achieved with the proposed system. This will enable sampling the density fluctuations at this high time resolution. Finally, the design considerations and system optimization using the SOS code are presented.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Diffusion processes in Al2O3 scales - Void growth, grain growth, and scale growth

The internal microstructure and growth kinetics of Al2O3 scales on Ni-15Cr-13Al (wt percent) are investigated by TEM and analyzed in relation to models of diffusivity. Polished arc-melted specimens were oxidized in 1-atm air at 1100 C for 0.1, 1.0, and 20 hours and ion-thinned for TEM at 100 kV. The frequency distribution of void size and grain size is determined for different oxidation times and scale depths. The kinetics of microvoid growth and of grain and scale growth are plotted and related via simplified models to lattice and grain-boundary oxygen diffusivity, respectively. Good agreement is found between model predictions and data obtained by Oishi and Kingery (1960) on oxygen diffusion in bulk Al2O3. The further implications and limitations of these findings are discssed.

Smialek, J. L.↗

NanoPSD: A software for automatic detection of Nano-Particle Shape Distribution in electron microscopy images

Accurate quantification of the size and morphology of nanoparticles from electron microscopy (EM) images is essential to understand growth mechanisms, surface reactivity, and functional behavior in nanoscale materials. Manual analysis remains slow, subjective, and difficult to reproduce in large datasets. We introduce NanoPSD (Nano-Particle Shape Distribution), an open-source and fully automated framework for quantitative particle detection and morphology analysis from EM images. NanoPSD integrates adaptive contrast enhancement, polarity-agnostic scale-bar detection, Optical Character Recognition (OCR)-based calibration, and classical segmentation via Otsu thresholding with morphological refinement. Particle contours are used to extract geometric descriptors, including equivalent circular diameter, aspect ratio, circularity, and solidity, enabling automated classification into spherical, rod-like, and aggregate morphologies. The framework supports both single-image and batch processing, generating publication-quality visualizations, LaTeX-ready tables, and structured comma-separated values (CSV) datasets. As a demonstration, we applied NanoPSD to plasma-synthesized nanoparticle samples diagnosed via transmission electron microscopy (TEM). The code produced statistically robust size and morphology distributions spanning a few to tens of nanometers with minimal user supervision. The pipeline demonstrates high reproducibility and scalability, processing large image collections with consistent calibration and output formatting. Its modular design enables seamless integration of future deep-learning-based segmentation models, providing a pathway toward intelligent, data-driven electron microscopy analysis.

36 MATERIALS SCIENCE↗

Molecular Weight Dependence of Methylcellulose Fibrillar Networks

Gelation of aqueous methylcellulose (MC) solutions upon heating has been shown to result from the formation of a network of semiflexible fibrils, with diameters of 15 ± 2 nm. Here, we investigate the impact of MC molecular weight on the elasticity and structure of aqueous gels at concentrations between 0.1 and 3 wt %. Small-amplitude oscillatory shear measurements conducted at a fixed concentration reveal that the gel modulus increases monotonically by a factor of 5 for weight-average molecular weights (M w ) between 22 and 550 kg/mol. Small-angle X-ray scattering data, fit to a semiflexible cylinder model, demonstrate that the fibril radius, Kuhn length, and volume fraction are approximately constant throughout this molecular weight range. Small-angle light scattering shows that the fibrillar-rich and fibrillar-depleted domains within the gel are associated with an essentially invariant heterogeneity correlation length. Direct visualization by cryo-TEM reveals that lower molecular weight MC forms fibrils of lower average length. The distribution of fibril lengths measured by cryo-TEM and the distribution of the polymer chain contour lengths are similar, especially for shorter chains, and these features are correlated to network connectivity. We propose that the underlying fibril structure consists of bundles of polymer chains with a preferred orientation coincident with the fibril axis, while the fibril diameter is controlled by a circumferential helical pitch associated with the single chain Kuhn length and interactions between chains.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Coupling of ion temperature gradient and trapped electron modes in the presence of impurities in tokamak plasmas

The coupling of ion temperature gradient (ITG or η{sub i}) mode and trapped electron mode (TEM) in the presence of impurity ions is numerically investigated in toroidal collisionless plasmas, using the gyrokinetic integral eigenmode equation. A framework for excitations of the ITG modes and TEMs with respect to their driving sources is formulated first, and then the roles of impurity ions played in are analyzed comprehensively. In particular, the characteristics of the ITG and TEM instabilities in the presence of impurity ions are emphasized for both strong and weak coupling (hybrid and coexistent) cases. It is found that the impurity ions with inwardly (outwardly) peaked density profiles have stabilizing (destabilizing) effects on the hybrid (namely the TE-ITG) modes in consistence with previous works. A new finding of this work is that the impurity ions have stabilizing effects on TEMs in small η{sub i} (η{sub i}≤1) regime regardless of peaking directions of their density profiles whereas the impurity ions with density gradient L{sub ez}=L{sub ne}/L{sub nz}>1 (L{sub ez}<1) destabilize (stabilize) the TEMs in large η{sub i} (η{sub i}≥1) regime. In addition, the dependences of the growth rate, real frequency, eigenmode structure, and wave spectrum on charge concentration, charge number, and mass of impurity ions are analyzed in detail. The necessity for taking impurity ion effects on the features of turbulence into account in future transport experimental data analyses is also discussed.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Microstructural Evolution of NF709 Steel under In-situ Ion Irradiations at Room Temperature to 600 deg. C

NF709 is one of the advanced austenitic stainless steels considered for the advanced reactor systems which are characterized by high temperature, intense radiation and potentially corrosive environments. NF709 is a nitrogen-stabilized and niobium-strengthened alloy, and it provides strength nearly double that for conventional 304 and 316 stainless steels at a temperature range of 600-750 deg. C. In addition, this alloy demonstrates excellent metallurgical stability and high-temperature creep resistance, which is critical for advanced fast-reactor structural materials. Nevertheless, there is very limited irradiation data on NF709 to date, and its radiation-resistance is to be proved. It this paper, we studied the radiation response of NF709 by using the in-situ ion irradiation at the Intermediate Voltage Electron Microscopy (IVEM)- Tandem Facility, located at Argonne National Lab (ANL) and the systematic post-irradiation characterizations using transmission electron microscopy (TEM) were conducted.

36 MATERIALS SCIENCE↗

Characterizing the Three-Dimensional Structure of Block Copolymers via Sequential Infiltration Synthesis and Scanning Transmission Electron Tomography

Understanding and controlling the three-dimensional structure of block copolymer (BCP) thin films is critical for utilizing these materials for sub-20 nm nanopatterning in semiconductor devices, as well as in membranes and solar cell applications. Combining an atomic layer deposition (ALD) based technique for enhancing the contrast of BCPs in transmission electron microscopy (TEM) together with scanning TEM (STEM) tomography reveals and characterizes the three-dimensional structures of poly(styrene-block-methyl methacrylate) (PS-b-PMMA) thin films with great clarity. Sequential infiltration synthesis (SIS), a block-selective technique for growing inorganic materials in BCPs films in ALD, and an emerging tool for enhancing the etch contrast of BCPs, was harnessed to significantly enhance the high-angle scattering from the polar domains of BCP films in the TEM. The power of combining SIS and STEM tomography for three dimensional (3D) characterization of BCPs films was demonstrated with the following cases: self-assembled cylindrical, lamellar, and spherical PS-PMMA thin films. In all cases, STEM tomography has revealed 3D structures that were hidden underneath the surface, including: 1) the 3D structure of defects in cylindrical and lamellar phases, 2) non-perpendicular 3D surface of grain boundaries in the cylindrical phase, and 3) the 3D arrangement of spheres in body centered cubic (BCC) and hexagonal closed pack (HCP) morphologies in the spherical phase. The 3D data of the spherical morphologies was compared to coarse-grained simulations and assisted in validating the simulations’ parameters. STEM tomography of SIS-treated BCP films enables the characterization of the exact structure used for pattern transfer, and can lead to better understating of the physics which is utilized in BCP lithography.

Block copolymers↗

Investigating Processes of Nanocrystal Formation and Transformation via Liquid Cell TEM

Recent ex situ observations of crystallization in both natural and synthetic systems indicate that the classical models of nucleation and growth are inaccurate. However, in situ observations that can provide direct evidence for alternative models have been lacking due to the limited temporal and spatial resolution of experimental techniques that can observe dynamic processes in a bulk solution. Here we report results from liquid cell transmission electron microscopy studies of nucleation and growth of Au, CaCO3, and iron oxide nanoparticles. We show how these in situ data can be used to obtain direct evidence for the mechanisms underlying nanoparticle crystallization as well as dynamic information that provide constraints on important energetic parameters not available through ex situ methods.

Nielsen, Michael H.↗

Characterization and adsorption performance of Pb(II) on CuO nanorods synthesized by the hydrothermal method

Highlights: • The nanorods of CuO were synthesized by a hydrothermal route without any surfactant. • X-ray diffraction showed monoclinic structure with space group C{sub 2/c}. • The nanorods show relatively high adsorption capacity for the removal of Pb(II). • The adsorption kinetics could be fitted well by the pseudo-second-order model. • The equilibrium data can be fitted well using the Langmuir isotherm model - Abstract: Copper oxide (CuO) nanorods were synthesized by hydrothermal method. The detailed structural, compositional and optical characterization of this material was also evaluated with XRD, FT-IR, EDS, and UV–vis spectroscopy, which confirmed that the obtained nanorods are well-crystallized CuO and possess good optical properties. SEM and TEM studies revealed that the as-synthesized CuO nanorods are uniform with an average diameter of 17 nm. The adsorption activity of the CuO nanostructures was studied. The adsorption results showed that the CuO nanorods are an effective and efficient adsorbent for the removal of Pb(II) ions. The influence of various operational parameters such as the pH of the solution, the contact time and the initial concentrations were also studied and the results were discussed. The estimated maximum lead ion adsorption capacity of the CuO nanorods was found to be 188.67 mg g{sup −1} at an optimum pH of 6.

36 MATERIALS SCIENCE↗