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At least 199 records · Page 11

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DOE OSTI2022

Dual-scale folding in cutting of commercially pure aluminum alloys

We examine a, hitherto, little-studied and curious machining chip morphology, with tell-tale signs of folding at two different length scales, that is common in cutting of certain ductile and highly strain-hardening metals like soft aluminum alloys, tantalum and niobium. This chip morphology does not appear in the usual catalogues of common chip types. The mechanics of formation of the “dual-scale folded chip” is studied in model material systems of commercially pure aluminum alloys (AA 1100 and AA 8040), that prominently exhibit this chip morphology. The flow, folding and associated plastic instabilities are investigated using micro/macro structure observations of the chip in a plane-strain cutting framework, with high-speed in situ imaging and image analysis of material flow; and force measurements. The smaller-scale folding is shown to develop in the primary deformation zone while the larger-scale folding occurs as the chip traverses the rake face of the tool. The resulting chip is composed of irregularly-spaced large folds, superimposed onto which are the quasi periodic small folds. The representative wavelengths of the two folds differ on average by an order of magnitude, 0.1 mm vs. 2 mm. The observations reveal a direct coupling between the material flow and chip morphology, and how specific attributes of the dual-scale folded chip arise from the flow mechanism. Plastic buckling is found to play a key role in the folding at both length scales. The small-scale folds are characteristic of a sinuous plastic flow mode, while the large-scale folding is characterized by buckling and stick-slip along the tool rake face, triggered by adhesive pinning of the chip to the tool. Important consequences of the dualscale folding are very large cutting forces, and force oscillations of large amplitude, despite the alloys being very soft, only ~ 25 HV. Here, the dual-scale folding is why many of these alloys are classified as “gummy” to machine. Since the dual-scale folded chip is associated with large cutting forces and poor surface quality, there is much to be gained by disrupting this flow type in practical machining applications. Methods for controlling the folding to improve machining performance with the gummy alloys are briefly discussed.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Strengthening Mechanisms and Deformation Behavior of Industrially-Cast and Lab-Cast Dual-Phase High Entropy Alloy

An iron-rich high entropy alloy Al 0.65 CoCrFe 2 Ni comprising of both FCC and BCC phases was designed and fabricated using induction melting at a large industrial scale and suction casting at a small lab scale. Spinodally decomposed interdendritic regions were uniformly distributed in the industrially melted alloy, and a finer dendritic structure with smaller sized spinodal structures was observed in the alloy suction cast at lab scale. The suction cast alloy fabricated at the lab scale exhibited significantly higher compressive yield strength compared to the industrially cast alloy. The relative strengthening contributions in the alloys due to solid solution, grain boundary, dislocation interactions and interphase boundary were analyzed. Dislocation hardening was the major contributor responsible for the higher strength of the SC alloy. The deformation behavior in the alloys was examined with the help of orientation image mapping. Finally, intense slip band formation at large strains in the industrially melted alloy indicates that cold working can be an effective technique to enhance the strength of the dual-phase high entropy alloy processed at a large scale.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Spatially co-registered wide-field nonlinear optical imaging of living and complex biosystems in a total internal reflection geometry

Nonlinear optical microscopy that leverages an objective based total internal reflection (TIR) excitation scheme is an attractive means for rapid, wide-field imaging with enhanced surface sensitivity. Through select combinations of distinct modalities, one can, in principle, access complementary chemical and structural information for various chemical species near interfaces. Here, we report a successful implementation of such a wide-field nonlinear optical microscope system, which combines coherent anti-Stokes Raman scattering (CARS), two-photon fluorescence (TPF), second harmonic generation (SHG), and sum frequency generation (SFG) modalities on the same platform. The intense optical fields needed to drive these high order nonlinear optical processes are achieved through the use of femtosecond pulsed light in combination with the intrinsic field confinement induced by TIR over a large field of view. The performance of our multimodal microscope was first assessed through the experimental determination of its chemical fidelity, intensity and polarization dependences, and spatial resolution using a set of well-defined model systems. Subsequently, its unique capabilities were validated through imaging complex biological systems, including Hydrangea quercifolia pollen grains and Pantoea sp. YR343 bacterial cells. Specifically, the spatial distribution of different molecular groups in the former was visualized via vibrational contrast mechanisms of CARS, whereas co-registered TPF imaging allowed the identification of spatially localized intrinsic fluorophores. We further demonstrate the feasibility of our microscope for wide-field CARS imaging on live cells through independent characterization of cell viability using spatially co-registered TPF imaging. Overall, this approach to TIR enabled wide-field imaging is expected to provide new insights into bacterial strains and their interactions with other species in the rhizosphere in a time-resolved and chemically selective manner.

47 OTHER INSTRUMENTATION↗

DOE OSTI2022

Nonnuclear Experimental Capabilities to Support Design, Development, and Demonstration of Microreactors

This work provides a summary of selected experimental capabilities being developed to support nonnuclear testing and demonstration of technology in support of microreactors under the U.S. Department of Energy’s (DOE’s) Microreactor Program. Major capabilities include the Single Primary Heat Extraction and Removal Emulator (SPHERE) and the Microreactor Agile Non-nuclear Experimental Test Bed (MAGNET). The SPHERE facility allows for controlled testing of the steady-state and transient heat rejection capabilities of a single heat pipe using electrical heaters that simulate nuclear heating. The facility is capable of monitoring axial temperature profiles along the heat pipe and surrounding test articles during startup, steady-state operation, and transients. Instrumentation includes noncontact infrared thermal imaging, surface thermocouples, spatially distributed fiber optic temperature and strain sensors, electrical power meters, and a water-cooled, gas-gap calorimeter for quantifying heat rejection from the heat pipe. The facility can be operated under both vacuum and inert-gas conditions. The MAGNET facility is a large-scale, 250-kW electrically heated microreactor test bed to enable nonnuclear experimental evaluation of a variety of microreactor concepts. It can be supplied to electrically heat a scaled section of a microreactor and further test the capabilities of heat rejection systems. The initial MAGNET experiments will support technology maturation and reduce uncertainty and risk associated with the design, operation, and deployment of monolithic heat pipe–based reactors. However, this test bed can broadly be applied to multiple microreactor concepts to evaluate a wide range of thermal-hydraulic and structural phenomena such as interface coupling with power conversion units and other collocated systems. MAGNET can evaluate integral thermomechanical effects during electrical heating of an array of heat pipes in a larger test article. Examples of initial testing will include thermal stresses in the monolith and the impact of debonding of a heat pipe from the core block and how that failure could impact surrounding heat pipes, i.e., understanding the potential for cascading failure. This work also discusses some modeling capabilities that can support experiment design, analysis, and interpretation, including the heat pipe code Sockeye and a comparison of thermal-structural simulations performed using ABAQUS and STAR-CCM+.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

DOE OSTI2020

Effects of surface undulations on asymmetric X-ray diffraction: a rocking-curve topography study

The results are reported of an X-ray diffraction study of an Si crystal designed and fabricated for very asymmetric diffraction from the 333 reflection for X-ray energies of 8.100 and 8.200 keV. A crystal with an asymmetry angle of 46 ± 0.1° between the surface and the (111) planes was studied. The grazing angles of incidence were near 1.08 and 0.33° for these two energies, respectively. Features arising from surface undulations were not observed at 8.100 keV, but were observed at 8.200 keV. The results at 8.100 keV allow an alternative explanation based on strain near the surface to be ruled out. Topographic images were obtained as a function of rocking angle, and in the case of 8.200 keV the surface morphology is evident. Finally, the results are found to be in agreement with dynamical X-ray diffraction calculations made with the Takagi–Taupin equations specialized to a surface having convex or concave features, as reported in the accompanying paper [Macrander (2020). J. Appl. Cryst. 53 , 793–799].

36 MATERIALS SCIENCE↗

DOE OSTI2020

System and method for testing true stress and true strain

A true stress testing system broadly comprising a force input machine, an imaging system, and a computer. The imaging system includes a light source for projecting a light beam at the specimen in a first direction and a camera positioned on an opposite side of the specimen for receiving portions of the light beam not blocked by the specimen such that a shadow image of the specimen is created via the camera. The computer may determine a minimum dimension of the specimen perpendicular to the first direction at a point in time over a plurality of points along the force axis via the shadow image of the specimen such that the processor accounts for changes in position of the minimum dimension along the specimen. A true stress of the specimen may then be determined according to the minimum dimension of the specimen perpendicular to the first direction at the point in time.

42 ENGINEERING↗

DOE OSTI2023

Neutron Imaging of Al6061 Prepared by Solid-State Friction Stir Additive Manufacturing

Solid-state Friction Stir Additive Manufacturing has recently gained attention as a result of its capacity to fabricate large-scale parts while preserving the mechanical properties of the feedstock material. However, the correlation between the quality of layer-by-layer bonding of the deposited metal and processing parameters has remained unknown. Neutron imaging techniques, with 90% total transmission per cm, are employed for Al6061 parts fabricated by MELD ® Technology as a non-destructive evaluation approach for the first time to investigate the layer-by-layer structure of a stadium-shaped ingot in different sections. The post-processed results show the fabricated parts with an optimized set of processing parameters are void-free. However, the hydrocarbon-based feedstock lubricant segregates between the layers, which consequently may lead to non-uniform weaker mechanical properties along the build direction and stimulate crack initiation during mechanical loading. The tensile test results show 14% lower strain-to-failure values in alleged contaminated areas in transmission imaging results. Additionally, layer bonding is significantly impacted by hot-on-hot and hot-on-cold layer deposition schemes, especially for larger layer thicknesses.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Single-colony MALDI mass spectrometry imaging reveals spatial differences in metabolite abundance between natural and cultured Trichodesmium morphotypes

Trichodesmium, a globally significant N 2 -fixing marine cyanobacterium, forms extensive surface blooms in nutrient-poor ocean regions. These blooms consist of a dynamic assemblage of Trichodesmium species that form distinct colony morphotypes and are inhabited by diverse microorganisms. Trichodesmium colony morphotypes vary in ecological niche, nutrient uptake, and organic molecule release, differentially impacting ocean carbon and nitrogen biogeochemical cycles. Here, we assessed the poorly studied spatial abundance of metabolites within and between three morphologically distinct Trichodesmium colonies collected from the Red Sea. We also compared these results with two morphotypes of the cultivable Trichodesmium strain IMS101. Using matrix-assisted laser desorption/ionization (MALDI) mass spectrometry imaging (MSI) coupled with liquid extraction surface analysis (LESA) tandem mass spectrometry (MS2), we identified and localized a wide range of small metabolites associated with single-colony Trichodesmium morphotypes. Our untargeted MALDI-MSI approach revealed 80 unique features (metabolites) shared between Trichodesmium morphotypes. Discrimination analysis showed spatial variations in 57 shared metabolites, accounting for 62% of the observed variation between morphotypes. The greatest variations in metabolite abundance were observed between the cultured morphotypes compared to the natural colony morphotypes, suggesting substantial differences in metabolite production between the cultivable strain IMS101 and the naturally occurring colony morphotypes that the cultivable strain is meant to represent. This study highlights the variations in metabolite abundance between natural and cultured Trichodesmium morphotypes and provides valuable insights into metabolites common to morphologically distinct Trichodesmium colonies, offering a foundation for future targeted metabolomic investigations.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2020

The effect of microstructure on the relationship between grain boundary sliding and slip transmission in high purity aluminum

The relationship between grain boundary sliding (GBS) and slip transmission is investigated experimentally at grain boundaries in 99.99% aluminum with a through-thickness, coarse grained microstructure deformed in tension at 190 °C. Using scanning electron microscope enabled digital image correlation (SEM-DIC) and electron backscatter diffraction (EBSD), high resolution strain fields and microstructural information were measured to examine the influence of microstructural neighborhoods on interactions between GBS and slip transmission and strain localization. Several distinct cases are presented that highlight important microstructural factors that govern deformation near grain boundaries. The findings include (1) direct transmission and GBS were anti-compatible and facilitated by opposing boundary types (low misorientation and high energy grain boundaries respectively); (2) increased GBS activity was correlated with decreased indirect transmission behavior; (3) GBS accommodation at triple junctions was enabled by intragranular plasticity; and (4) the local intragranular plastic strain discontinuity between grains determined the magnitude of GBS gradients. Finally, this work provides insight into the nature of these mechanisms and can be used to identify strain transfer criteria that can lead to improved GBS-sensitive crystal plasticity models.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Uncovering the three-dimensional structure of upconverting core–shell nanoparticles with multislice electron ptychography

In photon upconverting core–shell nanoparticles, structure strongly dictates performance. Typical imaging in scanning transmission electron microscopy has sufficient resolution to probe the atomic structure of these nanoparticles, but contrast, dose, and projection limitations make conventional methods insufficient for fully characterizing these structures. Phase retrieval techniques provide a promising alternative imaging mode, and, in particular, multislice electron ptychography can recover depth-dependent information. Here, we study beam-sensitive photon upconverting core–shell nanoparticles with a multislice ptychography approach using a low electron dose to avoid damage. Large strain fields arise in these heterostructures due to the mismatch in lattice parameter between the core and the shell. We reconstruct both a nanoparticle that appears defect-free and one that has a large break in the side and map the distribution of strain in 3D by computing distortion fields from high-resolution potential images of each slice. In the defect-free nanoparticle, we observe twisting of the shell, while in the broken nanoparticle, we measure the 3D position of the crack, the core, and dislocations. These results highlight the advantage of multislice electron ptychography to recover 3D information from a single scan, even under strict electron dose requirements from beam-sensitive samples.

74 ATOMIC AND MOLECULAR PHYSICS↗

DOE OSTI2022

Influence of strain and dislocations on GaSb/GaAs quantum dots: From nested to staggered band alignment

We investigate the influence of strain and dislocations on band alignment in GaSb/GaAs quantum dot systems. Composition profiles from cross-sectional scanning tunneling microscopy images are interpolated onto a finite element mesh in order to calculate the distribution of local elastic strain, which is converted to a spatially varying band alignment using deformation potential theory. Our calculations predict that dislocation-induced strain relaxation and charging lead to significant local variations in band alignment. Furthermore, misfit strain induces a transition from a nested (type I) to a staggered (type II) band alignment. Although dislocation-induced strain relaxation prevents the type I to type II transition, electrostatic charging at dislocations induces the staggered band alignment once again.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2026

Adaptively coupled phase retrieval in multi-peak Bragg coherent diffraction imaging

Recent advances in Bragg coherent diffraction imaging (BCDI) experimental techniques permit routine measurement of multiple Bragg peaks from a single crystalline grain. The resulting images contain the full lattice distortion vector field which can be differentiated to provide lattice strain and rotation. With the advent of fourth-generation synchrotron light sources, such multi-peak datasets are produced at high rates, facilitating the need for rapid phase retrieval of the multiple peaks and subsequent image analysis. Here we describe and demonstrate a new implementation of a coupled phase retrieval technique for multi-peak BCDI which simultaneously treats each Bragg peak of the dataset and produces a three-dimensional image of the crystal's morphology and lattice distortion field. In addition, this method uses the redundant information contained in the various Bragg diffraction patterns to detect and suppress spurious signal appearing on the detector in a subset of the measurements. Compared with manual data editing, adaptive coupling produces a more consistent phase profile in reciprocal space and sharper surfaces in direct space, with no significant difference in computational cost. These improvements reduce the need for manual preprocessing and enable robust high-throughput analysis of multi-peak BCDI data, supporting near-real-time strain microscopy at modern synchrotron facilities.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Experimental and theoretical study of the restrained shrinkage cracking of early age well cement

The shrinkage cracking occurring in oil & gas well cement material is a major factor that reduces the cement sheath integrity and impairs the durability of an underground well. Shrinkage mainly takes place in the early hydration period of the cement, and the resulting restrained shrinkage cracking can form a leaking network for oil & gas or carbon dioxide stored in an underground reservoir. It is thus important to understand the early age behavior of well cement and the leaking pathway formation in the well. This study describes the application of the digital image correlation (DIC) method as a tool to measure the strain development and crack distributions of well cement in the lab during early phase changes. A theoretical model is presented to calculate the stress distribution built up in the cement sheath during early ages of well cement hydration, which helps to interpret the experimental observations and determine the major factors influencing the cracking sequences. This study presents the whole hydration – drying shrinkage – and cracking mechanism of early age well cement under restrained ring conditions experimentally and theoretically. Finally, the results offer useful insights on the key material and geometric parameters which control the fracture of a well cementing structure.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Strain-Induced asymmetry and on-site dynamics of silicon defects in graphene

In the last decade, the atomically-focused electron beams utilized in scanning transmission electron microscopes (STEMs) have been shown to induce a broad set of local structural transformations in materials, opening pathways for directing material synthesis and modification atom-by-atom. The mechanisms underlying these transformations remain largely unknown, due to the intractability of modeling the myriad of reaction pathways that can be accessed through high-energy electron scattering. The information on materials’ structure and dynamics that can be extracted from STEM images is similarly left underexplored. Here, we report the observation of anomalous on-site dynamics of individual silicon impurity atoms in graphene during STEM imaging. Density functional theory-based structural optimizations of anisotropically-strained molecular nanographenes reveal two distinct (but nearly degenerate) stable structures for four-fold coordinated silicon impurities, where interconversion between the two structures manifests slight changes of the silicon position within the lattice site. Implications for defect-based strain engineering in graphene are discussed.

36 MATERIALS SCIENCE↗

DOE OSTI2021

In-Situ SEM High Strain Rate Testing of Large Diameter Micropillars Followed by TEM and EBSD Postmortem Analysis

Background Dislocation dynamic simulations are intended as a tool to understand and predict the mechanical behavior of metallic materials, but its prediction has never been directly verified by experiments due to differences in specimen strain rate and size. Objective In this work, a comprehensive experimental framework is proposed to attempt direct comparison between experiments and discrete dislocation dynamics (DDD) modelling. Methods By integrating high-throughput sample fabrication and a customized testing apparatus, the sample size and strain rate typically employed in DDD simulations are explored experimentally. Constitutive properties such as stress-strain response are measured, and microstructural information is obtained from transmission electron microscopy (TEM) imaging, electron backscatter diffraction (EBSD), and TEM-based orientation mapping. Results Magnesium and copper were selected, as case studies, to demonstrate the newly developed experimental procedure. Measured stress-strain responses for Mg are consistent with those obtained with a miniaturized Hopkison bar experiments. Furthermore, by exploiting the validated workflow, the effect of strain rate on micropillar heterogeneous deformation and associated dislocation plasticity were revealed. Conclusion The work establishes a methodology for the systematic study of not only metals but also other materials and structures at the microscale and high strain rates.

42 ENGINEERING↗

DOE OSTI2023

A MHz X-ray diffraction set-up for dynamic compression experiments in the diamond anvil cell

An experimental platform for dynamic diamond anvil cell (dDAC) research has been developed at the High Energy Density (HED) Instrument at the European X-ray Free Electron Laser (European XFEL). Advantage was taken of the high repetition rate of the European XFEL (up to 4.5 MHz) to collect pulse-resolved MHz X-ray diffraction data from samples as they are dynamically compressed at intermediate strain rates (≤10 3 s −1 ), where up to 352 diffraction images can be collected from a single pulse train. The set-up employs piezo-driven dDACs capable of compressing samples in ≥340 µs, compatible with the maximum length of the pulse train (550 µs). Results from rapid compression experiments on a wide range of sample systems with different X-ray scattering powers are presented. A maximum compression rate of 87 TPa s −1 was observed during the fast compression of Au, while a strain rate of ∼1100 s −1 was achieved during the rapid compression of N 2 at 23 TPa s −1 .

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

DOE OSTI2020

Complete Strain Mapping of Nanosheets of Tantalum Disulfide

Quasi-two-dimensional (quasi-2D) materials hold promise for future electronics because of their unique band structuresthat result in electronic and mechanical properties sensitive to crystal strains in all three dimensions. Quantifying crystal strain is a prerequisite to correlating it with the performance of the device, and calls for high resolution but spatially resolved rapid characterization methods. Here we show that using fly-scan nano X-ray diffraction we can accomplish a tensile strain sensitivity below 0.001% with a spatial resolution of better than 80 nm over a spatial extent of 100 µm on quasi 2D flakes of 1T-TaS2. Coherent diffraction patterns were collected from a ~100 nm thick sheet of 1T-TaS2 by scanning 12keV focused X-ray beam across and rotating the sample. We demonstrate that the strain distribution around micron and sub-micron sized ‘bubbles’ that are present in the sample may be reconstructed from these images. The experiments use state of the art synchrotron instrumentation, and will allow rapid and non-intrusive strain mapping of thin film samples and electronic devices based on quasi 2D materials.

nano X-ray diffraction↗

DOE OSTI2023

Strain and crystallographic identification of the helically concaved gap surfaces of chiral nanoparticles

Identifying the three-dimensional (3D) crystal plane and strain-field distributions of nanocrystals is essential for optical, catalytic, and electronic applications. However, it remains a challenge to image concave surfaces of nanoparticles. Here, we develop a methodology for visualizing the 3D information of chiral gold nanoparticles ≈ 200 nm in size with concave gap structures by Bragg coherent X-ray diffraction imaging. The distribution of the high-Miller-index planes constituting the concave chiral gap is precisely determined. The highly strained region adjacent to the chiral gaps is resolved, which was correlated to the 432-symmetric morphology of the nanoparticles and its corresponding plasmonic properties are numerically predicted from the atomically defined structures. This approach can serve as a comprehensive characterization platform for visualizing the 3D crystallographic and strain distributions of nanoparticles with a few hundred nanometers, especially for applications where structural complexity and local heterogeneity are major determinants, as exemplified in plasmonics.

36 MATERIALS SCIENCE↗