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DOE OSTI2020

High Compression‐Induced Conductivity in a Layered Cu–Br Perovskite

Abstract We show that the onset pressure for appreciable conductivity in layered copper‐halide perovskites can decrease by ca. 50 GPa upon replacement of Cl with Br. Layered Cu–Cl perovskites require pressures >50 GPa to show a conductivity of 10 −4 S cm −1 , whereas here a Cu–Br congener, (EA) 2 CuBr 4 (EA=ethylammonium), exhibits conductivity as high as 2×10 −3 S cm −1 at only 2.6 GPa, and 0.17 S cm −1 at 59 GPa. Substitution of higher‐energy Br 4p for Cl 3p orbitals lowers the charge‐transfer band gap of the perovskite by 0.9 eV. This 1.7 eV band gap decreases to 0.3 eV at 65 GPa. High‐pressure X‐ray diffraction, optical absorption, and transport measurements, and density functional theory calculations allow us to track compression‐induced structural and electronic changes. The notable enhancement of the Br perovskite's electronic response to pressure may be attributed to more diffuse Br valence orbitals relative to Cl orbitals. This work brings the compression‐induced conductivity of Cu‐halide perovskites to more technologically accessible pressures.

Jaffe, Adam↗

DOE OSTI2026

Self‐Limiting Polymerization‐Induced Crystallization‐Driven Self‐Assembly (SL‐PI‐CDSA) Enables Templated Synthesis of Chiral Plasmonic, Hybrid 2D Hexagonal Assemblies

Examples of self-regulating synthetic self-assembly are relatively few, with most known chemical systems relying on kinetic rather than thermodynamic control. Herein, we demonstrate the rapid generation (t ≤ 5 min) of size-tunable ultralow dispersity (Ð ≤ 1.01) 2D hexagonal nanosheets governed by self-limiting self-assembly (SLSA). Self-assembly in natural systems occurs with exquisite control of structure, function, and dimension. We demonstrate that key aspects of biological assembly can be rationally applied toward the development of bottom-up approaches for the construction of chiral nanomaterials. To this end, self-limiting polymerization-induced crystallization-driven self-assembly (SL-PI-CDSA) of modular and templating aryl isocyanide (AIC) monomers yields functional 2D assemblies permitting post-polymerization/assembly modifications. Detailed study of the internal and external structure of the hexagonal nanosheets reveals topological defects which offer mechanistic insights into both their assembly and subsequent utilization. Specifically, these features enable fabrication of chiral hybrid organic–inorganic nanomaterials incorporating chiral plasmonic metal nanoparticles (MNPs). Our results suggest that the synergistic interplay of template-driven confinement and hierarchical chirality induce symmetry breaking of in situ-generated gold MNPs. We anticipate that the platform presented will facilitate fabrication of new hybrid, chiral organic–inorganic nanostructures.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Relationship between microstructure evolution and properties enhancement of carbon nanotubes‐filled polybutylene terephthalate/polypropylene blends induced by thermal annealing

Abstract Thermal annealing induced microstructure evolution and properties enhancement of polybutylene terephthalate/polypropylene/carbon nanotubes (PBT/PP/CNTs) nanocomposites was methodically investigated. The electrical conductive PBT/PP/CNTs nanocomposites with a low percolation threshold were obtained by simple melt blending due to the selective location of the CNTs in PBT phase and the formation of the double percolation structure. Thermal annealing further remarkably decreased the volume resistivity of the nanocomposites, with the maximum reduction of seven orders of magnitude. Scanning electron microscope observation and rheology tests demonstrated that the relatively large CNTs agglomerates were redistributed to build more homogeneous CNTs networks after annealing. The phase coalescence during annealing promoted the formation of the more perfect co‐continuous structure. These phenomena helped to enhance the electrical conductivity of the nanocomposites. Flexural properties of the nanocomposites were also enhanced after annealing, which might be due to the more effective stress transfer between the polymer and CNTs induced by the reconstructed CNTs networks. The nanocomposites obtained in this study possess excellent electrical and mechanical properties, which can be applied to the fields of sensors, electromagnetic interference shielding, anti‐static materials, and so forth.

Shang, Mengyao↗

DOE OSTI2020

Intercalation-Induced Reversible Electrochromic Behavior of Two-Dimensional Ti 3 C 2 T x MXene in Organic Electrolytes

MXenes, a large family of two-dimensional materials, have attracted tremendous attention due to their unique physical and chemical properties. Reversible ion intercalation between MXene layers allows modification of the optical, thermal, magnetic, and chemical properties. The electrochemical charge/discharge of MXenes in aqueous electrolytes was reported to lead to reversible electrochromic behavior. In this work, the electrochromic effect of semitransparent Ti 3 C 2 T x MXene film was probed by electrochemical intercalation of Li ions. Correspondingly, a peak shift of 100 nm was observed in the UV-vis spectrum. By combining in-situ Raman spectroscopy, in-situ X-ray diffraction, and density functional theory calculations, we show that the electrochromic shift is primarily due to the formation of robust O-Li bonds and the emerging bands induced changes of inter-band excitations. Finally, understanding the mechanism of electrochromic behavior in Ti 3 C 2 T x lays the foundations of designating 2D materials with durable, controllable, and efficient intercalation-induced electrochromic behaviors.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2022

Broccoli seed extract rich in polysaccharides and glucoraphanin ameliorates DSS ‐induced colitis via intestinal barrier protection and gut microbiota modulation in mice

Abstract BACKGROUND Broccoli has received widespread attention because of its anti‐inflammatory and antioxidant effects. The present study aimed to explore the composition of broccoli seed extract (BSE) and its effect on colitis induced by dextran sulfate sodium (DSS). RESULTS BSE mainly comprises glucoraphanin and polysaccharides composed of arabinose, galactose, glucose and mannose. Animal experiments suggested that BSE intervention effectively reversed body weight loss, suppressed the levels of proinflammatory interleukin‐6, tumor necrosis factor‐α and interleukin‐1β, and elevated the levels of anti‐inflammatory interleukin‐10 and the activities of superoxide dismutase and glutathione in DSS‐induced colitis mice. According to histopathologic and immunohistochemical analysis of colon tissue, BSE intervention may repair the intestinal barrier by upregulating mRNA levels and the expression of tight junction proteins (claudin‐1, occludin and zonula occludens‐1). Gas chromatography–mass spectrometry (MS) analysis demonstrated that cecal short‐chain fatty acids in mice with BSE administration were significantly increased compared with the model group. Sulforaphane and sulforaphane‐ N ‐acetylcysteine were only detected in BSE group mice by ultra‐performance liquid chromatography‐MS analysis. In addition, BSE intervention evidently increased the abundance of Alistipeds , Coriobacteriaceae UCG‐002 and Bifidobacterium and decreased the abundance of Escheichia‐Shinella , Lachnospiraceae others , Parabacteroides , Ruminococcaceae others and Turicibacter , which possibly promoted carbohydrate metabolism and short‐chain fatty acid production. CONCLUSION The present study aimed to elucidate the effect of BSE on colitis and found that BSE, as a novel food ingredient, has great potential for the improvement of colitis. © 2022 Society of Chemical Industry.

Wu, Jiaying↗

DOE OSTI2022

Oxides and Nitrides with Asymmetric Pore Structure from Block Copolymer Co–Assembly and Non–Solvent Induced Phase Separation

Materials combining an asymmetric pore structure with mesopores everywhere enable high surface area accessibility and fast transport, making them attractive for e.g., energy conversion and storage applications. Block copolymer (BCP)/inorganic precursor co-assembly combined with non-solvent induced phase separation (NIPS) provides a route to materials in which a mesoporous top surface layer merges into an asymmetric support with graded porosity along the film normal and mesopores throughout. Here, the co-assembly and non-solvent-induced phase separation (CNIPS) of poly(isoprene)-b-poly(styrene)-b-poly(4-vinylpyridine) (ISV) triblock terpolymer and titanium dioxide (TiO 2 ) sol-gel nanoparticlesare reported. Heat-treatment in air results in free-standing asymmetric porous TiO 2 . Further thermal processing in ammonia results in free-standing asymmetric porous titanium nitride (TiN). processing changes alter structural membrane characteristics is demonstrated. Changing the CNIPS evaporation time results in various membrane cross-sections ( finger-like to sponge-like). Further, oxide and nitride material composition, crystallinity, and porosity are tuned by varying thermal processing conditions. Finally, thermal processing condition effects are probed on phase-pure asymmetric nitride membrane behavior using cyclic voltammetry to elucidate their influence, e.g., on specific capacitance. Results provide further insights into improving asymmetric and porous materials for applications including energy conversion and storage, separation, and catalysis and motivate a further expansion of CNIPS to other (in)organic materials.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2021

Controlling hydrocarbon transport and electron beam induced deposition on single layer graphene: Toward atomic scale synthesis in the scanning transmission electron microscope

Abstract Focused electron beam induced deposition (FEBID) is a direct write technique for depositing materials on a support substrate akin to 3D printing with an electron beam (e‐beam). Opportunities exist for merging this existing technique with aberration‐corrected scanning transmission electron microscopy to achieve molecular‐ or atomic‐level spatial precision. Several demonstrations have been performed using graphene as the support substrate. A common challenge that arises during this process is e‐beam‐induced hydrocarbon deposition, suggesting greater control over the sample environment is needed. Various strategies exist for cleaning graphene in situ. One of the most effective methods is to rapidly heat to high temperatures, for example, 600℃ or higher. While this can produce large areas of what appears to be atomically clean graphene, mobile hydrocarbons can still be present on the surfaces. Here, we show that these hydrocarbons are primarily limited to surface migration and demonstrate an effective method for interrupting the flow using e‐beam deposition to form corralled hydrocarbon regions. This strategy is effective for maintaining atomically clean graphene at high temperatures where hydrocarbon mobility can lead to substantial accumulation of unwanted e‐beam deposition.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Sorption-induced polymer rearrangement: approaches from molecular modeling

With the growing need for chemical separation and chemical storage solutions, polymeric adsorbents have emerged as a promising class of candidate materials because of their potentially tunable sorption properties, membrane structure and relatively cost consciousness. Moreover, the developing field of polymeric membrane materials has shown particular success at integrating both experimental and computational studies. However, these material systems are known to suffer from varying degrees of induced membrane structural rearrangement upon adsorbate uptake, and thus many polymeric membrane performance metrics are often considered to degrade with an increasing number of ‘guest’ species. In this mini–review, we highlight methodology tradeoffs and provide insights into atomistic molecular simulations used to study adsorption with flexible frameworks, which have the potential to predict separation, storage or catalytic capabilities a priori to experimental efforts. Specifically, molecular simulation methods that have been applied to provide predictions of polymeric membrane properties that have included consideration for sorbate–induced polymer chain rearrangement, swelling and/or plasticization are reviewed. Here, the examples and methodologies described provide demonstrations of the applicability of simulations as an approach to understand adsorption–based phenomena at an atomistic/molecular level, and as a tool to carry out screening studies aimed at efficiently providing analysis for a diversity of polymeric adsorbent–adsorbate systems.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Reaction‐induced morphology control in block copolymers

Abstract Controlling the self‐assembly behaviors of block copolymers (BCPs) is a focal point of many research thrusts due to their broad use in various applications. While BCP molecular weight, volume fraction, and chemical identities are key thermodynamic parameters to determine their morphology, an emergent method in this area is through reaction‐induced changes to the characteristics of a BCP in situ , which provides access to multiple morphologies and domain sizes from a single parent polymer, as well as enabling the formation of metastable morphologies which may be difficult to attain otherwise. This work provides a focused review about the current state of reaction‐induced morphology control in BCPs in both solution and solid states. Furthermore, we provide a forward‐looking perspective on the future opportunities of understanding and employing reaction engineering to manipulate and advance BCP self‐assembly. © 2023 Society of Industrial Chemistry.

Robertson, Mark↗

DOE OSTI2026

Capturing soil moisture and salinity changes in flooded coastal forests using electrical resistivity and induced polarization

Geophysical methods provide high-resolution spatial measurements of physical quantities sensitive to changes in soil moisture and salinity and can be used to monitor soil hydrological responses to flooding. However, extracting quantitative hydrological information from geophysical data remains challenging. In this study, we extended existing petrophysical models to estimate soil moisture and salinity from electrical measurements to address this challenge. We manipulated two hydrologically isolated 2000 m 2 experimental plots by simultaneously inundating them with 265 m 3 of either freshwater or estuarine water. Repeated electrical resistivity and induced polarization measurements were used to image the water and solute infiltration along two transects that are 100 and 42 m in length. Petrophysical models derived from laboratory multi-salinity electrical measurements were used to estimate changes in soil moisture and fluid salinity from field measurements of real and imaginary conductivity during the ecosystem-scale flooding experiment. The real conductivity increased by ∼100% in the freshwater plot and ∼570% in the saltwater plot. The change in imaginary conductivity in the freshwater plot was <1 mS/m, whereas that of the estuarine water plot was ∼5 mS/m. Real conductivity shows dependence on soil moisture content with a coefficient of determination (R 2 ) > 0.7, while the imaginary conductivity shows a dependence on soil salinity with R 2 > 0.6. The results validate the use of electrical resistivity for estimating changes in soil moisture content in response to flooding. Combining electrical resistivity imaging with induced polarization measurements provides the possibility to account for changes in pore fluid conductivity.

Adebayo, Moses B. [Univ. of Toledo, OH (United Sta↗

DOE OSTI2025

Control of machining-induced residual stress via tool geometry and process parameter modification

Distortion generated in machined, monolithic, thin-walled aerospace components due to residual stresses leads to significant material and economic waste in the manufacturing industry. Inherent residual stress (IRS) present in stock materials combines with machining-induced residual stress (MIRS) to influence the final machined part distortion. It is hypothesized that MIRS can be controlled, based on the part geometry, through deliberate cutting tool geometry and process parameter modifications to negate the effect of IRS on distortion, consequently resulting in distortion-free parts. A finite element (FE) orthogonal cutting model is developed to study how tool geometry and process parameters influence machining-induced residual stress (MIRS). Orthogonal cutting experiments are performed on Al 7075-T651 samples to measure cutting forces and MIRS. A cutting force dynamometer is used to measure forces during cutting and a novel digital image correlation (DIC) based hole drilling technique is employed to measure the near-surface residual stress (RS) in the cut samples. These data are subsequently utilized to validate the FE prediction model. Various cases of cutting simulations involving different depths of cut, tool tip radii, and rake angles are performed to study their effects on RS. Similar to prior literature, increasing the depth of cut, tool tip radius, or rake angle is found to promote the formation of near-surface tensile stresses. The competing effects of material plowing and temperature are shown to determine the type of RS at the end of the cut. Moreover, a window of variation of RS (up to ± 400 MPa) is estimated within the given range of conditions, allowing for the control of MIRS through tool and process modification.

Mathews, Ritin [ORNL] (ORCID:0000000301440828)↗

DOE OSTI2026

Radon-induced backgrounds in the NEXT-100 experiment

The NEXT-100 detector at the LSC aims at the first competitive search for the 0νββ decay using a high-pressure $^{136}$Xe electroluminescent time projection chamber. The first low-background run of NEXT-100 at 3.95 bar has been devoted to the measurement of the radon-induced backgrounds impacting this search. The contributions from both the internal and external airborne radon have been evaluated. The internal $^{222}$Rn activity is found to be (0.95±0.04(stat)±0.09(sys)) Bq/m$^{3}$, while no traces of $^{220}$Rn have been observed. Most of the $^{222}$Rn progeny plate-out on the surface of the cathode of the detector, leading to a rate of Rn-induced $^{214}$Bi of (0.97±0.05(stat)±0.10(sys)) Hz for visible energies above 400 keV. The corresponding background index in the 0νββ region of interest is evaluated as (7.3±1.5(stat)±0.8(sys))×10$^{−4}$ counts/(keV·kg·yr) after selection of the fully contained events. This background index is reduced to ∼4×10$^{−5}$ counts/(keV·kg·yr) by applying a topological selection requiring only one double-electron-like track in the events. This value is one order of magnitude below the total radiogenic background expectation in NEXT-100. By analyzing the correlation of the airborne radon activity and the measured rate of events in NEXT-100, it is concluded that the detector operates in a virtually radon-free environment thanks to the radon abatement system of the LSC.[graphic not available: see fulltext]

Cortes-Parra, C. [Valencia U., IFIC] (ORCID:000000↗

DOE OSTI2021

Pyrolysis temperature and soil depth interactions determine PyC turnover and induced soil organic carbon priming

Pyrogenic organic carbon (PyC) is a complex, heterogeneous class of thermally altered organic substrates, but its dynamics and how its behavior changes with soil depth remain poorly understood. We conducted a laboratory incubation study to investigate the interactive effects of pyrolysis temperature and soil depth on the turnover of PyC compared to its precursor wood and native SOC (NSOC). We incubated dual-labeled (13C and 15N) jack pine pyrogenic organic matter produced at 300 °C (PyC300), 450 °C (PyC450), and their precursor pine wood in a fine-loamy, mixed-conifer forest soil for 745 days. A mixture of surface (0–10 cm) and subsurface (50–70 cm) forest soils, with and without labeled biomass were incubated in the dark at 55% soil water field capacity and 25 °C. Total 13C from PyC and wood mineralized as 13C-CO2 (as % of C added to soil) declined with an increase in pyrolysis temperature as follows: 54 ± 7.7% for wood, 3.1 ± 0.2% for PyC300, and 0.94 ± 0.08% for PyC450. Furthermore, after 2 years, soil depth interacted with pyrolysis temperature to affect C turnover, with total wood C losses significantly declining from 70.6% in surface soils to 37.5% in subsurface soil, while total losses of PyC300 and PyC450 were unaffected by differences between surface and subsurface soils. Wood induced negative priming (i.e., decreased mineralization rates) in surface soil at days 3 and 60, while PyC300 induced positive priming (i.e., increased mineralization rates) in subsurface soil at day 60. After 2 years, unlabeled NSOC losses increased from 9.2 ± 0.8% of NSOC in unamended treatments to 16.5 ± = 2.6% of NSOC with PyC450 additions. Our results suggest that PyC pyrolyzed at a given temperature can mineralize at similar rates between soil depths, and high amounts of PyC450 in subsurface soils can stimulate NSOC losses. These findings indicate that soil depth imposes critical controls on PyC dynamics belowground.

13C-labeling↗

DOE OSTI2025

Pressure-induced cation and vacancy disorder-order transition and near-zero τ f in deficient hexagonal perovskite Ba 8 ZnTa 6 O 24 dielectrics

Pressure applications can enable the tuning of atomic/defect ordering and provide access to new functional materials. Here, in this study, we report that pressure-induced structural transformation featuring disorder-order transition of both cations and vacancies in the 8-layer deficient hexagonal perovskite tantalate dielectrics Ba 8 ZnTa 6 O 24 , which transformed the structure from twin to shift and remarkably lowered the temperature coefficient of resonant frequency τ f down to near zero (∼0.56 ppm/°C) from 38 ppm/°C for the twinned precursor. The atomic scale STEM-HAADF and EDS results confirm the ordering of Zn in the Ta host at the nanometer scale in the shifted material featuring well-ordered Ba 8 ZnTa 6 O 24 slabs intergrown with Ba 3 ZnTa 2 O 9 and Ba 5 Ta 4 O 15 monolayers and anti-phase grain boundaries as planar defects. The pressure-induced twin-shift structural transformation of Ba 8 ZnTa 6 O 24 features the rare constant concentration of the hexagonal stacked layers, which is allowed by the vacancy ordering at the central layers of face-shared octahedral (FSO) trimers avoiding the FSO B-B repulsion, and remarkably the faster cationic ordering kinetics compared with the 2:1 ordered complex perovskites. Although the inclusion of numerous planar defects and the oxidizable atomic defects led to significant p-type conduction and inhomogeneous electrical microstructures, resulting in an extraordinarily high extrinsic dielectric loss for the high-pressure shifted Ba 8 ZnTa 6 O 24 pellet, the intrinsically near-zero τ f could make the shifted Ba 8 ZnTa 6 O 24 perovskite an ideal microwave dielectric resonator candidate if the defects could be eliminated.

high pressure↗

DOE OSTI2023

In Situ X-ray Diffraction Investigation of Hydrogen Effects on Deformation-Induced Phase Transformation in Forged and Additively Manufactured 304L Stainless Steels

Here, this study utilized high energy synchrotron x-ray diffraction to probe microstructural evolution during uniaxial deformation of conventionally manufactured and additively manufactured (AM) 304L stainless steel with and without internal hydrogen. The objective of this effort is to highlight the effect of hydrogen on deformation-induced martensite phase transformations in austenitic stainless steels. Solute hydrogen depresses the required applied strain to initiate austenite transformation to ε-martensite and α'-martensite in both forged and AM stainless steel. Similarly, the total fraction of transformation product is larger when the microstructure is saturated with hydrogen. Deformation induced phase transformations also lead to a variation in strain partitioning behavior, which is linked to the chemical composition and stacking fault energy of the starting and hydrogen-charged materials.

36 MATERIALS SCIENCE↗

DOE OSTI2020

High-energy synchrotron x-ray study of deformation-induced martensitic transformation in a neutron-irradiated Type 316 stainless steel

An unusual tensile deformation behaviour in the form of a propagating band along the sample gauge was observed in two neutron-irradiated 316 stainless steel samples during room-temperature tests, leading to a combination of high strength and high ductility. These bands were not observed in an unirradiated counterpart. With the help of in situ high-energy synchrotron x-ray diffraction, the phase-specific crystal information was tracked at different deformation levels in each sample. Post-irradiation and post-deformation samples were examined using electron microscopy to characterize various microstructural features. All samples displayed a deformation-induced martensitic phase transformation, which was identified as a second strain-hardening mechanism accompanying the dislocation hardening. The deformation-induced martensitic transformation was rationalized by the effect of applied stress on the effective martensite start temperature. The results showed that the irradiation did not alter the dislocation hardening and the martensitic transformation mechanisms, but the increased yield strength in irradiated materials facilitated the localized phase transformation at the onset of plastic deformation, in contrast to the unirradiated material which required pre-straining. The hardening effect of the martensitic transformation reduced the tendency towards necking and mitigated the loss of ductility in the irradiated material by carrying the deformation in the form of a propagating band. Despite the beneficial effect from the martensitic transformation, this study indicates that this mechanism cannot not be activated at typical operating temperatures of nuclear reactors.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Non-compact oxide-island growth induced by surface phase transition of the intermetallic NiAl during vacuum annealing

Crystal structure and composition are inter-dependent and decoupling their effects on surface reactivity is challenging. Using low-energy electron microscopy to spatially and temporally resolve the oxide film growth during the oxidation of NiAl(100), we differentiate such coupled effects by monitoring oxide growth while simultaneously fine-tuning the surface structure and composition during oxidation. We demonstrate that the oxidation of chemically ordered surfaces results in compact oxide island growth whereas non-compact oxide growth during the surface phase transition. By incorporating the surface phase transition induced chemical disordering into kinetic Monte Carlo simulations, we illustrate that the non-compact oxide growth is induced by the composition effect on the surface diffusion of oxygen, which can be described by the concept of “ant in the labyrinth”.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Irradiation induced void spheroidization, shrinkage and migration in Cu at elevated temperatures: An in situ study

We show understanding the void evolution in irradiation environment is of great interest and significance, as irradiation-induced voids typically lead to pronounced volumetric swelling and degradation of mechanical properties. In situ studies on the irradiation response of nanovoids at elevated temperature remain limited. In this work, we performed systematic in situ 1 MeV Kr ++ irradiations on Cu with nanovoids in a transmission electron microscope up to 350 °C. The in situ studies revealed intriguing void spheroidization, shrinkage and migration. Furthermore, the morphology evolution and migration of nanovoids showed a strong dependence on irradiation temperature and initial void size. Post-irradiation analyses identified defect clusters in the form of stacking fault tetrahedrons, and the remaining large faceted nanovoids. The underlying mechanisms of irradiation-induced void spheroidization and shrinkage were discussed based on phase-field modeling.

36 MATERIALS SCIENCE↗