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At least 541 records · Page 30

SIMS Analysis of d18O and d13C of Carbonate Cements in Shale & Mudstone. Final report

This project has had two primary goals: 1) improving new technology for in situ microanalysis of stable isotope ratios by SIMS (secondary ion mass spectrometry) and 2) evaluating the importance of in situ analysis for studies of carbonate cements within shales of the Bakken Petroleum System. The systematic relations of stable isotope ratios provide an important tool to help resolve critical questions in geology. Stable isotope analysis of carbonate cements in shale constrain many topics of interest to DOE including: CO2 sequestration, climate change, and the genesis and quality of rock reservoirs for petroleum, natural gas, and water. However, this evidence is often preserved as fine-scale zonation, which is homogenized by conventional bulk analysis of powders. Recently, analysis of ultra-small spots in polished samples at the University of Wisconsin WiscSIMS Lab. has documented stable isotope zoning in carbonates and other diagenetic cements at smaller scales than previously possible. We have made detailed studies of oxygen and carbon isotope ratios in diagenetic cements from shales of the Bakken Formation from the Williston basin and elsewhere. The Bakken contains both reservoir and source rocks for petroleum. Hydrofracturing has greatly enhanced production of oil in these tight reservoirs. The sediments contain zoned carbonate cements with growth textures that record multiple events. The growth of carbonate (dolomite) cements has been proposed to control reservoir quality, but previous stable isotope studies of homogenized powders could not resolve individual generations of cement and this proposal remains untested. Our better characterization of the multiple growth zones in these carbonates will aid in understanding the genesis of these tight reservoirs and the production of unconventional oil and gas. This study has also developed SIMS standards for analysis of all compositions of Ca-Mg-Fe carbonate and selected Mn-carbonates and hydromagnesite. We have refined techniques for improved accuracy of SIMS stable isotope analysis, and for sub-1-micron spot sizes. We have established protocols for mapping and correlating sample analyses at micron-scale using QGIS software.

04 OIL SHALES AND TAR SANDS↗

Microstructural Analysis of Powder Metallurgy Tool Steels in the Context of Abrasive Wear Behavior: A New Computerized Approach to Stereology

The present work describes a new methodology designed to characterize the microstructures of tool steels containing carbide hard phases, with the focus set on their abrasive wear resistance. A series of algorithms were designed and implemented in MATLAB® to (i) recognize each of the features of interest, (ii) measure relevant quantities and (iii) characterize each of the phases and the alloy in function of attributes usually neglected in wear description applications: size distribution, shape and contiguity of the hard phases. The new framework incorporates new parameters to describe each one of these attributes, as observed in SEM micrographs. All three aforementioned stages contain novel contributions that can be potentially beneficial to the field of materials design in general and to the field of alloy design for severely abrasive environments in particular. Models of known geometry and micrographs of different powder metallurgy steels were analyzed, and the obtained results were compared with the obtained by the linear intercept method. The relation between the new parameters and the ones available in the scientific literature is also discussed.

36 MATERIALS SCIENCE↗

Property-Graded Stainless Steel 316L by Selective Laser Melting: Characterization & Design

Abstract The purpose of this research work is to characterize and inform the design of (mechanical) property-graded bulk structures made from a single metallic alloy via a laser powder bed fusion (LPBF) process, with an end goal of creating repeatable/reproducible functionally-graded additively manufactured (FGAM) parts. This paper specifically investigates the manufacture of stainless steel (SS) 316L structures via a pulsed selective laser melting (SLM) process, and the underlying causes of property variations (within a functionally-acceptable range) through various material characterization techniques. For this, a design of experiments spanning the volumetric energy density (VED) based process parameter design space was utilized to investigate the range of functionally-acceptable physical/mechanical properties achievable in SS 316L. Five sample conditions (made via different process parameter combinations) were down-selected for in-depth microstructure analysis and mechanical/physical property characterization; these were suitably selected to impart a wide and controllable property range (209–318 HV hardness, 90–99.9% relative density, and 154–211 GPa modulus). It was observed that property variations resulted from combinations of porosity types/amounts, martensitic phase fractions, and grain sizes. Based on these findings, property-graded standard test specimens were designed and manufactured for further investigation—tensile specimens having a monotonic hardness change along its gauge length, four-point bending specimens with varying elastic moduli as a function of the distance from the neutral axis, and Moore’s rotating beam fatigue specimens with moduli variations based on the distance from the center. Altogether, this work lays the foundation for understanding and designing the local and global mechanical performance of FGAM bulk structures.

Engineering↗

Fused filament fabrication of thermoplastic polyurethane composites with microencapsulated phase-change material

Here, the present study examines the thermal energy storage (TES) effectiveness and printability of microencapsulated phase-change material (MEPCM) combined with thermoplastic polyurethane (TPU) for fused filament fabrication (FFF). Two formulations were assessed: 24D MEPCM, which changes phase at 24 ° C, compounded with TPU pellets and 43D MEPCM, which changes phase at 43 ° C, integrated with TPU powder. These combinations are designed to evaluate the effectiveness of the form of the TPU (pellets versus powder) in the FFF process. The investigation includes a comprehensive analysis of thermal characteristics, encompassing phase-change temperature, latent heat of fusion, thermal conductivity, and thermal decomposition, which are assessed through differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA). Additionally, mechanical properties, including stress-strain behavior, are examined to evaluate material suitability for TES applications, while microstructural visualization is used to provide deeper insights into material performance, structural integrity, and the quality of printed components. The 24D MEPCM and TPU pellets formulation experienced a significant loss of approximately 39.6% of PCM during filament extrusion and printing, resulting in a reduced effective latent heat. Therefore, further characterization of the pellet formulation was discontinued due to excessive leakage. In contrast, the 43D MEPCM and TPU powder formulation demonstrated minimal PCM loss, with the 60 wt.% composition achieving an effective latent heat of 132 J/g. This value represents the highest effective latent heat currently documented in the literature for PCM-polymer-composite materials produced using an FFF-based additive manufacturing process.

25 ENERGY STORAGE↗

Location-Specific Microstructure Characterization Within AM Bench 2022 Nickel Alloy 718 3D Builds

Abstract The Additive Manufacturing Benchmark Test Series (AM Bench) is a broad effort to produce rigorous measurement datasets for validating AM computer simulations across the range of processing, structure, and properties, for many additive manufacturing (AM) build methods and material classes. Here, the microstructures of nickel alloy 718 AM Bench 2022 test artifacts produced using laser-based powder bed fusion (PBF-LB), in both as-built and fully heat-treated conditions, are examined. Cross sections are primarily characterized using large area scanning electron microscopy (SEM) electron backscatter diffraction (EBSD) and example analyses of the crystallographic textures are described. These data are part of a large set of in situ and ex situ measurements from both three-dimensional builds and laser tracks on bare plates. All the measurement data are available online with download links at www.nist.gov/ambench .

Levine, L. E. (ORCID:0000000334484229)↗

Characterization of fusion welded ceramics in the SiC-ZrB 2 -ZrC system

Various SiC-ZrB 2 -ZrC ceramics were joined by fusion welding to determine the maximum silicon carbide content that could be joined. Commercial powders were hot pressed, machined, and preheated to 1450 °C before joining with a tungsten inert gas welding torch at 160–200 A. Resulting welds were cross-sectioned and analyzed to determine which compositions were weldable and to characterize microstructural evolution in welded samples. As compositions approached the ternary eutectic, the welds had smaller SiC grains and exhibited better weldability. Penetration depth of welds was controlled by a combination of current input and welding speed. Here, the ternary eutectic in the system was found at 36.9 ± 1.3 vol% SiC, 42.7 ± 1.5 vol% ZrB 2 , and 20.4 ± 1.9 vol% ZrC and its melting temperature was 2330 ± 23 °C. A ternary phase diagram for the SiC-ZrB 2 -ZrC was constructed and proposed via microstructural analysis of arc melted pellets on binary joins between each binary eutectic and the ternary eutectic in the system.

36 MATERIALS SCIENCE↗

Dipolar Spin Ice Regime Proximate to an All-In-All-Out Néel Ground State in the Dipolar-Octupolar Pyrochlore Ce 2 Sn 2 O 7

The dipolar-octupolar (DO) pyrochlores, R 2 M 2 O 7 ( R = Ce , Sm , Nd ), are key players in the search for realizable novel quantum spin liquid (QSL) states as a large parameter space within the DO pyrochlore phase diagram is theorized to host QSL states of both dipolar and octupolar nature. New single crystals and powders of Ce 2 Sn 2 O 7 , synthesized by hydrothermal techniques, present an opportunity for a new characterization of the exchange parameters in Ce 2 Sn 2 O 7 using the near-neighbor X Y Z model Hamiltonian associated with DO pyrochlores. Utilizing quantum numerical linked cluster expansion fits to heat capacity and magnetic susceptibility measurements, and classical Monte Carlo calculations to the diffuse neutron diffraction of the new hydrothermally grown Ce 2 Sn 2 O 7 samples, we place Ce 2 Sn 2 O 7 ’s ground state within the ordered dipolar all-in-all-out (AIAO) Néel phase, with quantum Monte Carlo calculations showing a transition to long-range order at temperatures below those accessed experimentally. Indeed, our new neutron diffraction measurements on the hydrothermally grown Ce 2 Sn 2 O 7 powders show a broad signal at low scattering wave vectors, reminiscent of a spin ice, in striking contrast from previous powder neutron diffraction on samples grown from solid-state synthesis, which found diffuse scattering at high scattering wave vectors associated with magnetic and suggested an octupolar quantum spin ice state. We conclude that new hydrothermally grown Ce 2 Sn 2 O 7 samples host a finite-temperature proximate dipolar spin ice phase, above the expected transition to AIAO Néel order. Published by the American Physical Society 2024

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Predicting phase transformation kinetics during metal additive manufacturing using non-isothermal Johnson-Mehl-Avrami models: Application to Inconel 718 and Ti-6Al-4V

Here, a computational model was developed to predict solid-state phase transformation kinetics within mechanical parts during metal additive manufacturing processes. This model is a modified version of the Johnson-Mehl-Avrami model for non-isothermal phase transformations that can be applied to various material systems undergoing solid-state phase transformations. Using the thermal history of an additive manufacturing fabricated mechanical part, along with the necessary thermodynamic data and kinetic information as inputs, the model outputs the history of phase fraction evolution during the build process. The model was applied to an Inconel 718 part built by powder bed fusion and a Ti-6Al-4V part built by directed energy deposition. Microstructure characterization and mechanical testing were performed for the validation of the model.

36 MATERIALS SCIENCE↗

Rare earth ion-adsorption clays in the presence of iron at basic pH: Adsorption mechanism and extraction method

In this work, the uptake mechanism and influence of iron (Fe) co-adsorption on the binding of rare-earth elements (REEs) on kaolinite have been investigated. REEs and varying concentrations of Fe were co-adsorbed onto kaolinite at pH 10.5. Inductively coupled plasma mass spectrometry (ICP-MS), powder X-ray diffraction (PXRD), and X-ray photoelectron spectroscopy (XPS) were used to characterize how Fe co-adsorption influenced the uptake mechanism of REEs on kaolinite. Elemental analysis by ICP-MS revealed that the REE concentrations on kaolinite were unaffected by the presence of Fe. Crystal structure of kaolinite, determined by PXRD, was not altered after REE and Fe co-adsorption. XPS suggests that the adsorbed Fe is in the form of FeOOH, while the greatly attenuated REE XPS signals upon Fe co-adsorption implies that REEs are encapsulated by Fe species. Based on these results, we conclude that FeOOH layers were formed on top of REEs on the surface of kaolinite. Synthesized REE-Fe-kaolinite samples respond poorly to ion-exchange leaching, indicating that Fe is detrimental to the REE ion-exchange efficiency. The inhibition of ion-exchange REE extraction appears to be due to the passivating FeOOH layers. In contrast to ion-exchange methods, reductive leaching was found to dissolve the FeOOH passivating layers and liberate REEs such that they became available for ion-exchange leaching.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Reinforcing blade-cast photocatalytic-titania thin film by titanate nanotubes

Highlights: • Suspension-based photocatalysts are inferior to thin-films due to separation issues. • Hydrothermal TiO{sub 2} nanotubes and sol-gel Ti(n-OBu){sub 4} blends were tape casted on glass. • Optimum blend composition yields mechanical stability due to the tubes reinforcing effect. • At optimum gel content the nanotube bundles are smoothed without stabilizers added. • Surface accessibility and mass transfer dominate the photocatalytic dye degradation. - Abstract: Titanate nanotubes/titania gel blends were prepared as composite sol-gel material, deposited on a glass substrate using a doctor blade and calcined in order to create thin films. In order to get an insight in titania nanotubes’ ability to reinforce thin films, drying control chemical agents were not used. The effects of titanate nanotubes to titanium n-butoxide ratio on surface morphology, phase composition, mechanical stability and photocatalytic activity were studied. Characterization of the thin films was carried out by means of optical and scanning electron microscopy, powder X-ray diffraction, synchrotron radiation grazing incidence X-ray diffraction and mechanical stability testing. Photocatalytic properties of the obtained thin films were evaluated on the basis of methylene blue degradation. Moderate blends exhibit favourable microstructural features while the dye degradation rate was greater for films with a greater amount of titanate nanotubes.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Cold Spray Field Deployment Evaluation for Double-Shell Tank 241-AN-105

This report highlights the documentation that supported Cold Spray field deployment in double-shell tank (DST) 241-AN-105 (AN-105) in July of 2025. This work was a collaborative effort between VRC Metal Systems (VRC), Robotic Technologies of Tennessee (RTT), the Hanford Tank Waste Operation and Closure (H2C) Chief Technology Office, H2C Tank Farm Projects Engineering, H2C Tank and Pipeline Integrity (TAPI) and H2C Ultrasonic Testing (UT) Operations & Support. Since 2019, the Chief Technology Office has been developing Cold Spray technology for refurbishing Hanford’s DSTs (RPP-RPT-65015). This technology is particularly relevant for addressing localized corrosion within the annulus of the DSTs by propelling metal powder particles at supersonic speeds to targeted areas. This process results in high-quality coatings characterized by high bond strength and low porosity result.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Relationships between toughness and microstructure of reaction bonded Si3N4

Fracture toughnesses of nominally identical batches of reaction bonded silicon nitride (RBSN) differed significantly (about 2.0 and about 2.7 MPa sq rt m). Detailed fractographic and microstructural characterizations investigated underlying factors. Subtile differences between high and low toughness RBSN and between constituent Si powders have been revealed through SEM/FEG, TEM, BET, Hg-porosimetry, and XRD. The results illustrate the need for behavioral models to guide microstructural design and to interpret properties of brittle materials with intermediate levels of porosity.

Lightfoot, Annamarie↗

Aerogel Beads as Cryogenic Thermal Insulation System

An investigation of the use of aerogel beads as thermal insulation for cryogenic applications was conducted at the Cryogenics Test Laboratory of NASA Kennedy Space Center. Steady-state liquid nitrogen boiloff methods were used to characterize the thermal performance of aerogel beads in comparison with conventional insulation products such as perlite powder and multilayer insulation (MLI). Aerogel beads produced by Cabot Corporation have a bulk density below 100 kilograms per cubic meter (kg/cubic m) and a mean particle diameter of 1 millimeter (mm). The apparent thermal conductivity values of the bulk material have been determined under steady-state conditions at boundary temperatures of approximately 293 and 77 kelvin (K) and at various cold vacuum pressures (CVP). Vacuum levels ranged from 10(exp -5) torr to 760 torr. All test articles were made in a cylindrical configuration with a typical insulation thickness of 25 mm. Temperature profiles through the thickness of the test specimens were also measured. The results showed the performance of the aerogel beads was significantly better than the conventional materials in both soft-vacuum (1 to 10 torr) and no-vacuum (760 torr) ranges. Opacified aerogel beads performed better than perlite powder under high-vacuum conditions. Further studies for material optimization and system application are in progress.

Fesmire, J. E.↗

Novel Sample-handling Approach for XRD Analysis with Minimal Sample Preparation

Sample preparation and sample handling are among the most critical operations associated with X-ray diffraction (XRD) analysis. These operations require attention in a laboratory environment, but they become a major constraint in the deployment of XRD instruments for robotic planetary exploration. We are developing a novel sample handling system that dramatically relaxes the constraints on sample preparation by allowing characterization of coarse-grained material that would normally be impossible to analyze with conventional powder-XRD techniques.

Sarrazin, P.↗

Ultra-Light Ultra-Strong Proppants

The present invention provides a method of preparing a proppant material by heating a reaction mixture comprising a plurality of oxides in a reactive atmosphere to a temperature above the melting point of the reaction mixture to form a melt, and then allowing the melt to solidify in a mold in the form of spherical particles. The present invention also provides a method of preparing a proppant material by heating a reaction mixture comprising a plurality of oxides and one or more additives in a reactive atmosphere to a temperature below the melting point of the reaction mixture to form a powder including one or more reaction products, and then processing the powder to form spherical particles. The present invention also provides a proppant material including spherical particles characterized by a specific gravity of about 1.0 to 3.0 and a crush strength of at least about 10,000 psi.

Ravi, Vilupanur A.↗

Fabrication and Thermoelectric Characterization of Transition Metal Silicide-Based Composite Thermocouples

Metal silicide-based thermocouples were fabricated by screen printing thick films of the powder compositions onto alumina tapes followed by lamination and sintering processes. The legs of the embedded thermocouples were composed of composite compositions consisting of MoSi2, WSi2, ZrSi2, or TaSi2 with an additional 10 vol % Al2O3 to form a silicide–oxide composite. The structural and high-temperature thermoelectric properties of the composite thermocouples were examined using X-ray diffraction, scanning electron microscopy and a typical hot–cold junction measurement technique. MoSi2-Al2O3 and WSi2-Al2O3 composites exhibited higher intrinsic Seebeck coefficients (22.2–30.0 µV/K) at high-temperature gradients, which were calculated from the thermoelectric data of composite//Pt thermocouples. The composite thermocouples generated a thermoelectric voltage up to 16.0 mV at high-temperature gradients. The MoSi2-Al2O3//TaSi2-Al2O3 thermocouple displayed a better performance at high temperatures. The Seebeck coefficients of composite thermocouples were found to range between 20.9 and 73.0 µV/K at a temperature gradient of 1000 °C. There was a significant difference between the calculated and measured Seebeck coefficients of these thermocouples, which indicated the significant influence of secondary silicide phases (e.g., Mo5Si3, Ta5Si3) and possible local compositional changes on the overall thermoelectric response. The thermoelectric performance, high sensitivity, and cost efficiency of metal silicide–alumina ceramic composite thermocouples showed promise for high-temperature and harsh-environment sensing applications.

47 OTHER INSTRUMENTATION↗