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At least 235 records · Page 13

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DOE OSTI2022

Versatile soil gas concentration and isotope monitoring: optimization and integration of novel soil gas probes with online trace gas detection

Abstract. Gas concentrations and isotopic signatures can unveil microbial metabolisms and their responses to environmental changes in soil. Currently, few methods measure in situ soil trace gases such as the products of nitrogen and carbon cycling or volatile organic compounds (VOCs) that constrain microbial biochemical processes like nitrification, methanogenesis, respiration, and microbial communication. Versatile trace gas sampling systems that integrate soil probes with sensitive trace gas analyzers could fill this gap with in situ soil gas measurements that resolve spatial (centimeters) and temporal (minutes) patterns. We developed a system that integrates new porous and hydrophobic sintered polytetrafluoroethylene (sPTFE) diffusive soil gas probes that non-disruptively collect soil gas samples with a transfer system to direct gas from multiple probes to one or more central gas analyzer(s) such as laser and mass spectrometers. Here, we demonstrate the feasibility and versatility of this automated multiprobe system for soil gas measurements of isotopic ratios of nitrous oxide (δ18O, δ15N, and the 15N site preference of N2O), methane, carbon dioxide (δ13C), and VOCs. First, we used an inert silica matrix to challenge probe measurements under controlled gas conditions. By changing and controlling system flow parameters, including the probe flow rate, we optimized recovery of representative soil gas samples while reducing sampling artifacts on subsurface concentrations. Second, we used this system to provide a real-time window into the impact of environmental manipulation of irrigation and soil redox conditions on in situ N2O and VOC concentrations. Moreover, to reveal the dynamics in the stable isotope ratios of N2O (i.e., 14N14N16O, 14N15N16O, 15N14N16O, and 14N14N18O), we developed a new high-precision laser spectrometer with a reduced sample volume demand. Our integrated system – a tunable infrared laser direct absorption spectrometry (TILDAS) in parallel with Vocus proton transfer reaction mass spectrometry (PTR-MS), in line with sPTFE soil gas probes – successfully quantified isotopic signatures for N2O, CO2, and VOCs in real time as responses to changes in the dry–wetting cycle and redox conditions. Broadening the collection of trace gases that can be monitored in the subsurface is critical for monitoring biogeochemical cycles, ecosystem health, and management practices at scales relevant to the soil system.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2025

High temperature tensile properties of H13 tool steel fabricated via binder jet additive manufacturing

H13 is one of the most used steels for hot work tooling applications like die casting. Binder jet additive manufacturing (BJAM) offers a cost-effective solution to fabricate tools with performance enhancing features like internal cooling channels. While full densification of BJAM H13 has been demonstrated in the literature, the room and high temperature tensile properties of the material, and the effect of post-process treatments like hot isostatic pressing (HIP), and heat treatment (HT) are unknown. Here we use HIP+HT to obtain a combination of ultimate tensile strength (UTS) and elongation to failure that is superior to H13 fabricated via laser powder bed fusion and wire arc additive manufacturing. HIP+HT BJAM H13 has a superior UTS (1836 MPa) compared with conventionally processed (1671 MPa) H13 but has lower plastic elongation. We report that as-sintered samples have an extensive network of continuous grain boundary (GB) carbides that contribute to brittle fracture. HIP+HT results in partial dissolution of GB carbides and formation of a fine martensitic microstructure resulting in superior tensile strength and elongation compared with as-sintered H13. We use thermo-kinetic calculations to rationalize the effects of HIP+HT on microstructure and properties.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Material jet printing of transparent ceramic Yb:YAG planar waveguides

A new, to the best of our knowledge, 3D additive manufacturing technique utilizing particle-loaded ink jet printing to fabricate transparent ceramic Yb:YAG planar waveguides for laser gain media was demonstrated. Rheological optimization of YAG particle-loaded inks resulted in successful droplet formation and printing resolution. Planar waveguides composed of a Yb:YAG guide encased in undoped YAG cladding were printed with guide thicknesses ranging between 25 and 350 µm and consolidated to high optical quality via solid-state sintering. Sufficiently low optical (1–3%/cm) and intermodal scatter allowed single-mode propagation with a core/clad index difference of Δ n ∼ 5.0 × 10 − 4 (corresponding to 3 at.% Yb). The waveguides were cladding-pumped longitudinally with a 940 nm diode array resulting in 23.6% slope efficiency in 2 ms pulsed operation.

36 MATERIALS SCIENCE↗

NASA NTRS1997

Influence of High Cycle Thermal Loads on Thermal Fatigue Behavior of Thick Thermal Barrier Coatings

Thick thermal barrier coating systems in a diesel engine experience severe thermal Low Cycle Fatigue (LCF) and High Cycle Fatigue (HCF) during engine operation. In the present study, the mechanisms of fatigue crack initiation and propagation, as well as of coating failure, under thermal loads which simulate engine conditions, are investigated using a high power CO2 laser. In general, surface vertical cracks initiate early and grow continuously under LCF and HCF cyclic stresses. It is found that in the absence of interfacial oxidation, the failure associated with LCF is closely related to coating sintering and creep at high temperatures, which induce tensile stresses in the coating after cooling. Experiments show that the HCF cycles are very damaging to the coating systems. The combined LCF and HCF tests produced more severe coating surface cracking, microspallation and accelerated crack growth, as compared to the pure LCF test. It is suggested that the HCF component cannot only accelerate the surface crack initiation, but also interact with the LCF by contributing to the crack growth at high temperatures. The increased LCF stress intensity at the crack tip due to the HCF component enhances the subsequent LCF crack growth. Conversely, since a faster HCF crack growth rate will be expected with lower effective compressive stresses in the coating, the LCF cycles also facilitate the HCF crack growth at high temperatures by stress relaxation process. A surface wedging model has been proposed to account for the HCF crack growth in the coating system. This mechanism predicts that HCF damage effect increases with increasing temperature swing, the thermal expansion coefficient and the elastic modulus of the ceramic coating, as well as the HCF interacting depth. A good agreement has been found between the analysis and experimental evidence.

Zhu, Dongming↗

DOE OSTI2025

Additive manufacturing of amorphous metal soft magnetic composites

Soft magnet alloys are used as magnetic cores for electric motors, transformers, wind turbines and other power generation systems. Soft magnetic cores are expensive and time consuming to manufacture in the complex shapes required for next-generation devices using conventional press and sinter powder metallurgy. The objective of this effort is to additively manufacture high performance soft magnets, with reduced cost and reduced material waste and 10x lower energy (core) loss at the high operating frequencies of many electric machines. Laser powder bed fusion additive manufacturing is used as the fabrication method. Electrical steel and amorphous alloys atomized powders are used as a feedstock materials. Magnetic cores are printed in topology optimized structures such as the Hilbert curve because this has been shown to reduce energy losses by minimizing the eddy currents that circulate within the magnet at high frequencies. In our project, we succeed in printing FeSi 3.5wt% and FeSi 6.5wt% electrical steels, and iron-based soft magnetic amorphous alloys in the shape of Hilbert and Peano curve topology optimized structures. We found that the Peano curve has a higher cut-off frequency than the Hilbert curve, and that amorphous alloys have high cut-off frequencies and higher mechanical hardness than electrical steels. Processing conditions such as laser power, scan speed, and hatching pattern were optimized to achieve high density prints, and optimize magnetic performance. We find that the printing of amorphous alloy soft magnetic cores may be technoeconomically feasible for large scale applications such as transformers, for which supply chain issues and the labor costs of manual fabrication of magnetic cores is prohibitive in some cases.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Titanium Dioxide Nanomaterial Ink Production Through Laser Ablation Synthesis in Solution for Printed Electronics Applications

Flexible and printed electronics have become increasingly popular as they make possible the production of flexible, low-cost, multifunction devices that are unachievable through traditional manufacturing methods. The printed films are significantly impacted and thus limited by the existing ink production process. Herein, an alternate technique of generating high-quality titanium dioxide (TiO 2 ) nanoparticle ink compatible with aerosol jet printing using laser ablation synthesis in solution (LASiS) is showcased. Dynamic light scattering data and transmission electron microscopy confirm the particle size distribution. UV–vis measurements are performed, and the Beer–Lambert relationship is used to determine the concentration of the generated ink. The inks generated at two different repetition rates are compared: 200 kHz and 1 MHz. X-Ray diffraction analysis of the aerosol jet printed thin film post-thermal sintering confirms the grain size and phase purity of the printed thin films. This work demonstrates the effectiveness of the LASiS technique in producing printable nanoparticle inks with little-to-no postprocessing.

36 MATERIALS SCIENCE↗

NASA NTRS2008

Failure Mechanisms and Life Prediction of Thermal and Environmental Barrier Coatings under Thermal Gradients

Ceramic thermal and environmental barrier coatings (TEBCs) will play an increasingly important role in gas turbine engines because of their ability to further raise engine temperatures. However, the issue of coating durability is of major concern under high-heat-flux conditions. In particular, the accelerated coating delamination crack growth under the engine high heat-flux conditions is not well understood. In this paper, a laser heat flux technique is used to investigate the coating delamination crack propagation under realistic temperature-stress gradients and thermal cyclic conditions. The coating delamination mechanisms are investigated under various thermal loading conditions, and are correlated with coating dynamic fatigue, sintering and interfacial adhesion test results. A coating life prediction framework may be realized by examining the crack initiation and propagation driving forces for coating failure under high-heat-flux test conditions.

Zju, Dongming↗

DOE OSTI2025

Laser-induced slip casting as an additive manufacturing approach for silicon carbide

Here, this work presents processing silicon carbide (SiC) with the laser-induced slip casting (LIS) additive manufacturing (AM). SiC was stabilized in water with polyethyleneimine (PEI) dispersant, and SiC slurries were made with rheology for LIS printing. High-density ceramic parts were printed, followed by single-step binder burnout and sintering. The printed parts achieved 93–95 % of theoretical density. X-ray computed tomography (XCT) revealed a small distribution of flaws exceeding 100 microns. The mechanical properties were measured in both parallel and perpendicular to the printing layers, and the orientation with layers perpendicular to the bending moment resulted in higher strength compared to the parallel direction. Porosity resulting from processing and large inclusions of boron carbide (B4C) were the root cause of failure in the measured samples. Despite these defects through this effort, this new approach demonstrates promise for green forming of SiC with densities greater than 95 % theoretical and tensile strengths above 250 MPa.

Additive Manufacturing↗

NASA NTRSDate not supplied

3D Microwave Imaging of Impact Damage in Composites

This presentation presents the results of detecting impact damage in woven composites using a 3D microwave imaging system. The microwave results are compared to laser scanner results. After demonstrating the system on two composite samples, the multi-functionality of the system is discussed. They microwave systems ability to detect changes in permittivity of dielectrics is demonstrated by imaging RTV underneath space shuttle tiles, and the detection of sintered regolith simulant when buried in loose regolith simulant.

William (Cy) Wilson↗

NASA NTRS1986

NDE reliability and process control for structural ceramics

The reliability of microfocus x-radiography and scanning laser acoustic microscopy for detecting microvoids in silicon nitride and silicon carbide was statistically evaluated. Materials- and process-related parameters that influenced the statistical findings in research samples are discussed. The use of conventional x-radiography in controlling and optimizing the processing and sintering of an Si3N4-Si02-Y203 composition designated NASA 6Y is described. Radiographic evaluation and guidance helped develop uniform high-density Si3N4 modulus-of-rupture bars with improved four-point flexural strength (857, 544, and 462 MPa at room temperature, 1200 C, and 1370 C, respectively) and reduced strength scatter.

Baaklini, G. Y.↗

NASA NTRS1987

NDE reliability and process control for structural ceramics

The reliability of microfocus X-radiography and scanning laser acoustic microscopy for detecting microvoids in silicon nitride and silicon carbide was statistically evaluated. Materials- and process-related parameters that influenced the statistical findings in research samples are discussed. The use of conventional X-radiography in controlling and optimizing the processing and sintering of an Si3N4-SiO2-Y2O3 composition designated NASA 6Y is described. Radiographic evaluation and guidance helped develop uniform high-density Si3N4 modulus-of-rupture bars with improved four-point flexural strength (857, 544, and 462 MPa at room temperature, 1200 C, and 1370 C, respectively) and reduced strength scatter.

Baaklini, G. Y.↗

NASA NTRS1997

Thermal Fatigue Testing of ZrO2-Y2O3 Thermal Barrier Coating Systems using a High Power CO2 Laser

In the present study, the mechanisms of fatigue crack initiation and propagation, and of coating failure, under thermal loads that simulate diesel engine conditions, are investigated. The surface cracks initiate early and grow continuously under thermal Low Cycle Fatigue (LCF) and High Cycle Fatigue (HCF) stresses. It is found that, in the absence of interfacial oxidation, the failure associated with LCF is closely related to coating sintering and creep at high temperatures. Significant LCF and HCF interactions have been observed in the thermal fatigue tests. The fatigue crack growth rate in the ceramic coating strongly depends on the characteristic HCF cycle number, N*(sub NCF), which is defined as the number of HCF cycles per LCF cycle. The crack growth rate is increased from 0.36 microns/LCF cycle for a pure LCF test to 2.8 microns/LCF cycle for a combined LCF and HCF test at N*(sub NCF) about 20,000. A surface wedging model has been proposed to account for the HCF crack growth in the coating systems. This mechanism predicts that HCF damage effect increases with increasing surface temperature swing, the thermal expansion coefficient and the elastic modulus of the ceramic coating, as well as with the HCF interacting depth. A good agreement has been found between the analysis and experimental evidence.

Zhu, Dongming↗

NASA NTRS1985

Directed-energy process technology efforts

A summary of directed-energy process technology for solar cells was presented. This technology is defined as directing energy or mass to specific areas on solar cells to produce a desired effect in contrast to exposing a cell to a thermal or mass flow environment. Some of these second generation processing techniques are: ion implantation; microwave-enhanced chemical vapor deposition; rapid thermal processing; and the use of lasers for cutting, assisting in metallization, assisting in deposition, and drive-in of liquid dopants. Advantages of directed energy techniques are: surface heating resulting in the bulk of the cell material being cooler and unchanged; better process control yields; better junction profiles, junction depths, and metal sintering; lower energy consumption during processing and smaller factory space requirements. These advantages should result in higher-efficiency cells at lower costs. The results of the numerous contracted efforts were presented as well as the application potentials of these new technologies.

Alexander, P.↗

DOE OSTI2024

Electrophoretic deposition for improved trace element homogeneity in silica reference materials

Spatially-resolved analysis requires homogeneous reference materials (RMs) to make reliable quantitative measurements. Here we previously developed an electrophoretic deposition (EPD) method for fabrication of glassy microanalytical RMs with superior platinum-group element homogeneity **[1], and now include further dopants. For 39 trace elements, we analyzed dopant homogeneity in sintered silica (SiO 2 ) samples consolidated either mechanically by die-pressing (DP) or by EPD. A set of EPD and DP samples was made from each of two nanoparticle feedstocks produced by variations of the Stöber process **[2]. Spatially-resolved dopant distribution was characterized in all samples by laser-ablation inductively-coupled plasma mass spectrometry (LA-ICP-MS). In both sample sets, homogeneity of most trace elements was substantially improved by EPD relative to their DP counterpart.

36 MATERIALS SCIENCE↗

NASA NTRS1984

NDE for heat engine ceramics

Radiographic, ultrasonic, and scanning laser acoustic microscopy (SLAM) techniques were used to characterize silicon nitride and silicon carbide MOR bars in various stages of fabrication. Conventional and microfocus x-ray techniques were found capable of detecting minute high density inclusions in as-received powders, green compacts, and fully densified specimens. Significant density gradients in sintered bars were observed by radiography, ultrasonic velocity, and SLAM. Ultrasonic attenuation was found sensitive to microstructural variations due to grain and void morphology and distribution. SLAM was also capable of detecting voids, inclusions, and cracks in finished test bars. It was determined that thermoacoustic microscopy techniques have promise for application to green and densified ceramics.

Klima, S. J.↗

DOE OSTI2025

A snapshot of high-entropy alloy processing techniques and their effects on resulting mechanical properties

High-entropy alloys (HEAs) exhibit exceptional strength, corrosion resistance, and thermal stability, making them promising candidates for nuclear, aerospace, and other extreme applications. While most prior work has focused on compositional design, manufacturing techniques themselves can alter microstructure and mechanical properties as dramatically as alloy chemistry. This review compiles and compares the effects of processing routes—including arc melting, induction melting, mechanical alloying with spark plasma sintering, and additive manufacturing—on the structure and properties of HEAs. Quantitative comparisons highlight, for example, that SPS-processed alloys can achieve ∼20–45 % higher yield and tensile strength than arc-melted counterparts, while Bridgman solidification produces nearly single-crystal structures with elongation to failure exceeding 80 %. Additive manufacturing routes such as selective laser melting offer fine microstructures but also introduce anisotropy and porosity, leading to yield strengths spanning 100–600 MPa for the same composition. By synthesizing such results, this review provides actionable insight into how processing routes interact with HEA core effects (high entropy, lattice distortion, sluggish diffusion, and cocktail effect) to determine performance, thereby offering a practical guide for optimizing manufacturing strategies.

36 MATERIALS SCIENCE↗

NASA NTRS1986

NDE of advanced ceramics

Radiographic, ultrasonic, and scanning laser acoustic microscopy (SLAM) techniques were used to characterize silicon nitride and silicon carbide modulus-of-rupture test specimens in various stages of fabrication. Conventional and microfocus X-ray techniques were found capable of detecting minute high-density inclusions in as-received powders, green compacts, and fully densified specimens. Significant density gradients in sintered bars were observed by radiography, ultrasonic velocity, and SLAM. Ultrasonic attenuation was found sensitive to microstructural variations due to grain and void morphology and distribution. SLAM was capable also of detecting voids, inclusions, and cracks in finished test bars. Consideration is given to the potential for applying thermoacoustic microscopy techniques to green and densified ceramics. Some limitations and the detection probability statistics of the aforementioned nondestructive evaluation (NDE) processes are also discussed.

Klima, S. J.↗

NASA NTRS1986

NDE of structural ceramics

Radiographic, ultrasonic, scanning laser acoustic microscopy (SLAM), and thermo-acoustic microscopy techniques were used to characterize silicon nitride and silicon carbide modulus-of-rupture test specimens in various stages of fabrication. Conventional and microfocus X-ray techniques were found capable of detecting minute high density inclusions in as-received powders, green compacts, and fully densified specimens. Significant density gradients in sintered bars were observed by radiography, ultrasonic velocity, and SLAM. Ultrasonic attenuation was found sensitive to microstructural variations due to grain and void morphology and distribution. SLAM was also capable of detecting voids, inclusions and cracks in finished test bars. Consideration is given to the potential for applying thermo-acoustic microscopy techniques to green and densified ceramics. The detection probability statistics and some limitations of radiography and SLAM also are discussed.

Klima, S. J.↗