Results for “In situ processing” — Page 99

DOE OSTI2020

Correlation of SWIR imaging with LPBF 304L stainless steel part properties

In the Laser Powder Bed Fusion (LPBF) process, the local thermal history can vary significantly over a part as the heat transfer characteristics and the laser scan path are geometry dependent. The variations introduce the potential for defects that lead to part failure, some of which are difficult to identify non-destructively with common ex-situ evaluation techniques. These defects include significant microstructural and mechanical property differences in the part interiors. In this paper, thermal features are extracted from in-situ Short-Wave Infrared (SWIR) imaging measurements to compile voxel based part representations and understand how the complexities in the thermal history affect part performance. The deviations in thermal features due to different laser processing parameters and complex scan pathing are explored. Empirical correlations are developed to map thermal features with the engineering properties (bulk yield strength, area percentage porosity, and local state) of 304L stainless steel parts manufactured by LPBF. Processing modes (insufficient melting and keyholing) are determined by mapping part property measurements with multiple thermal features. Generating the relationships between thermographic measurements and resulting SLM part properties lays the foundation for in-situ part qualification.

36 MATERIALS SCIENCE↗

NASA NTRS2010

In Situ Instrumentation for Sub-Surface Planetary Geochemistry

Novel instrumentation is under development at NASA's Goddard Space Flight Center, building upon earth-based techniques for hostile environments, to infer geochemical processes important to formation and evolution of solid bodies in our Solar System. A prototype instrument, the Pulsed Neutron Generator Gamma Ray and Neutron Detectors (PNG-GRAND), has a 14 MeV pulsed neutron generator coupled with gamma ray and neutron detectors to measure quantitative elemental concentrations and bulk densities of a number of major, minor and trace elements at or below the surfaces with approximately a meter-sized spatial resolution down to depths of about 50 cm without the need to drill. PNG-GRAND's in situ a meter-scale measurements and adaptability to a variety of extreme space environments will complement orbital kilometer-scale and in-situ millimeter scale elemental and mineralogical measurements to provide a more complete picture of the geochemistry of planets, moons, asteroids and comets.

Bodnarik, J.↗

NASA NTRS2013

Evaluation of GEOS-5 Sulfur Dioxide Simulations During the Frostburg, MD 2010 Field Campaign.

Sulfur dioxide (SO2) is a major atmospheric pollutant with a strong anthropogenic component mostly produced by the combustion of fossil fuel and other industrial activities. As a precursor of sulfate aerosols that affect climate, air quality, and human health, this gas needs to be monitored on a global scale. Global climate and chemistry models including aerosol processes along with their radiative effects are important tools for climate and air quality research. Validation of these models against in-situ and satellite measurements is essential to ascertain the credibility of these models and to guide model improvements. In this study the Goddard Chemistry, Aerosol, Radiation, and Transport (GOCART) module running on-line inside the Goddard Earth Observing System version 5 (GEOS-5) model is used to simulate aerosol and SO2 concentrations. Data taken in November 2010 over Frostburg, Maryland during an SO2 field campaign involving ground instrumentation and aircraft are used to evaluate GEOS-5 simulated SO2 concentrations. Preliminary data analysis indicated the model overestimated surface SO2 concentration, which motivated the examination of mixing processes in the model and the specification of SO2 anthropogenic emission rates. As a result of this analysis, a revision of anthropogenic emission inventories in GEOS-5 was implemented, and the vertical placement of SO2 sources was updated. Results show that these revisions improve the model agreement with observations locally and in regions outside the area of this field campaign. In particular, we use the ground-based measurements collected by the United States Environmental Protection Agency (US EPA) for the year 2010 to evaluate the revised model simulations over North America.

Air Quality Campaign↗

NASA NTRSDate not supplied

Pt/HTCC Alumina based Electronic Packaging System and Integration Processes for High Temperature Harsh Environment Applications

Electronic devices capable of operation at 500°C are required for long term Venus surface missions, as well as for in situ monitoring and control of next generation aeronautical engines. High temperature sensors and electronics can also find many applications in military, and energy and automobile industries. Various silicon carbide (SiC) sensors and electronic devices have been developed for operation at 500 °C, and a compatible packaging system is needed for long term test and deployment of these high temperature devices. High temperature co-fired ceramics (HTCC) alumina with platinum (Pt) conductor was proposed for high temperature electronic packaging. A prototype Pt/HTCC alumina packaging system including chip-level package and circuit board has been briefly reported previously for long-term electrical testing of SiC integrated circuits at 500 °C, and brief testing at much higher temperatures. HTCC alumina is an excellent dielectric material with acceptable dielectric constant and low dielectric loss over wide temperature and frequency ranges. Pt is chemically noble and can be co-fired with HTCC alumina in air ambient producing a viable electronic packaging material system for high temperature applications. This paper presents a more detailed description of this packaging system including prototype low power packages and circuit boards based on HTCC alumina and Pt metallization for 500°C and other harsh environment applications. The key technical considerations for chip-level packaging and circuit board assembly, including materials and processes for 500 °C durable wire-bonding and SiC die attach, and integration of multi-chip circuit boards, are presented. Experimental test results of this packaging approach applied to SiC integrated circuits at 500 °C and 700°C are discussed as well.

High temperature↗

NASA NTRSDate not supplied

Pt/HTCC Alumina based Electronic Packaging System and Integration Processes for High Temperature Harsh Environment Applications

Electronic devices capable of operation at 500°C are required for long term Venus surface missions, as well as for in situ monitoring and control of next generation aeronautical engines. High temperature sensors and electronics can also find many applications in military, and energy and automobile industries. Various silicon carbide (SiC) sensors and electronic devices have been developed for operation at 500 °C, and a compatible packaging system is needed for long term test and deployment of these high temperature devices. High temperature co-fired ceramics (HTCC) alumina with platinum (Pt) conductor was proposed for high temperature electronic packaging. A prototype Pt/HTCC alumina packaging system including chip-level package and circuit board has been briefly reported previously for long-term electrical testing of SiC integrated circuits at 500 °C, and brief testing at much higher temperatures. HTCC alumina is an excellent dielectric material with acceptable dielectric constant and low dielectric loss over wide temperature and frequency ranges. Pt is chemically noble and can be co-fired with HTCC alumina in air ambient producing a viable electronic packaging material system for high temperature applications. This paper presents a more detailed description of this packaging system including prototype low power packages and circuit boards based on HTCC alumina and Pt metallization for 500°C and other harsh environment applications. The key technical considerations for chip-level packaging and circuit board assembly, including materials and processes for 500 °C durable wire-bonding and SiC die attach, and integration of multi-chip circuit boards, are presented. Experimental test results of this packaging approach applied to SiC integrated circuits at 500 °C and 700°C are discussed as well.

electronic packaging↗

NASA NTRS2001

Ice Nucleation in Deep Convection

The processes controlling production of ice crystals in deep, rapidly ascending convective columns are poorly understood due to the difficulties involved with either modeling or in situ sampling of these violent clouds. A large number of ice crystals are no doubt generated when droplets freeze at about -40 C. However, at higher levels, these crystals are likely depleted due to precipitation and detrainment. As the ice surface area decreases, the relative humidity can increase well above ice saturation, resulting in bursts of ice nucleation. We will present simulations of these processes using a large-eddy simulation model with detailed microphysics. Size bins are included for aerosols, liquid droplets, ice crystals, and mixed-phase (ice/liquid) hydrometers. Microphysical processes simulated include droplet activation, freezing, melting, homogeneous freezing of sulfate aerosols, and heterogeneous ice nucleation. We are focusing on the importance of ice nucleation events in the upper part of the cloud at temperatures below -40 C. We will show that the ultimate evolution of the cloud in this region (and the anvil produced by the convection) is sensitive to these ice nucleation events, and hence to the composition of upper tropospheric aerosols that get entrained into the convective column.

Jensen, Eric↗

DOE OSTI2025

A Universal Design of Lithium Anode via Dynamic Stability Strategy for Practical All‐Solid‐State Batteries

Abstract All‐solid‐state Li‐metal battery (ASSLB) chemistry with thin solid‐state electrolyte (SSE) membranes features high energy density and intrinsic safety but suffers from severe dendrite formation and poor interface contact during cycling, which hampers the practical application of rechargeable ASSLB. Here, we propose a universal design of thin Li‐metal anode (LMA) via a dynamic stability strategy to address these issues. The ultra‐thin LMA (20 μm) is in situ constructed with uniform highly Li‐ion conductive solid‐electrolyte interphase and composite‐polymer interphase (CPI) via electroplating process. As a result, the passivation layer with poor Li‐ion conduction on Li anode can be dissolved and small surface resistance can be achieved due to the good compatibility of CPI to SSEs. The cycling of Li symmetric cell with Li 6 PS 5 Cl thin film electrolyte (<100 μm) shows a high critical current density of >2.0 mA cm −2 with excellent cycling stability at 1.0 mA cm −2 . The ASSLBs paring with Ni‐rich LiNi 0.6 Mn 0.2 Co 0.2 O 2 cathode demonstrated the feasibility of engineered LMA design by presenting good rate capability from 0.1 C to 1.0 C at room temperature, as well as long‐term cycling stability (81 % retention after 100 cycles). This work represents a general pathway to make thin dendrite‐free LMA available for high‐energy‐density ASSLBs.

Deng, Tao [Department of Chemical and Biomolecular↗

DOE OSTI2025

A Universal Design of Lithium Anode via Dynamic Stability Strategy for Practical All‐Solid‐State Batteries

Abstract All‐solid‐state Li‐metal battery (ASSLB) chemistry with thin solid‐state electrolyte (SSE) membranes features high energy density and intrinsic safety but suffers from severe dendrite formation and poor interface contact during cycling, which hampers the practical application of rechargeable ASSLB. Here, we propose a universal design of thin Li‐metal anode (LMA) via a dynamic stability strategy to address these issues. The ultra‐thin LMA (20 μm) is in situ constructed with uniform highly Li‐ion conductive solid‐electrolyte interphase and composite‐polymer interphase (CPI) via electroplating process. As a result, the passivation layer with poor Li‐ion conduction on Li anode can be dissolved and small surface resistance can be achieved due to the good compatibility of CPI to SSEs. The cycling of Li symmetric cell with Li 6 PS 5 Cl thin film electrolyte (<100 μm) shows a high critical current density of >2.0 mA cm −2 with excellent cycling stability at 1.0 mA cm −2 . The ASSLBs paring with Ni‐rich LiNi 0.6 Mn 0.2 Co 0.2 O 2 cathode demonstrated the feasibility of engineered LMA design by presenting good rate capability from 0.1 C to 1.0 C at room temperature, as well as long‐term cycling stability (81 % retention after 100 cycles). This work represents a general pathway to make thin dendrite‐free LMA available for high‐energy‐density ASSLBs.

Deng, Tao [Department of Chemical and Biomolecular↗

DOE OSTI2025

Interaction between dissolution and precipitation during olivine carbonation: Implications for CO 2 mineralization

Large-scale carbonation of olivine is considered a promising approach for in situ mineral carbonation, offering a permanent and stable method for CO 2 storage. A critical aspect of this process is understanding how dissolution and precipitation interact, as this could drive fracturing and enhance further reactions. In this study, we conducted carbonation experiments on olivine using CO 2 -saturated aqueous solutions of NaHCO 3 and NaCl. Two experimental setups were used: one representing an open geochemical system and the other a closed system, corresponding to reaction-limited and flow-limited scenarios, respectively. Further, post-reaction textural analysis using scanning electron microscopy (SEM) revealed surface coatings of reaction products in the closed system, while etch pits and etch channels were prevalent in the open system. Although no direct evidence of reaction-driven fracturing was observed, etch pits and etch channels may serve as initiation points for subcritical crack formation and growth, potentially maintaining permeability and exposing new unreacted surfaces. Using linear elastic fracture mechanics (LEFM) model, we estimate that microcracks could propagate under a pressure of 0.1 GPa if reaction products accumulate within the etch pits. Our findings offer new insights into the mechanisms governing olivine carbonation.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2025

A novel approach to increase accuracy in remotely sensed evapotranspiration through basin water balance and flux tower constraints

Remote sensing-derived evapotranspiration (RSET) products capture the spatiotemporal variations of evapotranspiration (ET) from field to basin scales with unprecedented details. However, their accuracy varies across RSET estimation methods and diverse hydroclimate regions. While ET modeling efforts to account for biophysical processes and controlling parameters have made good progress in recent years, a parallel approach of integrating in-situ ET with RSET could reduce biases in RSET products. Basin water balance ET (WBET) and flux tower ET are widely applied to evaluate RSET accuracy, yet such ET measurements are rarely used for RSET bias corrections, especially for large area applications. To address this issue, we propose a novel approach: the water balance equivalence (WABE) method, which generates spatially continuous WBET for correcting biases in RSET products. The WABE method computes synthetic WBET by integrating observed WBET and flux tower-derived FLUXCOM ET, which fills the spatial gaps of observed WBET and generates a spatially continuous WBET dataset. Synthetic WBET (2002–2015 annual average) of eight-digit hydrologic unit code (HUC8) basins across the conterminous United States (CONUS), constituting 44 % (887 out of 2035 basins) of CONUS basins, was determined within 2.0 % (RMSE = 12 %) of observed WBET at CONUS and between 1–12 % (RMSE = 3–33 %) across 18 regions in CONUS. With WABE-based bias corrections, the overall annual bias of RSET decreased from 10 % (RMSE = 34 %) to 6 % (RMSE = 26 %) across 37 flux tower sites. The WABE method offers a new approach for RSET accuracy improvement and shows great promise for large area implementations with a potential to yield substantial benefits for building accurate basin water budgets and water management decisions.

Khand, Kul↗

DOE OSTI2023

Inhibit the strain accumulation for 5V spinel cathode by mitigating the phase separation during high voltage stage

LiNi 0.5 Mn 1.5 O 4 (LNMO) spinel cathode is a potential cathode material for high-power, low-cost lithium-ion batteries (LIBs) due to its low raw material cost, high operating voltage and efficient lithium-ion transport channel. However, LNMO suffers from structural stability due to the two-phase-transformation during charge/discharge process, leading to poor cycling performance. Here, to address the issues, we have constructed a homogeneous aggregated LNMO cathode with a multifaceted primary particle, namely the LNMO with single-crystal secondary particles (SSP LNMO). Ex situ and in situ characterizations including the synchrotron X-ray diffraction, the neutron diffraction and full pouch cell validated that the SSP LNMO exhibit a single solid-solution reactions with a restrained lattice evolution during the delithiation/lithiation process. This is in contrast to the normal LNMO cathode, which demonstrates a significant two-phase transition from spinel Li 1-x Ni 0.5 Mn 1.5 O 4 to rock-salt MnO 2 at high voltage. Therefore, the SSP LNMO has greatly improved cycle life compared to the normal LNMO cathode. Overall, this study demonstrates the possibility of constructing LNMO based on primary-grain morphology modulation to improve the intrinsic stability of LIBs.

25 ENERGY STORAGE↗

DOE OSTI2025

Aldehyde cool-flame chemistry explains a missing source of organic acids

Combustion emission is a significant source of organic acids, impacting atmospheric chemistry and climate. Their formation mechanisms, however, remain poorly understood, leading to underestimation in kinetic models. We investigate the cool-flame oxidation of key combustion intermediates—C 1 –C 4 aldehydes and benzaldehyde. Using in-situ synchrotron vacuum ultraviolet photoionization mass spectrometry, we observe the direct conversion of aldehydes to organic acids, a process enhanced by HO 2 radicals. Quantum chemistry calculations reveal that the reaction of RC(O)O 2 with HO 2 on the singlet potential energy surface contributes to organic acids. Incorporating this pathway into a kinetic model significantly improves organic acid prediction. Despite the high-temperature nature of engine combustion, significant spatial and temporal inhomogeneities (e.g., near-wall regions and crevice volumes) lead to localized cool-flame conditions, facilitating organic acid formation and emission. Elucidating the acid formation under cool-flame conditions provides a critical mechanism for accurately modelling anthropogenic organic acid emissions and developing mitigation strategies.

SVUV-PIMS↗

DOE OSTI2022

A combined TEM and SAXS study of the growth and self-assembly of ultrathin Pt nanowires

Ultrathin Pt nanowires possess high activity for various electrocatalytic applications. However, little work has focused on understanding their growth mechanisms. Herein, we utilize a combination of time-dependent, ex situ transmission electron microscopy (TEM) and small angle x-ray scattering (SAXS) techniques to observe the growth process in addition to associated surfactant-based interactions. TEM images indicate that initially nanoparticles are formed within 30 s; these small 'seed' particles quickly elongate to form ultrathin nanowires after 2 min. These motifs remain relatively unchanged in size and shape up to 480 min of reaction. Complementary SAXS data suggests that the initial nanoparticles, which are coated by a surfactant bilayer, arrange into a bcc superlattice. With increasing reaction time, the bcc lattice disappears as the nanoparticles grow into nanowires, which then self-assemble into a columnar hexagonal structure in which the individual nanowires are covered by a CTAB monolayer. The hexagonal structure eventually degrades, thereby leading to the formation of lamellar stacking phases comprised of surfactant bilayers. To the best of our knowledge, this is the first time that SAXS has been used to monitor the growth and self-assembly of Pt nanowires. In conclusion, these insights can be used to better understand and rationally control the formation of anisotropic motifs of other metallic nanostructures.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2025

Interface-sensitive microwave loss in superconducting tantalum films sputtered on c-plane sapphire

Quantum coherence in superconducting circuits has increased steadily over the last decades because of a growing understanding of the various loss mechanisms. Recently, tantalum (Ta) emerged as a promising material to address microscopic sources of loss found on niobium (Nb) or aluminum (Al) surfaces. However, the effects of film and interface microstructure on low-temperature microwave loss are still not well understood. Here, in this study, we present a systematic study of the structural and electrical properties of Ta and Nb films sputtered on c-plane sapphire at varying growth temperatures. As growth temperature was increased, our results show that the onset of epitaxial growth of α -phase Ta correlates with lower Ta surface roughness, higher critical temperature, and higher residual resistivity ratio, but surprisingly also correlates with a significant increase in loss at microwave frequency. Notably, this high level of loss is not observed in Nb films prepared in the same way and having very similar structure. By experimentally controlling the surface on which the Ta film is nucleated, we determine that the source of loss was only present in samples having an epitaxial Ta/sapphire interface and show that it was apparently mitigated by either growing a thin, epitaxial Nb interlayer between the Ta film and the substrate or by intentionally treating, and effectively damaging, the sapphire surface with an in situ argon plasma before Ta growth. In addition to elucidating this interfacial microwave loss, this work provides adequate process details to aid reproducible growth of low-loss Ta films across fabrication facilities.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2022

Revisiting metastable immiscibility in SiO 2 –Al 2 O 3 : Structure and phase separation of supercooled liquids and glasses

Understanding and controlling liquid–liquid phase separation in aluminosilicates is crucial for optimizing glass properties. However, the metastable nature of aluminosilicates’ phase separation has made it difficult to study experimentally, and uncertainty persists regarding the compositional and temperature extents of the miscibility gap. Here, we present new experimental evidence that suggests a consolute temperature between 1440 and 1590°C and endmember compositions of 7 and 62 mol.% Al 2 O 3 for the phase-separated glasses. Using containerless melt processing, deeply supercooled liquids over the 0–60 mol.% Al 2 O 3 range are probed with in situ small- and wide-angle X-ray scattering, which simultaneously reveals changes in nanoscale density heterogeneity and atomic structure. Correlations between phase separation and atomic coordination environments are compared for liquids and glasses. Pair distribution function analysis shows mean O–(Si + Al) coordination increases with Al 2 O 3 content and decreases with temperature.

36 MATERIALS SCIENCE↗

DOE OSTI2025

A low-temperature, one-step synthesis for monazite can transform monazite into a readily usable advanced nuclear waste form

It has been demonstrated that monazite-type materials are excellent candidates for nuclear waste forms, and hence, their facile synthesis is of great importance for the needed sequestration of existing nuclear waste. The synthesis of monazite, LaPO 4 , requires inconveniently high temperatures near 1000°C and generally involves the conversion of the presynthesized rhabdophane, LaPO 4 •nH 2 O, to the LaPO 4 monazite phase. During this structure transformation, the rhabdophane converts irreversibly to the thermodynamically stable monoclinic monazite structure. A low-temperature (185° to 260°C) mild hydrothermal acid-promoted synthesis of monazite is described that can both transform presynthesized rhabdophane or assemble reagents to the monoclinic monazite structure. The pH dependence of this reaction is detailed, and its applicability to the LnPO 4 (Ln = La, Ce, Pr, Nd, Sm-Gd), Ca 0.5 Th 0.5 PO 4 , and Sr 0.5 Th 0.5 PO 4 systems is discussed. The crystal growth of Ca 0.5 Th 0.5 PO 4 and Sr 0.5 Th 0.5 PO 4 is described, and their crystal structures were reported. In situ x-ray diffraction studies, performed as a function of temperature, provide insight into the structure transformation process.

Biogeochemistry↗

DOE OSTI2024

In situ potassium and hydrogen ion exchange into a cubic zirconium silicate microporous material

The selective separation of ions from aqueous systems, and even in the human body, is a crucial to overall environmental management and health. Nanoporous materials are widely known for their selective removal of cations from aqueous media, and therefore have been targeted for use as a pharmaceutical to treat hyperkalemia. This study investigated the detailed crystallographic molecular mechanisms that control the potassium ion selectivity in the nanoporous cubic zirconium silicate (CZS) related materials. Using time-resolved in situ Raman spectroscopy and time-resolved in situ X-ray diffraction, the selectivity mechanisms were determined to involve a synchronous cation-cation repulsion process that serves to open a favorable coordination bonding environment for potassium, not unlike the ion selectivity filter process found in potassium ion channels in proteins. Enhancement of ion exchange was observed when the CZS material was in a partial protonated state (≈3:1 Na:H), causing an expansion of the unit-cell volume, enlargement of the 7 member-ring window, and distortion of framework polyhedra, which allowed increased accessibility to the cage structures and resulted in rapid irreversible potassium ion exchange.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2022

Vehicle Technology Office Battery Project (FY22Q4 Quarterly Report)

The project has two primary objectives: (1) down select three-dimensional (3D) printing and post-processing approaches for solid-state electrolyte (SSE) / cathode integration, and (2) understand battery failure mechanisms via ex situ and in situ characterization.

25 ENERGY STORAGE↗