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DOE OSTI2022

Effect of thermal aging on corrosion behavior of duplex stainless steels

Abstract Despite their exceptional mechanical and corrosion properties, duplex stainless steels (DSS) have not found widespread use in high-temperature applications due to concerns over thermal aging and embrittlement at elevated operational temperatures (> 300 °C). The present study investigated the effect of thermal aging time on the electrochemical properties of lean and standard grade DSS that are exposed to a range of pressurized water reactors containing LiOH and H 3 BO 3 . The results indicated that the electrolyte chemistry plays a significant role in the corrosion behavior of the DSS alloys. Corrosion resistance decreased with thermal aging time for all DSS alloys; however, standard grade DSS (2205 and 2209-w) alloys showed better corrosion resistance than lean grades (2003, 2101, 2101-w). The presence of dissolved oxygen in the electrolytes resulted in a significant increase in corrosion rate for the DSS alloys, but it did not affect the general trend of corrosion rates with aging time. All DSS alloys became vulnerable to pitting corrosion due to chloride addition, but the pitting resistance decreased with increasing thermal aging time. Increased boron B content resulted in degradation of corrosion resistance of the DSS alloys, while minor changes in pH did not show a significant change in corrosion resistance. Mechanical and metallurgical characterization coupled with electrochemical characterization of the DSS alloys gave a comprehensive insight into the effects of thermal aging on the electrochemical response of the DSS. Graphical abstract

Murkute, Pratik (ORCID:0000000278636346)↗

DOE OSTI2020

Report Documenting Activity for Second Alloy 709 Commercial Heat

SUMMARY Qualification of the advanced austenitic stainless steel material Alloy 709 for use in Section III Division 5 of the American Society of Mechanical Engineers (ASME) Boiler and Pressure Vessel Code is being pursued by the US Department of Energy Advanced Reactor Technology Program. Qualification of this alloy will allow its use in design and construction of components for elevated temperature nuclear reactor systems. Code qualification requires extensive characterization of three commercial scale heats of the alloy. This report describes progress in procuring the second of three required heats of Alloy 709 plate from ATI Flat Rolled Products.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

NASA NTRS1992

Influence of the preshock temperature on shock effects in quartz

Shock metamorphic features are the prime indicators for recognizing impact phenomena on Earth and other planetary bodies. Although the pressure dependence of shock features is well known, information about the influence of the preshock temperature is almost lacking. Especially in the case of large-scale impacts like Sudbury, it is expected that deep-seated crustal rocks were subjected to shock at elevated temperatures. Therefore, we continued to perform shock experiments at elevated temperatures on less than 0.5-mm thin disks of single crystal quartz cut parallel to the (1010) face. All recovered quartz samples were investigated by universal stage, spindle stage, and a newly developed density gradient technique. Errors of refractive index and density measurements are +/- 0.0005 and +/- 0.002 g/cu cm respectively. Our investigations indicate that shock metamorphic features are strongly dependent on the preshock temperature. This statement has far-reaching implications with respect to shock wave barometry that is based on data from recovery experiments at room temperature. These datasets might be applicable only to low-temperature target rocks. Moreover, this study demonstrates that shock recovery experiments are definitely required for understanding the complete pressure-temperature regime of shock metamorphism on planetary bodies.

Langenhorst, F.↗

NASA NTRS1994

Influence of high pressure hydrogen environment on creep deformation of Mo-Re, Haynes 188, and NARloy-Z alloys

The present study focuses on the investigation of the influence of hydrogen on the mechanical properties of three types of alloys at elevated temperatures. The reasons for the consideration of hydrogen effects are the potential use of hydrogen as a coolant in gas-cooled reactors and fuel in advanced hypersonic vehicles. The materials used in hydrogen atmosphere must not be embrittled by hydrogen at ambient temperature and should have good strength in hydrogen atmosphere at elevated temperature. The paucity of information concerning the mechanical performance in hydrogen atmosphere at elevated temperature has been a limiting factor in the selection and design of structural components for operation in hydrogen environment.

Sastry, S. M. L.↗

DOE OSTI2021

Theoretical predictive screening of noble-metal-containing M 3 AuC 2 (M = Ti, V, and Cr) MAX phases

Using first-principles density functional theory (DFT), the ground state physical properties of the newly synthesized noble-metal-containing Ti 3 AuC 2 MAX phase have been investigated. The effect of transition-element Ti replacement (V and Cr) on physical properties, including structural, elastic, electronic, thermal, and optical are presented. The optimized lattice parameters of Ti 3 AuC 2 MAX phase are in good agreement with the experimental values and decrease when we replace Ti with V and then Cr. The magnetic properties of M 3 AuC 2 are predicted by using generalized gradient approximation (GGA) incorporating onsite electron correlation parameter (Hubbard U parameter) within DFT. Out of three studied MAX phases, V 3 AuC 2 and Cr 3 AuC 2 phases exhibit magnetism. The thermodynamical stability of M 3 AuC 2 (M = Ti, V, and Cr) phases is discussed by the formation enthalpy with respect to their most competing phases. The electronic structure reveals that these phases have metallic nature and are electrically anisotropic. The M-element replacement has an effect on the bonding properties of M 3 AuC 2 . The bonding between M-C is in the order of Cr 3 AuC 2 > V 3 AuC 2 > Ti 3 AuC 2 according to their peak positions and heights of density of states in the occupied site, which is also confirmed from the charge density distribution. The elastic properties indicate that M 3 AuC 2 phases are ductile, machinable, less stiff, and better resistant to thermal shock and are elastically anisotropic. To understand the properties of M 3 AuC 2 for the extreme environment, we employed a quasi-harmonic Debye model at the pressure and temperature range of 0–50 GPa and 0–1600 K, respectively. Additionally, we evaluated thermal conductivity and melting temperature to further understand the potential of these MAX phases in coating applications at elevated temperature. In relation to optical properties, these MAX phases have a reasonable absorption coefficient in the visible as well as in the ultra-violet regions. The reflectivity of M 3 AuC 2 phases is polarization dependent and of 45 % against the visible region, which reveals its potential as coating material to minimize solar heating.

312 MAX phases↗

DOE OSTI2025

Reactive Transport Modeling of Hydrogen Production from Serpentinization of Olivine

Hydrogen production from serpentinization of ultramafic rocks represents a promising natural pathway for generating carbon-free energy, yet its kinetics and controlling factors remain incompletely understood. A key challenge in advancing serpentinization research lies in the heterogeneity of porosity and permeability in rocks, which leads to nonuniform fluid velocity fields, as well as uncertainties in estimating reactive surface area and identifying appropriate mineral reaction equilibria. Additional complexities arise from the role of dissolved SiO 2 , Fe 2+ /Fe 3+ partitioning, and the limited effect of pH variations within the strongly alkaline regime on hydrogen yields. These challenges hinder straightforward extrapolation from laboratory tests to practical applications of hydrogen production from natural rocks. Here, in this work, we address these questions using a simulation-based reactive transport modeling framework calibrated against controlled laboratory experiments reported elsewhere. The model couples geochemical kinetics, multiphase flow, and mineralogical feedbacks, enabling systematic evaluation of how surface area, dissolved silica concentration, Fe redox state, temperature, and pressure govern serpentinization and H2 generation. We find that surface area exerts the strongest control on reaction rates and hydrogen yields, while Fe 2+ /Fe 3+ ratios act as secondary modulators. Elevated dissolved silica concentrations suppress hydrogen production but accelerate serpentine precipitation, whereas increasing pH beyond 12 within the strongly alkaline regime produces only marginal gains. Finally, we demonstrate that integrating targeted experiments with calibrated simulations offers a powerful and efficient approach for predicting hydrogen yields and assessing parameter trade-offs in industrial-scale applications. This integration can substantially reduce the experimental burden while improving predictive capability, thereby enhancing both the mechanistic understanding and the practical feasibility of hydrogen production from serpentinization.

08 HYDROGEN↗

NASA NTRS1979

Efficient solar cells by space processing

Thin films of electron beam evaporated silicon were deposited on molybdenum, tantalum, tungsten and molybdenum disilicide under ultrahigh vacuum conditions. Mass spectra from a quadrapole residual gas analyzer were used to determine the partial pressure of 13 residual gases during each processing step. Surface contamination and interdiffusion were monitored by in situ Auger electron spectrometry. The presence of phosphorus in the silicon was responsible for attaining elevated temperatures with silicide formations. Heteroepitaxial silicon growth was sensitive to the presence of oxygen during deposition, the rate and length of deposition as well as the substrate orientation.

Schmidt, F. A.↗

NASA NTRS1993

Extraction of oxygen from the Mars atmosphere using glow-discharge and permeation techniques

Oxygen can be extracted from carbon dioxide via thermal dissociation at elevated temperatures. However, temperatures in excess of 1000 K are needed to effect significant levels of dissociation. The experiments reported here have examined the feasibility of using a glow-discharge in low-pressure carbon dioxide to produce increased atomic oxygen yields at lower temperatures (on the order of 800 K). The experiments have shown that when silver membranes are used simultaneously as anodes for the glow discharge and as permeable membranes for oxygen separation, oxygen yields which are comparable to the permeation rates for pure oxygen, can be produced. Since the silver membrane can be employed as the electrode interface between Mars atmosphere and a stabilized-zirconia electrochemical pump, glow-discharge enhancement can be considered as a complementary technology which can be used with the zirconia-based oxygen extraction systems described previously by others. Not only can glow-discharge be used to increase oxygen yields at lowered temperatures, but it can also be considered as a possible way to avoid filtration and compression of Mars atmosphere, since the glow-discharge can be sustained in Mars ambient pressures.

Wu, Dongchuan↗

NASA NTRS2011

Thermal Stability of a 4 Meter Primary Reflector for the Scanning Microwave Limb Sounder

thermal distortion↗

DOE OSTI2020

Probing the surface chemistry for reverse water gas shift reaction on Pt(1 1 1) using ambient pressure X-ray photoelectron spectroscopy

Using ambient pressure XPS (APXPS), we explored carbon dioxide (CO 2 ) adsorption and CO 2 hydrogenation on Pt(1 1 1) single crystal surface to observe the activation of CO 2 and the subsequent reaction mechanism. In pure CO 2 , we observed CO adsorbates and adsorbed oxygen on Pt(1 1 1) derived from CO 2 dissociation at room temperature. The introduction of H 2 (at a pressure ratio of 1:1 (H 2 :CO 2 )) increased the production of CO across all temperatures by facilitating the removal of surface oxygen. As a consequence, the surface could expose sites that could then be utilized for producing CO. Under these conditions, the reverse water–gas shift (RWGS) reaction was observed starting at 300 °C. At higher H 2 partial pressure (10:1 (H 2 :CO 2 )), the RWGS reaction initiated at a lower temperature of 200 °C and continued to enhance the conversion of CO 2 with increasing temperatures. Our results revealed that CO 2 was activated on a clean Pt(1 1 1) surface through the dissociation mechanism to form adsorbed CO and O at room temperature and at elevated temperatures. Introducing H 2 facilitated the RWGS as adsorbed oxygen was consumed continuously to form H 2 O, and adsorbed CO desorbed from the surface at elevated temperatures. This work clearly provides direct experimental evidence for the surface chemistry of CO 2 dissociation and demonstrates how hydrogen impacts the RWGS reaction on a platinum surface.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2022

Creep and Fatigue Characterization of High Strength Alloy Thin Sections in Advanced CO2 Heat Exchangers

The objective of this work was to characterize and model elevated temperature creep and fatigue behavior for thin sheet and foil forms of gamma-prime strengthened alloys in wrought form and as-processed folded and brazed constructions. This work was motivated by the demanding temperature and pressure service conditions of the GEN3 Concentrated Solar Power (CSP) and supercritical CO2 (sCO2) power cycle working fluid. More specifically, the possibility of leveraging the superior creep strength of gamma-prime alloys in folded-fin and brazed-plate heat exchanger constructions. Gamma-prime alloys represent a step-change in raw-material strength over solid-solution strengthened alloys. And the folded-fin and brazed-plate heat exchanger architecture is lightweight and leverages cost-effective material stock forms. The investigation contained two parallel paths. (1) The first is referred to as a fundamental investigation where Oak Ridge National Laboratory conducts uniaxial creep testing on thin sheet and foil in wrought form. This effort aimed to serve as a benchmark against a relatively sparse existing database and a baseline comparison for path number 2. (2) The second path is referred to as the practical investigation where Brayton Energy manufactures plate-fin heat exchangers and performs pressurized creep and fatigue testing. This effort aimed to de-risk heat exchanger manufacturing process for service under sCO2 CSP conditions. A total of 14 uniaxial creep tests were completed using Haynes 282 thin sheet and foil. A variety of heat treatments were specified to coincide with path number 2. Baseline metallography of test samples and creep strength performance are contained. Benchmarks relatively to existing thick-form Haynes 282 are made, as well as to other thin-form Nickel-based superalloys. Description of a wrought-form modeling approach for thin gamma-prime alloys is also discussed. A total of 11 pressurized creep and fatigue tests were completed successfully with Haynes 282 heat exchanger prototypes. Manufacturing processing details, testing details, testing results, and failure analysis are discussed. Additionally, creep modeling techniques to predict failure are discussed, and modeling to support technological-to-market. In conclusion, Haynes 282 foils were demonstrated to yield rupture two-to-three orders of magnitude higher than Haynes 230 foils under similar conditions. And the manufactured heat exchanger prototypes demonstrated strength similar to the wrought constituents. Both of which contribute to elevated performance potential or cost savings in practice. Discussion is included.

14 SOLAR ENERGY↗

DOE OSTI2023

Numerical Investigation of the characteristics of pressurized biomass-oxy-combustion

As a second generation of oxy-fuel combustion technologies, pressurized oxy-combustion has a potential to improve the process efficiency and economy. With the modern decarbonization needs, biomass combustion is considered to be nearly CO2 neutral, and thus co-firing biomass with coal in an oxy-combustion process can achieve a negative CO2 balance. The size of the biomass fuel particles is a key parameter in an entrained flow combustor because large biomass particles, exceeding some threshold size, may only partially be burnt due to the restrictions on the heat transport, thereby diminishing the combustion efficiency. While such a threshold particle size has been scrutinized at an atmospheric pressure, the present study extends the analysis to elevated pressures. Specifically, two scenarios were set up, for experimental-scale and full-scale pressurized oxy-combustors, with the threshold sizes of biomass particles appearing 0.5 mm and 5 mm, respectively, without temperature gradient in biomass particles. With temperature gradient, the parametric study included the particles in the range from 0.15 mm to 5 mm. It is shown that the thermal-thin model is applicable to spherical biomass particles not exceeding 0.15 mm. The impact of the heating rate on biomass particle devolatilization was also investigated and the biomass devolatilization could happen in less than 1 second; the same amount of heat energy could induce different volatile release rates.

Li, Lei↗

NASA NTRS1972

Solid-gas phase equilibria and thermodynamic properties of cadmium selenide.

Accurate vapor pressures are determined through direct weight loss measurements using the Knudsen effusion technique. The experimental data are evaluated by establishing the mode of vaporization and determining the heat capacity of cadmium selenide at elevated temperatures. Additional information is obtained through a second- and third-law evaluation of data, namely, the heat of formation and the absolute entropy of cadmium selenide. A preferential loss of selenium during the initial heating of CdSe is observed, which leads to a deviation in stoichiometry.

Sigai, A. G.↗

DOE OSTI2022

Porosity evolution during heating of copper made from powder by friction extrusion

Here, friction extrusion was used to compact and extrude solid copper rod from feedstock powders. Following extrusion, considerable porosity was observed throughout the extrudate cross section due to the entrained porosity in the feedstock material and the extrusion process. The thermal stability of the extrudate was investigated via a series of heat treatments. Porosity evolution exhibited three distinct stages—an unchanged plateau (0°C–300°C) followed by an abrupt increase (400°C–500°C) and ultimately a reduction, as the temperature increases (>500°C). The peak porosity measured was ~25%. The underlying driving force for pore evolution is described as the competition between the internal pore pressure, material strength, and sintering kinetics, as a function of temperature. The observed porosity evolution and driving force are not expected to be limited to copper. Thus, this manuscript reveals an important consideration regarding elevated-temperature thermal stability as advanced manufacturing methods involving direct powder extrusion are explored.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Tetragonal BaCoO 3 : A Co 4+ Ferromagnetic Mott Insulator

We report the stabilization of the metastable body-centered tetragonal (BCT) phase of BaCoO 3 (BCT-BaCoO 3 ) under high-pressure (15 GPa) and hightemperature (1200 °C) conditions using a mixture precursor. This double perovskite adopts the EuTiO 3 -type structure (space group I4/mcm), as confirmed by powder Xray diffraction and high-resolution STEM. X-ray photoelectron spectroscopy indicates a predominant Co 4+ oxidation state without detectable oxygen vacancies. Magnetization and heat capacity measurements reveal ferromagnetic ordering at T C ∼ 107 K, attributable to the BCT-BaCoO 3 phase. Above this temperature, the mixed-phase sample exhibits Curie−Weiss paramagnetism, a low-spin to high-spin crossover upon cooling, and a possible intermediate-spin state at elevated temperatures. Resistivity data indicates insulating behavior with weak magnetoresistance. DFT and DFT + DMFT calculations suggest that the insulating state originates from an orbitally selective transition sensitive to the nominal valence of the Co-d shell. The metastable BCT-BaCoO 3 phase cannot be retained in pure form at ambient pressure but can be stabilized by embedding it in a disordered mixture, offering a potential route to discover and preserve other high-pressure phases under ambient conditions.

Magnetic properties↗

NASA NTRS1988

Improved Li/BCX (thionyl chloride) cells for space applications

New NASA requirements for the screening of lithium cells for space applications involve thermal soaks at elevated temperatures (149 C). The BCX DD and C size cells have been redesigned to pass this test with only marginal losses in capacity as was done previously for the D cells. In addition, the pressure increases in cells subjected to this high temperature environment have been characterized showing that the earlier designs failed this exposure due to lack of void volume. An improve BCX chemistry has been demonstrated which significantly improves voltage delay problems encountered after partial discharge and storage of the cells.

Clark, W. D. K.↗

NASA NTRS1999

Chemical Vapor Deposition at High Pressure in a Microgravity Environment

In this paper we present an evaluation of critical requirements of organometallic chemical vapor deposition (OMCVD) at elevated pressure for a channel flow reactor in a microgravity environment. The objective of using high pressure is to maintain single-phase surface composition for materials that have high thermal decomposition pressure at their optimum growth temperature. Access to microgravity is needed to maintain conditions of laminar flow, which is essential for process analysis. Based on ground based observations we present an optimized reactor design for OMCVD at high pressure and reduced gravity. Also, we discuss non-intrusive real-time optical monitoring of flow dynamics coupled to homogeneous gas phase reactions, transport and surface processes. While suborbital flights may suffice for studies of initial stages of heteroepitaxy experiments in space are essential for a complete evaluation of steady-state growth.

McCall, Sonya↗

NASA NTRS2011

A Deployable 4 Meter 180 to 680 GHz Antenna for the Scanning Microwave Limb Sounder

The Scanning Microwave Limb Sounder (SMLS) is a space-borne heterodyne radiometer which will measure pressure, temperature and atmospheric constituents from thermal emission between 180 and 680 GHz. SMLS, planned for the Global Atmospheric Composition Mission of the NRC Decadal Survey, uses a novel toric Cassegrain antenna to perform both elevation and azimuth scanning. These provide better horizontal and temporal resolution and coverage than were possible with elevation-only scanning at typical Low-Earth orbit spacing in the two previous MLS satellite instruments. Development of the SMLS antenna was the focus of a 2006 Small Business Innovative Research (SBIR) program whose phase II culminated in the fabrication and thermal stability testing of a composite demonstration model of the SMLS primary reflector. This reflector has the full 4m height and 1/3 the width planned for flight. An Instrument Incubator Program (IIP) titled "A deployable 4 Meter 180 to 680 GHz antenna for the Scanning Microwave Limb Sounder" continues development of the SMLS antenna with the study of 5 topics: 1) detailed mathematical modeling of the antenna patterns from which we simulate geophysical parameter retrievals in order to establish FOV performance requirements; 2) thorough correlation of finite element model predictions with measurements made on the SBIR reflector. We will again measure deformations of this reflector, under more flight-like thermal gradients, using higher precision metrology techniques available in a new large-aperture facility at JPL; 3) fabrication of a full-width primary reflector whose asbuilt surface figure will better meet the figure requirements of SMLS than did the SBIR reflector; 4) integration of the primary with other reflectors, and with residual front ends built in a 2007 IIP, in a breadboard antenna; and finally 5) RF testing of the breadboard on a Near Field Range at JPL. We report on significant progress in 3 areas of the current IIP: development of the mathematical model to predict SMLS antenna patterns and their application in a preliminary set of geophysical retrievals; the correlation between surface deformation predicted by finite element models and measurement in the 2009 isothermal stability tests of the SBIR, with implications for the thermal gradient testing to be performed at JPL; and aspects of the conceptual design of the full-width primary reflector to be fabricated and tested in the 2nd and 3rd years of the IIP.

heterodyne radiometer↗