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DOE OSTI2020

Elevated-temperature cyclic properties of advanced manufactured materials

Microreactor developers at the 2019 GAIN Microreactors workshop expressed a need for advanced manufacturing to fabricate microreactor components. Powder metallurgy (PM) hot isostatic pressing (HIP) is more mature than other advanced manufacturing techniques for the following reasons: 1. a code case exists for Section III, Division 1, Subsection NB components of light water reactors to be manufactured using PM HIP Alloy 316L, and 2. tensile and creep properties have been shown to be equivalent to wrought material for Type 316 stainless steel and Grade 91. Thus, PM HIP is more readily deployable in the near term. Elevated-temperature cyclic properties of PM-HIP materials, however, have not been established. The scope of testing for Code qualification could be significantly reduced compared to a new material for the following reasons: 1. only a limited amount of time consuming creep testing would be required, and 2. testing of fatigue and creep-fatigue behavior could be reduced if it can be demonstrated that the properties are comparable to wrought material. The objective of this work package is to develop an understanding of the relationship of advanced materials processing on the material characteristics as they relate to elevated-temperature component design and construction. This will be achieved by the following: • Elevated-temperature fatigue and creep-fatigue testing of PM HIP and wrought Alloy 316L. • Fracture and microstructural characterization of the PM HIP and wrought Alloy 316L. • Analysis of the elevated-temperature fatigue and creep-fatigue properties of PM HIP Alloy 316L. • Draft a report evaluating the elevated-temperature fatigue and creep-fatigue properties of PM HIP Alloy 316L. • Pursue procurement of Alloy 316H and Grade 91 manufactured using PM HIP. • Initiate scoping studies of the procured Alloy 316H or Grade 91 manufactured using PM HIP contingent upon successful material procurement.

36 MATERIALS SCIENCE↗

NASA NTRS1989

Static tensile and tensile creep testing of four boron nitride coated ceramic fibers at elevated temperatures

Six types of uncoated ceramic fibers were static tensile and tensile creep tested at various elevated temperatures. Three types of boron nitride coated fibers were also tested. Room temperature static tensile tests were initially performed on all fibers, at gage lengths of 1, 2, and 4 inches, to determine the magnitude of end effects from the gripping system used. Tests at one elevated temperature, at gage lengths of 8 and 10 inches, were also conducted, to determine end effects at elevated temperatures. Fiber cross sectional shapes and areas were determined using scanning electron microscopy. Creep testing was typically performed for 4 hours, in an air atmosphere.

Coguill, Scott L.↗

DOE OSTI2020

Stimulation of Insect Herbivory by Elevated Temperature Outweighs Protection by the Jasmonate Pathway

Rising global temperatures are associated with increases in the geographic range, population size, and feeding voracity of insect herbivores. Although it is well established that the plant hormone jasmonate (JA) promotes durable resistance to many ectothermic herbivores, little is known about how JA-mediated defense is influenced by rising temperatures. Here, we used the Arabidopsis-Trichoplusia ni (cabbage looper) interaction to investigate the relative contribution of JA and elevated temperature to host resistance. Video monitoring of T. ni larval behavior showed that elevated temperature greatly enhanced defoliation by increasing the bite rate and total time spent feeding, whereas loss of resistance in a JA-deficient mutant did not strongly affect these behaviors. The acceleration of insect feeding at elevated temperature was not attributed to decreases in wound-induced JA biosynthesis, expression of JA-responsive genes, or the accumulation of defensive glucosinolates prior to insect challenge. Quantitative proteomic analysis of insect frass, however, provided evidence for a temperature-dependent increase in the production of T. ni digestive enzymes. Our results demonstrate that temperature-driven stimulation of T. ni feeding outweighs the protective effects of JA-mediated resistance in Arabidopsis, thus highlighting a potential threat to plant resilience in a warming world.

59 BASIC BIOLOGICAL SCIENCES↗

NASA NTRSDate not supplied

Nb-1Zr L-PBF In-situ Alloying and Elevated Temperature Mechanical Performance

Nb-1Zr is a readily-fabricable, dispersion-strengthened niobium alloy with improved elevated temperature properties compared to commercially pure niobium. This moderate strength niobium alloy is desirable in thermal management systems for fission power and propulsion applications; however, pre-alloyed spherical feedstock is generally unavailable. Laser powder bed fusion (L-PBF) in-situ alloying of a Nb-1Zr chemistry was performed using a pure niobium feedstock coated with 1 wt% of zirconium-based ceramic compound nano-powders. The additively manufactured material was mechanically tested at elevated temperatures in a controlled environment in the as-built condition. For comparison, traditionally manufactured wrought feedstock was also tested under identical conditions. Examination of the materials’ microstructure and elevated temperature mechanical response aimed to determine the Zr-compound nano-powder addition with the best performance, and the overall feasibility of the in-situ alloying approach.

Niobium-based alloys↗

NASA NTRS1988

Static tensile and tensile creep testing of five ceramic fibers at elevated temperatures

Static tensile and tensile creep testing of five ceramic fibers at elevated temperature was performed. J.P. Stevens, Co., Astroquartz 9288 glass fiber, Nippon Carbon, Ltd., (Dow Corning) Nicalon NLM-102 silicon carbide fiber, and 3M Company Nextel 312, 380, and 480 alumina/silica/boria fibers were supplied in unsized tows. Single fibers were separated from the tows and tested in static tension and tensile creep. Elevated test temperatures ranged from 400 to 1300 C and varied for each fiber. Room temperature static tension was also performed. Computer software was written to reduce all single fiber test data into engineering constants using ASTM Standard Test Method D3379-75 as a reference. A high temperature furnace was designed and built to perform the single fiber elevated temperature testing up to 1300 C. A computerized single fiber creep apparatus was designed and constructed to perform four fiber creep tests simultaneously at temperatures up to 1300 C. Computer software was written to acquire and reduce all creep data.

Zimmerman, Richard S.↗

NASA NTRS1989

Static tensile and tensile creep testing of five ceramic fibers at elevated temperatures

Static tensile and tensile creep testing of five ceramic fibers at elevated temperature was performed. J.P. Stevens, Co., Astroquartz 9288 glass fiber; Nippon Carbon, Ltd., (Dow Corning) nicalon NLM-102 silicon carbide fiber; and 3M Company Nextel 312, 380, and 480 alumina/silica/boria fibers were supplied in unsized tows. Single fibers were separated from the tows and tested in static tension and tensile creep. Elevated test temperatures ranged from 400 C to 1300 C and varied for each fiber. Room temperature static tension was also performed. Computer software was written to reduce all single fiber test data into engineering constants using ASTM Standard Test Method D3379-75 as a reference. A high temperature furnace was designed and built to perform the single fiber elevated temperature testing up to 1300 C. A computerized single fiber creep apparatus was designed and constructed to perform four fiber creep tests simultaneously at temperatures up to 1300 C. Computer software was written to acquire and reduce all creep data.

Zimmerman, Richard S.↗

DOE OSTI2026

In situ TEM annealing of neutron-irradiated Ti reveals a two-stage mechanism for elevated temperature radiation damage recovery

Understanding how irradiation-induced defects evolve at elevated temperatures is of critical importance to predicting materials' behavior under steady-state and accident scenarios. However, such mechanistic insight into microstructural evolution is limited by the nature of ex situ annealing and subsequent imaging. Here we show direct observation and quantification of defect recovery in neutron-irradiated Ti using in situ transmission electron microscopy (TEM) annealing experiments. In agreement with our prior work, and at temperatures below the irradiation temperature (T irr = 300 °C), dislocation loops are observed to glide. At elevated temperatures (>500 °C), dislocation lines become mobile and promote significant recovery of the microstructure. These mechanisms challenge the established electron irradiation-based model for radiation damage recovery, which originally suggests dissolution of static defect clusters, and demonstrates the importance of in situ characterization in understanding defect evolution in irradiated materials.

Hirst, Charles A. [Univ. of Michigan, Ann Arbor, M↗

DOE OSTI2021

Charge collection in h -BN neutron detectors at elevated temperatures

Many of the neutron detector applications are in the environments with harsh conditions such as high temperatures. We report here the measurements of charge collection parameters of hexagonal boron nitride (h-BN) detectors at elevated temperatures, including the electron mobility-lifetime product (μτ) and surface recombination field (s/μ). It was found that μτ is increased, while s/μ is decreased as temperature increases. The temperature dependence of the surface recombination field (s/μ) revealed that electrons trapped in the surface states tend to thermally activate to the bulk region at higher temperatures with an activation energy of about 0.22 eV, leading to a reduction in the density of the charged surface states at elevated temperatures. Consequently, the charge collection efficiency is enhanced at elevated temperatures due to a reduced surface recombination field and increased electron mobility-lifetime product. The results suggested that h-BN neutron detectors are favorable for high temperature operation.

47 OTHER INSTRUMENTATION↗

NASA NTRS1990

Elevated temperature crack growth in aluminum alloys: Tensile deformation of 2618 and FVS0812 aluminum alloys

Understanding the damage tolerance of aluminum alloys at elevated temperatures is essential for safe applications of advanced materials. The objective of this project is to investigate the time dependent subcritical cracking behavior of powder metallurgy FVS0812 and ingot metallurgy 2618 aluminum alloys at elevated temperatures. The fracture mechanics approach was applied. Sidegrooved compact tension specimens were tested at 175, 250, and 316 C under constant load. Subcritical crack growth occurred in each alloy at applied stress intensity levels (K) of between about 14 and 25 MPa/m, well below K (sub IC). Measured load, crack opening displacement and displacement rate, and crack length and growth rate (da/dt) were analyzed with several continuum fracture parameters including, the C-integral, C (sub t), and K. Elevated temperature growth rate data suggest that K is a controlling parameter during time dependent cracking. For FVS0812, da/dt is highest at 175 C when rates are expressed as a function of K. While crack growth rate is not controlled by C (sub t) at 175 C, da/dt appears to better correlate with C (sub t) at higher temperatures. Creep brittle cracking at intermediate temperatures, and perhaps related to strain aging, is augmented by time dependent transient creep plasticity at higher temperatures. The C (sub t) analysis is, however, complicated by the necessity to measure small differences in the elastic crack growth and creep contributions to the crack opening displacement rate. A microstructural study indicates that 2618 and FVS0812 are likely to be creep brittle materials, consistent with the results obtained from the fracture mechanics study. Time dependent crack growth of 2618 at 175 C is characterized by mixed transgranular and intergranular fracture. Delamination along the ribbon powder particle boundaries occurs in FVS0812 at all temperatures. The fracture mode of FVS0812 changes with temperature. At 175 C, it is characterized as dimpled rupture, and at 316 C as mixed matrix superplastic rupture and matrix-dipersoid debonding.

Leng, Yang↗

NASA NTRS1971

Fatigue of four stainless steels, four titanium alloys, and two aluminum alloys before and after exposure to elevated temperatures for up to three years

Elevated temperature effects on fatigue life of tensile stressed titanium alloys, aluminum alloys, and stainless steels

Illg, W.↗

NASA NTRS1986

Grain boundary oxidation and fatigue crack growth at elevated temperatures

Fatigue crack growth rate at elevated temperatures can be accelerated by grain boundary oxidation. Grain boundary oxidation kinetics and the statistical distribution of grain boundary oxide penetration depth were studied. At a constant delta K-level and at a constant test temperature, fatigue crack growth rate, da/dN, is a function of cyclic frequency, nu. A fatigue crack growth model of intermittent micro-ruptures of grain boundary oxide is constructed. The model is consistent with the experimental observations that, in the low frequency region, da/dN is inversely proportional to nu, and fatigue crack growth is intergranular.

Liu, H. W.↗

NASA NTRS1986

Grain boundary oxidation and fatigue crack growth at elevated temperatures

Liu, H. W.↗

DOE OSTI2026

Experimental and Multiscale Modeling Insights for Radiation-Driven Neptunium Redox Processes at Elevated Temperatures

Studies of the radiation-driven reactions of actinide elements at elevated temperatures are extremely limited, but important given that radiation heating of used nuclear fuel can affect the radiolytically promoted actinide redox processes occurring in hydroprocessing environments. Under these conditions, the high concentration of nitric acid present makes the reaction of actinides, such as neptunium, with nitric acid radiolysis products significant. Therefore, here we present derivation of the rate coefficients for the reaction of pentavalent neptunium with the nitrate radical at elevated temperature, resulting in Eyring and Arrhenius parameters for this important reaction. Here, we also revisit our previously published multiscale model predictions for radiation-induced neptunium redox chemistry and present an iteration which successfully operates over a wider range of nitric acid concentrations, 0.1–6.0 M.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

NASA NTRS2006

Life Limiting Behavior in Interlaminar Shear of Continuous Fiber-Reinforced Ceramic Matrix Composites at Elevated Temperatures

Interlaminar shear strength of four different fiber-reinforced ceramic matrix composites was determined with doublenotch shear test specimens as a function of test rate at elevated temperatures ranging from 1100 to 1316 C in air. Life limiting behavior, represented as interlaminar shear strength degradation with decreasing test rate, was significant for 2-D crossplied SiC/MAS-5 and 2-D plain-woven C/SiC composites, but insignificant for 2-D plain-woven SiC/SiC and 2-D woven Sylramic (Dow Corning, Midland, Michigan) SiC/SiC composites. A phenomenological, power-law delayed failure model was proposed to account for and to quantify the rate dependency of interlaminar shear strength of the composites. Additional stress rupture testing in interlaminar shear was conducted at elevated temperatures to validate the proposed model. The model was in good agreement with SiC/MAS-5 and C/SiC composites, but in poor to reasonable agreement with Sylramic SiC/SiC. Constant shear stress-rate testing was proposed as a possible means of life prediction testing methodology for ceramic matrix composites subjected to interlaminar shear at elevated temperatures when short lifetimes are expected.

Choi, Sung R.↗

DOE OSTI2023

Effects of elevated-temperature deposition on the atomic structure of amorphous Ta 2 O 5 films

Brownian thermal noise as a result of mechanical loss in optical coatings will become the dominant source of noise at the most sensitive frequencies of ground-based gravitational-wave detectors. Experiments found, however, that a candidate material, amorphous Ta 2 O 5 , is unable to form an ultrastable glass and, consequently, to yield a film with significantly reduced mechanical loss through elevated-temperature deposition alone. X-ray scattering PDF measurements are carried out on films deposited and subsequently annealed at various temperatures. Inverse atomic modeling is used to analyze the short and medium range features in the atomic structure of these films. Furthermore, in silico deposition simulations of Ta 2 O 5 are carried out at various substrate temperatures and an atomic level analysis of the growth at high temperatures is presented. It is observed that upon elevated-temperature deposition, short range features remain identical, whereas medium range order increases. After annealing, however, both the short and medium range orders of films deposited at different substrate temperatures are nearly identical. A discussion on the surface diffusion and glass transition temperatures indicates that future pursuits of ultrastable low-mechanical-loss films through elevated temperature deposition should focus on materials with a high surface mobility, and/or lower glass transition temperatures in the range of achievable deposition temperatures.

36 MATERIALS SCIENCE↗

NASA NTRS2005

Promoted Metals Combustion at Ambient and Elevated Temperatures

Promoted combustion testing of materials, Test 17 of NASA STD-6001, has been used to assess metal propensity to burn in oxygen rich environments. An igniter is used at the bottom end of a rod to promote ignition, and if combustion is sustained, the burning progresses from the bottom to the top of the rod. The physical mechanisms are very similar to the upward flammability test, Test 1 of NASA STD-6001. The differences are in the normal environmental range of pressures, oxygen content, and sample geometry. Upward flammability testing of organic materials can exhibit a significant transitional region between no burning to complete quasi-state burning. In this transitional region, the burn process exhibits a probabilistic nature. This transitional region has been identified for metals using the promoted combustion testing method at ambient initial temperatures. The work given here is focused on examining the transitional region and the quasi-steady burning region both at conventional ambient testing conditions and at elevated temperatures. A new heated promoted combustion facility and equipment at Marshall Space Flight Center have just been completed to provide the basic data regarding the metals operating temperature limits in contact with oxygen rich atmospheres at high pressures. Initial data have been obtained for Stainless Steel 304L, Stainless Steel 321, Haynes 214, and Inconel 718 at elevated temperatures in 100-percent oxygen atmospheres. These data along with an extended data set at ambient initial temperature test conditions are examined. The pressure boundaries of acceptable, non-burning usage is found to be lowered at elevated temperature.

Engel, Carl D.↗

NASA NTRS1976

Fatigue crack growth at elevated temperature 316 stainless steel and H-13 steel

Crack growths were measured at elevated temperatures under four types of loading: pp, pc, cp, and cc. In H-13 steel, all these four types of loading gave nearly the same crack growth rates, and the length of hold time had negligible effects. In AISI 316 stainless steel, the hold time effects on crack growth rate were negligible if the loading was tension-tension type; however, these effects were significant in reversed bending load, and the crack growth rates under these four types of loading varied considerably. Both tensile and compressive hold times caused increased crack growth rate, but the compressive hold period was more deleterious than the tensile one. Metallographic examination showed that all the crack paths under different types of loading were largely transgranular for both CTS tension-tension specimens and SEN reversed cantilever bending specimens. In addition, an electric potential technique was used to monitor crack growth at elevated temperature.

Chen, W. C.↗

NASA NTRS1995

A study of elevated temperature testing techniques for the fatigue behavior of PMCS: Application to T650-35/AMB21

An experimental study was conducted to investigate the mechanical behavior of a T650-35/AMB21 eight-harness satin weave polymer composite system. Emphasis was placed on the development and refinement of techniques used in elevated temperature uniaxial PMC testing. Issues such as specimen design, gripping, strain measurement, and temperature control and measurement were addressed. Quasi-static tensile and fatigue properties (R(sub sigma) = 0.1) were examined at room and elevated temperatures. Stiffness degradation and strain accumulation during fatigue cycling were recorded to monitor damage progression and provide insight for future analytical modeling efforts. Accomplishments included an untabbed dog-bone specimen design which consistently failed in the gage section, accurate temperature control and assessment, and continuous in-situ strain measurement capability during fatigue loading at elevated temperatures. Finally, strain accumulation and stiffness degradation during fatigue cycling appeared to be good indicators of damage progression.

Gyekenyesi, Andrew L.↗