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At least 19 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Key Degradation Products in Nitroplasticizer Thermal Aging

Upon thermal aging, nitroplasticizer (NP) can thermally degrade and release numerous degradation products depending on aging conditions. In this report, we summarize our recent findings, a library of key degradation products in the NP thermal aging is provided. The library contains 25 identified species with their corresponding MS/MS spectrum and intensity profiles, which are derived from our 44-month thermal aging experiment of NP conducted in air, nitrogen, and water at room temperature (RT), 38, 45, 55, and 64°C. To provide a comprehensive yet simplified overview of NP degradation, we summarized the proposed mechanisms of HONO elimination and decomposition, acid generation, PBNA nitrosation and nitration, acid-catalyzed hydrolyses of NP and polynitrated PBNAs, as well as the formation of NP degradants. As the last part of a series of publications and reports on the investigation of NP degradation mechanisms, this work further unfolds complex chemistry that occurs in the entire aging process of NP.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Probing the fatigue enhancement in a thermally aged cast duplex stainless steel by in situ neutron diffraction

After long-term thermal aging at 400 °C for 3000 h and 10,000 h, a cast duplex stainless steel exhibits promoted fatigue performance, including enhanced three-stage cyclic hardening and prolonged fatigue life. Utilizing in situ neutron diffraction, the phase-specific stresses are resolved, and their evolutions over entire fatigue cycling reveal the underlying mechanisms of the fatigue enhancement. It is found that the ferrite phase bears a much higher stress than the austenite matrix under both as-received and aged conditions. The enhanced cyclic hardening in Stage I is attributed to the strengthening of both phases due to thermal aging, while the enhancement in Stage III results from the martensitic transformation induced strengthening. The fatigue life is prolonged thanks to the cyclic hardening and the delay of martensitic transformation in the austenite phase after thermal aging.

Yu, Dunji↗
DOE OSTI2025

Long-term thermal aging behavior and strength reduction in a laser powder bed fusion 316H stainless steel

The long-term thermal stability of structural alloys is essential for ensuring the safe and reliable operation of nuclear reactors and other power plants. While extensive research has explored the effects of thermal aging on conventional stainless steels, the behavior of additively manufactured (AM) alloys remains less understood. This study examines the thermal aging response of laser powder bed fusion (LPBF) 316H stainless steel (SS) at temperatures ranging from 550 °C to 750 °C over durations of up to 10,000 h (approximately 1.14 years). Advanced characterization techniques, including electron microscopy and synchrotron X-ray diffraction, were used to investigate dislocation recovery and phase evolution. Based on these findings, a time-temperature-precipitation (TTP) diagram was developed for LPBF 316H SS, revealing a 10- to100-fold acceleration in precipitation kinetics compared to wrought 316H SS. A physics-informed model was calibrated using the short-term experimental data, enabling predictions of average precipitate sizes, volume fractions of M 23 C 6 and Laves phases, and changes in molybdenum solute concentration for aging up to 1 × 10⁶ h (114 years). These microstructural insights were further utilized to estimate yield strength and extrapolate strength reduction factors over the extended aging period. Despite the accelerated aging kinetics, LPBF 316H SS demonstrated superior yield strength retention compared to its wrought counterpart. In conclusion, this study establishes a framework for evaluating long-term performance using short-term experimental data and supports the accelerated qualification of AM materials for high-temperature structural applications.

Laser powder bed fusion↗
NASA NTRS1987

Effect of long-term thermal aging on coated Celion/LARC-160 composites

Coated and uncoated unidirectional laminates of Celion (Trademark)/LARC-160 graphite/polyimide were thermally aged in air at temperatures of 204, 260, and 316 C for various times up to 15,000 hours. Selected panels were coated with a high temperature coating resin (polyphenyl quinoxaline--PPQ): 1) edges only; 2) top and bottom only; 3)completely; or 4) not at all. Periodically during aging, panels were removed from the ovens, weighed, and short beam shear (SBS) specimens cut from selected locations in the panels. The protective coating did not influence the retention of SBS strength during thermal aging but did not lessen the amount of weight-loss incurred. The integrity of the PPQ coating was completely destroyed during aging at 316 C.

Nelson, James B.↗
DOE OSTI2024

Thermal aging effects on crosslinked polyethylene cable insulation with decabromodiphenyl ether flame retardant alternative

Decabromodiphenyl ether (decaBDE) has been extensively used as a flame retardant in several applications, including nuclear electrical cable insulation. However, decaBDE has been identified as a persistent, bioaccumulative and toxic (PBT) substance, leading to regulatory scrutiny. The Environmental Protection Agency (EPA) published a regulation on January 6, 2021, aimed at phasing out the manufacturing, processing, and distribution of decaBDE. This rule set a compliance deadline of March 8, 2021, for the manufacture and processing of decaBDE, and an extended deadline of January 6, 2023, for specific applications including wire and cable insulation in nuclear power generation facilities. In response to such regulations, RSCC, a major supplier of safety-related electrical cables and associated products to the U.S. nuclear industry updated the formula of their crosslinked polyethylene (XLPE) insulation to replace the historically used decaBDE flame retardant with an acceptable alternative. This change from the previous decaBDE-containing XLPE prompted interest in comparative performance of the two material formulations, especially with respect to characteristics relevant to safety-related function such as thermal and radiation resistance. RSCC graciously provided samples of wire insulated with the decaBDE-containing XLPE formulation and corresponding wire insulated with XLPE of the new formulation, containing a decaBDE alternative. In this work we compare characteristics of the two formulations and a previously produced commercial version of the RSCC decaBDE-containing XLPE insulation subjected to thermal aging at 150 °C and 165 °C. The comparison was focused on mechanical durability, thermal stability in the oxidative environment, and chemical structures. Briefly, • Tensile elongation at break (EAB) results showed loss of mechanical elasticity with longer aging time, as expected. Aging time dependence of EAB did not differ between the decaBDE-containing and decaBDE-alternative samples. • Subtle differences between the two materials can be detected from Fourier-transform infrared spectroscopy (FTIR) absorbance spectra in the range below 1700 cm -1 , are assumed to be related to decomposition of flame retardant additives during thermal aging. • The oxidation induction time (OIT) data seemed to show that the unaged decaBDE-containing XLPE material is more thermally stable than the unaged decaBDE-alternative material, but the discrepancy in OIT decreased with aging time and the OIT values of the two materials became similar starting with the 4 th day of aging at 165 °C. This thermal aging investigation confirmed that the mechanical durability, a key property monitored for cable qualification, was not significantly affected by the modification of the formulation with a decaBDE alternative flame-retardant system in the investigated thermal aging conditions. Further studies on the same sets of materials exposed to thermal and gamma radiation aging would further inform comparison of the materials safety-related function.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Effect of Thermal Aging on Microstructure and Stress Corrosion Cracking Behavior of an Alloy 152 1st Layer Butter Weldment

Nickel-based Alloy 690 and the associated weld Alloys 52 and 152 are typically used for nozzle penetrations in replacement heads for pressurized water reactor (PWR) vessels, because of their excellent overall resistance to general corrosion and environmental degradation, primarily stress corrosion cracking (SCC). However, many of the existing PWRs are expected to operate for 40- 80 years. Likewise, water-cooled small modular reactors (SMRs) will use Ni-Cr alloys and are expected to receive initial operating licenses for 60 years. Hence, the thermal stability of Ni-Cr alloys is critical for the long-term performance of both existing and advanced nuclear power plants, and possibly spent fuel storage containers. The objective of this research is to understand the microstructural changes occurring in high-Cr, Ni-based Alloy 152 weldments during long time exposure to the reactor operating temperatures, and the effect of these changes on the service performance. One area of particular concern is the potential for long range ordering (LRO), i.e. formation of the intermetallic Ni2Cr phase under prolonged exposure to reactor temperatures and/or irradiation, which can increase strength, decrease ductility, and cause dimensional changes or lead to in-service embrittlement of components made with these alloys. Hence, this research focused on the microstructural evolution and the SCC response of Alloy 152 under accelerated thermal aging. The materials studied involved three heats of Alloy 152 used to produce a dissimilar metal weld (DMW) joining an Alloy 690 plate to an Alloy 533 low alloy steel (LAS) plate, thermally aged at three different temperatures (370°C, 400°C and 450°C) for different durations up to 75,000h (equivalent to 60 years of reactor service). The microstructural characterization by means of synchrotron X-ray conducted in small, 0.2 mm - step line scans in the high-deformation regions of the weld root – covering areas spanning from the weld heat affected zone (HAZ) in Alloy 690 to the weld and weld butter on LAS - did not show evidence of LRO in any of the three Alloy 152 heats aged at 370°C and 450°C to an equivalent of 60 years of service. However, the first weld butter layer has high levels of deformation and is highly susceptible to SCC even in its non-aged condition. Nanohardness testing confirmed the extreme hardening with aging (ΔHV ≅ 100) at two locations within this weldment. In absence of LRO, hardening is suspected to be due to thermally-induced Cr carbide precipitation and coarsening. Testing in a primary water environment of the 1st layer of Alloy 152 weld butter aged at 370°C to a 60-year service equivalent revealed a fatigue and corrosion fatigue crack growth responses similar to those measured on the un-aged alloys. Similarly, the SCC CGR response of the aged weld butter does not appear to show a deterioration in performance, however, the difficult-to-test weldment geometry may affect the test results.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗
NASA NTRS1982

Effects of 50,000 hours of thermal aging on graphite/epoxy and graphite/polyimide composites

Thermal effects on tensile strengths of advanced composite systems have been determined for exposure times of 100 to 50,000 hours (5.7 years). Exposures were conducted at both ambient and reduced pressures at two temperatures for each composite. At the completion of the various aging periods, specimens were removed from the specially constructed aging furnaces, visually examined, and tensile tested at elevated temperature. After tensile testing, many of the thermal aging specimens were examined using a scanning electron microscope. Results of these studies are presented, and the changes in properties and the degradation mechanisms during high-temperature aging are discussed and illustrated using metallographic techniques.

Kerr, J. R.↗
DOE OSTI2024

Latent Pitfalls in Microstructure-Based Modeling for Thermally Aged 9Cr-1Mo-V Steel (Grade 91)

A case study was conducted on a mechanistic model development that predicted tensile strength deterioration with thermal aging of 9Cr-1Mo-V steel in supporting the 60-year design life expected for advanced nuclear reactors. For property prediction beyond practical testing times, mechanistic modeling is highly desired, as it taps into the physics of structure–property relationships and therefore can generate reliable results for extrapolation. Meanwhile, as mechanistic models are often complicated, reflecting the intricacy of microstructure and strengthening mechanisms, pitfalls that are difficult to detect often exist. Here, this paper discusses latent pitfalls that are common in mechanistic modeling or specific in this 9Cr-1Mo-V case development through using the American Society of Mechanical Engineers verification and validation in computational solid mechanics (ASME V&V 10) standard for evaluating credibility of modeling in materials engineering. Suggestions are also made for enhancing reliability of microstructure-based modeling.

36 MATERIALS SCIENCE↗
NASA NTRS1979

Effect of thermal aging on the tribological properties of polyimide films and polyimide-bonded graphite fluoride films

The effect of thermal aging on the weight loss, adherence, friction and wear of polyimide films and polyimide-bonded graphite fluoride films applied to 440C-HT stainless steel disks and to 304 stainless steel thin foils was studied. The films were exposed at temperatures of 315, 345, 370 or 400 C for 100 hours or more and then evaluated at temperatures of 25, 315 or 345 C in atmospheres of dry or moist air. Polyimide films were found to be brittle after thermal exposure; but polyimide-bonded graphite fluoride films possessed good adherence and gave low friction and wear results. Thus, polyimide-bonded graphite fluoride films appear to be good candidates for solid lubrication applications where long thermal soaks are prevalent.

Fusaro, R. L.↗
NASA NTRS1985

Effects of real-time thermal aging on graphite/polyimide composites

As part of a program to evaluate high-temperature advanced composites for use on supersonic cruise transport aircraft, two graphite/polyimide composites have been aged at elevated temperatures for times up to 5.7 years. Work on the first, HT-S/710 graphite/polyimide, was started in 1974. Evaluation of the second polyimide, Celion 6000/LARC-160, began in 1980. Baseline properties are presented, including unnotched and notched tensile data as a function of temperature, compression, flexure, shear, and constant-amplitude fatigue data at R = 0.1 and R = -1. Tensile specimens were aged in ovens where pressure and aging temperatures were controlled for various times up to and including 50,000 hours. Changes in tensile strength were determined and plotted as a function of aging time. The HT-S/710 composite aged at 450 F and 550 F if compared to the Celion 6000/LARC-160 composite aged at 350 F and 450 F. After tensile testing, many of the thermal aging specimens were examined using a scanning electron microscope. Results of these studies are presented, and changes in properties and degradation mechanisms during high-temperature aging are discussed and illustrated using metallographic techniques.

Haskins, J. F.↗
NASA NTRS1982

Surface characterization and failure analysis of thermally aged, polyimide bonded titanium

This study of high temperature stable adhesive systems using 6Al-4V titanium adherends found that certain adhesive/adherends exhibit a change from cohesive to adhesive failure mode during long term 450 F thermal aging. Lap-shear specimens which exhibited adhesive failures were subjected to failure analysis using scanning transmission electron microscopy (STEM) and surface analysis techniques. Data is presented which supports the conclusion of interfacial failures for these samples.

Peters, P. D.↗
DOE OSTI2025

Microstructure and Mechanical Properties of Scaled Thermally Aged LPBF 316H SS Builds

As part of the US Department of Energy’s Advanced Materials and Manufacturing Technologies program’s mission to accelerate qualification of advanced manufacturing pathways for nuclear applications, laser powder bed fusion (LPBF) 316H stainless steel (SS) has been selected as a model system to develop a rapid code case framework. This effort directly addresses the grand challenges of (1) expanding the limited portfolio of materials currently codified for elevated-temperature nuclear structural service under Section III, Division 5 of the American Society of Mechanical Engineers’ Boiler and Pressure Vessel Code; and (2) significantly reducing qualification timelines that traditionally exceed a decade. The strategic importance of LPBF 316H lies in its immediate industrial relevance, existing data foundation from wrought 316H, and alignment with ongoing code case development for LPBF 316L. Prior work revealed accelerated precipitation of deleterious secondary phases and reduced creep ductility in as-printed LPBF 316H. Building on that prior research, FY 2025 activities focused on establishing an understanding of the key failure mechanisms of crept 316H specimens to aid in code case development and on evaluating stress relief (SR) parameters on the high-temperature performance and thermal aging induced degradation of tensile and fracture behavior in LPBF 316H.

36 MATERIALS SCIENCE↗
NASA NTRS2001

Damage Assessment of Creep Tested and Thermally Aged Udimet 520 Using Acousto-Ultrasonics

Due to elevated temperatures and excessive stresses, turbine components may experience creep behavior. As a result, it is desirable to monitor and assess the current condition of such components. This study employed the Acousto-Ultrasonics (AU) method in an effort to monitor the state of the material at various percentages of used up creep life in the nickel base alloy, Udimet 520. A stepped specimen (i.e., varying cross sectional area) was employed which allowed for a postmortem nondestructive evaluation (NDE) analysis of the various levels of used up life. The overall objectives here were two fold: First, a user friendly, graphical interface AU system was developed, and second the new AU system was applied as an NDE tool to assess distributed damage resulting from creep. The experimental results demonstrated that the AU method shows promise as an NDE tool capable of detecting material changes as a function of used up creep life. Furthermore, the changes in the AU parameters were mainly attributed to the case of combined load and elevated temperature (i.e., creep) and not simply because of a timed exposure at elevated temperature (i.e., heat treatment or thermal aging).

Gyekenyesi, Andrew L.↗
NASA NTRS1985

Long-term thermal aging of Celion/V378A composite materials

Celion 6000/V378A graphite/bismaleimide composite materials were aged in air at temperatures of 177, 204, 232 and 260 deg C for various times up to 15,000 hours. Three unidirectional specimen types were aged: short beam shear (SBS), flexure, and 153 mm square panels. Aged specimens of V378A laminates exhibited excellent thermal stability. Extensive cracking was observed during aging on the 0 deg edges of the unidirectional laminates. These cracks penetrated as deep as 12 mm from the edge. The cracking appeared to have little or no effect on the observed properties of the laminates. The study indicates that the useful life of unrestrained unidirectional graphite/V378A laminates is 10,000 hours or greater at 177 C to 232 C and 2,000 to 2,000 hour at 260 C.

Nelson, J. B.↗
NASA NTRS1980

Comparison of the weight loss and adherence of nine different polyimide films thermally aged at 315 C and 350 C in air

Thermal exposure experiments at 315 and 350 C were performed in air on nine different types of polyimides applied to thin 304 stainless steel foils. The tests were conducted to determine which polyimide was the most thermally stable and adherent when subjected to long exposure times at elevated temperatures. One polyimide designated PIC-7 was found to be more thermally stable than the others; however, it did not possess the adherent properties of PIC-2 and PIC-5. It was concluded that as far as thermal stability and adherence are concerned, five of the polyimides are more suitable for high temperature applications than the other four.

Fusaro, R. L.↗
NASA NTRS1983

Thermal aging of graphite/polyimide composites

Celion 6000/PMR-15, Celion 6000/LARC-160, and Celion 6000/RK-99 graphite/polyimides were aged in circulating air ovens at temperatures of 202, 232, 260, and 288 C for various times, up to 15,000 h. Three unidirectional specimens were studied: short-beam-shear (SBS), flexure, and 153-mm square panels. The interior region of the square panels exhibited little or no property degradation. Based on the individually aged SBS specimen results, the relative thermal-oxidative stability from highest to lowest is as follows: PMR-15, LARC-160, RK-99, Celion 6000/PMR-15 and Celion 6000/LARC-160 laminates retained at least 80 percent of their initial flexural strengths for the duration of aging at each temperature. Celion 6000/RK-99 laminates exhibited a 20 to 50 percent loss of flexural strength at all aging temperatures. All three graphite/polyimide laminate materials degraded preferentially at the specimen edge perpendicular to the fibers.

Nelson, J. B.↗
DOE OSTI2025

Microstructure & Mechanical Properties of Scaled Thermally Aged LPBF 316H SS Builds

As part of the US Department of Energy’s Advanced Materials and Manufacturing Technologies program’s mission to accelerate qualification of advanced manufacturing pathways for nuclear applications, laser powder bed fusion (LPBF) 316H stainless steel (SS) has been selected as a model system to develop a rapid code case framework. This effort directly addresses the grand challenges of (1)expanding the limited portfolio of materials currently codified for elevated-temperature nuclear structural service under Section III, Division 5of the American Society of Mechanical Engineers’ Boiler and Pressure Vessel Code; and (2) significantly reducing qualification timelines that traditionally exceed a decade. The strategic importance of LPBF 316H lies in its immediate industrial relevance, existing data foundation from wrought 316H, and alignment with ongoing code case development for LPBF 316L.Prior work revealed accelerated precipitation of deleterious secondary phases and reduced creep ductility in as-printed LPBF 316H. Building on that prior research, FY2025activities focused on establishing an understanding of the key failure mechanisms of crept 316H specimens to aid in code case development and on evaluating stress relief (SR) parameters on the high-temperature performance and thermal aging-induced degradation of tensile and fracture behavior in LPBF316H.

36 MATERIALS SCIENCE↗
DOE OSTI2025

The Effect of Thermal Aging on the Performance of High-Cr Ni-based Alloys in Primary Water Environment

Nickel-based Alloy 690, and the associated weld Alloys 52 and 152, are used for nozzle penetrations in replacement heads for pressurized water reactor (PWR) vessels. They are chosen for their excellent overall resistance to general corrosion and environmental degradation, primarily stress corrosion cracking (SCC). However, many of the existing PWRs are expected to operate beyond their first or second license renewal (e.g., 40 to 60 years or beyond 60 years). Hence, the thermal stability of Ni-Cr alloys is a potential concern for the long-term performance of both existing and advanced nuclear power plants. Moreover, Ni-Cr alloys are being considered for high-level radioactive waste disposal containers that will be required to contain the waste for at least 10,000 years.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗