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At least 19 records

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

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

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.

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.

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.

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.

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.

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

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.

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.

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.

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.

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

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

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

Weight loss, adherence, friction and wear of polyimide films and polyimide-bonded graphite fluoride films applied to stainless steel disks and to 304 stainless steel thin foils were studied. The films were exposed at temperatures of 315 D, 345 D, 370 D, or 400 C for 100 hours or more and then evaluated at temperatures of 25 D, 315 D, 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 possessed good adherence and gave low friction and wear results. Polyimide-bonded graphite fluoride films appear to be good candidates for solid lubrication applications where long thermal soaks are prevalent.

Fusaro, R. L.

Edge crack growth of thermally aged graphite/polyimide composites

Laminates of Celion 6000/LARC-160 and Celion 6000/PMR-15 graphite/polyimide composite materials were aged in air at temperatures of 202, 232, 260 and 288 C for various times up to 15,000 hours. Three unidirectional specimen types 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, whereas both laminate materials degraded and cracked preferentially at the specimen edge perpendicular to the fibers. Using a dye penetrant, the specimens were X-rayed and the crack depth measured as a function of time and temperature. A time temperature superposition of the crack data was successfully performed using an Arrhenius form for the shift factor. A direct correlation was found for edge crack depth and SBS strength for the LARC-160 laminates but the correlation for PMR-15 laminates was more complex.

Nelson, J. B.