A thorough understanding of interactions between graphite and fluoride fuel salts is crucial, as graphite is a promising candidate for the moderator of molten salt reactors. This study investigates the infiltration of fluoride fuel salts into graphite and the fluorination of graphite by these salts under various pressures and temperatures. A high-pressure salt infiltration test apparatus was developed to examine the infiltration of NaF-KF-UF 4 and NaF-BeF 2 -UF 4 -ZrF 4 fuel salts into two types of graphite at high temperatures. For tests using NaF-BeF 2 -UF 4 -ZrF 4 , two different temperatures were selected to assess the impact of temperature on threshold pressure. The study observed salt infiltration into graphite at pressures exceeding its threshold pressure, and the threshold pressure for infiltration was lower at the higher temperature. In addition, the formation of carbon fluorides on the surface of post-test graphite specimens was identified.

The United States Department of Energy Office of Fossil Energy and the Ohio Coal Development Office (OCDO) have led a U.S. consortium tasked with development of the materials technology necessary to build an advanced-ultra-Supercritical (A-USC) steam boiler and turbine with steam temperatures up to 760°C (1400°F). Part of this effort has focused on the need for higher temperature capable materials for steam turbine components, specifically cast nickel-base superalloys such as Haynes 282 alloy. As the size of the needed components is much larger than is capable of being produced by vacuum casting methods typically used for these alloys, an alternative casting process has been developed to produce the required component sizes in Haynes 282 alloy. The development effort has progressed from production of sub-scale sand castings to full size sand and centrifugal castings. The aim of this work was to characterize the microstructure and properties of a nickel alloy 282 casting with section size and casting weights consistent with a full sized component. A 2720 kg (6000 lbs.) nickel alloy 282 sand casting was produced and heat treated at MetalTek International. The casting was a half valve body configuration with a gating system simulated and optimized to be consistent with a full sized part. Following casting, heat treatment and NDE inspections, the half valve body was sectioned and tested. Tensile and high temperature creep was performed on material from different casting section thicknesses. Further analysis of the microstructure was carried out using light microscopy (LM), scanning electron microscopy (SEM), and X-ray spectroscopy (EDS). The paper also presents the mechanical properties obtained from the various sections of the large casting.

The pursuit of reduced emissions and increased efficiency in ultra-critical steam plants has led to the investigation of systems operating at temperatures up to 720°C and pressures up to 300 bars, necessitating the use of nickel-based alloys. This study focuses on control valves manufactured from Alloy 617, designed for steam temperatures of 725°C, examining specific challenges in their design and manufacture, including machining and welding processes. Initial operational experiences with the valve at 725°C are presented, along with ongoing tribological investigations of nickel-based alloys at 725°C, as standard material pairings with optimized wear behavior are unsuitable at such elevated temperatures. These investigations aim to develop material pairings that can maintain good wear behavior under these extreme conditions.

As conventional coal-fired power plants seek to reduce greenhouse gas emissions by increasing efficiency, the temperature limitations of traditional ferritic/martensitic steels used in high-temperature components present a significant challenge. With Advanced Ultra Supercritical (A-USC) power plants proposing steam temperatures of 760°C, attention has turned to nickel-based superalloys as potential replacements, since ferritic/martensitic steels cannot withstand such extreme conditions. However, the current absence of cast nickel-based superalloys combining high strength, creep-resistance, and weldability has led to the development of cast analogs of wrought nickel-based superalloys, including H263, H282, and N105. This paper examines the alloy design criteria, processing experiences, as-processed and heat-treated microstructures, and selected mechanical properties of these materials while also discussing their potential for full-scale development.

The cast microstructure of 1st generation MoSiBTiC alloy composed of Mo solid solution (Mo ss ), Mo 5 SiB 2 , TiC phases largely affects tensile-creep behavior in the ultrahigh temperature region. Mo 5 SiB 2 phase crystallized during solidification is plate-like with a size of several tens of microns. The plate surface is parallel to the (001) basal plane, and the <100] directions preferentially grow along the cooling direction, and thereby Mo 5 SiB 2 has a strong texture while Moss and TiC show randomly-oriented distribution in a cast ingot. During creep, Mo 5 SiB 2 plates are largely rotated and Moss works as sticky ligament in the small-plate-reinforced metal-matrix composites. This may be the reason why the MoSiBTiC alloy exhibits large creep elongation and excellent creep resistance. In other words, the evolution of microstructures infers that the consummation of Mo 5 SiB 2 plate rotation may lead to the initiation of creep rapture process. Therefore, the unique microstructure formed during solidification provides the feature of good mechanical properties for the 1st generation MoSiBTiC alloy.

A 9% Cr steel containing cobalt and boron, X13CrMoCoVNbNB9-2-1, has been manufactured by electroslag remelting (ESR) to evaluate its performance and to compare its creep strength and microstructure to a forging made from electroslag hot-topping ingot. The evaluation results confirm that it is possible to produce rotor forgings with homogeneous composition and good properties by the ESR process. The results of creep rupture tests up to 5000 h indicate that the creep strength of the forging made from ESR ingot is similar to that of the forging produced by the electroslag hot-topping process. Martensitic lath microstructures with high density dislocations and the precipitations of M 23 C 6 , VX, NbX and M2X are observed after the quality heat treatments at the center portion of both forgings. There is no large difference in the martensitic lath widths, distributions, and sizes of those particles between both trial forgings.

Oxyfuel combustion efforts to burn fossil fuels with oxygen, for easier post-combustion CO 2 capture, include schemes to use flue gas to drive turbines for power generation. The environment examined here is 10% CO 2 and 0.2% O 2 , with the balance being steam, with temperatures ranging from 630 to 821 °C. The relatively high C and O 2 activities of this environment, as compared to pure steam, may lead to changes in oxidation behavior and mechanical properties. Oxidation coupons of Ni- and Co-base superalloys, in both bare metal and TBC coated conditions, were exposed to this environment for up to 1000 hours. The results of these exposures, in terms of mass gain and scale morphology, are presented.

This study demonstrates the Electro-Thermal Mechanical Testing (ETMT) system's capability to analyze the thermo-mechanical behavior of Inconel 718 (IN718) at a heating rate of 5 °C/s, achieving temperatures up to 950 °C. The temperature profile peaks at the sample's center and is approximately 25 °C at the extremes. Upon reaching 950 °C, the sample was aged for 30 hours before being rapidly quenched. This process froze the microstructure, preserving the phase transformations that occurred at various temperatures across the temperature parabolic gradient, which resulted in a complex gradient microstructure, providing a comprehensive map of phase transformations in IN718. The integration of thermal measurement, COMSOL modeling, scanning electron microscopy enabled a thorough characterization of the microstructural evolution in IN718, linking observed phases to the specific temperatures which provided a rapid screening of the effect of using different heating treatment routes.

A creep resistant martensitic steel, CPJ7, was developed with an operating temperature approaching 650°C. The design originated from computational modeling for phase stability and precipitate strengthening using fifteen constituent elements. Approximately twenty heats of CPJ7, each weighing ~7 kg, were vacuum induction melted. A computationally optimized heat treatment schedule was developed to homogenize the ingots prior to hot forging and rolling. Overall, wrought and cast versions of CPJ7 present superior creep properties when compared to wrought and cast versions of COST alloys for turbines and wrought and cast versions of P91/92 for boiler applications. For instance, the Larson Miller Parameter curve for CPJ7 at 650°C almost coincides with that of COST E at 620°C. The prolonged creep life was attributed to slowing down the process of the destabilization of the MX and M 23 C 6 precipitates at 650°C. The cast version of CPJ7 also revealed superior mechanical performance, well above commercially available cast 9% Cr martensitic steel or derivatives. The casting process employed slow cooling to simulate the conditions of a thick wall full-size steam turbine casing but utilized a separate homogenization step prior to final normalization and tempering. To advance the development of CPJ7 for commercial applications, a process was used to scale up the production of the alloy using vacuum induction melting (VIM) and electroslag remelting (ESR), and underlined the importance of melt processing control of minor and trace elements in these advanced alloys.

The time-dependent behavior of 9Cr creep strength enhanced ferritic (CSEF) steels has long fixated on the creep life recorded in uniaxial constant load creep tests. This focus is a consequence of the need to develop stress allowable values for use in the design by formulae approach of rules for new construction. The use of these simple rules is justified in part by the assumption that the alloys used will invariably demonstrate high creep ductility. There appears to be little awareness regarding the implication(s) that creep ductility has on structural performance when mechanical or metallurgical notches (e.g., welds) are present in the component design or fabricated component. This reduced awareness regarding the role of ductility is largely because low alloy CrMo steels used for very many years typically were creep ductile. This paper focuses on the structural response from selected tests that have been commissioned or executed by EPRI over the last decade. The results of these tests demonstrate unambiguously the importance that creep ductility has on long-term, time-dependent behavior. This is the second part of a two-part paper; Part I reviewed the selected tests and discussed them from a mechanical perspective. The association of performance with specific microstructural features is briefly reviewed in this paper and the remaining gaps are highlighted for consideration among the international community.

A new ferritic steel branded as Thor 115 has been developed to enhance high-temperature resistance. The steel design combines an improved oxidation resistance with long-term microstructural stability. The new alloy was extensively tested to assess the high-temperature time- dependent mechanical behavior (creep). The main strengthening mechanism is precipitation hardening by finely dispersed carbide (M 23 C 6 ) and nitride phases (MX). Information on the evolution of secondary phases and time-temperature-precipitation behavior of the alloy, essential to ensure long-term stability, was obtained by scanning transmission electron microscopy with energy dispersive spectroscopy, and by X-ray powder diffraction on specimens aged up to 50,000 hours. The material behavior was also tested in service conditions, to validate the laboratory results: Thor 115 tubing was installed in a HRSG power plant, directly exposed to turbine flue gasses. Tubing samples were progressively extracted, analyzed and compared with laboratory specimens in similar condition. This research shows the performance of Thor 115 regarding steam oxidation and microstructure evolution up to 25,000 exposure hours in the field. So far, no oxide microstructure difference is found between the laboratory and on field tubing: in both cases, the oxide structure is magnetite/hematite and Cr-spinel layers and the oxide thickness values lay within the same scatter band. The evolution of precipitates in the new alloy confirms the retention of the strengthening by secondary phases, even after long-term exposure at high temperature. The deleterious conversion of nitrides into Z phase is shown to be in line with, or even slower than that of the comparable ASME grade 91 steel.

Steam-side oxidation and the resultant exfoliation of iron-based scales cause unplanned shutdowns at coal-fired power generation plants. Exfoliate removal is currently limited to frequent unit cycling to minimize the volume of exfoliated scale, upgrading a plant with a “blow down” system, or installing a higher alloy. This paper discusses the rate of steam-side oxidation on Type 304H stainless steel (304H) tube after shot peening the internal surface with commercially available techniques. Shot peening the ID of Type 304H austenitic stainless steel superheater tubes has been shown to improve the overall oxidation resistance in steam. Decreasing the oxidation rate directly impacts the volume of exfoliated scale. The adherent spinel scales are thinner and more robust than non-shot peened tubes of the same alloy. Most of the improved oxidation resistance can be attributed to the presence of a spinel oxide layer combined with a continuous chromia layer formed near the steam-touched surfaces. The presence of a continuous chromia layer vastly reduces the outward diffusion of iron and minimizes the formation of iron-based scales that exfoliate. This work showed that a uniform cold-worker layer along the tube ID has a profound effect on oxidation resistance. Incomplete coverage allows oxidation to proceed in the non-hardened regions at a rate comparable to the oxidation rate on unpeened Type 304H.

Grade 91 creep strength-enhanced ferritic steel is a critical material in power generation, widely used for high-temperature, high-pressure tubing and piping applications. Its superior elevated-temperature strength derives from a distinctive microstructure of tempered martensite with uniformly dispersed secondary phases (carbides and carbo-nitrides). This microstructure, crucial for reliable service performance, is achieved through precise control of the manufacturing process, including steelmaking, hot forming, and final heat treatment. This investigation builds upon earlier research into the relationship between manufacturing parameters and short-term creep-rupture properties in T91 tubes, and a recent update that included test results exceeding 30,000 hours. This study presents a comprehensive metallurgical analysis of ruptured test specimens. The investigation focuses on correlating manufacturing parameters with not only creep strength but also material ductility and microstructural evolution during long-term exposure, providing valuable insights into the material’s behavior under extended service conditions.

Modified 9Cr-1Mo alloy steel has been developed over the last few decades and has since gained wide acceptance in the boiler industry for the production of a variety of pressure-critical components, including tubing, piping and headers. The properties of creep-strength enhanced ferritic steels such as grade 91 are critically dependent on manufacturing parameters such as steelmaking, hot deformation, heat treatment and welding. Since the applications for which this material is used impose strict requirements in terms of resistance, corrosion, and creep behavior, poor process control can severely compromise the service behavior. This work discusses the impact of total deformation during the rolling process, and heat treatment parameters on time-independent and time-dependent properties for grade 91. For this study, two heats with similar chemical composition were produced with different reduction ratios: to which, several normalizing and tempering combinations were applied. For each combination, the microstructure was characterized, including evaluation of segregation by metallographic examination, and analysis of secondary phase precipitates by means of X-ray powder diffraction. Mechanical testing and creep testing were performed. A comparison of results is presented, and recommendations on the optimal process parameters are provided to ensure reliable performance of grade 91 material.

Increasing the temperature capabilities of ferritic/martensitic 9-12% Cr steels can help in increasing the operating temperature of land-based turbines and minimize the use of expensive high-temperature alloys in the hot section. A creep resistant martensitic steel, JMP, was developed with the potential to operate at or above 650°C. The design of the alloys originated from computational modeling for phase stability and precipitate strengthening using fifteen constituent elements. Cobalt was used for increased solid solution strengthening, Si for oxidation resistance and different W and Mo concentrations for matrix strength and stability. The JMP steels showed increases in creep life compared to MARBN/SAVE12AD at 650°C for testing at various stresses between 138 MPa and 207 MPa. On a Larson-Miller plot, the performance of the JMP steels surpasses that of state-of-the-art MARBN steel. Approximately 21 years of cumulative creep data are reported for the JMP steels which encompasses various compositions. The relationships between composition-microstructure-creep properties are discussed including characterization of microstructures after >20,000 hours in creep.

Advanced UltraSupercritical (A-USC) Steam fossil power plants will operate at steam temperatures up to 760°C, which will require the use of Ni-based superalloys for steam boiler/superheater and turbine systems. In 2008, the Oak Ridge National Laboratory (ORNL) and the National Engineering Technology Laboratory/Albany (NETL/Albany) collaborated to make and test castings of Ni-based superalloys, which were previously only commercially available in wrought form. These cast Ni-based based alloys are envisioned for the steam turbine casing, but they may also be applicable to other large components that connect the steam supply to the steam turbine. ORNL and NETL/Albany have produced small vacuum castings of HR 282, Nimonic 105, Inconel 740, and alloy 263, which are precipitation-hardened Ni-based superalloys, as well as solid-solution superalloys such as alloys 625, 617 and 230. The initial alloy screening included tensile and creep-testing at 800°C to determine which alloys are best suited for the steam turbine casing application at 760°C. HR 282 has the best combination of high-temperature strength and ductility, making it a good candidate for the cast-casing application. Cast and wrought versions of HR 282 have similar creep-rupture strength, based on the limited data available to-date. Detailed comparisons to the other alloys and microstructures are included in this paper.

Simple and effective material examination methods are desired for the diffusion bonding process, so that bonding produced components, such as compact heat exchangers, can be used in nuclear applications. Optical microscopy of diffusion bond process samples is a quick way to examine diffusion bond-line microstructure and to evaluate material quality. The stacked nature of a diffusion bonded-block results in distinct regions of grain growth both at and away from the bond interface. Strong diffusion bond materials exhibit grain growth across the original bond interface plane, weak materials have little-to-no growth across. A series of 316H diffusion bonded specimens of differing quality and strength were examined using optical microscopy. The microstructure both at and away from the bond interface was examined over 15mm long sections of the bond-line. A metric for evaluating bond growth is proposed. This is defined as the Bond Line Growth Threshold (BLGT) and is evaluated as the percentage of the bond line with grains meeting the threshold. Here a fraction of the diffusion bond is considered bonded when its grains exceed a threshold of growth past the bond interface. The BLGT is determined through automated image processing methods.

This study explores the expanded applications of Alloy J513, a high-performance material traditionally used in cast engine valvetrain components, for powder metallurgy and surface cladding applications. While already recognized for its superior heat and wear resistance at a lower cost compared to cobalt-based hardfacing materials, J513 demonstrates additional advantages in powder metallurgy applications due to its ability to achieve desired powder characteristics through atomization without requiring post-atomization annealing. Through experimental investigation based on fundamental metallurgical principles and cladding engineering processes, the presented research demonstrates J513’s exceptional weldability and favorable weldment structure compared to conventional cobalt-based alloys. The study establishes crucial relationships between weldment behavior and unit energy input, providing valuable insights for advanced cladding techniques while highlighting J513’s potential as a sustainable alternative to traditional nickel- and cobalt-based alloys in various manufacturing processes, including surface overlay and additive manufacturing.

A new alloy design concept for creep- and corrosion-resistant, fully ferritic alloys was proposed for high-temperature structural applications in current/future fossil-fired power plants. The alloys, based on the Fe-30Cr-3Al (in weight percent) system with minor alloying additions of Nb, W, Si, Zr and/or Y, were designed for corrosion resistance though high Cr content, steam oxidation resistance through alumina-scale formation, and high-temperature creep performance through fine particle dispersion of Fe 2 (Nb,W)-type Laves phase in the BCC-Fe matrix. Theses alloys are targeted for use in harsh environments such as combustion and/or steam containing atmospheres at 700°C or greater. The alloys, consisting of Fe-30Cr-3Al-1Nb-6W with minor alloying additions, exhibited a successful combination of oxidation, corrosion, and creep resistances comparable or superior to those of commercially available heat resistant austenitic stainless steels. An optimized thermo-mechanical treatment combined with selected minor alloying additions resulted in a refined grain structure with high thermal stability even at 1200°C, which improved room-temperature ductility without sacrificing the creep performance. The mechanism of grain refinement in the alloy system is discussed.

There is a critical lack of data on the mechanical behavior of candidate structural materials for advanced nuclear reactors under molten halide salt environments. Limited legacy data from the molten salt reactor experiment (MSRE) program showed a significant reduction in creep rupture strength of a Ni-base alloy in molten fluoride salt. With ongoing efforts to commercialize different molten salt reactor concepts, the industry can considerably benefit from quantitative information on the impact of molten halide salts on the engineering properties such as creep and fatigue strength of materials of interest. The present work aims to assess the role of molten salt corrosion on the creep behavior of three alloys 316H, 617 and 282 at 650-816 °C. Creep tests were conducted in fluoride (FLiNaK) and chloride (NaCl-MgCl 2 ) salts. Initial results from the ongoing testing will be presented which suggest that the molten salt environment caused a 25-50% reduction in creep rupture lifetime compared to air exposures. Physics-based corrosion and creep models were employed to gain some insights into the potential degradation mechanisms.