The current research adopts a novel approach by integrating correlative microscopy and machine learning in order to study creep cavitation in an ex-service 9%Cr 1%Mo Grade 91 ferritic steel. This method allows for a detailed investigation of the early stages of the creep life, enabling identification of features most prone to damage such as precipitates and the ferritic crystal structure. The microscopy techniques encompass Scanning Electron Microscopy (SEM) imaging and Electron Back-scattered Diffraction (EBSD) imaging, providing insights into the two-dimensional distribution of cavitation. A methodology for acquiring and analysing serial sectioning data employing a Plasma Focused Ion Beam (PFIB) microscope is outlined, complemented by 3D reconstruction of backscattered electron (BSE) images. Subsequently, cavity and precipitate segmentation was performed with the use of the image recognition software, DragonFly and the results were combined with the 3D reconstruction of the material microstructure, elucidating the decoration of grain boundaries with precipitation, as well as the high correlation of precipitates and grain boundaries with the initiation of creep cavitation. Comparison between the 2D and 3D results is discussed.

In order to comprehensively assess creep damage of 18Cr-9Ni-3Cu-Nb-N steel (ASME SA-213 S30432), which is widely used in critical high-temperature regions of heat transfer tubes of ultrasupercritical (USC) boilers, our investigation centered on the σ phase. This phase undergoes formation and coarsening during prolonged thermal exposure. We developed a technique to estimate operational heating metal temperatures by analyzing average particle size of the σ phase (MLAS-EX). By extracting a certain number of σ phase from the largest particle size, it is possible to select the σ phase that nucleated and grew in the early stage of heating. The correlation between the average particle size and the Hollomon-Jaffe Parameter (HJP), a parameter of heating temperature and time, allows precise estimation of the heating metal temperature. Our validation demonstrates that the replica method, which is a nondestructive method and effective for evaluating actual plants, is also applicable. Using our newly developed technique for estimating heating metal temperature, it is possible to predict the remaining creep life of heat transfer tubes based on data related to creep rupture characteristics, working stress and operating time. The developed method has already been successfully applied to evaluate the creep life of several actual boilers.

Modified 9Cr-1Mo steel was manufactured via laser powder bed fusion (LPBF) using gas atomized powders under various building conditions. Dense samples were obtained at an energy density of 111-125 J/mm 3 . As-built samples were subjected to a normalization and tempering heat treatments. The microstructure of the as-built sample exhibits a duplex structure, comprising coarse columnar δ-ferrite grains and fine martensite grains. In addition, a small amount of retained austenite phase was observed at the interface between δ-ferrite and martensite. The formation of δ-ferrite is attributed to the extremely rapid solidification that occurs during the LPBF process, while martensite is obtained through the phase transformation because of the thermal cycles experienced during the process. The area fraction of δ-ferrite and martensite can be controlled by adjusting the LPBF parameters. Typical as-built microstructure morphology characterized by the columnar δ- ferrite was eliminated after the heat treatments, resulting in a tempered martensitic microstructure that is identical with that obtained through the conventional process. However, an increase in prior austenite grain size was observed when the area fraction of δ-ferrite in the as-built condition was high, due to faster phase transformation kinetics of martensite than that of δ-ferrite during the normalization. This suggests that the prior austenite grain size can be controlled by optimizing the area fraction of δ-ferrite and martensite in the as-built microstructure.

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.

Alloy 718 is an important class of Nb-bearing Ni-based superalloys for high-temperature applications, such as compressor disks/blades and turbine disks in gas turbine systems. The service temperature of this alloy is, however, limited below 650 °C probably due to the degradation of its strengthening phase γ"-Ni3Nb. Aiming at understanding and improving creep properties of 718-type alloys, we investigated creep behaviors of alloy 718 and alloy Ta-718 where different types of γ" phases, Ni3Nb and Ni3Ta, were precipitated, respectively. Creep tests were conducted at 700 °C under stress conditions of 400 and 500 MPa for the two alloys in aged conditions. It was found that while the minimum creep rates were comparable in the two alloys, the creep rate acceleration was lower in alloy Ta-718 than in alloy 718 under the creep conditions studied. Microstructural observations on the specimens before and after the creep tests suggested that the γ" precipitates were distinguishably finer in alloy Ta-718 than in alloy 718 throughout the creep tests. The formation of planar defects and shearing of γ" precipitates occurred frequently in the alloy 718 specimen. The observed creep deformations were discussed in terms of the critical resolved shear stress due to shearing of γ" particles by strongly paired dislocations.

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.

The microstructure of MoSiBTiC alloys is very complex, with three to four constituent phases and characteristic structures such as fine precipitates and lamellar structures. To perform the microstructural analysis efficiently, image segmentation was first performed for each phase of the microstructural images. Utilizing the Trainable Weka Segmentation method based on machine learning, the required segmentation time was dramatically reduced. Furthermore, by pre-adjusting the contrast of the images, the segmentation could be performed accurately for gray phases with different shades of gray. In addition, the U-Net method, based on deep learning, could perform highly accurate segmentation of characteristic microstructures consisting of multiple phases. The correlations between microstructural features and hardness were investigated using the segmented images in this study. The findings revealed that the volume fraction of each phase and the number of TiC clusters within the field of view significantly influenced hardness. This suggests that the hardness of MoSiBTiC alloys may be controlled by controlling the amount of TiC precipitates.

High gamma prime Ni-based superalloys comprising ≥3.5 % Al are difficult to weld due to high propensity of these materials to weld solidification, heat affected zone liquation, and stress-strain cracking. In this study the root cause analysis of cracking and overview on the developed weldable Ni-based superalloys for repair of turbine engine components manufactured from equiaxed (EA), directionally solidified (DS), and single crystal (SX) materials as well as for 3D AM is provided. It is shown that the problem with the solidification and HAZ liquation cracking of turbine engine components manufactured from EA and DS superalloys was successfully resolved by modification of welding materials with boron and silicon to provide a sufficient amount of eutectic at terminal solidification to promote self-healing of liquation cracks along the weld - base material interface. For crack repair of turbine engine components and 3D AM ductile LW4280, LW7901 and LCT materials were developed. It is shown that LW7901 and LCT welding materials comprising 30 - 32 wt.% Co produced sound welds by GTAW-MA on various SX and DS materials. Welds demonstrated high ductility, desirable combination of strength and oxidation properties for tip repair of turbine blades. Examples of tip repair of turbine blades are provided.

To maximize the mechanical properties of Ni-base superalloys, solution heat treatment is essential to sufficiently homogenize the dendritic segregations formed during solidification. To investigate the homogenization behavior during solution heat treatment, a Ni-base single crystal superalloy, TMS-238, was heat treated under various conditions; temperatures ranging from 1573 to 1613 K for times ranging from 2 to 100 h. After solution heat treatment, the average concentrations of Re, an element that exhibits the highest degree of segregation, in dendrite core and inter-dendritic regions were analyzed. From these results, apparent diffusion constants, D app , were determined based on a proposed homogenization model. Obtained D app values were significantly smaller than the diffusion constant of Re in Ni, strongly suggesting that the apparent diffusion coefficients should be obtained experimentally when using the target alloy.

An attempt is being made to develop novel Ni-Mo-W-Cr-Al-X alloys with ICME approach with critical experimental/simulations and processing/microstructural characterization/property evaluation and performance testing has been adopted. In this work, based on thermodynamic modeling five alloy compositions with varying Mo/W and two alloys with high tungsten modified with the addition of Al or Ti were selected and prepared. The newly developed alloys were evaluated for their response to thermal aging in the temperature range of 700 to 850 °C and corrosion in the KCl-NaCl-MgCl 2 salt under suitable conditions. Thermally aged and post-corrosion test samples were characterized to ascertain phase transformations, microstructural changes and corrosion mechanisms. Al/Ti modified alloys showed significant change in hardness after 400 hours aging at 750°C, which was found to be due to the presence of fine γ’/γ” precipitates along with plate-shaped W/Mo-rich particles. These alloys show comparable molten salt corrosion resistance as commercial alloys at 750°C for 200-hour exposures. The good corrosion behavior of these alloys may be attributed to the formation of a protective multicomponent Al-or Ti-enriched oxide as well as the unique microstructure.

Diffusion bonding is a key manufacturing process for nucleation applications including compact heat exchangers. Accurately predicting the alloy's behavior during the diffusion bonding process presents challenges, primarily due to the intricate interplay of microstructural evolution and physical processes such as compressive loading, temperature history, and component migration. The current study develops a phase-field model designed to simulate the diffusion bonding in 316H stainless steel, a material with exceptional high-temperature strength, corrosion resistance and suitability to high-pressure conditions. Our model incorporates a multi-phase, multi-component framework that aligns the experimental observations with the grain growth and heterogeneous nucleation, where arbitrary external compressive load and temperature history are considered. The simulations focus on grain nucleation, growth, and microstructure evolutions across diffusion bonding line under a variety of temperature profiles, mechanical loads, and surface roughness conditions, mirroring experimental setups. Our model predicts consistent simulation results with experiments in terms of the grain size and distribution near the bonding area, offering a better understanding of the diffusion bonding mechanism and the manufacturing process for building reliable compact heat exchangers.

Supercritical carbon dioxide cooling during machining has been identified as an effective measure to mitigate the risk of stress corrosion cracking in materials utilized in the primary circuit of light water reactors, particularly in pressure vessel structural steels. This study aims to compare two different cooling methods, the novel supercritical carbon dioxide and conventional high pressure soluble oil, employed during both milling and turning processes for SA508 Grade 3 Class 2 and AISI 316L steels. As the surface conditions of materials are critical to fatigue properties, such as crack initiation and endurance life, the fatigue performance of both cooling methods for each process were then evaluated and the impact on properties determined. To compare the potential benefits of supercritical carbon dioxide cooling against conventional soluble oil cooled machining, fatigue specimens were machined using industry relevant CNC machine tools. Surface finish and machining methods were standardized to produce two different specimen types, possessing dog- bone (milled) and cylindrical (turned) geometries. Force-controlled constant amplitude axial fatigue testing at various stress amplitudes was undertaken on both specimen types in an air environment and at room temperature using a stress ratio of 0.1. The fatigue performance of the supercritical carbon dioxide cooled specimens revealed substantially greater endurance lives for both SA508 and 316L materials, when compared with specimens machined using high pressure soluble oil cooling.

The microstructural evolution of the MoSiBTiC alloy by rapid solidification and its effect on oxidation and mechanical properties were investigated in this study. A Mo-5Si-10B-10Ti-10C (at%) alloy was produced by a conventional arc-melting technique in an Ar atmosphere, and then it was rapidly solidified by tilt-casting into a rod-shaped copper hearth. Vickers hardness values increased drastically above 1000 Hv due to the microstructure refinement through rapid solidification. They rose from the center toward the outer surface, ranging from about 1100 to 1300 Hv. Interestingly, the oxidation resistance of the rapidly solidified MoSiBTiC alloy at 1100 °C was dramatically improved, probably due to the microstructure refinement effect with ultrafine grains. However, the fracture toughness value of the rapidly solidified MoSiBTiC alloy was about 8 MPa·m 1/2 , less than half of the cast and heat-treated MoSiBTiC alloy previously reported. Heat treatment and composition optimization will further improve the performance of the rapidly solidified MoSiBTiC alloy.

Damage in the grade 91 steel partially transformed zone of weld heat affected zones has historically been associated with many different types of microstructural features. Features described as being responsible for the nucleation of creep damage include particles such as laves phase, coarse M 23 C 6 , inclusions, nitrides, or interactions between creep strong and creep week grains, grain boundaries and potentially other sources. Few studies have attempted to link the observations of damage on scales of increasing detail from macro, to micro, to nano. Similarly, assessments are not made on a statistically relevant basis using 2D or 3D microscopy techniques. In the present paper, 2D assessment using scanning electron microscopy (SEM) and quantification techniques such as energy dispersive X-ray spectroscopy (EDS) and electron backscatter diffraction (EBSD) are utilized in combination with 3D serial sectioning of large volumes using plasma focused ion beam milling (P-FIB) and simultaneous EDS to evaluate an interrupted cross-weld creep test. Moreover, the sample selected for examination was from a feature cross-weld creep test made using a parent material susceptible to the evolution of creep damage. The test conditions were selected to give creep brittle behaviour and the sample was from a test interrupted at an estimated life fraction of 60%. The findings from these evaluations provide perspective on the features in the microstructure responsible for the nucleation and subsequent growth of the observed damage.

Creep strength of Grade 91 steels has been reviewed and allowable stress of the steels has been revised several times. Allowable stress regulated in ASME Boiler and Pressure Vessel Code of the steels with thickness of 3 inches and above was reduced in 1993, based on the re-evaluation with long-term creep rupture data collected from around the world. After steam leakage from long seam weld of hot reheat pipe made from Grade 122 steel in 2004, creep rupture strength of the creep strength enhanced ferritic (CSEF) steels has been reviewed by means of region splitting method in consideration of 50% of 0.2% offset yield stress (half yield) at the temperature, in the committee sponsored by the Ministry of Economy, Trade and Industry (METI) of Japanese Government. Allowable stresses in the Japanese technical standard of Grade 91 steels have been reduced in 2007 according to the above review. In 2010, additional long-term creep rupture data of the CSEF steels has been collected and the re-evaluation of creep rupture strength of the steels has been conducted by the committee supported by the Federation of Electric Power Companies of Japan, and reduction of allowable stress has been repeated in 2014. Regardless of the previous revision, additional reduction of the allowable stress of Grade 91 steels has been proposed by the review conducted in 2015 by the same committee as 2010. Further reduction of creep rupture strength of Grade 91 steels has been caused mainly by the additional creep rupture data of the low strength materials. A remaining of segregation of alloying elements has been revealed as one of the causes of lowered creep rupture strength. Improvement in creep strength may be expected by reducing segregation, since diffusional phenomena at the elevated temperatures is promoted by concentration gradient due to segregation which increases driving force of diffusion. It has been expected, consequently, that the creep strength and allowable stress of Grade 91 steels can be increased by proper process of fabrication to obtain a homogenized material free from undue segregation.

A newly developed ferritic heat-resistant steel; 9Cr-3W-3Co-Nd-B steel has higher creep rupture strength both in the base metal and welded joints than the conventional high-Cr ferritic heat-resistant steels. The creep rupture strengths of 9Cr-3W-3Co-Nd-B steel welded joints were below the lower limit of the base metal in long-term creep stage more than 20,000 hours. The creep rupture position was heat-affected zone (HAZ) from 1.0 to 1.5 mm apart from the fusion line on the welded joint specimen ruptured at 34,966 hours. The equiaxed subgrains and coarsened precipitates were observed in HAZ of the ruptured specimen. In order to clarify the creep fracture mechanism of the welded joints, the microstructures of HAZ were simulated by heat cycle of weld, then observed by EBSD analysis. Fine austenite grains formed along the prior austenite grain boundaries in the material heated just above A C3 transformation temperature, however there were no fine grains such as conventional steel welded joints. The prior austenite grain boundaries were unclear in the material heated at 1050 °C. The creep rupture life of the material heated at just above A C3 transformation temperature exceeded the lower limit of base metal and there was no remarkable degradation, although it was shorter than the other simulated materials. It is, therefore, concluded that the creep fracture of 9Cr-3W-3Co-Nd-B steel welded joint in long-term stage occurred at HAZ heated at from just above A C3 transformation temperature to 1050 °C. It is speculated that the fine austenite grains formed along the prior austenite grain boundaries and inhomogeneous microstructures cause the coarsening precipitates and recovery of lath structure during long-term creep deformation.

The formation of periodically arrayed rows of very fine Fe 2 Hf Laves phase particles was recently found in 9 wt. % chromium ferritic matrix through interphase precipitation along a reaction path of δ-ferrite → γ-austenite + Fe 2 Hf with a subsequent phase transformation of the γ phase into the α-ferrite phase. One of the problems on the formation of the fine Laves phase dispersion is a poor heat treatability; the interphase precipitation (δ-Fe→γ-Fe+Fe 2 Hf) is competitive with the precipitation of Laves phase from the δ phase in the eutectoid-type reaction pathway (δ→δ+Fe 2 Hf). In the present work, the effect of supersaturation on the precipitation of Laves phase from δ phase (δ→δ+Fe 2 Hf) and the δ→γ transformation in the reaction pathway was investigated by changing the Hf and Cr contents. The results obtained suggest that it is effective to have a high supersaturation for the precipitation of Laves phase and an adequately high supersaturation for the δ→γ transformation at the same time in order to widen the window of the interphase precipitation

Creep strength enhanced ferritic steels like T/P 91 and T/P 92 are widely used for the fabrication of pressure vessel components in the petro-chemical and thermal power industry. Today, a new generation of 9-12% Cr CSEF steels like MARBN, Save12AD, G115 and Super VM12 are entering into the market. All CSEF steels require an accurate post-weld heat treatment after welding. This paper discusses the impact of chemical composition on Ac1 as well as the transformation behavior during post-weld heat treatment in a temperature range below and above Ac1. The Ac1 temperature of weld metals with variations in chemical composition has been determined and thermodynamic calculations has been carried out. Simulations of heat treatment cycles with variations in temperature have been carried out in a quenching dilatometer. The dilatation curves have been analyzed in order to detect any phase transformation during heating or holding at post weld heat treatment. Creep rupture tests have been carried out on P91 and Super VM12 type weld metals in order to investigate the effect of sub- and intercritical post weld heat treatment on creep rupture strength.

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.

Microstructure change during creep at 650°C has been examined for a high-B 9%Cr steel by FIB-SEM serial sectioning 3D observation, Nano-SIMS, SEM, EBSD and TEM. The precipitates formed in the steel were M 23 C 6 , Laves phase, and a quite small amount of MX. For as-tempered steel, precipitation of M 23 C 6 on the prior austenite grain boundaries was clearly found, while precipitation of the Laves phase was not confirmed during tempering. The volume fraction of the Laves phase gradually increased with elapsed time, while M 23 C 6 appeared to increase once and decrease afterward, based on the comparison between the 2,754 h ruptured sample and the 15,426 h ruptured sample. Nano-SIMS measurements have revealed that B segregates on the prior austenite grain boundaries during normalizing, and it dissolves into M 23 C 6 .