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.

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.

25Cr-20Ni-Nb-N (Tp310HCbN) steel is a promising austenitic steel for applications in superheater tubes in coal fired thermal power plants due to the high creep strength and oxidation resistance. In this work, the microstructural evolution of this material during heat treatment and thermal ageing has been investigated. The investigations were carried out by Light Optical Microscopy (LOM), Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM) and Energy Dispersive Spectroscopy (EDS). Besides, equilibrium and Scheil calculations were carried out using the thermodynamic software MatCalc to analyse the stable phases and the solidification process, respectively. Precipitation calculations during solution annealing and subsequent ageing at 650 and 750°C were performed to predict the phase fraction and precipitates radius up to 10.000h ageing time. SEM and TEM investigations of aged specimens revealed the presence of six different precipitates: M 23 C 6 , Cr 2 N, sigma, Z-phase, eta-phase (Cr 3 Ni 2 Si(C,N)) and Nb(C,N). These precipitates were predicted and confirmed by MatCalc simulations. The calculated phase fraction and mean radius show good agreement with experimental data. Finally, simulations of different Cr-, C- and N-content in Tp310HCbN were performed.

This paper presents comprehensive test results of thick-walled VM12 steel pipes containing 12% chromium, vanadium, and tungsten, with cobalt addition. The primary objective was to verify welding technologies for boiler superheater thick-walled components and characterize the strength, technological properties, and microstructure of welded joints produced at RAFAKO S.A. The extensive research program encompassed a broad range of tests on both parent material and welded joints, including mechanical property assessments at room temperature, creep resistance evaluations, low-cycle fatigue testing at room temperature and 600°C (1120°F), and detailed macro- and microstructural examinations. Furthermore, the investigation included a comprehensive microstructural stability assessment using light microscopy (LM), scanning electron microscopy (SEM), and transmission electron microscopy (TEM), conducted after fatigue resistance testing at room and elevated temperatures, following additional annealing at 700°C (1,920°F), and after 1,000 hours of exposure for both parent material and welded joints. These investigations were conducted as part of the COST 536 Action, representing a collaborative effort to understand and characterize high-temperature creep-resistant steels like VM12 for advanced power generation applications.

Alumina-forming austenitic stainless steels (AFAs) are potential materials for boiler/steam turbine applications in next generation fossil fuel power plants. They display a combination of good high temperature creep strength, excellent oxidation resistance and low cost. A recently-developed AFA alloy based on Fe-14Cr-32Ni-3Nb-3Al-2Ti (wt.%) shows better creep performance than a commercially-available Fe-based superalloy. In this paper we used scanning electron microscopy and transmission electron microscopy to study the fracture surfaces and cracking behavior in relation to the precipitates present in creep failure samples of this alloy tested at either 750°C/100 MPa or 700°C/170 MPa. It was found that most cracks are formed along the grain boundaries with precipitate-free zones beside the grain boundaries potentially providing the path for propagation of cracks.

Inconel alloy 740H is designated for boiler sueprheater/reheater tubes and main steam/header pipes application of advanced ultra-supercritical (A-USC) power plant at operating temperatures above 750°C. Microstructure evolution and precipitates stability in the samples of alloy 740H after creep-rupture test at 750°C, 800°C and 850°C were characterized in this paper by scanning electron microscopy, transmission electron microscopy and chemical phase analysis in details. The phase compositions of alloy 740H were also calculated by thermodynamic calculation. The research results indicate that the microstructure of this alloy keeps good thermal stability during creep-rupture test at 750°C, 800°C and 850°C. The precipitates are MC, M 23 C 6 and γ′ during creep-rupture test. The temperature of creep test has an important effect on the growth rate of γ′ phase. No harmful and brittle σ phase was found and also no γ′ to η transformation happened during creep. Thermodynamic calculations reveal almost all the major phases and their stable temperatures, fractions and compositions in the alloy. The calculated results of phase compositions are consistent with the results of chemical phase analysis. In brief, except of coarsening of γ′, Inconel alloy 740H maintains the very good structure stability at temperatures between 750°C and 850°C.

The microstructural evolution of the Ni-based superalloy CMSX-4 including the change in gamma prime size and distribution and the degree of rafting has been examined in detail using field emission gun scanning electron microscopy (FEGSEM) and transmission electron microscopy (TEM) after high temperature degradation and rejuvenation heat treatments. The relationship between the microstructure, mechanical properties and the applied heat treatment procedures has been investigated. It is shown that there are significant differences in the rafting behaviour, the size of the ‘channels’ between the gamma prime particles, the degree of rafting and the size of the tertiary gamma prime particles in each of the different microstructural conditions studied. Chemical segregation investigations were carried out to establish the cause of reduced mechanical properties of the rejuvenated sample after high temperature degradation compared to an as-received sample after the same degradation procedure. The results indicate that although the microstructure of as-received and rejuvenated samples were similar, the chemical segregation was more pronounced in the rejuvenated samples, suggesting that chemical segregation from partitioning of the elements during rejuvenation was not completely eliminated. The aim of this research is to provide greater understanding of the suitability of rejuvenation heat treatments and their role in the extension of component life in power plant applications.

An iron aluminide (Fe 3 Al) intermetallic coating was deposited onto F22 (2.25Cr-1Mo) steel substrate using a JP-5000 high velocity oxy-fuel (HVOF) thermal spray system. The as-sprayed coating was characterized by electron microscopy, X-ray diffraction, oxidation, and adhesion. Fe 3 Al coated steel specimens were exposed to a mixed oxidizing/sulfidizing environment of N 2 -10%CO-5%CO 2 -2%H 2 O-0.12%H 2 S (by volume) at 500, 600, 700, and 800°C for approximately seven days. All specimens gained mass after exposure, inversely proportional to temperature increases. Representative cross-sectioned specimens from each temperature underwent scanning electron microscopy (SEM) and X-ray mapping examination. Results are presented in terms of corrosion weight gain and product formation. The research evaluated the effectiveness of an HVOF-sprayed Fe 3 Al coating in protecting a steel substrate exposed to a fossil energy environment.

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.

The newly developed 12%Cr steel Super VM12 is characterized by excellent creep rupture strength properties (better than Grade 92) and enhanced steam oxidation resistance of 12%Cr steels such as VM12-SHC. Balanced properties profile of the new steel development in comparison to the existing well-established steels such as Grade 91 and Grade 92, opens opportunities for its application as construction material for components in existing or future high-efficiency power plants. In this study the oxidation behavior of typical 9%Cr steels was compared with the new steel development. The oxide scale morphologies and compositions of different oxide layers as function of temperature and exposure time in steam-containing atmospheres were characterized using light optical metallography, Scanning Electron Microscopy (SEM). Creep testing has been carried out in the temperature range between 525°C and 700°C. Selected creep specimens were investigated using the Transmission Electron Microscopy and the Atom Probe Tomography techniques.

Long-term creep tested specimens of the advanced austenitic stainless steel Super 304H were subjected to detailed metallographic analysis with an emphasis on the relationship between creep induced cavities (voids) and microstructural features. The creep specimens were tested between 873 and 973 K (600 and 700°C) at stresses between 110 and 340 MPa, with rupture times up to ~1.8 x 10 8 s (50,000 hours). To characterize damage, the distributions of creep cavities along the length of the gage section were determined and microstructural features associated with the cavities were investigated using optical microscopy and scanning electron microscopy.

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 recently developed 12%Cr steel VM12-SHC is characterized by very good creep properties at temperatures up to 620°C. This new material development exhibits an excellent oxidation resistance in steam atmospheres at the typical application temperature but also at temperatures up to 650°C. In comparison to the existing 9% Cr grades T/P91 and T/P92, VM12-SHC steel opens due to its excellent oxidation behavior, new possibilities for its application as a heat exchanger boiler component. It was found that outside its application temperature range VM12-SHC also shows, as all 9-12%Cr steels, the appearance of the so called Z-phase. This effect was investigated to understand its influence on creep properties of this class of ferritic/martensitic steels aiming at controlling the microstructure stabilities for future grade developments. Creep testing has been carried out in the temperature range between 525°C and 700°C. Selected crept specimens have been investigated using light optical microscopy, SEM with EDX and TEM. In this study, the oxidation behavior of a number of typical martensitic 9-12%Cr steels was compared with the newly developed 12% Cr steel VM12-SHC. The compositions and morphologies of oxide scales formed after 5000 h exposure steels in simulated steam environments as function of temperature were characterized by light optical metallography and scanning electron microscopy (SEM) with energy dispersive X-ray analysis (EDX).

CrMoV cast steels are widely utilized for steam turbine and valve casings, and are subjected to operating and loading conditions which can promote damage mechanisms such as thermal fatigue, creep, erosion, etc. These components are subjected to variable, and sometimes severe conditions because of flexible operation. Therefore, there is a growing need for weld repair techniques including those which do not mandate post weld heat treatment (PWHT), e.g. so-called ‘temper bead’ weld repair. In this study, a simulated weld repair was performed using a temper bead technique. The maximum hardness in the heat affected zone (HAZ) CrMoV steel was ≤400HV. The integrity of the repair methodology was investigated using destructive testing, including hardness mapping, Charpy impact tests, tensile tests, low cycle fatigue and cross-weld creep, and the microstructure was assessed using light optical microscopy and scanning electron microscopy (SEM).

In this study, 25Cr2Ni2Mo1V filler metal was deposited to weld low pressure steam turbine shafts, which are operated in fossil power plants. A comparison experiment was conducted on the weld metals (WMs) before and after varied various aging duration from 200 hours up to 5000 hours at 350 ℃. Microstructure was characterized by means of scanning electron microscopy (SEM) and electron back-scattered diffraction (EBSD) techniques. In addition, mechanical properties of corresponding specimens were evaluated, e.g. Vickers microhardness, Charpy V impact toughness and tensile strength. It is shown that the tensile strength remained stable while impact energy value decreased with increasing aging duration. Based on the experiment above, it was concluded that the variation of mechanical properties can be attributed to the redissolution of carbides and reduction of bainite lath substructure.

The A-USC technology is still under development due to limited number of materials complying with the requirements of high creep strength and high performance in highly aggressive corrosion environments. Development of power plant in much higher temperatures than A-USC is currently impossible due to the materials limitation. Currently, nickel-based superalloys besides advanced austenitic steels are the viable candidates for some of the A-USC components in the boiler, turbine, and piping systems due to higher strength and improved corrosion resistance than standard ferritic or austenitic stainless steels. The paper, presents the study performed at 800 °C for 3000 hours on 3 advanced austenitic steels; 309S, 310S and HR3C with higher than 20 Cr wt% content and 4 Ni-based alloys including: two solid-solution strengthened alloys (Haynes 230), 617 alloy and two (γ’) gamma - prime strengthened materials (263 alloy and Haynes 282). The high temperature oxidation tests were performed in water to steam close loop system, the samples were investigated analytically prior and after exposures using Scanning Electron Microscopy (SEM) coupled with Energy Dispersive Spectrometry (EDS), and X-Ray Diffractometer (XRD). Mass change data have been examined every 250 hours.

In the present study a creep resistant, ferritic steel, based on the chemical composition of Crofer 22 H, was analysed regarding microstructure and particle evolution. Because of the preceding hot-rolling process formation of sub-grain structures was observed, which disappears over time. Additionally formation of particle-free zones close to high angle grain boundaries was observed. These zones are considered to be responsible for long-term material failure by lacking particle hardening and thus a concentration of deformation. Therefore in-depth analyses by transmission and scanning electron microscopy were performed to investigate dislocation behaviour in these areas

A 10%Cr martensitic steel with 3%Co and 0.008%B exhibits extremely long creep rupture time of approximately 40000 h under an applied stress of 120 MPa at a temperature of 650°C. The steel’s microstructure after creep tests interrupted at different creep stages was examined by transmission and scanning electron microscopy. It was shown that superior creep resistance of this steel was attributed to slow increase in creep rate at the first stage of tertiary creep whereas the rapid acceleration of creep rate took place only at the short second stage of tertiary creep. Transition from minimum creep rate stage to tertiary creep was found to be accompanied by coarsening of Laves phase particles, whereas M 23 C 6 – type carbides demonstrated high coarsening resistance under creep condition. Strain-induced formation of Z-phase does not affect the creep strength under applied stress of 120 MPa due to nanoscale size of Z-phase particles.

The steam oxidation behaviour of boiler tubes and steam piping components is a limiting factor for improving the efficiency of the current power plants. Spallation of the oxide scales formed during service can cause serious damage to the turbine blades. Vallourec has implemented an innovative solution based on an aluminum diffusion coating applied on the inner surface of the T/P92 steel. The functionality of this coating is to protect the tubular components against spallation and increase the actual operating temperature of the metallic components. In the present study, the newly developed VALIORTM T/P92 product was tested at the EDF La Maxe power plant (France) under 167b and 545°C (steam temperature). After 3500h operation, the tubes were removed and characterized by Light Optical Metallography (LOM), Scanning Electron Microscopy (SEM), with Energy Dispersive X-ray spectrometry (EDX) and X-Ray Diffraction (XRD). The results highlight the excellent oxidation resistance of VALIORTM T/P92 product by the formation of a protective aluminum oxide scale. In addition, no enhanced oxidation was observed on the areas close to the welds. These results are compared with the results obtained from laboratory steam oxidation testing performed on a 9%Cr T/P92 steel with and without VALIORTM coating exposed in Ar-50%H 2 O at 650°C.

This study investigates the impact of adding small amounts of rare earth (RE) elements on the properties and microstructures of SA335P91 steel welds. The RE elements were incorporated into the weld metal using a coating process. The researchers then proposed an optimal RE formula aimed at achieving improved properties and microstructures. To evaluate the effectiveness of this approach, various tests were conducted on both welds with and without RE additions. These tests included tensile testing (both at room and high temperatures), impact testing, metallographic analysis to examine the microstructure, determination of phase transformation points, scanning electron microscopy, and X-ray diffraction. The results revealed that the addition of RE elements has the potential to enhance the properties and modify the microstructure of SA335P91 welds.