This study investigates the mechanisms of temper embrittlement in 410 martensitic stainless steel, a material widely used in steam turbine blades due to its excellent corrosion resistance and high strength achieved through quenching and tempering heat treatments. While the material’s hardness and impact toughness strongly depend on tempering temperatures, significant embrittlement occurs around 540°C, manifesting as decreased Charpy impact energy alongside increased strength and hardness. To understand this phenomenon at the nanometer scale, high-resolution transmission electron microscopy (TEM) analysis was performed, focusing on electron diffraction patterns along the <110>α-Fe and <113>α-Fe zone axes. The analysis revealed distinctive double electron diffraction spots at 1/3(211) and 2/3(211) positions, with lattice spacing of approximately 3.5 Å—triple the typical α-bcc lattice spacing (1.17 Å). These regions were identified as metastable “zones” resembling ω-phase structures, potentially responsible for the embrittlement. While this newly identified phase structure may not fully explain the complex mechanisms of temper embrittlement, it provides valuable insights for developing improved alloying and heat treatment methods to mitigate embrittlement in martensitic steels.

A FeCrMnNi concentrated solid-solution alloy was irradiated with a 2 MeV proton beam up to 1 dpa and 6 dpa at temperatures of 400 °C and 600 °C. The microstructural changes induced by irradiation were characterized using Transmission Electron Microscopy (TEM). In samples irradiated at 400 °C, Frank loops were the predominant form of lattice damage at 1 dpa, whereas small defect clusters were more prevalent at 6 dpa. For the sample irradiated to 1 dpa at 600 °C, both Frank loops and small defect clusters were present in similar density. Nanoindentation was employed to assess the changes in mechanical properties (hardness) post-irradiation, revealing significant hardening in all irradiated samples. The results indicated that the hardening effect began to saturate at 1 dpa or earlier. Additionally, nanoindentation creep tests with a 1200-second dwell period produced stress exponents comparable to those obtained from conventional creep testing. The findings suggest a shift in the deformation mechanism from dislocation glide to dislocation climb in the sample irradiated to 6 dpa at 400 °C.

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.

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.

Modified 9Cr-1Mo steel (ASTM Gr.91) is widely used in components of fossil fueled power plants around the world today. This grade of steel has however been shown to exhibit significant variations in creep life and creep ductility, which has led to premature in-service failures. The aim of this work is to define potential metallurgical risk factors that lead to this variation in performance. To achieve this, a set of creep test samples that represent a wide range in this variation of creep behavior in this steel grade have been studied in detail. As a first stage in this characterization the macro-scale chemical homogeneity of the materials were mapped using micro-XRF. Understanding the segregation behavior also allows quantification of microstructural parameters in both segregated and non-segregated areas enabling the variations to be determined. For example this showed a significant increase in the number per unit area of Laves phase particles in high compared with low Mo content areas. To study the effect of MX particles on segregation a methodology combining SEM and TEM was employed. This involved chemically mapping the larger V containing particles using EDS in the SEM in segregated and unsegregated areas and then comparing the results to site-specific TEM analysis. This analysis showed that although the average size of the V containing samples is in the expected 0-50 nm size range, these particles in some samples had a wide size distribution range, which significantly overlaps with the M 23 C 6 size distribution range. This together with the segregation characteristics has important implications for determining meaningful quantitative microstructural data from these microstructurally complex materials.

The microstructures and mechanical properties of T122 steel used for superheater tube of the boiler in a 1000 MW ultra supercritical power plant after service for 83,000h at 590℃ were investigated, and compared with data of that served for 56,000h in previous studies. The results show that compared with T122 tube sample service for 56,000h, the tensile properties at room temperature and the size of precipitated phase exhibit few differences, but the lath martensites features are apparent, and the Brinell hardness value are obviously higher. SEM and TEM experiments show that the substructure is still dominated by lath martensite. A few lath martensites recover, subgrains appear and equiaxe, and the dislocation density in grains is relatively low. A large number of second-phase particles precipitated at boundaries of original austenite grains and lath martensite phases, which are mainly M 23 C 6 and Laves phases.

This study presents a characterization of the microstructural evolutions taking place in a 9%Cr martensitic cast steel subjected to fatigue and creep-fatigue loading. Basis for this study of investigation is an extensive testing program performed on a sample heat of this type of steel by conducting a series of service-like high temperature creep-fatigue tests. The major goal here was to systematically vary specific effects in order to isolate and describe relevant damage contributing mechanisms. Furthermore, some of the tests have been interrupted at several percentages of damage to investigate not only the final microstructure but also their evolution. After performing those tests, the samples were examined using transmission electron microscopy (TEM) to characterize and quantify the microstructural evolutions. The size distribution of subgrains and the dislocation density were determined by using thin metal foils in TEM. A recovery process consisting of the coarsening of the subgrains and a decrease of the dislocation density was observed in different form. This coarsening is heterogeneous and depends on the applied temperature, strain amplitude and hold time. These microstructural observations are consistent with the very fast deterioration of creep properties due to cyclic loading.

Nickel-based Alloy 617B (DIN 2.4673) and Alloy C-263 (DIN 2.4650) with high creep strength and good fabricability are promising material candidates for the design of next generation coal-fired “Advanced Ultra-Super-Critical A-USC” power plants with advanced steam properties and thus higher requirements on the material properties. Microstructural studies of the precipitation hardened alloy C-263 were performed with Electron Microscopy (TEM) with respect to their strengthening precipitates like carbides and intermetallic gamma prime. Specimens were subjected to different ageing treatments at elevated temperatures for different times. The microstructural results of the investigated nickel alloy C-263 are presented and discussed with respect to their correlation with required properties for A-USC, e.g. the mechanical properties, the creep resistance and the high temperature stability and compared to Alloy 617B. The manufacturing procedure for the prematernal and forgings as well as for thin walled tube components for A-USC power plants is presented.

By utilizing computational thermodynamics in a Design of Experiments approach, it was possible to design and manufacture nickel-base superalloys that are strengthened by the eta phase (Ni3Ti), and that contain no gamma prime (Ni3Al,Ti). The compositions are similar to NIMONIC 263, and should be cost-effective, and have more stable microstructures. By varying the aging temperature, the precipitates took on either cellular or Widmanstätten morphologies. The Widmanstätten-based microstructure is thermally stable at high temperatures, and was found to have superior ductility, so development efforts were focused on that microstructure. High temperature tensile test and creep test results indicated that the performance of the new alloys was competitive with NIMONIC 263. SEM and TEM microscopy were utilized to determine the deformation mechanisms during creep.

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.

Austenitic and super-austenitic stainless steels are a critical component of the spectrum of high temperature materials. With respect to power generation, alloys such as Super 304H and NF709 span a gap of capability between ferritic and martensitic high chromium steels and nickel-based alloys in boiler tube applications for both conventionally fired boilers and heat-recovery steam generators (HRSG). This research explores a wrought version of a cast austenitic stainless steel, CF8C-Plus or HG10MNN, which offers promise in creep strength at relatively low cost. Various manufacturing techniques have been employed to explore the impact of wrought processing on nano-scale microstructure and ultimately performance, especially in high temperature creep. Transmission electron microscopy has been used to quantify and characterize the creep-strengthening particles examining the relationship between traditional melting and extrusion as compared to powder metallurgy.

ASME Grade 91 steel seam-welded elbow pipe, which has been used in a USC plant (A-Plant) for about 6 × 10 4 h, was investigated to clarify the microstructure and remaining creep life of the material at long-term region. SEM and TEM observations were conducted on specimens cut from the welded portions of the intrados and extrados of the elbow, and the number density of creep voids in fine-grained HAZ was measured in the wall-thickness direction. Then, creep rupture tests were performed to examine the remaining life of each portion of the base metal and welded joint. On the basis of the results, it was suggested that the microstructural changes were small and that the cumulative creep damage was also small for the elbow pipe during its use at the USC plant for about 6 × 10 4 h. The present result was compared with the result of an investigation on Grade 91 steel elbow used in another USC plant (B-Plant) for about 5 × 10 4 h. The A-Plant material had a creep life about ten times longer than that of the B-Plant material for not only the base metals but also the welded joint. Through the comparison of the investigation results, it was suggested that the difference in the creep deformation property between the base metals of the elbows was the main reason for the difference in their creep lives.

In order to evaluate long term creep strength of modified 9Cr ferritic steels, the system free energy of creep ruptured specimens at both 650 and 700 °C is evaluated as the sum of chemical free energy, strain energy and surface energy, which are obtained by a series of experiments, i.e., chemical analysis using extracted residues, X-ray diffraction, and scanning transmission electron microscopy. Change ratio of the system free energy and creep stress showed the relationship with one master curve irrespective of creep conditions, indicating that the steel ruptures when the applied stress exceeds a limited stress depending on the microstructural state expressed by the change ratio of system free energy. Furthermore, it was found that dominant factor of the change ratio was the chemical free energy change. On the basis of these results, long term creep strength of the steel was evaluated at 700 °C, for example, 19MPa at 700 °C after 10 5 h. It is concluded that long term creep strength of modified 9Cr ferritic steels can be predicted by the system free energy concept using the ruptured specimens with various creep conditions.

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.

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.

In order to study the effect of precipitation strengthening by MX precipitates on the restriction of microstructure degradation in 9 mass% Cr ferritic heat-resistant steels, V, Nb additioned model steels were evaluated by microstructure analysis through TEM and EBSD with reference to the creep test and creep interrupting test. VN precipitation increased the creep strength if the content was higher than 0.02%. Simultaneous addition of Nb and V in the specimen resulted in the complex NbC-VN precipitates even in the as-heat-treated specimens. The coherent and fine-needle-type VN was also detected in the steel. These precipitates are expected to increase the creep strength according to the creep strain curves. V variation up to 0.02% did not affect the crystallographic character of the grain boundary in the as-heat-treated specimens. Nb variation affected the crystallographic character of the grain boundary significantly because of the grain refinement effect of NbC. VN precipitation during the creep test restricted the crystallographic misorientation-angle-profile degradation. Integrating all intragranular precipitates, VN, restricts the crystallographic degradation significantly. The long-term creep test results and the precise precipitation analysis will be disclosed by the presentation.

Contrary to expectations, long-term performance of creep stress enhanced ferritic steels (CSEF) falls short of predictions based on short-term data. This discrepancy is attributed to the formation and growth of creep voids, leading to reduced ductility. This study investigates cavities in creep-tested P92 steel, revealing an association with large ceramic particles (1-2 μm) in standard samples. Three distinct particle compositions were identified: boron nitride (BN), manganese sulfide, and γ-Al 2 O 3 . Statistical analysis showed a strong correlation between BN particles and cavity formation. Using a 3D “slice and view” technique with a focused ion beam/field emission gun scanning electron microscope (FIB-FEGSEM), the study revealed irregular shapes for both cavities and associated particles. Furthermore, analysis of the head-gauge transition area (lower stress exposure) showed small cavities near BN particles, suggesting preferential nucleation on these hard, irregular features. These findings strongly support the hypothesis that BN particles play a key role in cavity nucleation, impacting the long-term performance of P92 steel.

High nitrogen steel was manufactured by solid state nitriding and Laminate- rolling at laboratory to study the nitride morphology and creep properties through the TEM, EPMA and creep strain test. Nitriding made the nitride dispersing steels possible. Solid state nitriding of thin plates and those laminate rolling enabled the high nitrogen containing thick plate steel. Precipitated coarse nitrides during the nitriding resolved by normalizing and re-precipitated by tempering finely. Needle type VN was detected in V containing high nitrogen steels. Its coherency seems to affect the creep strength significantly. V precipitated steels indicated the higher creep strength than the steels without VN precipitation. Thermodynamically stable precipitates like VN increases the creep rupture strength. Ti and Zr containing high nitrogen steels also will be evaluated and discussed by the presentation.

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).