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.

Miniature specimen tests are necessary to assess the mechanical properties of new fuel cladding alloys for next-generation nuclear reactors. The small specimen allows for extensive testing programs from limited volumes of material. However, there is a lack of testing equipment to perform high-temperature mechanical tests on the miniature specimen. This work presents the development of a high-temperature creep test system for miniature specimens with in situ scanning electron microscope (SEM) testing capability for real-time characterization. Here, we discuss the challenges of the development of the system, such as gripping the samples, loading, heating, cooling mechanisms, and strain measurement. The equipment is used to investigate the creep behavior of FeCrAl alloy Kanthal APMT, and the results are compared with conventional creep test data from the same batch of this material.

According to ASME Case N-888-3, Similar and Dissimilar Metal Welding Using Ambient Temperature SMAW or Machine GTAW Temper Bead Technique, a 48 hr waiting period before conducting the final nondestructive examination (NDE) is required when ferritic filler weld metal is used. The purpose of the 48 hr hold is to confirm the absence of hydrogen-induced cracking in the temper bead heat-affected zone. In previous research, the effect of post-weld heat treatment (PWHT) and temper bead welding (TBW) on the hydrogen-induced cracking (HIC) susceptibility in the coarse-grained heat-affected zone (CGHAZ) in welds of SA-508, P-No. 3 Group 3, pressure vessel steel was investigated using the Delayed Hydrogen Cracking Test (DHCT). In that previous study, the Gleeble thermomechanical simulator was used to generate six CGHAZ microstructural conditions: as-welded (AW), PWHT, and AW with single a TBW reheat at 675, 700, 725, and 735°C. Hydrogen was introduced to the specimen through cathodic charging under in situ constant tensile stress. The HIC susceptibility for these microstructures was ranked by the DHCT at a diffusible hydrogen level significantly exceeding typical GTAW and SMAW processes. The work described in this paper investigates the susceptibility to HIC of these same CGHAZ microstructures with DHCT at variable current densities, further ranking each condition. Test results were analyzed by fracture surface examination of failed tests, and cross-section microstructural analysis under a scanning electron microscope (SEM). Future steps include evaluating critical hydrogen content levels using gas chromatography for each condition. The results from this study will be used to consider potential elimination of the NDE hold time requirement in Case N-888-3 when ferritic weld metal is used.

18Cr-9Ni-3Cu-Nb-N steel is widely used for heat exchanger tubes such as super-heaters and reheaters of ultra-super critical power generation boilers. In this study, long-term creep rupture tests were carried out on 18Cr-9Ni-3Cu-Nb-N seamless steel tubes of 7 heat materials, and the specimens of 2 heat materials with different creep rupture strengths were observed by ultra-low voltage scanning electron microscope after creep rupture tests. The results of the investigation of the creep rupture specimens and the coverage ratios of M 23 C 6 on grain boundary were different. The cause of this was estimated to be the difference in B content between the 2 heat materials. Creep rupture tests with different final ST temperatures were also carried out using the same heat material, and it was revealed that the higher final ST temperature, the higher the creep rupture strength. As the final ST temperature is higher, the amount of Nb(C, N) solid solution in the matrix increases, and the amount of precipitation of NbCrN and M 23 C 6 increases during creep, therefore it is assumed that the creep rupture strength increases.

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.

Material properties and damage mechanisms exhibit significant variation across weldments. Micro tensile (MT) testing of specimens machined from specific narrow weldment zones is one method to characterize local property variation. Although limited, the literature data on micro-tensile specimen testing reports on low-temperature behavior. However, cross-weld local material data at high service temperatures have not been reported yet. In the present study, MT tests are conducted across similar P22 and P91 steel welds at 550°C and 600°C, respectively. To study deformation mechanisms and the role of surface condition on properties, specimens with different surface conditions (machined, polished, and electropolished) are tested. Two different loading rates of 0.2 mm/min and 0.5 mm/min are used to study the effect of loading rate on deformation and mechanical properties. Variations in weldment material properties are presented as a function of specimen surface conditions and loading speeds. Deformation behavior is studied on the side surfaces of tested micro-tensile specimens using SEM. Deformation is correlated to the microstructural constituent observed on side surfaces.

Martensitic 9Cr steels have been developed which are strengthened by boron in order to stabilize the microstructure and improve their long-term creep strength. Boron plays a key role in these steels by stabilising the martensitic laths by decreasing the coarsening rate of M 23 C 6 carbides, which act as pinning points in the microstructure. In this work two modified FB2 steel forgings are compared. Both forgings have similar compositions but one underwent an additional remelting process during manufacture. Creep tests showed that this additional processing step resulted in a significant increase in time to failure. In order to investigate the effect of the processing route on microstructural evolution during aging and creep, a range of advanced electron microscopy techniques have been used including ion beam induced secondary electron imaging and High Angle Annular Dark Field (HAADF) imaging in the Scanning Transmission Electron Microscope. These techniques have enabled the particle population characteristics of all the second phase particles (M 23 C 6 , Laves phase, BN and MX) to be quantified for materials from both forging processes. These quantitative data have enabled a better understanding of how the processing route affects the microstructural evolution of FB2 steels.

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.

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.

The necessity to reduce carbon dioxide emissions of new fossil plant, while increasing net efficiency has lead to the development of not only new steels for potential plant operation of 650°C, but also cast nickel alloys for potential plant operation of up to 700°C and maybe 750°C. This paper discusses the production of prototype MarBN steel castings for potential plant operation up to 650°C, and gamma prime strengthened nickel alloys for advanced super critical plant (A-USC) operation up to 750°C. MarBN steel is a modified 9% Cr steel with chemical concentration of Cobalt and tungsten higher than that of CB2 (GX-13CrMoCoVNbNB9) typically, 2% to 3 Co, 3%W, with controlled B and N additions. The paper will discuss the work undertaken on prototype MarBN steel castings produced in UK funded research projects, and summarise the results achieved. Additionally, within European projects a castable nickel based super alloy has successfully been developed. This innovative alloy is suitable for 700°C+ operation and offers a solution to many of the issues associated with casting precipitation hardened nickel alloys.

Advanced austenitic stainless steels, such as Super 304H, have been used in reheater and superheater tubes in supercritical and ultra-supercritical power plants for many years now. It is important to characterize the microstructure of ex-service reheater and superheater tubes as this will help researchers understand the long-term microstructural evolution and degradation of the material, which can impact the performance and lifetime of the components that are in service. In this research, the microstructure of an ex-service Super 304H reheater tube that has been in service for 99,000 hours at an approximate metal temperature of 873K (600°C) has been characterized. The characterization techniques used were electron microscopy-based and included imaging and chemical analysis techniques. Seven phases were observed as a result of the characterization work. The phases observed were MX carbonitrides rich in niobium, copper-rich particles, M 23 C 6 , sigma phase, Z phase, a cored phase, and a BCC phase.

Additive manufacturing (AM) is a process where, as the name suggests, material is added during production, in contrast to techniques such as machining, where material is removed. With metals, AM processes involve localised melting of a powder or wire in specific locations to produce a part, layer by layer. AM techniques have recently been applied to the repair of gas turbine blades. These components are often produced from nickel-based superalloys, a group of materials which possess excellent mechanical properties at high temperatures. However, although the microstructural and mechanical property evolution during the high temperature exposure of conventionally produced superalloy materials is reasonably well understood, the effects of prolonged high temperature exposure on AM material are less well known. This research is concerned with the microstructures of components produced using AM techniques and an examination of the effect of subsequent high temperature exposures. In particular, the paper will focus on the differences between cast and SLM IN939 as a function of heat treatment and subsequent ageing, including differences in grain structure and precipitate size, distribution and morphology, quantified using advanced electron microscopy techniques.

Up to now, the amount of supercritical boilers in China has ranked number one in the world. Many supercritical boilers have run for more than 100,000 hours. Creep becomes one of the main reasons for supercritical boiler tubes failure. In this article, the failure of superheater tubes in a supercritical boiler was analyzed, the microstructural evolution of austenitic stainless steel tubes were studied, a full investigation into the failure cause was carried out involving in visual examination, optical microscope, SEM, TEM and XRD. The results show, sigma phase precipitates in this austenitic steel with the extension of service time, sigma precipitates form at grain boundaries by continuous chain. Sigma precipitates are hard and brittle, weaken grain boundaries and cause microscopic damage, eventually lead to boiler tubes failure.

A novel salt-bath nitrocarburizing process recently developed forms a lithium-iron compound-oxide layer on the surface of steel in concurrence with a nitride layer by adding lithium ions to the molten salt. This process has already been successfully applied to mass-produced products. However, the microstructure and its formation process of the surface layer in alloyed steels during the nitrocarburizing process have not yet been fully understood. In this study, we focus on the effect of Si and Cr, which are included in a common die steel, on the microstructure of an oxide layer of a nitrocarburized alloy. The alloys used in this study are Fe-0.4wt%C, Fe-0.4wt%C-2.0wt%Si, and Fe-0.4wt%C-2.0wt%Cr. These alloys were arc melted into button ingots under an Ar atmosphere. The ingots were annealed at 1123 K for 1.0 h, followed by air cooling and double tempering at 873 K, similar to the heat treatments employed to hot-die steels. Salt-bath nitrocarburizing was carried out at 823 K for 0.1-10 h. The microstructures of the cross-sectional surface layers of the samples were examined using an optical microscope and FE-SEM. Elemental mapping as well as phase identification of the surface layers were done by EDS, XRD, and GD-OES. In the Fe-C binary alloy, a thin continuous oxide layer of α-LiFeθ 2 formed first on the outermost surface, and a thick iron nitride layer developed underneath the oxide layer, with aligned oxide particles along the grain boundaries of the nitrogen compound layer. In the case of Si addition, the outermost oxide layer became thinner and an additional oxide layer consisting of α-LiFeθ 2 and (Li,Fe) 3 Siθ 4 formed between the outer oxide layer and nitrogen compound layer, and the formation of the oxide particles in the nitrogen compound layer was fully suppressed. In the case of Cr addition, internal oxide particles formed in the nitrogen compound layer, similar to those in the binary steel, although an continuous oxide layer of CrfN,O) formed in between those layers. On the basis of these results, the inner oxide layer formed with Si addition contributes to improving the frictional wear characteristics in die steels.

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.

The inspection and evaluation of defects in the welds of P92 high temperature reheater header with a diameter of about 1000mm and a wall thickness of about 100 mm have been done by means of hardness test, nondestructive testing on the surface, ultrasonic testing, metallographic and component sampling. By analyzing the results of on-site test and samples removed from the component, it is found that cracks existing in the welds are hydrogen induced delayed cracks. During the welding process and post-heating treatment (hydrogen bake-out), dehydrogenation was insufficient. This fact, combined with welding residual stresses resulted in the observed hydrogen induced cracking.

A failure of the upper casing of the circulation pump led to a big damage in the PP Staudinger unit 5 on 12th of May 2014. According to the §18(2) BetrSichV an extensive root cause analysis (RCA) was started. From the beginning on different lines of activities were initiated to handle the situation with the required diligence. Decisions were made, taking into account safety regulations, possibility of repair and best practice engineering. Following the board decision to repair the unit 5, a lot of detailed work was done. All of the performed work packages were linked in different timelines and needed to meet in the key points. Consequently it was a challenge to achieve the agreed date of unit 5 restart on 15th of January 2015. The unit restart on the targeted date was a proof of the excellent collaboration between all involved parties. The presentation gives a summarizing overview about the damage, the main results of the RCA and the repair activities.

In order to assist in developing mechanistic and computational models for understanding the performance of current Fe-base waterwall tubing, characterization has been performed on three field-exposed low alloy steel waterwall tubes. The waterside oxide thickness was characterized using standard metallographic techniques. Alloy and oxide chemical composition was characterized using electron microprobe analysis. Waterside scale thickness was measured as a function of location. Agreement between the measured and predicted values based on likely rate constants was poor.

In order to establish a creep damage assessment method for 47Ni-23Cr-23Fe-7W (HR6W), which is a candidate material of A-USC, microstructure observation of creep interrupted specimens and ruptured specimen was conducted, and the creep damage process was examined. Creep tests were conducted under conditions of 800°C, 70 MPa, 700°C, and 100 MPa. For creep damage assessment, an optical microscope was used for replicas sampled from the outer surface of specimens, and crack ratio at grain boundaries was assessed. The results indicated that creep voids and cracks were initiated at grain boundaries from about 0.35 of creep life ratio, and crack ratio increased drastically after creep life ratio of 0.65. This crack ratio was almost the same regardless of the specimen shape Therefore, the method to assess crack ratio using replicas is considered to be an effective method for creep damage assessment of HR6W. An increase in the crack ratio due to an increase in creep life ratio showed the same trend as the change in elongation of creep interrupted specimens. Microstructure observations were conducted with interrupted specimens using SEM-ECCI (Electron Channeling Contrast Imaging) in order to clarify the cause of acceleration creep. The results showed that sub-boundary developed significantly near grain boundaries, which indicates that sub-boundary development may cause acceleration.

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.