Structural changes in P92-type steel after creep at temperature of 600°C under a stress of 140 MPa were investigated. The steel was solution treated at 1050°C and tempered at 780°C. The structure in the grip portion of the creep specimen changed scarcely after creep exposure for 6876 h. In contrast, the structural changes in the gage and neck sections were characterized by transformation of the tempered martensite lath structure into relatively coarse subgrain structure. The formation of a well-defined subgrain structure in the gage and neck sections was accompanied by the coarsening of M 23 C 6 carbides and precipitations of Laves phase during creep. Mechanisms of grain boundary pinning by precipitates are discussed.

In order to clarify the effect of stress state on microstructural changes during creep, the microstructure was observed in the central part of the cross section of the fine-grained heat-affected zone (FGHAZ) and in the surface region of the FGHAZ in Gr.92 steel welded joint. Creep tests were performed under constant load in air at 650°C, using cross-weld specimens. The creep strength of welded joint was lower than that of base metal. Type IV fracture occurred in the long-term. Creep voids were detected in the FGHAZ after the fracture. Number of creep voids was higher in the central part of the cross section of the FGHAZ than in the surface region of the FGHAZ. It was checked the multiaxiality of stress during creep was higher in the central part of the cross section of the FGHAZ than in the surface region of the FGHAZ. The recovery of dislocation structure occurred after creep in the base metal and the FGHAZ. Mean subgrain size increased with increasing time to rupture. However, there was no difference of change of subgrain size during creep in the central part of the cross section of the FGHAZ and in the surface region of the FGHAZ. The growth of M 23 C 6 carbide and MX carbonitrides was observed during creep in the base metal and the FGHAZ. Laves phase precipitation occurred during creep. There was no difference of the change of mean diameter of MX carbonitrides in the central part of the cross section of the FGHAZ and in the surface region of the FGHAZ after creep. However, the growth rate of M 23 C 6 carbide in the FGHAZ was much higher in the central part of the cross section than in the surface region.

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.

Laser additive manufacturing (AM) is being considered by the nuclear industry to manufacture net- shape components for advanced reactors and micro reactors. Part-to-part and vendor-to-vendor variations in part quality, microstructure, and mechanical properties are common for additively manufactured components, attributing to the different processing conditions. This work demonstrates the use of microstructurally graded specimen as a high throughput means to establish the relationship between process-microstructure-creep properties. Through graded specimen manufacturing, multiple microstructures, correlated to the processing conditions, can be produced in a single specimen. The effects of a solution annealing heat treatment on the microstructure and creep properties of AM 316H are investigated in this work. Using digital image correlation (DIC), the creep strain can be calculated in these graded regions, allowing for multiple microstructures to be probed in a single creep test. The solution annealing heat treatment was not sufficient in recrystallization of the large, elongated grains in the AM material; however, it was sufficient in removing the cellular structure commonly found in AM processed alloys creating a network of subgrains in their place. The resulting changes in microstructure and mechanical properties are presented. The heat treatment was found to generally increase the minimum creep rate, reduce the minimum creep rate, and reduce the ductility. Significant amounts of grain boundary carbides and cavitation were observed.

Microstructure in the gage sections of ruptured GX12CrMoWVNbN10-1-1 cast steel specimens was examined after creep tests under applied stresses ranging from 120 to 160 MPa at T=893 K. The microstructure after tempering consisted of laths with an average thickness of 332 nm. The tempered martensite lath structure was characterized by M 23 C 6 -type carbide particles with an average size of about 105 nm, and MX carbonitrides with an average size of about 45 nm. Precipitation of Laves phase occurred during creep test. The structural changes in the gauge section of the samples were characterized by the evolution of relatively large subgrains with remarkably lowered density of interior dislocations within former martensite laths. MX carbonitrides and M 23 C 6 -type carbide particles increase in size slightly under long-term creep. Microstructural degradation mechanisms during creep in GX12CrMoWVNbN10-1-1 cast steel are discussed.

9-10%Cr-3%Co martensitic steels are the prospective materials for elements of boilers, tubes and pipes for fossil power plants which are able to work at ultra-supercritical parameters of steam (T=620-650°C, P=25-30 MPa). The effect of creep on the microstructure of the 10 wt.%Cr-3Co- 3W-0.2Re martensitic steel was investigated in the condition of 650°C and an applied stress of 140 MPa, time to rupture was more than 8500 h. Previously, this steel was subjected to the normalizing at 1050°C and tempering at 770°C. This heat treatment provided the hierarchical tempered martensite lath structure with the mean size of prior austenite grains of 59 μm and with high dislocation density (2×10 14 m -2 ) within martensitic laths. Boundary M 23 C 6 and M 6 C carbides and randomly distributed within matrix Nb-rich MX carbonitrides were detected after final heat treatment. The addition of Re in the steel studied positively affected creep at 650°C/140 MPa and stabilized the tempered martensite lath structure formed during 770°C-tempering. The formation of the subgrains in the gage section was accompanied by the coarsening of M 23 C 6 carbides and precipitations of Laves phase with fine sizes during creep. No depletion of Re and Co from the solid solution during creep was revealed whereas W content decreased from 3 to 1 wt.% for first 500 h of creep. Reasons of improved creep as well as mechanisms of grain boundary pinning by precipitates are discussed.

Small punch creep testing (SPCT) is a small-scale, accelerated creep test that allows for the determination of creep data using a limited amount of material. The question, however, remains how the data generated by this technique correlate to more established techniques such as uniaxial testing and ultimately to predictions regarding the remaining service life of a plant component. This empirical study investigated the microstructure-to-property relationship of welded 9-12%Cr steels as measured using SPCT. Virgin P91 (X10CrMoVNb9-1) steel was joined to service exposed X20 (X20CrMoV12-1) steel using two different filler materials (X20 and P91) via fusion welding. Site-specific samples were extracted from the parent plates, heat affected zones and weld metals using electro-discharge machining. Small punch creep testing were performed using a 276 N load at a temperature of 625°C. The untested sample microstructures were quantitatively characterized using a range of electron microscopy techniques to determine the precipitate (M 23 C 6 , MX) spacing, subgrain sizes and dislocation densities for each region of the weldments. Multiple linear regression analysis found that the subgrain size (λsg) played the largest contribution to the SPCT rupture life. The heat affected zones had the lowest SPCT rupture times (49-68 hours), which corresponded to the largest subgrain sizes (1.1-1.3 μm). The P91 parent plate material had the longest SPCT rupture time (349 hours), which corresponded to the lowest subgrain size (0.8 μm). The P91 weld metal sample showed lower initial deflection rates during the SPC testing, however the presence of non-metallic SiO 2 inclusions in this zone contributed to accelerated brittle failure.

Microstructural analyses by FE-SEM and TEM were performed on a ferritic heat-resisting steel that contained 12mass% chromium and 2mass% tungsten to characterize its multi-scale structure, consisting of prior austenite grains, packets, blocks, subgrains and precipitates. The size distributions of the block, subgrains and precipitates were quantitatively evaluated before and after a creep-fatigue test to relate them to their creep-fatigue property. Our results showed that the occupancy of precipitates on prior austenite grain boundaries increased markedly and subgrains became coarse during the creep-fatigue test, while block size did not change. It is suggested that the growth of grain boundary precipitates and coarse subgrains plays an important role in the intergranular fracture mechanism caused by creep-fatigue.

In order to clarify the effect of stress and strain on microstructural changes during creep for T91 steel, creep interrupted tests were performed at 600°C for 10000h, 20000h, 30000h, 50000h and 70000h. The steel studied was T91 steel with high Ni content (0.28mass%) in the range of specification. Changes of dislocation structure and precipitates distributions were observed for the grip and gauge portions of creep interrupted samples. The subgrain size gradually increased with increasing creep time up to 50000h in both the grip and gauge portions. However, the subgrain size abruptly increased after 50000h in the gauge portion as compared with the grip portion. Decrease in dislocation density inside subgrain was promoted in the gauge portion as compared with the grip portion. The size of M 23 C 6 gradually increased with increasing creep time up to 50000h in both the grip and gauge portions. The increase in M 23 C 6 size was accelerated after 50000h in the gauge portion as compared with the grip portion. The Z phase formation was promoted in the gauge portion as compared with the grip portion. The number density of all kinds of particles gradually decreased with increasing creep time in the gauge and grip potions. After 50000h, the number density rapidly decreased in the gauge portion as compared with the grip portion.

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 improve thermal efficiency of fossil-fired power plants through increasing steam temperature and pressure high strength martensitic 9-12%Cr steels have extensively been used, and some power plants have experienced creep failure in high temperature welds after several years operations. The creep failure and degradation in welds of longitudinally seam-welded Cr- Mo steel pipes and Cr-Mo steel tubes of dissimilar metal welded joint after long-term service are also well known. The creep degradation in welds initiates as creep cavity formation under the multi-axial stress conditions. For the safety use of high temperature welds in power plant components, the complete understanding of the creep degradation and establishment of creep life assessment for the welds is essential. In this paper creep degradation and initiation mechanism in welds of Cr-Mo steels and high strength martensitic 9-12%Cr steels are reviewed and compared. And also since the non-destructive creep life assessment techniques for the Type IV creep degradation and failure in high strength martensitic 9-12%Cr steel welds are not yet practically established and applied, a candidate way based on the hardness creep life model developed by the authors would be demonstrated as well as the investigation results on the creep cavity formation behavior in the welds. Additionally from the aspect of safety issues on welds design an experimental approach to consider the weld joint influence factors (WJIF) would also be presented based on the creep rupture data of the large size cross-weld specimens and component welds.

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.

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.

Conventional time-temperature-parameter (TTP) methods often overestimate long-term creep rupture life of creep strength enhanced high Cr ferritic steels. The cause of the overestimation is studied on the basis of creep rupture data analysis on Gr.91, 92 and 122 steels. There are four regions with different values of stress exponent n for creep rupture life commonly in stress-rupture data of the three ferritic steels. Activation energies Q for rupture life in the regions take at least three different values. The values of n and Q decrease in a longer-term region. The decrease in Q value is the cause of the overestimation of long-term rupture life predicted by the conventional TTP methods neglecting the change in Q value. Therefore, before applying a TTP method creep rupture data should be divided into several data sets so that Q value is unique in each divided data set. When this multi-region analysis is adopted, all the data points of the steels can be described accurately, and their long-term creep life can be evaluated correctly. Substantial heat-to-heat and grade-to-grade variation in their creep strength is suggested under recent service conditions of USC power boilers.

9-12%Cr martensitic steels can be applied to the next highest temperature components such as boiler tracts, steam pipelines and turbines of advanced ultra-supercritical power plants with steam temperatures of 650°C. New 10%Cr martensitic steels with high B and low N contents can be a worthy candidate for use in production because it has superior creep resistance. At the same time, resistance to cyclic and dynamic loads is very important. In this work, we studied the low cycle fatigue (LCF) properties at room and elevated (500-650°C) temperatures and Charpy impact toughness at temperatures ranging from -196…100°C of advanced 10% Cr martensitic steel with high B and low N contents. The effect of new alloying scheme and corresponding peculiarities of M 23 C 6 carbides on the low cycle fatigue resistance and impact toughness of the 10%Cr martensitic steel is analyzed. It is revealed that fine and densely distributed carbides has no effect on the fatigue resistance except for the slight improvement of fatigue life at small strain amplitudes and shift the ductile-brittle transition temperature (DBTT) to higher but satisfactory value of +10°C as compared to other high-chromium martensitic steels.

Large heat-to-heat variation of creep rupture strength in weldments of mod.9Cr-1Mo steels was observed in the creep rupture tests conducted for two different heats at 600°C and 650°C. One heat showed consistently lower time-to-rupture than the other for 130-60MPa at 600°C. Detailed microstructural investigations revealed that the number density of precipitates in the weaker heat was remarkably lower than that associated with the stronger heat through most of the creep region. Accordingly, heat-to-heat variation of creep rupture strength was attributed to the difference in the precipitate strengthening effects throughout creep. Equilibrium calculation predicted that the smaller phase fraction of M 23 C 6 and VN precipitates due to the lower content of chromium and lower ratio of nitrogen/aluminum in the weaker heat. However, given that long-term creep rupture strength at 650°C converged for the two heats, the microstructure including precipitates may settle into a similar level for subsequent longer hours even at 600°C.

This work deals with the potential of microstructurally based modeling of the creep deformation of martensitic steels. The motivation for the work stems from the ever increasing demand for higher efficiency and better reliability of modern thermal power plants. Service temperatures of 600°C and stress levels up to 100 MPa are currently the typical requirements on critical components. High creep and oxidation resistance are the main challenges for a lifetime 10+ years in steam atmosphere. New materials may fulfill these requirements; however, the save prediction of the creep resistance is a difficult challenge. The model presented in this work takes into consideration the initial microstructure of the material, its evolution during thermal and mechanical exposure and the link between microstructural evolution and creep deformation rate. The model includes the interaction between the relevant microstructural constituents such as precipitates, grain- lath- and subgrain boundaries and dislocations. In addition, the material damage is included into the model. The applicability of the model is then demonstrated on standard creep resistant alloys. Contrary to phenomenological models, this approach can be tested against microstructural data of creep loaded samples and thus provides higher reliability. Nevertheless, potential improvements are discussed and future developments are outlined.

The size and distribution of the Laves phase particles in a 9.85Cr-3Co-3W-0.13Mo-0.17Re- 0.03Ni-0.23V-0.07Nb-0.1C-0.002N-0.008B steel subjected to creep rupture test at 650°C under an applied stresses of 160-200 MPa with a step of 20 MPa were studied. After heat treatment consisting of normalizing of 1050°C and tempering of 770°C, M 23 C 6 and Fe 3 W 3 C carbides with the mean sizes of 67±7 and 40±5 nm, respectively, were revealed along the boundaries of prior austenite grains and martensitic laths whereas round NbX carbonitrides were found within martensitic laths. During creep metastable Fe 3 W 3 C carbides dissolved and the stable Laves phase particles precipitated; volume fraction of Laves phase increases with time. The Laves phase particles nucleated on the interfacial boundaries Fe 3 W 3 C/ferrite during first 100 h of creep and provided effective stabilization of tempered martensitic lath structure until their mean size less than 150 nm.

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.

A trial weld joint of COST F and COST FB2 steels was produced using the GTAW HOT-WIRE method in conditions used in industry for production of welding steam turbine rotors. Conventional long-term creep tests (CCT) to the rupture of this weldment and the base materials were carried out at temperatures ranging from 550 °C to 650 °C in the stress range from 70 to 220 MPa (the longest time to rupture was above 52,000 hours). Creep rupture strength was evaluated using Larson-Miller parameter model. Assessment of microstructure was correlated with the creep strength. Precipitation of Laves phase and structure recovery during creep exposures were the main reasons for the failure which occurred in the heat affected zone of steel COST F. The recently developed simulative accelerated creep testing (ACT) on thermal-mechanical simulator allows the microstructural transformation of creep-resisting materials in a relatively short time to a state resembling that of multiyear application under creep conditions. ACT of samples machined from various positions in the weldment was performed at 600 °C under 100 MPa. Changes in the hardness and the microstructures of the samples, which underwent both types of creep tests, were compared. Small sample creep test (SPCT), another alternative method how to obtain information about the creep properties of materials when only a limited amount of test material is at disposal, were performed. It was shown that the same stress-temperature dependence and relationships are valid in the SPCT as in the CCT. Using a simple load-based conversion factor between the SPCT test and the CCT test with the same time to rupture, the results of both test types can be unified.