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

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

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

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

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

Modified 9Cr-1Mo alloy steel has been developed over the last few decades and has since gained wide acceptance in the boiler industry for the production of a variety of pressure-critical components, including tubing, piping and headers. The properties of creep-strength enhanced ferritic steels such as grade 91 are critically dependent on manufacturing parameters such as steelmaking, hot deformation, heat treatment and welding. Since the applications for which this material is used impose strict requirements in terms of resistance, corrosion, and creep behavior, poor process control can severely compromise the service behavior. This work discusses the impact of total deformation during the rolling process, and heat treatment parameters on time-independent and time-dependent properties for grade 91. For this study, two heats with similar chemical composition were produced with different reduction ratios: to which, several normalizing and tempering combinations were applied. For each combination, the microstructure was characterized, including evaluation of segregation by metallographic examination, and analysis of secondary phase precipitates by means of X-ray powder diffraction. Mechanical testing and creep testing were performed. A comparison of results is presented, and recommendations on the optimal process parameters are provided to ensure reliable performance of grade 91 material.

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

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.

In order to understand the microstructural evolution during service that 9Cr steels experience it is important to be able to quantify key microstructural parameters that define the characteristics of the secondary phases (e.g. precipitated phases and inclusions) and the steel matrix. The average size of M 23 C 6 , Laves phase and MX particles in these materials have been reported in many studies, however comparability between these studies is compromised by variations in technique and different/incomplete reporting of procedure. This paper provides guidelines on what is required to accurately measure these parameters in a reproducible way, taking into account macro-scale chemical heterogeneities and the statistical number of particles required to make meaningful measurements. Although international standards do exist for inclusion analysis, these standards were not developed to measure the number per unit area of hard particles that can act as creep cavity nucleation sites. In this work a standardized approach for measuring inclusions from this perspective is proposed. In addition the associated need to understand the segregation characteristics of the material are described, which in addition to defining the area that needs to be analysed to measure the average number of inclusions per unit area, also allows the maximum number of inclusions per unit area to be determined, a parameter which is more likely to define the damage tolerance of the material.

High Cr ferritic steels have been developed for the large components of fossil power plants due to their excellent creep resistance, low thermal expansion, and good oxidation resistance. Development works to improve the operating temperature of these steels mainly focused on the high mechanical properties such as solid solution strengthening and precipitation hardening. However, the knowledge of the correlation between Laves phase precipitation and oxidation behavior has not clarified yet on 9Cr ferritic steels. This research will be focused on the effect of precipitation of Laves phase on steam oxidation behavior of Fe-9Cr alloy at 923 K. Niobium was chosen as the third element to the Fe- 9Cr binary system. Steam oxidation test of Fe-9Cr (mass%) alloy and Fe-9Cr-2Nb (mass%) alloy were carried out at 923 K in Ar-15%H 2 O mixture for up to 172.8 ks. X-ray diffraction confirms the oxide mainly consist of wüstite on the Fe-9Cr in the initial stage while on Nb added samples magnetite was dominated. The results show that the Fe-9Cr- 2Nb alloy has a slower oxidation rate than the Fe-9Cr alloy after oxidized for 172.8 ks

Effects of alloying additions of Ti or Mo to a simplified chemical composition of the γ′′-Ni 3 Nb strengthened type Ni-based alloy 718 on the precipitation mode of δ-Ni 3 Nb phase were investigated to aim at designing grain boundaries using the δ phase for raising temperature capability of the γ′′ strengthened Ni-based wrought alloys. In the base alloy of Ni-22Cr-16Fe-3.5Nb, the δ phase precipitated at the grain boundaries of the matrix phase in a platelet form by continuous precipitation mode at temperatures above 1273K (1000°C) but in a lamellar morphology by discontinuous precipitation mode below that temperature. The boundary temperature where the continuous/discontinuous precipitation mode changes was raised by addition of 1 % Ti and lowered by addition of 5% Mo. The increase in the boundary temperature by Ti addition can be considered to have occurred by an increase in the solvus temperature of γ′′ phase. The decrease in the boundary temperature by Mo addition can be interpreted by the reduction of the strain energy caused by the coherent γ′′ precipitates and/or the volume change by the formation of δ phase from the γ/γ′′ phases, which may promote the continuous precipitation with respect to the discontinuous precipitation.

The behavior of strain-induced abnormal grain growth (AGG) in superalloy 718 has been investigated using compression testing and subsequent heat treatment below the d-phase solvus temperature of 980 °C. The nuclei of AGG grains were slightly newly recrystallized grains by a nucleation because small grains without dislocation was observed in the as- deformed microstructure. AGG was caused by the difference in intragranular misorientation (related to the stored strain energy in a grain) between dynamic recrystallized grains and deformed matrix. The initiation of AGG was retarded with decreasing plastic strain and produced microstructures consisted of larger grains having more complex morphology. It was observed that grain boundary migrated locally in the direction perpendicular to, or mainly in the direction parallel to the S3 {111} twin boundaries along with the formation of high-order twins. As a result of multiple twinning, AGG grains seemed to evolve with the growing directions changed.

Directional coarsening of the γ' phase (rafting) in Ni-based single crystal superalloys during creep at 1273 K was simulated by the phase-field method. The inelastic strain introduced in the γ phase was assumed to be composed of plastic strain (ε p ) and creep strain (ε c ). The simulations were performed with various sets of values of material parameters and the magnitude of external tensile stress. We let a feed-forward neural network learn the simulation data in order to enable fast and exhaustive prediction of the time to rafting, t raft . From the analysis based on the trained neural network, it has been shown that t raft becomes longer with increasing magnitude of γ/γ' lattice misfit, with decreasing creep coefficient, and with increasing yield stress of the γ phase (σγ ys ). The sensitivity of t raft to σ γ ys is high when the ratio of ε p to the total inelastic strain (ε p + ε c ) is high.

The relationship between the hot workability and the precipitation morphology of γ′ phase in the Alloy U520 was examined with a focus on the presence of γ′-nodule. To change the morphology of γ’ phase, forged bars of the Alloy U520 were solution treated followed by cooling process with the cooling rates of 5~100 K/h. After the heat treatment, both γ’ phases of intragranular particle and nodule along grain boundaries were observed, and the both sizes increased by slowing down the cooling rate. That is, the area fraction of γ’-nodule increased from about 0.1 % in the sample cooled at 100 K/h to about 70 % at 5 K/h. In Gleeble tension test, the slow-cooled samples basically exhibited higher ductility than water-quenched samples below the γ′-solvus temperature. However, the ductility was maximized in the sample cooled at 20 K/h, and excessive decrease of cooling rate resulted in a drop in ductility. EBSD analysis revealed that dynamic recrystallization (DRX) was often occurred in grain interior but suppressed at γ′-nodule area, indicating that presence of γ′-nodule had a negative influence on hot workability at subsolvus temperature.

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.

Alloy 718 is one of the most useful heat-resistant alloys for important device components that require high-temperature properties. In order to obtain excellent mechanical properties, it is necessary to form fine grains, for which the pinning effect of the δ phase can be used in some cases. To precipitate a sufficient amount for the pinning effect, time-consuming isothermal heat treatments are required. Thus, a metallurgical method with a shortened holding time would improve production efficiency considerably. Our goal is to optimize the forging process to control grain size by utilizing the δ phase, and the purpose of this study was to investigate the influence of the initial microstructure of the precipitated γ″ phase on δ-phase precipitation behavior in Alloy 718. As a solute treatment, Alloy 718 was heated at 1050 °C for 4 h, followed by heating of some samples at 870 °C for 10 h to precipitate the γ″ phase. The specimen with precipitated γ″ phase showed more precipitated δ phase than that under the solute condition by comparing results of heating at 915 °C. This suggested that utilizing the γ″ phase promoted δ-phase precipitation, and it is thus expected to shorten the heat treatment time for δ-phase precipitation.

The cast microstructure of 1st generation MoSiBTiC alloy composed of Mo solid solution (Mo ss ), Mo 5 SiB 2 , TiC phases largely affects tensile-creep behavior in the ultrahigh temperature region. Mo 5 SiB 2 phase crystallized during solidification is plate-like with a size of several tens of microns. The plate surface is parallel to the (001) basal plane, and the <100] directions preferentially grow along the cooling direction, and thereby Mo 5 SiB 2 has a strong texture while Moss and TiC show randomly-oriented distribution in a cast ingot. During creep, Mo 5 SiB 2 plates are largely rotated and Moss works as sticky ligament in the small-plate-reinforced metal-matrix composites. This may be the reason why the MoSiBTiC alloy exhibits large creep elongation and excellent creep resistance. In other words, the evolution of microstructures infers that the consummation of Mo 5 SiB 2 plate rotation may lead to the initiation of creep rapture process. Therefore, the unique microstructure formed during solidification provides the feature of good mechanical properties for the 1st generation MoSiBTiC alloy.

Understanding of the thermomechanical processing that affects microstructures is important to develop new alloys, because the mechanical properties of Ti alloys depend on the microstructures. In our previous study, we found Sn deteriorated the oxidation resistance, while Nb improved the oxidation resistance. Then, we have focused on Ti-Al-Nb-Zr alloys which Nb was added instead of Sn. Zr was added for solid solution strengthening. In this study, the formation of microstructures by thermomechanical processing and the effect of microstructure on the mechanical properties were investigated using the Ti-13Al-2Nb-2Zr (at%) alloy. The samples heat-treated in the β+α phase followed by furnace cooling after processed in the β+α phase formed the equiaxed or the ellipsoid α phase surrounded by the β phase. On the other hand, the sample heat-treated in the β+α phase followed by furnace cooling after processed in the β phase formed the lamellar microstructure. The compression strengths of the equiaxed α structure processed at two temperatures in the β+α phase were almost the same. While creep life of the bi-modal structure was drastically changed by processing temperature.

High-temperature shape memory alloys (HTSMAs) are expected to be utilized for actuators in high temperature environments such as thermal power plants and jet engines. NIMS has designed TiPd shape memory alloys because high martensitic phase transformation temperature of TiPd around 570 ° C is expected to be high-temperature shape memory alloys. However, the strength of the austenite phase of TiPd is low and the perfect recovery was not obtained. Then, strengthening of TiPd by addition of alloying elements has been attempted, but the complete recovery was not obtained. Therefore, high entropy alloys (HEA, multi-component equiatomic or near equiatomic alloys) were attempted for HTSMA. The severe lattice distortion and the sluggish diffusion in HEA are expected to contribute strong solid-solution hardening of HTSMA. In this study, multicomponent alloys composed of Ti-Pd-Pt-Ni-Zr were prepared and the phase transformation, shape memory properties, and mechanical properties were investigated.

MoSiBTiC alloy is a promising material for advanced aerospace applications and next generation high pressure turbine blades in jet engines and gas turbines. It mainly consists of Mo solid solution, TiC and Mo 5 SiB 2 phases and has creep strength much stronger than Ni-base superalloys and better than SiC/SiC ceramic matrix composites. Furthermore, the fracture toughness of the alloy is much better (>15 MPa(m) 1/2 ) than Mo-Si-B ternary alloys (<10 MPa(m) 1/2 ) even if the volume fraction of Mo solid solution is less than 50 %. The improvement of fracture toughness would be caused not only by the continuity of Mo solid solution in solidification microstructure but also by TiC phase affecting as a fracture-resistant phase. In order to understand the microstructure evolution during solidification and the effect of TiC phase on the fracture toughness of the MoSiBTiC alloy, Mo-Ti-C ternary model alloys are dealt with in this study. Then, (1) liquidus surface projection and (2) isothermal section and the elastic moduli of TiC phase in equilibrium with Mo solid solution were focused on. The obtained liquidus surface projection suggests that the ternary transition peritectic reaction (L+ Mo 2 C->Mo+TiC) takes place in Mo-rich region. At 1800 °C, TiC phase in equilibrium with Mo phase contains at least 20.2 at% Mo and the Mo/TiC/Mo 2 C three phase region should exist around Mo-15Ti-10C.