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The Institute for Materials Science, Welding and Forming (IWS) conducts extensive research on modern martensitic 9-12% Cr steels intended for use in environmentally friendly power plants. Their comprehensive research program encompasses mechanical testing of base and weld metals, analysis of creep and damage mechanisms, weldability studies, microstructural evolution during creep, mathematical modeling of precipitation and coarsening kinetics, and simulation of complex heat treatments and creep deformation behavior. Through these interconnected projects, which are briefly described, IWS develops a thorough understanding of these materials while working toward a quantitative model of their creep behavior.

The morphology of γ/γ' microstructures in single crystal superalloys is known to evolve during service conditions according to established materials science principles, potentially offering a novel approach for failure analysis. This study investigated the morphological changes in γ/γ' microstructures of CMSX-4, a single crystal Ni-base superalloy, under various loading conditions. The experimental parameters included tensile and compressive stress levels, loading temperature, loading rate, monotonic versus cyclic loading, and multi-axial stress states. Results demonstrated that the γ/γ' microstructures exhibited highly sensitive responses to these loading conditions. A newly developed quantitative image analysis method was used to characterize these morphological changes, and the findings were compiled into a two-dimensional map to facilitate failure analysis and other engineering applications.

The highest creep rupture strength of recent 9-12% Cr steels which have seen practical application is about 130 MPa at 600°C and 100,000 h. While the 630°C goal may be realized, much more work is needed to achieve steam temperatures up to 650°C. Conventional alloy development techniques can be slow and it is possible that mathematical models can define the most economical path forward, perhaps leading to novel ideas. A combination of mechanical property models based on neural networks, and phase stability calculations relying on thermodynamics, has been used to propose new alloys, and the predictions from this work were published some time ago. In the present work we present results showing how the proposed alloys have performed in practice, considering long term creep data and microstructural observations. Comparisons are also made with existing enhanced ferritic steels such as Grade 92 and other advanced 9-12%Cr steels recently reported.

The fall-off of oxide scale with poor adhesion inside superheater/reheater tubes in boilers for (ultra) supercritical power unit is the main cause of accidents such as superheater/reheater blockage, tube explosion and solid particle erosion in the steam turbine which cause serious economic losses. However, there is still no method for testing and assessing the adhesion of oxide scale inside the tube. A method for testing the adhesion of corrosion products in tubes by spiral lines is proposed in this paper, and the accuracy of adhesion evaluation is improved by adopting the image recognition method.

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.

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.

Grade 91 creep strength-enhanced ferritic steel is a critical material in power generation, widely used for high-temperature, high-pressure tubing and piping applications. Its superior elevated-temperature strength derives from a distinctive microstructure of tempered martensite with uniformly dispersed secondary phases (carbides and carbo-nitrides). This microstructure, crucial for reliable service performance, is achieved through precise control of the manufacturing process, including steelmaking, hot forming, and final heat treatment. This investigation builds upon earlier research into the relationship between manufacturing parameters and short-term creep-rupture properties in T91 tubes, and a recent update that included test results exceeding 30,000 hours. This study presents a comprehensive metallurgical analysis of ruptured test specimens. The investigation focuses on correlating manufacturing parameters with not only creep strength but also material ductility and microstructural evolution during long-term exposure, providing valuable insights into the material’s behavior under extended service conditions.

The creep degradation/life assessment for high temperature critical component materials is absolutely needed to assure the long-term service operation and there is little experience with the service exposure of the high temperature components made of newly developed Ni-based alloys. In this study, therefore, the creep degradation assessment study on the Ni-based alloys, Alloy 617 and HR6W was conducted based on the hardness method, because the hardness measurement is a useful and simple technique for the materials characterization for any kind of high temperature-serviced steels and alloys. As the result, it was found that the hardness was increased by not only precipitation due to thermal aging but also creep stress/strain, and there existed linear relationship between the applied stress and creep-induced hardness increase. Also the hardness scatter measured was increased along with the progress of creep hardening and damage progressing in terms of creep life consumed. Those findings suggested that the creep life assessment of Ni-based alloys would be possible by means of hardness measurement. The paper also deals with the role and perspective development of non destructive damage detecting techniques, and life assessment issues on Ni-based alloys for A-USC power applications.

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.

This study aims to elucidate the chemical compositions and microstructural factors that affect longterm creep rupture strength and creep rupture ductility using multiple heats of Gr.92 steel. Evaluating the reduction behavior in long-term creep rupture strength, we propose a relative creep rupture strength value, which is expressed as the logarithmic ratio of the estimated creep strength for each rupture time exceeding 10,000 hours, with 10,000 hours as the reference. Higher initial hardness correlates with greater pronounced strength reduction in the long-term regime. While smaller prior austenite grain sizes lead to greater reductions in creep rupture strength, this effect diminishes above 30 μm. However, no clear correlation was observed between Cr content and creep strength reduction in this study. Brittle creep ruptures with smooth test specimens were observed just below the extensometer ridge in the parallel section of test specimen, indicating notch weakening. Even in heats with excellent creep ductility, the amount of inclusions tended to be higher than in heats with lower creep ductility. Factors other than inclusions also seem to influence long-term creep ductility.

In thermal power plants, weldments of all currently used martensitic 9% chromium steels are prone to Type IV cracking in the fine-grained region of the heat-affected zone (HAZ). Japanese researchers have introduced a new martensitic steel for ultra-supercritical (USC) steam conditions that demonstrates resistance to Type IV cracking. This study compares a modified version of this boron-nitrogen balanced advanced 9Cr-3W-3Co steel with CB2, the most promising 9% Cr steel developed through the European research initiative COST, in terms of weldability. The HAZ was analyzed using the "Heat-Affected Zone Simulation" technique with a Gleeble 1500 thermo-mechanical simulator. Basic optical microscopy was complemented by advanced electron microscopy techniques, including energy-filtered TEM (EFTEM), electron energy loss spectroscopy (EELS), electron backscatter diffraction (EBSD), and energy-dispersive X-ray analysis (EDX). Phase transformations in the HAZ were directly observed using in situ X-ray diffraction with synchrotron radiation at the Advanced Photon Source (APS) of Argonne National Laboratory, IL, USA. Although both steels exhibited similar transformation behavior, their resulting microstructures after the weld thermal cycle differed significantly. At peak temperatures above 1200°C, delta ferrite formed and remained stable down to room temperature due to rapid cooling in both steels. While CB2 exhibited conventional coarse-grained (CG), fine-grained (FG), and intercritical HAZ regions, the boron-nitrogen balanced 9Cr steel did not develop a fine-grained HAZ. Since Type IV cracking primarily occurs in the FGHAZ, this alloy shows strong potential for eliminating Type IV cracking as a major life-limiting factor in heat-resistant steel weldments.

The mechanical behavior of a cast form of an advanced austenitic stainless steel, CF8C-Plus, is compared with that of its wrought equivalent in terms of both tensile and creep-rupture properties and estimated allowable stress values for pressurized service at temperatures up to about 850°C. A traditional Larson-Miller parametric model is used to analyze the creep-rupture data and to predict long-term lifetimes for comparison of the two alloy types. The cast CF8C-Plus exhibited lower yield and tensile strengths, but higher creep strength compared to its wrought counterpart. Two welding methods, shielded-metal-arc welding (SMAW) and gas-metal-arc welding, met the weld qualification acceptance criteria in ASME BPVC Section IX for the cast CF8C-Plus. However, for the wrought CF8C-Plus, while SMAW and gas-tungsten-arc welding passed the tensile acceptance criteria, they failed the side bend tests due to lack of fusion or weld metal discontinuities.

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.

This study investigates the steam oxidation behavior of Alloy 699 XA, a material containing 30 wt.% chromium and 2 wt.% aluminum that forms protective oxide scales in low-oxygen conditions. The research compares four variants of the alloy: conventional bulk material, a laser powder bed fusion (LPBF) additively manufactured version, and two modified compositions. The modified versions include MAC-UN-699-G, optimized for gamma-prime precipitation, and MAC-ISIN-699, which underwent in-situ internal nitridation during powder atomization. All variants were subjected to steam oxidation testing at 750°C and 950°C for up to 5000 hours, with interim analyses conducted at 2000 hours. The post-exposure analysis employed X-ray diffraction (XRD) to identify phase development and scanning electron microscopy with energy dispersive spectroscopy (SEM/EDS) to examine surface morphology, cross-sectional microstructure, and chemical composition. This study addresses a significant knowledge gap regarding the steam oxidation behavior of 699 XA alloy, particularly in its additively manufactured state.

Creep-fatigue crack formation (endurance) and crack growth rate data are necessary inputs for assessing the structural integrity and for estimating the design life of high temperature components in power generation and aircraft engine industries. Ensuring consistency in the reported test data, as well as an understanding of the inherent scatter and its source in the data, are both necessary for assuring quality and limitations of the analyses that rely on the data. In 2008, the American Society for Testing and Materials (ASTM) under the umbrella of its subcommittees E08.05 on Cyclic Deformation and Crack Formation and E08.06 on Crack Growth, and the sponsorship of Electric Power Research Institute (EPRI) through its international experts’ working group on creep-fatigue embarked on the task of developing separate standard test methods for creep-fatigue crack formation and creep-fatigue crack growth. The first standard entitled, “E-2714-09: Standard Test Method for Creep-fatigue Testing” was developed in 2009 and was followed up with a round-robin consisting of 13 laboratories around the world for testing the newly developed standard. This paper discusses the results of this round-robin concluded in 2012 using the widely used P91 steel that led to the formulation of the Precision and Bias statement contained in the version of the ASTM standard E2714 that was successfully balloted in the year 2013.

The creep resistance of 9-12% Cr steels is significantly influenced by the presence and stability of different precipitate populations. Numerous secondary phases grow, coarsen and, sometimes, dissolve again during heat treatment and service. Based on the software package MatCalc, the evolution of these precipitates during the thermal treatment of the COST 522 steel CB8 is simulated from the cooling process after cast solidification to heat treatment and service up to the aspired service life time of 100.000h. On basis of the results obtained from these simulations in combination with a newly implemented model for evaluation of the maximum threshold stress by particle strengthening, the strengthening effect of each individual precipitate phase, as well as the combined effect of all phases is evaluated - a quantification of the influence of Z-Phase formation on the long-term creep behaviour is thus made possible. This opens a wide field of application for alloy development and leads to a better understanding of the evolution of microstructural components as well as the mechanical properties of these complex alloys.

The measurement of damage from high temperature solid particle erosion (HTSPE) can be a lengthy process within the laboratory with many lab-based systems requiring sequential heat and cooling of the test piece to enable mass and/or scar volume measurements to be made ex situ. Over the last few years a new lab-based system has been in development at the National Physical Laboratory which has the ability to measure the mass and volume change of eroded samples in situ without the need to cool the sample. Results have previously been shown demonstrating the in situ mass measurement, more recently the in situ volume measurement capability has been added and used to evaluate the erosion performance of additively manufactured materials. Selective laser melting (SLM) is an advanced manufacturing method which is growing in popularity and application. It offers the ability to manufacture low volume complex parts and has been used in rapid prototyping. As the technique has developed there is increasing interest to take advantage of the ability to manufacture complex parts in one piece, which in some case can be more cost and time effective than traditional manufacturing routes. For all the benefits of SLM there are some constraints on the process, these include porosity and defects in the materials such as ‘kissing bonds’, surface roughness, trapped powder and microstructural variation. These features of the processing route may have implications for component performance such as strength, fatigue resistance wear and erosion. To investigate this further SLM IN718 has been used to evaluate factors such as surface roughness, microstructure and morphology on the erosion performance as measured in situ and compared with conventional produced wrought IN718 material.