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.

Metallographic tests, micro-hardness tests, mechanics performance tests and Energy Dispersion Spectrum (EDS) were conducted for a 2.25Cr-1Mo main steam pipe weldment served for more than 32 years. Microstructural evolution of the 2.25Cr-1Mo base metal and weld metal was investigated. Degradation in micro-hardness and tensile properties were also studied. In addition, the tensile properties of subzones in the ex-service weldment were characterized by using miniature specimens. The results show that obvious microstructural changes including carbide coarsening, increasing inter lamella spacing and grain boundary precipitates occurred after long-term service. Degradation in micro-hardness is not obvious. However, the effects of long term service on tensile deformation behavior, ultimate tensile strength and yield stress are remarkable. Based on the yield stress of micro-specimens, the order of different subzones is: WM>HAZ>BM, which is consistent with the order of different subzones based on micro-hardness. However, the ultimate tensile strength and fracture strain of HAZ are lower than BM.

The goal of improving the efficiency of pulverized coal power plants has been pursued for decades. The need for greater efficiency and reduced environmental impact is pushing utilities to ultra supercritical conditions (USC), i.e. steam conditions of 760°C and 35 MPa. The long-term creep strength and environmental resistance requirements imposed by these conditions are clearly beyond the capacity of the currently used ferritic steels and other related alloys. Consequently, new materials based on austenitic stainless steels and nickel-base superalloys are being evaluated as candidate materials for these applications. In the present work, the nickel-base superalloys CCA617, Haynes 230 and Inconel 740, and an austenitic stainless steel Super З04H, were evaluated. The materials were aged for different lengths of time at temperatures relevant to USC applications and the corresponding microstructural changes were characterized by x-ray diffraction, optical, scanning and transmission electron microscopy, with particular attention being given to the structure, morphology and compositions of phases (including γ, γ’, carbides, ordered phases, etc.) and the nature, density and distribution of dislocations and other defects. The results are presented and discussed in light of accompanying changes in microhardness.

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.

The harsh operating conditions of Advanced Ultra-Supercritical (A-USC) power plants, i.e., steam operation conditions up to 760°C (1400°F)/35 MPa (5000 psi), require the use of Ni-based alloys with high temperature performance. Currently, the U.S. Department of Energy Fossil Energy program together with Electric Power Research Institute (EPRI) and Energy Industries of Ohio (EIO) is pursuing a Component Test (Comets) project to address material- and manufacturing-related issues for A-USC applications. Oak Ridge National Laboratory (ORNL) is supporting this project in the areas of mechanical and microstructure characterization, weld evaluation, environmental effect studies, etc. In this work, we present results from these activities on two promising Ni-based alloys and their weldments for A-USC applications, i.e., Haynes 282 and Inconel 740H. Detailed results include microhardness, tensile, air and environmental creep, low cycle fatigue, creep-fatigue, environmental high cycle fatigue, and supporting microstructural characterization.

The presented work summarizes the results of more than 10 years of research at TU Graz and TU Chemnitz and partners on a martensitic boron and nitrogen stabilized 9Cr3W3Co (MARBN) steel grade. The design philosophy of MARBN steels is presented and critical issues regarding boron and nitrogen balance are discussed. Microstructural characterization of two different laboratory heats, is presented and efforts in European projects towards an upscaling of melts are presented. Base material creep testing data at 650 °C up to 50.000 hours is presented and assessed to commercial alloys such as ASTM grades P91 and P92. An increase of creep rupture stress of more than +20% was recorded. Oxidation tests in steam at 650°C revealed an anomalous response of the material. Several specimens exhibited excellent oxidation resistance commonly only seen for grades of higher chromium content. The anomalous oxidation behaviour is identified and discussed, although the causes remain yet unclear. Results of manufacturing, characterization and testing of different MARBN welds, including gas-tungsten-arc-, gas-metal-arc-, friction stir and electron beam welds reveal a microstructure memory effect in the heat affected zone, so that no uniform fine-grained zone is present. The behaviour of crosswelds during long-term creep testing at 650 °C up to more than 32.000 hours is assessed and the susceptibility to Type IV cracking is discussed. The manuscript summarizes research of more than 10 years, presents current research activities on MARBN and describes open questions for an alloy identified as a promising martensitic steel grade for elevated temperature components.

The Institute of Materials Science, Welding and Forming (IWS) conducts research activities on ferritic/martensitic 9-12% Cr steels through an interconnected network of projects. These projects focus on mechanical properties of base and weld metals, microstructural characterization of creep and damage kinetics, weldability, microstructure analysis during creep, modeling of precipitation and coarsening kinetics, and deformation behavior under creep loading. The individual projects are briefly described, outlining the conceptual approach towards quantitatively describing the creep behavior of 9-12% Cr steels. The research efforts aim to comprehensively understand and model the creep performance of these advanced steel grades by investigating their microstructural evolution, damage mechanisms, precipitation kinetics, and deformation characteristics under creep conditions. The integrated projects examine both base metals and welded joints, providing insights into material properties, weldability, and microstructure-property relationships critical for their application in high-temperature components.

The US Advanced Ultra-Supercritical (A-USC) Consortium conducted an extensive program to evaluate available superalloys for use in rotors for steam turbines operating at a nominal temperature of 760 °C (1400 °F). Alloys such as 282, Waspaloy, 740H, 720Li, and 105 were tested in the form of bar supplied from the alloy producers. Ultimately, alloy 282 was down-selected for the turbine rotor based on its combination of creep strength, phase stability, ductility, and fatigue resistance. The next step in development was to produce a full-size rotor forging for testing. A team was established consisting of GE Power (project management and testing), Wyman-Gordon (forging and testing) and Special Metals (melting and billetizing) to pursue the work. A research license to melt the alloy was obtained from Haynes International. The first step of the development was to devise a triple melt (VIM-ESR-VAR) practice to produce 610 mm (24 inch) diameter ingot. Two ingots were made, the first to define the VAR remelting parameters and the second to make the test ingot utilizing optimum conditions. Careful attention was paid to ingot structure to ensure that no solidification segregation occurred. A unique homogenization practice for the alloy was developed by the US Department of Energy (DOE) and National Energy Technology Laboratory (NETL). Billetization was performed on an open die press with three upset and draw stages. This procedure produced an average grain size of ASTM 3. A closed die forging practice was developed based on compressive flow stress data developed by Wyman Gordon Houston for the consortium project. Multiple 18 kg forgings were produced to define the forging parameters that yielded the desired microstructure. The project culminated with a 2.19 metric ton (4830 lb), 1.22 m (48 inch) diameter crack-free pancake forging produced on Wyman Gordon’s 50,000 ton press in Grafton, MA. The forging process produced a disk with an average grain size of ASTM 8 or finer. Forging cut-up, microstructural characterization, and mechanical property testing was performed by GE Power. Fatigue and fracture toughness values of the disk forging exceeded those previously reported for commercially available rolled bar.

Due to their excellent high temperature oxidation resistance, utilities worldwide are adopting advanced austenitic stainless steels (A-ASS) for critical plant components, such as heat exchangers, as they aim to achieve higher operating conditions. However, challenges may be encountered in developing life assessment and life management strategies for such components. This is because conventional methods used for life assessment, such as measuring steam side oxide scale thickness in ferritic and conventional austenitic material to predict tube metal temperature, may not be successfully applied to A-ASS. In such instances, tracking the formation and evolution of microstructural features during service, may offer a possible method to predict the temperature of these steels. For such metallurgy based lifing strategy to be successful, it is essential to develop a good understanding of microstructure evolution in these steels. In this work one heat of Super 304H, that has been creep tested at 600°C, 650°C and 700°C, with applied stress ranging from 110 to 340 MPa, is characterized using a combination of advanced characterization tools and image analysis methods. The amount of sigma phase formed at the gauge and grip sections of the samples is quantified and the methodology used to quantify this phase is presented. From the results, a time-temperature-transformation diagram for sigma formation is developed.

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.

Future, flexible thermal energy conversion systems require new, demand-optimized high-performance materials. In order to provide a basis for the targeted development of fatigue-resistant, cost-effective steel grades, the microstructural damage to materials and the failure of conventional and novel steels were investigated in thermo-mechanical fatigue and fatigue crack propagation experiments. Based on the results, improved, ferritic “HiperFer” (High performance Ferrite) steels were designed, produced and characterized. A brief description of the current state of development is given.

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 .

Continuous and extensive works have been going to develop 700°C A-USC (Advanced Ultra Super Critical) power plants worldwide. Since Japanese national project launched in 2008, Ni based alloy HR6W (45Ni-24Fe-23Cr-7W-Ti, ASME Code Case 2684) was selected as one of the promising candidate materials of A-USC boiler tube and pipe for long-term creep strength evaluation and field exposure test. In the present study, to establish the creep damage and life assessment method for Ni based alloy component, long-term creep rupture properties, microstructural stability, and creep damage morphology of HR6W weldment were experimentally investigated. Creep tests of HR6W weldment were conducted at temperature range of 700 to 800°C for durations up to 70,000 hours. Failure behavior of creep void formation and creep crack growth was identified, and damage mechanism of weldment during creep were discussed and characterized. Furthermore, uniaxial interrupted creep tests were carried out, the creep damage evaluation was conducted and life assessment approach was proposed based on the metallographic quantification evaluation of creep void and microstructure evolution. It demonstrated the possibility and validity to evaluate creep damage of Ni based alloy component with creep void and microstructure parameters.

The present study presents a detailed investigation on the evolution of the microstructure during welding on virgin and long-term service exposed (creep aged 1 = 535°C; 16.1 MPa; 156 kh and creep aged 2 = 555°C; 17.0 MPa; 130 kh) 12% Cr (X20CrMoV11-1) martensitic steel. This study was carried out in order to understand the impact of welding on prior creep exposed Tempered martensite ferritic (TMF) steel and to explain the preferential failure of weldments in the fine grained heat affected zone (FGHAZ) of the creep aged material side instead of the new material side. Gleeble simulation (Tp = 980°C; heating rate = 200 °C/s; holding time = 4 seconds) of the FGHAZ was performed on the materials to create homogeneous microstructures for the investigation. Quantitative microstructural investigations were conducted on the parent plate and simulated FGHAZ materials using advanced electron microscopy to quantify: a) voids, b) dislocation density, c) sub-grains, and d) precipitates (M 23 C 6 , MX, Laves, Z-phase) in the materials. Semi-automated image analysis was performed using the image analysis software MIPARTM. The pre-existing creep voids in the creep aged parent material and the large M 23 C 6 carbides (Ø > 300 nm) in the FGHAZ after welding are proposed as the main microstructural contributions that could accelerate Type IV failure on the creep aged side of TMF steel weldments.

Inconel alloy 740H is designated for boiler sueprheater/reheater tubes and main steam/header pipes application of advanced ultra-supercritical (A-USC) power plant at operating temperatures above 750°C. Microstructure evolution and precipitates stability in the samples of alloy 740H after creep-rupture test at 750°C, 800°C and 850°C were characterized in this paper by scanning electron microscopy, transmission electron microscopy and chemical phase analysis in details. The phase compositions of alloy 740H were also calculated by thermodynamic calculation. The research results indicate that the microstructure of this alloy keeps good thermal stability during creep-rupture test at 750°C, 800°C and 850°C. The precipitates are MC, M 23 C 6 and γ′ during creep-rupture test. The temperature of creep test has an important effect on the growth rate of γ′ phase. No harmful and brittle σ phase was found and also no γ′ to η transformation happened during creep. Thermodynamic calculations reveal almost all the major phases and their stable temperatures, fractions and compositions in the alloy. The calculated results of phase compositions are consistent with the results of chemical phase analysis. In brief, except of coarsening of γ′, Inconel alloy 740H maintains the very good structure stability at temperatures between 750°C and 850°C.

In this study, 25Cr2Ni2Mo1V filler metal was deposited to weld low pressure steam turbine shafts, which are operated in fossil power plants. A comparison experiment was conducted on the weld metals (WMs) before and after varied various aging duration from 200 hours up to 5000 hours at 350 ℃. Microstructure was characterized by means of scanning electron microscopy (SEM) and electron back-scattered diffraction (EBSD) techniques. In addition, mechanical properties of corresponding specimens were evaluated, e.g. Vickers microhardness, Charpy V impact toughness and tensile strength. It is shown that the tensile strength remained stable while impact energy value decreased with increasing aging duration. Based on the experiment above, it was concluded that the variation of mechanical properties can be attributed to the redissolution of carbides and reduction of bainite lath substructure.

New Fe-base ferritic alloys based on Fe-30Cr-3Al-Nb-Si (wt.%) were proposed with alloy design concepts and strategies targeted at improved performance of tensile and creep-rupture properties, environmental compatibilities, and weldability, compared to Grade 91/92 type ferritic-martensitic steels. The alloys were designed to incorporate corrosion and oxidation resistance from high Cr and Al additions and precipitate strengthening via second-phase intermetallic precipitates (Fe2Nb Laves phase), with guidance from computational thermodynamics. The effects of alloying additions, such as Nb, Zr, Mo, W, and Ti, on the properties were investigated. The alloys with more than 1 wt.% Nb addition showed improved tensile properties compared to Gr 91/92 steels in a temperature range from 600-800°C, and excellent steam oxidation at 800°C as well. Creep-rupture properties of the 2Nb-containing alloys at 700°C were comparable to Gr 92 steel. The alloy with a combined addition of Al and Nb exhibited improved ash-corrosion resistance at 700°C. Additions of W and Mo were found to refine the Laves phase particles, although they also promoted the coarsening of the particle size during aging. The Ti addition was found to reduce the precipitate denuded zone along the grain boundary and the precipitate coarsening kinetics.

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.

A new martensitic steel for power generation applications was developed: Tenaris High Oxidation Resistance (Thor) is an evolution of the popular ASTM grade 91, offering improved steam oxidation resistance and better long-term microstructural stability, with equal or better creep strength. Thanks to its design philosophy, based on consolidated metallurgical knowledge of microstructural evolution mechanisms, and an extensive development performed in the last decade, Thor was engineered to overcome limitations in the use of ASTM grade 91, above 600 °C, particularly related to scale growth and liftoff. After laboratory development, Thor was successfully validated at the industrial level. Several heats up to 80 metric tons were cast at the steel shop, hot rolled to tubes of various dimensions, and heat treated. Trial heats underwent extensive characterization, including deep microstructural examination, mechanical testing in the as-received condition and after ageing, long-term creep and steam oxidation testing. This paper presents an overview of metallurgical characterization performed on laboratory and industrial Thor material, including microstructural examination and mechanical testing in time-independent and time-dependent regimes. Data relevant to the behavior and the performance of Thor steel are also included.

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.