Search Results for crystallographic analysis

This paper investigates the cause of premature failures in certain Grade 91 steel components used in UK power plants. The failures were linked to both low material hardness and specific chemical compositions that fell within ASTM specifications but had a low nitrogen-to-aluminum ratio (N:Al). The investigators examined eight material batches, including those involved in failures, new stock, and in-service components with similar properties. Testing confirmed these materials had lower creep resistance compared to standard Grade 91 steel. Microscopic analysis revealed the presence of large aluminum nitride precipitates, which limited the formation of beneficial vanadium nitride precipitates, leading to reduced creep strength. These findings suggest that even within the ASTM specification limits, a low N:Al ratio can negatively impact the performance of Grade 91 steel.

In order to study the effect of precipitation strengthening by MX precipitates on the restriction of microstructure degradation in 9 mass% Cr ferritic heat-resistant steels, V, Nb additioned model steels were evaluated by microstructure analysis through TEM and EBSD with reference to the creep test and creep interrupting test. VN precipitation increased the creep strength if the content was higher than 0.02%. Simultaneous addition of Nb and V in the specimen resulted in the complex NbC-VN precipitates even in the as-heat-treated specimens. The coherent and fine-needle-type VN was also detected in the steel. These precipitates are expected to increase the creep strength according to the creep strain curves. V variation up to 0.02% did not affect the crystallographic character of the grain boundary in the as-heat-treated specimens. Nb variation affected the crystallographic character of the grain boundary significantly because of the grain refinement effect of NbC. VN precipitation during the creep test restricted the crystallographic misorientation-angle-profile degradation. Integrating all intragranular precipitates, VN, restricts the crystallographic degradation significantly. The long-term creep test results and the precise precipitation analysis will be disclosed by the presentation.

In this study, fatigue crack propagation behavior at lower temperature in single crystal nickel-base superalloys was investigated experimentally and analytically. Four types of compact specimens with different combinations of crystal orientations in loading and crack propagation directions were prepared, and fatigue crack propagation tests were conducted at room temperature and 450°C. It was revealed in the experiments that the crack propagated in the shearing mode at room temperature, while the cracking mode transitioned from the opening to shearing mode at 450°C. Both the crack propagation rate and the transition behavior were strongly influenced by the crystallographic orientations. To interpret these experimental results, crystal plasticity finite element analysis was carried out, taking account some critical factors such as elastic anisotropy, crystal orientations, 3-D geometry of the crack plane and the activities of all 12 slip systems in the FCC crystal. A damage parameter based on the slip plane activities derived from the crystal plasticity analysis could successfully rationalize the effect of primary and secondary orientations on the crystallographic cracking, including the crack propagation paths and crack propagation rates under room temperature. The proposed damage parameter could also explain the transition from the opening to crystallographic cracking observed in the experiment under 450°C.

The creep strength and ductility of Grade P22 steel (2¼ Cr) was measured at 600°C under standard uniaxial tensile conditions at 150MPa. Test specimens were prepared by solution heat treatment at austenitization temperatures ranging from 900°C - 1200°C followed by normalization at 900°C before continuous air cooling to room temperature. In addition to specimens tested in the solution treated state, creep tests were also performed after tempering. The variable austenitization temperatures gave rise to different prior austenite grain (PAG) sizes, which in turn influenced the crystallographic packet and block boundary misorientation angle distribution. The latter parameters were measured using electron backscattered diffraction which also allowed partial reconstruction of the PAG boundaries. The time to creep failure at 600°C increased as function of PAG size up to approximately 70µm, but significantly decreased when the average prior austenite grain size measured approximately 108 µm. However, the minimum creep rate decreased even up to the largest PAG size with corresponding decrease in creep ductility. The stability of the crystallographic packet and block boundaries influences the high strength-low ductility for the large PAGs in comparison to the dominant effect of PAG boundaries at the smallest grain size where extensive recovery and recrystallization reduces creep strength.

Recently advanced ultra-super critical (A-USC) pressure power plants with 700°C class steam parameters have been under development worldwide. Japanese material R&D program for A- USC beside the plant R&D program started in 2008, launched in 2007 under the METI/NEDO foundation includes not only alloy design explores and novel ideas for developing new steels and alloys that can fill critical needs in building 700°C class advanced power plants, but also fundamental studies on creep strength and degradation assessment, which are absolutely needed to assure the long-term safe use of newly developed steels and alloys at critical temperature conditions, for instance, 650°C for ferritic steels, 700°C for austenitic steels and 750°C for Ni- based alloys. This program concept has been based on the lessons from materials issues recently experienced in the creep strength enhanced ferritic steels used for 600°C class ultra-super critical power plants. Particular outputs from the program up to now are recognized as the ferritic steel having the creep strength of 100MPa at 650°C beyond 30,000h without any Type IV degradation and as the austenitic steel developed by means of inter-metallic compounds precipitation strengthening of grain boundary which should be strongest in creep ever found. Concurrently great progresses have been seen in the research works with positron annihilation life monitoring method applicable to various kinds of defects, structural free energy values, small punch creep test data for very limited interest area, crystallographic analyses, optimum time-temperature parameter regional creep rupture curve fitting method, hardness model, etc. which would highly contribute to find out and establish the structural parameters affecting to creep strength and degradation resulting in accurately estimating the 100,000h creep strength.

Ni-base superalloys used for hot section hardware of gas turbine systems experience thermomechanical fatigue (TMF), creep, and environmental degradation. The blades and vanes of industrial gas turbines (IGTs) are made from superalloys that are either directionally-solidified (DS) or cast as single crystals (SX). Consequently, designing and evaluating these alloys is complex since life depends on the crystallographic orientation in addition to the complexities related to the thermomechanical cycling and the extent of hold times at elevated temperature. Comparisons between the more complex TMF tests and simpler isothermal low cycle fatigue (LCF) tests with hold times as cyclic test methods for qualifying alternative repair, rejuvenation, and heat-treatment procedures are discussed. Using the extensive set of DS and SX data gathered from the open literature, a probabilistic physics-guided neural network is developed and trained to estimate life considering the influence of crystallographic orientation, temperature, and several other cycling and loading parameters.

Two Z-phase strengthened test steels with similar chemical composition were studied. The main difference in composition is the addition of 1 wt% Cu into one of the steels (referred to as “ZCu”). Mechanical testing was performed. The impact strength is very different: 3 J vs. 46.3 J, for the original and the Z-Cu steel, respectively. In the original steel that contains no Cu, much more Laves-phase (Fe 2 (W,Mo)) precipitates had formed along the prior austenite grain boundaries than in the steel with Cu addition. This is believed to be the reason for the difference in impact strength. Furthermore, the Cu addition also influenced the morphology of Laves-phase precipitates; fine rod-shaped instead of coarse equiaxed Laves-phase particles were observed in Z-Cu steel in comparison to the original steel. No partitioning of Cu into the Laves-phase particles was detected by using atom probe tomography (APT). The main function of Cu seems to be the formation of Cu precipitates that act as nucleation site for Laves-phase.

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.

The current research adopts a novel approach by integrating correlative microscopy and machine learning in order to study creep cavitation in an ex-service 9%Cr 1%Mo Grade 91 ferritic steel. This method allows for a detailed investigation of the early stages of the creep life, enabling identification of features most prone to damage such as precipitates and the ferritic crystal structure. The microscopy techniques encompass Scanning Electron Microscopy (SEM) imaging and Electron Back-scattered Diffraction (EBSD) imaging, providing insights into the two-dimensional distribution of cavitation. A methodology for acquiring and analysing serial sectioning data employing a Plasma Focused Ion Beam (PFIB) microscope is outlined, complemented by 3D reconstruction of backscattered electron (BSE) images. Subsequently, cavity and precipitate segmentation was performed with the use of the image recognition software, DragonFly and the results were combined with the 3D reconstruction of the material microstructure, elucidating the decoration of grain boundaries with precipitation, as well as the high correlation of precipitates and grain boundaries with the initiation of creep cavitation. Comparison between the 2D and 3D results is discussed.

As part of the Boiler Materials for Ultrasupercritical Coal Power Plants program, sponsored by the United States (U.S.) Department of Energy (DOE) and the Ohio Coal Development Office (OCDO), the steamside oxidation and oxide exfoliation behavior of candidate alloys have been thoroughly evaluated in steam at temperatures between 620°C and 800°C (1148°F and 1472°F) for times up to 10,000 hours. The results from this test program indicate that the oxidation rates and oxide morphologies associated with steamside oxidation are a strong function of the crystallographic lattice structure and the chromium content of the material. Oxide exfoliation correlates to oxide thickness. The time required to reach the critical oxide thickness for exfoliation can be estimated based on oxidation kinetic relationships. For austenitic stainless steels, shot peening is effective in reducing steamside oxidation/exfoliation, but the efficacy of this technique is limited by the operating temperature. Nickel-based alloys exhibit very low oxidation/exfoliation rates, but have a propensity to form aluminum/titanium oxides along near surface grain boundaries.

In this study, the role of minor alloying additions in 347H stainless steels (UNS34709, ASTM A240/240M) on creep-rupture properties at 650-750°C and microstructure evolution during isothermal exposure at 750°C has been investigated, aiming to provide the experimental dataset as boundary conditions of physics-based modeling for material/component life prediction. Four different 347H heats containing various amounts of boron and nitrogen additions were prepared and evaluated. The combined additions of B and N are found to stabilize the strengthening secondary M 23 C 6 carbides and retarding the transition from M 23 C 6 to sigma phase precipitates during thermal exposure. The observed kinetics of microstructure evolution reasonably explains the improvement of creep-rupture properties of 347H stainless steels with the B and N additions.

The creep behavior of a γ-TiAl based alloy at 1073 K was investigated, examining three different microstructures: equiaxed γ (Eγ), γ/γ fully lamellar (FLγ), and equiaxed γ with α 2 phase on grain boundaries (Eγα 2 ). The aim was to understand the influence of lamellar interfaces and grain boundary α 2 phase on creep behavior. Initially, creep rates were consistent across all specimens upon loading. However, Eγ exhibited a gradual decrease in creep rate compared to Eγα 2 and FLγ. Notably, the minimum creep rate of Eγ was one order of magnitude lower than that of Eγα 2 and FLγ. Conversely, Eγα 2 and FLγ displayed a slight acceleration and the longest rupture strain, albeit with the shortest rupture time compared to Eγ. Upon microstructural analysis of of the creep-test specimens, it was observed that numerous dynamic recrystallized grains (DXGs) and sub-grains formed along grain boundaries and interiors in Eγ, whereas they were limited to the region along grain boundaries in FLγ. In contrast, very few DXGs were formed in Eγα 2 . These findings indicate that γ/γ interfaces inhibit the extension of DXGs into grain interiors, suggesting that the grain boundary α 2 phase effectively suppresses the formation of DXGs.

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.

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.

This study demonstrates the Electro-Thermal Mechanical Testing (ETMT) system's capability to analyze the thermo-mechanical behavior of Inconel 718 (IN718) at a heating rate of 5 °C/s, achieving temperatures up to 950 °C. The temperature profile peaks at the sample's center and is approximately 25 °C at the extremes. Upon reaching 950 °C, the sample was aged for 30 hours before being rapidly quenched. This process froze the microstructure, preserving the phase transformations that occurred at various temperatures across the temperature parabolic gradient, which resulted in a complex gradient microstructure, providing a comprehensive map of phase transformations in IN718. The integration of thermal measurement, COMSOL modeling, scanning electron microscopy enabled a thorough characterization of the microstructural evolution in IN718, linking observed phases to the specific temperatures which provided a rapid screening of the effect of using different heating treatment routes.

TAF steel is a Japanese high-boron 10.5% Cr martensitic stainless steel known for its exceptional high-temperature creep strength. Its high boron content (300-400 ppm) limited practical applications due to reduced hot workability in large turbine components. Recent research suggests that increasing boron content while adjusting nitrogen levels could enhance creep properties by promoting fine vanadium carbonitride formation while preventing boron nitride formation. This study presents microstructural investigations, particularly using transmission electron microscopy, focusing on precipitation characteristics and long-term precipitate evolution within the COST 536 framework.

The power industry has been faced with continued challenges around decarbonization and additive manufacturing (AM) has recently seen increased use over the last decade. The use of AM has led to significant design changes in components to improve the overall efficiency of gas turbines and more recently, hot-section components have been fabricated using AM nickel-base superalloys, which have shown substantial benefits. This paper will discuss and summarize extensive studies led by EPRI in a novel AM nickel-base superalloy (ABD·900-AM). A comprehensive high temperature creep testing study including >67,000 hours of creep data concluded that ABD-900AM shows improved properties compared to similar ~35% volume fraction gamma prime strengthened nickel-base superalloys fabricated using additive methods. Several different creep mechanisms were identified and various factors influencing high temperature behavior, such as grain size, orientation, processing method, heat treatment, carbide structure, chemistry and porosity were explored. Additional studies on the printability, recyclability of powder, wide range of process parameters and several other factors have also been studied and results are summarized. A summary on the alloy -by-design approach and accelerated material acceptance of ABD-900AM through extensive testing and characterization is further discussed. Numerous field studies and examples of field use cases in ABD-900AM are also evaluated to showcase industry adoption of ABD-900AM.

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.

Strengthening of Ni-based superalloys is in principle designed using GCP (Geometrically Close-packed phase) of Ni 3 Al-γ' (L1 2 ). However, game-changing microstructural design principle without relying on γ' phase will be needed for further development of the alloys. We are currently constructing a novel microstructure design principle, using thermodynamically stable TCP (Topologically Close-packed phase) for grain boundaries, together with GCP other than γ' phase for grain interiors, based on grain boundary precipitation strengthening (GBPS) mechanism. One of the promising systems is Ni-Cr-Mo ternary system, where TCP of NiMo (oP112) phases, μ (hR13) and P (oP56), together with GCP of Ni 3 Mo (oP8) and Ni 2 Cr (oP6) exists. In this study, thus, phase equilibria among A1 (fcc)/TCP/GCP phases in Ni-Cr-Mo and Ni-Cr-W systems have been examined at temperature range from 973 K to 1073 K, based on experiment and calculation. In Ni-Cr-Mo system, Ni 2 (Cr, Mo) with oP6 Pearson symbol, which is stable at about 873 K in Ni-Cr binary system, is formed to exist even at 1073 K. oP6 phase is coherently formed in A1 matrix with a crystallographic orientation of {110} A1 // (100) oP6 , <001>Α1 // [010]oP6, indicating GCP at composition range around Ni-15Cr-15Mo as island. In Mo-rich region there is Α1/NiMo/oP6 three-phase coexisting region, whereas another three-phase coexisting region of Α1/P/oP6 exists in Cr-rich region. Based on vertical section, it is possible to design microstructure with TCP at grain boundaries, together with oP6 phase within grain interiors by two-step heat treatment.

Advanced UltraSupercritical (A-USC) Steam fossil power plants will operate at steam temperatures up to 760°C, which will require the use of Ni-based superalloys for steam boiler/superheater and turbine systems. In 2008, the Oak Ridge National Laboratory (ORNL) and the National Engineering Technology Laboratory/Albany (NETL/Albany) collaborated to make and test castings of Ni-based superalloys, which were previously only commercially available in wrought form. These cast Ni-based based alloys are envisioned for the steam turbine casing, but they may also be applicable to other large components that connect the steam supply to the steam turbine. ORNL and NETL/Albany have produced small vacuum castings of HR 282, Nimonic 105, Inconel 740, and alloy 263, which are precipitation-hardened Ni-based superalloys, as well as solid-solution superalloys such as alloys 625, 617 and 230. The initial alloy screening included tensile and creep-testing at 800°C to determine which alloys are best suited for the steam turbine casing application at 760°C. HR 282 has the best combination of high-temperature strength and ductility, making it a good candidate for the cast-casing application. Cast and wrought versions of HR 282 have similar creep-rupture strength, based on the limited data available to-date. Detailed comparisons to the other alloys and microstructures are included in this paper.