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

The time-dependent behavior of 9Cr creep strength enhanced ferritic (CSEF) steels has long fixated on the creep life recorded in uniaxial constant load creep tests. This focus is a consequence of the need to develop stress allowable values for use in the design by formulae approach of rules for new construction. The use of simple Design by Formula rules is justified in part by the assumption that the alloys used will invariably demonstrate high creep ductility. There appears to be little awareness regarding the implication(s) that creep ductility has on structural performance when mechanical or metallurgical notches (e.g., welds) are present in the component design or fabricated component. This reduced awareness regarding the role of ductility is largely because low alloy CrMo steels used for very many years typically were creep ductile. This paper focuses on the structural response from selected tests that have been commissioned or executed by EPRI over the last decade. The results of these tests demonstrate unambiguously the importance that creep ductility has on long-term, time-dependent behavior. The metallurgical findings from the selected tests are the focus of the Part II paper. The association of performance with notch geometry, weld strength, and other potential contributing factors will be highlighted with a primary objective of informing the reader of the variability, and heat-specific behavior that is observed among this class of alloys widely used in modern thermal fleet components and systems.

Carbon migration in narrow-gap welding joints of dissimilar steels has been studied using bead-on-plate specimens to determine the factors that influence the formation of a soft ferrite structure in the carbon-depleted zone. Carbon migration was found to occur during tempering, with a ferrite structure formed at the intersection of multiple layers due to severe carbon migration. This was attributed to a steep gradient in Cr content caused by the low fusion penetration at the intersection. Experimental results and the relationship between fusion penetration and weld bead alignment confirmed that low fusion penetration is the main cause of ferrite-structured carbon depleted zones.

For last half century the development of creep strength enhanced ferritic steels has been continued and presently ASME grades 91, 92 and 122 extremely stronger than conventional low alloy steels have extensively been used worldwide in high efficient power plants. However the use of these creep strength enhanced 9-12%Cr steels is limited to around 630°C or 650°C at maximum in terms of high temperature strength and oxidation resistance. Consequently the appearance of ferritic steels standing up to higher temperature of around 700°C to substitute of high strength austenitic steels is strongly desired. Under the state, the addition of high nitrogen to ferritic steels is attracting considerable attention because of improving high temperature strength and oxidation resistance of them. This work was done to evaluate the oxidation resistance of high nitrogen steels and to investigate the effect nitrogen and microstructure on oxidation resistance using 9-15%Cr steels with about 0.3% nitrogen manufactured by means of Pressurized Electro- Slag Remelting (PESR) method in comparison with ASME grades 91 and 122. As a result, high nitrogen ferritic steels showed excellent oxidation resistance comparing with nitrogen-free steels and ASME grades 91 and 122. The oxidation resistance of 9%Cr ferritic steels depends on the nitrogen content in the each steel. That is, the weight gain decreases with an increase in nitrogen content. Moreover, the oxide scale of high nitrogen steel contained a high concentration of Cr. It is conjectured that, in high temperature oxidation, nitrogen plays a key role in promoting the formation of the oxide scale which has high concentration of Cr, inhibiting oxidation from proceeding. And also it was found that the oxidation resistance of the high nitrogen steels does not depend greatly on Cr content but on their microstructure. The oxidation resistance of high nitrogen ferritic heat-resistant steels increased as the fraction of martensite structure increased. These results indicate for high nitrogen steels Cr diffusion along grain boundaries is further promoted resulting in the formation of protective oxide scale having high Cr concentration. Furthermore as new findings it was confirmed that the Cr diffusion in substrate of steels to form Cr concentrated oxide scale on the metal surface is accelerated by nitrogen while suppressed by carbon in matrix of steel.

Modified 9Cr-1Mo steel was manufactured via laser powder bed fusion (LPBF) using gas atomized powders under various building conditions. Dense samples were obtained at an energy density of 111-125 J/mm 3 . As-built samples were subjected to a normalization and tempering heat treatments. The microstructure of the as-built sample exhibits a duplex structure, comprising coarse columnar δ-ferrite grains and fine martensite grains. In addition, a small amount of retained austenite phase was observed at the interface between δ-ferrite and martensite. The formation of δ-ferrite is attributed to the extremely rapid solidification that occurs during the LPBF process, while martensite is obtained through the phase transformation because of the thermal cycles experienced during the process. The area fraction of δ-ferrite and martensite can be controlled by adjusting the LPBF parameters. Typical as-built microstructure morphology characterized by the columnar δ- ferrite was eliminated after the heat treatments, resulting in a tempered martensitic microstructure that is identical with that obtained through the conventional process. However, an increase in prior austenite grain size was observed when the area fraction of δ-ferrite in the as-built condition was high, due to faster phase transformation kinetics of martensite than that of δ-ferrite during the normalization. This suggests that the prior austenite grain size can be controlled by optimizing the area fraction of δ-ferrite and martensite in the as-built microstructure.

NiAl precipitates with the B2 structure are known to be effective in increasing the strength of ferritic heat-resistant steels. The strengthening mechanism by the NiAl precipitates was examined using Fe-21Al-2Ni and Fe-23Al-6Ni (at%) single crystals. As a result, the difference in primary slip system between the bcc matrix and the NiAl precipitates is responsible for strong hardening. The B2-NiAl phase was precipitated in the bcc matrix satisfying the cube-on-cube orientation relationship with small misfit strain. The primary slip direction of the bcc matrix and the NiAl precipitates are <111> and <001>, respectively. However, in the ferritic alloys, the NiAl precipitates were cut by paired 1/2<111> dislocations in the bcc matrix, resulting in the hardening. The size and volume fraction of the NiAl precipitates strongly influenced the strength. The stress increase by the NiAl precipitates was also discussed quantitatively based on the precipitation hardening theory. Based on the experimental results obtained by the single crystal study, we developed Fe-Al-Ni-Cr-Mo ferritic heat-resistant alloy containing the NiAl precipitates. The alloy exhibited excellent creep properties at 923 K.

Fossil fuels continue to be the primary source of energy in the U.S and worldwide. In order to improve the efficiency of fossil power plants, advanced structural materials need to be developed and deployed to meet the need of high temperature creep resistance and corrosion resistance. Examples include creep strength enhanced ferritic (CSEF) steels, austenitic stainless steels, nickel-based superalloys, and oxide dispersion strengthened alloys. Welding is extensively used in construction of fossil power plants. The performance of the weld region can be critical to the safe and economical operation of fossil power plants. Degradations in performance such as reduced creep strength and premature failure in the weld region (e.g. Type IV failure in ferritic steels) are examples of longstanding welding and weldability problems for boiler and other components. In the past, extensive studies have been carried out to characterize the different microstructures in different regions of a weld, and to a certain extent, to establish the correlations between the microstructure and the creep strength. However, the metallurgical or microstructural induced local stress/strain variations have been seldom quantified. In addition, it has been long recognized that, due to the sharp microstructure and property gradients in the weld and HAZ, the standard creep testing procedure for the base metal can produce erroneous results when used for weld testing.

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.

Creep behavior and degradation of creep properties of advanced 9-12%Cr ferritic steels are phenomena of major practical relevance, often limiting the lives of power plant components and structures designed to operate for long periods under stress at elevated temperatures. Because life expectancy is, in reality, based on the ability of the material to retain its high-temperature creep strength for a period of at least twice the projected design life, methods of creep property assessment based on physical changes in the material that are likely to occur during service exposure rather than simple parametric extrapolation of the short-term data are necessary. This work attempts to highlight the problem areas just in this respect. The proposed approaches are illustrated by recent experimental results on advanced high creep strength 9-12%Cr ferritic- martensitic steels (P91 and P92).

The effect of a reduced-temperature austenization treatment on the microstructure and strength of two ferritic-martensitic steels was studied. Prototypic 9% and 12% Cr steels, modified 9Cr-1Mo (ASME T/P91) and Type 422 stainless (12Cr-1Mo-W-V), respectively, were austenized at the standard 1050°C and an off-normal 925°C, both followed by tempering at 760°C. The reduced austenization temperature was intended to simulate potential inadequate austenization during field construction of large structures. The microstructure, tensile behavior, and creep strength were characterized for both steels treated at each condition. While little change in microstructure was observed for the modified 9Cr-1Mo steel, the creep strength was reduced at higher temperatures and in long duration tests. The microstructure of the Type 422 stainless in the off-normal condition consisted of polygonized ferrite instead of tempered martensite. In this case the creep strength was reduced for short duration tests (less than ~1000 hr), but not for long duration tests. Slight reductions in tensile strength were observed at room temperature and elevated temperatures of 450,550, and 650°C.

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.

In the present study a creep resistant, ferritic steel, based on the chemical composition of Crofer 22 H, was analysed regarding microstructure and particle evolution. Because of the preceding hot-rolling process formation of sub-grain structures was observed, which disappears over time. Additionally formation of particle-free zones close to high angle grain boundaries was observed. These zones are considered to be responsible for long-term material failure by lacking particle hardening and thus a concentration of deformation. Therefore in-depth analyses by transmission and scanning electron microscopy were performed to investigate dislocation behaviour in these areas

In order to develop an Fe/Ni dissimilar-weld rotor structure for an Advanced Ultra Super Critical turbine, fundamental studies on the metallurgical properties of Fe/Ni welds are needed. In the work reported in this paper, we studied the microstructure evolution and creep rupture properties of Fe/Ni weld joints with different compositions. Investigation of thermally aged Fe/Ni diffusion couples revealed that Fe-based ferritic steel and Alloy 617 weld joints with a large difference in Cr content showed strong C diffusion at the weld interface. This decreased the creep rupture life of the weld joint, caused by coarsening of a martensitic structure near the interface. Analysis using Fe/Ni diffusion couples and thermodynamic calculations suggested that the driving force of C diffusion is the chemical potential gradient at the interface, and the difference in Cr content between Fe and Ni accelerates the C diffusion.

A new alloy design concept for creep- and corrosion-resistant, fully ferritic alloys was proposed for high-temperature structural applications in current/future fossil-fired power plants. The alloys, based on the Fe-30Cr-3Al (in weight percent) system with minor alloying additions of Nb, W, Si, Zr and/or Y, were designed for corrosion resistance though high Cr content, steam oxidation resistance through alumina-scale formation, and high-temperature creep performance through fine particle dispersion of Fe 2 (Nb,W)-type Laves phase in the BCC-Fe matrix. Theses alloys are targeted for use in harsh environments such as combustion and/or steam containing atmospheres at 700°C or greater. The alloys, consisting of Fe-30Cr-3Al-1Nb-6W with minor alloying additions, exhibited a successful combination of oxidation, corrosion, and creep resistances comparable or superior to those of commercially available heat resistant austenitic stainless steels. An optimized thermo-mechanical treatment combined with selected minor alloying additions resulted in a refined grain structure with high thermal stability even at 1200°C, which improved room-temperature ductility without sacrificing the creep performance. The mechanism of grain refinement in the alloy system is discussed.

This study investigated the creep rupture strength and microstructure evolution in welded joints of high-boron, low-nitrogen 9Cr steels developed by NIMS. The welds were fabricated using the GTAW process and Inconel-type filler metal on steel plates with varying boron content (47-180 ppm). Creep rupture tests were conducted at 923K for up to 10,000 hours. Despite their higher boron content, these steels exhibited good weldability. Welded joints of the boron steel displayed superior creep properties compared to conventional high-chromium ferritic steel welds like P92 and P122. Notably, no Type IV failures were observed during creep testing. Welding introduced a large-grained microstructure in the heat-affected zone (HAZ) heated to the austenite transformation temperature (Ac3 HAZ). This contrasts with the grain refinement observed in the same region of conventional heat-resistant steel welds. Interestingly, the grain size in this large microstructure was nearly identical to that of the base metal. Analysis of the simulated Ac3 HAZ revealed crystal orientation distributions almost identical to those of the original specimen. This suggests a regeneration of the original austenite structure during the alpha-to-gamma phase transformation. Simulated Ac3 HAZ structures of the boron steel achieved creep life nearly equivalent to the base metal. The suppression of Type IV failure and improved creep resistance in welded joints of the boron steels are likely attributed to the large-grained HAZ microstructures and stabilization of M 23 C 6 precipitates. The optimal boron content for achieving the best creep resistance in welded joints appears to lie between 90 and 130 ppm, combined with minimized nitrogen content.

The time-dependent behavior of 9Cr creep strength enhanced ferritic (CSEF) steels has long fixated on the creep life recorded in uniaxial constant load creep tests. This focus is a consequence of the need to develop stress allowable values for use in the design by formulae approach of rules for new construction. The use of these simple rules is justified in part by the assumption that the alloys used will invariably demonstrate high creep ductility. There appears to be little awareness regarding the implication(s) that creep ductility has on structural performance when mechanical or metallurgical notches (e.g., welds) are present in the component design or fabricated component. This reduced awareness regarding the role of ductility is largely because low alloy CrMo steels used for very many years typically were creep ductile. This paper focuses on the structural response from selected tests that have been commissioned or executed by EPRI over the last decade. The results of these tests demonstrate unambiguously the importance that creep ductility has on long-term, time-dependent behavior. This is the second part of a two-part paper; Part I reviewed the selected tests and discussed them from a mechanical perspective. The association of performance with specific microstructural features is briefly reviewed in this paper and the remaining gaps are highlighted for consideration among the international community.

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.

To save fossil fuel resources and to reduce CO 2 emissions, considerable effort has been directed toward researching and developing heat-resistant materials that can help in improving the energy efficiency of thermal power plants by increasing their operational temperature and pressure conditions. Instead of conventional 9-12Cr ferritic heat-resistant steels with a tempered martensitic microstructure, we developed “Precipitation Strengthened 15Cr Ferritic Steel” based on a new material design concept: a solid-solution treated ferrite matrix strengthened by precipitates. Creep tests for 15Cr-1Mo-6W-3Co-V-Nb steels with ferrite matrix strengthened by a mainly Laves phase (Fe 2 W) showed that the creep strengths of 15Cr ferritic steel at temperatures ranging from 923 K to 1023 K were twice as high as those of conventional 9Cr ferric heat-resistant steel. 15Cr steels have higher steam oxidation resistance than that of conventional steel in the same temperature range as the creep tests. Thus, the new material design concept of heat-resistant steel pro- vides improved creep strength and steam oxidation resistance. We are attempting to determine the optimum compositions, especially that of carbon, in order to improve the high-temperature creep strength.

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.

Creep brittle behaviour in tempered martensitic, creep strength enhanced ferritic (CSEF) steels is linked to the formation of micro voids. Details of the number of voids formed, and the tendency for reductions in creep strain to fracture are different for the different CSEF steels. However, it appears that the susceptibility for void nucleation is related to the presence of trace elements and hard non-metallic inclusions in the base steel. A key factor in determining whether the inclusions present will nucleate voids is the particle size. Thus, only inclusions of a sufficient size (the critical inclusion size is directly linked to the creep stress) will act directly as nucleation sites. This paper compares results from traditional uniaxial laboratory creep testing with data obtained under multiaxial conditions. The need to understand and quantify how metallurgical and structural factors interact to influence creep damage and cracking is discussed and the significant benefits available through the use of high quality steel making and fabrication procedures are highlighted. Details of component behaviour are considered as part of well-engineered, Damage Tolerant, design methods.