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.

MarBN steels, originally developed by Professor Fujio Abe at NIMS Japan, have undergone significant advancement in the UK through a series of government-funded collaborative projects (IMPACT, IMPEL, INMAP, IMPULSE, and IMPLANT). These initiatives have achieved several major milestones, including operational power plant trials, full-scale extruded pipe production, matching welding consumable development, and most notably, the creation of IBN-1—a new steel demonstrating 30-45% higher creep strength than Grade 92. However, like other creep strength-enhanced ferritic steels, IBN-1 shows reduced creep ductility under the lower stress conditions typical of operational use. Since adequate creep ductility is essential for component damage tolerance and effective in-service monitoring, this study investigates the effects of an alternative normalizing and tempering heat treatment on cast IBN-1. The research presents creep rupture test results showing improved ductility and analyzes the microstructural mechanisms responsible for this enhancement.

The microstructures of an advanced Ta-added 9Cr-3Co-2W-Mo steel with increased boron content that has been homogenized at different temperatures were investigated. The chains of coarse W-rich particles were observed in the steel after homogenization at 1150°C for 24 h. These particles remained in the microstructure after normalization and tempering. Such additional dispersion hardening in the initial state of the studied steel decreased the creep rate in transient region. However, the duration of steady state creep and overall creep time was increased in the samples homogenized at 1200°C. Despite of the presence of coarse W-rich particles, the impact toughness of the low-temperature- homogenized steel in the tempered condition was significantly higher than that of the steel homogenized at 1200°C

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

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

Two materials with different purity of 2.25Cr-1Mo steel thick weld joint were prepared and creep rupture behavior was investigated by large sized specimens. For high purity material, two types of challenging heat treatment was tried to modify the original microstructural conditions. Weld joints were made and large sized creep test specimens were machined. Creep tests were performed at 903K, 40MPa. Specimen made from low purity material fractured at fine grained heat affected zone (FGHAZ) and showed so-called Type IV cracking. On the other hand, specimen made from high purity material showed maximum creep damage at weld metal. In the case of specimens applied challenging heat treatment, remarkably high ductility were observed at fracture. Regarding 2.25Cr-1Mo steel, it was confirmed that the suppression of Type IV cracking had been basically achieved by past improvement on purity level. At the same time, improvement of heat treatment condition was found to have further effect. Because of improved creep properties of high purity material, properties of weld metal had rose up to be the next issue to be examined. At least, taking care on layout design of weld beads to avoid creating wide spread fine grained portion is desired.

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.

Creep strength degradation behavior of normalized and tempered 2.25Cr-1.6W-V-Nb(Gr.23) steel was investigated by conducting extra long-term creep rupture tests. Creep strength drop was observed in long-term creep range at 600°C and above, while signs of a creep strength drop were not identified at 550°C and 575°C. Creep strength drop of around 110 MPa at 600°C was caused not by the effect of oxidation but rather by a change of the deformation mechanism or the weakening of deformation resistance by the microstructural change during creep. The effect of oxidation was significant for causing a further creep strength drop in the range which exceeded 20,000 h in rupture time at 600°C. As a result, the creep strength at 60 MPa and 600°C was almost the same regardless of long tempered or aged steel.

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.

The effect of boron nitrides (BN) and aluminum nitrides (AlN) on long-term creep life and rupture ductility has been investigated for martensitic 9 to 12Cr steels at 550 to 700 °C. The BN particles form in 9 to 12Cr steels during normalizing heat treatment at 1050 to 1150 °C, suggesting no change in the amount of BN particles during creep. On the other hand, the AlN particles gradually form during creep at 550 to 700 °C, decreasing the concentration of nitrogen free from the AlN particles. The degradation in creep life takes place more significantly with test duration in the steels containing high Al but not in those containing the BN particles. The rupture ductility is evaluated by using a semi-logarithmic diagram of the RA and total elongation, showing the necking dominant and void swelling dominant regions. The BN and AlN particles are responsible for the degradation in RA at low stresses and long times by accelerating the formation of creep voids at interfaces between the BN and AlN particles and alloy matrix.

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.

The addition of boron without the formation of any boron nitrides during normalizing heat treatment at high temperature minimizes the degradation in creep strength of both base metal and welded joints of 9Cr steel at 650 °C and long times. The enrichment of soluble boron near prior austenite grain boundaries (PAGBs) by the segregation is essential for the reduction of coarsening rate of M 23 C 6 carbides in the vicinity of PAGBs, enhancing boundary and subboundary hardening, and also for the production of same microstructure between the base metal and heat-affected-zone (HAZ) in welded joints, indicating no Type IV fracture in HAZ. Excess addition of boron and nitrogen promotes the formation of boron nitrides during normalizing, which reduces the soluble boron concentration and accelerates the degradation in creep rupture ductility at long times. 9Cr- 3W-3Co-VNb steel with 120 - 150 ppm boron and 60 - 90 ppm nitrogen (MARBN) exhibits not only much higher creep strength of base metal than Gr.92 but also substantially no degradation in creep strength due to Type IV fracture at 650 °C. The pre-oxidation treatment in Ar gas promotes the formation of protective Cr 2 O 3 scale on the surface of 9Cr steel, which significantly improves the oxidation resistance in steam at 650 °C.

Creep strength enhanced ferritic (CSEF) steels, particularly modified 9Cr steels Grade 91 and 92, are increasingly used in advanced coal-fired power plants for header and steam piping construction. While these materials typically enter service after receiving a standard high-temperature normalizing treatment followed by lower temperature tempering to achieve optimal microstructure, practical situations like welding operations may expose components to additional heat treatment exceeding the Ac 1 , and potentially the Ac 3 , temperature before returning to tempering temperature. This research examines the effects of simulated post weld heat treatments (PWHT) on Grade 91 and 92 materials using dilatometer-controlled heating and cooling rates, with peak temperatures below Ac 1 , between Ac 1 and Ac 3 , and above Ac 3 , followed by heat treatment at 750°C for 2 hours. Hardness measurements revealed significant reduction when exceeding the Ac 1 temperature, while advanced electron microscopy, including electron back scatter diffraction, was employed to analyze changes in martensite laths and grain structure, along with detailed carbide size distribution analysis using both scanning and transmission electron microscopy. The findings are discussed in terms of how such PWHT overshoots might affect mechanical properties during high-temperature service.

A 9Cr-3W-3Co-VNbBN steel, designated MARBN ( MAR tensitic 9Cr steel strengthened by B oron and N itrides), has been alloy-designed and subjected to long-term creep and oxidation tests for application to thick section boiler components in USC power plant at 650 o C. The stabilization of lath martensitic microstructure in the vicinity of prior austenite grain boundaries (PAGBs) is essential for the improvement of long-term creep strength. This can be achieved by the combined addition of 140ppm boron and 80ppm nitrogen without any formation of boron nitrides during normalizing at high temperature. The addition of small amount of boron reduces the rate of Ostwald ripening of M 23 C 6 carbides in the vicinity of PAGBs during creep, resulting in stabilization of martensitic microstructure. The stabilization of martensitic microstructure retards the onset of acceleration creep, resulting in a decrease in minimum creep rate and an increase in creep life. The addition of small amount of nitrogen causes the precipitation of fine MX, which further decreases the creep rates in the transient region. The addition of boron also suppresses the Type IV creep-fracture in welded joints by suppressing grain refinement in heat affected zone. The formation of protective Cr 2 O 3 scale is achieved on the surface of 9Cr steel by several methods, such as pre-oxidation treatment in Ar gas, Cr shot-peening and coating of thin layer of Ni-Cr alloy, which significantly improves the oxidation resistance of 9Cr steel in steam at 650 o C. Production of a large diameter and thick section pipe and also fabrication of welds of the pipe have successfully been performed from a 3 ton ingot of MARBN.

Recent years high strength 9Cr1MoNbV steel developed in USA has been major material in boiler high temperature components with the increase of steam parameters of coal fired thermal power plants. As the microstructure of this steel is tempered martensite, it is known that the softening occurs in HAZ of the weldment. In the creep rupture test of these welded joints the rupture strength is lower than that of the parent metal, and sometimes this reduction of strength is caused by TypelV cracking. To develop an effective method to improve the rupture strength of welded joint, advanced welding procedure and normalizing-tempering heat treatment after weld was proposed. 9Cr1MoNbV plates with thickness of 40-50mm were welded by 10mm width automatic narrow gap MAG welding procedure using specially modified welding material. After normalizing at 1,050°C and tempering at 780°C, material properties of the welded joints were examined. Microstructure of HAZ was improved as before weld, and rupture strength of the welded joints was equal to that of the parent metal. The long term rupture strength of the welded joints was confirmed in the test exceeded 30,000hours. This welding procedure has been applied to seam weld of hot reheat piping and headers in USC boilers successfully.

This paper explores the low cycle fatigue (LCF) and creep-fatigue properties of a hot-forged, normalized, and tempered 9Cr-1Mo ferritic steel. This steel offers good performance in high-temperature applications (up to 873K) in power plants and reactors. The steel was forged into 70 mm diameter rods and then heat-treated with normalizing (1313K for 1 hour, air cooling) and tempering (1033K for 1 hour, air cooling). LCF tests were conducted at 300-873K with varying strain amplitudes and strain rates to understand the influence of both factors. Additionally, some specimens were aged at different temperatures for 10,000 hours before testing. Finally, creep-fatigue interaction tests were performed at 823K and 873K using tensile hold times ranging from 1 to 30 minutes.