Search Results for ion beam induced secondary electron imaging

Martensitic 9Cr steels have been developed which are strengthened by boron in order to stabilize the microstructure and improve their long-term creep strength. Boron plays a key role in these steels by stabilising the martensitic laths by decreasing the coarsening rate of M 23 C 6 carbides, which act as pinning points in the microstructure. In this work two modified FB2 steel forgings are compared. Both forgings have similar compositions but one underwent an additional remelting process during manufacture. Creep tests showed that this additional processing step resulted in a significant increase in time to failure. In order to investigate the effect of the processing route on microstructural evolution during aging and creep, a range of advanced electron microscopy techniques have been used including ion beam induced secondary electron imaging and High Angle Annular Dark Field (HAADF) imaging in the Scanning Transmission Electron Microscope. These techniques have enabled the particle population characteristics of all the second phase particles (M 23 C 6 , Laves phase, BN and MX) to be quantified for materials from both forging processes. These quantitative data have enabled a better understanding of how the processing route affects the microstructural evolution of FB2 steels.

A detailed examination has been carried out of the microstructural evolution and mechanical properties of samples of T91 and T92 steels which have been subjected to both a ‘normal’ pre­service heat treatment and an extended stress relief heat treatment at 765°C for up to 16 hours. The samples have subsequently been creep tested to failure at different stresses ranging from 66 to 112 MPa. In each case, a reduction in rupture time was observed of 20-30% in the samples which had experienced the additional stress relief heat treatment compared to those which had not. It is shown that these data, when compared with the mean values expected from European Creep Collaborative Committee (ECCC) Datasheets, result in a reduction in stress of approximately 10% of the mean value predicted from the ECCC data, which is within the allowable scatter band.

For VM12-SHC 11-12 wt. % Cr steel, there have been no systematic investigations to define the regions or characterise the microstructures within the heat-affected zone (HAZ) of weldments. In similar steels, these regions relate to the Ac 1 and Ac 3 transformation temperatures and can affect weldment performance. In this study, controlled thermal cycles were applied to VM12-SHC parent metal using a dilatometer and the Ac 1 and Ac 3 temperatures were measured for various heating rates. The Ae 1 and Ae 3 temperatures were also calculated by thermodynamic equilibrium modeling. Through dilatometry, thermal cycles were then applied to simulate the microstructures of the classically defined HAZ regions. The microstructural properties of each simulated material were investigated using advanced electron microscopy techniques and micro-hardness testing. It was found that the simulated HAZ regions could be classified as; (1) the completely transformed (CT) region, with complete dissolution of pre-existing precipitates and complete reaustenitisation; (2) the partially transformed (PT) region, exhibiting co-existing original martensite with nucleating austenite microstructures with partial dissolution of precipitates; and (3) the over tempered (OT) region, with no phase transformation but precipitate coarsening and decreased hardness.

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.

This study investigates the microstructure evolution of Type 316H stainless steel, focusing on the identification of major precipitates using advanced characterization techniques. The precipitation sequence at service temperatures of 650°C is identified as M 23 C 6 , followed by Laves phase, grain boundary (GB) sigma phase, and inter-granular sigma phase. At 750°C, the sequence progresses from M 23 C 6 to Laves phase, GB sigma phase, chi phase, and intra-granular sigma phase, with the chi phase forming intra- and inter-granularly after 5,000 hours of aging. During the formation of the sigma and chi phases, carbides and Laves phases dissolve. A Monte Carlo model has been developed to predict detailed microstructure evolution during long-term aging, calibrated using quantitative precipitate evolution measurements of Type 316H. After validation, the model aligns well with experimental data, offering a method to predict the microstructure of Type 316H and potentially other austenitic stainless steels over the lifespan of power plants.

Grade 92 steel has been widely applied in the power generation industry for use as steam pipes, headers, tubes, etc. owing to a good combination of creep and corrosion resistance. For the welding of thick section pipes, a multi-pass submerged arc welding process is typically used to achieve sufficient toughness in the weld. To relieve the internal stress in the welds and to stabilise their microstructures, a post weld heat treatment (PWHT) is commonly applied. The heat treatment conditions used for the PWHT have a significant effect on both the resulting microstructure and the creep behaviour of the welds. In this study, interrupted creep tests were carried out on two identical Grade 92 welds that had been given PWHTs at two different temperatures: 732°C and 760°C. It was found that the weld with the lower PWHT temperature had a significantly reduced stain rate during the creep test. In addition, microstructural examination of the welds revealed that the primary location of creep damage was in the heat affected zone in the sample with the lower PWHT temperature, whereas it was in the weld metal in the sample with the higher PWHT temperature. To understand the effect of the different PWHT temperatures on the microstructure, initially the microstructures in the head portions of the two creep test bars were compared. This comparison was performed quantitatively using a range of electron/ion microscopy based techniques. It was apparent that in the sample subjected to the higher PWHT temperature, larger Laves phase particles occurred and increased matrix recovery was observed compared with the sample subjected to the lower PWHT temperature.

Extensive research and development has been undertaken in the UK on MarBN steels. These were first proposed by Professor Fujio Abe from NIMS in Japan. Within the UK, progress has been made towards commercialisation of MarBN-type steel through a series of Government funded industrial collaborative projects (IMPACT, IMPEL, INMAP and IMPULSE). As part of the IMPACT project, which was led by Uniper Technologies, boiler tubes were manufactured from the MarBN steel developed within the project, IBN1, and installed on the reheater drums of Units 2 and 3 of Ratcliffe-on-Soar Power Station. The trial tubes were constructed with small sections of Grade 91 tubing on either side of the IBN1 to allow direct comparison after the service exposure. This is the world’s first use of a MarBN steel on a full-scale operational power plant. In September 2018 the first tube was removed having accumulated 11,727 hours operation and 397 starts. This paper reports microstructural and oxidation analysis, that has been undertaken by Loughborough University as part of IMPULSE project, and outlines future work to be carried out.

Friction Stir Layer Deposition on a Cu-containing high-entropy alloy (HEA) has been performed for its suitability of the core component of nuclear materials. Excellent irradiation resistance in this Cu-containing HEA has been reported previously. Friction stir layer deposition (FSLD) offers a solid-state deformation processing route to metal additive manufacturing, in which the feed material undergoes severe plastic deformation at elevated temperatures. Some of the key advantages of this process are fabrication of fully dense material with fine, equiaxed grain structures. This work reports the detailed microstructure of the FSLD product, and it discusses the grain refinement and micro-hardness variation observed in FSLD product.

A FeCrMnNi concentrated solid-solution alloy was irradiated with a 2 MeV proton beam up to 1 dpa and 6 dpa at temperatures of 400 °C and 600 °C. The microstructural changes induced by irradiation were characterized using Transmission Electron Microscopy (TEM). In samples irradiated at 400 °C, Frank loops were the predominant form of lattice damage at 1 dpa, whereas small defect clusters were more prevalent at 6 dpa. For the sample irradiated to 1 dpa at 600 °C, both Frank loops and small defect clusters were present in similar density. Nanoindentation was employed to assess the changes in mechanical properties (hardness) post-irradiation, revealing significant hardening in all irradiated samples. The results indicated that the hardening effect began to saturate at 1 dpa or earlier. Additionally, nanoindentation creep tests with a 1200-second dwell period produced stress exponents comparable to those obtained from conventional creep testing. The findings suggest a shift in the deformation mechanism from dislocation glide to dislocation climb in the sample irradiated to 6 dpa at 400 °C.

Large heat-to-heat variation of creep rupture strength in weldments of mod.9Cr-1Mo steels was observed in the creep rupture tests conducted for two different heats at 600°C and 650°C. One heat showed consistently lower time-to-rupture than the other for 130-60MPa at 600°C. Detailed microstructural investigations revealed that the number density of precipitates in the weaker heat was remarkably lower than that associated with the stronger heat through most of the creep region. Accordingly, heat-to-heat variation of creep rupture strength was attributed to the difference in the precipitate strengthening effects throughout creep. Equilibrium calculation predicted that the smaller phase fraction of M 23 C 6 and VN precipitates due to the lower content of chromium and lower ratio of nitrogen/aluminum in the weaker heat. However, given that long-term creep rupture strength at 650°C converged for the two heats, the microstructure including precipitates may settle into a similar level for subsequent longer hours even at 600°C.

The Advanced Materials and Manufacturing Technologies (AMMT) program is aiming at the accelerated incorporation of new materials and manufacturing technologies into nuclear-related systems. Complex Ni-based components fabricated by laser powder bed fusion (LPBF) could enable operating temperatures at T > 700°C in aggressive environments such as molten salts or liquid metals. However, available mechanical properties data relevant to material qualification remains limited, in particular for Ni-based alloys routinely fabricated by LPBF such as IN718 (Ni- 19Cr-18Fe-5Nb-3Mo) and Haynes 282 (Ni-20Cr-10Co-8.5Mo-2.1Ti-1.5Al). Creep testing was conducted on LPBF 718 at 600°C and 650°C and on LPBF 282 at 750°C. finding that the creep strength of the two alloys was close to that of wrought counterparts. with lower ductility at rupture. Heat treatments were tailored to the LPBF-specific microstructure to achieve grain recrystallization and form strengthening γ' precipitates for LPBF 282 and γ' and γ" precipitates for LPBF 718. In-situ data generated during printing and ex-situ X-ray computed tomography (XCT) scans were used to correlate the creep properties of LPBF 282 to the material flaw distribution. In- situ data revealed that spatter particles are the potential causes for flaws formation in LPBF 282. with significant variation between rods based on their location on the build plate. XCT scans revealed the formation of a larger number of creep flaws after testing in the specimens with a higher initial flaw density. which led to a lower ductility for the specimen.

This study examines the corrosion resistance of additively manufactured 316L stainless steel (SS) for nuclear applications across three environments: pressurized water reactor primary water (PWR PW), hot concentrated nitric acid, and seawater. Wire-feed laser additive manufacturing (WLAM) specimens showed oxidation behavior similar to wrought 316L SS in PWR PW, though stress corrosion cracking (SCC) susceptibility varied with heat treatment. In nitric acid testing, laser powder bed fusion (L-PBF) specimens demonstrated superior corrosion resistance compared to conventional SS, primarily due to improved intergranular corrosion resistance resulting from cleaner feedstock powder and rapid solidification rates that minimized grain boundary segregation. Laser metal deposition (LMD) repair studies in seawater environments successfully produced dense, crack-free repairs with good metallurgical bonding that matched the substrate’s mechanical properties while maintaining corrosion resistance. These results emphasize the importance of corrosion testing for additively manufactured components and understanding how their unique microstructures affect performance.