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At least 73 records · Page 4

Microstructural Characterization of Alloy 617 Crept into the Tertiary Regime

The microstructure of Alloy 617 was characterized following creep tests interrupted at total creep strains ranging from 2-20%. A range of creep temperatures (750-1000oC) and initial creep stresses (10-145 MPa) produced creep test durations ranging from 1 to 5800 hours. Image analysis of optical photomicrographs on longitudinal sections of the gage length was used to document the fraction of creep porosity as a function of creep parameters. Creep porosity was negligible below tertiary creep strains of 10% and increased with tertiary creep strain, thereafter. For a given temperature and total creep strain, creep porosity increased with decreasing creep stress. Creep porosity increased linearly with duration of the creep experiment. TEM performed on the gage sections did not reveal significant creep cavity formation on grain boundaries at the sub-micron level. It was concluded that the onset of tertiary creep did not result from creep cavitation and more likely arose due to the formation of low energy dislocation substructures with increasing tertiary strain.

Alloy 617↗

Microstructural Characterization of the Second High Fluence Baffle-Former Bolt Retrieved from a Westinghouse Two-loop Downflow Type PWR

As one of the pressurized water reactor (PWR) internal components, baffle-former bolts (BFBs) are subjected to significant mechanical stress and neutron irradiation from the reactor core during the plant operation. Over the long operation period, these conditions lead to potential degradation and reduced load-carrying capacity of the bolts. In support of evaluating long-term operational performance of materials used in core internal components, the Oak Ridge National Laboratory (ORNL), through the Department of Energy (DOE), Light Water Reactor Sustainability (LWRS) Program, Materials Research Pathway (MRP) has harvested two high fluence BFBs from a commercial Westinghouse two-loop downflow type PWR. The two bolts of interest, i.e. bolts # 4412 and 4416, were withdrawn from service in 2011 as part of a preventative replacement plan. No identification of cracking or potential damage was found for these bolts during their removal in 2011. However, the bolts required a lower torque for removal from the baffle structure than the original torque specified during installation. Irradiation displacement damage levels in the bolts range from 15 to 41 displacements per atom. The goal of this project is to perform detailed microstructural and mechanical property characterization of BFBs following in-service exposures. The information from these bolts will be integral to the LWRS program initiatives in evaluating end of life microstructure and properties. Furthermore, valuable data will be obtained that can be incorporated into model predictions of long-term irradiation behavior and compared to results obtained in high flux experimental reactor conditions. In this report, we present our latest study in FY22 on microstructural characterizations of the second high fluence baffle-former bolt, i.e., bolt # 4412. Analytical electron microscopy and atom probe tomography characterization were performed. The radiation-induced defects in the material add to the large wealth of knowledge for neutron-induced defects in 304/316 grades of stainless steels, specifically for radiation-induced precipitation after high fluence commercial PWR irradiation. The main findings are summarized as follows: 1) The cavity size was considerably larger in the bolt thread section than in the bolt head, with the bolt thread section having a bimodal distribution of cavities greater than ~6 nm in diameter and less than ~3 nm in diameter. The bolt head only had the small-sized cavities. In addition, there was a denuded zone of large cavities near grain boundaries in the thread section of the bolt. 2) Radiation-induced precipitation in the BFB #4412 was highly complex, with the volume fraction, size, and number density of Ni/Si and Cu-rich precipitates depending strongly on the radiation temperature/dose. In many cases, co-precipitates of adjoined clusters were found with Ni/Si-rich precipitates sandwiched between Cu-rich clusters and Mo/Cr/P-rich clusters. 3) Solute segregation out of solution was highest for most solutes in the thread section of the bolt #4412 with the exception of Cu, which experienced more separation out of solution into Curich clusters in the bolt head section. This highlights the difference in the mechanisms for precipitation of Ni/Si clusters, which have the Ni 3 Si phase composition, and precipitation of Cu-rich clusters. 4) There appear to be multiple simultaneous influences that affect the microstructural variation along the length of the bolt that overcomes the ~2X difference in irradiation dose between the bolt head and the bolt thread. The irradiation temperature, thermal/fast neutron ratio variation, potential strain gradient, and exposure to PWR coolant water that each section of the bolt sees may have more influence on the microstructural evolution than the total irradiation dose. The bolt thread and shank, with higher temperature, higher relative fast neutron flux, higher strain, and exposure to coolant but lower dose, underwent more enhanced cavity formation, precipitation, and solute segregation than the bolt head section.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

Microstructural characterization and comparison of Ti-6Al-4V manufactured with different additive manufacturing processes

In this work, the microstructures of Ti-6Al-4V manufactured by different additive manufacturing (AM) processes have been characterized and compared. The microstructural features that were characterized are the α lath thickness, grain boundary α (GB-α) thickness, prior β grain size and α colony size. In addition, the microhardnesses were also measured and compared. The microstructure of shaped metal deposited (SMD) Ti-6Al-4V material showed the smallest variations in α lath size, whereas the material manufactured with laser metal wire deposition-0 (LMwD-0) showed the largest variation. The prior β grain size was found to be smaller in material manufactured with powder bed fusion (PBF) as compared with corresponding material manufactured with the directed energy deposition (DED) processes. Parallel bands were only observed in materials manufactured with DED processes while being non-present in material manufactured with PBF processes.

36 MATERIALS SCIENCE↗

Microstructure Characterization of Fiber Laser Welds of S690QL High-Strength Steels

The use of fiber laser welding to join S690QL steels has attracted interest in the field of construction and assembly. Herein, 13-mm-thick S690QL welded joints were obtained without filler materials using the fiber laser. The as-welded microstructures and the impact energies of the joints were characterized and measured using electron microscopy in conjunction with high-resolution transmission electron images, X-ray diffraction, and impact tests. The results indicated that a single-sided welding technique could be used to join S690QL steels up to a thickness of 12 mm (fail to fuse the joint in the root) when the laser power is equal to 12 kW (scan speed 1 m/min). Double-side welding technique allows better weld penetration and better control of heat distribution. Observation of the samples showed that the fusion zone exhibited bainitic and martensitic microstructures with increased amounts of martensites (Ms) compared with the base materials. Also, the grains in the fusion zone increased in coarseness as the heat input was increased. The fusion zone exhibited increased hardness (397 HV{sub 0.2}) while exhibiting a simultaneous decrease in the impact toughness. The maximum impact energy value of 26 J was obtained from the single-side-welded sample, which is greater than those obtained from the double-side-welded samples (maximum of 18 J). Many more dislocations and plastic deformations were found in the fusion zone than the heat-affected zone in the joint, which hardened the joints and lowered the impact toughness. The microstructures characterized by FTEM–energy-dispersive X-ray spectrometer also exhibited laths of M, as well as stacking faults and dislocations featuring high-density, interfacial structure ledges that occur between the high-angle grain boundaries and the M and bainite.

36 MATERIALS SCIENCE↗

Microstructural Characterization of FeCrAl C26M Tubes

The present report summarizes the initial nanoindentation characterization of a FeCrAl alloy, C26M. Microstructural analysis using electron backscatter diffraction showed a highly textured system with the axial surface favoring orientations near the [110] and the longitudinal surface near the [111]. A large spread of grain sizes was observed from a few μm’s to 100 μm with an average grain size of ~70 μm. Nanoindentation with a Berkovich tip measured a similar hardness and modulus of ~4.4 GPa and ~240 GPa on the two surfaces, respectively. Mounting specimens in epoxy was found to be the cause of a lower stiffness and, consequently, a lower hardness and modulus value. Spherical nanoindentation was measured on the longitudinal surface of the tube to determine the nanoindentation modulus and nanoindentation yield strength. Using a 10 μm tip, the measured modulus was ~220 GPa and the yield strength was ~1.4 GPa. Indentation with a 100 μm tip resulted in a measured modulus value of ~220 GPa and yield strength of ~1.1 GPa. Some early characterization of the differences in spherical nanoindentation response of the axial and longitudinal surfaces showed a small difference between the two, but a more detailed analysis with a stiffer mounting configuration is needed to draw conclusions.

36 MATERIALS SCIENCE↗

Report on initial development of a database of nuclear graphite characteristics based on microstructural characterization

This report outlines the current and future efforts to produce a comprehensive library of microstructures of nuclear graphite and carbon-based materials that are candidate materials for nuclear applications in the United States. This library must contain extensive characterizations of unirradiated graphite materials, a guide to some of the techniques used to characterize graphite, a compendium of characterization data of neutron-irradiated or oxidized material, and a compendium of microstructural information of carbon-based materials. These characterization efforts are being conducted at various length scales to understand these complex materials’ local structure and property relationships. Achieving this goal requires further developing or adapting advanced characterization techniques that capture graphite’s most relevant characteristics. Some of the general objectives of this project are to aid with the material selection, licensing, management, and core assessments of a graphite core by documenting the unirradiated microstructure of relevant grades or by characterizing the evolution of the microstructure under the reactor environment. Moreover, this project aims to provide additional information, guidelines for characterizing graphite, and a protocol to assess a nuclear graphite grade. This report also summarizes some of the initial results and some of the techniques commonly used to characterize nuclear graphite.

36 MATERIALS SCIENCE↗

Microstructural characterization of U-20Pu-10Zr-4Sb and U-20Pu-10Zr-4Sb-4Ln

Antimony is being investigated as a potential additive to metallic fuel to control fuel-cladding chemical interactions (FCCI). The most detrimental elements involved in FCCI are fission product lanthanides, leading to brittle intermetallics and low melting eutectic phases. Previous investigations of Sb as an additive focused on U-10Zr, in wt. %, as the fuel. The current investigation expands that to include Pu in the fuel. Here, two alloys, U-20Pu-10Zr-4Sb and U-20Pu-10Zr-4Sb-4Ln (wt. %, Ln=53Nd-25Ce-16Pr-6La) have been investigated using scanning electron microscopy (SEM) and transmission electron microscopy (TEM) to characterize the fuel as-cast microstructure and the microstructure after introduction of lanthanides. Sb reacts with Zr initially, forming Zr 2 Sb and Zr 5 Sb 3 , with as much as 20 at. % interstitial Pu present. In the presence of lanthanides, Sb forms Ln 4 Sb 3 with the lanthanides, containing ~14 at. % Pu. The Pu is substitutional for the lanthanides in the crystal lattice.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Microstructural characterization of plutonium oxalate and oxide particles by three-dimensional focused ion beam tomography

Focused ion beam (FIB) tomography was used to characterize three-dimensional (3D) internal microstructures of plutonium oxalate and oxide particles. Sequential two-dimensional (2D) sectioning and imaging using FIB and 3D image reconstruction were used to elucidate and distinguish internal pore microstructure and distribution in plutonium oxide particles calcined from plutonium oxalate precipitates. The results show that the plutonium oxide particles have a significant increase in pore volume fraction while retaining the exterior morphological shape of the corresponding oxalate precipitates. This technique enables the examination of the internal structure of radioactive microparticles for nuclear forensics that is not available with conventional microscopy.

36 MATERIALS SCIENCE↗

Microstructural Characterization of A709 Commercial Heats with Precipitation Treatment

This report discusses work conducted at Idaho National Laboratory in fiscal year 2022 associated with the precipitates in Alloy 709 (A709). The purpose of this work is to support the development of the A709 Code Cases to qualify A709 in Section III, Division 5 of the American Society of Mechanical Engineers Boiler and Pressure Vessel Code. This would permit the use of A709 for elevated-temperature nuclear construction. This work encompassed two broad goals. The first goal was to understand the microstructure of the second commercial heat of plate A709 purchased through the Advanced Reactors Technologies Program in both the solution-annealed and precipitation-treated conditions. Transmission electron microscopy was utilized to characterize these microstructures. Direct comparisons were then made between the solution-annealed and precipitation-treated conditions as well as between the first and second commercial heats of plate A709. The second goal was to understand the impact of variations in the time and temperature of the precipitation treatment on the properties of A709. The precipitation treatment temperature was varied from 750°C to 800°C for times ranging from 3 hours to 30 hours. The hardness of each precipitation treatment variation was measured. All of the precipitation treatment variations investigated besides a specimen from the second commercial heat of plate A709 precipitation treated at 800? for 9 hours met the room-temperature hardness requirement specified in ASTM A213 and SA-213 for UNS S31025. The hardness measured for the specimen from the second commercial heat of plate A709 that was precipitation treated at 800? for 9 hours is considered an outlier. The next step is to look at the extremes of the precipitation treatment variations investigated and conduct elevated-temperature mechanical testing. The purpose of this testing would be to assess if these time and temperature variations have any impact on the mechanical performance.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Microstructural characterization of laser metal powder deposited Alloy 718

Highlights: • In as-deposited condition γ′ and γ″ were found in the interdendritic regions. • JMatPro simulations confirmed accelerated precipitation in interdendritic regions. • Depletion of Niobium was still found in the dendritic core after heat treatment. • The depletion of Niobium were more noticeable when using a high heat input. • γ″ particles were less well-developed in the regions depleted of Niobium. - Abstract: A microstructural study of Laser Metal Powder Deposition (LMPD) of Alloy 718, using a low (40 J/mm) and high (100 J/mm) heat inputs (HIs) was performed. The microstructure was characterized in as-deposited condition as well as after a standard heat-treatment, using optical microscope (OM), scanning electron microscope (SEM) and Transmission Electron Microscope (TEM). Laves, MC-carbides, γ′ and γ″ are observed in the interdendritic areas of both conditions. However, the dendritic core only consists of γ-matrix. The high HI condition shows a slightly larger Primary Dendrite Arm Spacing (PDAS) as compared to the low HI condition. Additionally, the particle size of the Nb-rich constituents in the interdendritic regions (Laves-phase and Niobium carbide) is larger in the high HI sample. After heat-treatment, the Laves phase dissolves and is replaced by δ-phase in the interdendritic regions, while γ′, γ″ and MC-carbide remain in the interdendritic regions. However, the γ″ precipitates seems to be less developed in the dendritic core as compared to the interdendritic regions, especially in the high HI sample. This can be attributed to a heterogeneous distribution of Nb in the microstructure, with a lower Nb content in the dendritic core as compared to close to the interdendritic regions.

36 MATERIALS SCIENCE↗

Microstructural Characterization of Irradiated U{sub 0.17}ZrH{sub 1.6} Using Ultrasonic Techniques

In recent years, there has been an increased level of effort to understand the changes in microstructure that occur due to irradiation of nuclear fuel. The primary driver for this increased effort is the potential for designing new fuels that are safer and more reliable, in turn enabling new and improved reactor technologies. Much of the data on microstructural change in irradiated fuels is generated through a host of post irradiation examination techniques such as optical microscopy (OM), scanning electron microscopy (SEM), and transmission electron microscopy (TEM) to determine grain structure, porosity, crack geometry, etc. in irradiated fuels. Such 'traditional' examination techniques were recently used to characterize a novel new fuel consisting of U{sub 0.17}ZrH{sub 1.6} pellets bonded to zircaloy-2 cladded with lead-bismuth eutectic before and after irradiation. In addition to the conventional suite of post-irradiation examination tools, several nondestructive interrogation techniques exist which bring the potential for in-situ assessment of microstructural changes. One such method, ultrasonic examination, was tested on each of the samples. This paper describes the results of this examination. Ultrasonic measurements have a long and successful history of use for nondestructive materials characterization, including nondestructive evaluation (NDE) of degradation and damage, microstructure characterization, and measurement of physical parameters for process control. Ultrasonic NDE is critical to the nuclear power industry's in-service inspection program for maintaining pressure boundary integrity, and is being actively investigated for PIE of fuels. Ultrasonic measurements, typically performed at 10 MHz or higher, performed post irradiation show that fuel microstructural parameters, such as porosity and grain size, can be correlated to ultrasonic velocity. The objective of this examination was to assess the feasibility of using ultrasonic measurements on irradiated fuel to determine sensitivity to microstructural changes.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Microstructure characterization of laser welded Ti-6Al-4V fusion zones

The as-welded microstructure of laser-welded Ti-6Al-4V is characterized as a function of CO2 key-hole mode laser welding speed. Martensitic α′ is the predominant phase, with some α and retained β. Phase transformation is affected by the cooling rate through laser welding speed. A higher welding speed of 1.6 to 2.0 m/min produced more martensite α′ and less retained β in the welds. 1.4 m/min welding speed produced small amounts of α, besides the martensite α′. A trace of δ titanium hydride phase seems to have formed in the weld fusion zone. Moiré fringes are a common feature in the TEM microstructure, due to abundance of multi-phase interfaces. Tensile twins and clusters of dislocations indicate that plastic deformation has happened in the as-welded microstructure, indicating the local stress levels to be approaching the yield stress on-cooling during laser welding.

36 MATERIALS SCIENCE↗

Dissimilar Metal Weld Joints of P91/Ni Alloy: Microstructural Characterization of HAZ of P91 and Stress Analysis at the Weld Interfaces

Microstructure evolution and hardness were evaluated at the interface of two friction-welded transition joints between P91 and AISI 304 fabricated applying Inconel interlayers, viz. single-interlayer weld (P91/IN600/AISI304) and three-interlayer weld (P91/IN625/IN600/IN800H/AISI304). The welds were subjected to post-weld heat treatment at 1023 K for 1 h followed by air cooling and a long-term exposure at 973 K for 100, 250, and 500 h. A soft zone with the absence of lath martensite was noticed in both the welds which was located at the intercritical heat-affected zone of the welds. This zone was found to be extending with time toward the fine grain heat-affected zone by carbide precipitation and coarsening at the grain boundaries. Soft zone formation at the interface of the welds was found to be due to carbon diffusion. The presence of high-nickel-content alloy at the interface was proven to be beneficial in stopping carbon diffusion at the interface. Though soft zones existed in both the welds, better creep rupture life was observed for three-interlayer welds. Finite element analysis of these weld joints was performed for thermal loading followed by tensile loading. The results from this analysis indicated that thermal expansion also plays an important role in the failures of these dissimilar weld joints by creating high stress at the interface due to incompatibility.

36 MATERIALS SCIENCE↗

Microstructure characterization of heat affected zone after welding in Mod.9Cr–1Mo steel

The microstructure of the heat affected zone after welding was investigated in Mod.9Cr–1Mo steel, using TEM and STEM-EDX. The microstructure of thin foil was observed at the fusion line, and at the positions of 0.5 mm, 1.0 mm, 1.5 mm, 2.0 mm, 2.5 mm, 3.0 mm and 3.5 mm to the base metal side of the fusion line. Martensite structure with very fine lath and high dislocation density was confirmed at all positions. Twins with a twin plane of (112) were locally observed at all positions. Elemental mapping was obtained for all positions by means of STEM-EDX. Inclusions of mainly Si were formed at the fusion line but not at the other positions. No precipitates could be detected at the fusion line or at the position of 0.5 mm. On the other hand, MX particles were observed at the positions of 1.0 mm, 1.5 mm, 2.0 mm, 2.5 mm, 3.0 mm and 3.5 mm even after welding. M{sub 23}C{sub 6} particles were also confirmed at the positions of 2.0 mm, 2.5 mm, 3.0 mm and 3.5 mm. Very fine equiaxed grains were locally observed at the positions of 2.0 mm and 2.5 mm. The Cr content of the equiaxed grains was about 12 mass%, although the martensite area included about 8 mass% Cr. - Graphical abstract: Display Omitted - Highlights: • Nonequilibrium microstructure of heat affected zone was observed after welding in Mod.9Cr–1Mo steel. • Inclusions containing Si were detected at the fusion line. • Undissolved M{sub 23}C{sub 6} and MX particles were confirmed in heat affected zone. • Twins with a twin plane of (112) were locally observed at all positions. • Very fine ferrite grains with high Cr content were observed in fine grained heat affected zone.

36 MATERIALS SCIENCE↗

Formation Mechanisms and Microstructure Characterization of Al/Al{sub 3}Ni In-situ Composite by Compound Casting

The Compound casting method was used to produce an Al/Ni bimetal composite. The mechanisms of formation of the reinforcing intermetallic phases were studied and the produced bimetal composite’s microstructure was then characterized. The results showed that the Al/Ni interface consisted of two intermetallic layers including Al{sub 3}Ni{sub 2} and Al{sub 3}Ni. It is suggested that the Al{sub 3}Ni reinforcing particles of the composite originated from two sources. (1) Some Al{sub 3}Ni particles detached from the Al{sub 3}Ni layer formed at the interface between the Ni core and the Al melt and dispersed in the liquid Al and (2) Al-Al{sub 3}Ni eutectic phase, which formed during the solidification process. The increase in the temperature led to the formation of more reinforcing particles and extended the depth of dispersion of the particles in the Al matrix.

36 MATERIALS SCIENCE↗

Microstructural characterization of an SA508–309L/308L–316L domestic dissimilar metal welded safe-end joint

The microstructure of an SA508–309L/308L–316L domestic dissimilar metal welded safe-end joint was characterized in this work by optical microscopy, scanning electron microscopy (with electron back scattering diffraction) and micro-hardness testing. Epitaxial growth and competitive growth are evident in the 308L–316L fusion boundary regions. A martensite layer, carbon-depleted zones, and type-II and type-I boundaries are found in the SA508–309L fusion boundary regions, while only martensite and austenite mixed zones are observed in the SA508–308L fusion boundary regions. The microstructure near the fusion boundary and the microstructure transition in the SA508 heat affected zone are quite complex. Both for SA508–309L/308L and 308L–316L, the highest residual strain is located on the outside of the weldment. The residual strain and the grain boundary character distribution change with increasing distance from the fusion boundary in the heat affected zone of 316L. Micro-hardness measurements also reveal non-uniform mechanical properties across the weldment. - Highlights: • The microstructure of SA508 HAZ, especially near the FB, is very complex. • The outside of the dissimilar metal welded joint has the highest residual. • The micro-hardness distributions along the DMWJ are non-uniform.

36 MATERIALS SCIENCE↗

Microstructural characterization of a new mechanically alloyed Ni-base ODS superalloy powder

The microstructure of a new Ni-base oxide dispersion strengthened superalloy powder was studied for high temperature gas turbine applications after the mechanical alloying process. In this study, an atomized powder with a composition similar to the CMSX-10 superalloy was mechanically alloyed with yttria and Hf powders. The mechanically alloyed powder included only the supersaturated solid solution γ phase without γ′ and yttria provided by severe plastic deformation, while after the 3-step aging, the γ′ phase was precipitated due to the partitioning of Al and Ta to the γ′ and Co, Cr, Re, W, and Mo to the γ phase. Mechanical alloying modified the morphology of γ′ to the new coherent γ–γ′ nanoscale lamellar structure to minimize the elastic strain energy of the precipitation, which yielded a low lattice misfit of 0.16% at high temperature. The γ′ lamellae aligned preferentially along the elastically soft [100] direction. Also, the precipitated oxide particles were refined in the γ phase by adding Hf from large incoherent YAlO{sub 3} to fine semi-coherent Y{sub 2}Hf{sub 2}O{sub 7} oxide particles with the average size of 7 nm and low interparticle spacing of 76 nm. - Highlights: • A new Ni-base ODS superalloy powder was produced by mechanical alloying. • The nanoscale γ–γ′ lamellar structure was precipitated after the aging treatment. • Fine semi-coherent Y{sub 2}Hf{sub 2}O{sub 7} oxide particles were precipitated by addition of Hf.

36 MATERIALS SCIENCE↗

Microstructural characterization of dissimilar welds between Incoloy 800H and 321 Austenitic Stainless Steel

In this work, the microstructural character of dissimilar welds between Incoloy 800H and 321 Stainless Steel has been discussed. The microscopic examination of the base metals, fusion zones and interfaces was characterized using an optical microscope and scanning electron microscopy. The results revealed precipitates of Ti (C, N) in the austenitic matrix along the grain boundaries of the base metals. Migration of grain boundaries in the Inconel 82 weld metal was very extensive when compared to Inconel 617 weldment. Epitaxial growth was observed in the 617 weldment which increases the strength and ductility of the weld metal. Unmixed zone near the fusion line between 321 Stainless Steel and Inconel 82 weld metal was identified. From the results, it has been concluded that Inconel 617 filler metal is a preferable choice for the joint between Incoloy 800H and 321 Stainless Steel. - Highlights: • Failure mechanisms produced by dissimilar welding of Incoloy 800H to AISI 321SS • Influence of filler wire on microstructure properties • Contemplative comparisons of metallurgical aspects of these weldments • Microstructure and chemical studies including metallography, SEM–EDS • EDS-line scan study at interface.

36 MATERIALS SCIENCE↗