Laser based powder bed fusion (LPBF) and powder metallurgy via hot isostatic pressing (PM-HIP) are advanced manufacturing technologies for nuclear components. In the present study, stress corrosion crack (SCC) initiation susceptibility of LPBF 316L stainless steel post-treated by HIP, PM-HIP 316L and also wrought 316L specimens were evaluated in three typical light water reactor environments by U-bend testing and post-exposure characterizations. Results show that LPBF-HIP and PM-HIP 316L have lower SCC susceptibility compared to their wrought counterparts in the selected environments tested. The mechanisms for SCC behavior of samples were discussed.
The present study reports on the structure formation in thin epitaxial nickel-aluminum films (Ni1-xAlx; Al atomic fraction up to ) grown on MgO substrates by magnetron sputtering. Experimental and computational data demonstrate that for , the films exhibit the face-centered cubic random solid-solution Ni1-xAlx structure ( phase). Whereas in the range x = 0.11-0.24 the phase coexists with the ordered structure ( phase). The two phases are homogenously intermixed forming a strained coherent nanocomposite, which exhibits a single lattice parameter that expands as the Al content increases. Isothermal annealing of films containing of Al, coupled with structural and nano-mechanical characterization, reveal that the coherent nanocomposite retains its overall integrity for temperatures up to 673 K while the film hardness increases from (as deposited films) to . Further increase of the annealing temperature to 873 K and 1073 K causes the coherent nanocomposite to dissolve into distinct and phase domains and the hardness to decrease down to values of . These findings confirm the metastable nature of the as-deposited thin Ni1-xAlx alloy films and underpin the effectiveness of high supersaturation/undercooling for creating non-equilibrium phases and self-organized nanostructures upon synthesis of multicomponent materials.
Additively manufactured (AM) stainless steels (SS) are under consideration for molten salt reactors. However, molten salt corrosion of AM SS remains poorly understood. Here we present the mechanisms of corrosion of laser-based powder bed fused (LPBF) 316L SS in FLiNaK + 5 wt. % EuF3 molten salt at 650 °C. Microstructural features of dislocation cells, low-angle grain boundaries, and carbides appear to be the major underlying features influencing corrosion behavior. Corrosion-induced, salt-filled voids follow {100} crystallographic planes rather than AM-induced microstructural features. Dislocation cell structures retain Cr, and yet they appear to slow molten salt corrosion in the long run, with limited grain boundary migration observed. Larger Cr carbides disappear in the salt penetration regions, leaving only Mo carbides. Smaller carbides and remaining high Ni-enrichment layer slow down Cr depletion and molten salt penetration.
Constant-displacement bolt-loaded compact tension specimens of Nickel-based Alloy 52 were exposed to boiling water reactor environment for 12 years, followed by an additional 3 years in post-shutdown cold water conditions in a Swedish nuclear power plant test loop, under a stress intensity factor of 20 MPa root m. After outer surface decontamination and specimen opening, unexpected crack extensions of 3-4.5 mm were observed. The fracture surface and the cross-sectional deformation microstructure were examined by electron microscopies techniques down to the nanoscale. The oxide layer in the region exhibiting unexpected crack growth was notably thin, suggesting that it formed after exposure to elevated operating temperatures. The dominant fracture mode is transgranular, propagating along close-packed {111} planes. The grains contained heterogeneous microstructures with regions enriched in nanometer-sized Ti(N,C) and the zigzag crack paths did not traverse these regions strengthened areas. Extensive shear bands were present near the crack tips, indicating pronounced localized plasticity. Hydrogen reduces stacking fault energy, results in localized plasticity and enhances shear bands formation. Low temperature crack propagation with evident effects of hydrogen was considered as the potential cause of crack propagation in Alloy 52 in the absence of external dynamic loading under post-shutdown cold water chemistry.
The impact of 160 keV Ne ion irradiation on TRISO fuel surrogate samples was investigated, focusing on structural transformations in the buffer, transition, and the IPyC layers. Using various TEM techniques we analyzed the structural changes in the vicinity of the buffer-IPyC interface. The anisotropy texture analysis was based on the orientation distribution of the carbon (002) planes, determined from angular intensity variations along the (002) diffraction rings in SAED patterns, for both unirradiated and irradiated buffer, transition, and IPyC layers. We observed increasing texture up to 25-35 DPA followed by amorphization above 35-40 DPA. Using energy dispersive spectroscopy we observed a distinctive double peak in the Ne concentration profile within the buffer layer. The results indicate that the structure evolves significantly during irradiation and that these changes likely induce different ion penetration depths resulting abnormal Ne concentration profile. SRIM simulations provide complementary insights into the depth-dependent Ne concentration and DPA profiles. This research highlights the significant structural changes induced by Ne ion irradiation and the unique characteristics of the buffer layer’s response.
The laser powder bed fused (LPBFed) stainless steels showed anomalous and localized corrosion behavior in the nuclear reactor high-temperature water compared to their wrought counterparts, which affects their performance during plant operation. In this study, advanced microstructural characterization was performed on LPBFed 316 L sample along with wrought 316 L sample after corrosion tests to understand the underlying mechanisms. The results showed that an inhomogeneous/discontinuous inner oxide layer formed on LPBFed 316 L, in contrast to the continuous inner oxide layer on the wrought 316 L specimen. This discontinuous inner oxide layer was identified to consist of Cr-enriched nano-sized spinel oxide and the barrier layer features a Ni-enriched hexagonal close-packed Laves phase. Localized/preferential oxidation was found to occur along the cellular walls which were tangled with high density dislocations and decorated with Mn and Si-enriched nano-sized precipitates, and the nano-precipitates were observed in the core of dispersed Cr-enriched inner oxide crystals.
A full-scale dissimilar metal weld safe-end mock-up, precisely replicating a critical component of a modern nuclear power plant, was investigated. The brittle fracture behavior, carbide evolution and nanoscale elemental segregation in the heat-affected zone (HAZ) of low alloy steel (LAS) were analyzed under both post-weld heattreated and thermally-aged conditions (400 degrees C for 15,000 h, equivalent to 90 years of operation) using analytical electron microscopy and atom probe tomography. The observed increase in grain boundary (GB) decohesion and intergranular cracking on the fracture surface and the decrease of fracture toughness are primarily attributed to P and Mn segregation to GBs and the coarsening of carbides upon long-term thermal aging. The direct observations of significant elemental segregation to GBs and the consequent reduction in fracture toughness in the HAZ are unexpected for modern low-phosphorus LASs, highlighting potential concerns for evaluating the structural integrity of modern nuclear power plants.
The electrochemical behavior of laser powder bed fusion (LPBF) 316 L stainless steel subject to different heat-treatments (solution annealing and hot isostatic pressing) is compared to nuclear-grade wrought 316 L in pressurized water reactor primary water at 288 degrees C (with and without dissolved hydrogen) using current-time transients, cyclic voltammetry and electrochemical impedance spectroscopy (EIS). Analysis of spectra by the Mixed-Conduction Model revealed slower corrosion rates of LPBF 316 L than wrought 316 L, the effect being more pronounced in the presence of dissolved hydrogen. The characteristics of the barrier layer and the oxide film/coolant interface were irreversibly altered upon removal of dissolved hydrogen.
A SA508/Alloy 52 dissimilar metal weld (DMW) mock-up with double-sided Alloy 52 butterings, which is fully representative of Ringhals pressurizer surge nozzle DMW repair solution, was studied. The microstructure, crystal structure, elemental diffusion, carbide formation and macro-, micro-and nano-hardness of the SA508/ nickel-base Alloy 52 buttering fusion boundary (FB) were investigated. Three types of FBs were analyzed, i.e., narrow FB (-80-85% of whole FB), tempered martensitic transition region (-15%) and wide partially mixed zone (-1-2%). The different FB types were induced by the local heat flow and respective elementary diffusion, which significantly influence the local hardness mismatch across the DMW interface and the local brittle fracture behavior.
A narrow-gap SA508/Alloy 52 dissimilar metal weld (DMW) mock-up, fully representative of an actual nuclear component, was investigated in this work. The microstructure and carbides formed in the low alloy steel fusion boundary (FB) and heat affected zone (HAZ) can act as brittle fracture initiators and could influence the brittle fracture behavior. However, the amount of information available in the open literature on the microstructural changes and carbide formation in DMW occurring upon post-weld heat treatment and long-term thermal aging is very limited. The microstructure and carbide type, morphology and size in the carbide precipitation zone (CPZ, up to 1.5 ??m from FB), carbon depletion zone (CDZ, up to 40???50 ??m from FB) and HAZ (up to 2 mm from FB) of the plant-relevant DMW in post-weld heat-treated and thermally-aged (400 ???C for 15,000 h, corresponding to 90 years of operation) conditions were analyzed with analytical electron microscopy, wide-angle X-ray scattering and atom probe tomography. Long-term thermal aging increases the microhardness peak close to the FB, triples the width of the CPZ and coarsens the carbide size in the HAZ (up to a magnitude). There is no evidence of a significant phosphorus segregation to grain boundaries due to thermal aging.
Nanocellulose is increasingly proposed as a sustainable raw material having strong interparticle bonding. However, cellulose alone has limited bending and impact resistance. We newly observe self-assembly between crystalline nanocellulose (CNC) and ultrafine ground chemical-free calcium carbonate nanoparticles (UGCC). The suspension displays an intrinsic gel-like state, and heterogeneous adsorption occurs under the specific conditions where Brownian motion of both species is arrested by application of ultralow shear (0.01 s−1). In contrast, simple static aging of the mixture leads to autoflocculation of each species independently. The heterogeneous adsorption results in compound particle self-assembly leading to multi-level hierarchical structures depending on relative species size and concentration ratio. Fine particles from species 1 adsorb onto the coarser complementary particles of species 2 and vice versa. Depending also on whether CNC or UGCC particles are in excess, the structural assembly occurs primarily through either CNC–CNC hydrogen bonding or CaCO3–CaCO3 autogenous flocculation, respectively. Controlling the hierarchical composite structure bonding in this way, the resulting morphology can express dual or predominantly single either mineralic or cellulosic surface properties. Novel complex hybrid biocomposite materials can therefore be produced having designable compatibility across a broad range of both natural and oil-based polymeric materials. Both CNC and UGCC are exemplified here via commercial products.
Atomic layer deposition (ALD) was used to deposit a protective overcoating (Al2O3) on an industrially relevant Co-based Fischer-Tropsch catalyst. A trimethylaluminium/water (TMA/H2O) ALD process was used to prepare ∼0.7-2.2 nm overcoatings on an incipient wetness impregnated Co-Pt/TiO2 catalyst. A diffusion-reaction differential equation model was used to predict precursor transport and the resulting deposited overcoating surface coverage inside a catalyst particle. The model was validated against transmission electron (TEM) and scanning electron (SEM) microscopy studies. The prepared model utilised catalyst physical properties and ALD process parameters to estimate achieved overcoating thickness for 20 and 30 deposition cycles (1.36 and 2.04 nm respectively). The TEM analysis supported these estimates, with 1.29 ± 0.16 and 2.15 ± 0.29 nm average layer thicknesses. In addition to layer thickness estimation, the model was used to predict overcoating penetration into the porous catalyst. The model estimated a penetration depth of ∼19 μm, and cross-sectional scanning electron microscopy supported the prediction with a deepest penetration of 15-18 μm. The model successfully estimated the deepest penetration, however, the microscopy study showed penetration depth fluctuation between 0-18 μm, having an average of 9.6 μm.
Using common and high resolution transmission electron microscopy (TEM), we study the magnetic and crystal phase structures as well as their evolution in Ni50Mn25Ga20Fe5 magnetic shape memory material with high Curie point. The particular alloying by Fe and changing thickness of the TEM foil enable us to observe all martensitic phases known in Ni-Mn-Ga Heusler alloy system and their respective transitions simultaneously. Starting from cubic austenite at about 10 nm foil thickness, the structure evolves via peculiar interleaved stripes of austenite and five-layered modulated 10M martensite to pure 10M phase with a low density of stacking faults at 40 nm thickness. With further increasing thickness, the 10M phase transforms gradually to seven-layered modulated 14M martensite with an increased density of stacking faults. Finally, the non-modulated tetragonal NM phase appears within the 14M phase by detwinning of nanotwins forming the modulated phases. High resolution TEM further confirms that nanotwinning and stacking faults are inherent structure features tightly connected with the lattice modulation and intermartensite transformations. Overall, the evolution of average lattice shows the same general trend, an increasing simple shear with (1 (1) over bar0) shuffling plane, across the whole phase sequence. Additionally, we found large local variation of lattice parameters in all phases, which is is ascribed to strong lattice softening in the vicinity of the martensitic transformation and high density of stacking faults in 14M martensite lattice.
A non-equiatomic AlCoCr0.75Cu0.5FeNi alloy has been identified as a potential high strength alloy, whose microstructure and consequently properties can be widely varied. In this research, the phase structure, hardness, and magnetic properties of AlCoCr0.75Cu0.5FeNi alloy fabricated by laser powder bed fusion (LPBF) are investigated. The results demonstrate that laser power, scanning speed, and volumetric energy density (VED) contribute to different aspects in the formation of microstructure thus introducing alterations in the properties. Despite the different input parameters studied, all the as-built specimens exhibit the body-centered cubic (BCC) phase structure, with the homogeneous elemental distribution at the micron scale. A microhardness of up to 604.6 ± 6.8 HV0.05 is achieved owing to the rapidly solidified microstructure. Soft magnetic behavior is determined in all as-printed samples. The saturation magnetization (Ms) is dependent on the degree of spinodal decomposition, i.e., the higher degree of decomposition into A2 and B2 structure results in a larger Ms. The results introduce the possibility to control the degree of spinodal decomposition and thus the degree of magnetization by altering the input parameters of the LPBF process. The disclosed application potentiality of LPBF could benefit the development of new functional materials.
With the continued scenario of the COVID-19 pandemic, the world is still seeking out-of-the-box solutions to break its transmission cycle and contain the pandemic. There are different transmission routes for viruses, including indirect transmission via surfaces. To this end, we used two relevant viruses in our study. The severe acute respiratory syndrome coronavirus 2 (SARS-CoV-2) causing the pandemic and human norovirus (HuNV), both known to be transmitted via surfaces. Several nanoformulations have shown attempts to inhibit SARS-CoV-2 and other viruses. However, a rigorous, similar inactivation scheme to inactivate the cords of two tedious viruses (SARS-CoV-2 Alpha variant and HuNV) is lacking. The present study demonstrates the inactivation of the SARS-CoV-2 Alpha variant and the decrease in the murine norovirus (MNV, a surrogate to HuNV) load after only one minute of contact to surfaces including copper–silver (Cu–Ag) nanocomposites. We thoroughly examined the physicochemical characteristics of such plated surfaces using diverse microscopy tools and found that Cu was the dominanting element in the tested three different surfaces (~56, ~59, and ~48 wt%, respectively), hence likely playing the major role of Alpha and MNV inactivation followed by the Ag content (~28, ~13, and ~11 wt%, respectively). These findings suggest that the administration of such surfaces within highly congested places (e.g., schools, public transportations, public toilets, and hospital and live-stock reservoirs) could break the SARS-CoV-2 and HuNV transmission. We suggest such an administration after an in-depth examination of the in vitro (especially on skin cells) and in vivo toxicity of the nanocomposite formulations and surfaces while also standardizing the physicochemical parameters, testing protocols, and animal models.
Three possible twinning modes, Type I, Type II, and compound, as well as corresponding twin boundaries in 2H martensite of Cu69.4Ni3.4Al27.2 single crystal, were studied by X-ray diffraction (XRD) and high-resolution transmission electron microscopy (HRTEM). The results are discussed with regard to the sharply different twinning stress or twin-boundary mobility. In self-accommodated martensite, all three modes not only coexist but are crystallographically coupled. The compound twin boundary is a coherent coplanar mirror plane with the smallest twinning shear. The Type II twin boundary is also a coherent strain-free interface. The high index rational approximation of Type II twin boundary was determined by trace analysis with the help of stereographic projection. The approximation is in good agreement with irrational indices calculated from elastic continuum. The Type I boundary is the most complex interface associated with high stress and high density of stacking faults inside the twin bands. Using HRTEM, two different stressed boundaries of Type I were confirmed. The intrinsic twinning mode in Cu-Ni-Al alloy is the compound twinning. In compression, the Type II twinning is the major deformation twinning mode. During deformation the Type I twins are eliminated, leaving Type II twinning bands with compound twins. The observed differences between the atomic structure of different twin boundaries can contribute significantly to the sharp differences in twinning stress.
The entropy changes in successive martensitic phase transformations in Ni-Mn-Ga Heusler alloys can be used to realize enhanced magnetocaloric properties. A detailed study of phase transformations of one such alloy, Ni 2.15 Mn 0.85 Ga ( $\Delta Q =4900$ J/kg at 343 K, under 140 kOe), is reported here. Upon cooling, the paramagnetic cubic (L2 1 ) austenitic phase transforms into a ferromagnetic 7M modulated monoclinic martensitic phase. This phase is stable in a narrow temperature range, and upon further cooling, it transforms into a non-modulated ferromagnetic tetragonal (L1 0 ) phase. The separation between the equilibrium temperatures of the austenitic and tetragonal martensitic phases is only ~50 K. The alloy undergoes reversible temperature-induced martensitic and inter-martensitic phase transformations with thermal hysteresis of about 25 K. The conclusions from the detailed study of the phase transformations lead to new possibilities to enhance the magnetocaloric effect (MCE) using the entropy associated with multi-structural transformations.
An equiatomic CrFeNiMn alloy was consolidated using pulsed electric current sintering (PECS) from gas atomized (GA) powder. A range of sintering temperatures was applied to determine its impact on the received microstructure and material properties. It was found that the phase structure of the disc shape sintered samples varied greatly depending on the sintering temperature. According to X-ray diffraction (XRD) the surface of the samples contained a noticeable amount of BCC phase while in the middle of the sample cross sections no BCC phase was found. Ball milling of the gas atomized powder prior to sintering for 25 h increased the density and hardness of the sintered sample from 98.3% to 99% and from 200 HV to 300 HV, respectively. At the same time, the ultimate tensile strength increased from 700 MPa to 1000 MPa and the elongation at fracture decreased from 40% to 25%. The enhanced hardness and tensile strength were attributed to the grain refinement caused by milling the powder prior to sintering. Milling of the powder resulted in a reduction in grain size of the sintered material from 5.7 mu m to 1.9 mu m when sintered at 1100 degrees C for 5 min. The grain refinement was also found to affect the deformation mechanisms. While the deformation of the samples prepared directly from GA powder was accommodated by the cell-forming process and deformation twinning, milling refined the initial microstructure to such an extent that deformation twinning was suppressed. In summary, a single phase equiatomic CrFeNiMn alloy can be achieved by pulsed electric current sintering of gas atomized powder. Sintering at temperatures above 1100 degrees C results in a single-phase FCC structure excluding the surface of the samples. Milling of the starting powder increases the density and strength and decreases the grain size of the sintered material. Decrease in grain size also suppresses deformation twinning and promotes dislocation cell formation. As the CrFeNiMn alloy system does not contain cobalt as an alloying element it shows great promise to be used in nuclear applications. The CrFeNiMn alloy showed good phase stability during tensile testing by not undergoing phase transformation contrary to metastable austenitic stainless steel where martensite transformations take place.
Four different types of crystalline and fibrillar nanocellulosic materials with different functional groups (sulfate, carboxylate, amino-silane) are produced and used to disperse commercial multiwalled carbon nanotubes (MWCNT). Aqueous nanocellulose/MWCNT dispersions are drop-cast on tetrahedral amorphous carbon (ta-C) substrates to obtain highly stable composite electrodes. Their electrochemical properties are studied using cyclic voltammetry (CV) measurements with Ru(NH3)(6)(2+/3+), IrCl62-/3- redox probes, in electrolytes of different ionic strengths. All studied nanocellulose/MWCNT composites show excellent stability over a wide potential range (-0.6 to +1 V) in different electrolytes. Highly anionic and more porous fibrillar nanocellulosic composites indicate strong electrostatic and physical enrichment of cationic Ru(NH3)(6)(2+/3+) in lower-ionic-strength electrolytes, while lesser anionic and denser crystalline nanocellulosic composites show no such effects. This study provides essential insights into developing tailorable nanocellulose/carbon nanomaterial hybrid platforms for different electrochemical applications, by altering the constituent nanocellulosic material properties.
Compact layers containing embedded semiconductor particles consolidated using pulsed electric current sintering exhibit intense, broadband near-infrared reflectance. The composites consolidated from nano- or micro-silica powder have a different porous microstructure which causes scattering at the air-matrix interface and larger reflectance primarily in the visible region. The 3 mm thick composite compacts reflect up to 72% of the incident radiation in the near-infrared region with a semiconductor microinclusion volume fraction of 1% which closely matches predictions from multiscale Monte Carlo modeling and Kubelka-Munk theory. Further, the calculated spectra predict an improvement of the reflectance by decreasing the average particle size or broadening the standard deviation. The high reflectance is achieved with minimal dissipative losses and facile manufacturing, and the composites described herein are well-suited to control the radiative transfer of heat in devices at high temperature and under harsh conditions.