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At least 1,315 records · Page 73

Lattice strain evolution and load partitioning during creep of a Ni-based superalloy single crystal with rafted γ' microstructure

In-situ neutron diffraction measurements were performed on monocrystalline samples of the Ni-based superalloy CMSX-4 during N-type γ' raft formation under the tensile creep conditions of 1150 °C/100 MPa, and subsequently on a rafted sample under the low temperature/high stress creep conditions of 715 °C/825 MPa. During 1150 °C/100 MPa creep, the γ' volume fraction decreased from ~70% to ~50%, the lattice parameter misfit was partly relieved, and the load was transferred from the creeping γ matrix to the γ' precipitates. On cooling back to room temperature, a fine distribution of γ' precipitates formed in the γ channels, and these precipitates were present in the 715 °C/825 MPa creep regime. Under low temperature/high stress creep, the alloy with rafted γ' microstructure exhibited superior creep strength to the cuboidal γ' microstructure produced following a standard heat-treatment. A lengthy creep incubation period was observed, believed to be associated with {111}$\langle$110$\rangle$ dislocations hindering propagation of {112}$\langle$110$\rangle$ dislocations. Following the creep incubation period, extensive macroscopic creep strain accumulated during primary creep as the γ phase yielded. Lastly, the diffraction data suggest a loss of precipitate/matrix coherency in the (0k0) interfaces as creep strain accumulated.

36 MATERIALS SCIENCE↗

Lattice parameter misfit evolution during creep of a cobalt-based superalloy single crystal with cuboidal and rafted gamma-prime microstructures

A [h00] oriented Co-based superalloy single crystal was crept under tension at 940 °C=100 MPa, resulting in a P-type raft morphology with extensive particle coalescence along the [h00] loading direction. However, particle coalescence was also observed in two perpendicular directions on the (h00) plane, normal to the loading axis. Tensile creep experiments were performed with in-situ neutron diffraction at 800 °C=500 MPa on this initially rafted $\gamma$ microstructure, and for comparison at (i) 900 °C=260 MPa, and at (ii) 750 °C=875 MPa, both with initially cuboidal $\gamma$ microstructures. The alloy was shown to exhibit a positive lattice parameter misfit, and during the first hour of creep at 900 °C=260 MPa, the lattice parameter evolution indicated changes in phase composition associated with $\gamma$ dissolution as the alloy achieved phase equilibrium at 900 °C. For all three in-situ creep measurements, there was a significant divergence of the $\gamma$ and g lattice parameters as creep proceeded. The lattice parameter misfit values between the precipitates and the matrix approached their unconstrained values during creep, and were notably large compared to those of Ni-based superalloys. This is indicative of a loss of coherency at the precipitate/matrix interfaces. Such a loss of coherency at the precipitate/matrix interfaces will likely degrade certain mechanical properties such as fatigue resistance, as has been shown for the Ni-based superalloys.

36 MATERIALS SCIENCE↗

Loop and void damage during heavy ion irradiation on nanocrystalline and coarse grained tungsten: Microstructure, effect of dpa rate, temperature, and grain size

Displacement damage, through heavy ion irradiation was studied on two tungsten grades (coarse grained tungsten (CGW) and nanocrystalline and ultrafine grained tungsten (NCW)) using different displacement per atom rates and different irradiation temperatures (RT and 1050 K). Percentage of <111> and <100> type loops at the irradiation conditions was determined. Irradiation damage in the microstructure was quantified using average loop areas and densities (method A) and loop areal fraction in the grain matrices under 2-beam diffraction conditions (method B). Average values of <111> and <100> loops were calculated from method A. Loop coalescence was shown to occur for CGW at 0.25 dpa. Using both methods of quantifying microstructural damage, no effect of dpa rate was observed and damage in CGW was shown to be the same at RT and 1050 K. Swelling from voids observed at 1050 K was quantified. The loop damage in NCW was compared to CGW at the same diffraction and imaging conditions. NCW was shown to possess enhanced irradiation resistance at RT regarding loop damage and higher swelling resistance at 1050 K compared to CGW. For irradiation at 1050 K, the NCW was shown to have a similar defect densities to the CGW which is attributed to higher surface effects in the CGW, vacancy loop growth to voids and a better sink efficiency in the CGW deduced from the vacancy distribution profiles from Kinetic Monte Carlo simulations. Loop density and swelling was shown to have similar values in grains sizes that range from 80-600 nm. No loop or void denuded zones occurred at any of the irradiation conditions. This work has a collection of experiments and conclusions that are of vital importance to materials and nuclear communities.

36 MATERIALS SCIENCE↗

Microstructure and residual elastic strain at graphite nodules in ductile cast iron analyzed by synchrotron X-ray microdiffraction

The microstructure and residual elastic strain at graphite nodules (GNs) in ductile cast iron produced using either a fast or slow cooling rate have been characterized using synchrotron 3D X-ray Laue microdiffraction. The results demonstrate that thermal stress is introduced during cooling and that part of this stress is relaxed by plastic deformation of the polycrystalline ferrite matrix. It is observed that the plastic deformation is accommodated by the formation of dislocations and dislocation boundaries, which are organized in a cell structure. The dislocation density quantified based on the microstructure is most pronounced at the GN/matrix interface around small GNs in the fast cooled sample. Residual elastic strain is also present, which is mainly compressive with a maximum of 6.0–9.9 &times; 10 -4 near the GNs. Gradients of plastic deformation and elastic strain field around the GNs are observed. The results document for the first time that both the elastic strain field and the plastic strain field averaged over the grains around the GNs is approximately scaling with GN size and not affected by the cooling rate. The experimental data are compared with simulations by a finite element method, and agreement and disagreement are considered in detail.

36 MATERIALS SCIENCE↗

Effects of ternary alloy additions on the microstructure of highly immiscible Cu alloys subjected to severe plastic deformation: An evaluation of the effective temperature model

Phase evolution in dilute, strongly immiscible Cu-Mo, Cu-Mo-Ni, and Cu-Mo-Ag alloys during severe plastic deformation at low-temperature has been experimentally investigated. For the Cu95Mo05 alloy, Mo nanoparticles are formed, ~10 nm in diameter, as part of a steady state microstructure, with less than ~1 at.% Mo dissolved in the matrix. Addition of 10 or 20 at.% Ni to this binary alloy results in a significant increase in the Mo solubility, whereas comparable additions of Ag has a corresponding little effect. The steady state microstructures of alloys during ball milling of elemental powders are very similar to those during HPT processing of initially homogeneous solutions. The results are discussed in terms of an effective temperature model. Model MD simulations are presented to help relate the predictions of the effective temperature model to atomistic mechanisms.

36 MATERIALS SCIENCE↗

Nanoscale conditions for ductile void nucleation in copper: vacancy condensation and the growth-limited microstructural state

Ductile rupture or tearing usually involves structural degradation from the nucleation and growth of voids and their coalescence into cracks. Although some materials contain preexisting pores, the first step in failure is often the formation of voids. Because this step can govern both the failure strain and the fracture mechanism, it is critical to understand the mechanisms of void nucleation and the enabling microstructural configurations which give rise to nucleation. To understand the role of dislocations during void nucleation, the present study presents ex-situ cross-sectional observations of interrupted deformation experiments revealing incipient, subsurface voids in a copper material containing copper oxide inclusions. The local microstructural state was evaluated using electron backscatter diffraction (EBSD), electron channeling contrast (ECC), transmission electron microscopy (TEM), and transmission kikuchi diffraction (TKD). Surprisingly, before substantial growth and coalescence had occurred, the deformation process had resulted in the nucleation of a high density of nanoscale (≈50 μm) voids in the deeply deformed neck region where strains were on the order of 1.5. Such a proliferation of nucleation sites immediately suggests that the rupture process is limited by void growth, not nucleation. With regard to void growth, analysis of more than 20 microscale voids suggests that dislocation boundaries facilitate the growth process. The present observations call into question prior assumptions on the role of dislocation pile-ups and provide new context for the formulation of revised ductile rupture models. While the focus of this study is on damage accumulation in a highly ductile metal containing small, well-dispersed particles, these results are also applicable to understanding void nucleation in engineering alloys.

36 MATERIALS SCIENCE↗

Neutron irradiation-induced microstructure damage in ultra-high temperature ceramic TiC

Titanium carbide (TiC) is an ultra-high temperature ceramic with potential as a structural material candidate for advanced reactor concepts. However, the irradiation tolerance of TiC is not well understood. Here, we reveal the key irradiation damage microstructure degradation processes in TiC using mixed spectrum neutron irradiations at dose of ~2 displacements per atom (dpa) at temperatures of ~220, 620, and 1115 °C, combined with state-of-art microstructure characterization using transmission electron microscopy (TEM) and high-resolution TEM (HRTEM). The helium injection (~65 atomic parts per million) produced by neutron transmutation also occurred in the sample. TiC was observed to form irradiation-induced interstitial-type dislocation loops and He-stabilized cavities. At 220 and 620 °C, the analysis of the electron diffraction patterns, rel-rod imaging and HRTEM revealed that the dislocation loops were faulted Frank loops with Burgers vector b Frank = 1/3<111> lying on {111} planes. A detailed Burgers vector identification performed by the g.b technique revealed that the dislocation loops forming at 1115 °C were unfaulted, edge-type, with Burgers vectors b = a<100> and a/2<110> with corresponding {100} and {110} habit planes. Using continuum mechanics, we estimated the critical radius at which a faulted dislocation loop transitions to a perfect loop to be 9 nm. Further, no amorphization occurred in TiC under-investigated irradiation conditions while macroscopic swelling under point defect swelling regime was observed. He-stabilized cavities were detected at 1115 °C, but not at lower temperature irradiation. These observations indicate the onset of long-range vacancy migration in TiC occurs between 620 and 1115 °C.

36 MATERIALS SCIENCE↗

The correlation between microstructure and nanoindentation property of neutron-irradiated austenitic alloy D9

The microstructure and nanomechanical properties of three samples of the modified stainless steel (referred as the alloy D9) were systematically characterized after neutron irradiation in the Advanced Test Reactor. The samples were irradiated to 5.0, 8.2, and 9.2 displacements per atom at 448, 430, and 683°C, respectively. The evolutions of dislocation loops, cavities, and radiation-induced precipitates were quantitatively studied to reveal their dose and temperature dependencies. Nanohardness and nanoindentation creep tests were conducted at room temperature on the irradiated samples. Unexpected radiation hardening was observed in the highest-temperature-irradiated sample due to the formation of an unknown type of Ni- and Si-rich precipitates whose contributions to the radiation and mechanical performances of the alloy were discussed. We provide the radiation-microstructure-property correlations of alloy D9 with new insights, which can benefit the development and optimization of advanced austenitic alloys for future nuclear applications.

36 MATERIALS SCIENCE↗

Direct observations and characterization of crack closure during microstructurally small fatigue crack growth via in-situ high-energy X-ray characterization

This study provides direct observation of the crack closure mechanism of a naturally occurring, tortuous, 3D microstructurally small fatigue crack (SFC) in additively manufactured Inconel 718. In-situ non-destructive characterization is performed using high-energy X-ray diffraction techniques to capture the evolution of the 3D microstructure and micromechanical response in the vicinity of the crack front. Based on the stress state of twelve grains analyzed at the crack tip, the crack closure events of the SFC front was found to be spatially heterogeneous with respect to loading progression governed by the local stress state of the grains (specifically the stress reversal from compression to tension). From this analysis, three grains that displayed different degrees of crack closure were further investigated, based on the orientation of the crack relative to the grains and the associated modality of crack growth. The stress normal to the crack plane and the associated degree of Mode I crack behavior were correlated with events of the crack opening earlier during the loading cycle. This was further corroborated by diffraction spot spreading analysis that quantified the crystallographic lattice distortion caused by the opening crack. Additionally, the detailed characterization of the opening behavior of the grains located at the crack tip and their associated states of stress elucidates the mechanism governing crack closure and will inform future modeling efforts of this phenomenon.

36 MATERIALS SCIENCE↗

Domain wall motion across microstructural features in polycrystalline ferroelectric films

This paper describes the effect of microstructural features such as grain boundaries and triple points on the pinning of domain wall motion in perovskite Pb(Zr 0.52 Ti 0.48 )O 3 (PZT) films on polycrystalline SrRuO 3 /SrTiO 3 substrates. Here, spatial variability in the collective domain wall dynamics was assessed using non-linearity mapping via Band Excitation Piezoresponse Force Microscopy (BE-PFM). Collocating the non-linearity maps with triple point locations (as visualized by EBSD) allowed for exploration of the effects that local microstructure (e.g., grain boundary) have on domain wall motion. It was found that the extrinsic behavior varied with both the misorientation angle and the proximity to the grain boundary. The width of influence of individual grain boundaries on the motion of domain walls was a function of the character of the grain boundary; random grain boundaries exhibit deeper minima in α d /d 33,initial and larger widths of influence (up to 905 nm) compared to coincident site lattice (CSL) boundaries (up to 572 nm). Additionally, triple points containing larger numbers of random boundaries exhibited non-Rayleigh behavior to greater distances, suggesting that the triple point provides either a deep potential minimum or a region where domain wall motion is unfavorable.

36 MATERIALS SCIENCE↗

Exploring the relationship between deposition method, microstructure, and performance of Nb/Si-based superconducting coplanar waveguide resonators

Superconducting quantum circuits (SQC) are one of the most promising hardware platforms for quantum computing, yet their performance is currently limited by the presence of various structural defects inside the circuit's structure. Despite impressive progress in the past decade, a precise understanding of the origin of these defects from various fabrication processes and their impact on coherence is still lacking. Here, in this study, we performed a comprehensive investigation on the microstructure, superconductivity, and resonator quality factor of Nb films deposited by high-power impulse magnetron sputtering (HiPIMS) and direct current (DC) magnetron sputtering. A suite of characterization techniques, including electron microscopy with spectroscopy, secondary ion mass spectrometry, magneto-optical microscopy, and pump-probe reflectivity spectroscopy is used. We reveal that niobium (Nb) resonators fabricated using HiPIMS exhibit a smaller average grain size, thicker surface oxide with larger thickness variations (rougher surface), and a thicker amorphous Nb/Si interface layer compared to samples deposited by DC sputtering. We identified that the amorphous Nb oxides (mainly located at the Nb surface and along the grain boundaries) and Nb-Si amorphous layers (at the Nb/Si interface) are major and potential sources of two-level system (TLS), while off-stochiometric oxides and suboxides of Nb close to the surface, crystalline defects (i.e., dislocations at grain boundary, point defects introduced during deposition) are main contributors of non-TLS sources. Our findings clarify the relationship between different defects and coherence loss mechanisms, highlighting the importance of material microstructure control on performance optimization in SQC.

36 MATERIALS SCIENCE↗

Correlating aluminum layer deposition rates, Josephson junction microstructure, and superconducting qubits’ performance

An ultra-thin aluminum oxide layer is a key component for Josephson junctions (JJ) in superconducting quantum bits (qubits). This layer serves as a barrier layer for Cooper pairs tunneling between the superconducting electrodes and significantly influences the overall performance of the junction. In this study, we investigate the impact of aluminum deposition rates on the microstructure and chemical variation of the aluminum oxide layer, as well as the device's yields and qubits’ lifetimes. Surprisingly, although the oxide layer roughness and thickness variation improve noticeably with an increasing Al deposition rate from 0.5 Å/s to 5 Å/s, the qubit's coherence time is almost unchanged. We attribute this to the fact that Cooper pairs tunnel only through the thinnest region of the barrier. Additionally, we revealed a stress-induced grain boundary sliding short-circuit failure mechanism in the JJ. Our discovery provides a vital understanding of oxide microstructure and JJ functionality, which are critical for improving the coherence time of superconducting qubits.

Coherence time↗

Informed unsupervised machine learning analysis of dislocation microstructure from high-resolution differential aperture X-ray structural microscopy data

This study leverages high-resolution differential-aperture X-ray structural microscopy (DAXM) to probe the local dislocation structure in deformed 304L-stainless steel at small strain, by measuring the lattice rotation and deviatoric elastic strain with a sub-micron resolution. For a single grain in a polycrystalline specimen, the measured lattice rotation field over the measured volume exhibited a multimodal distribution while the deviatoric elastic strain showed a single-mode distribution. An unsupervised Cauchy mixture machine learning model was developed to resolve the multimodal distribution of the lattice rotation. By mapping the lattice rotation data associated with each Cauchy peak in the model back onto the measured volume, we identify contiguous regions of the crystal rotated near the average values corresponding to the peaks of the overall rotation distribution. These regions represent the grain subdivision in the microstructure. Finally, the dislocation density tensor was also computed and its norm was laid over the rotation field to detect the subgrain boundaries. This step provided a validation of the Cauchy mixture model for the analysis of the lattice rotation distribution. The current study highlights the integration of advanced X-ray microscopy techniques with data-driven analysis methods to uncover detailed microstructure scales in deformed crystals.

Machine learning; Lattice rotation; High-energy X-↗

Characterizing the microstructures of mammalian enamel by synchrotron phase contrast microCT

The enamel of mammalian teeth is a highly mineralized tissue that must endure a lifetime of cyclic contact and is inspiring the development of next-generation engineering materials. Attempts to implement enamel-inspired structures in synthetic materials have had limited success, largely due to the absence of a detailed understanding of its microstructure. Here, the present work used synchrotron phase-contrast microCT imaging to evaluate the three-dimensional microstructure of enamel from four mammals including Lion, Gray Wolf, Snow Leopard, and Black Bear. Quantitative results of image analysis revealed that the decussation pattern of enamel consists of discrete diazone (D) and parazone (P) bands of rods organized with stacking arrangement of D+/P/D-/P in all mammals evaluated; the D+ and D- refer to distinct diazone bands with juxtaposed rod orientations from the reference plane. Furthermore, the rod orientations in the bands can be described in terms of two principal angles, defined here as the pitch and yaw. While the pitch angle increases from the outer enamel to a maximum (up to ≈ 40°) near the dentin enamel junction, minimal spatial variations are observed in yaw across the enamel thickness. There are clear differences in the decussation parameters of enamel across species that are interpreted here with respect to the structural demands placed on their teeth. The rod pitch and band width of enamel are identified as important design parameters and appear to be correlated with the bite force quotient of the four mammals evaluated.

36 MATERIALS SCIENCE↗

Additively manufactured novel Al-Cu-Sc-Zr alloy: Microstructure and mechanical properties

An in-depth understanding of microstructure and resultant properties is paramount in the design of a novel alloy system, especially for additive manufacturing (AM). The present investigation aims to characterize a prototypical AM Al alloy with great potential for structural applications. An Al-1.5Cu-0.8Sc-0.4Zr alloy designed using integrated computational material engineering was printed using the laser powder bed fusion AM process. This novel alloy shows promising combination of strength and ductility in as-built and peak-aged conditions. This improvement in the tensile properties is attributed to the presence of both coherent L1 2 Al 3 Sc/Al 3 (Sc,Zr) precipitates and Cu-rich regions. The microstructures were studied via extensive microscopy at different length scales using X-ray microscopy, scanning electron microscopy, and transmission electron microscopy. Fractography revealed that the columnar grain boundaries in as-built condition allow easy slip transfer as compared to the equiaxed grains, with the apex of the melt pool acting as the crack nucleation site. Furthermore, the peak aged condition resulted in improved strength while marginally sacrificing ductility due to precipitates decorating dislocations, grain boundaries and melt pool boundaries thus acting as obstacles to slip transfer.

36 MATERIALS SCIENCE↗

Viewing is understanding: Graphite microstructure effects on infiltrated molten salt distribution revealed by 3D neutron tomography

Molten salt infiltration in the pore network of nuclear graphite may cause unwanted changes to graphite's local structure and mechanical and thermal properties. A detailed and comprehensive understanding of molten salt intrusion (distribution across sample cross section and penetration depth) is needed to assess its effects. Here, in this work, we report on an improved methodology for the use of neutron imaging (computed tomography) to evaluate salt penetration and distribution of a wide range of graphite grades with diverse microstructures. Neutron tomography data were acquired on the same graphite sample before and after salt intrusion; the 3D reconstructed volumes were digitally co-registered and subtracted. The difference in neutron attenuation coefficient represents direct visualization of FLiNaK (LiF–NaF–KF) salt distribution in the salt-impregnated graphite samples. This improved methodology was applied to investigate the effect of exposure times (12 h and 336 h) and of graphite microstructure when exposed to FLiNaK at 750 °C and 3 bar (gauge) pressure, starting from flowing argon at near atmospheric pressure. The results show that medium-grained and fine-grained graphites evolve to equilibrium at significantly different rates: fast salt uptake in medium-grained graphites produces salt deposits throughout the volume of graphite specimens, whereas salt infiltration in fine-grained graphites is much slower and limited to exposed surfaces.

FLiNaK infiltration↗

Microstructural characterization and equibiaxial flexural strength of CeO 2 and Ti-doped CeO 2

In this study, the synthesis of CeO 2 and titanium dioxide (TiO 2 ) doped CeO 2 (TDC) monoliths are investigated, and their fracture strength is assessed using an equibiaxial flexure testing technique at room temperature. Pellets were synthesized using conventional powder processing and sintering methods to produce the desired characteristics. The TiO 2 dopant concentration was optimized at 0.1 wt % TiO 2 to obtain dense, solid-solution pellets with an enhanced grain microstructure. A ball-on-ring fixture was used to obtain the TRS and Weibull parameters of over 30 pellets for CeO 2 and 0.1 wt % TDC to compare fracture behavior. The TRS of CeO 2 pellets ranged from 88 to 160 MPa and the TRS of 0.1 wt % TDC pellets ranged from 102 to 171 MPa, both being consistent with published values. Weibull parameters, such as characteristic strength and Weibull modulus, were extracted as 129 MPa and 8.5 for CeO 2 and 150 MPa and 9.3 for 0.1 wt % TDC, respectively. Although Hertzian contact damage was observed on compressive surfaces, failure initiation occurred on the tensile surfaces of both types of samples. Fracture surface analysis for CeO 2 indicated a predominantly intergranular fracture while 0.1 wt % TDC had a predominantly transgranular fracture mode. Finally, the TRS of 0.1 wt % TDC resulted in increased Weibull parameters when compared to CeO 2 , indicating sample chemistry and microstructure impact mechanical behavior for these samples.

36 MATERIALS SCIENCE↗

Effect of lot microstructure variations on detonation performance of the triaminotrinitrobenzene (TATB)-Based insensitive high explosive PBX 9502

PBX 9502 is an important insensitive high explosive due to its combination of safety properties and detonation performance. It is a polymer-bonded formulation consisting of 95 wt.% 1,3,5-triamino-2,4,6-trinitrobenzene (TATB) as the high explosive crystal, bound with Kel F-800 (FK-800), a co-polymer of chlorotrifluoroethylene and vinylidene-fluoride. Two different types are used, one known as virgin that uses only pristine manufactured TATB, and a second known as recycled that has 50 wt.% of its TATB reclaimed from machining scraps of previously pressed virgin PBX 9502. Recycled lots have a higher percentage of fine particles compared to virgin lots, due to the fracturing and damage sustained by TATB crystals during pressing. We examine the influence that this TATB microstructure difference between virgin and recycled PBX 9502 has on detonation performance properties. New rate-stick geometry diameter effect, detonation front shape and cylinder expansion test data are obtained for two previously uncharacterized virgin lots and one recycled lot of PBX 9502. This is combined with previously published data for one virgin and one recycled lot for evaluation purposes. Detonation shock dynamics model calibrations are conducted on each of the five lots to provide an assessment of the detonation timing characteristics of virgin versus recycled PBX 9502 lots. For two of the virgin lots, detonations propagate slower in the rate-stick geometry than those in the two recycled lots. However, the other virgin lot tested has propagation rates comparable to that of the recycled lots for larger diameter rate-sticks. The latter result, though, is shown to be geometry dependent and depends on the range of detonation curvatures accessed in different geometries. New copper-confined, cylinder expansion tests are conducted on each of the three virgin and two recycled lots to obtain detonation product Jones-Wilkins-Lee equations of state, enabling an assessment of the metal push capabilities for each of the five lots. We find that the metal push capabilities, characterized by the evolution of the heat of detonation with volume, are similar between the virgin and recycled lots. Thus, changes in microstructure between different PBX 9502 lots seemingly affect the rate of reaction, but not the overall energy content.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗