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Microstructure characterization by X-ray tomography and EBSD of porous FeCr produced by liquid metal dealloying
Highlights: • FeCr-Ni precursors were dealloyed in a Mg bath to give FeCr-Mg bicontinuous structure. • FeCr-Mg bicontinuous structure was immersed in HNO{sub 3} solution to get porous FeCr. • (FeCr){sub x}-Ni{sub 1−x} precursors are fully FCC phase while porous FeCr are fully BCC phase. • Composition & dealloying parameters are key parameters for controlling microstructure - Abstract: Liquid metal dealloying is a promising technique to get nanoporous materials which are attractive for their excellent functional properties. From a (FeCr){sub x}-Ni{sub 1−x} precursor, it is possible to get porous FeCr with this technique. While immersing precursors in a molten Mg bath, Ni atoms selectively migrate into the Mg bath. After cooling down to room temperature, the resulting microstructure is a bi-continuous structure of FeCr and Mg (with Ni in solid solution). A final etching step removes the Mg solid-state solution phase. Precursors with different compositions were dealloyed and imaged in 3D. From X-ray tomography images, porous FeCr characteristics as solid fraction, phase size, specific surface were extracted. EBSD maps were acquired on samples before and after dealloying. We will show that precursor composition is a key parameter to control pores and grains size while dealloying parameters (time and temperature) are key parameters to control ligaments size and in fine specific surface. By controlling precursor composition and dealloying parameters it is now possible to get dealloyed nanoporous metals with desired grain and porous microstructure by liquid metal dealloying.
A boundary-based approach to the multiscale microstructural characterization of a W-Ni-Fe tungsten heavy alloy
Here, a combination electron backscattered diffraction and transmission electron microscopy based approach has been implemented to study the effects of purposefully introduced anisotropy in a tungsten heavy alloy (WHA) through hot-rolling. Particular attention has been paid to changes in number and proportion of various boundary types from a quantitative standpoint; incorporating qualitative behavioral observations from prior analyses to generate experimentally-validated bases for the examination and application of a microstructure which exhibits an optimal balance of strength and ductility. It is asserted that a combination of increased temperatures during rolling and additional isothermal hold time for the post-rolling annealing steps may lead to a reduction in unfavorable textural components due to rolling in the W-phase and a decrease in premature fracture due to W-W microcracking respectively. This is expected to further increase the proportion of interphase boundaries and improve the ductility of these rolled structures, producing a superior rolled WHA microstructure.
A Summary of the Microstructural Characterization Results for the A709 Commercial Heats
To improve high temperature strength for advanced nuclear reactors, it is necessary to qualify additional structural materials for introduction into the American Society of Mechanical Engineers (AMSE) Boiler and Pressure Vessel Code (BPVC). Specifically, Alloy 709 was identified as a material for Sodium-cooled Fast Reactors to enhance time-dependent mechanical properties compared to 316H stainless steel, a code qualified high temperature alloy. Idaho National Laboratory (INL) and Oak Ridge National Laboratory (ORNL) performed initial microstructure and mechanical property testing on a third, commercial heat of Alloy 709 stainless steel. The Alloy 709 plate was produced by Allegheny Technology Inc. (ATI) and in the solution annealed condition. The chemical composition was within the limits for an American Society of Testing and Materials (ASTM) A213 specification for seamless tube for material UNS S31025. Grain size was measured as an average ASTM size of 6.5, which was larger than the ASTM 7 required according to ASTM A213 for seamless tube. The chemical composition was within the limits for an ASTM A213, and the room temperature tensile tests and hardness data met ASTM A213 specifications. Creep-fatigue results showed similar behavior to previous heats of Alloy 709.
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.
Microstructural characterization of laser micro-welded Nitinol wires
Highlights: • FIB technique was used in the preparation of TEM foils of laser micro-welded joint. • Phase content in various zones of laser micro-welded Nitinol wires was revealed. • Welding induces the R-phase formation in HAZ and intermetallics precipitation in FZ. - Abstract: Laser micro-welding has been considered one of the most promising joining methods of manufacturing Nitinol biomedical devices. However, there is still a lack of understanding about how laser micro-welding influences the microstructure. This work attempts to reveal the phase content within various microstructural zones of laser micro-welded crossed Nitinol wires by transmission electron microscopy (TEM) with the assistance of the focused ion beam (FIB) technique. The base metal is composed of a single austenite phase (B2). The fusion zone exhibits the coexistence of austenite matrix and several intermetallics (T{sub 2}Ni, TiNi{sub 3} and Ti{sub 3}Ni{sub 4}). The precipitation of R-phase was observed in HAZ with B2 matrix due to thermally induced stresses during welding.
Rapid Solidification of Sn-Cu-Al Alloys for High-Reliability, Lead-Free Solder: Part I. Microstructural Characterization of Rapidly Solidified Solders
Particles of Cu x Al y in Sn-Cu-Al solders have previously been shown to nucleate the Cu 6 Sn 5 phase during solidification. In this study, the number and size of Cu 6 Sn 5 nucleation sites were controlled through the particle size refinement of Cu x Al y via rapid solidification processing and controlled cooling in a differential scanning calorimeter. Cooling rates spanning eight orders of magnitude were used to refine the average Cu x Al y and Cu 6 Sn 5 particle sizes down to submicron ranges. The average particle sizes, particle size distributions, and morphologies in the microstructures were analyzed as a function of alloy composition and cooling rate. Deep etching of the samples revealed the three-dimensional microstructures and illuminated the epitaxial and morphological relationships between the Cu x Al y and Cu 6 Sn 5 phases. Transitions in the Cu 6 Sn 5 particle morphologies from faceted rods to nonfaceted, equiaxed particles were observed as a function of both cooling rate and composition. Initial solidification cooling rates within the range of 10 3 to 10 4 °C/s were found to be optimal for realizing particle size refinement and maintaining the Cu x Al y /Cu 6 Sn 5 nucleant relationship. In addition, little evidence of the formation or decomposition of the ternary-β phase in the solidified alloys was noted. As a result, solidification pathways omitting the formation of the ternary-β phase agreed well with observed room temperature microstructures.
Microstructural Characterization and Simulation of High Temperature Inelastic Deformation and Fracture of Al-Li 2070
A combined experimental and simulation investigation is carried out to characterize the high temperature deformation behavior of a recently developed Al-Li alloy, AA2070, over a temperature range including typical forging temperatures. Focus is placed on providing explanations for the temperature-dependent plastic and fracture behavior observed for this material using macroscale tensile tests, microscale imaging and analysis, and physics-based micromechanical modeling. It is shown that AA2070 experiences non-monotonic elongation to failure with a rise in temperature. Detailed fractography and microstructural analysis, including dynamic recrystallization analysis, provide insight into this interesting and practically useful behavior. In addition, a validated crystal plasticity model is called upon to explain the unique texture observed in the necked region of the ductile tensile specimen. The insights provided by this investigation will allow improved design of high temperature forming operations for AA2070 and similar alloys which can extend the application of third generation Al-Li alloys.
Rheological and microstructural characterization of aqueous suspensions of carbon black and reduced graphene oxide
Carbon black is often used as a conductivity enhancer in battery electrodes. Reduced graphene oxide is another conducting material, with a high aspect ratio sheet-like morphology, and offers the possibility of generating a conducting network at loadings that are small compared to carbon black. Suspensions of conducting carbon, active materials and binders are typically coated on current collectors during the formation of electrodes. The rheology of these suspensions is an important indicator of the connectivity of particles in the suspension and impacts the electrical conductivity as well as the thickness of the coated layer. In this work, the rheology and microstructures of aqueous suspensions of para-aminobenzoic acid terminated carbon black (CB) with and without reduced graphene oxide (RGO) were investigated. The CB loading varied between 0.05 wt.% -10 wt.%, while the samples containing RGO had an RGO loading of 0.05 wt.%. The pH of the suspension was varied from 7.5 to 3. The carboxyl groups on the CB surface are deprotonated at pH 7.5, making the particles hydrophilic. Protonation of the carboxylate groups at pH 3 makes the particles partially hydrophobic. Suspensions of CB showed Newtonian behavior at all loadings for pH 7.5, and at loadings below 1.5 wt.% for pH 3. They are shear thinning at loadings between 1.5–10 wt.%. Interestingly, the low shear viscosity is non-monotonic with CB loading, rising up to a CB loading of 7.5 wt.%, and then dropping at 10 wt.%. Cryogenic scanning electron microscopy (SEM) showed CB particles forming aggregates at pH 3 for CB loadings greater than 1.5 wt.%. At pH 3, addition of 0.05 wt.% RGO resulted in a viscosity increase for suspensions containing 0.5 wt.% CB, as the RGO formed connections with CB particles that enhanced network formation. Adding RGO had little effect on suspensions that had 1.5 wt.% CB. The combination of SEM imaging and suspension rheology provides insight into the particle connectivity for the carbon-based materials studied here. These insights will be useful in determining coating conditions for slurries used in rechargeable battery electrodes.
Mechanical and Microstructural Characterization of Low-Temperature Neutron Irradiated Zircaloy-4
Zr-based alloys, namely Zircaloy-2, Zircaloy-4, ZIRLO, or M5, have been used in light water reactors (LWRs) as structural materials (cladding, pressure tubes, and etc.). Under irradiation conditions, especially at harsh pressurized water reactor (PWR) conditions, these Zr alloys can undergo embrittlement due to corrosion, hydriding, and irradiation induced stresses. This ultimately leads to the severe degradation of Zr-alloys and increase the probability of fuel failure. While various research efforts have been conducted in developing better Zr-based alloys to withstand these harsh environments, there is a considerable amount of Zr-alloy characteristics, such as change in mechanical properties under irradiation conditions and its relationship to the materials microstructure, that need to be studied. This present study has focused on investigation of mechanical and microstructural properties of Zircaloy-4 under low temperature (80 - 100 deg. C) neutron irradiation conditions. Some of the samples studied were also hydrided to evaluate influence of hydride precipitates in the material. (authors)
Microstructure characterization and electrical transport of nanocrystalline ZrO{sub 2}–CeO{sub 2} solid solution
Graphical abstract: - Highlights: • Monoclinic ZrO{sub 2} phase has been changed to cubic ZrO{sub 2} phase within a short milling. • Conductivity increases due to change of phase from monoclinic to cubic. • A maximum has been observed in the s–T curve. • A transformation from −ve to +ve ac magnetoconductance has been observed. - Abstract: Nanocrystalline ZrO{sub 2}–CeO{sub 2} (ZC) solid solution is synthesized by high energy ball-milling the powder mixture of monoclinic (m) ZrO{sub 2}–10 mol% CeO{sub 2} in air medium. X-ray powder diffraction (XRD) patterns show that the method IS effective to synthesize cubic (c) ZrO{sub 2} phase within a short milling time. Formation mechanism, structural and microstructural changes of different phases and relative phase abundances have been estimated by Rietveld analysis of XRD patterns. The dc conductivity has been enhanced due to monoclinic to cubic phase transformation. A transformation from small polaron hopping to correlated barrier hoping has been observed from the of temperature dependence frequency exponent study. A crossover from negative to positive ac magnetoconductance has been observed at temperature T = 280 K and 230 K for unmilled (ZC0H) and 8 h (ZC8H) milled samples, respectively.
Property evaluation and microstructure characterization of the A3-3 matrix graphite - 18440
Spherical fuel elements with TRISO fuel will be used in the pebble-bed high temperature gas-cooled nuclear reactor. The fuel will be located within the center region of the elements, and will be suspended in, and surrounded by a shell of matrix graphite. The matrix graphite provides structural support to the fuel, prevents fuel damage, and allows for heat transfer from the fuel to the coolant. The raw materials for the matrix graphite, type A3-3, includes 64 wt% natural flake graphite, 16 wt% artificial graphite and 20 wt% phenol resin binder. After the final heat treatment, the resulting A3-3 matrix is composed of 71 wt% natural graphite, 18 wt% artificial graphite, and 11 wt% phenol resin-derived coke carbon. The microstructure of A3-3 matrix graphite has direct influences on the material properties, which are crucial to maintaining the integrity and safety of the fuel elements. This presentation will discuss microstructure features, such as lattice, and crystal parameters, porosity, pore size and distribution, and anisotropy. The multiple physical, mechanical and thermal properties of this material, including: elastic modulus, mechanical strength, and oxidation property will also be presented. (authors)
Microstructural characterization of random packings of cubic particles
Understanding the properties of random packings of solid objects is of critical importance to a wide variety of fundamental scientific and practical problems. The great majority of the previous works focused, however, on packings of spherical and sphere-like particles. We report the first detailed simulation and characterization of packings of non-overlapping cubic particles. Such packings arise in a variety of problems, ranging from biological materials, to colloids and fabrication of porous scaffolds using salt powders. In addition, packing of cubic salt crystals arise in various problems involving preservation of pavements, paintings, and historical monuments, mineral-fluid interactions, CO 2 sequestration in rock, and intrusion of groundwater aquifers by saline water. Not much is known, however, about the structure and statistical descriptors of such packings. We have developed a version of the random sequential addition algorithm to generate such packings, and have computed a variety of microstructural descriptors, including the radial distribution function, two-point probability function, orientational correlation function, specific surface, and mean chord length, and have studied the effect of finite system size and porosity on such characteristics. Here, the results indicate the existence of both spatial and orientational long-range order in the packing, which is more distinctive for higher packing densities.
Microstructural Characterization of As-Cast MP-1 Experiment U-10Mo Alloy
The Mini-Plate-1 (MP-1) test is the first in a series of fuel testing campaigns with the purpose of achieving regulatory qualification for the U-10Mo monolithic plate-type fuel system. The objective of MP-1 is to assess fuel performance behavior of fuel plates fabricated by a commercial fuel fabricator (BWX Technologies, Inc.) and make sure that the fuel maintains mechanical integrity and geometric stability and behaves in a stable and predictable manner. As a part of MP1 fabrication campaign several castings were prepared. The castings were vacuum induction melted using HEU pieces mixed with a master alloy made up of DU and molybdenum pieces. The Master Alloy was poured by a commercial vendor. There was little mixing during melting. A three-plate mold was utilized to form three U-10Mo plates per melt pour. The work described here shows that the resulting microstructure varies greatly from one cast plate to another, and from the top to the bottom of each cast plate. The extent of variation in microstructural features such as grain size, second phase particle (SPP) distribution and morphology, microsegregation of constituents within the dendritic microstructure, porosity, and casting abnormalities are presented and discussed.
Microstructural Characterization and High Strain Rate Plastic Flow Behavior of SMAW Armox500T Steel Joints from Spherical Indentation Experiments
Static indentation and uniaxial compression tests have been conducted on Armox500T steel and its weldments to predict the constraint factor (CF), i.e., ratio of Meyer’s hardness to uniaxial flow stress. Series of dynamic indentation experiments were carried out at impact velocities ranging from 5 to 300 m/s to estimate dynamic hardness as a function of average strain. Subsequently, dynamic indentation (DI) test data and CF determined under static indentation conditions have been used to study the high strain rate plastic flow behavior of Armox500T weldments in comparison with the base metal. It was observed that flow stress for Armox500T and its weldments under dynamic loading conditions (10{sup 4} s{sup −1}) are significantly higher than flow stress measured under static loading conditions (10{sup −3} s{sup −1}). The plastic flow behavior computed from DI is in good agreement with the data evaluated through conventional split Hopkinson pressure bar technique. Further, the study of the microstructure of base metal and weldments by optical microscopy and SEM revealed a considerable variation in the microstructure.
In-situ hydrogen microstructural characterization of Si heterojunction passivation: Addressing V OC degradation and mitigation pathways
Si heterojunction (SHJ) solar cells have demonstrated record efficiency >27%, approaching the theoretical limit of ≈ 29%, primarily due to best surface/interface defect passivation provided by deposited thin layers of hydrogenated amorphous silicon (a-Si:H). Such excellent surface/interface passivation reduces recombination loss and result in >100 mV improvement of cell open circuit voltage (V OC ) to ≈ 750 mV, thus the cell efficiency. However, fielded SHJ modules exhibit loss of V OC and hence efficiency over time in years, presumably due to degradation related to a-Si:H layers. This adversely affects the technology’s market acceptance, and levelized cost of energy (LCOE). It is hypothesized that the origin of a-Si:H degradation is somehow related to the presence of weak Si–Si bonds and hydrogen in a-Si:H films. The objective of this project is to test this hypothesis by directly measuring chemical and structural changes occurring within SHJ component layers and solar cells. This is achieved by developing an innovative in-situ Fourier transform infrared (FTIR) spectrometry apparatus to monitor hydrogen microstructural changes occurring within amorphous silicon and decipher hydrogen evolution kinetics over time when samples are exposed to heat and/or light stress. These in-situ measured hydrogen microstructural changes are correlated to the changes in effective minority carrier lifetime (τ eff ), implied V OC (iV OC ), surface recombination velocity (S), and cell V OC . These mechanistic understandings will provide critical guidance to mitigate the V OC -driven degradation of SHJ solar cell performance. Passivation optimization and degradation analysis of individual SHJ component structures were achieved through systematic deposition of three symmetric structures and the completed SHJ solar cell structure. The three symmetric structures used were intrinsic a-Si:H [(i)a-Si:H] layers in a bilayer structure, intrinsic and p-type doped stacked layers [(i-p)a-Si:H] representing the front heterojunction in the SHJ cell, and intrinsic and n-typed doped stacked layers [(i-n)a-Si:H] representing the back-side back surface field (BSF) in the SHJ cell. State-of-the-art passivation qualities are demonstrated by a champion iV OC of 740 mV for the (i)a-Si:H layers, and the (i-n)a-Si:H symmetric structure. A 725 mV iV OC is observed for the (i-p)a-Si:H symmetric structure. These symmetric passivated SHJ component structures were subsequently subjected to different accelerated lifetime (ALT) stressors to identify which conditions contribute the most to iV OC degradation. Degradation of the thin (10 nm) (i)a-Si:H passivation layers without any additional overlying layers is minimal; complexity of this study arises due to unavoidable surface oxidation of (i)a-Si:H layer during most of the stress application, which is likely irrelevant for a full SHJ cell configuration with overlying protective layers. The iV OC degradation of symmetric structures is found to occur primarily at the (i-p)a-Si:H passivation stack under dark heat stress with associated hydrogen loss from the (p)a-Si:H layer. An activation energy for increase in S (defect creation) of 0.65 eV can be correlated to the activation energy of ≈ 0.4 eV for hydrogen loss from the (i-p)a-Si:H stack. This also suggests the presence of weakly bonded hydrogen in the (p)a-Si:H films, which effuses out of the film stack at such low activation energy. When light and heat stress are applied together, similar hydrogen loss from (i-p)a-Si:H stack is observed, however, does not appreciably degrade iV OC or increase S. This is an important result and departure from direct correlation between hydrogen loss and defect creation. This perhaps indicates additional defect chemistries or annealing that might be occurring in the presence of light requiring further detailed defect measurements. The full SHJ cell structure used for this project is depicted in Fig.1(d). SHJ cells with an initial V OC ≈ 700 mV were fabricated and subjected to similar ALT stress conditions. Cell V OC is found to degrade the most under dark heat stress and is confirmed by observed hydrogen migration out of the (i-p)a-Si:H stack. However, hydrogen cannot escape from the cell stack, it accumulates near the (p)a-Si:H/ITO contact interface, where ITO acts as a barrier preventing hydrogen loss. Furthermore, light-heat combined stress does not degrade V OC appreciably, confirming the occurrence of a defect annealing process.
Microstructural characterization and mechanical properties of a novel TiC-based cermet bonded with Ni3(Al,Ti) and NiAl duplexalloy
A novel TiC/Ni{sub 3}(Al,Ti)-NiAl composite has been designed and synthesized by in-situ reactive hot-pressing a mixture of Ti{sub 3}AlC{sub 2} and Ni powders. After hot-press sintering at 1500 °C and 30 MPa, almost fully dense composite was obtained and the in-situ formed TiC grains were well-bonded with Ni{sub 3}(Al,Ti) and NiAl alloys. Due to the nanolaminated structure in Ti{sub 3}AlC{sub 2} materials that weakly bonded Al layers are more prone to be out-diffused from Ti{sub 3}AlC{sub 2} lattice than that of Ti atoms. The deintercalated AlTi atoms would react with Ni to give rise to the formation of Ni{sub 3}(Al,Ti) and NiAl alloys, and meanwhile a crystal lattice structure transformation happened from hexagonal Ti{sub 3}AlC{sub 2} to cubic lattice TiC. The formation of phases, grains morphologies, sintering behavior and mechanical properties were associated with sintering temperature. The as prepared TiC/Ni{sub 3}(Al,Ti)-NiAl composite under 1500 °C exhibited superior mechanical properties comparing with the counterparts fabricated under 1350 °C and 1400 °C because of the enhanced microstructures and eliminations of pores. Hardness, flexural strength and fracture toughness of the TiC/Ni{sub 3}(Al,Ti)-NiAl composite at room temperature were determined as 9.9 ± 0.35 GPa, 665 ± 26 MPa and 10.23 ± 0.4 MPa·m{sup 1/2}, respectively. Interestingly, the flexural strength and fracture toughness increases with temperature rising from 600 to 800 °C, the maximum of flexural strength and fracture toughness could reach 775 ± 25 MPa and 11.6 ± 0.4 MPa·m{sup 1/2} at 800 °C.
Microstructural characterization and mechanical properties of high power ultrasonic spot welded aluminum alloy AA6111–TiAl6V4 dissimilar joints
Aluminum alloy AA6111 and TiAl6V4 dissimilar alloys were successfully welded by high power ultrasonic spot welding. No visible intermetallic reaction layer was detected in as-welded AA6111/TiAl6V4 welds, even when transmission electron microscopy was used. The effects of welding time and natural aging on peak load and fracture energy were investigated. The peak load and fracture energy of welds increased with an increase in welding time and then reached a plateau. The lap shear strength (peak load) can reach the same level as that of similar Al–Al joints. After natural aging, the fracture mode of welds transferred from ductile fracture of the softened aluminum to interfacial failure due to the strength recovery of AA6111. - Highlights: • Dissimilar Al/Ti welds were produced by high power ultrasonic spot welding. • No visible intermetallic reaction layer was detected on weld interface. • The lap shear strength can reach the same level as that of similar Al–Al joints. • The fracture mode becomes interfacial failure after natural aging.