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All sourcesNASA NTRSDOE OSTI
DOE OSTI2018

Correction to: Interfacial Microstructural Evolution and Metallurgical Bonding Mechanisms for IN718 Superalloy Joint Produced by Hot Compressive Bonding

First Online: 21 June 2018 The authors would like to acknowledge the financial support given by the National Key Research and Development Program (Grant Number 2016YFB0300401), National Natural Science Foundation of China (Grant Number U1508215), Key Program of the Chinese Academy of Sciences (Grant Number ZDRW-CN-2017-1), and the National Natural Science Foundation of China (Grant Number 51774265). The authors would also like to thank Bijun Xie and Yifeng Guo for their help in the experimental work.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Multiscale mechanical behavior and microstructure evolution of extruded magnesium alloy sheets: Experimental and crystal plasticity analysis

Highlights: • Experimental stress-strain responses were reproduced by CPFE simulation based on Voronoi grains on three strain paths. • Textures predicted by simulation were in accordance with the ones measured by EBSD at the strain of 0.085. • Deformation heterogeneity in slip-dominated cases was found more significant than that in twin-favored case. • For slip-dominated cases, both high m′ value and high SFs in adjacent grains are responsible for strain localization. - Abstract: A phenomenological crystal plasticity finite element (CPFE) model based on Voronoi grains was applied to reproduce basic deformation features of a hot-extruded magnesium alloy sheet under various strain paths. Corresponding experimental investigations, including mechanical tests, electron back scattered diffraction (EBSD) measurements and optical observation, were also carried out as either a validation or a supplement of the numerical results. Predicted average stress-strain responses and texture evolution are in good accordance with measured ones. Furthermore, deformation heterogeneity at the mesoscopic and intergranular scale were investigated based on the proposed model. At the mesoscale, the heterogeneity in the slip-dominated cases tends to develop continuously, whereas the heterogeneity is retarded in twin-favored deformation. At the intergranular scale, it is concluded from the slip-dominated case that a high slip-transfer parameter and high Schmid factors (SFs) of principal slip systems in adjacent grains could accommodate higher local strain.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Theoretical Investigation of Microstructure Evolution and Deformation of Zirconium Under Cascade Damage Conditions

This work is based on our reaction-diffusion model of radiation growth of Zr-based materials proposed recently in "On the Origin of Radiation Growth of HCP Crystals". In "On the Origin of Radiation Growth of HCP Crystals", the equations for the strain rates in unloaded pure crystal under cascade damage conditions of, e.g., neutron or heavy-ion irradiation were derived as functions of dislocation densities, which include contributions from dislocation loops, and spatial distribution of their Burgers vectors. The model takes into account the intra-cascade clustering of self-interstitial atoms and their one-dimensional diffusion; explains the growth stages, including the break-away growth of pre-annealed samples; and accounts for some striking observations, such as of negative strain in prismatic direction, and co-existence of vacancy- and interstitial-type prismatic loops. In this report, the change of dislocation densities due to accumulation of sessile dislocation loops is taken into account explicitly to investigate the dose dependence of radiation growth. The dose dependence of climb rates of dislocations is calculated, which is important for the climb-induced glide model of radiation creep. The results of fitting the model to available experimental data and some numerical calculations of the strain behavior of Zr for different initial dislocation structures are presented and discussed. The computer code RIMD-ZR.V1 (Radiation Induced Microstructure and Deformation of Zr) developed is described and attached to this report.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗
DOE OSTI2018

Microstructure evolution and mechanical properties of magnesium alloys containing long period stacking ordered phase

Magnesium alloys containing rare earth (RE) in conjunction with other alloying elements, such as Zn, have drawn increasing interest due to their high strength, high ductility and high creep-resistance with the existence of long period stacking ordered (LPSO) phase. Although the LPSO phase has been studied over a decade, the question remains how it impacts the mechanical properties of Mg-RE-X alloys, where X represents a metallic element with its atomic radius smaller than Mg. This paper provides a tutorial review of the current status on the role of LPSO phase in manipulating the mechanical properties in Mg-RE-X based alloys, where some outstanding issues are also highlighted and discussed.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Friction of Metals: A Review of Microstructural Evolution and Nanoscale Phenomena in Shearing Contacts

The friction behavior of metals is directly linked to the mechanisms that accommodate deformation. We examine the links between mechanisms of strengthening, deformation, and the wide range of friction behaviors that are exhibited by shearing metal interfaces. Specifically, the focus is on understanding the shear strength of nanocrystalline and nanostructured metals, and conditions that lead to low friction coefficients. Grain boundary sliding and the breakdown of Hall–Petch strengthening at the shearing interface are found to generally and predictably explain the low friction of these materials. While the following is meant to serve as a general discussion of the strength of metals in the context of tribological applications, one important conclusion is that tribological research methods also provide opportunities for probing the fundamental properties and deformation mechanisms of metals.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Mechanical Properties and Microstructure Evolution During Bending–Unbending Deformation of Pure Titanium Sheet

In this study, the pure titanium sheets with thickness of 1 mm are deformed 1-5 times in the form of bending–unbending cyclic deformation. The bending angles before and after unbending are 120° and 180°, respectively. Mechanical properties of samples during cyclic deformation, including M/(BH){sup 2}-surface strain curve and spring back in each bending cycle, have been investigated. Moreover, the twinning/detwinning behavior and texture evolution in three typical bending layers (i.e., the tensile layer, neutral layer and compressive layer) in cyclic deformation have been tested by EBSD and TEM, and analyzed systematically. The results indicate that the most intensive twins, consist of similar proportion of tensile and compressive ones, distribute in the inner layer after 1st bending. While they disappear almost entirely after 1st unbending. The twins in outer layer could also be detwinned, and the new twins could be activated during 1st unbending. Besides, the twin density increases obviously and the residual twins could not be detwinned clearly after multiple passes of cyclic deformation. Moreover, the Schmid factor along the σ{sub 2} direction functions in the activation of twin variants regardless of the three-direction stress states.

36 MATERIALS SCIENCE↗
NASA NTRS2024

Microstructural Evolution of the Civet Cat Norite (72255)

The ‘Civet Cat Norite’ is a ~ 2.5 cm clast within the Apollo impact melt breccia sample 72255 collected during Apollo 17 EVA 2 at Boulder 1. The norite is primarily composed of plagioclase and orthopyroxene with fine-scale exsolution lamellae of augite. The plagioclase and orthopyroxene (OPX) coexist with minor quartz and augitic clinopyroxene (CPX), and accessory apatite, baddeleyite, chromite, ilmenite, loveringite, merrillite, rutile and zircon. The major minerals range from 1 to 4 mm in size and show a cataclastic texture indicated by banding of the light and dark phases]. The chemical composition of the orthopyroxene, augitic exsolution lamellae, and exsolved oxides suggest the norite crystallized in the lower crust of the Moon (10 – 70 km depth) and was subsequently excavated by impact(s). Shock pressure estimates for the norite range from 15 – 35 GPa based on maskeleynite formation within the plagioclase, kink banding in pyroxenes, and granular recrystallization in the accessory phosphates. Previous Rb-Sr and 40 Ar/ 39 Ar analyses recalculated with modern decay constants yield relatively young ages of 4.16 ± 0.05 Ga and 3.99 ± 0.03 Ga, respectively. However, recent U-Pb analyses of some zircon grains from within the Civet Cat yield an age of 4.45 ± 0.03 Ga. While this is the oldest age for any rock recovered from the Moon, the full age spread of zircon from the Civet Cat range from ca. 4.46 to 4.02 Ga, indicating variable Pb-loss and complicating interpretation of the primary age. Recent atom probe analyses indicate minimal Pb mobilization within the oldest zircon grain from Civet Cat, supporting the interpretation that these ancient zircon ages reflect the age of the norite, rather than an apparent antiquity caused by reverse discordance. To investigate the potential antiquity and deep crustal origin of the Civet Cat norite, we have undertaken high resolution microstructural analyses of the major, minor, and accessory minerals to characterize the primary igneous textures and secondary overprinting by impact and metamorphism. The employed analytical techniques include scanning electron microscope-based electron backscatter diffraction (EBSD) analyses, electron probe microanalyzer (EPMA) chemical analyses, and transmission electron microscopy (TEM) of pyroxene, plagioclase, quartz, zircon, and phosphates.

T M Erickson↗
DOE OSTI2017

Microstructural Evolution of NF709 Steel under In-situ Ion Irradiations at Room Temperature to 600 deg. C

NF709 is one of the advanced austenitic stainless steels considered for the advanced reactor systems which are characterized by high temperature, intense radiation and potentially corrosive environments. NF709 is a nitrogen-stabilized and niobium-strengthened alloy, and it provides strength nearly double that for conventional 304 and 316 stainless steels at a temperature range of 600-750 deg. C. In addition, this alloy demonstrates excellent metallurgical stability and high-temperature creep resistance, which is critical for advanced fast-reactor structural materials. Nevertheless, there is very limited irradiation data on NF709 to date, and its radiation-resistance is to be proved. It this paper, we studied the radiation response of NF709 by using the in-situ ion irradiation at the Intermediate Voltage Electron Microscopy (IVEM)- Tandem Facility, located at Argonne National Lab (ANL) and the systematic post-irradiation characterizations using transmission electron microscopy (TEM) were conducted.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Microstructural evolution of a carbon modified single crystal Ni-base superalloy

The effects of heat treatments and long term exposures of C-containing modifications of CMSX-4 were examined. Some of the alloys examined also contained additions of boron or nitrogen. Significant changes to as-cast carbide morphologies were observed. Long-term exposure caused significant MC carbide decomposition and formation of Cr-rich secondary carbides on or near to decomposing carbides. Increased topologically close-packed phase formation occurred in some cases, while, in other alloys no topologically close-packed phases were observed. All three modifications experienced more {gamma} Prime coarsening than baseline CMSX-4. - Highlights: Black-Right-Pointing-Pointer Thermal exposures of C-modified CMSX-4 resulted in changes to MC morphologies. Black-Right-Pointing-Pointer Script, MC carbide networks transformed during heat treatment. Black-Right-Pointing-Pointer Exposure caused MC decomposition and formation of Cr-rich secondary carbides. Black-Right-Pointing-Pointer TCP phase formation was affected by alloy content. Black-Right-Pointing-Pointer All three modifications experienced more {gamma} Prime coarsening than baseline CMSX-4.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Microstructural evolution in NaNbO{sub 3}-based antiferroelectrics

Our recent study found that CaZrO{sub 3} doping can effectively enhance the antiferroelectric P phase in NaNbO{sub 3} ceramics, leading to a double polarization hysteresis loop characteristic of a reversible antiferroelectric ↔ ferroelectric phase transition [Shimizu et al., Dalton Trans. 44, 10763 (2015)]. Here, a thorough transmission electron microscope study was performed to illustrate the CaZrO{sub 3} doping-assisted antiferroelectricity stabilization. In parallel to the bright-field imaging and selected area electron diffraction from multiple zone axes, detailed dark-field imaging was utilized to determine the superlattice structural origins, from either oxygen octahedral tilting or antiparallel cation displacements. By analogy with Pb(Zr{sub 1−x}Ti{sub x})O{sub 3} and rare-earth doped BiFeO{sub 3} systems, the chemical substitutions are such as to an induced polar-to-antipolar transition that is consistent with a tolerance factor reduction. The resultant chemical pressure has a similar effect to the compressive hydrostatic pressure where the antiferroelectric state is favored over the ferroelectric state.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Microstructural evolution and growth behavior of intermetallic compounds at the liquid Al/solid Fe interface by synchrotron X-ray radiography

Highlights: • A layered and tongue-like η phase was in-situ observed by synchrotron radiation X-ray radiography. • The coalescence of η phase bottom resulted in dissolution, further increasing the growth rate. • The θ phase growth behavior with different morphologies during cooling was analyzed. - Abstract: The growth of Inter-Metallic Compounds (IMCs) with dissolution was investigated on the liquid Al/solid Fe interconnection by using synchrotron radiation real-time imaging technology. At the initial stage of holding at 850 °C, a layer of the η-Fe{sub 2}Al{sub 5} phase formed at the interface, and tongue-like η grew into α-Fe. The tongue-like η phase had a stronger (001) texture than the layered phase. The coalescence of tongue-like η started at the bottom, followed by the dissolution of IMCs, which leads to a further increase in its growth rate. During solidification stage, the dotted, needle-like and flake θ-FeAl{sub 3} phases were sequentially formed.

36 MATERIALS SCIENCE↗
DOE OSTI2010

Grain growth and microstructural evolution of yttrium aluminum garnet nanocrystallites during calcination process

An yttrium aluminum garnet (YAG) precursor precipitate was synthesized by urea method using yttria (Y{sub 2}O{sub 3}) and aluminum nitrate (Al(NO{sub 3}){sub 3}.9H{sub 2}O) as raw materials. The fresh wet precipitate was dried by supercritical carbon dioxide (CO{sub 2}) fluid and the resulting powder was calcined at temperatures from 600 to 1600 {sup o}C. Crystallization of YAG was detected at 800 {sup o}C, and completed at 900 {sup o}C. HRTEM images of the YAG product obtained above 900 {sup o}C revealed crystallographically specific oriented attachment along the [1 1 2] direction. Based on the observation of the particle morphology a possible growth mechanism of YAG nanoparticles was presented. The fast increase on the average crystallite size of YAG at temperatures from 900 to 1300 {sup o}C is attributed to the crystallographically specific oriented attachment growth process. As the growth process proceeds at higher temperatures, oriented attachment based growth becomes less important because of the increase on particle size, and the self-integration assisted by the Ostwald ripening becomes dominant.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Microstructure evolution in TRIP-aided seamless steel tube during T-shape hydroforming process

Transformation-induced plasticity aided seamless steel tube comprising of ferrite, bainite, and metastable austenite was processed through forging, piercing, cold-drawing, and two-stage heat treatment. T-shape hydroforming is a classic forming method for experimental research and practical production. The current work studied austenite-to-martensite transformation and microcrack initiation and propagation of the tube during T-shape hydroforming using electron backscattering diffraction, scanning electron microscopy, and transmission electron microscopy. The strain distribution in the bcc-phase and fcc-phase was studied by evaluating changes in the average local misorientation. Compared to the compressive stress, metastable austenite with similar strain surrounding or inside the grains transformed easier under tensile loading conditions. The inclusions were responsible for microcrack initiation. The propagation of the cracks is hindered by martensite/austenite constituent due to transformation induced plasticity effect. The volume fraction of untransformed retained austenite decreased with increase in strain implying transformation-induced plasticity effect. - Highlights: • Hydroformed tubes processed via TRIP concept • EBSD provided estimate of micro local strain. • Retained austenite hinders propagation of microcracks.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Microstructural evolution and micromechanical properties of gamma-irradiated Au ball bonds

The effect of gamma radiation on the mechanical and structural properties of gold ball bonds was investigated. Gold wires from thermosonic wire bonding were exposed to gamma rays from a Cobalt-60 source at a low dose (5 Gy). The load–depth curve of nanoindentation for the irradiated gold wire bond has an apparent staircase shape during loading compared to the as-received sample. The hardness of the specimens calculated from the nanoindentation shows an increase in value from 0.91 to 1.09 GPa for specimens after exposure. The reduced elastic modulus for irradiated specimens significantly increased as well, with values from 75.18 to 98.55 GPa. The change in intrinsic properties due to gamma radiation was investigated using dual-focused ion beam and high-resolution transmission electron microscope analysis. The dual-focused ion beam and high-resolution transmission electron microscope images confirmed the changes in grain structure and the presence of dislocations. The scanning electron microscope micrographs of focused ion beam cross sections showed that the grain structure of the gold became elongated and smaller after exposure to gamma rays. Meanwhile, high-resolution transmission electron microscopy provided evidence that gamma radiation induced dislocation of the atomic arrangement. - Highlights: • Nanoindentation technique provides a detailed characterisation of Au ball bond. • P–h curve of irradiated Au ball bond shows an apparent pop-in event. • Hardness and reduced modulus increased after exposure. • Elongated and smaller grain structure in irradiated specimens • Prevalent presence of dislocations in the atomic arrangement.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Microstructure evolution and mechanical properties of nano-SiCp/AZ91 composite processed by extrusion and equal channel angular pressing (ECAP)

Nano-SiCp/AZ91 magnesium matrix composite was fabricated by stir casting. The as-cast ingots were extruded at 350 °C, then processed by equal channel angular pressing (ECAP) at various temperatures (250 °C, 300 °C and 350 °C). Grains are significantly refined after the extrusion and the ECAP. A basal fibre texture was detected by neutron diffraction after the extrusion, which inclines about 45° to the extrusion direction (ED) after the ECAP. Nano-scaled SiC particles agglomerate in the as-cast composite. After the extrusion, the agglomeration tends to form continuous or discontinuous strips along the extrusion direction. By application of the ECAP, the agglomerated SiC particles are partly dispersed and the strips formed during the extrusion tend to be thinner and broken with the increasing pass number. The yield tensile strength (YTS) and the ultimate tensile strength (UTS) of the composite are dramatically increased after the extrusion. ECAP for one pass at various temperatures further increases the strength, however, the YTS decreases with the increasing ECAP temperature and the pass number. The Orowan equations predict the maximum YTS of the composite may be up to 400 MPa providing SiC particles are homogenously distributed in the matrix. - Highlights: •Nano-scaled SiC particles were successfully added into AZ91 by stirring casting. •Agglomeration of nano-particles were improved by extrusion and ECAP. •Yield strength of the composite is 328 MPa after one pass of ECAP. •Further ECAP process with optimized parameters may fully disperse nano-particles. •Yield strength is predicted to up to 400 MPa when particles are fully dispersed.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Microstructure evolution during the precipitation and growth of fully coherent DO{sub 22} superlattice in an Ni-Cr-W alloy

The ordering transformation occurring in a model Ni-Cr-W superalloy during prolonged exposure to proper temperature has been investigated systematically. It is demonstrated that nanometer-sized precipitates with a DO{sub 22} structure can precipitate in the Ni-Cr-W alloy by means of simple aging treatment at 650–700 °C. The mechanism of transformation to DO{sub 22} superlattice has been determined to be continuous ordering based on the results of high resolution transmission electron microscopy investigation and variation trend in Vickers microhardness. Different variants of DO{sub 22} phase can coexist in the matrix with no signs of overaging as aging time increases, indicating it has a high thermal stability. The precipitates of DO{sub 22} superlattice has been found to be of ellipsoidal shape which results in the greatest reduction of strain energy. The interfaces between DO{sub 22} precipitates and matrix have been revealed to be coherent at the atomic scale, resulting in considerable coherency strain attributing to the lattice misfit between DO{sub 22} particle and matrix. Because of the high-density nanometer-sized DO{sub 22} phase, the microhardness of the alloy has been improved remarkably after aging treatment. - Graphical abstract: Different variants of the DO{sub 22} superlattice can coexist in the matrix, and the interface between precipitate and the matrix remain coherence at the atomic scale. The three dimensional form of the DO{sub 22} precipitates constructed from three mutually perpendicular projections is an ellipsoidal stick, and the directions of elongations are along the longest axis of the unit cell for DO{sub 22} phase. - Highlights: •The DO{sub 22} phase precipitated in the Ni-Cr-W alloy has a high thermal stability. •The morphology of DO{sub 22} superlattice has been determined to be ellipsoid. •The interface between DO{sub 22} phase and matrix are fully coherent at the atomic scale. •Different variants of DO{sub 22} phase occur equiprobably. •The alloy strength can be improved dramatically by the nanoscale DO{sub 22} particles.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Microstructural evolution of P92 ferritic/martensitic steel under Ar{sup +} ion irradiation at elevated temperature

Irradiation damage in P92 ferritic/martensitic steel irradiated by Ar{sup +} ion beams to 7 and 12 dpa at elevated temperatures of 290 Degree-Sign C, 390 Degree-Sign C and 550 Degree-Sign C has been investigated by transmission electron microscopy, scanning electron microscopy and atomic force microscopy. The precipitate periphery (the matrix/carbide interface) was amorphized only at 290 Degree-Sign C, while higher irradiation temperature could prevent the amorphization. The formation of the small re-precipitates occurred at 290 Degree-Sign C after irradiation to 12 dpa. With the increase of irradiation temperature and dose, the phenomenon of re-precipitation became more severe. The voids induced by irradiation were observed after irradiation to 7 dpa at 550 Degree-Sign C, showing that high irradiation temperature ({>=} 550 Degree-Sign C) was a crucial factor which promoted the irradiation swelling. Energy dispersive X-ray analysis revealed that segregation of Cr and W in the voids occurred under irradiation, which may influence mechanical properties of P92 F/M steel. - Graphical Abstract: High density of small voids, about 2.5 nm in diameter, was observed after irradiation to 12 dpa at 550 Degree-Sign C, which was shown in panel a (TEM micrograph). As shown in panel b (SEM image), a large number of nanometer-sized hillocks were formed in the surface irradiated at 550 Degree-Sign C, and the mean size was {approx} 30 nm. The formation of the nanometer-sized hillocks might be due to the voids that appeared as shown in TEM images (panel a). High irradiation temperature ({>=} 550 Degree-Sign C) was a crucial factor for the formation of void swelling. Highlights: Black-Right-Pointing-Pointer Small carbides re-precipitated in P92 matrix irradiated to 12 dpa at 290 Degree-Sign C. Black-Right-Pointing-Pointer High density of voids was observed at 550 Degree-Sign C. Black-Right-Pointing-Pointer Segregation of Cr and W in voids occurred under irradiation.

36 MATERIALS SCIENCE↗
DOE OSTI2017

In Situ GIWAXS Analysis of Solvent and Additive Effects on PTB7 Thin Film Microstructure Evolution during Spin Coating

The influence of solvent and processing additives on the pathways and rates of crystalline morphology formation for spin-coated semiconducting PTB7 (poly[[4,8-bis[(2- ethylhexyl)oxy]benzo[1,2-b:4,5-b']dithiophene-2,6-diyl][3-fluoro-2-[(2-ethylhexyl)- carbonyl]-thieno[3,4-b]thiophenediyl]]) thin films is investigated by in situ grazing incident wide angle x-ray scattering (GIWAXS) and optical reflectance, to better understand polymer solar cell (PSC) optimization approaches. In situ characterization of PTB7 film formation from chloroform (CF), chlorobenzene (CB), and 1,2-dichlorobenzene (DCB) solutions, as well as CB solutions with 1% and 3% v/v of the processing additives 1-chloronapthalene (CN), diphenyl ether (DPE), and 1,8-diiodooctane (DIO), reveals multiple crystallization pathways with: i) single-solvent systems exhibiting rapid (<3s) crystallization after a solvent boiling point-dependent film thinning transition, ii) solvent + additive systems exhibiting different crystallization pathways and crystallite formation times from minutes (CN, DPE) to 2 1.5 hours (DIO). Here, identifying crystalline intermediates has implications for bulk-heterojunction PSC morphology optimization via optimized spin-casting processes.

36 MATERIALS SCIENCE↗