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NASA NTRS1994

Microstructural evolution of diamond growth during HFCVD

High resolution transmission electron microscopy (HRTEM) was used to study the nucleation and growth mechanism of diamond by hot filament chemical vapor deposition (HFCVD) process. A novel technique has shown a direct evidence for the formation of the diamond-like carbon layer 8-14 nm thick in which small diamond micro-crystallites were embedded. These diamond micro-crystallites were formed as a result of transformation of diamond-like carbon into diamond. The diamond micro-crystallites present in the amorphous diamond-like carbon layer provided nucleation sites for diamond growth. Large diamond crystallites were observed to grow from these micro-crystallites. The mechanism of diamond growth will be presented based on experimental findings.

TRT-EXPERIMENTAL↗

DOE OSTI2022

Microstructural evolution and precipitation in γ-LiAlO 2 during ion irradiation

Polycrystalline γ-LiAlO 2 pellets were sequentially irradiated with 120 keV He + and 80 keV D 2 + ions to the fluences of 1 × 10 17 and 2 × 10 17 (He + + D + )/cm 2 at 573 K. Additional irradiation was performed to a fluence of 2 × 10 17 (He + + D + )/cm 2 at 773 K. The irradiated pellets were characterized using scanning transmission electron microscopy, time-of-flight secondary ion mass spectrometry, and grazing incidence x-ray diffraction. Lattice damage, amorphization, and fractures are observed with no evidence for the formation of secondary-phase precipitates in the pellets irradiated up to an ion fluence of 2 × 10 17 (He + + D + )/cm 2 at 573 K. In contrast, faceted precipitates with sizes larger than 100 nm formed in a pellet irradiated to 2 × 10 17 (He + + D + )/cm 2 at 773 K. Analyses of the diffraction and composition data suggest that the precipitates have a spinel-type structure, likely a non-stoichiometric LiAl 5 O 8 with Li depletion. This could be an intermediate phase with Li atoms at the octahedral and possibly tetrahedral sites as well. It is speculated that as the dose increases, Li loss will continue and the precipitates will approach a composition of alumina primarily in phases of α-Al 2 O 3 and amorphized Al 2 O 3 .

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

DOE OSTI2018

Evolution of microstructure and microtexture during hot deformation in an advanced P/M nickel base superalloy

Highlights: • Microstructural evolution of PM superalloy sensitive to temperature and strain rate. • Highest DRX with finer grained structure at higher temperatures and strain rates. • Dominance of DDRX showed by serrated grain boundaries and misorientation gradient. • Weak microtextural evolution inclined towards [110] fiber compression texture seen. In the present study, the effect of hot deformation parameters on the microstructural evolution is investigated for an experimental powder metallurgy nickel superalloy. The hot isostatically pressed (HIPed) alloy is isothermally hot compressed at constant true strain rate over wide temperatures (1000 °C, 1050 °C, 1100 °C, 1150 °C) and strain rates (0.001 s{sup −1}, 0.01 s{sup −1}, 0.1 s{sup −1}, 1 s{sup −1}) regimes. Electron Back-Scattered Diffraction (EBSD) characterization of the hot deformed samples is carried out to evaluate the microstructural evolution, grain boundary characteristics, and microtextural behaviour. The strong dependence of dynamic recrystallization characteristics on the hot deformation conditions is divulged through EBSD derived colour inverse pole figure maps endorsed by grain/twin boundary characteristics and misorientation gradient. Dynamic recrystallization (DRX) is maximized at higher deformation temperatures, whereas limited DRX is observed at lower deformation temperatures, especially at higher strain rates. The dominance of discontinuous dynamic recrystallization (DDRX) is manifested through bulged/serrated grain boundaries resulting in the formation of necklace microstructure corroborated by grain boundary cumulative misorientation gradient. Although random microtexture is revealed in both deformed and recrystallized microstructures, the tendency towards the formation of 110 fiber compression texture is apparently evident.

36 MATERIALS SCIENCE↗

DOE OSTI2019

Effect of Heat Treatment on Microstructure Evolution and Mechanical Properties of Selective Laser Melted Inconel 718 Alloy

The microstructure characteristics of the selective laser melted Inconel 718 alloy under as-deposited, homogenization + solution + aging (HSA) and solution + aging (SA) conditions were studied. The anisotropy and heterogeneity of mechanical properties under different conditions were also investigated. Under the as-deposited condition, the morphology and size of the grains are heterogeneous. The dendrite structures which grow nearly perpendicular to the molten pool traces, accompanying interdendritic Laves phase, can be observed within the grains. The dendrite structure completely disappeared, and the Laves phases embedded in the interdendritic regions also dissolved into the matrix to precipitate γ′ and γ″ phases after heat treatments. Fully recrystallized grains were obtained under the HSA condition, while only incomplete recrystallized grains were obtained under the SA condition. However, the characteristics of γ′ and γ″ phases are very similar under the HSA and SA conditions. Significant improvement in strength after heat treatments was due to the dissolution of undesirable Laves phase and the precipitation of γ′ and γ″ phases. For all the three conditions, different tensile properties were observed depending on the orientation of the specimens. The scatter of mechanical properties is notable, and heat treatments increased the scatter of mechanical properties.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Microstructure evolution of T91 irradiated in the BOR60 fast reactor

In this paper, microstructures of T91 neutron irradiated in the BOR60 reactor at five temperatures between 376 °C and 524 °C to doses between 15.4 and 35.1 dpa were characterized using transmission electron microscopy (TEM), scanning transmission electron microscopy (STEM), and atom probe tomography (APT). Type a<100> dislocation loops were observed at 376–415 °C and network dislocations dominated at 460 °C and 524 °C. Cavities appeared in a bimodal distribution with a high density of small bubbles less than 2 nm at irradiation temperatures between 376 °C and 415 °C. Small bubbles were also observed at 460 °C and 524 °C but cavities greater than 2 nm were absent. Enrichment of Cr, Ni, and Si at the grain boundary was observed at all irradiation temperatures. Radiation-induced segregation (RIS) of Cr, Ni and Si appeared to saturate at 17.1 dpa and 376 °C. The temperature dependence of RIS of Cr, Ni and Si at the grain boundary, which showed a peak Cr enrichment temperature of 460 °C and a lower peak Ni and Si enrichment temperature of ~400 °C, was consistent with observations of RIS of Cr in proton irradiated T91, suggesting that the same RIS mechanism may also apply to BOR60 irradiated T91. G-phase and Cu-rich precipitates were observed at 376–415 °C but were absent at 460 °C and 524 °C. Finally, the absence of G-phase at 524 °C could be related to the minimal segregation of Ni and Si in that condition.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

NASA NTRS2016

Microstructure Evolution and Durability of Advanced Environmental Barrier Coating Systems for SiC/SiC Ceramic Matrix Composites

Environmental barrier coated SiC-SiC ceramic matrix composites (CMCs) systems will play a crucial role in next generation turbine engines for hot-section component applications because of their ability to significantly increase engine operating temperatures with improved efficiency, reduce engine weight and cooling requirements. Advanced HfO2 and rare earth silicate environmental barrier coatings (EBCs), along with multicomponent hafnium and rare earth silicide EBC bond coats have been developed. The coating degradation mechanisms in the laboratory simulated engine thermal cycling, and fatigue-creep operating environments are also being investigated. This paper will focus on the microstructural and compositional evolutions of an advanced environmental barrier coating system on a SiC-SiC CMC substrate during the high temperature simulated durability tests, by using a Field Emission Gun Scanning Electron Microscopy, Energy Dispersive Spectroscopy (EDS) and Wavelength Dispersive Spectroscopy (WDS). The effects of Calcium-Magnesium-Alumino-Silicate (CMAS) from road sand or volcano-ash deposits on the degradation mechanisms of the environmental barrier coating systems will also be discussed. The detailed analysis results help understand the EBC-CMC system performance, aiming at the durability improvements to achieve more robust, prime-reliant environmental barrier coatings.

ceramic matrix composites↗

DOE OSTI2019

Influence of Single-Point Incremental Force Process Parameters on Forming Characteristics and Microstructure Evolution of AA-6061 Alloy Sheet

Single-point incremental forming (SPIF) process comprises a set of process variables, such as forming tool diameter, vertical pitch, spindle rotation speed, and tool velocity, which may affect the forming behavior of the sheet to be deformed. The objective of this work is to study the effect of SPIF process parameters on forming characteristics and microstructure development for the AA-6061 (T6) aluminum alloy sheet. The SPIF experiments and finite element (FE) simulations were performed at different process parameters to achieve conical shapes from the AA-6061 blanks. The effect of process parameters on forming forces, thickness uniformity in wall region of the cone and surface roughness of the blank was analyzed. A detailed microstructure study was performed to analyze the effect of process variables on microstructure and texture evolution during the SPIF process. This study reveals that the process parameters are likely to influence the texture development especially at high tool diameter and vertical pitch values. Therefore, suitability and consequences of using different combinations of tool diameter and vertical pitch values are discussed for AA-6061 alloy.

36 MATERIALS SCIENCE↗

NASA NTRSDate not supplied

Three-dimensional in Situ Observations of Polycrystalline Microstructure Evolution During Directional Solidification of Transparent Alloys Aboard the ISS and Quantitative Comparison with Numerical Modeling

Cellular/dendritic microstructures formed during solidification have a crucial influence on the mechanical properties of a wide range of structural alloys. By minimizing the amount of gravity-induced convection in the liquid, directional solidification experiments using transparent organic alloys conducted in the DECLIC-DSI onboard the International Space Station have provided unique 3D in situ observations of the spatiotemporal evolution of the solid-liquid interface during the formation of cellular and dendritic microstructures under purely diffusive growth conditions in polycrystalline samples containing several grains with a small misorientation with respect to the temperature gradient. Those observations have made it possible to perform benchmark quantitative comparisons with the predictions of state-of-the-art phase-field simulations of microstructure formation in 3D on experimentally relevant length and time scales. This talk will report quantitative comparisons between microgravity experiments and phase-field simulations in succinonitrile-camphor alloys of two different compositions that shed new light on the role of subgrain boundaries in the spatiotemporal evolution of the primary cellular spacing and the selection of dendritic array structures.

Kaihua Ji↗

NASA NTRSDate not supplied

Three-Dimensional In Situ Observations of Polycrystalline Microstructure Evolution During Directional Solidification of Transparent Alloys Aboard the ISS and Quantitative Comparison with Numerical Modeling

Cellular/dendritic microstructures formed during solidification have a crucial influence on the mechanical properties of a wide range of structural alloys. By minimizing the amount of gravity-induced convection in the liquid, directional solidification experiments using transparent organic alloys conducted in the DECLIC-DSI onboard the International Space Station have provided unique 3D in situ observations of the spatiotemporal evolution of the solid-liquid interface during the formation of cellular and dendritic microstructures under purely diffusive growth conditions. Those observations have made it possible to perform benchmark quantitative comparisons with the predictions of state-of-the-art phase-field simulations of microstructure formation in 3D on experimentally relevant length and time scales. This talk will report quantitative comparisons between microgravity experiments and phase-field simulations in succinonitrile-camphor alloys of two different compositions, which shed new light on the selection of dendritic array structures, and on roles of macroscopic curvatures and subgrain boundaries between grains with a small misorientation with respect to the temperature gradient in the spatiotemporal evolution of the primary cellular spacing.

Kaihua Ji↗

DOE OSTI2016

A variational treatment of material configurations with application to interface motion and microstructural evolution

We present a unified variational treatment of evolving configurations in crystalline solids with microstructure. The crux of our treatment lies in the introduction of a vector configurational field. This field lies in the material, or configurational, manifold, in contrast with the traditional displacement field, which we regard as lying in the spatial manifold. We identify two distinct cases which describe (a) problems in which the configurational field's evolution is localized to a mathematically sharp interface, and (b) those in which the configurational field's evolution can extend throughout the volume. The first case is suitable for describing incoherent phase interfaces in polycrystalline solids, and the latter is useful for describing smooth changes in crystal structure and naturally incorporates coherent (diffuse) phase interfaces. These descriptions also lead to parameterizations of the free energies for the two cases, from which variational treatments can be developed and equilibrium conditions obtained. For sharp interfaces that are out-of-equilibrium, the second law of thermodynamics furnishes restrictions on the kinetic law for the interface velocity. The class of problems in which the material undergoes configurational changes between distinct, stable crystal structures are characterized by free energy density functions that are non-convex with respect to configurational strain. For physically meaningful solutions and mathematical well-posedness, it becomes necessary to incorporate interfacial energy. This we have done by introducing a configurational strain gradient dependence in the free energy density function following ideas laid out by Toupin (Arch. Rat. Mech. Anal., 11, 1962, 385-414). The variational treatment leads to a system of partial differential equations governing the configuration that is coupled with the traditional equations of nonlinear elasticity. The coupled system of equations governs the configurational change in crystal structure, and elastic deformation driven by elastic, Eshelbian, and configurational stresses. As a result, numerical examples are presented to demonstrate interface motion as well as evolving microstructures of crystal structures.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Microstructural evolution of a silicon carbide-carbon coated nanostructured ferritic alloy composite during in-situ Kr ion irradiation at 300°C 450°C

This work focuses on irradiation behaviors of a novel silicon carbide and carbon coated nanostructured ferritic alloy (SiC-C@NFA) composite for potential applications as a cladding and structural material for next generation nuclear reactors. The SiC-C@NFA samples were irradiated with 1 MeV Kr ions up to 10 dpa at 300 and 450 °C. Microstructures and defect evolution were studied in-situ at the IVEM-Tandem facility at Argonne National Laboratory. The effects of ion irradiation on various phases such as α-ferrite matrix, (Fe,Cr) 7 C 3 , and (Ti,W)C precipitates were evaluated. The α-ferrite matrix showed a continuous increase in dislocation density along with spatial ordering of dislocation loops (or loop strings) at >5 dpa. The size of the dislocation loops at 450 °C was larger than that at 300 °C. The nucleation and growth of new (Ti,W)C precipitates in α-ferrite grains were enhanced with the ion dose at 450 °C. This study provides new insight into the irradiation resistance of the SiC-C@NFA system.

(FeCr)(7)C-3↗

DOE OSTI2019

Investigation of the mechanical and microstructural evolution of a Cu based bulk metallic glass during ion irradiation

Ion irradiation and annealing experiments were performed on Cu 60 Zr 20 Hf 10 Ti 10 bulk metallic glass (BMG) specimens to investigate their irradiation- and temperature-induced microstructural and mechanical property evolution. For the ion irradiations, samples were exposed to 9 MeV Ni 3+ ions to a midrange (~1.2 μm depth) dose of 10 displacements per atom (dpa) at temperatures ranging from room temperature to 360 °C (the corresponding peak dose at ~2.8 μm depth was ~25 dpa). Bulk X-ray diffraction (XRD) and transmission electron microscopy (TEM) characterization revealed that the alloy did not crystallize during irradiation up to 290 °C but did partially crystallize at 360 °C. XRD analysis revealed that the crystallization which occurred in the sample irradiated at 360 °C was caused by thermal effects instead of irradiation displacement damage. Subsequent Rietveld refinement analysis of the XRD measurements revealed the presence of two distinct crystal phases, namely a CuTiZr hexagonal structure belonging to the P63/mmc space group and a CuTi tetragonal structure belonging to the P4/mmm space group. Nanoindentation experiments revealed that no pronounced hardness changes occurred in the specimens irradiated at room temperature and 290°C, although significant hardening was observed in the sample irradiated at 360 °C. The significant increase in the hardness at 360°C was ascribed to thermally induced partial crystallization of the alloy instead of the ion irradiation. In general, the results of the nanoindentation experiments and XRD characterization suggest that although the Cu BMG exhibits good stability during irradiation at temperatures up to 290 °C it is not suitable for irradiation environments where the temperature is 360 °C for extended periods of time. The Lam and Chong extrapolation method, which has been used to study the indentation size effect (ISE) in amorphous alloys, was employed to quantify how irradiation and temperature affect this type of behavior in the BMG. However, the poor linear fitting of the indentation hardness data by this model indicate that a new ISE model is likely needed to quantify indentation hardening in BMGs.

36 MATERIALS SCIENCE↗

DOE OSTI2017

Microstructural evolution in Fe-20Cr-25Ni austenitic alloys under proton irradiation at 670 ºC

Austenitic stainless steels (SSs) are widely used in different components of nuclear plants. The NF709 (20Cr-25Ni-1.5MoTiNb) class of alloy was recently selected for development as a candidate structural material for sodium-cooled fast reactors due to its improved creep and corrosion resistance compared with 300-series austenitic SSs. This requires new understanding of the radiation response of the 709 class alloys. In this study, we correlated the mechanical changes with the proton-induced microstructural and chemical evolutions of a 20Cr-25Ni model alloy M709 and a 20Cr-25Ni-1.5MoNb alloy A709. The irradiation was conducted using 2 MeV protons at 670 ± 20 ºC to achieve 1.5 displacements per atom (dpa) at the middle of the proton project range. Sample characterization was achieved using nanoindentation, focused ion beam (FIB), scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS) and transmission electron microscopy techniques (TEM).

Chen, Tianyi↗

DOE OSTI2019

Effects of Multiple Laser Peening impacts on Mechanical Properties and Microstructure Evolution of 40CrNiMo Steel

The effects of multiple laser peening impacts on mechanical properties and microstructure of 40CrNiMo steel were investigated. The surface residual stress and microhardness of the samples with different treatments were measured. The surface morphologies, tensile behavior and microstructure of the samples before and after laser peening were compared and analyzed. The experimental results showed that laser peening, especially multiple laser peening impacts has significant effects on the microhardness, residual stress and microstructure of 40CrNiMo steel. The surface roughness and the depth of the pit increased with increasing the impact times. After 3 laser peening impacts, the surface microhardness, compressive residual stress, the strength and ductility were significantly improved. Meanwhile, some microstructures, such as sub-grains, the precipitation of carbide and dislocations were also induced in the surface layer. Additionally, the microscopic strengthening mechanism of multiple laser peening impacts on the mechanical properties of 40CrNiMo steel was analyzed in detail.

36 MATERIALS SCIENCE↗

DOE OSTI2017

Microstructural evolution and thermal stability after aging of a cobalt-containing martensitic bearing steel

The microstructural changes and thermal stability of a cobalt-containing martensitic heat resistance bearing steel have been investigated in this paper. The hardness variation showed a progressive hardness decrease associated with coarsening of fine carbides at elevated temperatures. The precipitation of secondary phases during tempering at 500 °C for 10 h and 100 h has been characterized and identified in detail using transmission electron microscopy. The results revealed that the aging treatment induced very fine secondary M{sub 6}C precipitates which were responsible for the secondary hardening peak when tempered at 500 °C for 30 h. But the hardness gradually decreased due to the coarsening of M{sub 6}C carbide and other secondary phases (such as μ phase, σ phase, and χ phase) precipitation when the samples were tempered over 30 h at 500 °C. - Highlights: •Retained austenite fraction was reduced after cryogenic treatment. •Secondary hardening was responsible for M{sub 6}C precipitates. •TEM study to investigate different phases characteristics •Coarsening of carbides during aging has a significant effect on mechanical properties.

36 MATERIALS SCIENCE↗

DOE OSTI2017

Probing Novel Microstructural Evolution Mechanisms in Aluminum Alloys Using 4D Nanoscale Characterization

Dispersions of nanoscale precipitates in metallic alloys have been known to play a key role in strengthening, by increasing their strain hardenability and providing resistance to deformation. Although these phenomena have been extensively investigated in the last century, the traditional approaches employed in the past have not rendered an authoritative microstructural understanding in such materials. The effect of the precipitates’ inherent complex morphology and their 3D spatial distribution on evolution and deformation behavior have often been precluded. This study reports, for the first time, implementation of synchrotron-based hard X-ray nanotomography in Al–Cu alloys to measure kinetics of different nanoscale phases in 3D, and reveals insights behind some of the observed novel phase transformation reactions. The experimental results of the present study reconcile with coarsening models from the Lifshitz–Slyozov–Wagner theory to an unprecedented extent, thereby establishing a new paradigm for thermodynamic analysis of precipitate assemblies. Lastly, this study sheds light on the possibilities for establishing new theories for dislocation–particle interactions, based on the limitations of using the Orowan equation in estimating precipitation strengthening.

36 MATERIALS SCIENCE↗

NASA NTRS1993

The microstructural evolution, crystallography, and thermal processing of ultrahigh carbon Fe-1.85 pct C melt-spun ribbon

A study is presented to determine if fine microstructures could be achieved using rapid solidification to produce a fine-grained fully austenitic starting structure and then using thermal processing cycles to produce an even finer ferrite-cementite structure. The evolution, mechanisms of grain refinement, and crystallography of the resultant microstructures were examined by TEM. A thermal processing cycle consisted of quenching the ribbon in liquid nitrogen, tempering at 600 C for 10 sec, 'upquenching' to 750 C for 10 sec, and subsequently quenching again in liquid nitrogen. The heat-treatment resulted in martensite grains with sizes of about 1 micron or less in both length and thickness and cementite particles of 0.4 micron or less. It is concluded that these microstructures could be used for producing fine-grained ultrahigh carbon steels of very high strength without the brittleness associated with the formation of coarse carbide particles of the loss of strength due to graphite formation.

Spanos, G.↗

DOE OSTI2013

Shape memory properties and microstructural evolution of rapidly solidified CuAlBe alloys

In this work, the effects of Be addition on the microstructure and phase transformation temperatures of Cu–12Al–xBe (x = 0.4, 0.5 and 0.6 wt.%) shape memory alloys fabricated by using the arc-melting and melt-spinning techniques have been investigated. X-ray diffraction analysis revealed that the arc-melted alloys consisted of austenitic β{sub 1}, martensitic β{sub 1}′ and γ{sub 2} precipitate phases, whereas melt-spun ribbons were composed of a fully martensitic phase. The average grain size of martensitic phases in melt-spun ribbons was determined by electron microscopy images, showing a decrease with increasing Beryllium (Be) amount. Moreover, it was found that the Be addition in the arc-melted alloys had a distinct effect on the morphology of the γ{sub 2} precipitate phase. Transmission electron microscopy analysis showed that the thickness of martensitic plates in the melt-spun ribbons reduced with increasing Be addition. In a differential scanning calorimeter analysis, no martensitic transformation (M{sub s}) peak was observed in arc-melted alloys, but it was clearly detected in melt-spun ribbons, in which M{sub s} decreased dramatically with increasing Be addition. The improvement in the shape memory ability of melt-spun ribbons was explained in terms of the refinement in grain size and martensitic plates. - Highlights: • The CuAlBe SMAs were produced by means of arc-melter and melt-spinner techniques. • MT was directly obtained in melt-spuns without any intermediate process. • The transformation temperatures decreased with increasing Be amount. • The thickness of martensitic plates in the ribbons reduced with increasing Be. • SMP of CuAl was improved by the addition of Be together with rapid solidification.

36 MATERIALS SCIENCE↗