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NASA NTRS1998

Microstructural Development of Directionally Solidified Hg(1-x)Zn(x)Se Alloys

Hg(1-x)Zn(x)Se alloys have been studied as an alternative to HgCdTe for the detection of electromagnetic radiation, because the shorter ZnSe and HgSe bonds were predicted to improve lattice stability. Previous studies showed that optical properties were stable with time and that the microhardness was higher than for HgTe based alloys. However, for this material to be commercially viable, compositional variations must be reduced, and the distribution of defects induced by the growth process must be understood. The basic structural properties of bulk materials were characterized, and dislocation etch pit densities were measured to determine whether the addition of Zn to the HgSe lattice reduced the potential for dislocation formation. Hg(0.9)Zn(0.1)Se alloys were directionally solidified using a modified Bridgman-Stockbarger method and in an applied magnetic field. Radial compositional variations were greatly reduced when solidification occurred in an applied magnetic field. The combination of a convex liquid-solid interface shape and a method for reduced wetting produced boules that were a single crystal after reaching full diameter. Observed surface features indicated ampoule wetting could be eliminated using a graphite getter. Microstructural characteristics were greatly improved over HgCdTe alloys, In six boules, a total of only one twin was observed, and no inclusions were found. A method for polishing and producing dislocation etch pits was developed for these alloys, revealing dislocation etch pit densities one to two orders of magnitude less than HgTe based alloys. A kink in the thermal profile during processing of one boule generated more dislocations than did lattice mismatch due to compositional variations. The results of this investigation indicate this alloy has improved microstructural properties and resistance to dislocation formation compared with similar II-VI alloys, and should be further investigated for the detection of electromagnetic radiation.

Cobb, S. D.↗

NASA NTRSDate not supplied

Investigation of the effect of etch pits on the material properties of carbon fiber structures

It is well known that etch pits are formed on carbon surfaces during their consumption in reactive gas environments such as during ablation of carbon-based thermal protection system (TPS) materials. These pits start out from atomic defects on the carbon surface, grow in size and then ultimately lead to the complete removal of the solid carbon material [1, 2]. However, the effect of such etch pits on the material properties of carbon ablators such as FiberForm are poorly understood, as the maximum size of pits are on the order of microns in size, which makes them hard to observe experimentally. Hence, we have developed a module within the Porous Microstructure Analysis code PuMA [3] that can generate etch pits on an arbitrary material surface, with a prescribed distribution of pit size and density. Figure 1 shows a FiberForm sample with artificially generated pits of varying radii and pit density. We use this newly developed module to calculate material properties of FiberForm, which is the base material for one of the most commonly used TPS materials - Phenolic Impregnated Carbon Ablator (PICA). The detailed microstructure of FiberForm in PuMA will either be generated synthetically or obtained from X-ray microtomography [4]. Our simulations show that material properties such as the thermal conductivity and tortuosity decrease with increasing degree of pitting. This will be helpful to more accurately predict the degradation of carbon-based TPS during ablation, and furthermore may allow us to identify previously unknown TPS failure modes due to pitting.

PuMA↗

NASA NTRS2019

Coordinated Analysis of an Ion Irradiated Carbonaceous Chondrite Suggests Complex Space Weathering Effects

Surfaces of airless planetary bodies are exposed to micrometeorite bombardment and solar wind irradiation which alter the microstructural, compositional, and optical properties of regoliths over time. These processes are collectively known as space weathering, and they complicate the interpretation of remote sensing data and the subsequent characterization of airless surfaces. Within the next 5 years, NASA’s OSIRIS-REx (Origins, Spectral Interpretation, Resource Identification, Security, Regolith Explorer) and JAXA (Japan Aerospace Exploration Agency)’s Hayabusa2 missions will return samples from C-type asteroids Bennu and Ryugu, respectively. Compared to the Moon and S-type asteroids, our understanding of the space weathering of C-complex asteroids is limited. In order to maximize scientific return from remote sensing data and to prepare for the analysis of returned samples from these missions, we must better understand the effects of space weathering on hydrated, organic-rich materials. We can do so by simulating these processes in the laboratory. In this study, we simulate solar wind exposure through ion irradiation of the CM2 carbonaceous chondrite Murchison - a suitable analog for C-complex asteroids. Here, we present coordinated analyses of a sample before and after ion irradiation.

Laczniak, D. L.↗

DOE OSTI2020

In situ high-temperature X-ray diffraction study of Sc-doped titanium oxide nanocrystallites

Titanium dioxide is an inexpensive wide-gap highly ionic semiconductor with striking photocatalytic capabilities in several heterogeneous photoredox reactions. A small crystal size is desirable to maximize the surface area, since photocatalytic reactions occur at the surface of a photocatalyst. Presented in this work are the synthesis and microstructural characterization of 4 at.% Sc-doped TiO 2 (4SDT) prepared by water-based co-precipitation. The crystal structure of 4SDT was examined via in situ high-temperature powder X-ray diffraction experiments from 25 to 1200°C. Rietveld analysis revealed single-phase anatase up to 875°C, while at 900°C the anatase-to-rutile phase transformation occurred and at higher temperatures additional reflections of Sc-rich phases (Sc 2 TiO 5 from 975°C and Ti 3 Sc 4 O 12 or Sc 2 O 3 at 1200°C) were observed. Debye function analysis (DFA) was applied to model the total scattering pattern directly in reciprocal space, allowing the reconstruction of Ti vacancies. Both Rietveld and DFA methods were applied to estimate the nanocrystallite size and shape with consistent growth in crystallite size with temperature: an ellipsoid shape with equatorial ~4.7 nm / axial (001) ~6.9 nm at 25°C to equatorial ~27.9 nm / axial (001) ~39.6 nm at 900°C refined by Rietveld analysis, versus a cylinder shape with D a , b = 4.3 nm and size dispersion σ ab = 1.5 nm, L c = 4.9 nm and σ c = 2.3 nm at 25°C to D a , b = 21.4 nm, σ ab = 8.3 nm, L c = 23.9 and σ c = 10.9 nm at 900°C estimated by DFA. The microstructural changes obtained by Rietveld and DFA methods were supported by high-resolution transmission electron microscopy image analysis, as well as by the less direct nitrogen sorption techniques that provide information on the size of non-agglomerated and dense particles. The Ti site-occupancy factor showed a linear increase from 0.6–0.8 at 25°C to unity at 900°C for anatase, and from ~0.7 at 900°C to unity at 1200°C for rutile, via Rietveld analysis and DFA.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Enhancement of γ/γ’ Microstructured Cobalt Superalloys Produced from Atomized Powder by Creating a Harmonic Structure

A material’s properties must be continuously improved to meet the demands of extreme conditions in high-temperature applications. It is demonstrated that γ-γ’ Co-based superalloys could surpass the yield stress of Ni-based superalloys at high temperature due to the γ-γ’ structure. The powders were subjected to a harmonic modification in order to refine the grain structure on the surface and to activate the sintering process. This study examines how harmonic structure affects microstructure and mechanical properties at high temperatures. Spark Plasma Sintering (SPS) was used for consolidation to maintain the ultrafine grain size microstructure of the powder. Compression tests were conducted from room temperature (RT) to 750 °C to assess the mechanical properties of the material. Yield stress values obtained from harmonic structures are four times higher than those obtained from cast alloys.

36 MATERIALS SCIENCE↗

NASA NTRS1986

The evolution and growth of Al2O3 scales on beta-NiAl

The formation and growth of Al2O3 scales on (beta)-NiAl were studied using electron microscopy and other analytical techniques to gain an understanding of the oxidation properties of (beta)-NiAl and of alumina-forming alloys, in general. The transient and mature stages of oxidation were studied as well as the transformation stage during which the oxide scale transforms from metastable Al2O3 phases to the thermodynamically stable alpha-Al2O3 phase. The transient oxidation stages were studied at 800 deg C and for short times at 1100C. At 800C, the scales consist predominantly of delta-Al2O3 which forms by cation vacancy ordering in the defective spinel lattice of gamma-Al2O3. At 1100C, a fast-growth morphology of theta-Al2O3 forms as a surface layer over delta-Al2O3. For both oxidation temperatures, the scales are often epitaxially oriented with respect to the metal. The transient scales grow by outward cation diffusion as evidenced by surface growth morphologies. The transformation to alpha-Al2O3 occurs within 1 hour at 1100C by a nucleation and radial growth process. The large volume decrease associated with the transformation results in a highly strained alpha-Al2O3 microstructure. A change in scale growth mechanism from outward cation to inward anion diffusion allows transient surface morphologies to be smoothed by surface diffusion. The mature stage of oxidation involves the growth of an alpha-Al2O3 scale having the lacey morphology formed as a result of the gamma yields alpha transformation. Growth of the scale occurs by counterdiffusion along grain boundaries resulting in ridges formed by impingement of alpha-Al2O3 nuclei during the transformation stage. Also scale growth occurs by inward oxygen diffusion through healed cracks; the cracks result from transformation stresses. The measured growth rates of scales having the lacey morphology are an order of magnitude less than fine-grained alpha-Al2O3 scales. Metal orientations were found to have a large effect on oxide morpholoies during all stages of oxidation.

Doychak, J. K.↗

DOE OSTI2025

Holistic Microstructure Control Strategies in Photopolymerization‐Induced Phase Separation of Acrylate Systems

Open porous materials, known for their large surface area and interconnected structures, are essential in various applications, including batteries, ion exchange, catalysis, filtration, and electronic waste recycling. A critical aspect of the functionality of porous membranes is the precise control of pore size and morphology. Photopolymerization-induced phase separation (photo-PIPS) offers a convenient and versatile methods for creating porous structures. However, controlling the porous morphology remains challenging due to the complex interplay between thermodynamics, polymerization kinetics, and monomer structures, which makes it difficult to establish the relationship between processing conditions and resulting morphology in photo-PIPS. Herein, a physics-based phase-field model capable of generating and characterizing the microstructures of porous materials based on both average and localized features is developed. Using the phase-field simulations as test bed, the effects of polarity, light intensity, and curing temperature, as well as the previously unexplored roles of chain transfer agents and substrates, on the morphology of the resulting porous microstructure are investigated. Experiments are performed to verify the results predicted by the simulations. This work lays out a comprehensive guide for designing PIPS-derived porous microstructures and offers practical engineering strategies for tailoring microstructure-level topology and size of pores for application-specific needs.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Machinability comparison of additively manufactured and traditionally wrought Ti-6Al-4V alloys using single-point cutting

Post-machining is often needed to provide high dimensional accuracy and fine surface finish for additively manufactured Ti-6Al-4V (Ti64). The material inhomogeneity, such as pores and microstructures, can affect the machining behavior of this already difficult-machine alloy. This study adopts a holistic approach to compare the machinability of additively manufactured and traditionally wrought Ti64 in terms of key machining factors, including forces, temperature, and vibration and the major machining outcomes including tool life, surface finish, and dimensional accuracy. Stress-relief annealing is applied to each of the part conditions as a secondary variable to observe the additional effects. The results show that AM is not particularly more difficult to machine in terms of cutting force and temperature, but it creates high cutting vibrations across a wide range of frequencies (to and over 5 kHz). The high vibrations do not lead to worse surface finish or dimensional accuracy but tend to worsen the tool life by chipping off the cutting edge. The vibration can be attributed to the brittle martensitic microstructure found in additively manufactured Ti64, which is also evidenced by the more serrated chips. Stress-relieving is found to change the microstructure and reduce the level of vibration to that of the wrought counterpart.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Crystalline Loading of Lipophilic Coenzyme Q10 Pharmaceuticals within Conjugated Carbon Aerogel Derivatives

Low-density aerogel materials currently are being considered for applications in controlling the rate of release for small-molecule pharmaceuticals in vivo. In particular, silica (SiO2) aerogels are an intriguing platform for controlling both the absolute amount of drug loading, but also the crystalline state of small molecule pharmaceuticals has been shown to affect drug release kinetics. To date, loading silica aerogel materials with crystalline pharmaceuticals typically require dissolving small molecules in a supercritical solvent (i.e., CO2) before drying to recover the aerogel/drug composite. Here we demonstrate a simple and low-cost method for controlling the crystallinity of the model drug coenzyme Q10 (CoQ10) within carbon aerogel materials by rationally controlling the chemical microstructure of the aerogel to exhibit ?-conjugated (sp2) chemical bonding. In particular, both pyrolyzed graphene and nanodiamond aerogels exhibit enhanced intrinsic drug loading capacity and CoQ10 crystallinity over a broad range of sp2 surface-curvature. In contrast, amorphous carbon aerogel materials are observed to load CoQ10 pharmaceuticals with strictly amorphous microstructure.

Lim, Mathew↗

DOE OSTI2020

Multilayered microstructures with shape memory effects for vertical deployment

This paper presents a fabrication and characterization of multilayered microstructures with shape memory effects enabling large vertical deployment under electro-thermal actuation. Our previous research demonstrated vertical deployment of such microstructures by the effect of thermal mismatch. Development of equiatomic NiTi layers in the multilayered microstructure is investigated further for shape memory effects. Multilayered microstructures are built by sputtered NiTi layers and a lift-off process. Negative photoresist ma-N1420 enables clean lift-off of 500 nm thick NiTi layers by forming a significant undercut profile after development. The parametric study on co-sputter powers for Ti and Ni 50 Ti 50 targets suggests that 100 W RF on Ti target and 200 W DC on Ni 50 Ti 50 target can deposit Ni 49.62 Ti 50.38 layers. X-Ray Diffraction (XRD) and Atomic Force Microscopy (AFM) were used to study the crystal structures and surface topography of NiTi layers. XRD results of post-annealed Ni 49.62 Ti 50.38 layers show coexistence of austenite and martensitic phases at room temperature, suggesting that the transformation temperature of such NiTi layers should be approximate 20 °C. The surface topography of Ni 49.62 Ti 50.38 layers reveals substantial increase of surface roughness at ambient conditions after the annealing. Experimental verification of the multilayered microstructure for vertical deployment was carried out by Signatone Probe Station and Dual Scanning Electron Microscope/Focused Ion Beam (SEM/FIB) system. Finally, a vertical deployment of the two-dimensional (2D) multilayered microstructures for three-dimensional (3D) can be detected by applying a constant voltage of 0.04 V, and the expected 3D deployment displacement is enlarged from 2 μm to 10 μm by introducing the shape memory effect.

42 ENGINEERING↗

DOE OSTI2025

Hydrogen diffusion induced dislocation transformations in a nickel superalloy

The diffusion of hydrogen in metals and alloys induces embrittlement that can adversely affect the structural properties. We examine the adsorption and diffusion of hydrogen in Inconel-718 (IN-718), and scrutinize the ensuing effects on the dislocation behavior in the alloy to elucidate the fundamental mechanisms of hydrogen-microstructure interactions from classical molecular simulations. Hydrogen adsorption increases with time until the surface saturates, while hydrogen diffusion exhibits strong temperature dependence, with diffusion coefficients converging above 1300 K regardless of the initial hydrogen concentration in the alloy. The diffusion in IN-718 is significantly sluggish than in pure Ni, Fe, or Cr, and is strongly impacted by hydrogen concentrations, resulting in an order of magnitude higher diffusion coefficient for hydrogen (10-14 m2/s relative to 10-15 m2/s) at high concentrations, especially below 600 K. Hydrogen diffusion coefficient varies from 10-12 to 10-15 m2/s in IN-718 depending on temperature (500–1400 K). More critically, our results reveal that increasing hydrogen concentration induces microstructural changes in the alloy, transforming perfect dislocations into stair-rods and Shockley partials, with higher temperatures favoring the latter. The results are significant for hydrogen fuel applications to gain insights into the materials chemistry for designing safer and more efficient propulsion systems, particularly in high-performance environments related to controlled hydrogen combustion applications.

Banerjee, Tanumoy↗

NASA NTRSDate not supplied

Simulation of etch pit formation through active sites in carbon fiber micro-structures

Erosion of carbon due to oxidation does not occur uniformly but through localized etch pit formation as a result of active surface sites. In this work we demonstrate a newly developed capability to capture pitting of carbon fiber microstructures such as FiberForm, which is commonly used as the base material for NASA’s spacecraft ablative thermal protection systems (TPS). The simulations are performed at the meso-scale in order to capture the pit formation and growth using direct simulation Monte Carlo (DSMC), specifically using the Stochastic PArallel Rarefied-gas Time-accurate Analyzer (SPARTA) code. Legacy and latest models both assume uniform reactivity of carbon surface sites with oxygen even at the meso-scale level. However, in reality the carbon surface has locally different reaction rates due to the presence of defects at the atomic scale. The defective nature of these sites enhances their reactivity with atmospheric gases compared to the non-defective sites (2-3 orders of magnitude) and are termed as “active sites”. Thus, these sites tend to be the first to react and eventually get removed through the formation of gasses such as CO, CO2, and CN. Their removal results in all the neighboring atoms becoming defective, thus leading to chain reaction of localized carbon removal and formation of etch pits. Capturing the formation of pits during the ablation simulation of carbon micro-structures is critical to predicting their structural failure. Recently a detailed surface chemistry framework was developed in SPARTA, capable of incorporating various reaction mechanisms such as adsorption, desorption, Eley-Rideal (ER) and Langmuir-Hinshelwood (LH) mechanisms. We have implemented the capability of a single surface having multiple site sets with different reactivities within this framework. We have used this feature to model the presence of active sites on carbon surfaces, whose reactivity is orders of magnitude higher than that of the passive sites due to the presence of defects. The active site fraction is a property of surface elements within SPARTA and is directly proportional to the local reactivity of each surface element. By introducing an initial distribution of the active site fraction across the carbon surface and propagating it in a manner that mimics the evolution of real reacting carbon surfaces, we can capture the formation and growth of etch pits as a result of surface consumption reactions such as oxidation.

DSMC↗

NASA NTRSDate not supplied

Simulation of Etch Pit Formation in DSMC Through Active Sites in Carbon Fiber Micro-Structures

Erosion of carbon due to oxidation does not occur uniformly but through localized etch pit formation because of active surface sites. In this work we demonstrate a newly developed capability to capture pitting of carbon fiber microstructures such as FiberForm, which is commonly used as the base material for NASA’s spacecraft ablative thermal protection systems (TPS). The simulations are performed at the meso-scale in order to capture the pit formation and growth using direct simulation Monte Carlo (DSMC), specifically using the Stochastic PArallel Rarefied-gas Time-accurate Analyzer (SPARTA) code. Legacy and latest models both assume uniform reactivity of carbon surface sites with oxygen even at the meso-scale level. However, in reality the carbon surface has locally different reaction rates due to the presence of defects at the atomic scale. The defective nature of these sites enhances their reactivity with atmospheric gases compared to the non-defective sites (2-3 orders of magnitude) and are termed as “active sites”. Thus, these sites tend to be the first to react and eventually get removed through the formation of gases such as CO, CO2, and CN. Their removal results in all the neighboring atoms becoming defective, thus leading to chain reaction of localized carbon removal and formation of etch pits. Capturing the formation of pits during the ablation simulation of carbon micro-structures is critical to predicting their structural failure. Recently a detailed surface chemistry framework was developed in SPARTA, capable of incorporating various detailed surface reaction mechanisms. We have implemented the capability of a single surface having multiple site sets with different reactivities within this framework. We have used this feature to model the presence of active sites on carbon surfaces, whose reactivity is orders of magnitude higher than that of the passive sites due to the presence of defects. The active site fraction is a property of surface elements within SPARTA and is directly proportional to the local reactivity of each surface element. By introducing an initial distribution of the active site fraction across the carbon surface and propagating it in a manner that mimics the evolution of real reacting carbon surfaces, we can capture the formation and growth of etch pits as a result of surface consumption reactions such as oxidation.

DSMC↗

NASA NTRSDate not supplied

DSMC Simulation of Etch Pit Formation Through Active Sites in Carbon Fiber Micro-Structures

DSMC↗

DOE OSTI2021

Additive manufacturing of cobalt-based alloy on tool steel by directed energy deposition

Cladding hard-surfacing alloys on tool steel is an effective approach to enhance the surface properties of tool steel. In this study, a Co-based alloy was deposited on tool steel by Directed Energy Deposition (DED) following a three-factor three-level design of experiment matrix with varied laser power, scan speed, and powder flow rate. The microstructure of the deposits was characterized using scanning electron microscopy (SEM). The residual stress on the surface of the samples was measured by the X-ray diffraction (XRD) sin2? technique. The parameters that produced promising deposits were used to fabricate samples for tensile test, four-point bending test, Charpy impact test, and hardness measurement. Our result reveals that the processing parameters have a significant role in the residual stress of the coatings. Residual stress reduces with the increase of laser energy density. Cracks were found at samples with energy density below a threshold. Tensile testing of the coating/substrate combined structure reveals fracture at the coatings with an ultimate tensile strength of 633.9 ± 54.7 MPa. The bi-material interface survived the tensile test, indicating a strong interfacial bond. The four-point bending test of coating/substrate laminates shows an ultimate flexure strength of 860.6 ± 36.9 MPa. Cracks initiated from the coatings ignored the interface and penetrated the substrate, suggesting a solid bi-material bond. Charpy impact test shows the absorbed energy of coating/substrate laminates is more than doubled that of the substrate.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Microstructural banding of directed energy deposition-additively manufactured 316L stainless steel

The microstructures of 316 L stainless steel created by rapid solidification are investigated here by comparing the similar microstructures of individual hatches of directed energy deposition additive manufacturing (DED-AM) and those of single, laser surface-melted tracks formed on a solid plate. High recoil pressure, which is exponentially dependent on the laser beam power density, induces convection of the melt pool, which causes formation of microstructural bands in the as-solidified microstructure. The microstructural bands are associated with changes in the chromium concentration and are a significant component of the inhomogeneous microstructure of DED-AM.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Effect of Hot Isostatic Pressing on the Microstructure and Mechanical Properties of Additively Manufactured Ti Alloys

A previous SAND report, SAND2020-11353 described the basic metallurgical and surface roughness properties of additively manufactured Ti-64 material made using a powder bed fusion process. As part of that work, material was post-processed using a hot isostatic press (HIP) to densify and heat treat the material. This report is meant as an addendum to the original report and to provide specific data on material processed with HIP. The main focus of this report is to show the effects of HIP on the microstructure and mechanical properties of AM Ti-64 and Ti-5553.

36 MATERIALS SCIENCE↗

NASA NTRS2016

The Microstructure of Lunar Micrometeorite Impact Craters

The peak of the mass flux of impactors striking the lunar surface is made up of objects approximately 200 micrometers in diameter that erode rocks, comminute regolith grains, and produce agglutinates. The effects of these micro-scale impacts are still not fully understood. Much effort has focused on evaluating the physical and optical effects of micrometeorite impacts on lunar and meteoritic material using pulsed lasers to simulate the energy deposited into a substrate in a typical hypervelocity impact. Here we characterize the physical and chemical changes that accompany natural micrometeorite impacts into lunar rocks with long surface exposure to the space environment (12075 and 76015). Transmission electron microscope (TEM) observations were obtained from cross-sections of approximately 10-20 micrometers diameter craters that revealed important micro-structural details of micrometeorite impact processes, including the creation of npFe (sup 0) in the melt, and extensive deformation around the impact site.

Noble, S. K.↗