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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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All sourcesNASA NTRSDOE OSTI
NASA NTRS2004

Quantification Of 4H- To 3C-Polymorphism In Silicon Carbide (SiC) Epilayers And An Investigation Of Recombination-Enhanced Dislocation Motion In SiC By Optical Emission Microscopy (Oem) Techniques

Environments that impose operational constraints on conventional silicon-(Si) based semiconductor devices frequently appear in military- and space-grade applications. These constraints include high temperature, high power, and high radiation environments. Silicon carbide (SiC), an alternative type of semiconductor material, has received abundant research attention in the past few years, owing to its radiation-hardened properties as well as its capability to withstand high temperatures and power levels. However, the growth and manufacture of SiC devices is still comparatively immature, and there are severe limitations in present crystal growth and device fabrication processes. Among these limitations is a variety of crystal imperfections known as defects. These imperfections can be point defects (e.g., vacancies and interstitials), line defects (e.g., edge and screw dislocations), or planar defects (e.g., stacking faults and double-positioning boundaries). All of these defects have been experimentally shown to be detrimental to the performance of electron devices made from SiC. As such, it is imperative that these defects are significantly reduced in order for SiC devices to become a viable entity in the electronics world. The NASA Glenn High Temperature Integrated Electronics & Sensors Team (HTIES) is working to identify and eliminate these defects in SiC by implementing improved epitaxial crystal growth procedures. HTIES takes two-inch SiC wafers and etches patterns, producing thousands of mesas into each wafer. Crystal growth is then carried out on top of these mesas in an effort to produce films of improved quality-resulting in electron devices that demonstrate superior performance-as well as fabrication processes that are cost-effective, reliable, and reproducible. In this work, further steps are taken to automate HTIES' SiC wafer inspection system. National Instruments LabVIEW image processing and pattern recognition routines are developed that are capable of quantifying and mapping defects on both the substrate and mesa surfaces, and of quantifying polymorphic changes in the grown materials. In addition, an optical emission microscopy (OEM) system is developed that will facilitate comprehensive study of recombination-enhanced dislocation motion (REDM).

Speer, Kevin M.↗
DOE OSTI2014

Nucleation and growth of Pt nanoparticles on reduced and oxidized rutile TiO{sub 2} (110)

The nucleation and growth of Pt nanoparticles (NP’s) on rutile TiO{sub 2} (110) surfaces with O on-top atoms (oxidized TiO{sub 2}), surface O vacancies, and H adatoms, respectively (reduced TiO{sub 2}), was studied by means of scanning tunneling microscopy (STM) experiments and density functional theory calculations. At room temperature, Pt was found to be trapped at O on-top atoms and surface O vacancies, leading to rather small Pt NP’s. In contrast, on surfaces with H adatoms the mobility of Pt was much larger. As a result, large Pt NP's were found at room temperature on TiO{sub 2} (110) surfaces with H adatoms. However, at ∼150 K the diffusion of Pt was kinetically hindered on all TiO{sub 2} (110) surfaces considered. STM data acquired after vacuum-annealing at 800 K showed comparable results on all TiO{sub 2} (110) surfaces because the diffusion of Pt is not influenced by surface defects at such high temperatures.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2016

Characterization of bond line discontinuities in a high-Mn TWIP steel pipe welded by HF-ERW

In this work, the microstructure and defects in a high-frequency electrical resistance welded (HF-ERW) pipe of high-Mn twinning-induced plasticity (TWIP) steel were characterized. The microstructure of the base metal and the bond line were examined using both optical microscopy and scanning electron microscopy. The features of the bond line were similar to those of conventional steel. Simultaneously, the circumferential ductility was evaluated via a flaring test. It was concluded that the deterioration of the circumferential ductility in a high-Mn TWIP steel pipe was caused by irregular shaped oxide defects and a penetrator that had been formed during welding. Specifically, the penetrator, which is composed of MnO and Mn{sub 2}SiO{sub 4}, was found to be the most influential on the circumferential ductility of the welded pipe. The penetrator was analyzed using both an electron probe micro analyzer and transmission electron microscopy, and the formation sequence of the penetrator was evaluated. - Highlights: •This study focused on applying the HF-ERW process to the seam welding of expandable pipe using TWIP steels. •For improvement of the circumferential ductility, deterioration factors were characterized. •Penetrator which would mainly deteriorate the circumferential ductility consisted of round MnO and Mn{sub 2}SiO{sub 4}. •Metallurgical evidence of existing theory regarding the mechanism of defect formation during the HF-ERW was characterized.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Structural properties and dielectric function of graphene grown by high-temperature sublimation on 4H-SiC(000-1)

Understanding and controlling growth of graphene on the carbon face (C-face) of SiC presents a significant challenge. In this work, we study the structural, vibrational, and dielectric function properties of graphene grown on the C-face of 4H-SiC by high-temperature sublimation in an argon atmosphere. The effect of growth temperature on the graphene number of layers and crystallite size is investigated and discussed in relation to graphene coverage and thickness homogeneity. An amorphous carbon layer at the interface between SiC and the graphene is identified, and its evolution with growth temperature is established. Atomic force microscopy, micro-Raman scattering spectroscopy, spectroscopic ellipsometry, and high-resolution cross-sectional transmission electron microscopy are combined to determine and correlate thickness, stacking order, dielectric function, and interface properties of graphene. The role of surface defects and growth temperature on the graphene growth mechanism and stacking is discussed, and a conclusion about the critical factors to achieve decoupled graphene layers is drawn.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2015

Change in equilibrium position of misfit dislocations at the GaN/sapphire interface by Si-ion implantation into sapphire—I. Microstructural characterization

Much research has been done to reduce dislocation densities for the growth of GaN on sapphire, but has paid little attention to the elastic behavior at the GaN/sapphire interface. In this study, we have examined effects of the addition of Si to a sapphire substrate on its elastic property and on the growth of GaN deposit. Si atoms are added to a c-plane sapphire substrate by ion implantation. The ion implantation results in scratches on the surface, and concomitantly, inhomogeneous distribution of Si. The scratch regions contain a higher concentration of Si than other regions of the sapphire substrate surface, high-temperature GaN being poorly grown there. However, high-temperature GaN is normally grown in the other regions. The GaN overlayer in the normally-grown regions is observed to have a lower TD density than the deposit on the bare sapphire substrate (with no Si accommodated). As compared with the film on an untreated, bare sapphire, the cathodoluminescence defect density decreases by 60 % for the GaN layer normally deposited on the Si-ion implanted sapphire. As confirmed by a strain mapping technique by transmission electron microscopy (geometric phase analysis), the addition of Si in the normally deposited regions forms a surface layer in the sapphire elastically more compliant than the GaN overlayer. The results suggest that the layer can largely absorb the misfit strain at the interface, which produces the overlayer with a lower defect density. Our results highlight a direct correlation between threading-dislocation density in GaN deposits and the elastic behavior at the GaN/sapphire interface, opening up a new pathway to reduce threading-dislocation density in GaN deposits.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Scanning tunneling microscopic and spectroscopic studies on a crystalline silica monolayer epitaxially formed on hexagonal SiC(0001{sup ¯}) surfaces

An epitaxial silicon-oxide monolayer of chemical composition of Si{sub 2}O{sub 3} (the Si{sub 2}O{sub 3} layer) formed on hexagonal SiC(0001{sup ¯}) surfaces has been observed by scanning tunneling microscopy (STM). Filled- and empty-state STM images with atomic resolution support the previously reported model. Typical structural defects in the Si{sub 2}O{sub 3} layer are found to be missing SiO{sub n} (n = 1, 2, 3) molecules. The band gap of the Si{sub 2}O{sub 3} layer obtained by point tunneling spectroscopy is 5.5±0.5 eV, exhibiting considerable narrowing from that of bulk SiO{sub 2}, 8.9 eV. It is proposed that the Si{sub 2}O{sub 3} layer is suitable as a relevant interface material for formation of SiC-based metal-oxide-semiconductor devices.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2021

Nearly hyperuniform, nonhyperuniform, and antihyperuniform density fluctuations in two-dimensional transition metal dichalcogenides with defects

Hyperuniform many-body systems in d-dimensional Euclidean space R d are characterized by completely suppressed (normalized) infinite-wavelength density fluctuations, and appear to be endowed with novel exotic physical properties. Recently, hyperuniform systems of disordered varieties have been observed in the context of various atomic-scale two-dimensional (2D) materials. Here, we analyze the effects of localized defects on the density fluctuations across length scales and on the hyperuniformity property of experimental samples of two-dimensional transition metal dichalcogenides. In particular, we extract atomic coordinates from time series annular dark field-scanning transmission electron microscopy (ADF-STEM) imaging data of 2D tungsten chalcogenides with the 2H structure (Te-doped 2H-WSe 2 ) showing continuous development and evolution of electron-beam induced defects, and construct the corresponding chemical-bonding informed coordination networks between the atoms. We then compute a variety of pair statistics and bond-orientational statistics to characterize the samples. At low defect concentrations, the corresponding materials are nearly hyperuniform, characterized by significantly suppressed scattering at the zero wave-number limit (omitting forward/ballistic scattering). As more defects are introduced, the (approximate) hyperuniformity of the materials is gradually destroyed, and the system becomes non-hyperuniform even when the material still contains a significant amount of crystalline regions. At high defect concentrations, the structures become antihyperuniform with diverging (normalized) large-scale density fluctuations, mimicking those typically observed at the thermal critical points associated with phase transitions. Overall, the defected materials possess varying degrees of orientation order, and there is apparently no intermediate hexatic phase emerging. To understand the observed nearly hyperuniform density fluctuations in the slightly defected materials, we construct a minimalist structural model and demonstrate that the experimental samples can be essentially viewed as perturbed honeycomb crystals with small correlated displacements and double chalcogen vacancies. Moreover, the small correlated displacements alone can significantly degrade hyperuniformity of the perfect honeycomb structure. Therefore, even a small amount of vacancies, when coupled with correlated displacements, can completely destroy hyperuniformity of the system.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2014

Synthesis of Bi{sub 2}S{sub 3} with different sulfur content by conventional high temperature solid state solvothermal route

Bismuth sulfide (Bi{sub 2}S{sub 3}) is a binary chalcogenide compound material belonging to V-VI group of semiconductors. Because of its direct band gap of 1.3 eV and high figure of merit (ZT) value, it is widely used as a thermo electronic-cooling material based on the Peltier effect. The electrical and optical property of Bi{sub 2}S{sub 3} material is strongly dependent on stoichiometric composition, defect chemistry and structure. In this study, we have synthesized Bi{sub 2}S{sub x} (x = 3.15, 3.30, 3.45) compound material with different sulfur content by conventional high temperature solid state solvothermal reaction of bismuth and sulfur. X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive x-ray spectroscopy (EDXS) analysis of synthesized compound materials were carried out to observe crystallinity, surface morphology and composition of elements in the compound. The optical analysis revealed that energy band gap decreases with increase of sulfur content.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2022

Structural and optical properties of cubic GaN on U-grooved Si (100)

Cubic GaN epitaxy on large-area U-grooved silicon (100) dies is demonstrated by metalorganic chemical vapor deposition, and its structural and optical properties are reported. Scanning electron, atomic force, and transmission electron microscopy studies reveal that cubic GaN shows no discernible threading dislocations and a low stacking fault density of 3.27 ± 0.18 × 10 4 cm –1 . Temperature-dependent photoluminescence studies reveal as-grown cubic GaN band edge emission internal quantum efficiency as 25.6% ± 0.9%. Selective etching of the low-temperature AlN buffer layer, SiO 2 sidewalls, and hexagonal-phase GaN is demonstrated, which increases the cubic GaN band edge emission internal quantum efficiency to 31.6% ± 0.8%. This increase is attributed to the decrease in the radiative recombination lifetime via the removal of defective hexagonal-phase GaN. Altogether, cubic GaN on U-grooved silicon with high structural and optical quality is reported, promising its suitability for next-generation devices.

36 MATERIALS SCIENCE↗
NASA NTRS1996

Silicon Carbide Epitaxial Films Studied by Atomic Force Microscopy

Silicon carbide (SiC) holds great potential as an electronic material because of its wide band gap energy, high breakdown electric field, thermal stability, and resistance to radiation damage. Possible aerospace applications of high-temperature, high-power, or high-radiation SiC electronic devices include sensors, control electronics, and power electronics that can operate at temperatures up to 600 C and beyond. Commercially available SiC devices now include blue light-emitting diodes (LED's) and high-voltage diodes for operation up to 350 C, with other devices under development. At present, morphological defects in epitaxially grown SiC films limit their use in device applications. Research geared toward reducing the number of structural inhomogeneities can benefit from an understanding of the type and nature of problems that cause defects. The Atomic Force Microscope (AFM) has proven to be a useful tool in characterizing defects present on the surface of SiC epitaxial films. The in-house High-Temperature Integrated Electronics and Sensors (HTIES) Program at the NASA Lewis Research Center not only extended the dopant concentration range achievable in epitaxial SiC films, but it reduced the concentration of some types of defects. Advanced structural characterization using the AFM was warranted to identify the type and structure of the remaining film defects and morphological inhomogeneities. The AFM can give quantitative information on surface topography down to molecular scales. Acquired, in part, in support of the Advanced High Temperature Engine Materials Technology Program (HITEMP), the AFM had been used previously to detect partial fiber debonding in composite material cross sections. Atomic force microscopy examination of epitaxial SiC film surfaces revealed molecular-scale details of some unwanted surface features. Growth pits propagating from defects in the substrate, and hillocks due, presumably, to existing screw dislocations in the substrates, were imaged. Away from local defects, step bunching was observed to yield step heights of hundreds of angstroms, with possible implications for the uniformity of dopants incorporated in SiC devices during fabrication. The quantitative topographic data from the AFM allow the relevant defect information to be extracted, such as the size and distribution of step bunching and the Burgers vector of screw dislocations. These atomic force microscopy results have furthered the understanding of the dynamic epitaxial SiC growth process. A model describing the observed hillock step bunching has been proposed. This cooperation between researchers involved in crystal growth, electronic device fabrication, and surface structural characterization is likely to continue as atomic force microscopy is used to improve SiC films for high-temperature electronic devices for NASA's advanced turbine engines and space power devices, as well as for future applications in the automotive industry.

Source record↗
DOE OSTI2023

In situ observation of medium range ordering and crystallization of amorphous TiO 2 ultrathin films grown by atomic layer deposition

The evolution of medium range ordering (MRO) and crystallization behavior of amorphous TiO 2 films grown by atomic layer deposition (ALD) were studied using in situ four-dimensional scanning transmission electron microscopy. The films remain fully amorphous when grown at 120 °C or below, but they start showing crystallization of anatase phases when grown at 140 °C or above. The degree of MRO increases as a function of temperature and maximizes at 140 °C when crystallization starts to occur, which suggests that crystallization prerequires the development of nanoscale MRO that serves as the site of nucleation. In situ annealing of amorphous TiO 2 films grown at 80 °C shows enhancement of MRO but limited number of nucleation, which suggests that post-annealing develops only a small portion of MRO into crystal nuclei. The MRO regions that do not develop into crystals undergo structural relaxation instead, which provides insights into the critical size and degree of ordering and the stability of certain MRO types at different temperatures. In addition, crystallographic defects were observed within crystal phases, which likely negate corrosion resistance of the film. Our result highlights the importance of understanding and controlling MRO for optimizing ALD-grown amorphous films for next-generation functional devices and renewable energy applications.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Defect evolution in single crystalline tungsten following low temperature and low dose neutron irradiation

The tungsten plasma-facing components of fusion reactors will experience an extreme environment including high temperature, intense particle fluxes of gas atoms, high-energy neutron irradiation, and significant cyclic stress loading. Irradiation-induced defect accumulation resulting in severe thermo-mechanical property degradation is expected. For this reason, and because of the lack of relevant fusion neutron sources, the fundamentals of tungsten radiation damage must be understood through coordinated mixed-spectrum fission reactor irradiation experiments and modeling. In this study, high-purity (110) single-crystal tungsten was examined by positron annihilation spectroscopy and transmission electron microscopy following low-temperature (~90 °C) and low-dose (0.006 and 0.03 dpa) mixed-spectrum neutron irradiation and subsequent isochronal annealing at 400, 500, 650, 800, 1000, 1150, and 1300 °C. The results provide insights into microstructural and defect evolution, thus identifying the mechanisms of different annealing behavior. Following 1 h annealing, ex situ characterization of vacancy defects using positron lifetime spectroscopy and coincidence Doppler broadening was performed. The vacancy cluster size distributions indicated intense vacancy clustering at 400 °C with significant damage recovery around 1000 °C. Coincidence Doppler broadening measurements confirm the trend of the vacancy defect evolution, and the S–W plots indicate that only a single type of vacancy cluster is present. Furthermore, transmission electron microscopy observations at selected annealing conditions provide supplemental information on dislocation loop populations and visible void formation. This microstructural information is consistent with the measured irradiation-induced hardening at each annealing stage. This provides insight into tungsten hardening and embrittlement due to irradiation-induced matrix defects.

Hu, Xunxiang↗
DOE OSTI2025

Influence of Process Parameter and Build Rate Variations on Defect Formation in Laser Powder Bed Fusion SS316L

Laser powder bed fusion (LPBF) is an additive manufacturing process that has gained interest for its material fabrication due to multiple advantages, such as the ability to print parts with small feature sizes, good mechanical properties, reduced material waste, etc. However, variations in the key process parameters in LPBF may result in the instantiation of porosity defects and variation in build rate. Particularly, volumetric energy density (VED) is a variable that encapsulates a number of those parameters and represents the amount of energy input from the laser source to the feedstock. VED has been traditionally used to inform the quality of the printed part but different values of VED are presented as optimal values for certain material systems. An optimal VED value can be maintained by changing the key process parameters so that various combinations yield a constant value. In this study, an optimal constant VED value is maintained while printing SS316L with variable key processing parameters. Porosity analysis is performed using optical microscopy, as well as X-ray computed tomography, to reveal the volume density and distribution of those pores. Two primary defect categories are identified, namely lack of fusion and porosity induced by balling defects. The findings indicate that, even at optimal VED, variations in process parameters can significantly influence defect type, underscoring the sensitivity of defect formation to the variation of these parameters. Furthermore, a minor change in the build rate, driven by adjustments in process parameters, was found to influence defect categories. These findings emphasize that fine tuning the process parameters and build rate is essential to minimize defects. Finally, fiducial marks have been identified as a source of unintentional porosity defects. These results enable the refinement of process parameters, ultimately optimizing LPBF to achieve enhanced material density and expedite the printing.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Epitaxial Si encapsulation of highly misfitting SiC quantum dot arrays formed on Si (001)

This work examines Si overgrowth to encapsulate 3C-SiC quantum dot arrays epitaxially grown on Si substrates. Using transmission electron microscopy, we show how the crystalline quality of the Si cap depends on the growth conditions. Overgrowth at 300 °C leads to a planar, epitaxial Si cap, but with small crystallographic rotations in the cap above each quantum dot. At 400 °C growth temperature, Si exhibits reduced sticking to the SiC, leading to a non-planar cap. However, a two-step process, with thin layer grown at 250 °C followed by growth at 500 °C, leads to a planar cap with a much-reduced density of defects.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Effects of thermal annealing process on the electrical properties of p{sup +}-Si/n-SiC heterojunctions

The effects of thermal annealing process on the interface in p{sup +}-Si/n-SiC heterojunctions fabricated by using surface-activated bonding are investigated. It is found by measuring their current-voltage (I-V) characteristics that the reverse-bias current and the ideality factor decreased to 2.98 × 10{sup −6} mA/cm{sup 2} and 1.03, respectively, by annealing the junctions at 1000 °C. Observation by using transmission electron microscopy indicates that an amorphous layer with a thickness of ∼6 nm is formed at the unannealed interface, which vanishes after annealing at 1000 °C. No structural defects at the interface are observed even after annealing at such a high temperature.

36 MATERIALS SCIENCE↗
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 OSTI2014

Suppression of tin precipitation in SiSn alloy layers by implanted carbon

By combining transmission electron microscopy and Rutherford backscattering spectrometry, we have identified carbon related suppression of dislocations and tin precipitation in supersaturated molecular-beam epitaxial grown SiSn alloy layers. Secondary ion mass spectrometry has exposed the accumulation of carbon in the SiSn layers after high temperature carbon implantation and high temperature thermal treatment. Strain-enhanced separation of point defects and formation of dopant-defect complexes are suggested to be responsible for the effects. The possibility for carbon assisted segregation-free high temperature growth of heteroepitaxial SiSn/Si and GeSn/Si structures is argued.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2016

Composition analysis of coaxially grown InGaN multi quantum wells using scanning transmission electron microscopy

GaN nanotubes with coaxial InGaN quantum wells were analyzed by scanning transmission electron microscopy in order to determine their structural properties as well as the indium distribution across the InGaN quantum wells. For the latter, two process steps are necessary. First, a technique to prepare cross-sectional slices out of the nanotubes has been developed. Second, an existing scanning transmission electron microscopy analysis technique has been extended with respect to the special crystallographic orientation of this type of specimen. In particular, the shape of the nanotubes, their defect structure, and the incorporation of indium on different facets were investigated. The quantum wells preferentially grow on m-planes of the dodecagonally shaped nanotubes and on semipolar top facets while no significant indium signal was found on a-planes. An averaged indium concentration of 6% to 7% was found by scanning transmission electron microscopy analysis and could be confirmed by cathodoluminescence measurements.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗