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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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At least 847 records · Page 47
All sourcesNASA NTRSDOE OSTI
DOE OSTI2016

Analysis of microstructure in electro-spark deposited IN718 superalloy

The microstructure of electro-spark deposited (ESD) superalloy IN718 was studied by the use of scanning electron microscopy (SEM), electron backscatter diffraction (EBSD), transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS) techniques. In converse to general assumption, the extremely high cooling rate involved in the ESD process did not produce partitionless solidification that is devoid of second phase microconstituents in the material, nano-sized Laves phase and MC carbide particles were observed within the deposited layer. Notwithstanding the several thermal cycles involved in the process, the extremely low heat input of the process produced a deposited region that is free of the main strengthening phase of the alloy, γ″ phase precipitates, which is in contrast to what have been reported on laser deposition. Nevertheless, application of the standard full heat treatment of the alloy resulted in extensive formation of the γ″ phase precipitates and δ phase precipitates, the most stable secondary phase of the alloy, with nearly, if not complete, dissolution of the Laves phase particles. Furthermore, the XPS analysis done in the study revealed the formation of nano-oxides within the deposited layer, which increased the microhardness of the superalloy in the as-deposited condition and inhibited its grain growth during post-process heat treatment. The microstructure analysis done in this work is crucial to the understanding of properties of the superalloy processed by the ESD technique. - Highlights: •Electron microscopy analyses of electro-spark deposited IN 718 superalloy were performed. •Nano-sized secondary phase particles were observed within the deposited layer. •The study shows that the ESD did not produce partitionless solidification of the alloy.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Electrochemical Investigations of Magnetic Co{sub 3}O{sub 4} Nanoparticles as an Active Electrode for Supercapacitor Applications

This attempt reports on cobalt oxide (Co{sub 3}O{sub 4}) nanoparticles (NPs) prepared through the traditional chemical reflux method to examine the behavior of supercapacitor performance. The synthesized NPs were characterized using several analytical tools such as ultraviolet-visible spectroscopy (UV), Fourier-transform infrared spectroscopy (FTIR), X-ray diffraction (XRD) pattern, and scanning electron microscope (SEM) with energy dispersive X-ray spectroscopy (EDX). Moreover, the electrochemical performance was analyzed using galvanostatic charge and discharge studies (GCD), cyclic voltammetry (CV) studies as well as electrochemical impedance spectroscopy (EIS). The cubical phase of Co{sub 3}O{sub 4} was identified from the XRD pattern and also the average crystalline size was measured by Scherrer’s equation. FTIR confirmed the functional group of Co{sub 3}O{sub 4} NPs. SEM images revealed the hexagonal-shaped nanoflakes-like morphology of the sample. From the elemental analysis, the formation of pure Co{sub 3}O{sub 4} NPs by means of high purity and composition ratio of cobalt with oxygen was found. Vibrating sample magnetometer (VSM) plot scrutinized the magnetic performance of Co{sub 3}O{sub 4} NPs{sub .} The Co{sub 3}O{sub 4} NPs modified electrode has delivered maximum specific capacitance as 1413 Fg{sup −1} at a current density of 1 Ag{sup −1} which maintains tremendous cycling stability within the retention ratio of 98.4% after 1000 cycles. .

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2018

Organic Dye Degradation Under Solar Irradiation by Hydrothermally Synthesized ZnS Nanospheres

The green synthesis of ZnS nanospheres using Citrus limetta (sweet lime) juice as a capping agent through a conventional hydrothermal method was studied. The particle size, morphology, chemical composition, band gap, and optical properties of the synthesized ZnS nanospheres were characterized using x-ray diffraction spectroscopy, field emission scanning electron microscopy, high-resolution transmission electron microscopy, and ultraviolet–visible spectroscopy. The photocatalytic activity of the ZnS nanospheres was evaluated by degradation of rhodamine B (RhB) and methyl orange (MO) under solar irradiation. Upon 150 min of solar irradiation, the extent of degradation was 94% and 77% for RhB and MO, respectively.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2018

Alternative PWHT to Improve High-Temperature Mechanical Properties of Advanced 9Cr Steel Welds

Creep-resistant 9Cr steels are extremely important in thermal power generation industry due to their marked resistance to creep and corrosion. The weldability of these alloys is critical since they are used in welded construction equipment. The required mechanical properties are achieved after post-weld heat treatment. This study examined the effect of different post-weld heat treatments on microstructure and mechanical properties of creep strength-enhanced 9Cr steel welding deposits. It was obtained with an experimental flux-cored arc welding wire used under protective gas (Ar-20% CO{sub 2}). The heat treatments used were: (1) tempering (760 °C × 2 h), (2) solubilizing (1050 °C × 1 h) + tempering (760 °C × 2 h) and (3) solubilizing (1150 °C × 1 h) + first tempering (660 °C × 3 h) + second tempering (660 °C × 3 h). All-weld metal chemical composition was analyzed, and hot tensile tests were carried out at different temperatures. Charpy-V impact tests and Vickers microhardness measurements were also performed. Microstructures were studied using x-ray diffraction and optical and scanning electron microscopy. In all cases, a martensitic matrix with intergranular and intra-granular precipitates was detected. In the as-welded condition, δ-ferrite was also found. Microhardness dropped, and the impact energy increased with post-weld heat treatments. The highest hot tensile strength result was achieved with samples submitted to austenization at 1150 °C and double tempering at 660 °C.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Novel Co{sub 3}O{sub 4} porous polyhedrons derived from metal–organic framework toward high performance for electrochemical energy devices

Co{sub 3}O{sub 4} polyhedrons with porous structure have been synthesized simply by annealing Prussian blue analogue (PBA) Co{sub 3}[Co(CN){sub 6}]{sub 2} polyhedrons at 400 °C in air. The product was characterized by a series of techniques, such as X-ray Diffraction (XRD), Field Emission Scanning Electron Microscopy (FESEM), Transmission Electron Microscopy (TEM), High-resolution TEM (HRTEM), X-ray Photoelectron Spectroscopy (XPS), and Brunauer–Emmett–Teller (BET) gas adsorption. Interestingly, when evaluated as an anode material for lithium-ion batteries (LIBs), the Co{sub 3}O{sub 4} porous polyhedrons manifested high reversible capacity (about 1200 mAh g{sup −1} at 50 mA g{sup −1}) and excellent cycling performance. Moreover, they also exhibited a high specific capacitance of 110 Fg{sup −1} when used as an electrode in the supercapacitor. It is suggested that the special morphology and porous nanostructure lead to the promising electrochemical properties. - Graphical abstract: Novel and complicated mesoporous architectures of Co{sub 3}O{sub 4} have been fabricated by thermal decomposition of Prussian Blue Analog (PBA) Co{sub 3}[Co(CN){sub 6}]{sub 2} polyhedrons which obtained at the room temperature. When Co{sub 3}O{sub 4} product was evaluated for Li-ion batteries (LIBs), they exhibited high reversible capacity of 1000 mAh g{sup −1} with excellent cycle life because of the hollow/porous structure. Display Omitted.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2015

Gas sensing behaviour of Zn doped SnO{sub 2} nanostructures

In the present study pure and Zn-doped nanoparticles has been synthesized for gas sensing application. The synthesized nanoparticles were characterized by XRD (X-ray Diffraction), FESEM (Field emission scanning electron microscopy), UV-visible absorption spectroscopy and Raman spectroscopy. FESEM results revealed that nanoparticles were spherical. XRD and Raman spectroscopy confirmed tetragonal rutile phase of nanoparticles. No peak correspond to dopant has been observed in the doped nanoparticles suggesting that dopant gets incorporated into the lattice sites of SnO{sub 2}. The band gap of SnO{sub 2} nanoparticles was found to decrease on doping with Zn. The enhanced sensing response of doped nanoparticles towards ethanol vapour is attributed to the presence of oxygen vacancies and decrease in crystallite size of doped nanoparticles.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Microstructure of selective laser melted CM247LC nickel-based superalloy and its evolution through heat treatment

The selective laser melting of high temperature alloys is of great interest to the aerospace industry as it offers the prospect of producing more complex geometries than can be achieved with other manufacturing methods. In this study, the microstructure of the nickel-based superalloy, CM247LC, has been characterised following selective laser melting and after a post deposition heat treatment below the γ′ solvus temperature. In the as-deposited state, scanning electron microscopy with electron backscatter diffraction revealed a fine, cellular microstructure with preferential alignment of 〈001〉 along the build direction. A high dislocation density was seen at the periphery of the cells, indicating substantial localised deformation of the material. Fine primary MC carbides were also observed in the inter-cellular regions. High-resolution transmission electron microscopy identified the occurrence of very fine γ′ precipitates, approximately 5 nm in diameter, dispersed within the gamma phase. After heat treatment, the elongated cell colonies were observed to partially coalesce, accompanied by a decrease in dislocation density, producing columnar grains along the build direction. Cuboidal γ′ precipitates approximately 500 nm in diameter were observed to form in the recrystallised grains, accompanied by larger γ′ precipitates on the grain boundaries.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Towards bend-contour-free dislocation imaging via diffraction contrast STEM

Dislocation imaging using transmission electron microscopy (TEM) has been an invaluable tool for characterizing crystallographic defects in metals. Compared to conventional TEM imaging, diffraction contrast imaging scanning transmission electron microscopy (DCI STEM) with appropriate setting can provide better defect contrast with almost negligible bend contour artifacts, enabling more effective analysis of dislocation structures. Here, we investigated why STEM can suppresses bend contour, and how dislocation contrast behaves along with different STEM imaging parameters. Using a body-centered cubic HT-9 ferritic/martensitic alloy as an example, a simple procedure and operational theory are described at the beginning to help set up DCI STEM experiments. Comparing with conventional TEM and the STEM strictly complying with the principle of reciprocity, we found that a pair of STEM convergence and collection semi-angles, α S and β S , a few milliradians in size is essential for bend-contour-free defect imaging. It works in concert such that the convergence STEM probe opens up the reciprocal space, and then a comparable collection region evens out the rocking-curve oscillation and alleviates bend contours from the reciprocal space. This fundamental advantage is unique in DCI STEM. Practical guidelines regarding STEM parameters and specimen orientation and thickness are then provided for DCI STEM dislocation imaging. Lastly, we show that coupling DCI STEM with spectrum images of electron energy loss spectroscopy and of energy-dispersive X-ray Spectroscopy offers a comprehensive characterization of crystallographic defects and chemical information of complex microstructures.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2018

The Removal of Acid Violet 90 from Aqueous Solutions Using PANI and PANI/Clinoptilolite Composites: Isotherm and Kinetics

Polyaniline (PANI) and polyaniline/Gördes-clinoptilolite (PANI/GC) composite materials were synthesized by the chemical oxidative polymerization technique and used in the adsorption of Acid Violet 90 metal-complex dye (AV 90). The samples were characterized by X-ray diffractions, nitrogen adsorption–desorption isotherms, scanning electron microscopes and Fourier transform infrared. The effect of initial pH (2–8), sorbent dosage (0.5–4.0 g/L) and initial dye concentrations (50–400 mg/L) on adsorption onto PANI and PANI/GC were examined in a batch system. Langmuir, Freundlich and Temkin isotherm models were used to investigate the adsorption mechanism of AV 90 on PANI and PANI/GC. Langmuir isotherm model for PANI/GC and Freundlich isotherm model for PANI were fitted well with the experimental data. The highest dye uptake capacities were obtained with Langmuir isotherm model as 153.85 mg/g and 72.46 mg/g for PANI and PANI/GC, respectively. In order to determine the adsorption kinetics, pseudo first-order and second-order kinetic models were studied. As a result, the adsorption of AV 90 dye on PANI and PANI/GC was better identified with Pseudo second-order kinetic model than the first one.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2018

Structural and Mechanical Properties of Zr-Si-N Coatings Deposited by Arc Evaporation at Different Substrate Bias Voltages

ZrN and Zr-Si-N coatings were formed using vacuum-arc plasma fluxes deposition system at the substrate bias voltage (U{sub B}) ranged from − 50 to − 220 V on HS6-5-2 steel substrates. The structural, mechanical and tribological properties were characterized using x-ray diffraction, atomic force microscopy, scanning electron microscopy, optical microscopy, nanoindentation and ball-on-disk test. The surface roughness parameter Ra of ZrN coatings is lower than Zr-Si-N coatings. Both roughness Ra of Zr-Si-N coatings and the number of surface defects with mainly small dimensions to 1 µm decrease with increasing negative substrate bias voltage. The addition of silicon to ZrN significantly reduces the crystallite size, from about 18.3 nm for ZrN coating to 6.4 nm for Zr-Si-N coating both deposited at the same U{sub B} = − 100 V and 7.8 nm for U{sub B} = − 150 V. The hardness of Zr-Si-N coatings increases to about 30 GPa with the increase in negative substrate bias voltage (U{sub B} = − 220 V). Adhesion of the coatings tested is high, and critical load is above 80 N and reduces with U{sub B} increase. Coefficient of friction determined using AFM shows similar trend as surface roughness in microscale.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Photovoltaic performance of Ag-doped CdS quantum dots for solar cell application

Graphical abstract: Photovoltaic performance of un-doped and Ag-doped CdS quantum dots were studied. The enhancement in photovoltaic performance might be due to the increase in carrier concentration and additional energy level creation due to Ag doping in FTO/TiO{sub 2}/Ag-doped CdS QDs solar cell. - Highlights: • Un-doped and Ag-doped CdS QDs were successfully deposited on TiO{sub 2}/FTO. • Optical response was found to be high for 3% Ag-doped CdS QDs. • The absorption edge for the 3% Ag-doped CdS was found to be 550 nm. • The highest power conversion efficiency was 1.25% for 3% Ag-doped CdS QDs. - Abstract: Un-doped and Ag-doped CdS quantum dots (QDs) were deposited on spin coated TiO{sub 2} photoanode material by Successive Ionic Layer Adsorption and Reaction (SILAR) method. Systematic investigations were carried out in the deposited un-doped and Ag-doped CdS QDs using powder X-ray diffraction (PXRD), field emission scanning electron microscopy (FESEM) and UV–vis-NIR spectrum. Finally, the FTO/TiO{sub 2}/un-doped CdS and FTO/TiO{sub 2}/Ag-doped CdS QDs were successfully assembled to study the photovoltaic performance under standard one sun illumination of AM 1.5, 100 mW/cm{sup 2}. Photovoltaic parameters, such as short-circuit photocurrent density, open circuit voltage, fill factor and conversion efficiency were found to be 1.37 mA/cm{sup 2}, 0.72 V, 61.5% and 0.61% respectively, for un-doped CdS. Ag-doped CdS QDs shows enhanced photovoltaic parameters such as short-circuit photocurrent density, open circuit voltage, fill factor and conversion efficiency which were 2.35 mA cm{sup 2}, 0.74 V, 71.8% and 1.25% respectively.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Influence of Te and Se doping on ZnO films growth by SILAR method

The AIP Successive ionic layer adsorption and reaction (SILAR) is an economic and simple method to growth thin films. In this study, SILAR method is used to growth Selenium (Se) and Tellurium (Te) doped zinc oxide (ZnO) thin films with different doping rates. For characterization of the films X-ray diffraction (XRD), absorbance and scanning electron microscopy (SEM) are used. XRD results are showed well-defined strongly (002) oriented crystal structure for all samples. Also, absorbance measurements show, Te and Se concentration are proportional and inversely proportional with band gap energy, respectively. SEM measurements show that the surface morphology and thickness of the material varied with Se and/or Te and varying concentrations.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2016

Effect of intermetallic compounds on the thermal conductivity of Ti-Cu composites

Ti films were deposited by magnetron sputtering on polycrystalline Cu substrates. The samples were annealed at different temperatures and characterized by x-ray diffraction for phase identification, scanning electron microscopy, and energy dispersive spectrometry for microstructure and composition and transient thermoreflectance for thermal conductivity and interface thermal conductance. The results showed that the diffused layer of Ti in Cu contained intermetallic compounds and solid solution of Ti in Cu. The thermal conductivity of the diffused layer is reduced, and the thickness increased for higher annealing temperature. The interface thermal conductance also decreased for higher temperature of annealing. A stable Cu{sub 4}Ti phase was formed after annealing at 725 °C with thermal conductivity of 10 W m{sup −1} K{sup −1}. The interface thermal conductance between the intermetallic compound and the solid solution of Ti in Cu also was reduced to 30 MW m{sup −2} K{sup −1}. The effective thermal resistance of the diffused layer and the interface was found to increase for higher annealing temperature.

36 MATERIALS SCIENCE↗
DOE OSTI2016

TREAT reactor LEU fuel-clad chemical interaction empirical modeling analysis

DOE is converting TREAT (Transient Reactor Test) facility from its existing highly enriched uranium (HEU) core to a low-enriched uranium (LEU) core. In order to assess the magnitude of chemical interaction between fuel and cladding materials during physical contact under expected TREAT operational limits, planned transients tests, and reactivity accident scenarios, a combination of experimental testing and thermodynamic modeling was performed to predict the expected chemical interactions among fuel and cladding chemical constituents. Thermodynamic calculations were then validated with empirical data from experiments that emulate TREAT's expected upper operational limits. Pellet samples composed of LEU oxide powder dispersed in a graphite matrix had intimate contact with zirconium-based alloy cladding. The samples were subjected to long-term isothermal heating under high vacuum. Specimen characterization consisted of scanning electron microscopy, x-ray diffraction analysis, and x-ray tomography. ThermoCalc software and Ellingham's diagrams were used for thermodynamic calculations. The X-ray tomography and SEM analysis of the pellets showed a homogeneous distribution of UO{sub 2} particles within the graphite matrix with isolated larger UO{sub 2} agglomerates. The SEM analysis showed the formation of a lamellar structure between the large UO{sub 2} agglomerate and the graphite matrix. This is an indication that diffusion is taking place at a rather moderate temperature and reaction time during the pellet fabrication. Secondary phases, with high Al and Mg content, were detected inside a UO{sub 2} agglomerate using SEM in SE/EBSD mode and chemical analysis with EDS. LEU feedstock impurities, as Al and Mg, seem to promote the chemical reactivity between UO{sub 2} particles and graphite matrix. XRD analysis of a pellet sample showed the presence of UO{sub 2} and graphite, but no other crystalline phases were detected with this technique. Thermodynamic analysis through the use of Ellingham diagrams showed that within TREAT's operational to reactivity accident temperature (278-820 Celsius degrees), UO{sub 2} can be reduced to U metal by Zr due to a more favorable ΔG for the oxidation of Zr.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2016

Microstructure and partitioning behavior characteristics in low carbon steels treated by hot-rolling direct quenching and dynamical partitioning processes

In this work, a new process and composition design are proposed for “quenching and partitioning” or Q&P treatment. Three low carbon steels were treated by hot-rolling direct quenching and dynamical partitioning processes (DQ&P). The effects of proeutectoid ferrite and carbon concentration on microstructure evolution and mechanical properties were investigated. The present work obtained DQ&P prototype steels with good mechanical properties and established a new notion on compositions for Q&P processing. Microstructures were characterized by means of electro probe microanalyzer (EPMA), scanning electron microscopy (SEM), electron backscatter diffraction (EBSD), transmission electron microscopy (TEM) and X-ray diffraction (XRD), especially the morphology and size of retained austenite. Mechanical properties were measured by uniaxial tensile tests. The results indicated that introducing proeutectoid ferrite can increase the volume fraction of retained austenite and thus improve mechanical properties. TEM observation showed that retained austenite included the film-like inter-lath austenite and blocky austenite located in martensite/ferrite interfaces or surrounded by ferrites. It was interesting that when the carbon concentration is as low as ~ 0.078%, the film-like inter-lath untransformed austenite cannot be stabilized to room temperature and almost all of them transformed into twin martensite. The blocky retained austenite strengthened the interfaces and transformed into twin martensite during the tensile deformation process. The PSEs of specimens all exceeded 20 GPa.%. - Highlights: •This study focused on a new process: Q&P process applying dynamical partitioning. •Ferrite can increase the volume fraction of retained austenite. •The film-like austenite and the blocky austenite were observed. •The low carbon steels treated by new process reached PSEs higher than 20 GPa.%.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Evolution of Optical Diffraction Patterns on Disordered Woodpile Photonic Structures

Using three-dimensional direct laser writing, ordered and disordered photonic woodpile structures have been produced. An ideal woodpile is formed by layers of parallel “logs” turned through 90° with respect to logs of the previous layer. The disorder was specified by a random deviation in the angle with respect to their parallel arrangement in each layer of the woodpile. The quality of samples was tested by scanning electron microscopy. The optical diffraction patterns were studied experimentally on microsamples with different degrees of disorder and structure periods. With an increase in the degree of the disorder, the diffraction patterns changed qualitatively with the preservation of the zero diffraction order and formation of a speckle field pattern by higher diffraction orders.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2024

Determination of α lamellae orientation in a β-Ti alloy using electron backscatter diffraction

The spatial orientation of α lamellae in a metastable β-Ti matrix of Timetal LCB (Ti–6.8 Mo–4.5 Fe–1.5 Al in wt%) was examined and the orientation of the hexagonal close-packed α lattice in the α lamella was determined. For this purpose, a combination of methods of small-angle X-ray scattering, scanning electron microscopy and electron backscatter diffraction was used. The habit planes of α laths are close to {111} β , which corresponds to (1$\bar3$20) α in the hexagonal coordinate system of the α phase. The longest α lamella direction lies approximately along one of the $\langle$110$\rangle$ β directions which are parallel to the specific habit plane. Taking into account the average lattice parameters of the β and α phases in aged conditions in Timetal LCB, it was possible to index all main axes and faces of an α lath not only in the cubic coordinate system of the parent β phase but also in the hexagonal system of the α phase.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Degradation of Components After Exposure in a Biomass Pyrolysis System

X-ray diffraction, electron probe microanalysis, and scanning transmission electron microscopy with focused ion beam lift-out sample preparation techniques were used to study corrosion products in a 304L (UNS S30403) stainless steel fluidized-bed reactor segment from Iowa State University’s Pyrolysis Process Development Unit Facility. This reactor segment is particularly valuable because a detailed history of operation time, temperature, and biomass feedstock was available. As previously reported for a range of stainless steel pyrolysis-related equipment, external scaling and internal attack along alloy grain boundaries were observed. Here, the scaling was primarily associated with O, although S, Ca, K, Si, Mg, and P were also detected in the outer scale regions. However, unlike those other recent advanced characterization analyses, in this instance the internal alloy grain boundary attack was not directly related to S. Rather, only internal oxidation and localized nanoporosity were observed along the alloy grain boundaries, with associated local nanoscale Cr depletion and Ni enrichment. Mechanistic implications of this finding are discussed.

36 MATERIALS SCIENCE↗