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Results for “Optical Microscopy”

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 289 records · Page 16
All sourcesNASA NTRSDOE OSTI
DOE OSTI2014

Carbon impurities on graphene synthesized by chemical vapor deposition on platinum

We report nanocrystalline carbon impurities coexisting with graphene synthesized via chemical vapor deposition on platinum. For certain growth conditions, we observe micron-size island-like impurity layers which can be mistaken for second graphene layers in optical microscopy or scanning electron microscopy. The island orientation depends on the crystalline orientation of the Pt, as shown by electron backscatter diffraction, indicating growth of carbon at the platinum surface below graphene. Dark-field transmission electron microscopy indicates that in addition to uniform single-crystal graphene, our sample is decorated with nanocrystalline carbon impurities with a spatially inhomogeneous distribution. The impurity concentration can be reduced significantly by lowering the growth temperature. Raman spectra show a large D peak, however, electrical characterization shows high mobility (∼8000 cm{sup 2}/Vs), indicating a limitation for Raman spectroscopy in characterizing the electronic quality of graphene.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2016

Identification of sigma and chi phases in duplex stainless steels

The aim of this work is to find out the most suitable method for detecting and analyzing accurately the formation conditions of secondary phases, particularly Sigma-phase (σ-phase) and Chi-phase (χ-phase) in duplex stainless steels (UNS S32205 and UNS S32750). The microstructure was characterized after a solution annealing at 1080 °C followed by an isothermal heating at 830 °C for different time ranges, ranging from 1 min to 9 h, in order to enlighten the controversial point concerning the mechanism of χ-phase nucleation in relation with the σ-phase. Etched samples were observed using optical microscopy (MO), and scanning electron microscopy (FESEM) with a backscattered electron detector (BSE) was used on unetched samples. Compositional microanalysis (EDS) was carried out for identifying the different phases present in the steels. Sigma phase was easily observed using different etching procedures, whereas χ-phase was only clearly detected with FESEM–BSE on unetched samples. The compositional analyses showed that the molybdenum content in χ-phase almost doubles the content of this element in σ-phase, and as a result the kinetics of nucleation and growth were also found to be remarkably faster when the alloy content in the steel is higher. In addition, chromium nitrides and carbides were also observed to precipitate as a result of the heat treatments and, in the case of the chromium nitrides, they act as a favorable site for the nucleation of σ-phase and χ-phase. - Highlights: • Microscopy was used on heat treated duplex steels for microstructure identification. • FESEM–BSE observation on unetched samples provided the best contrast between phases. • Analyses of carbides, nitrides, chi and sigma phases were possible by EDS and WDS. • Chromium nitrides act as favorable site for the nucleation of chi and sigma phases. • Secondary phases nucleation kinetics are faster in superduplex than in duplex steels.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Design and development of liquid filled polymeric fibers with flexure rate viscoelastic properties

The design and development of a novel category of bi-component polymeric fibers, made of a polymeric sheath and a liquid core is described. To understand and to analyze the flow of molten polymer and liquid within a spin pack, we built a macroscale analogon where co-flow of polymer and liquid is investigated systematically. The macroscale analogon is composed of a glass cylinder with a finite length and a coaxial capillary. The inner fluid flows in the capillary and at its outlet meets the outer fluid flowing inside the glass cylinder. The fluids are pumped into the setup using pressurized bottles with controlled flow rates. A high-speed camera is placed in front of the glass cylinder to record the transient and the steady flow of the two phases and the morphology of their interface during co-flow. We systematically analyzed the combination of various fluids and different injection channel geometries, and used these findings to design a customized spin pack. Extrusion trials with molten polymers and specific liquids resulted in the production of liquid filled polymeric fibers (LFF) with different amounts of liquid from 3% to 33%vol. and diameters from 150μm to 1mm. Fiber morphology has been investigated with the help of optical microscopy and computer tomography, in order to analyze both surface and core morphology. Mechanical characterization of fibers has been carried out with special care to the damping capacity of such fibers using two different methods: two point bending tests to evaluate the energy dissipation of fibers upon bending at low frequency values (0.005-0.5Hz), and analysis of vibration reduction to determine the quality factor at the resonance frequency of the 1{sup st} and 3{sup rd} vibration mode.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Visibility of two-dimensional layered materials on various substrates

For the investigation of 2D layered materials such as graphene, transition-metal dichalcogenides, boron nitride, and their heterostructures, dedicated substrates are required to enable unambiguous identification through optical microscopy. A systematic study is conducted, focusing on various 2D layered materials and substrates. The simulated colors are displayed and compared with microscopy images. Additionally, the issue of defining an appropriate index for measuring the degree of visibility is discussed. For a wide range of substrate stacks, layer thicknesses for optimum visibility are given along with the resulting sRGB colors. Further simulations of customized stacks can be conducted using our simulation tool, which is available for download and contains a database featuring a wide range of materials.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2014

Optical characterization of femtosecond laser induced active channel waveguides in lithium fluoride crystals

We successfully realized broad-band light-emitting color center waveguides buried in LiF crystals by using femtosecond laser pulses. The characterization of the waveguides was performed by optical microscopy, photoluminescence spectra, loss measurements and near-field profiling. The experimental results show that the direct-writing fabrication process induces low-index contrast active channel waveguides: their wavelength-dependent refractive index changes, estimated from 10{sup −3} to 10{sup −4} depending on the writing conditions, allow supporting few modes at visible and near-infrared wavelengths.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2014

Study of aging effects in a Ti-6AL-4V alloy with Widmanstätten and equiaxed microstructures by non-destructive means

When the Ti-6Al-4V alloy is over-aged at 500-600°C, nanometer-sized α{sub 2} (Ti{sub 3}Al) phases can be homogeneously precipitated inside α phases, thereby leading to the additional improvement of mechanical properties. The present study was concerned with the effects of over-aging on thermoelectric power (TEP) measurements in a Ti-6Al-4V alloy. Widmanstätten and equiaxed microstructures containing fine and agr{sub 2} (Ti{sub 3}Al) particles were obtaining by over-aging a Ti-6Al-4V alloy. Over-aging heat treatments were conducted at 515°C, 545°C and 575°C for different aging times. In order to find out the factors affecting the variation in the TEP, the over-aging samples were examined by optical microscopy (OM) and (SEM) scanning electron microscopy. In particular, we studied the behavior of the physical material property hardness, an important parameter of the Ti-6Al-4V alloy mechanical properties, with respect to the variation in the aging time and temperature. It was found that the TEP measurements reveal an increase in the magnitude of the absolute TEP value of the over-aged Widmanstätten and equiaxed microstructures with regards to the unaged condition for different aging times, with a somewhat higher value at 515°C.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Application of gamma-ray radiography and gravimetric measurements after accelerated corrosion tests of steel embedded in mortar

The accelerated corrosion by the impressed current technique is widely used in studies of concrete durability since it has the advantage that tests can be carried out within reasonable periods of time. In the present work the relationship between the applied current density and the resulting damage on the reinforcing steel, by applying optical microscopy, scanning electron microscopy, gamma-ray radiography and gravimetric measurements, was studied by means of the implementation of accelerated corrosion tests on reinforced mortar. The results show that the efficiency of the applied current is between 1 and 77%, regardless of the applied current density, the water/cement ratio and the mortar cover depth of the specimens. The results show the applicability of the gamma-ray radiography technique to detect localized corrosion of steel rebars in laboratory specimens.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Structural-scale levels of development of inelastic martensitic deformation during isothermal loading of submicrocrystalline titanium nickelide in premartensitic condition

The results are presented of an experimental investigation into the regularities and mechanisms of the development of thermoelastic martensitic transformation in submicrocrystalline alloy Ti{sub 49.4}Ni{sub 50.6} with different ways of thermo-power actions using the methods of optical microscopy in situ and X-ray diffraction. The peculiarities of localization of martensite transformation at the meso- and macroscale levels in this alloy with submicrocrystalline structure are considered. Experimental data on the relay mechanism of propagation of the martensitic transformation are presented. The interrelation between the localization of the martensitic transformation on the meso-and macroscale levels and deformation behavior under isothermal loading alloy Ti{sub 49.4}Ni5{sub 0.6} in submicrocrystalline condition are shown and discussed.

36 MATERIALS SCIENCE↗
DOE OSTI2019

The Influence of Shell Mold Composition on the As-cast Macro- and Micro-structure of Thin-Walled IN713C Superalloy Castings

In the investment casting process, the building of ceramic layers around the wax pattern is the main time-consuming stage. Increasing their number ensures sufficient mechanical properties, but also lengthens the whole process, including drying time and preheating of the mold. Four molds for casting Ni-based superalloy IN713C were strengthened by glass fibers, included in the slurry, and metal powder, of Al, Cu, Fe or Ni, in the coverage. Castings were subjected to microstructural investigations in order to find out if the new design can be promising for the manufacture of jet engine components. Bend tests revealed that the green strengths of all new molds were higher, at least 3.65 MPa, than that of the unmodified molds, 3.0 MPa. Optical microscopy revealed that the composition of a mold had a strong influence on stereological parameters of equiaxed IN713C grains. Microstructural observation and hardness measurements of castings revealed differences in the volume fraction of strengthening phases, porosity and hardness. The microstructure due to the complex chemical composition of IN713C consisted of several phases including ternary eutectics as a consequence of L → γ + Ni{sub 7}Zr{sub 2} + (Nb, Zr)C.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Impact of solvents and supercritical CO{sub 2} drying on the morphology and structure of polymer-based biofilms

In the present work, two-dimensional systems based on biodegradable polymers such as poly(ε-caprolactone) (PCL), poly(ethylene oxide) (PEO) and polylactic acid (PLA) are fabricated by means of a sustainable approach which consists in inducing phase separation in solutions of such polymers and “green” solvents, namely ethyl lactate (EL) and ethyl acetate (EA). The extraction of the solvent is promoted by a controlled drying process, which is performed in either air or supercritical CO{sub 2}. The latter can indeed act as both an antisolvent, which favors the deposition of the polymer by forming a mixture with EL and EA, and a plasticizing agent, whose solvation and transport properties may considerably affect the microstructure and crystallinity of the polymer films. The morphological, topographical and crystalline properties of the films are tailored through a judicial selection of the materials and the processing conditions and assessed by means of thermal analyses, polarized optical microscopy, scanning electron microscopy and confocal interferometric microscopy. The results show that the morphological and crystalline properties of the films are strongly dependent on the choice of both the polymer/solvent system and the operating conditions during the drying step. In particular, the morphological, topographical and thermal properties of films prepared starting from highly crystalline polymers, namely PCL and PEO, are greatly affected by the crystallization of the material. Conversely, the less crystalline PLA forms almost completely amorphous films.

36 MATERIALS SCIENCE↗
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 OSTI2016

Light-responsive polymer microcapsules as delivery systems for natural active agents

In this work we report the preparation and the release behavior of UV-responsive polymeric microcapsules containing essential oils as a core. The oil acted also as a monomer solvent during polymerization. Accordingly, the potentially toxic organic solvent traditionally used was replaced with a natural active substance, resulting in a more sustainable functional system. Polymer shell was based on a lightly cross-linked polyamide containing UV-sensitive azobenzene moieties in the main chain. The micro-sized capsules were obtained via interfacial polycondensation in o/w emulsion, and their mean size was measured via Dynamic Light Scattering. Shape and morphology were analyzed through Scanning Electron and Optical Microscopy. UV-responsive behavior was evaluated via spectrofluorimetry, by assessing the release kinetics of a fluorescent probe molecule upon UV light irradiation (λ{sub max}=360 nm). The irradiated samples showed an increase in fluorescence intensity, in accordance with the increase of the probe molecule concentration in the release medium. As for the un-irradiated sample, no changes could be detected demonstrating the effectiveness of the obtained releasing system.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2018

Quantification of Porosity in Ceramic Matrix Composites Using Thermography

Thermography is one of the Non-Destructive Evaluation methods used to qualitatively estimate the amount of porosity in as-manufactured ceramic matrix composite (CMC) parts. Through-transmission (TT) thermography allows for comparison of thermal diffusivity caused by differences in material density and porosity at different locations in the part. In this study, volume fraction of pores and its distribution in CMC samples containing different amounts of porosity was quantified using optical microscopy and X-ray computed tomography scans. TT thermography was done on the same specimens and images were analyzed to determine the distribution of thermal diffusivity. Comparison of porosity measurements and thermal diffusivity images shows an inverse correlation. A simple two-phase analytical model describing this relationship is derived for composites and its solution is shown to compare favorably with experimental data. In the absence of porosity data, the model can be used to estimate porosity directly from thermal diffusivity data.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Experimental Investigation of the Impact of Cathode Grade on Sludge Formation at the Cathode Block-Aluminum Interface of Hall–Héroult Cells

The presence of resistive sludge on the cathode surface in Hall–Héroult cells can increase the aluminum production costs and reduces cell lifetime. Modern cells with graphitized cathode blocks generally operate satisfactorily but some are exhibiting excessive deposit formation, thus lower performances. Little attention has ever been given to the role of the cathode grade and its properties on sludge formation. In this investigation, five graphitized industrial cathode grades with varying properties are tested on a bench scale aluminum electrolysis setup with cathodic current density of 0.9 A/cm{sup 2}, under a nitrogen atmosphere at 1233 K (960 °C) for 8 hours with initial bath composition of 10 pct alumina, cryolite ratio of 2.2, 5 pct CaF{sub 2} and no point feeding. Postmortem characterization includes Rietveld refinement of deposits, optical microscopy and SEM-EDS observations of the carbon-aluminum interface. Sludge located near the center of the cathode surface was generated during the experiments despite the absence of point feeding. The sludge profile was variable among grades and could be related to the horizontal and vertical thermal conductivities of the blocks. This study has pushed further the understanding of the mechanisms of sludge formation and dissolution concerning the cathode grade properties.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Tribological Behavior of a Cr{sub 2}O{sub 3} Ceramic Coating/Steel Couple Under Dry Sliding and Heavy Loading Conditions

This work evaluates the effects of heavy loadings on a Cr{sub 2}O{sub 3} ceramic coating/steel couple under dry sliding and in conditions similar to those occurring in heavy-duty diesel engines. Two types of wear tests were performed by a standard pin-on-disc tribometer under high constant and variable loads. Before wear tests, microstructure and mechanical properties of coating and steel were determined by optical emission spectrometry, optical microscopy, roughness, microhardness and x-ray diffractometry (XRD). The friction coefficient was directly calculated by the tribometer. The wear rate of Cr{sub 2}O{sub 3} ceramic coating was evaluated by the wear volume and that of pins by weighing them before and after tests. The wear tracks on pins and coating surfaces were analyzed by XRD and by scanning electron microscopy with energy-dispersive spectroscopy. For all loads except the lowest constant one, the results indicated high friction and wear involving material removal from the coating surface, through a severe-oxidational wear associated with extensive cracking of the surface of the coating, softening of the carburizing steel and removal of the carburized layer of pins. The wear mechanism was mild-oxidational under the lowest constant load, which was therefore suggested as the limit for acceptable performance of the sliding couple under study.

36 MATERIALS SCIENCE↗
DOE OSTI2016

A study of transient FGR by integral LOCA tests

A study of transient fission gas release (FGR) was performed by means of two out-of-pile LOCA tests in a hot cell facility. Irradiated fuel rod segments with lengths of roughly 80 mm and burnups of 64 MWd/kgU were subjected to simulated water-cooled reactor LOCA transients in an integral LOCA test device. The segments were heated to a maximum temperature of 1000 Celsius degrees and the increase in rod inner pressure resulting from fission gas release and increased gas temperature during the transient was measured. The first release of gas occurred at temperatures close to 450 Celsius degrees, which suggests a burst release mechanism that may be linked to the onset of grain boundary fracturing. At the end of the simulated transients, gas samples were taken from the fuel rod segments for study by gas mass spectroscopy. The transient fission gas release was measured and amount to roughly 13 % of the calculated pre-test rod inventory of Kr and Xe. Isotopic ratios of the released gas indicated that transient FGR originated from the whole pellet and not only the pellet periphery. The tested segments were also studied by light-optical microscopy to determine pellet porosity, pellet crack pattern and fuel fragmentation. The extent of fine fuel fragmentation was found to be small and limited to the periphery of the fuel. The determined amount of transient fission gas release can be added to the database of fuel rod design codes to more accurately describe the LOCA cladding strains and burst temperatures in the future.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗
DOE OSTI2013

Giant secondary grain growth in Cu films on sapphire

Single crystal metal films on insulating substrates are attractive for microelectronics and other applications, but they are difficult to achieve on macroscopic length scales. The conventional approach to obtaining such films is epitaxial growth at high temperature using slow deposition in ultrahigh vacuum conditions. Here we describe a different approach that is both simpler to implement and produces superior results: sputter deposition at modest temperatures followed by annealing to induce secondary grain growth. We show that polycrystalline as-deposited Cu on α-Al{sub 2}O{sub 3}(0001) can be transformed into Cu(111) with centimeter-sized grains. Employing optical microscopy, x-ray diffraction, and electron backscatter diffraction to characterize the films before and after annealing, we find a particular as-deposited grain structure that promotes the growth of giant grains upon annealing. To demonstrate one potential application of such films, we grow graphene by chemical vapor deposition on wafers of annealed Cu and obtain epitaxial graphene grains of 0.2 mm diameter.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Characterization of X80 and X100 Microalloyed Pipeline Steel Using Quantitative X-ray Diffraction

Quantitative X-ray diffraction characterization of four (4) X80 and three (3) X100 microalloyed steels was undertaken. The effect of through-thickness position, processing parameters, and composition on the measured crystallite size, microstrain, and J index (relative magnitude of crystallographic texture) was determined. Microstructure analysis using optical microscopy, scanning electron microscopy, transmission electron microscopy, and electron-backscattered diffraction was also undertaken. The measured value of microstrain increased with increasing alloy content and decreasing cooling interrupt temperature. Microstructural features corresponding to crystallite size in the X80 steels were both above and below the detection limit for quantitative X-ray diffraction. The X100 steels consistently exhibited microstructure features below the crystallite size detection limit. The yield stress of each steel increased with increasing microstrain. The increase in microstrain from X80 to X100 is also associated with a change in microstructure from predominantly polygonal ferrite to bainitic ferrite.

36 MATERIALS SCIENCE↗