Synthesis by sol-gel process, structural and optical properties of nanoparticles of zinc oxide doped vanadium

NASA Astrophysics Data System (ADS)

El Ghoul, J.; Barthou, C.; El Mir, L.

2012-06-01

We report the elaboration of vanadium-doped ZnO nanoparticles prepared by a sol-gel processing technique. In our approach, the water for hydrolysis was slowly released by esterification reaction followed by a supercritical drying in ethyl alcohol. Vanadium doping concentration of 10 at.% has been investigated. After treatment in air at different temperatures, the obtained nanopowder was characterised by various techniques such as scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and photoluminescence (PL). Analysis by scanning electron microscopy at high resolution shows that the grain size increases with increasing temperature. Thus, in the case of thermal treatment at 500 °C in air, the powder with an average particle size of 25 nm shows a strong luminescence band in the visible range. The intensity and energy position of the obtained PL band depends on the temperature measurement increase. The mechanism of this emission band is discussed.

Effect of supercritical fluid density on nanoencapsulated drug particle size using the supercritical antisolvent method.

PubMed

Kalani, Mahshid; Yunus, Robiah

2012-01-01

The reported work demonstrates and discusses the effect of supercritical fluid density (pressure and temperature of supercritical fluid carbon dioxide) on particle size and distribution using the supercritical antisolvent (SAS) method in the purpose of drug encapsulation. In this study, paracetamol was encapsulated inside L-polylactic acid, a semicrystalline polymer, with different process parameters, including pressure and temperature, using the SAS process. The morphology and particle size of the prepared nanoparticles were determined by scanning electron microscopy and transmission electron microscopy. The results revealed that increasing temperature enhanced mean particle size due to the plasticizing effect. Furthermore, increasing pressure enhanced molecular interaction and solubility; thus, particle size was reduced. Transmission electron microscopy images defined the internal structure of nanoparticles. Thermal characteristics of nanoparticles were also investigated via differential scanning calorimetry. Furthermore, X-ray diffraction pattern revealed the changes in crystallinity structure during the SAS process. In vitro drug release analysis determined the sustained release of paracetamol in over 4 weeks.

Effect of supercritical fluid density on nanoencapsulated drug particle size using the supercritical antisolvent method

PubMed Central

Kalani, Mahshid; Yunus, Robiah

2012-01-01

The reported work demonstrates and discusses the effect of supercritical fluid density (pressure and temperature of supercritical fluid carbon dioxide) on particle size and distribution using the supercritical antisolvent (SAS) method in the purpose of drug encapsulation. In this study, paracetamol was encapsulated inside L-polylactic acid, a semicrystalline polymer, with different process parameters, including pressure and temperature, using the SAS process. The morphology and particle size of the prepared nanoparticles were determined by scanning electron microscopy and transmission electron microscopy. The results revealed that increasing temperature enhanced mean particle size due to the plasticizing effect. Furthermore, increasing pressure enhanced molecular interaction and solubility; thus, particle size was reduced. Transmission electron microscopy images defined the internal structure of nanoparticles. Thermal characteristics of nanoparticles were also investigated via differential scanning calorimetry. Furthermore, X-ray diffraction pattern revealed the changes in crystallinity structure during the SAS process. In vitro drug release analysis determined the sustained release of paracetamol in over 4 weeks. PMID:22619552

Nanoscale Investigation of Grain Growth in RF-Sputtered Indium Tin Oxide Thin Films by Scanning Probe Microscopy

NASA Astrophysics Data System (ADS)

Lamsal, B. S.; Dubey, M.; Swaminathan, V.; Huh, Y.; Galipeau, D.; Qiao, Q.; Fan, Q. H.

2014-11-01

This work studied the electronic characteristics of the grains and grain boundaries of indium tin oxide (ITO) thin films using electrostatic and Kelvin probe force microscopy. Two types of ITO films were compared, deposited using radiofrequency magnetron sputtering in pure argon or 99% argon + 1% oxygen, respectively. The average grain size and surface roughness increased with substrate temperature for the films deposited in pure argon. With the addition of 1% oxygen, the increase in the grain size was inhibited above 150°C, which was suggested to be due to passivation of the grains by the excess oxygen. Electrostatic force microscopy and Kelvin probe force microscopy (KPFM) images confirmed that the grain growth was defect mediated and occurred at defective interfaces at high temperatures. Films deposited at room temperature with 1% oxygen showed crystalline nature, while films deposited with pure argon at room temperature were amorphous as observed from KPFM images. The potential drop across the grain and grain boundary was determined by taking surface potential line profiles to evaluate the electronic properties.

Evidence of Momentum Conservation at a Nonepitaxial Metal/Semiconductor Interface Using Ballistic Electron Emission Microscopy

NASA Technical Reports Server (NTRS)

Bell, L. D.

1996-01-01

Ballistic-Electron-Emission Microscopy (BEEM) spectroscopy has been performed on Au/Si(111) structures as a function of Au thickness and temperature. At 77 K a direct signature of parallel momentum conservation at the Au/Si interface is observed in the BEEM spectra. The variation in spectral shape with both Au thickness and temperature places restrictions on allowable values of inelastic and elastic mean-free paths in the metal, and also requires the presence of multiple electron passes within the Au layer. An independent indication of multiple reflections is directly observed in the attenuation of BEEM current with Au thickness.

Phonon shift in chemically exfoliated WS2 nanosheet

NASA Astrophysics Data System (ADS)

Sarkar, Abdus Salam; Pal, Suman Kalyan

2018-04-01

We have synthesized few layer WS2 nanosheets in a low boiling point solvent. Few layer of WS2 sheets are characterized by various techniques such as UV-visible and Raman spectroscopy, transmission electron microscopy (TEM), atomic force microscopy (AFM) and scanning electron microscopy (SEM). UV-Vis absorption spectra confirm the well dispersed in isopropyl alcohol. SEM and TEM images indicate the sheet like morphology of WS2. Atomic force microscopy image and room temperature Raman spectroscopy confirm the exfoliation of few layer (4-5 layer) of WS2. Further, Raman spectroscopy was used as a meteorology tool to determine the temperature co-efficient. We have systematically investigated the temperature dependent Raman spectroscopic behavior of few layer WS2. Our results depict the softening of the Raman modes E12g in plane vibration and A1g out of plane vibration with increasing the temperature from 77 K to 300 K. Softening of the Raman modes could be explained in terms of the double resonance which is active in the layered materials. The observed temperature coefficients for two Raman peaks E12g and A1g, are - 0.022 cm-1 and -0.009 cm-1, respectively.

Optical properties of hydrothermally synthesized TGA-capped CdS nanoparticles: controlling crystalline size and phase

NASA Astrophysics Data System (ADS)

Tavakoli Banizi, Zoha; Seifi, Majid

2017-10-01

TGA-capped CdS nanoparticles were obtained in the presence of thioglycolic acid (TGA) as capping agent via a facile hydrothermal method at relatively low temperature and over a short duration. As-synthesized TGA-capped CdS nanoparticles were characterized by x-ray diffraction, scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectra, photoluminescence spectroscopy, Ultraviolet-visible spectroscopy and energy-dispersive x-ray spectroscopy. The products had spherical shapes, although their crystalline size and phase was dependent on temperature and time of the reaction. Photoluminescence spectra showed that the fluorescence intensity decreased when increasing the reaction time and temperature.

Method for local temperature measurement in a nanoreactor for in situ high-resolution electron microscopy.

PubMed

Vendelbo, S B; Kooyman, P J; Creemer, J F; Morana, B; Mele, L; Dona, P; Nelissen, B J; Helveg, S

2013-10-01

In situ high-resolution transmission electron microscopy (TEM) of solids under reactive gas conditions can be facilitated by microelectromechanical system devices called nanoreactors. These nanoreactors are windowed cells containing nanoliter volumes of gas at ambient pressures and elevated temperatures. However, due to the high spatial confinement of the reaction environment, traditional methods for measuring process parameters, such as the local temperature, are difficult to apply. To address this issue, we devise an electron energy loss spectroscopy (EELS) method that probes the local temperature of the reaction volume under inspection by the electron beam. The local gas density, as measured using quantitative EELS, is combined with the inherent relation between gas density and temperature, as described by the ideal gas law, to obtain the local temperature. Using this method we determined the temperature gradient in a nanoreactor in situ, while the average, global temperature was monitored by a traditional measurement of the electrical resistivity of the heater. The local gas temperatures had a maximum of 56 °C deviation from the global heater values under the applied conditions. The local temperatures, obtained with the proposed method, are in good agreement with predictions from an analytical model. Copyright © 2013 Elsevier B.V. All rights reserved.

Heat- and electron-beam-induced transport of gold particles into silicon oxide and silicon studied by in situ high-resolution transmission electron microscopy.

PubMed

Biskupek, Johannes; Kaiser, Ute; Falk, Fritz

2008-06-01

In this study, we describe the transport of gold (Au) nanoparticles from the surface into crystalline silicon (Si) covered by silicon oxide (SiO(2)) as revealed by in situ high-resolution transmission electron microscopy. Complete crystalline Au nanoparticles sink through the SiO(2) layer into the Si substrate when high-dose electron irradiation is applied and temperature is raised above 150 degrees C. Above temperatures of 250 degrees C, the Au nanoparticles finally dissolve into fragments accompanied by crystallization of the amorphized Si substrate around these fragments. The transport process is explained by a wetting process followed by Stokes motion. Modelling this process yields boundaries for the interface energies involved.

Use of light, scanning electron microscopy and bioassays to evaluate parasitism by entomopathogenic fungi of the red scale insect of palms (Phoenicococcus marlatti Ckll., 1899).

PubMed

Asensio, L; Lopez-Llorca, L V; López-Jiménez, J A

2005-01-01

We have evaluated the parasitism of the red scale insect of the date palm (Phoenicococcus marlatti) by entomopathogenic fungi, using light microscopy (LM), scanning electron microscopy (SEM) and low temperature scanning electron microscopy (LTSEM). Beauveria bassiana, Lecanicillium dimorphum and Lecanicillium cf. psalliotae, were inoculated directly on the scale insects or on insect infested plant material. We found that L. dimorphum and L. cf. psalliotae developed on plant material and on scale insects, making infection structures. B. bassiana was a bad colonizer of date palm leaves (Phoenix dactylifera L.) and did not parasite the scale insects.

Dispersion of Co/CNTs via strong electrostatic adsorption method: Thermal treatment effect

DOE Office of Scientific and Technical Information (OSTI.GOV)

Akbarzadeh, Omid, E-mail: omid.akbarzadeh63@gmail.com; Abdullah, Bawadi, E-mail: bawadi-abdullah@petronas.com.my; Subbarao, Duvvuri, E-mail: duvvuri-subbarao@petronas.com.my

The effect of different thermal treatment temperature on the structure of multi-walled carbon nanotubes (MWCNTs) and Co particle dispersion on CNTs support is studied using Strong electrostatic adsorption (SEA) method. The samples tested by N{sub 2}-adsorption, field emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM). N{sub 2}-adsorption results showed BET surface area increased using thermal treatment and TEM images showed that increasing the thermal treatment temperature lead to flaky CNTs and defects introduced on the outer surface and Co particle dispersion increased.

Determination of the coalescence temperature of latexes by environmental scanning electron microscopy.

PubMed

Gonzalez, Edurne; Tollan, Christopher; Chuvilin, Andrey; Barandiaran, Maria J; Paulis, Maria

2012-08-01

A new methodology for quantitative characterization of the coalescence process of waterborne polymer dispersion (latex) particles by environmental scanning electron microscopy (ESEM) is proposed. The experimental setup has been developed to provide reproducible latex monolayer depositions, optimized contrast of the latex particles, and a reliable readout of the sample temperature. Quantification of the coalescence process under dry conditions has been performed by image processing based on evaluation of the image autocorrelation function. As a proof of concept the coalescence of two latexes with known and differing glass transition temperatures has been measured. It has been shown that a reproducibility of better than 1.5 °C can be obtained for the measurement of the coalescence temperature.

Room temperature synthesis of Cu₂O nanospheres: optical properties and thermal behavior.

PubMed

Nunes, Daniela; Santos, Lídia; Duarte, Paulo; Pimentel, Ana; Pinto, Joana V; Barquinha, Pedro; Carvalho, Patrícia A; Fortunato, Elvira; Martins, Rodrigo

2015-02-01

The present work reports a simple and easy wet chemistry synthesis of cuprous oxide (Cu2O) nanospheres at room temperature without surfactants and using different precursors. Structural characterization was carried out by X-ray diffraction, transmission electron microscopy, and scanning electron microscopy coupled with focused ion beam and energy-dispersive X-ray spectroscopy. The optical band gaps were determined from diffuse reflectance spectroscopy. The photoluminescence behavior of the as-synthesized nanospheres showed significant differences depending on the precursors used. The Cu2O nanospheres were constituted by aggregates of nanocrystals, in which an on/off emission behavior of each individual nanocrystal was identified during transmission electron microscopy observations. The thermal behavior of the Cu2O nanospheres was investigated with in situ X-ray diffraction and differential scanning calorimetry experiments. Remarkable structural differences were observed for the nanospheres annealed in air, which turned into hollow spherical structures surrounded by outsized nanocrystals.

Electron microscopy observations of radiation damage in irradiated and annealed tungsten

NASA Astrophysics Data System (ADS)

Grzonka, J.; Ciupiński, Ł.; Smalc-Koziorowska, J.; Ogorodnikova, O. V.; Mayer, M.; Kurzydłowski, K. J.

2014-12-01

In the present work tungsten samples were irradiated with W6+ ions with a kinetic energy of 20 MeV in order to simulate radiation damage by fast neutrons. Two samples with cumulative damage of 2.3 and 6.36 displacements per atom were produced. The scanning transmission electron microscopy investigations were carried out in order to determine structure changes resulting from the irradiation. The evolution of the damage with post implantation annealing in the temperature range 673-1100 K was also assessed. Damage profiles were studied at cross-sections. Scanning transmission electron microscopy studies of the lamellae after annealing revealed aggregation of defects and rearrangement as well as partial healing of dislocations at higher temperatures. The results confirm the higher density of radiation-induced dislocations in the near surface area of the sample (1.8 * 1014 m-2) in comparison with a deeper damage area (1.5 * 1014 m-2). Significant decrease of dislocation density was observed after annealing with a concurrent growth of dislocation loops. Transmission electron microscopy analyses show that the dislocation loops are perfect dislocations with the Burgers vectors of b = ½[ 1 1 1].

Analysis of Carbon/Carbon Fragments From the Columbia Tragedy

NASA Technical Reports Server (NTRS)

Tallant, David R.; Simpson, Regina L.; Jacobson, Nathan S.

2005-01-01

The extensive investigation following the Space Shuttle Orbiter Columbia accident of February 1, 2003 determined that hot gases entered the wing through a breach in the protective reinforced carbon/carbon (RCC) leading edge. In the current study, the exposed edges of the recovered RCC from the vicinity of the breach are examined with scanning electron microscopy and Raman spectroscopy. Electron microscopy of the exposed edges revealed regions of pointed carbon fibers, characteristic of exposure to high temperature oxidizing gases. The Raman technique relates the observed 1350 and 1580 to 1600 cm(-1) bands to graphitic dom ains and their corresponding temperatures of formation. Some of the regions showed evidence of exposure temperatures beyond 2700 ?C during the accident.

Investigation on structural and electrical properties of Fe doped ZnO nanoparticles synthesized by solution combustion method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ram, Mast, E-mail: mastram1999@yahoo.com; Bala, Kanchan; Sharma, Hakikat

In the present study, nanoparticles of Fe doped zinc oxide (ZnO) [Zn{sub 1-x}Fe{sub x}O where x=0.0, 0.01, 0.02, 0.03 and 0.05] were prepared by cost effective solution combustion method. The powder X-ray diffractometry confirms the formation of single phase wurtzite structure. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were used to investigate the micrsostructure of Fe-doped ZnO nanoparticles. The DC electrical conductivity was found to increase with temperature and measurement was carried out in the temperature range of 300-473K. DC electrical conductivity increases with temperature and decreases with Fe doping concentration.

Epitaxial Growth and Electronic Structure of Half Heuslers Co1-xNixTiSb (001), Ni1-xCoxTiSn, and PtLuSb

DTIC Science & Technology

2016-01-09

studied in detail using scanning tunneling microscopy and angle resolved photoemission. For the doping levels achieved in cobalt titanium antimony, the...angle resolved photoemission. For the doping levels achieved in cobalt titanium antimony, the electron mobility at room temperature was comparable...scanning tunneling microscopy and angle resolved photoemission. For the doping levels achieved in cobalt titanium antimony, the electron mobility at room

Precipitation hardening behaviour of Al-Mg-Si alloy processed by cryorolling and room temperature rolling

NASA Astrophysics Data System (ADS)

Hussain, Maruff; Nageswara rao, P.; Singh, Dharmendra; Jayaganthan, R.

2018-04-01

The precipitation hardenable aluminium alloy (Al-Mg-Si) plates were solutionized and subjected to rolling at room temperature and liquid nitrogen temperature (RTR, CR) up to a true strain of ∼2.7. The rolled sheets were uniformly aged at room temperature and above room temperature (125 °C) to induce precipitation. The rolled and aged samples were analysed using differential scanning calorimetry (DSC), X-ray diffraction (XRD), transmission electron microscopy (TEM), hardness and tensile tests. The strength and ductility were simultaneously improved after controlled ageing of the cryorolled (CR) and room temperature rolled (RTR) samples. However, the increment in strength is more in RTR material than CR material with same ductility. Transmission electron microscopy analysis revealed the formation of ultrafine grains (UFG) filled with dislocations and nanosized precipitates in the CR and RTR conditions after ageing treatment. The behaviour of CR and RTR alloy is same under natural ageing conditions.

Synthesis of AuPd alloyed nanoparticles via room-temperature electron reduction with argon glow discharge as electron source.

PubMed

Yang, Manman; Wang, Zongyuan; Wang, Wei; Liu, Chang-Jun

2014-01-01

Argon glow discharge has been employed as a cheap, environmentally friendly, and convenient electron source for simultaneous reduction of HAuCl4 and PdCl2 on the anodic aluminum oxide (AAO) substrate. The thermal imaging confirms that the synthesis is operated at room temperature. The reduction is conducted with a short time (30 min) under the pressure of approximately 100 Pa. This room-temperature electron reduction operates in a dry way and requires neither hydrogen nor extra heating nor chemical reducing agent. The analyses using X-ray photoelectron spectroscopy (XPS) confirm all the metallic ions have been reduced. The characterization with X-ray diffraction (XRD) and high-resolution transmission electron microscopy (HRTEM) shows that AuPd alloyed nanoparticles are formed. There also exist some highly dispersed Au and Pd monometallic particles that cannot be detected by XRD and transmission electron microscopy (TEM) because of their small particle sizes. The observed AuPd alloyed nanoparticles are spherical with an average size of 14 nm. No core-shell structure can be observed. The room-temperature electron reduction can be operated in a larger scale. It is an easy way for the synthesis of AuPd alloyed nanoparticles.

Dipolar ferromagnetic phase transition in Fe3O4 nanoparticle arrays observed by Lorentz microscopy and electron holography

NASA Astrophysics Data System (ADS)

Yamamoto, Kazuo; Hogg, Charles R.; Yamamuro, Saeki; Hirayama, Tsukasa; Majetich, Sara A.

2011-02-01

Dipolar ferromagnetism formed in Fe3O4 nanoparticle arrays is revealed by Fresnel Lorentz microscopy and electron holography. Dipolar domain walls do not lie preferentially along macrograin boundaries but depend on the overall shape of the assembly, meaning magnetostatic energy dominates. The domain structures are imaged at different temperatures for both monolayer and bilayer arrays. The domain wall contrast in the monolayer region is visible until 575 °C, and the magnetic order parameter steeply drops toward the temperature. In the bilayer region, finer and more complicated domains are formed.

Synthesis and magnetic properties of single-crystalline Na2-xMn8O16 nanorods

PubMed Central

2011-01-01

The synthesis of single-crystalline hollandite-type manganese oxides Na2-xMn8O16 nanorods by a simple molten salt method is reported for the first time. The nanorods were characterized by powder X-ray diffraction, scanning electron microscopy, transmission electron microscopy, and a superconducting quantum interference device magnetometer. The magnetic measurements indicated that the nanorods showed spin glass behavior and exchange bias effect at low temperatures. The low-temperature magnetic behaviors can be explained by the uncompensated spins on the surface of the nanorods. PMID:21711626

In situ transmission electron microscopy study on the epitaxial growth of CoSi2 on Si(111) at temperatures below 150 C

NASA Technical Reports Server (NTRS)

Nieh, C. W.; Lin, T. L.

1989-01-01

This paper reports an in situ transmission electron microscopy study on the epitaxial growth of CoSi2 on Si(111) from a 10-nm-thick amorphous mixture of Co and Si in the ratio 1:2, which was formed by codeposition of Co and Si near room temperature. Nuclei of CoSi2 are observed in the as-deposited film. These nuclei are epitaxial and extend through the whole film thickness. Upon annealing, these columnar epitaxial CoSi2 grains grow laterally at temperatures as low as 50 C. The kinetics of this lateral epitaxial growth was studied at temperatures between 50 and 150 C. The activation energy of the growth process is 0.8 + or - 0.1 eV.

Preparation of high-strength Al-Mg-Si-Cu-Fe alloy via heat treatment and rolling

NASA Astrophysics Data System (ADS)

Liu, Chong-yu; Yu, Peng-fei; Wang, Xiao-ying; Ma, Ming-zhen; Liu, Ri-ping

2014-07-01

An Al-Mg-Si-Cu-Fe alloy was solid-solution treated at 560°C for 3 h and then cooled by water quenching or furnace cooling. The alloy samples which underwent cooling by these two methods were rolled at different temperatures. The microstructure and mechanical properties of the rolled alloys were investigated by optical microscopy, scanning electron microscopy, transmission electron microscopy, X-ray diffraction analysis, and tensile testing. For the water-quenched alloys, the peak tensile strength and elongation occurred at a rolling temperature of 180°C. For the furnace-cooled alloys, the tensile strength decreased initially, until the rolling temperature of 420°C, and then increased; the elongation increased consistently with increasing rolling temperature. The effects of grain boundary hardening and dislocation hardening on the mechanical properties of these rolled alloys decreased with increases in rolling temperature. The mechanical properties of the 180°C rolling water-quenched alloy were also improved by the presence of β″ phase. Above 420°C, the effect of solid-solution hardening on the mechanical properties of the rolled alloys increased with increases in rolling temperature.

Quantitative Analysis of Electron Beam Damage in Organic Thin Films

PubMed Central

2017-01-01

In transmission electron microscopy (TEM) the interaction of an electron beam with polymers such as P3HT:PCBM photovoltaic nanocomposites results in electron beam damage, which is the most important factor limiting acquisition of structural or chemical data at high spatial resolution. Beam effects can vary depending on parameters such as electron dose rate, temperature during imaging, and the presence of water and oxygen in the sample. Furthermore, beam damage will occur at different length scales. To assess beam damage at the angstrom scale, we followed the intensity of P3HT and PCBM diffraction rings as a function of accumulated electron dose by acquiring dose series and varying the electron dose rate, sample preparation, and the temperature during acquisition. From this, we calculated a critical dose for diffraction experiments. In imaging mode, thin film deformation was assessed using the normalized cross-correlation coefficient, while mass loss was determined via changes in average intensity and standard deviation, also varying electron dose rate, sample preparation, and temperature during acquisition. The understanding of beam damage and the determination of critical electron doses provides a framework for future experiments to maximize the information content during the acquisition of images and diffraction patterns with (cryogenic) transmission electron microscopy. PMID:28553431

Microscopic evolution of dielectric nanoparticles at different calcination temperatures synthesized via sol-gel auto-combustion

DOE Office of Scientific and Technical Information (OSTI.GOV)

Adil, Muhammad, E-mail: muhammadadil86@hotmail.com; Zaid, Hasnah Mohd, E-mail: hasnamz@petronas.com.my; Chuan, Lee Kean, E-mail: lee.kc@petronas.com.my

2015-07-22

Dielectric nano powder synthesis is carried by a simple and fast sol-gel auto-combustion method. The transformation of crystalline phases of as-synthesized nano powders is investigated through the detailed transmission electron microscopy (TEM), revealed the crystallographic alterations and morphological information even at lattice scale. From specific area electron diffraction (SAED) pattern, has specified the d-spacing and corresponding planes supported by the observed lattice fringes. The morphological characterization of nanoparticles is performed through field-emission scanning electron microscopy (FESEM), exhibiting the increment in particle size due to agglomeration with the increase in annealing temperature. Furthermore, EDX pattern has been used to verify themore » formation of nanoparticles by revealing the presence of required elements.« less

Transmission electron microscopy study of erbium silicide formation from Ti/Er stack for Schottky contact applications.

PubMed

Ratajczak, J; Łaszcz, A; Czerwinski, A; Katcki, J; Phillipp, F; Van Aken, P A; Reckinger, N; Dubois, E

2010-03-01

In this paper, we present results of transmission electron microscopy studies on erbium silicide structures fabricated under various thermal conditions. A titanium cap has been used as a protective layer against oxidation during rapid thermal annealing of an erbium layer in a temperature range of 300-700 degrees C. Both layers (200 nm Ti and 25 nm Er) were deposited by electron-beam sputtering. The investigations have shown that the transformation of the 25-nm-thick erbium into erbium silicide is completed after annealing at 500 degrees C. At higher temperatures, the formation of a titanium silicide layer above erbium silicide is observed. The lowest Schottky barrier has been measured in the sample annealed at 700 degrees C.

Microstructural stability of wrought, laser and electron beam glazed NARloy-Z alloy at elevated temperatures

NASA Technical Reports Server (NTRS)

Singh, J.; Jerman, G.; Bhat, B.; Poorman, R.

1993-01-01

Microstructure of wrought, laser, and electron-beam glazed NARloy-Z(Cu-3 wt.% Ag-0.5 wt.% Zr) was investigated for thermal stability at elevated temperatures (539 to 760 C (1,100 to 1,400 F)) up to 94 h. Optical and scanning electron microscopy and electron probe microanalysis were employed for studying microstructural evolution and kinetics of precipitation. Grain boundary precipitation and precipitate free zones (PFZ's) were observed in the wrought alloy after exposing to temperatures above 605 C (1,120 F). The fine-grained microstructure observed in the laser and electron-beam glazed NARloy-Z was much more stable at elevated temperatures. Microstructural changes correlated well with hardness measurements.

Introduction: A Symposium in Honor of Professor Sir John Meurig Thomas

NASA Astrophysics Data System (ADS)

Gai, P. L.; Saka, H.; Tomokiyo, Y.; Boyes, E. D.

2002-02-01

This issue is dedicated to Professor Sir John Meurig Thomas for his renowned contributions to electron microscopy in the chemical sciences. It is a collection of peer-reviewed leading articles in electron microscopy, based on the presentations at the Microscopy and Microanalysis (M&M) 2000 symposium, which was held to honor Professor Thomas's exceptional scientific leadership and wide-ranging fundamental contributions in the chemical applications of electron microscopy.The issue contains key papers by leading international researchers on the recent developments and applications of electron microscopy in the solid state and liquid state sciences. They include synthesis and characterization of silicon nitride nanorods, nanostructures of amorphous silica, electron microscopy studies of nanoscale structure and chemistry of Pt-Ru electrocatalysts of interest in direct methanol fuel cells, development of in situ wet-environmental transmission electron microscopy for the first nanoscale studies of dynamic liquid-catalyst reactions, strain analysis of silicon by finite element method and energy filtering convergent beam electron diffraction, applications of chemistry with electron microscopy, bismuth nanowires for applications in nanoelectronics technology, synthesis and characterization of quantum dots for superlattices and in situ electron microscopy at very high temperatures to study the motion of W5Si3 on [alpha][beta]-SiN3 substrates.We thank all the participants, including the invited speakers, contributors, and session chairs, who made the symposium successful. We also thank the authors and reviewers of the papers who worked assiduously towards the publication of this issue.We are very grateful to the Microscopy Society of America (MSA) for providing the opportunity to honor Professor Sir John Meurig Thomas. Organizational support from the MSA is also gratefully acknowledged.We thank Charles E. Lyman, editor in chief of Microscopy and Microanalysis for coordinating the publication of this issue and the entire journal staff for their efforts.

Degradation analysis of a Ni-based layered positive-electrode active material cycled at elevated temperatures studied by scanning transmission electron microscopy and electron energy-loss spectroscopy

NASA Astrophysics Data System (ADS)

Kojima, Y.; Muto, S.; Tatsumi, K.; Kondo, H.; Oka, H.; Horibuchi, K.; Ukyo, Y.

We investigate the local structural changes in a positive electrode of a lithium ion secondary battery (LiNi 0.8Co 0.15Al 0.05O 2 (NCA) as the active material) associated with charge-discharge cycling at elevated temperatures by scanning transmission electron microscopy (STEM) and electron energy-loss spectroscopy (EELS). STEM-EELS spectral imaging reveals the evolution of a NiO-like phase localized near the surface and grain boundary regions after many cycles. The amounts of capacity fading and resistance increase are discussed based on the results of the semiquantitative estimation of NiO-like and other product phases. We also identify the chemical state of lithium in the NiO-like phase substituting for Ni.

Ferromagnetism in sphalerite and wurtzite CdS nanostructures

PubMed Central

2013-01-01

Room-temperature ferromagnetism is observed in undoped sphalerite and wurtzite CdS nanostructures which are synthesized by hydrothermal methods. Scanning electron microscopy and transmission electron microscopy results indicate that the sphalerite CdS samples show a spherical-like shape and the wurtzite CdS ones show a flower-like shape, both of which are aggregated by lots of smaller particles. The impurity of the samples has been ruled out by the results of X-ray diffraction, selected-area electron diffraction, and X-ray photoelectron spectroscopy. Magnetization measurements indicate that all the samples exhibit room-temperature ferromagnetism and the saturation magnetization decreases with the increased crystal sizes, revealing that the observed ferromagnetism is defect-related, which is also confirmed by the post-annealing processes. This finding in CdS should be the focus of future electronic and spintronic devices. PMID:23294671

Yttria catalyzed microstructural modifications in oxide dispersion strengthened V-4Cr-4Ti alloys synthesized by field assisted sintering technique

NASA Astrophysics Data System (ADS)

Krishnan, Vinoadh Kumar; Sinnaeruvadi, Kumaran; Verma, Shailendra Kumar; Dash, Biswaranjan; Agrawal, Priyanka; Subramanian, Karthikeyan

2017-08-01

The present work deals with synthesis, characterisation and elevated temperature mechanical property evaluation of V-4Cr-4Ti and oxide (yttria = 0.3, 0.6 and 0.9 at%) dispersion strengthened V-4Cr-4Ti alloy processed by mechanical alloying and field-assisted sintering, under optimal conditions. Microstructural parameters of both powder and sintered samples were deduced by X-ray diffraction (XRD) and further confirmed with high resolution transmission electron microscopy. Powder diffraction and electron microscopy study show that ball milling of starting elemental powders (V-4Cr-4Ti) with and without yttria addition has resulted in single phase α-V (V-4Cr-4Ti) alloy. Wherein, XRD and electron microscopy images of sintered samples have revealed phase separation (viz., Cr-V and Ti-V) and domain size reduction, with yttria addition. The reasons behind phase separation and domain size reduction with yttria addition during sintering are extensively discussed. Microhardness and high temperature compression tests were done on sintered samples. Yttria addition (0.3 and 0.6 at.%) increases the elevated temperature compressive strength and strain hardening exponent of α-V alloys. High temperature compression test of 0.9 at% yttria dispersed α-V alloy reveals a glassy behaviour.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Rowland, Clare E.; Fedin, Igor; Diroll, Benjamin T.

Elevated temperature optoelectronic performance of semiconductor nanomaterials remains an important issue for applications. Here we examine two-dimensional CdSe nanoplatelets (NPs) and CdS/CdSe/CdS shell/core/shell sandwich NPs at temperatures ranging from 300-700 K using static and transient spectroscopies as well as in-situ transmission electron microscopy. NPs exhibit reversible changes in PL intensity, spectral position, and emission linewidth with temperature elevation up to ~500 K, losing a factor of ~8 to 10 in PL intensity at 400 K relative to ambient. Temperature elevation above ~500 K yields thickness dependent, irreversible degradation in optical properties. Electron microscopy relates stability of the NP morphology upmore » to near 600 K followed by sintering and evaporation at still higher temperatures. The mechanism of reversible PL loss, based on differences in decay dynamics between time-resolved photoluminescence and transient absorption, arise primarily from hole trapping in both NPs and sandwich NPs.« less

Structural, Morphological, and Electron Transport Studies of Annealing Dependent In2O3 Dye-Sensitized Solar Cell

PubMed Central

Mahalingam, S.; Abdullah, H.; Shaari, S.; Muchtar, A.; Asshari, I.

2015-01-01

Indium oxide (In2O3) thin films annealed at various annealing temperatures were prepared by using spin-coating method for dye-sensitized solar cells (DSSCs). The objective of this research is to enhance the photovoltaic conversion efficiency in In2O3 thin films by finding the optimum annealing temperature and also to study the reason for high and low performance in the annealed In2O3 thin films. The structural and morphological characteristics of In2O3 thin films were studied via XRD patterns, atomic force microscopy (AFM), field-emission scanning electron microscopy (FESEM), EDX sampling, and transmission electron microscopy (TEM). The annealing treatment modified the nanostructures of the In2O3 thin films viewed through FESEM images. The In2O3-450°C-based DSSC exhibited better photovoltaic performance than the other annealed thin films of 1.54%. The electron properties were studied by electrochemical impedance spectroscopy (EIS) unit. The In2O3-450°C thin films provide larger diffusion rate, low recombination effect, and longer electron lifetime, thus enhancing the performance of DSSC. PMID:26146652

A new genus and species of Nematalycidae (Acari: Endeostigmata)

USDA-ARS?s Scientific Manuscript database

Osperalycus tenerphagus, a new genus and species of Nematalycidae (Acari: Endeostigmata), is described from Ohio, USA, using light microscopy and low temperature scanning electron microscopy. Specimens were extracted from two different loam soils. This genus can be readily distinguished from the oth...

Three-dimensional morphology of GaP-GaAs nanowires revealed by transmission electron microscopy tomography.

PubMed

Verheijen, Marcel A; Algra, Rienk E; Borgström, Magnus T; Immink, George; Sourty, Erwan; Enckevort, Willem J P van; Vlieg, Elias; Bakkers, Erik P A M

2007-10-01

We have investigated the morphology of heterostructured GaP-GaAs nanowires grown by metal-organic vapor-phase epitaxy as a function of growth temperature and V/III precursor ratio. The study of heterostructured nanowires with transmission electron microscopy tomography allowed the three-dimensional morphology to be resolved, and discrimination between the effect of axial (core) and radial (shell) growth on the morphology. A temperature- and precursor-dependent structure diagram for the GaP nanowire core morphology and the evolution of the different types of side facets during GaAs and GaP shell growth were constituted.

Deformation mechanism study of a hot rolled Zr-2.5Nb alloy by transmission electron microscopy. II. In situ transmission electron microscopy study of deformation mechanism change of a Zr-2.5Nb alloy upon heavy ion irradiation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Long, Fei; Daymond, Mark R., E-mail: mark.daymond@queensu.ca; Yao, Zhongwen

2015-03-14

The effect of heavy-ion irradiation on deformation mechanisms of a Zr-2.5Nb alloy was investigated by using the in situ transmission electron microscopy deformation technique. The gliding behavior of prismatic 〈a〉 dislocations has been dynamically observed before and after irradiation at room temperature and 300 °C. Irradiation induced loops were shown to strongly pin the gliding dislocations. Unpinning occurred while loops were incorporated into or eliminated by 〈a〉 dislocations. In the irradiated sample, loop depleted areas with a boundary parallel to the basal plane trace were found by post-mortem observation after room temperature deformation, supporting the possibility of basal channel formation inmore » bulk neutron irradiated samples. Strong activity of pyramidal slip was also observed at both temperatures, which might be another important mechanism to induce plastic instability in irradiated zirconium alloys. Finally, (011{sup ¯}1)〈01{sup ¯}12〉 twinning was identified in the irradiated sample deformed at 300 °C.« less

Deformation mechanism study of a hot rolled Zr-2.5Nb alloy by transmission electron microscopy. II. In situ transmission electron microscopy study of deformation mechanism change of a Zr-2.5Nb alloy upon heavy ion irradiation.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Long, Fei; Daymond, Mark R.; Yao, Zhongwen

2015-03-14

The effect of heavy-ion irradiation on deformation mechanisms of a Zr-2.5Nb alloy was investigated by using the in situ transmission electron microscopy deformation technique. The gliding behavior of prismatic < a > dislocations has been dynamically observed before and after irradiation at room temperature and 300 degrees C. Irradiation induced loops were shown to strongly pin the gliding dislocations. Unpinning occurred while loops were incorporated into or eliminated by < a > dislocations. In the irradiated sample, loop depleted areas with a boundary parallel to the basal plane trace were found by post-mortem observation after room temperature deformation, supporting themore » possibility of basal channel formation in bulk neutron irradiated samples. Strong activity of pyramidal slip was also observed at both temperatures, which might be another important mechanism to induce plastic instability in irradiated zirconium alloys. Finally, {01 (1) over bar1}< 0 (1) over bar 12 > twinning was identified in the irradiated sample deformed at 300 degrees C.« less

Temperature Dependent Electron Transport Properties of Gold Nanoparticles and Composites: Scanning Tunneling Spectroscopy Investigations.

PubMed

Patil, Sumati; Datar, Suwarna; Dharmadhikari, C V

2018-03-01

Scanning tunneling spectroscopy (STS) is used for investigating variations in electronic properties of gold nanoparticles (AuNPs) and its composite with urethane-methacrylate comb polymer (UMCP) as function of temperature. Films are prepared by drop casting AuNPs and UMCP in desired manner on silicon substrates. Samples are further analyzed for morphology under scanning electron microscopy (SEM) and atomic force microscopy (AFM). STS measurements performed in temperature range of 33 °C to 142 °C show systematic variation in current versus voltage (I-V) curves, exhibiting semiconducting to metallic transition/Schottky behavior for different samples, depending upon preparation method and as function of temperature. During current versus time (I-t) measurement for AuNPs, random telegraphic noise is observed at room temperature. Random switching of tunneling current between two discrete levels is observed for this sample. Power spectra derived from I-t show 1/f2 dependence. Statistical analysis of fluctuations shows exponential behavior with time width τ ≈ 7 ms. Local density of states (LDOS) plots derived from I-V curves of each sample show systematic shift in valance/conduction band edge towards/away from Fermi level, with respect to increase in temperature. Schottky emission is best fitted electron emission mechanism for all samples over certain range of bias voltage. Schottky plots are used to calculate barrier heights and temperature dependent measurements helped in measuring activation energies for electron transport in all samples.

Electron microscopy analyses and electrical properties of the layered Bi{sub 2}WO{sub 6} phase

DOE Office of Scientific and Technical Information (OSTI.GOV)

Taoufyq, A.; Laboratoire Matériaux et Environnement LME, Faculté des Sciences, Université Ibn Zohr, BP 8106, Cité Dakhla, Agadir, Maroc; Département d‘Études des Réacteurs, Laboratoire Dosimétrie Capteurs Instrumentation, CEA Cadarache

2013-07-15

The bismuth tungstate Bi{sub 2}WO{sub 6} was synthesized using a classical coprecipitation method followed by a calcination process at different temperatures. The samples were characterized by X-ray diffraction, simultaneous thermogravimetry and differential thermal analysis (TGA/DTA), scanning and transmission electron microscopy (SEM, TEM) analyses. The Rietveld analysis and electron diffraction clearly confirmed the Pca2{sub 1} non centrosymmetric space group previously proposed for this phase. The layers Bi{sub 2}O{sub 2}{sup 2+} and WO{sub 4}{sup 2−} have been directly evidenced from the HRTEM images. The electrical properties of Bi{sub 2}WO{sub 6} compacted pellets systems were determined from electrical impedance spectrometry (EIS) and directmore » current (DC) analyses, under air and argon, between 350 and 700 °C. The direct current analyses showed that the conduction observed from EIS analyses was mainly ionic in this temperature range, with a small electronic contribution. Electrical change above the transition temperature of 660 °C is observed under air and argon atmospheres. The strong conductivity increase observed under argon is interpreted in terms of formation of additional oxygen vacancies coupled with electron conduction. - Graphical abstract: High resolution transmission electron microscopy: inverse fast Fourier transform giving the layered structure of the Bi{sub 2}WO{sub 6} phase, with a representation of the cell dimensions (b and c vectors). The Bi{sub 2}O{sub 2}{sup 2+} and WO{sub 4}{sup 2−} sandwiches are visible in the IFFT image. - Highlights: • Using transmission electron microscopy, we visualize the layered structure of Bi{sub 2}WO{sub 6}. • Electrical analyses under argon gas show some increase in conductivity. • The phase transition at 660 °C is evidenced from electrical modification.« less

Glancing angle deposition of sculptured thin metal films at room temperature

NASA Astrophysics Data System (ADS)

Liedtke, S.; Grüner, Ch; Lotnyk, A.; Rauschenbach, B.

2017-09-01

Metallic thin films consisting of separated nanostructures are fabricated by evaporative glancing angle deposition at room temperature. The columnar microstructure of the Ti and Cr columns is investigated by high resolution transmission electron microscopy and selective area electron diffraction. The morphology of the sculptured metallic films is studied by scanning electron microscopy. It is found that tilted Ti and Cr columns grow with a single crystalline morphology, while upright Cr columns are polycrystalline. Further, the influence of continuous substrate rotation on the shaping of Al, Ti, Cr and Mo nanostructures is studied with view to surface diffusion and the shadowing effect. It is observed that sculptured metallic thin films deposited without substrate rotation grow faster compared to those grown with continuous substrate rotation. A theoretical model is provided to describe this effect.

Thermomechanical and Thermochemical Behavior of a Hafnium-20 Percent Tantalum Alloy. Ph.D. Thesis - North Carolina State Univ., Raleigh

NASA Technical Reports Server (NTRS)

Howell, J. P.

1971-01-01

An investigation was conducted to determine the thermomechanical and thermochemical behavior of a high temperature, oxidation resistant, hafnium-20 percent tantalum alloy. The elastic and shear moduli of this alloy were determined in air up to 1000 C and in vacuum up to 2000 C using a mechanical resonance technique. The internal friction of the alloy was measured up to temperatures greater than 1400 C. Room temperature stress-strain behavior of the oxidized and unoxidized alloy was established. The effect of annealing on the elastic and shear moduli of the extruded rod material was investigated. The martensitic-type phase transformation occurring in the alloy was studied using hot stage metallography and electron microscopy. Static oxidation tests were conducted on the alloy at temperatures from 1000 C to 1700 C with weight gain measurements made as a function of time and temperatures. Surface morphology studies were conducted on the oxide coatings formed at the different temperatures using scanning electron microscopy and X-ray diffraction techniques.

In situ transmission electron microscopy of cadmium selenide nanorod sublimation

DOE PAGES

Hellebusch, Daniel J.; Manthiram, Karthish; Beberwyck, Brandon J.; ...

2015-01-23

In situ electron microscopy is used to observe the morphological evolution of cadmium selenide nanorods as they sublime under vacuum at a series of elevated temperatures. Mass loss occurs anisotropically along the nanorod’s long axis. At temperatures close to the sublimation threshold, the phase change occurs from both tips of the nanorods and proceeds unevenly with periods of rapid mass loss punctuated by periods of relative stability. At higher temperatures, the nanorods sublime at a faster, more uniform rate, but mass loss occurs from only a single end of the rod. Furthermore, we propose a mechanism that accounts for themore » observed sublimation behavior based on the terrace–ledge–kink (TLK) model and how the nanorod surface chemical environment influences the kinetic barrier of sublimation.« less

Analysis of composition and microstructures of Ge grown on porous silicon using Raman spectroscopy and transmission electron microscopy

NASA Astrophysics Data System (ADS)

Aouassa, Mansour; Jadli, Imen; Hassayoun, Latifa Slimen; Maaref, Hassen; Panczer, Gerard; Favre, Luc; Ronda, Antoine; Berbezier, Isabelle

2017-12-01

Composition and microstructure of Ge grown on porous silicon (PSi) by Molecular Beam Epitaxy (MBE) at different temperatures are examined using High Resolution Transmission Electron Microscopy (HRTEM) and Raman spectroscopy. Ge grown at 400 °C on PSi buffer produces a planar Ge film with high crystalline quality compared to Ge grown on bulk Si. This result is attributed to the compliant nature of PSi. Increasing growth temperature >600 °C, changes the PSi morphology, increase the Ge/Si intermixing in the pores during Ge growth and lead to obtain a composite SiGe/Si substrate. Ge content in the composite SiGe substrate can controlled via growth temperature. These substrates serve as low cost virtual substrate for high efficiency III-V/Si solar cells.

Study on the Growth Mechanism of K2Ti4O9 Crystal

NASA Astrophysics Data System (ADS)

Zhou, Xuesong; Fan, Jing; Wei, Xiaoli; Shen, Yi; Meng, Yanzhi

2018-04-01

Potassium hexatitanate (K2Ti4O9) whiskers were prepared by the kneading-drying-calcination method. After the preparation of products under different calcination temperatures and holding times, their morphology and structure were characterized by thermogravimetric and differential thermal, X-ray diffraction (XRD), scanning electron microscopy and transmission electron microscopy. The XRD analysis showed that the reaction mixture was completely converted to K2Ti4O9 crystals at 800 °C when the T/K ratio was 3. Based on the analysis of LS (liquid-solid) growth mechanism, the corresponding transformation reaction mechanism during the roasting was elucidated. K2Ti4O9 whiskers grow mainly through the parallel action at a low temperature. With the increase in temperature, the series effect is obvious.

Synthesis of CoOOH nanorods and application as coating materials of nickel hydroxide for high temperature Ni-MH cells.

PubMed

Hu, W K; Gao, X P; Geng, M M; Gong, Z X; Noréus, D

2005-03-31

Studies on nanoscale materials have received great interest in both fundamental and applied aspects in recent years. In this letter, we report the synthesis of CoOOH nanorods and their possible applications as coating materials on nickel hydroxide for high-temperature nickel-metal hydride (Ni-MH) cells. The morphology and structure of CoOOH nanorods and coated nickel hydroxide particles are investigated by transmission electron microscopy, X-ray diffraction, and scanning electron microscopy, respectively. The electrochemical properties in the cylindrical AA size Ni-MH cells are evaluated. Our results show that the Ni-MH cells, where the positive electrodes are composed of such nanometer sized CoOOH coatings, have a higher capacity available and good performance at elevated temperatures of >50 degrees C.

Chemical vapor deposition growth

NASA Technical Reports Server (NTRS)

Ruth, R. P.; Manasevit, H. M.; Kenty, J. L.; Moudy, L. A.; Simpson, W. I.; Yang, J. J.

1976-01-01

A chemical vapor deposition (CVD) reactor system with a vertical deposition chamber was used for the growth of Si films on glass, glass-ceramic, and polycrystalline ceramic substrates. Silicon vapor was produced by pyrolysis of SiH4 in a H2 or He carrier gas. Preliminary deposition experiments with two of the available glasses were not encouraging. Moderately encouraging results, however, were obtained with fired polycrystalline alumina substrates, which were used for Si deposition at temperatures above 1,000 C. The surfaces of both the substrates and the films were characterized by X-ray diffraction, reflection electron diffraction, scanning electron microscopy optical microscopy, and surface profilometric techniques. Several experiments were conducted to establish baseline performance data for the reactor system, including temperature distributions on the sample pedestal, effects of carrier gas flow rate on temperature and film thickness, and Si film growth rate as a function of temperature.

Analysis of liquid suspensions using scanning electron microscopy in transmission: estimation of the water film thickness using Monte-Carlo simulations.

PubMed

Xiao, J; Foray, G; Masenelli-Varlot, K

2018-02-01

Environmental scanning electron microscopy (ESEM) allows the observation of liquids under specific conditions of pressure and temperature. Moreover, when working in the transmission mode, that is in scanning transmission electron microscopy (STEM), nano-objects can be analysed inside a liquid. The contrast in the images is mass-thickness dependent as in STEM-in-TEM (transmission electron microscopy) using closed cells. However, in STEM-in-ESEM, as the liquid-vapour equilibrium is kept dynamically, the thickness of the water droplet remains unknown. In this paper, the contrasts measured in the experimental images are compared with calculations using Monte-Carlo simulations in order to estimate the thickness of water. Two examples are given. On gold nanoparticles, the thickness of a thick film can be estimated thanks to a contrast inversion. On core-shell latex particles, the grey level of the shell compared with those of the core and of the water film gives a relatively precise measurement of the water film thickness. © 2017 The Authors Journal of Microscopy © 2017 Royal Microscopical Society.

Kinetics of liquid-mediated crystallization of amorphous Ge from multi-frame dynamic transmission electron microscopy

DOE PAGES

Santala, M. K.; Raoux, S.; Campbell, G. H.

2015-12-24

The kinetics of laser-induced, liquid-mediated crystallization of amorphous Ge thin films were studied using multi-frame dynamic transmission electron microscopy (DTEM), a nanosecond-scale photo-emission transmission electron microscopy technique. In these experiments, high temperature gradients are established in thin amorphous Ge films with a 12-ns laser pulse with a Gaussian spatial profile. The hottest region at the center of the laser spot crystallizes in ~100 ns and becomes nano-crystalline. Over the next several hundred nanoseconds crystallization continues radially outward from the nano-crystalline region forming elongated grains, some many microns long. The growth rate during the formation of these radial grains is measuredmore » with time-resolved imaging experiments. Crystal growth rates exceed 10 m/s, which are consistent with crystallization mediated by a very thin, undercooled transient liquid layer, rather than a purely solid-state transformation mechanism. The kinetics of this growth mode have been studied in detail under steady-state conditions, but here we provide a detailed study of liquid-mediated growth in high temperature gradients. Unexpectedly, the propagation rate of the crystallization front was observed to remain constant during this growth mode even when passing through large local temperature gradients, in stark contrast to other similar studies that suggested the growth rate changed dramatically. As a result, the high throughput of multi-frame DTEM provides gives a more complete picture of the role of temperature and temperature gradient on laser crystallization than previous DTEM experiments.« less

Kinetics of liquid-mediated crystallization of amorphous Ge from multi-frame dynamic transmission electron microscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Santala, M. K., E-mail: melissa.santala@oregonstate.edu; Campbell, G. H.; Raoux, S.

2015-12-21

The kinetics of laser-induced, liquid-mediated crystallization of amorphous Ge thin films were studied using multi-frame dynamic transmission electron microscopy (DTEM), a nanosecond-scale photo-emission transmission electron microscopy technique. In these experiments, high temperature gradients are established in thin amorphous Ge films with a 12-ns laser pulse with a Gaussian spatial profile. The hottest region at the center of the laser spot crystallizes in ∼100 ns and becomes nano-crystalline. Over the next several hundred nanoseconds crystallization continues radially outward from the nano-crystalline region forming elongated grains, some many microns long. The growth rate during the formation of these radial grains is measured withmore » time-resolved imaging experiments. Crystal growth rates exceed 10 m/s, which are consistent with crystallization mediated by a very thin, undercooled transient liquid layer, rather than a purely solid-state transformation mechanism. The kinetics of this growth mode have been studied in detail under steady-state conditions, but here we provide a detailed study of liquid-mediated growth in high temperature gradients. Unexpectedly, the propagation rate of the crystallization front was observed to remain constant during this growth mode even when passing through large local temperature gradients, in stark contrast to other similar studies that suggested the growth rate changed dramatically. The high throughput of multi-frame DTEM provides gives a more complete picture of the role of temperature and temperature gradient on laser crystallization than previous DTEM experiments.« less

Imaging electron wave functions inside open quantum rings.

PubMed

Martins, F; Hackens, B; Pala, M G; Ouisse, T; Sellier, H; Wallart, X; Bollaert, S; Cappy, A; Chevrier, J; Bayot, V; Huant, S

2007-09-28

Combining scanning gate microscopy (SGM) experiments and simulations, we demonstrate low temperature imaging of the electron probability density |Psi|(2)(x,y) in embedded mesoscopic quantum rings. The tip-induced conductance modulations share the same temperature dependence as the Aharonov-Bohm effect, indicating that they originate from electron wave function interferences. Simulations of both |Psi|(2)(x,y) and SGM conductance maps reproduce the main experimental observations and link fringes in SGM images to |Psi|(2)(x,y).

Nanocrystals of [Cu3(btc)2] (HKUST-1): a combined time-resolved light scattering and scanning electron microscopy study.

PubMed

Zacher, Denise; Liu, Jianing; Huber, Klaus; Fischer, Roland A

2009-03-07

The formation of [Cu(3)(btc)(2)] (HKUST-1; btc = 1,3,5-benzenetricarboxylate) nanocrystals from a super-saturated mother solution at room temperature was monitored by time-resolved light scattering (TLS); the system is characterized by a rapid growth up to a size limit of 200 nm within a few minutes, and the size and shape of the crystallites were also determined by scanning electron microscopy (SEM).

Photosynthetic microorganism-mediated synthesis of akaganeite (beta-FeOOH) nanorods.

PubMed

Brayner, Roberta; Yéprémian, Claude; Djediat, Chakib; Coradin, Thibaud; Herbst, Fréderic; Livage, Jacques; Fiévet, Fernand; Couté, Alain

2009-09-01

Common Anabaena and Calothrix cyanobacteria and Klebsormidium green algae are shown to form intracellularly akaganeite beta-FeOOH nanorods of well-controlled size and unusual morphology at room temperature. X-ray diffraction (XRD), transmission electron microscopy (TEM), and scanning electron microscopy X-ray energy dispersive spectrometry (SEM-EDS) analyses are used to investigate particle structure, size, and morphology. A mechanism involving iron-siderophore complex formation is proposed and compared with iron biomineralization in magnetotactic bacteria.

Traveling interface modulations and anisotropic front propagation in ammonia oxidation over Rh(110)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Rafti, Matías; Institut für Physikalische Chemie und Elektrochemie, Leibniz-Universität Hannover, Callinstr. 3-3a, D-30167 Hannover; Borkenhagen, Benjamin

The bistable NH{sub 3} + O{sub 2} reaction over a Rh(110) surface was explored in the pressure range 10{sup −6}–10{sup −3} mbar and in the temperature range 300–900 K using photoemission electron microscopy and low energy electron microscopy as spatially resolving methods. We observed a history dependent anisotropy in front propagation, traveling interface modulations, transitions with secondary reaction fronts, and stationary island structures.

Development of an Integrated Thermocouple for the Accurate Sample Temperature Measurement During High Temperature Environmental Scanning Electron Microscopy (HT-ESEM) Experiments.

PubMed

Podor, Renaud; Pailhon, Damien; Ravaux, Johann; Brau, Henri-Pierre

2015-04-01

We have developed two integrated thermocouple (TC) crucible systems that allow precise measurement of sample temperature when using a furnace associated with an environmental scanning electron microscope (ESEM). Sample temperatures measured with these systems are precise (±5°C) and reliable. The TC crucible systems allow working with solids and liquids (silicate melts or ionic liquids), independent of the gas composition and pressure. These sample holder designs will allow end users to perform experiments at high temperature in the ESEM chamber with high precision control of the sample temperature.

Enhancement of Curie temperature of barium hexaferrite by dense electronic excitations

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sharma, Manju; Kashyap, Subhash C.; Gupta, Hem C.

2014-07-15

Curie temperature of polycrystalline barium hexaferrite (BaFe{sub 12}O{sub 19}), prepared by conventional solid state technique, is anomalously and significantly enhanced (by nearly 15%) by energetic heavy ion irradiation (150 MeV, Ag{sup 12+}) at ambient temperature due to dense electronic excitations Moderate fluence (1 × 10{sup 12} ions/cm{sup 2}) induces structural defects giving rise to above enhancement. As established by X-ray diffraction, scanning electron microscopy and Raman studies, higher fluence (1 × 10{sup 13} ions/cm{sup 2}) has structurally transformed the sample to amorphous phase with marginal change in magnetization and Curie temperature.

Investigation of Thermal Stability of P2-NaxCoO2 Cathode Materials for Sodium Ion Batteries Using Real-Time Electron Microscopy.

PubMed

Hwang, Sooyeon; Lee, Yongho; Jo, Eunmi; Chung, Kyung Yoon; Choi, Wonchang; Kim, Seung Min; Chang, Wonyoung

2017-06-07

Here, we take advantage of in situ transmission electron microscopy (TEM) to investigate the thermal stability of P2-type Na x CoO 2 cathode materials for sodium ion batteries, which are promising candidates for next-generation lithium ion batteries. A double-tilt TEM heating holder was used to directly characterize the changes in the morphology and the crystallographic and electronic structures of the materials with increase in temperature. The electron diffraction patterns and the electron energy loss spectra demonstrated the presence of cobalt oxides (Co 3 O 4 , CoO) and even metallic cobalt (Co) at higher temperatures as a result of reduction of Co ions and loss of oxygen. The bright-field TEM images revealed that the surface of Na x CoO 2 becomes porous at high temperatures. Higher cutoff voltages result in degrading thermal stability of Na x CoO 2 . The observations herein provide a valuable insight that thermal stability is one of the important factors to be considered in addition to the electrochemical properties when developing new electrode materials for novel battery systems.

Investigation of Thermal Stability of P2–Na xCoO 2 Cathode Materials for Sodium Ion Batteries Using Real-Time Electron Microscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hwang, Sooyeon; Lee, Yongho; Jo, Eunmi

In this paper, we take advantage of in situ transmission electron microscopy (TEM) to investigate the thermal stability of P2-type Na xCoO 2 cathode materials for sodium ion batteries, which are promising candidates for next-generation lithium ion batteries. A double-tilt TEM heating holder was used to directly characterize the changes in the morphology and the crystallographic and electronic structures of the materials with increase in temperature. The electron diffraction patterns and the electron energy loss spectra demonstrated the presence of cobalt oxides (Co 3O 4, CoO) and even metallic cobalt (Co) at higher temperatures as a result of reduction ofmore » Co ions and loss of oxygen. The bright-field TEM images revealed that the surface of Na xCoO 2 becomes porous at high temperatures. Higher cutoff voltages result in degrading thermal stability of Na xCoO 2. Finally, the observations herein provide a valuable insight that thermal stability is one of the important factors to be considered in addition to the electrochemical properties when developing new electrode materials for novel battery systems.« less

Investigation of Thermal Stability of P2–Na xCoO 2 Cathode Materials for Sodium Ion Batteries Using Real-Time Electron Microscopy

DOE PAGES

Hwang, Sooyeon; Lee, Yongho; Jo, Eunmi; ...

2017-05-11

In this paper, we take advantage of in situ transmission electron microscopy (TEM) to investigate the thermal stability of P2-type Na xCoO 2 cathode materials for sodium ion batteries, which are promising candidates for next-generation lithium ion batteries. A double-tilt TEM heating holder was used to directly characterize the changes in the morphology and the crystallographic and electronic structures of the materials with increase in temperature. The electron diffraction patterns and the electron energy loss spectra demonstrated the presence of cobalt oxides (Co 3O 4, CoO) and even metallic cobalt (Co) at higher temperatures as a result of reduction ofmore » Co ions and loss of oxygen. The bright-field TEM images revealed that the surface of Na xCoO 2 becomes porous at high temperatures. Higher cutoff voltages result in degrading thermal stability of Na xCoO 2. Finally, the observations herein provide a valuable insight that thermal stability is one of the important factors to be considered in addition to the electrochemical properties when developing new electrode materials for novel battery systems.« less

BASIC STUDIES IN PERCUTANEOUS ABSORPTION.

DTIC Science & Technology

FATTY ACIDS, *SKIN(ANATOMY), ABSORPTION, ALKYL RADICALS, AMIDES, DIFFUSION, ELECTRON MICROSCOPY, HUMIDITY, LABORATORY ANIMALS, LIPIDS, ORGANIC SOLVENTS, PENETRATION, PRIVATION, PROTEINS, RATS, TEMPERATURE, WATER

Formation of MoS2 inorganic fullerenes (IFs) by the reaction of MoO3 nanobelts and S.

PubMed

Li, Xiao Lin; Li, Ya Dong

2003-06-16

The reaction of MoO3 and S at temperatures higher than 300 degrees C in an argon atmosphere provides a convenient and effective method for the synthesis of MoS2 nanocrystalline substances. MoS2 nanotubes and fullerene-like nanoparticles have been obtained by the reaction at 850 degrees C under well-controlled conditions. The influences of reaction temperature and duration were carefully investigated in this paper. All of the nanostructures were characterized by Xray powder diffraction (XRD), transmission electron microscopy (TEM), and high-resolution transmission electron microscopy (HRTEM). A stepwise reaction model and rolling mechanism were proposed based on the experimental results.

The Role of Phase Changes in TiO2/Pt/TiO2 Filaments

NASA Astrophysics Data System (ADS)

Bíró, Ferenc; Hajnal, Zoltán; Dücső, Csaba; Bársony, István

2018-04-01

This work analyses the role of phase changes in TiO2/Pt/TiO2 layer stacks for micro-heater application regarding their stability and reliable operation. The polycrystalline Pt layer wrapped in a TiO2 adhesion layer underwent a continuous recrystallisation in a self-heating operation causing a drift in the resistance ( R) versus temperature ( T) performance. Simultaneously, the TiO2 adhesion layer also deteriorates at high temperature by phase changes from amorphous to anatase and rutile crystallite formation, which not only influences the Pt diffusion in different migration phenomena, but also reduces the cross section of the Pt heater wire. Thorough scanning electron microscopy, energy dispersive spectroscopy, cross-sectional transmission electron microscopy (XTEM) and electron beam diffraction analysis of the structures operated at increasing temperature revealed the elemental structural processes leading to the instabilities and the accelerated degradation, resulting in rapid breakdown of the heater wire. Owing to stability and reliability criteria, the conditions for safe operation of these layer structures could be determined.

Nanostructure ZnFe2O4 with Bacillus subtilis for Detection of LPG at Low Temperature

NASA Astrophysics Data System (ADS)

Goutham, Solleti; Kumar, Devarai Santhosh; Sadasivuni, Kishor Kumar; Cabibihan, John-John; Rao, Kalagadda Venkateswara

2017-04-01

The present study deals with the development of a chemical sensor for the detection of liquefied petroleum gas (LPG) at a low operating temperature using Zinc ferrite (ZnFe2O4)/ Bacillus subtilis ( B. subtilis) hybrid nanostructures. The nanostructure ZnFe2O4 and B. subtilis powder, taken in equal proportion was made into films using the spin coating technique. X-ray diffraction, thermal analysis, scanning electron microscopy, and transmission electron microscopy were used to study morphology, structure and crystallite size. The sensing properties of the hybrid structure were studied and excellent response was observed in the temperature range of 50-55°C for 400 ppm LPG, when compared to the individual components of the hybrid. The signal output of the proposed sensor were extremely stable for more than 30 days. This method proposes the usage of the biomolecule/metal oxide composites in electronics and helps to reduce the metal oxide usage.

Coarsening behaviour of M23C6 carbides in creep-resistant steel exposed to high temperatures

NASA Astrophysics Data System (ADS)

Godec, M.; Skobir Balantič, D. A.

2016-07-01

High operating temperatures can have very deleterious effects on the long-term performance of high-Cr, creep-resistant steels used, for example, in the structural components of power plants. For the popular creep-resistant steel X20CrMoV12.1 we analysed the processes of carbide growth using a variety of analytical techniques: transmission electron microscopy (TEM) and diffraction (TED), scanning electron microscopy (SEM), and electron backscatter diffraction (EBSD). The evolution of the microstructure after different aging times was the basis for a much better understanding of the boundary-migration processes and the growth of the carbides. We present an explanation as to why some locations are preferential for this growth, and using EBSD we were able to define the proper orientational relationship between the carbides and the matrix.

Microstructure, crystallography and nucleation mechanism of NANOBAIN steel

NASA Astrophysics Data System (ADS)

Huang, Yao; Zhao, Ai-min; He, Jian-guo; Wang, Xiao-pei; Wang, Zhi-gang; Qi, Liang

2013-12-01

The microstructure of bainite ferrite in NANOBAIN steel transformed at different temperatures was investigated by scanning electron microscopy, transmission electron microscopy, electron back-scattered diffraction, and vickers hardness tester in detail. It is found that the average width of bainitic ferrite (BF) plates can be refined to be thinner with the reduction of temperature (473-573 K), and the bainitic ferrite plates can reach up to 20-74 nm at 473 K. Crystallographic analysis reveals that the bainitic ferrite laths are close to the Nishiyama-Wasserman orientation relationship with their parent austenite. Temperature shows a significant effect on the variant selection, and a decrease in temperature generally weakens the variant selection. Thermodynamic analyses indicates that the Lacher, Fowler and Guggenheim (LFG) model is more suitable than the Kaufman, Radcliffe and Cohen (KRC) model dealing with NANOBAIN steel at a low temperature range. The free energy change Δ G γ→BF is about -1500 J·mol-1 at 473 K, which indicates that nucleation in NANOBAIN steel is the shear mechanism. Finally, the formation of carbon poor regions is thermodynamically possible, and the existence of carbon poor regions can greatly increase the possibility of the shear mechanism.

Effect of Scandium on the Interaction of Concurrent Precipitation and Recrystallization in Commercial AA3003 Aluminum Alloy

NASA Astrophysics Data System (ADS)

Tu, Yiyou; Qian, Huan; Zhou, Xuefeng; Jiang, Jianqing

2014-04-01

In the current study, the effect of Sc addition on the interaction of concurrent precipitation and recrystallization in commercial AA3003 aluminum alloy was investigated using optical microscopy, scanning electron microscopy, and transmission electron microscopy. In case of AA3003 alloy, which was cold rolled to a true strain of 2.20 and heated at a heating rate of 150 K/s, the onset of precipitation and ending of recrystallization are signified by the critical temperature, T C ~740 K (467 °C). There is a change in the shape of the recrystallized grains from pancake-like to equiaxed shape, as the annealing temperature increases greater than T C. In case of AA3003 alloy microalloyed with 0.4 wt pct of Sc, the high no. density precipitation of coherent Al3Sc precipitates always occurs before recrystallization because of the small nucleation barrier and high rate of decomposition. This leads to extremely coarse pancake-like recrystallization grains with high fraction of low-angle grain boundaries in the entire annealing temperature range, even at a high brazing temperature of 883 K (610 °C).

Microstructure and corrosion resistance of nitrogen-rich surface layers on AISI 304 stainless steel by rapid nitriding in a hollow cathode discharge

NASA Astrophysics Data System (ADS)

Li, Yang; He, Yongyong; Zhang, Shangzhou; Wang, Wei; Zhu, Yijie

2018-01-01

Nitriding treatments have been successfully applied to austenitic stainless steels to improve their hardness and tribological properties. However, at temperatures above 450 °C, conventional plasma nitriding processes decrease the corrosion resistance due to the formation of CrN phases within the modified layer. In this work, AISI 304 austenitic stainless steels were efficiently treated by rapid plasma nitriding at a high temperature of 530 °C in a hollow cathode discharge. The enhanced ionization obtained in the hollow cathode configuration provided a high current density and, consequently, a high temperature could be attained in a short time. The nitrided layers were characterized by X-ray diffraction, scanning electron microscopy, atomic force microscopy, transmission electron microscopy and X-ray photoelectron spectroscopy. The results indicated that the dual-layer structure of the nitrided layer consists of a high-N face-centered cubic structure with a free CrN precipitate outer (top) layer and a nitrogen-expanded austenite S-phase bottom layer. The rapid nitriding-assisted hollow cathode discharge technique permits the use of high temperatures, as high as 530 °C, without promoting degradation in the corrosion resistance of stainless steel.

Unraveling micro- and nanoscale degradation processes during operation of high-temperature polymer-electrolyte-membrane fuel cells

NASA Astrophysics Data System (ADS)

Hengge, K.; Heinzl, C.; Perchthaler, M.; Varley, D.; Lochner, T.; Scheu, C.

2017-10-01

The work in hand presents an electron microscopy based in-depth study of micro- and nanoscale degradation processes that take place during the operation of high-temperature polymer-electrolyte-membrane fuel cells (HT-PEMFCs). Carbon supported Pt particles were used as cathodic catalyst material and the bimetallic, carbon supported Pt/Ru system was applied as anode. As membrane, cross-linked polybenzimidazole was used. Scanning electron microscopy analysis of cross-sections of as-prepared and long-term operated membrane-electrode-assemblies revealed insight into micrometer scale degradation processes: operation-caused catalyst redistribution and thinning of the membrane and electrodes. Transmission electron microscopy investigations were performed to unravel the nanometer scale phenomena: a band of Pt and Pt/Ru nanoparticles was detected in the membrane adjacent to the cathode catalyst layer. Quantification of the elemental composition of several individual nanoparticles and the overall band area revealed that they stem from both anode and cathode catalyst layers. The results presented do not demonstrate any catastrophic failure but rather intermediate states during fuel cell operation and indications to proceed with targeted HT-PEMFC optimization.

Synthesis and characterization of nano TiO2-SiO2: PVA composite - a novel route

NASA Astrophysics Data System (ADS)

Venckatesh, Rajendran; Balachandaran, Kartha; Sivaraj, Rajeshwari

2012-07-01

A novel, simple, less time consuming and cost-effective sol-gel method has been developed to synthesize nano titania-silica with polyvinyl alcohol (PVA) composite relatively at low temperature in acidic pH. Titania sol is prepared by hydrolysis of titanium tetrachloride and was mixed with silicic acid and tetrahydrofuran mixture. The reaction was carried out under vigorous stirring for 6 h and dried at room temperature with the addition of PVA solution. The resulting powders were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, Fourier transform infrared (FT-IR), UV-visible spectroscopy and thermal techniques. The grain size of the particles was calculated by X-ray diffraction; surface morphology and chemical composition were determined from scanning electron microscopy-energy dispersive spectroscopy; metal oxide stretching was confirmed from FT-IR spectroscopy; bandgap was calculated using UV-visible spectroscopy, and thermal stability of the prepared composite was determined by thermogravimetric/differential thermal analysis. Since TiO2 got agglomerated on the surface of SiO2, effective absorptive sites increase which in turn increase the photocatalytic efficiency of the resulting composite.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhao, Donghui; Key Lab of Inorganic Coating Materials, Shanghai Institute of Ceramics, Chinese Academy of Sciences, 1295 Dingxi, Changning, Shanghai 200050; Zhu, Yingchun, E-mail: yzhu@mail.sic.ac.cn

In this article, the polymorph selection of calcium carbonate has been successfully achieved in water-soluble carboxymethyl chitosan aqueous solution at different temperatures (25-95 {sup o}C). Vaterite is formed in carboxymethyl chitosan solution 25 {sup o}C accompanied with trace of calcite, whereas pure aragonite is obtained at 95 {sup o}C. Scanning electron microscopy and transmission electron microscopy analyses show that the products are formed from the recrystallization of nanometer crystallites. Thermodynamic and kinetic analyses reveal that the polymorph of calcium carbonate is controlled and selected by kinetics in various temperatures. As a heterogeneous nucleator and stabilizing agent, carboxymethyl chitosan changes themore » nucleation and growth of calcium carbonate from thermodynamic into kinetic control. Under kinetic limitation, the reaction rate of aragonite increases along with the elevating of temperature and surpasses the rate of vaterite above 327 K.« less

Low-temperature MOCVD deposition of Bi2Te3 thin films using Et2BiTeEt as single source precursor

NASA Astrophysics Data System (ADS)

Bendt, Georg; Gassa, Sanae; Rieger, Felix; Jooss, Christian; Schulz, Stephan

2018-05-01

Et2BiTeEt was used as single source precursor for the deposition of Bi2Te3 thin films on Si(1 0 0) substrates by metal organic chemical vapor deposition (MOCVD) at very low substrate temperatures. Stoichiometric and crystalline Bi2Te3 films were grown at 230 °C, which is approximately 100 °C lower compared to conventional MOCVD processes using one metal organic precursors for each element. The Bi2Te3 films were characterized using scanning electron microscopy, high-resolution transmission electron microscopy and X-ray diffraction. The elemental composition of the films, which was determined by energy-dispersive X-ray spectroscopy and X-ray photoelectron spectroscopy, was found to be strongly dependent of the substrate temperature.

Devolatilization Studies of Oil Palm Biomass for Torrefaction Process through Scanning Electron Microscopy

NASA Astrophysics Data System (ADS)

Daud, D.; Abd. Rahman, A.; Shamsuddin, A. H.

2016-03-01

In this work, palm oil biomass consisting of empty fruit bunch (EFB), mesocarp fibre and palm kernel shell (PKS) were chosen as raw material for torrefaction process. Torrefaction process was conducted at various temperatures of 240 °C, 270 °C and 300 °C with a residence time of 60 minutes. The morphology of the raw and torrefied biomass was then observed through Scanning Electron Microscopy (SEM) images. Also, through this experiment the correlation between the torrefaction temperatures with the volatile gases released were studied. From the observation, the morphology structure of the biomass exhibited inter-particle gaps due to the release of volatile gases and it is obviously seen more at higher temperatures. Moreover, the change of the biomass structure is influenced by the alteration of the lignocellulose biomass.

A highly sensitive room temperature H2S gas sensor based on SnO2 multi-tube arrays bio-templated from insect bristles.

PubMed

Tian, Junlong; Pan, Feng; Xue, Ruiyang; Zhang, Wang; Fang, Xiaotian; Liu, Qinglei; Wang, Yuhua; Zhang, Zhijian; Zhang, Di

2015-05-07

A tin oxide multi-tube array (SMTA) with a parallel effect was fabricated through a simple and promising method combining chemosynthesis and biomimetic techniques; a biomimetic template was derived from the bristles on the wings of the Alpine Black Swallowtail butterfly (Papilio maackii). SnO2 tubes are hollow and porous structures with micro-pores regularly distributed on the wall. The morphology, the delicate microstructure and the crystal structure of this SMTA were characterized by super resolution digital microscopy, scanning electron microscopy, transmission electron microscopy and X-ray diffraction. The SMTA exhibits a high sensitivity to H2S gas at room temperature. It also exhibits a short response/recovery time, with an average value of 14/30 s at 5 ppm. In particular, heating is not required for the SMTA in the gas sensitivity measurement process. On the basis of these results, SMTA is proposed as a suitable new material for the design and fabrication of room-temperature H2S gas sensors.

Electrical conductivity and morphology of electrochemical synthesized polyaniline/CuO nano composites

NASA Astrophysics Data System (ADS)

Ashokkumar, S. P.; Yesappa, L.; Vijeth, H.; Niranjana, M.; Devendrappa, H.

2018-05-01

Polyaniline (PANI) and Polyaniline/CuO nanocomposite have been synthesized by using electrochemical deposition method. The composite was characterized using Fourier transform infra-red spectroscopy (FT-IR) to confirm the chemical interaction changes, micro structural morphology was done by Field Emission Scanning Electronic Microscopy (FESEM) and High Resolution Transmission Electron Microscopy (HRTEM). The dielectric constant and AC conductivity are found to increases with increase in temperature range (303 to 393K), these results shows enhancement in electrical conductivity due to effect of nanocomposite.

Metal-Coated Optical Fibers for High Temperature Applications

NASA Technical Reports Server (NTRS)

Zeakes, Jason; Murphy, Kent; Claus, Richard; Greene, Jonathan; Tran, Tuan

1996-01-01

A DC magnetron sputtering system has been used to actively coat optical fibers with hermetic metal coatings during the fiber draw process. Thin films of Inconel 625 have been deposited on optical fibers and annealed in air at 2000 F. Scanning electron microscopy and Auger electron microscopy have been used to investigate the morphology and composition of the films prior to and following thermal cycling. Issues to be addressed include film adhesion, other coating materials, and a discussion of additional applications for this novel technology.

Short review on chemical bath deposition of thin film and characterization

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mugle, Dhananjay, E-mail: dhananjayforu@gmail.com; Jadhav, Ghanshyam, E-mail: ghjadhav@rediffmail.com

2016-05-06

This reviews the theory of early growth of the thin film using chemical deposition methods. In particular, it critically reviews the chemical bath deposition (CBD) method for preparation of thin films. The different techniques used for characterizations of the chemically films such as X-ray diffractometer (XRD), Scanning electron microscopy (SEM), Transmission electron microscopy (TEM), Electrical conductivity and Energy Dispersive Spectroscopy (EDS) are discussed. Survey shows the physical and chemical properties solely depend upon the time of deposition, temperature of deposition.

Fabrication of bright and thin Zn₂SiO₄ luminescent film for electron beam excitation-assisted optical microscope.

PubMed

Furukawa, Taichi; Kanamori, Satoshi; Fukuta, Masahiro; Nawa, Yasunori; Kominami, Hiroko; Nakanishi, Yoichiro; Sugita, Atsushi; Inami, Wataru; Kawata, Yoshimasa

2015-07-13

We fabricated a bright and thin Zn₂SiO₄ luminescent film to serve as a nanometric light source for high-spatial-resolution optical microscopy based on electron beam excitation. The Zn₂SiO₄ luminescent thin film was fabricated by annealing a ZnO film on a Si₃N₄ substrate at 1000 °C in N₂. The annealed film emitted bright cathodoluminescence compared with the as-deposited film. The film is promising for nano-imaging with electron beam excitation-assisted optical microscopy. We evaluated the spatial resolution of a microscope developed using this Zn₂SiO₄ luminescent thin film. This is the first report of the investigation and application of ZnO/Si₃N₄ annealed at a high temperature (1000 °C). The fabricated Zn₂SiO₄ film is expected to enable high-frame-rate dynamic observation with ultra-high resolution using our electron beam excitation-assisted optical microscopy.

High indium content homogenous InAlN layers grown by plasma-assisted molecular beam epitaxy

NASA Astrophysics Data System (ADS)

Kyle, Erin C. H.; Kaun, Stephen W.; Wu, Feng; Bonef, Bastien; Speck, James S.

2016-11-01

InAlN grown by plasma-assisted molecular beam epitaxy often contains a honeycomb microstructure. The honeycomb microstructure consists of 5-10 nm diameter aluminum-rich regions which are surrounded by indium-rich regions. Layers without this microstructure were previously developed for nominally lattice-matched InAlN and have been developed here for higher indium content InAlN. In this study, InAlN was grown in a nitrogen-rich environment with high indium to aluminum flux ratios at low growth temperatures. Samples were characterized by high-resolution x-ray diffraction, atomic force microscopy, high-angle annular dark-field scanning transmission electron microscopy, and atom probe tomography. Atomic force microscopy showed InAlN layers grown at temperatures below 450 °C under nitrogen-rich conditions were free of droplets. InAlN films with indium contents up to 81% were grown at temperatures between 410 and 440 °C. High-angle annular dark-field scanning transmission electron microscopy and atom probe tomography showed no evidence of honeycomb microstructure for samples with indium contents of 34% and 62%. These layers are homogeneous and follow a random alloy distribution. A growth diagram for InAlN of all indium contents is reported.

Geometry of phase-separated domains in phospholipid bilayers by diffraction-contrast electron microscopy.

PubMed Central

Hui, S W

1981-01-01

The sizes and shapes of solidus (gel) phase domains in the hydrated molecular bilayers of dilauroylphosphatidylcholine/dipalmitoylphasphatidylcholine (DLPC/DPPC) (1:1) and phosphatidylserine (PS)/DPPC (1:2) are visualized directly by low dose diffraction-contrast electron microscopy. The temperature and humidity of the bilayers are controlled by an environmental chamber set in an electron microscope. The contrast between crystalline domains is enhanced by electron optical filtering of the diffraction patterns of the bilayers. The domains are seen as a patchwork in the plane of the bilayer, with an average width of 0.2-0.5 micrometer. The percentage of solidus area measured from diffraction-contrast micrographs at various temperatures agrees in general with those depicted by known phase diagrams. The shape and size of the domains resemble those seen by freeze-fracture in multilamellar vesicles. Temperature-related changes in domain size and in phase boundary per unit area are more pronounced in the less miscible DLPC/DPPC mixture. No significant change in these geometric parameters with temperature is found in the PS/DPPC mixture. Mapping domains by their molecular diffraction signals not only verifies the existance of areas of different molecular packing during phase separation but also provides a quantitative measurement of structural boundaries and defects in lipid bilayers. Images FIGURE 1 FIGURE 3 FIGURE 6 PMID:6894707

Room Temperature Ferromagnetism of Fe Doped Indium Tin Oxide Based on Dispersed Fe3O4 Nanoparticles

NASA Astrophysics Data System (ADS)

Okada, Koichi; Kohiki, Shigemi; Nishi, Sachio; Shimooka, Hirokazu; Deguchi, Hiroyuki; Mitome, Masanori; Bando, Yoshio; Shishido, Toetsu

2007-09-01

Transmission electron microscopy revealed that Fe3O4 nanoparticles with diameter of ≈200 nm dispersed in Fe doped indium tin oxide (Fe@ITO) powders exhibiting co-occurrence of room temperature ferromagnetism and superparamagnetism. Although we observed no X-ray diffraction peak from Fe related compounds for Fe0.19@ITO (ITO: In1.9Sn0.1O3) powders, the powders showed both hysteresis loop in field dependent magnetization at 300 K and divergence of zero-field-cooled magnetization from field-cooled magnetization. Scanning transmission electron microscopy with energy dispersive X-ray spectroscopy demonstrated that the nanoparticle with diameter of ≈200 nm consists of Fe and oxygen. Transmission electron diffraction revealed that crystal structure of the nanoparticle is inverse spinel type Fe3O4. The Fe3O4 crystalline phase by electron diffraction is consistent with the saturation magnetization of 1.3 μB/Fe and magnetic anomaly at ≈110 K observed for the powders.

Atomistic structures of nano-engineered SiC and radiation-induced amorphization resistance

NASA Astrophysics Data System (ADS)

Imada, Kenta; Ishimaru, Manabu; Sato, Kazuhisa; Xue, Haizhou; Zhang, Yanwen; Shannon, Steven; Weber, William J.

2015-10-01

Nano-engineered 3C-SiC thin films, which possess columnar structures with high-density stacking faults and twins, were irradiated with 2 MeV Si ions at cryogenic and room temperatures. From cross-sectional transmission electron microscopy observations in combination with Monte Carlo simulations based on the Stopping and Range of Ions in Matter code, it was found that their amorphization resistance is six times greater than bulk crystalline SiC at room temperature. High-angle bright-field images taken by spherical aberration corrected scanning transmission electron microscopy revealed that the distortion of atomic configurations is localized near the stacking faults. The resultant strain field probably contributes to the enhancement of radiation tolerance of this material.

Room temperature synthesis of rutile nanorods and their applications on cloth

NASA Astrophysics Data System (ADS)

Fei, Bin; Deng, Zhaoxiang; Xin, John H.; Zhang, Yihe; Pang, Geoffrey

2006-04-01

In order to achieve better photocatalytic performance, rutile nanorods dispersed in anatase and brookite phases were synthesized from titanium isopropoxide (TIP) in a concentrated HNO3 solution at room temperature (23 °C). X-ray diffraction results indicated that the percentage of rutile increased with increasing peptization time. Scanning electron microscopy and and high-resolution transmission electron microscopy measurements revealed that the nanosized titania particles mainly consisted of granular anatase and brookite, and rod-like rutile. It was interesting that the stability of the colloid increased with increasing nanoparticle concentration, and the tricrystalline titania showed a photocatalytic activity higher than that of pure anatase. These nanocrystals were applied onto cotton fabrics, and achieved a promising bactericidal photocatalytic activity and excellent protection against UV radiation.

Ab initio structure determination of nanocrystals of organic pharmaceutical compounds by electron diffraction at room temperature using a Timepix quantum area direct electron detector.

PubMed

van Genderen, E; Clabbers, M T B; Das, P P; Stewart, A; Nederlof, I; Barentsen, K C; Portillo, Q; Pannu, N S; Nicolopoulos, S; Gruene, T; Abrahams, J P

2016-03-01

Until recently, structure determination by transmission electron microscopy of beam-sensitive three-dimensional nanocrystals required electron diffraction tomography data collection at liquid-nitrogen temperature, in order to reduce radiation damage. Here it is shown that the novel Timepix detector combines a high dynamic range with a very high signal-to-noise ratio and single-electron sensitivity, enabling ab initio phasing of beam-sensitive organic compounds. Low-dose electron diffraction data (∼ 0.013 e(-) Å(-2) s(-1)) were collected at room temperature with the rotation method. It was ascertained that the data were of sufficient quality for structure solution using direct methods using software developed for X-ray crystallography (XDS, SHELX) and for electron crystallography (ADT3D/PETS, SIR2014).

Atomic layer deposition of high-density Pt nanodots on Al2O3 film using (MeCp)Pt(Me)3 and O2 precursors for nonvolatile memory applications

PubMed Central

2013-01-01

Pt nanodots have been grown on Al2O3 film via atomic layer deposition (ALD) using (MeCp)Pt(Me)3 and O2 precursors. Influence of the substrate temperature, pulse time of (MeCp)Pt(Me)3, and deposition cycles on ALD Pt has been studied comprehensively by scanning electron microscopy, transmission electron microscopy, and X-ray photoelectron spectroscopy. Therefore, Pt nanodots with a high density of approximately 2 × 1012 cm-2 have been achieved under optimized conditions: 300°C substrate temperature, 1 s pulse time of (MeCp)Pt(Me)3, and 70 deposition cycles. Further, metal-oxide-semiconductor capacitors with Pt nanodots embedded in ALD Al2O3 dielectric have been fabricated and characterized electrically, indicating noticeable electron trapping capacity, efficient programmable and erasable characteristics, and good charge retention. PMID:23413837

A hydrothermally synthesized LiFePO4/C composite with superior low-temperature performance and cycle life

NASA Astrophysics Data System (ADS)

Wu, Guan; Liu, Na; Gao, Xuguang; Tian, Xiaohui; Zhu, Yanbin; Zhou, Yingke; Zhu, Qingyou

2018-03-01

The LiFePO4/C composites have been successfully synthesized by a hydrothermal process, with the combined carbon sources of fructose and calcium lignosulfonate. The morphology and microstructure of LiFePO4/C were investigated by X-ray diffraction, scanning electron microscopy, transmission electron microscopy and Fourier transform infrared spectroscopy. The electrochemical properties were evaluated by the constant-current charge/discharge tests, cyclic voltammetry and electrochemical impedance spectroscopy. The uniform carbon coating layer derived from calcium lignosulfonate can effectively improve the electronic conductivity, lithium-ion diffusivity and surface stability of the LiFePO4/C composites and prevent the side reactions between the LiFePO4 particles and electrolytes. The LiFePO4/C composites display excellent rate capability, superior cycle life and outstanding low temperature performance, which are promising for lithium-ion battery applications in electrical vehicles and electrical energy storage systems.

Manipulating the Temperature of Sulfurization to Synthesize α-NiS Nanosphere Film for Long-Term Preservation of Non-enzymatic Glucose Sensors.

PubMed

Lin, Hsien-Sheng; Shi, Jen-Bin; Peng, Cheng-Ming; Zheng, Bo-Chi; Cheng, Fu-Chou; Lee, Ming-Way; Lee, Hsuan-Wei; Wu, Po-Feng; Liu, Yi-Jui

2018-04-19

In this study, alpha nickel sulfide (α-NiS) nanosphere films have been successfully synthesized by electroplating the nickel nanosheet film on the indium tin oxide (ITO) glass substrate and sulfuring nickel-coated ITO glass substrate. First, we electrodeposited the nickel nanosheet films on the ITO glass substrates which were cut into a 0.5 × 1 cm 2 size. Second, the nanosheet nickel films were annealed in vacuum-sealed glass ampoules with sulfur sheets at different annealing temperatures (300, 400, and 500 °C) for 4 h in vacuum-sealed glass ampoules. The α-NiS films were investigated by using X-ray diffraction (XRD), variable vacuum scanning electron microscopy (VVSEM), field emission scanning electron microscopy/energy dispersive spectrometer (FE-SEM/EDS), cyclic voltammogram (CV), electrochemical impedance spectroscopy (EIS), ultraviolet/visible/near-infrared (UV/Visible/NIR) spectra, and photoluminescence (PL) spectra. Many nanospheres were observed on the surface of the α-NiS films at the annealing temperature 400 °C for 4 h. We also used the high-resolution transmission electron microscopy (HR-TEM) for the analysis of the α-NiS nanospheres. We demonstrated that our α-NiS nanosphere film had a linear current response to different glucose concentrations. Additionally, our α-NiS nanosphere films were preserved at room temperature for five and a half years and were still useful for detecting glucose at low concentration.

Manipulating the Temperature of Sulfurization to Synthesize α-NiS Nanosphere Film for Long-Term Preservation of Non-enzymatic Glucose Sensors

NASA Astrophysics Data System (ADS)

Lin, Hsien-Sheng; Shi, Jen-Bin; Peng, Cheng-Ming; Zheng, Bo-Chi; Cheng, Fu-Chou; Lee, Ming-Way; Lee, Hsuan-Wei; Wu, Po-Feng; Liu, Yi-Jui

2018-04-01

In this study, alpha nickel sulfide (α-NiS) nanosphere films have been successfully synthesized by electroplating the nickel nanosheet film on the indium tin oxide (ITO) glass substrate and sulfuring nickel-coated ITO glass substrate. First, we electrodeposited the nickel nanosheet films on the ITO glass substrates which were cut into a 0.5 × 1 cm2 size. Second, the nanosheet nickel films were annealed in vacuum-sealed glass ampoules with sulfur sheets at different annealing temperatures (300, 400, and 500 °C) for 4 h in vacuum-sealed glass ampoules. The α-NiS films were investigated by using X-ray diffraction (XRD), variable vacuum scanning electron microscopy (VVSEM), field emission scanning electron microscopy/energy dispersive spectrometer (FE-SEM/EDS), cyclic voltammogram (CV), electrochemical impedance spectroscopy (EIS), ultraviolet/visible/near-infrared (UV/Visible/NIR) spectra, and photoluminescence (PL) spectra. Many nanospheres were observed on the surface of the α-NiS films at the annealing temperature 400 °C for 4 h. We also used the high-resolution transmission electron microscopy (HR-TEM) for the analysis of the α-NiS nanospheres. We demonstrated that our α-NiS nanosphere film had a linear current response to different glucose concentrations. Additionally, our α-NiS nanosphere films were preserved at room temperature for five and a half years and were still useful for detecting glucose at low concentration.

Solvothermal synthesis of hierarchical TiO2 nanostructures with tunable morphology and enhanced photocatalytic activity

NASA Astrophysics Data System (ADS)

Fan, Zhenghua; Meng, Fanming; Zhang, Miao; Wu, Zhenyu; Sun, Zhaoqi; Li, Aixia

2016-01-01

This paper presents controllable growth and photocatalytic activity of TiO2 hierarchical nanostructures by solvothermal method at different temperatures. It is revealed by scanning electron microscopy (SEM) and transmission electron microscopy (TEM) that the morphology of TiO2 can be effectively controlled as rose-like, chrysanthemum-like and sea-urchin-like only changing solvothermal temperature. BET surface area analysis confirms the presence of a mesoporous network in all the nanostructures, and shows high surface area at relatively high temperature. The photocatalytic activities of the photocatalysts are evaluated by the photodegradation of RhB under UV light irradiation. The TiO2 samples exhibit high activity on the photodegradation of RhB, which is higher than that of the commercial P25. The enhancement in photocatalytic performance can be attributed to the synergetic effect of the surface area, crystallinity, band gap and crystalline size.

Preparation of α-Fe2O3 nanotubes via electrospinning and research on their catalytic properties

NASA Astrophysics Data System (ADS)

Shao, Hao; Zhang, Xuebin; Chen, Fanyan; Liu, Shasha; Ji, Yi; Zhu, Yajun; Feng, Yi

2012-09-01

In this paper, smooth α-Fe2O3 nanotubes have been successfully synthesized by electrospinning of ferric nitrate-polyvinyl alcohol solution followed by calcination in air. The morphologies and structures of the samples were characterized by transmission electron microscopy, scanning electron microscopy and X-ray diffraction. The catalytic properties were studied by differential thermal analysis and thermogravimetric analysis. The results indicated that the as-prepared α-Fe2O3 nanotubes showed a continuous morphology and an extremely high degree of crystallization. The average inner and outer diameters of the obtained α-Fe2O3 nanotubes were about 60 nm and 100 nm, respectively. The obtained α-Fe2O3 nanotubes were able to lower the temperature of the high-temperature thermal decomposition of ammonium perchlorate, while they had little effect on the crystallographic phase transformation and the low-temperature thermal decomposition.

P-type sub-tungsten-oxide based urchin-like nanostructure for superior room temperature alcohol sensor

NASA Astrophysics Data System (ADS)

Yao, Yao; Yin, Mingli; Yan, Junqing; Liu, Shengzhong (Frank)

2018-05-01

Nanowires assembled sub-WO3 urchin-like nanostructures have been fabricated via a solvothermal method. The detailed structure and morphology features were characterized by X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM). The results reveal that the individual nanowires are grown along the [0 0 1] direction, and assembled together to form an urchin-like nanostructure. Sensing performance of the sub-WO3 was investigated toward alcohol vapor. At room temperature, the sensor devices based on the WO3-x exhibit significantly higher sensitivity comparing to that of the stoichiometric WO3. The superior sensing performance of this WO3-x sensor is ascribed to the large specific surface area and abundant oxygen vacancies. The obvious enhancement of the gas sensing property can be very useful for the future design and development of room temperature gas sensors for other volatile organic compounds.

CTAB assisted synthesis of tungsten oxide nanoplates as an efficient low temperature NOX sensor

NASA Astrophysics Data System (ADS)

Mehta, Swati S.; Tamboli, Mohaseen S.; Mulla, Imtiaz S.; Suryavanshi, Sharad S.

2018-02-01

Tungsten oxide nanoplates with porous morphology were effectively prepared by acidification using CTAB (HexadeCetyltrimethyl ammonium bromide) as a surfactant. For characterization, the synthesized materials were subjected to X-Ray powder diffraction (XRD), scanning electron microscopy (SEM), high resolution transmission electron microscopy (HRTEM), UV-Visible spectroscopy (UV-Vis) and surface area (BET) measurements. The morphology and size of the particles were controlled by solution acidity. The BET results confirmed that the materials are well crystallized and mesoporous in nature. The nanocrystalline powder was used to prepare thick films by screen printing on alumina substrate for the investigation of gas sensing properties. The gas response measurements revealed that the samples acidified using 10 M H2SO4 exhibits highest response of 91% towards NOX at optimum temperature of 200 °C for 100 ppm, and it also exhibits 35% response at room temperature.

Production of fullerenes and single-wall carbon nanotubes by high-temperature pulsed arc discharge

NASA Astrophysics Data System (ADS)

Sugai, Toshiki; Omote, Hideki; Bandow, Shunji; Tanaka, Nobuo; Shinohara, Hisanori

2000-04-01

Fullerenes and single-wall carbon nanotubes (SWNTs) have been produced for the first time by the high-temperature pulsed arc-discharge technique, which has developed in this laboratory. Fullerenes are identified quantitatively by high-performance liquid chromatography (HPLC), and scanning electron microscopy (SEM) and transmission electron microscopy (TEM) observations reveal a significant amount of production of bundles of SWNTs in soot. The pulse arc production of fullerenes and SWNTs favors the high-temperature (⩾1000 °C), long pulses (⩾1 ms) and a heavy rare gas such as Ar or Kr as a buffer gas. We have found that fullerenes and SWNTs have complementary relationships in their early stage of production. The details of the pulsed arc discharge have been obtained by observing the transition from the pulsed arc discharge to the steady arc discharge while increasing the pulse width.

Electron microscopy observation of TiO2 nanocrystal evolution in high-temperature atomic layer deposition.

PubMed

Shi, Jian; Li, Zhaodong; Kvit, Alexander; Krylyuk, Sergiy; Davydov, Albert V; Wang, Xudong

2013-01-01

Understanding the evolution of amorphous and crystalline phases during atomic layer deposition (ALD) is essential for creating high quality dielectrics, multifunctional films/coatings, and predictable surface functionalization. Through comprehensive atomistic electron microscopy study of ALD TiO2 nanostructures at designed growth cycles, we revealed the transformation process and sequence of atom arrangement during TiO2 ALD growth. Evolution of TiO2 nanostructures in ALD was found following a path from amorphous layers to amorphous particles to metastable crystallites and ultimately to stable crystalline forms. Such a phase evolution is a manifestation of the Ostwald-Lussac Law, which governs the advent sequence and amount ratio of different phases in high-temperature TiO2 ALD nanostructures. The amorphous-crystalline mixture also enables a unique anisotropic crystal growth behavior at high temperature forming TiO2 nanorods via the principle of vapor-phase oriented attachment.

Electron microscopy study of Ni induced crystallization in amorphous Si thin films

DOE Office of Scientific and Technical Information (OSTI.GOV)

Radnóczi, G. Z.; Battistig, G.; Pécz, B., E-mail: pecz.bela@ttk.mta.hu

2015-02-17

The crystallization of amorphous silicon is studied by transmission electron microscopy. The effect of Ni on the crystallization is studied in a wide temperature range heating thinned samples in-situ inside the microscope. Two cases of limited Ni source and unlimited Ni source are studied and compared. NiSi{sub 2} phase started to form at a temperature as low as 250°C in the limited Ni source case. In-situ observation gives a clear view on the crystallization of silicon through small NiSi{sub 2} grain formation. The same phase is observed at the crystallization front in the unlimited Ni source case, where a secondmore » region is also observed with large grains of Ni{sub 3}Si{sub 2}. Low temperature experiments show, that long annealing of amorphous silicon at 410 °C already results in large crystallized Si regions due to the Ni induced crystallization.« less

Spatially Resolved Nano-Scale Characterization of Electronic States in SrTiO3(001) Surfaces by STM/STS

NASA Astrophysics Data System (ADS)

Iwaya, Katsuya; Ohsawa, Takeo; Shimizu, Ryota; Hashizume, Tomihiro; Hitosugi, Taro

2012-02-01

We have performed low temperature scanning tunneling microscopy/spectroscopy (STM/STS) measurements on TiO2-terminated SrTiO3(001) thin film surfaces. The conductance map exhibited electronic modulations that were completely different from the surface structure. We also found that the electronic modulations were strongly dependent on temperature and the density of atomic defects associated with oxygen vacancies. These results suggest the existence of strongly correlated two-dimensional electronic states near the SrTiO3 surface, implying the importance of electron correlation at the interfaces of SrTiO3-related heterostructures.

Evolution of Metastable Defects and Its Effect on the Electronic Properties of MoS2 Films.

PubMed

Precner, M; Polaković, T; Qiao, Qiao; Trainer, D J; Putilov, A V; Di Giorgio, C; Cone, I; Zhu, Y; Xi, X X; Iavarone, M; Karapetrov, G

2018-04-30

We report on structural and electronic properties of defects in chemical vapor-deposited monolayer and few-layer MoS 2 films. Scanning tunneling microscopy, Kelvin probe force microscopy, and transmission electron microscopy were used to obtain high resolution images and quantitative measurements of the local density of states, work function and nature of defects in MoS 2 films. We track the evolution of defects that are formed under heating and electron beam irradiation. We observe formation of metastable domains with different work function values after annealing the material in ultra-high vacuum to moderate temperatures. We attribute these metastable values of the work function to evolution of crystal defects forming during the annealing. The experiments show that sulfur vacancies formed after exposure to elevated temperatures diffuse, coalesce, and migrate bringing the system from a metastable to equilibrium ground state. The process could be thermally or e-beam activated with estimated energy barrier for sulfur vacancy migration of 0.6 eV in single unit cell MoS 2 . Even at equilibrium conditions, the work function and local density of states values are strongly affected near grain boundaries and edges. The results provide initial estimates of the thermal budgets available for reliable fabrication of MoS 2 -based integrated electronics and indicate the importance of defect control and layer passivation.

Evolution of Metastable Defects and Its Effect on the Electronic Properties of MoS 2 Films

DOE PAGES

Precner, Marian; Polakovic, T.; Qiao, Qiao; ...

2018-04-30

Here, we report on structural and electronic properties of defects in chemical vapor-deposited monolayer and few-layer MoS 2 films. Scanning tunneling microscopy, Kelvin probe force microscopy, and transmission electron microscopy were used to obtain high resolution images and quantitative measurements of the local density of states, work function and nature of defects in MoS 2 films. We track the evolution of defects that are formed under heating and electron beam irradiation. We observe formation of metastable domains with different work function values after annealing the material in ultra-high vacuum to moderate temperatures. We attribute these metastable values of the workmore » function to evolution of crystal defects forming during the annealing. The experiments show that sulfur vacancies formed after exposure to elevated temperatures diffuse, coalesce, and migrate bringing the system from a metastable to equilibrium ground state. The process could be thermally or e-beam activated with estimated energy barrier for sulfur vacancy migration of 0.6 eV in single unit cell MoS 2. Even at equilibrium conditions, the work function and local density of states values are strongly affected near grain boundaries and edges. The results provide initial estimates of the thermal budgets available for reliable fabrication of MoS 2-based integrated electronics and indicate the importance of defect control and layer passivation.« less

Evolution of Metastable Defects and Its Effect on the Electronic Properties of MoS 2 Films

DOE Office of Scientific and Technical Information (OSTI.GOV)

Precner, Marian; Polakovic, T.; Qiao, Qiao

Here, we report on structural and electronic properties of defects in chemical vapor-deposited monolayer and few-layer MoS 2 films. Scanning tunneling microscopy, Kelvin probe force microscopy, and transmission electron microscopy were used to obtain high resolution images and quantitative measurements of the local density of states, work function and nature of defects in MoS 2 films. We track the evolution of defects that are formed under heating and electron beam irradiation. We observe formation of metastable domains with different work function values after annealing the material in ultra-high vacuum to moderate temperatures. We attribute these metastable values of the workmore » function to evolution of crystal defects forming during the annealing. The experiments show that sulfur vacancies formed after exposure to elevated temperatures diffuse, coalesce, and migrate bringing the system from a metastable to equilibrium ground state. The process could be thermally or e-beam activated with estimated energy barrier for sulfur vacancy migration of 0.6 eV in single unit cell MoS 2. Even at equilibrium conditions, the work function and local density of states values are strongly affected near grain boundaries and edges. The results provide initial estimates of the thermal budgets available for reliable fabrication of MoS 2-based integrated electronics and indicate the importance of defect control and layer passivation.« less

Effect of Annealing Temperature on Microstructure and Mechanical Properties of Hot-Dip Galvanizing DP600 Steel

NASA Astrophysics Data System (ADS)

Hai-yan, Sun; Zhi-li, Liu; Yang, Xu; Jian-qiang, Shi; Lian-xuan, Wang

Hot-dip galvanizing dual phase steel DP600 steel grade with low Si was produced by steel plant and experiments by simulating galvanizing thermal history. The microstructure was observed and analyzed by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The effect of different annealing temperatures on the microstructure and mechanical properties of dual-phase steel was also discussed. The experimental results show that the dual-phase steel possesses excellent strength and elongation that match EN10346 600MPa standards. The microstructure is ferrite and martensite. TEM micrograph shows that white ferrite with black martensite islands inlay with a diameter of around 1um and the content of 14 18%. The volume will expand and phase changing take the form of shear transformation when ferrite converted to martensite. So there are high density dislocations in ferrite crystalline grain near martensite. The martensite content growing will be obvious along with annealing temperature going up. But the tendency will be weak when temperature high.

Avoiding artefacts during electron microscopy of silver nanomaterials exposed to biological environments

PubMed Central

Goode, Angela E.; Skepper, Jeremy N.; Thorley, Andrew J.; Seiffert, Joanna M.; Chung, K. Fan; Tetley, Teresa D.; Shaffer, Milo S. P.; Ryan, Mary P.

2015-01-01

Electron microscopy has been applied widely to study the interaction of nanomaterials with proteins, cells and tissues at nanometre scale. Biological material is most commonly embedded in thermoset resins to make it compatible with the high vacuum in the electron microscope. Room temperature sample preparation protocols developed over decades provide contrast by staining cell organelles, and aim to preserve the native cell structure. However, the effect of these complex protocols on the nanomaterials in the system is seldom considered. Any artefacts generated during sample preparation may ultimately interfere with the accurate prediction of the stability and reactivity of the nanomaterials. As a case study, we review steps in the room temperature preparation of cells exposed to silver nanomaterials (AgNMs) for transmission electron microscopy imaging and analysis. In particular, embedding and staining protocols, which can alter the physicochemical properties of AgNMs and introduce artefacts thereby leading to a misinterpretation of silver bioreactivity, are scrutinised. Recommendations are given for the application of cryogenic sample preparation protocols, which simultaneously fix both particles and diffusible ions. By being aware of the advantages and limitations of different sample preparation methods, compromises or selection of different correlative techniques can be made to draw more accurate conclusions about the data. PMID:25606708

Porous Si nanowires for highly selective room-temperature NO2 gas sensing

NASA Astrophysics Data System (ADS)

Kwon, Yong Jung; Mirzaei, Ali; Gil Na, Han; Kang, Sung Yong; Choi, Myung Sik; Bang, Jae Hoon; Oum, Wansik; Kim, Sang Sub; Kim, Hyoun Woo

2018-07-01

We report the room-temperature sensing characteristics of Si nanowires (NWs) fabricated from p-Si wafers by a metal-assisted chemical etching method, which is a facile and low-cost method. X-ray diffraction was used to the the study crystallinity and phase formation of Si NWs, and product morphology was examined using scanning electron microscopy (SEM) and transmission electron microscopy (TEM). After confirmation of Si NW formation via the SEM and TEM micrographs, sensing tests were carried out at room temperature, and it was found that the Si NW sensor prepared from Si wafers with a resistivity of 0.001–0.003 Ω.cm had the highest response to NO2 gas (Rg/Ra = 1.86 for 50 ppm NO2), with a fast response (15 s) and recovery (30 s) time. Furthermore, the sensor responses to SO2, toluene, benzene, H2, and ethanol were nearly negligible, demonstrating the excellent selectivity to NO2 gas. The gas-sensing mechanism is discussed in detail. The present sensor can operate at room temperature, and is compatible with the microelectronic fabrication process, demonstrating its promise for next-generation Si-based electronics fused with functional chemical sensors.

Porous Si nanowires for highly selective room-temperature NO2 gas sensing.

PubMed

Kwon, Yong Jung; Mirzaei, Ali; Na, Han Gil; Kang, Sung Yong; Choi, Myung Sik; Bang, Jae Hoon; Oum, Wansik; Kim, Sang Sub; Kim, Hyoun Woo

2018-07-20

We report the room-temperature sensing characteristics of Si nanowires (NWs) fabricated from p-Si wafers by a metal-assisted chemical etching method, which is a facile and low-cost method. X-ray diffraction was used to the the study crystallinity and phase formation of Si NWs, and product morphology was examined using scanning electron microscopy (SEM) and transmission electron microscopy (TEM). After confirmation of Si NW formation via the SEM and TEM micrographs, sensing tests were carried out at room temperature, and it was found that the Si NW sensor prepared from Si wafers with a resistivity of 0.001-0.003 Ω.cm had the highest response to NO 2 gas (R g /R a  = 1.86 for 50 ppm NO 2 ), with a fast response (15 s) and recovery (30 s) time. Furthermore, the sensor responses to SO 2 , toluene, benzene, H 2 , and ethanol were nearly negligible, demonstrating the excellent selectivity to NO 2 gas. The gas-sensing mechanism is discussed in detail. The present sensor can operate at room temperature, and is compatible with the microelectronic fabrication process, demonstrating its promise for next-generation Si-based electronics fused with functional chemical sensors.

Nature and evolution of incommensurate charge order in manganites visualized with cryogenic scanning transmission electron microscopy

PubMed Central

Savitzky, Benjamin H.; Admasu, Alemayehu S.; Kim, Jaewook; Cheong, Sang-Wook; Hovden, Robert; Kourkoutis, Lena F.

2018-01-01

Incommensurate charge order in hole-doped oxides is intertwined with exotic phenomena such as colossal magnetoresistance, high-temperature superconductivity, and electronic nematicity. Here, we map, at atomic resolution, the nature of incommensurate charge–lattice order in a manganite using scanning transmission electron microscopy at room temperature and cryogenic temperature (∼93 K). In diffraction, the ordering wave vector changes upon cooling, a behavior typically associated with incommensurate order. However, using real space measurements, we discover that the ordered state forms lattice-locked regions over a few wavelengths interspersed with phase defects and changing periodicity. The cations undergo picometer-scale (∼6 pm to 11 pm) transverse displacements, suggesting that charge–lattice coupling is strong. We further unearth phase inhomogeneity in the periodic lattice displacements at room temperature, and emergent phase coherence at 93 K. Such local phase variations govern the long-range correlations of the charge-ordered state and locally change the periodicity of the modulations, resulting in wave vector shifts in reciprocal space. These atomically resolved observations underscore the importance of lattice coupling and phase inhomogeneity, and provide a microscopic explanation for putative “incommensurate” order in hole-doped oxides. PMID:29382750

Ultrafast core-loss spectroscopy in four-dimensional electron microscopy

PubMed Central

van der Veen, Renske M.; Penfold, Thomas J.; Zewail, Ahmed H.

2015-01-01

We demonstrate ultrafast core-electron energy-loss spectroscopy in four-dimensional electron microscopy as an element-specific probe of nanoscale dynamics. We apply it to the study of photoexcited graphite with femtosecond and nanosecond resolutions. The transient core-loss spectra, in combination with ab initio molecular dynamics simulations, reveal the elongation of the carbon-carbon bonds, even though the overall behavior is a contraction of the crystal lattice. A prompt energy-gap shrinkage is observed on the picosecond time scale, which is caused by local bond length elongation and the direct renormalization of band energies due to temperature-dependent electron–phonon interactions. PMID:26798793

A hot tip: imaging phenomena using in situ multi-stimulus probes at high temperatures

NASA Astrophysics Data System (ADS)

Nonnenmann, Stephen S.

2016-02-01

Accurate high temperature characterization of materials remains a critical challenge to the continued advancement of various important energy, nuclear, electronic, and aerospace applications. Future experimental studies must assist these communities to progress past empiricism and derive deliberate, predictable designs of material classes functioning within active, extreme environments. Successful realization of systems ranging from fuel cells and batteries to electromechanical nanogenerators and turbines requires a dynamic understanding of the excitation, surface-mediated, and charge transfer phenomena which occur at heterophase interfaces (i.e. vapor-solid, liquid-solid, solid-solid) and impact overall performance. Advancing these frontiers therefore necessitates in situ (operando) characterization methods capable of resolving, both spatially and functionally, the coherence between these complex, collective excitations, and their respective response dynamics, through studies within the operating regime. This review highlights recent developments in scanning probe microscopy in performing in situ imaging at high elevated temperatures. The influence of and evolution from vacuum-based electron and tunneling microscopy are briefly summarized and discussed. The scope includes the use of high temperature imaging to directly observe critical phase transition, electronic, and electrochemical behavior under dynamic temperature settings, thus providing key physical parameters. Finally, both challenges and directions in combined instrumentation are proposed and discussed towards the end.

New findings on tarsonemid mites (Prostigmata: Tarsonemidae) under the LT-SEM (Low Temperature Scanning Electron Microscopy) – The case of genera Daidalotarsonemus and Excelsotarsonemus

USDA-ARS?s Scientific Manuscript database

Daidalotarsonemus De Leon and Excelsotarsonemus Ochoa & Naskrecki are tarsonemids considered to be plant inhabiting genera. Both present complex structured bodies which are very difficult to be interpreted by traditional light microscopy techniques. Due to this most of the papers published have pres...

Cardiac Mitochondria l Membrane Stability after Deep Hypothermia using a Xenon Clathrate Cryostasis Protocol – an Electron Microscopy Study

PubMed Central

Sheleg, Sergey; Hixon, Hugh; Cohen, Bruce; Lowry, David; Nedzved, Mikhail

2008-01-01

We investigated a new cryopreservation method using xenon, a clathrate-forming gas, under medium pressure (100psi). The objective of the study was to determine whether this cryostasis protocol could protect cardiac mitochondria at cryogenic temperatures (below 100 degrees Celsius).We analyzed transmission electron microscopy images to obtain information about changes in mitochondrial morphology induced by cryopreservation of the hearts. Our data showed absence of mitochondrial swelling, rupture of inner and outer membranes, and leakage of mitochondrial matrix into the cytoplasm after applying this cryostasis protocol. The electron microscopy results provided the first evidence that a cryostasis protocol using xenon as a clathrate-forming gas under pressure may have protective effects on intracellular membranes. This cryostasis technology may find applications in developing new approaches for long-term cryopreservation protocols. PMID:18787624

Green synthesis of soya bean sprouts-mediated superparamagnetic Fe 3O 4 nanoparticles

NASA Astrophysics Data System (ADS)

Cai, Yan; Shen, Yuhua; Xie, Anjian; Li, Shikuo; Wang, Xiufang

2010-10-01

Superparamagnetic Fe 3O 4 nanoparticles were first synthesized via soya bean sprouts (SBS) templates under ambient temperature and normal atmosphere. The reaction process was simple, eco-friendly, and convenient to handle. The morphology and crystalline phase of the nanoparticles were determined from scanning electron microscopy (SEM), transmission electron microscopy (TEM), selected area electron diffraction (SAED), and X-ray diffraction (XRD) spectra. The effect of SBS template on the formation of Fe 3O 4 nanoparticles was investigated using X-ray photoemission spectroscopy (XPS) and Fourier-transform infrared spectroscopy (FT-IR). The results indicate that spherical Fe 3O 4 nanoparticles with an average diameter of 8 nm simultaneously formed on the epidermal surface and the interior stem wall of SBS. The SBS are responsible for size and morphology control during the whole formation of Fe 3O 4 nanoparticles. In addition, the superconducting quantum interference device (SQUID) results indicate the products are superparamagnetic at room temperature, with blocking temperature ( TB) of 150 K and saturation magnetization of 37.1 emu/g.

Microstructural Evolution of Secondary Phases in the Cast Duplex Stainless Steels CD3MN and CD3MWCuN

NASA Astrophysics Data System (ADS)

Kim, Yoon-Jun; Ugurlu, Ozan; Jiang, Chao; Gleeson, Brian; Chumbley, L. Scott

2007-02-01

The isothermal formation behavior of secondary phases in two types of duplex stainless steels (DSS), CD3MN and CD3MWCuN, was characterized. Samples were heat treated from 1 minute to 30 days at temperatures from 700°C to 900°C. Small carbide (M23C6) and nitride (Cr2N) precipitates, together with the intermetallic phases sigma and chi, were observed using scanning electron microscopy (SEM) and confirmed by transmission electron microscopy (TEM) analyses. Based on SEM analysis, time-temperature-transformation (TTT) curves for the sigma and chi phases were determined by measuring their volume fractions from backscattered electron micrographs of heat-treated and quenched sample cross sections. Resulting TTT curves showed that the maximum formation temperature for chi is lower than that for sigma, while the time to reach 1 vol pct formation is much less for sigma than it is for chi. The thermodynamic driving forces associated with the sigma and chi formation were assessed using Thermo-Calc.

Scalable high-mobility MoS2 thin films fabricated by an atmospheric pressure chemical vapor deposition process at ambient temperature

NASA Astrophysics Data System (ADS)

Huang, Chung-Che; Al-Saab, Feras; Wang, Yudong; Ou, Jun-Yu; Walker, John C.; Wang, Shuncai; Gholipour, Behrad; Simpson, Robert E.; Hewak, Daniel W.

2014-10-01

Nano-scale MoS2 thin films are successfully deposited on a variety of substrates by atmospheric pressure chemical vapor deposition (APCVD) at ambient temperature, followed by a two-step annealing process. These annealed MoS2 thin films are characterized with scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), micro-Raman, X-ray diffraction (XRD), transmission electron microscopy (TEM), UV-VIS-NIR spectrometry, photoluminescence (PL) and Hall Effect measurement. Key optical and electronic properties of APCVD grown MoS2 thin films are determined. This APCVD process is scalable and can be easily incorporated with conventional lithography as the deposition is taking place at room temperature. We also find that the substrate material plays a significant role in the crystalline structure formation during the annealing process and single crystalline MoS2 thin films can be achieved by using both c-plane ZnO and c-plane sapphire substrates. These APCVD grown nano-scale MoS2 thin films show great promise for nanoelectronic and optoelectronic applications.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mehlhorn, Michael; Morgenstern, Karina, E-mail: karina.morgenstern@rub.de

We compare the adsorption of oxygen molecules on Ag(100) at 60 K and at 100 K. At both temperatures, the molecules form islands. Differences between the species adsorbed at the two temperatures in both low-temperature scanning tunneling microscopy and inelastic electron tunneling spectroscopy are attributed to two different adsorption states, a chemisorbed state after 100 K adsorption and a physisorbed state after 60 K adsorption.

Investigation of Preparation and Mechanisms of a Dispersed Particle Gel Formed from a Polymer Gel at Room Temperature

PubMed Central

Zhao, Guang; Dai, Caili; Zhao, Mingwei; You, Qing; Chen, Ang

2013-01-01

A dispersed particle gel (DPG) was successfully prepared from a polymer gel at room temperature. The polymer gel system, morphology, viscosity changes, size distribution, and zeta potential of DPG particles were investigated. The results showed that zirconium gel systems with different strengths can be cross-linked within 2.5 h at low temperature. Scanning electron microscopy (SEM), transmission electron microscopy (TEM), and atomic force microscopy (AFM) results showed that the particles were polygonal particles with nano-size distribution. According to the viscosity changes, the whole preparation process can be divided into two major stages: the bulk gel cross-linking reaction period and the DPG particle preparation period. A polymer gel with a 3-dimensional network was formed in the bulk gel cross-linking reaction period whereas shearing force and frictional force were the main driving forces for the preparation of DPG particles, and thus affected the morphology of DPG particles. High shearing force and frictional force reduced the particle size distribution, and then decreased the zeta potential (absolute value). The whole preparation process could be completed within 3 h at room temperature. It could be an efficient and energy-saving technology for preparation of DPG particles. PMID:24324817

[Scanning electron microscopy of heat-damaged bone tissue].

PubMed

Harsanyl, L

1977-02-01

Parts of diaphyses of bones were exposed to high temperature of 200-1300 degrees C. Damage to the bone tissue caused by the heat was investigated. The scanning electron microscopic picture seems to be characteristic of the temperature applied. When the bones heated to the high temperature of 700 degrees C characteristic changes appear on the periostal surface, higher temperatura on the other hand causes damage to the compact bone tissue and can be observed on the fracture-surface. Author stresses the importance of this technique in the legal medicine and anthropology.

Formation and mechanism of nanocrystalline AZ91 powders during HDDR processing

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liu, Yafen; Fan, Jianfeng, E-mail: fanjianfeng@tyu

2017-03-15

Grain sizes of AZ91 alloy powders were markedly refined to about 15 nm from 100 to 160 μm by an optimized hydrogenation-disproportionation-desorption-recombination (HDDR) process. The effect of temperature, hydrogen pressure and processing time on phase and microstructure evolution of AZ91 alloy powders during HDDR process was investigated systematically by X-ray diffraction, optical microscopy, scanning electron microscopy and transmission electron microscopy, respectively. The optimal HDDR process for preparing nanocrystalline Mg alloy powders is hydriding at temperature of 350 °C under 4 MPa hydrogen pressure for 12 h and dehydriding at 350 °C for 3 h in vacuum. A modified unreacted coremore » model was introduced to describe the mechanism of grain refinement of during HDDR process. - Highlights: • Grain size of the AZ91 alloy powders was significantly refined from 100 μm to 15 nm. • The optimal HDDR technology for nano Mg alloy powders is obtained. • A modified unreacted core model of grain refinement mechanism was proposed.« less

Evolution of microstructure of Haynes 230 and Inconel 617 under mechanical testing at high temperatures

NASA Astrophysics Data System (ADS)

Hrutkay, Kyle

Haynes 230 and Inconel 617 are austenitic nickel based superalloys, which are candidate structural materials for next generation high temperature nuclear reactors. High temperature deformation behavior of Haynes 230 and Inconel 617 have been investigated at the microstructural level in order to gain a better understanding of mechanical properties. Tensile tests were performed at strain rates ranging from 10-3-10-5 s -1 at room temperature, 600 °C, 800 °C and 950 °C. Subsequent microstructural analysis, including Scanning Electron Microscopy, Transmission Electron Microscopy, Energy-Dispersive X-ray Spectroscopy, and X-Ray Diffraction were used to relate the microstructural evolution at high temperatures to that of room temperature samples. Grain sizes and precipitate morphologies were used to determine high temperature behavior and fracture mechanics. Serrated flow was observed at intermediate and high temperatures as a result of discontinuous slip and dynamic recrystallization. The amplitude of serration increased with a decrease in the strain rate and increase in the temperature. Dynamic strain ageing was responsible for serrations at intermediate temperatures by means of a locking and unlocking phenomenon between dislocations and solute atoms. Dynamic recrystallization nucleated by grain and twin bulging resulting in a refinement of grain size. Existing models found in the literature were discussed to explain both of these phenomena.

Facile synthesis of graphene on dielectric surfaces using a two-temperature reactor CVD system

NASA Astrophysics Data System (ADS)

Zhang, C.; Man, B. Y.; Yang, C.; Jiang, S. Z.; Liu, M.; Chen, C. S.; Xu, S. C.; Sun, Z. C.; Gao, X. G.; Chen, X. J.

2013-10-01

Direct deposition of graphene on a dielectric substrate is demonstrated using a chemical vapor deposition system with a two-temperature reactor. The two-temperature reactor is utilized to offer sufficient, well-proportioned floating Cu atoms and to provide a temperature gradient for facile synthesis of graphene on dielectric surfaces. The evaporated Cu atoms catalyze the reaction in the presented method. C atoms and Cu atoms respectively act as the nuclei for forming graphene film in the low-temperature zone and the zones close to the high-temperature zones. A uniform and high-quality graphene film is formed in an atmosphere of sufficient and well-proportioned floating Cu atoms. Raman spectroscopy, scanning electron microscopy and atomic force microscopy confirm the presence of uniform and high-quality graphene.

Electron emission from diamond films seeded using kitchen-wrap polyethylene

NASA Astrophysics Data System (ADS)

Varshney, D.; Makarov, V. I.; Saxena, P.; Guinel, M. J. F.; Kumar, A.; Scott, J. F.; Weiner, B. R.; Morell, G.

2011-03-01

Diamond has many potential electronic applications, but the diamond seeding methods are generally harsh on the substrates rendering them unsuitable for integration in electronics. We report a non-abrasive, scalable and economic process of diamond film seeding using kitchen-wrap polyethylene employing hot filament chemical vapour reaction of H2S/CH4/H2 gas mixtures on Cu substrates. The fabricated diamond films were characterized with scanning electron microscopy, transmission electron microscopy and Raman spectroscopy, which confirm that the deposited film consists of a microcrystalline diamond of size in the range 0.5-1.0 µm. The synthesized diamond films exhibit a turn-on field of about 8.5 V µm-1 and long-term stability. Diamond film synthesis using polyethylene will enable the integration of diamond heat sinks into high-power and high-temperature electronic devices.

Ab initio structure determination of nanocrystals of organic pharmaceutical compounds by electron diffraction at room temperature using a Timepix quantum area direct electron detector

PubMed Central

van Genderen, E.; Clabbers, M. T. B.; Das, P. P.; Stewart, A.; Nederlof, I.; Barentsen, K. C.; Portillo, Q.; Pannu, N. S.; Nicolopoulos, S.; Gruene, T.; Abrahams, J. P.

2016-01-01

Until recently, structure determination by transmission electron microscopy of beam-sensitive three-dimensional nanocrystals required electron diffraction tomography data collection at liquid-nitrogen temperature, in order to reduce radiation damage. Here it is shown that the novel Timepix detector combines a high dynamic range with a very high signal-to-noise ratio and single-electron sensitivity, enabling ab initio phasing of beam-sensitive organic compounds. Low-dose electron diffraction data (∼0.013 e− Å−2 s−1) were collected at room temperature with the rotation method. It was ascertained that the data were of sufficient quality for structure solution using direct methods using software developed for X-ray crystallography (XDS, SHELX) and for electron crystallography (ADT3D/PETS, SIR2014). PMID:26919375

Conduction at domain walls in oxide multiferroics

NASA Astrophysics Data System (ADS)

Seidel, J.; Martin, L. W.; He, Q.; Zhan, Q.; Chu, Y.-H.; Rother, A.; Hawkridge, M. E.; Maksymovych, P.; Yu, P.; Gajek, M.; Balke, N.; Kalinin, S. V.; Gemming, S.; Wang, F.; Catalan, G.; Scott, J. F.; Spaldin, N. A.; Orenstein, J.; Ramesh, R.

2009-03-01

Domain walls may play an important role in future electronic devices, given their small size as well as the fact that their location can be controlled. Here, we report the observation of room-temperature electronic conductivity at ferroelectric domain walls in the insulating multiferroic BiFeO3. The origin and nature of the observed conductivity are probed using a combination of conductive atomic force microscopy, high-resolution transmission electron microscopy and first-principles density functional computations. Our analyses indicate that the conductivity correlates with structurally driven changes in both the electrostatic potential and the local electronic structure, which shows a decrease in the bandgap at the domain wall. Additionally, we demonstrate the potential for device applications of such conducting nanoscale features.

Conduction at domain walls in oxide multiferroics.

PubMed

Seidel, J; Martin, L W; He, Q; Zhan, Q; Chu, Y-H; Rother, A; Hawkridge, M E; Maksymovych, P; Yu, P; Gajek, M; Balke, N; Kalinin, S V; Gemming, S; Wang, F; Catalan, G; Scott, J F; Spaldin, N A; Orenstein, J; Ramesh, R

2009-03-01

Domain walls may play an important role in future electronic devices, given their small size as well as the fact that their location can be controlled. Here, we report the observation of room-temperature electronic conductivity at ferroelectric domain walls in the insulating multiferroic BiFeO(3). The origin and nature of the observed conductivity are probed using a combination of conductive atomic force microscopy, high-resolution transmission electron microscopy and first-principles density functional computations. Our analyses indicate that the conductivity correlates with structurally driven changes in both the electrostatic potential and the local electronic structure, which shows a decrease in the bandgap at the domain wall. Additionally, we demonstrate the potential for device applications of such conducting nanoscale features.

Differences in Physical and Biochemical Properties of Thermus scotoductus SA-01 Cultured with Dielectric or Convection Heating.

PubMed

Cockrell, Allison L; Fitzgerald, Lisa A; Cusick, Kathleen D; Barlow, Daniel E; Tsoi, Stanislav D; Soto, Carissa M; Baldwin, Jeffrey W; Dale, Jason R; Morris, Robert E; Little, Brenda J; Biffinger, Justin C

2015-09-01

A thermophile, Thermus scotoductus SA-01, was cultured within a constant-temperature (65°C) microwave (MW) digester to determine if MW-specific effects influenced the growth and physiology of the organism. As a control, T. scotoductus cells were also cultured using convection heating at the same temperature as the MW studies. Cell growth was analyzed by optical density (OD) measurements, and cell morphologies were characterized using electron microscopy imaging (scanning electron microscopy [SEM] and transmission electron microscopy [TEM]), dynamic light scattering (DLS), and atomic force microscopy (AFM). Biophysical properties (i.e., turgor pressure) were also calculated with AFM, and biochemical compositions (i.e., proteins, nucleic acids, fatty acids) were analyzed by attenuated total reflectance-Fourier transform infrared (ATR-FTIR) spectroscopy. Gas chromatography-mass spectrometry (GC-MS) was used to analyze the fatty acid methyl esters extracted from cell membranes. Here we report successful cultivation of a thermophile with only dielectric heating. Under the MW conditions for growth, cell walls remained intact and there were no indications of membrane damage or cell leakage. Results from these studies also demonstrated that T. scotoductus cells grown with MW heating exhibited accelerated growth rates in addition to altered cell morphologies and biochemical compositions compared with oven-grown cells. Copyright © 2015, American Society for Microbiology. All Rights Reserved.

Atomistic structures of nano-engineered SiC and radiation-induced amorphization resistance

DOE PAGES

Imada, Kenta; Ishimaru, Manabu; Sato, Kazuhisa; ...

2015-06-18

In this paper, nano-engineered 3C–SiC thin films, which possess columnar structures with high-density stacking faults and twins, were irradiated with 2 MeV Si ions at cryogenic and room temperatures. From cross-sectional transmission electron microscopy observations in combination with Monte Carlo simulations based on the Stopping and Range of Ions in Matter code, it was found that their amorphization resistance is six times greater than bulk crystalline SiC at room temperature. High-angle bright-field images taken by spherical aberration corrected scanning transmission electron microscopy revealed that the distortion of atomic configurations is localized near the stacking faults. Finally, the resultant strain fieldmore » probably contributes to the enhancement of radiation tolerance of this material.« less

Improvement of critical current density in thallium-based (Tl,Bi)Sr(1.6)Ba(0.4)Ca2Cu3O(x) superconductors

NASA Technical Reports Server (NTRS)

Ren, Z. F.; Wang, C. A.; Wang, J. H.; Miller, D. J.; Goretta, K. C.

1995-01-01

Epitaxial (Tl,Bi)Sr(1.6)Ba(0.4)Ca2Cu3O(x) ((Tl,Bi)-1223) thin films on (100) single crystal LaAlO3 substrates were synthesized by a two-step procedure. Phase development, microstructure, and relationships between film and substrate were studied by X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). Resistance versus temperature, zero-field-cooled and field cooled magnetization, and transport critical current density (J(sub c)) were measured. The zero-resistance temperature was 105-111 K. J(sub c) at 77 K and zero field was greater than 2 x 10(exp 6) A/sq cm. The films exhibited good flux pinning properties.

Low-temperature scanning tunneling microscopy of ring-like surface electronic structures around Co islands on InAs(110) surfaces.

PubMed

Muzychenko, D A; Schouteden, K; Savinov, S V; Maslova, N S; Panov, V I; Van Haesendonck, C

2009-08-01

We report on the experimental observation by scanning tunneling microscopy at low temperature of ring-like features that appear around Co metal islands deposited on a clean (110) oriented surface of cleaved p-type InAs crystals. These features are visible in spectroscopic images within a certain range of negative tunneling bias voltages due to the presence of a negative differential conductance in the current-voltage dependence. A theoretical model is introduced, which takes into account non-equilibrium effects in the small tunneling junction area. In the framework of this model the appearance of the ring-like features is explained in terms of interference effects between electrons tunneling directly and indirectly (via a Co island) between the tip and the InAs surface.

Crystallization of TiO2 Nanotubes by In Situ Heating TEM

PubMed Central

Casu, Alberto; Lamberti, Andrea

2018-01-01

The thermally-induced crystallization of anodically grown TiO2 amorphous nanotubes has been studied so far under ambient pressure conditions by techniques such as differential scanning calorimetry and in situ X-ray diffraction, then looking at the overall response of several thousands of nanotubes in a carpet arrangement. Here we report a study of this phenomenon based on an in situ transmission electron microscopy approach that uses a twofold strategy. First, a group of some tens of TiO2 amorphous nanotubes was heated looking at their electron diffraction pattern change versus temperature, in order to determine both the initial temperature of crystallization and the corresponding crystalline phases. Second, the experiment was repeated on groups of few nanotubes, imaging their structural evolution in the direct space by spherical aberration-corrected high resolution transmission electron microscopy. These studies showed that, differently from what happens under ambient pressure conditions, under the microscope’s high vacuum (p < 10−5 Pa) the crystallization of TiO2 amorphous nanotubes starts from local small seeds of rutile and brookite, which then grow up with the increasing temperature. Besides, the crystallization started at different temperatures, namely 450 and 380 °C, when the in situ heating was performed irradiating the sample with electron beam energy of 120 or 300 keV, respectively. This difference is due to atomic knock-on effects induced by the electron beam with diverse energy. PMID:29342894

Graphene nanoplate-MnO2 composites for supercapacitors: a controllable oxidation approach

NASA Astrophysics Data System (ADS)

Huang, Huajie; Wang, Xin

2011-08-01

Graphene nanoplate-MnO2 composites have been synthesized by oxidising part of the carbon atoms in the framework of graphene nanoplates at ambient temperature. The composites were characterized by means of X-ray diffraction (XRD), Raman spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS) and cyclic voltammetry (CV). It was found that the oxidation extent of the carbon atoms in the graphene framework in these composites was dependent on the reaction time, which also influenced their microstructure, morphology and electrochemical properties. Compared with MnO2 nanolamellas, the nanocomposite prepared with a reaction time of 3 h reveals better electrochemical properties as a supercapacitor electrode material.Graphene nanoplate-MnO2 composites have been synthesized by oxidising part of the carbon atoms in the framework of graphene nanoplates at ambient temperature. The composites were characterized by means of X-ray diffraction (XRD), Raman spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS) and cyclic voltammetry (CV). It was found that the oxidation extent of the carbon atoms in the graphene framework in these composites was dependent on the reaction time, which also influenced their microstructure, morphology and electrochemical properties. Compared with MnO2 nanolamellas, the nanocomposite prepared with a reaction time of 3 h reveals better electrochemical properties as a supercapacitor electrode material. Electronic supplementary information (ESI) available: Fig. S1, AFM image (5 μm × 5 μm) of graphene nanoplate-MnO2 composite obtained at 3 h; Fig. S2, nitrogen adsorption/desorption isotherm of graphene nanoplate-MnO2 composite obtained at 3 h. See DOI: 10.1039/c1nr10229j

Dislocation mediated alignment during metal nanoparticle coalescence

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lange, A. P.; Samanta, A.; Majidi, H.

2016-09-13

Dislocation mediated alignment processes during gold nanoparticle coalescence were studied at low and high temperatures using molecular dynamics simulations and transmission electron microscopy. Particles underwent rigid body rotations immediately following attachment in both low temperature (500 K) simulated coalescence events and low temperature (~315 K) transmission electron microscopy beam heating experiments. In many low temperature simulations, some degree of misorientation between particles remained after rigid body rotations, which was accommodated by grain boundary dislocation nodes. These dislocations were either sessile and remained at the interface for the duration of the simulation or dissociated and cross-slipped through the adjacent particles, leadingmore » to improved co-alignment. Minimal rigid body rotations were observed during or immediately following attachment in high temperature (1100 K) simulations, which is attributed to enhanced diffusion at the particles' interface. However, rotation was eventually induced by {111} slip on planes parallel to the neck groove. These deformation modes led to the formation of single and multi-fold twins whose structures depended on the initial orientation of the particles. The driving force for {111} slip is attributed to high surface stresses near the intersection of low energy {111} facets in the neck region. The details of this twinning process were examined in detail using simulated trajectories, and the results reveal possible mechanisms for the nucleation and propagation of Shockley partials on consecutive planes. Deformation twinning was also observed in-situ using transmission electron microscopy, which resulted in the co-alignment of a set of the particles' {111} planes across their grain boundary and an increase in their dihedral angle. As a result, this constitutes the first detailed experimental observation of deformation twinning during nanoparticle coalescence, validating simulation results presented here and elsewhere.« less

Silicon Carbide Epitaxial Films Studied by Atomic Force Microscopy

NASA Technical Reports Server (NTRS)

1996-01-01

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.

In-situ High Temperature Phase Transformations in Ceramics

DTIC Science & Technology

2009-07-28

microscopy - SEM and transmission electron microscopy - TEM), have identified important microstructural considerations, such as the critical ...particularly with judicial design of the critical particle size and microstructure.12, 47, 48 Likewise, preliminary work indicates the possibility of high...toughening of fiber reinforced, fibrous monolithic or laminated ceramic matrix composites.49, 50 enstatite was above a 7 μm critical grain size

AlGaN/GaN high electron mobility transistor grown on GaN template substrate by molecule beam epitaxy system

NASA Astrophysics Data System (ADS)

Tsai, Jenn-Kai; Chen, Y. L.; Gau, M. H.; Pang, W. Y.; Hsu, Y. C.; Lo, Ikai; Hsieh, C. H.

2008-03-01

In this study, AlGaN/GaN high electron mobility transistor (HEMT) structure was grow on GaN template substrate radio frequency plasma assisted molecular beam epitaxy (MBE) equipped with an EPI UNI-Bulb nitrogen plasma source. The undoped GaN template substrate was grown on c-sapphire substrate by metal organic vapor phase epitaxy system (MOPVD). After growth of MOVPE and MBE, the samples are characterized by double crystal X-ray diffraction (XRD), transmission electron microscopy (TEM), field emission scanning electron microscopy (SEM), atomic force microscopy (AFM), and Hall effect measurements. We found that the RMS roughness of template substrate play the major role in got the high value of mobility on AlGaN/GaN HEMT. When the roughness was lower than 0.77 nm in a 25 μm x 25 μm area, the mobility of HEMT at the temperature of 77 K was over 10000 cm^2/Vs.

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

NASA Astrophysics Data System (ADS)

Wiskel, J. B.; Li, X.; Ivey, D. G.; Henein, H.

2018-06-01

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.

Electrical conduction at domain walls in multiferroic BiFeO3

NASA Astrophysics Data System (ADS)

Seidel, Jan; Martin, Lane; He, Qing; Zhan, Qian; Chu, Ying-Hao; Rother, Axel; Hawkridge, Michael; Maksymovych, Peter; Yu, Pu; Gajek, Martin; Balke, Nina; Kalinin, Sergei; Gemming, Sybille; Wang, Feng; Catalán, Gustau; Scott, James; Spaldin, Nicola; Orenstein, Joseph; Ramesh, Ramamoorthy

2009-03-01

We report the observation of room temperature electronic conductivity at ferroelectric domain walls in BiFeO3. The origin and nature of the observed conductivity is probed using a combination of conductive atomic force microscopy, high resolution transmission electron microscopy and first-principles density functional computations. We show that a structurally driven change in both the electrostatic potential and local electronic structure (i.e., a decrease in band gap) at the domain wall leads to the observed electrical conductivity. We estimate the conductivity in the wall to be several orders of magnitude higher than for the bulk material. Additionally we demonstrate the potential for device applications of such conducting nanoscale features.

Effect of Boron on the Strength and Toughness of Direct-Quenched Low-Carbon Niobium Bearing Ultra-High-Strength Martensitic Steel

NASA Astrophysics Data System (ADS)

Hannula, Jaakko; Kömi, Jukka; Porter, David A.; Somani, Mahesh C.; Kaijalainen, Antti; Suikkanen, Pasi; Yang, Jer-Ren; Tsai, Shao-Pu

2017-11-01

The effect of boron on the microstructures and mechanical properties of laboratory-control-rolled and direct-quenched 6-mm-thick steels containing 0.08 wt pct C and 0.02 wt pct Nb were studied. The boron contents were 24 ppm and a residual amount of 4 ppm. Two different finish rolling temperatures (FRTs) of 1093 K and 1193 K (820 °C and 920 °C) were used in the hot rolling trials to obtain different levels of pancaked austenite prior to DQ. Continuous cooling transformation (CCT) diagrams were constructed to reveal the effect of boron on the transformation behavior of these steels. Microstructural characterization was carried out using various microscopy techniques, such as light optical microscopy (LOM) and scanning electron microscopy-electron backscatter diffraction (SEM-EBSD). The resultant microstructures after hot rolling were mixtures of autotempered martensite and lower bainite (LB), having yield strengths in the range 918 to 1067 MPa with total elongations to fracture higher than 10 pct. The lower FRT of 1093 K (820 °C) produced better combinations of strength and toughness as a consequence of a higher degree of pancaking in the austenite. Removal of boron lowered the 34 J/cm2 Charpy-V impact toughness transition temperature from 206 K to 158 K (-67 °C to -115 °C) when the finishing rolling temperature of 1093 K (820 °C) was used without any loss in the strength values compared to the boron-bearing steel. This was due to the finer and more uniform grain structure in the boron-free steel. Contrary to expectations, the difference was not caused by the formation of borocarbide precipitates, as verified by transmission electron microscopy (TEM) investigations, but through the grain coarsening effect of boron.

Impact of temperature and nitrogen composition on the growth of GaAsPN alloys

NASA Astrophysics Data System (ADS)

Yamane, Keisuke; Mugikura, Shun; Tanaka, Shunsuke; Goto, Masaya; Sekiguchi, Hiroto; Okada, Hiroshi; Wakahara, Akihiro

2018-03-01

This paper presents the impact of temperature and nitrogen-composition on the growth mode and crystallinity of GaAsPN alloys. Reflection high-energy electron diffraction results combined with transmission electron microscopy analysis revealed that maintaining two-dimensional (2-D) growth required higher temperatures when nitrogen composition increased. Outside the 2-D growth windows, stacking faults and micro-twins were preferentially formed at {1 1 1} B planes rather than at the {1 1 1} A planes and anomalous growth was observed. The photoluminescence spectra of GaAsPN layers implies that the higher temperature growth is effective for reducing the nitrogen-related point defects.

Fresnel Lorentz Microscopy Imaging of Domains in Fe3O4 Nanoparticle Arrays

NASA Astrophysics Data System (ADS)

Majetich, S. A.; Evarts, E. R.; Hogg, C.; Yamamoto, K.; Hirayama, T.

2009-03-01

Fresnel Lorentz microscopy was used to study the magnetic domain structures of self-assembled nanoparticle arrays as a function of temperature, from 24 to 605 C. 11 nm diameter Fe3O4 nanoparticles with an edge-to-edge spacing of 2.5 nm form magnetic domains through magnetostatic interactions alone. At room temperature stripe domains were evident in monolayer arrays. The average domain size in monolayer regions is larger than that in bilayers. Mean field theories predict a reduced stabilization energy for bilayers, relative to that for monolayers. The domain wall positions were fairly stable up to 500 C, though the contrast in the walls diminished, indicating reduced magnetic order. Above 500 C there were large temperature-dependent changes. The walls surrounding the smaller domains disappeared at lower temperatures than those of the larger domains. Some magnetic contrast was visible up to 575 C, close to the Curie temperature of Fe3O4 (585 C). Transmission electron microscopy after cooling showed that the particle shape and position in the ordered arrays had been preserved during the high temperature imaging experiments.

Evaluation of high temperature dielectric films for high voltage power electronic applications

NASA Technical Reports Server (NTRS)

Suthar, J. L.; Laghari, J. R.

1992-01-01

Three high temperature films, polyimide, Teflon perfluoroalkoxy and poly-P-xylene, were evaluated for possible use in high voltage power electronic applications, such as in high energy density capacitors, cables and microelectronic circuits. The dielectric properties, including permittivity and dielectric loss, were obtained in the frequency range of 50 Hz to 100 kHz at temperatures up to 200 C. The dielectric strengths at 60 Hz were determined as a function of temperature to 250 C. Confocal laser microscopy was performed to diagnose for voids and microimperfections within the film structure. The results obtained indicate that all films evaluated are capable of maintaining their high voltage properties, with minimal degradation, at temperatures up to 200 C. However, above 200 C, they lose some of their electrical properties. These films may therefore become viable candidates for high voltage power electronic applications at high temperatures.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Rueda-Fonseca, P.; Orrù, M.; CNRS, Institut NEEL, F-38000 Grenoble

With ZnTe as an example, we use two different methods to unravel the characteristics of the growth of nanowires (NWs) by gold-catalyzed molecular beam epitaxy at low temperature. In the first approach, CdTe insertions have been used as markers, and the nanowires have been characterized by scanning transmission electron microscopy, including geometrical phase analysis and energy dispersive electron spectrometry; the second approach uses scanning electron microscopy and the statistics of the relationship between the length of the tapered nanowires and their base diameter. Axial and radial growth are quantified using a diffusion-limited model adapted to the growth conditions; analytical expressionsmore » describe well the relationship between the NW length and the total molecular flux (taking into account the orientation of the effusion cells), and the catalyst-nanowire contact area. A long incubation time is observed. This analysis allows us to assess the evolution of the diffusion lengths on the substrate and along the nanowire sidewalls, as a function of temperature and deviation from stoichiometric flux.« less

A simple and low temperature process for super-hydrophilic rutile TiO 2 thin films growth

NASA Astrophysics Data System (ADS)

Mane, R. S.; Joo, Oh-Shim; Min, Sun-Ki; Lokhande, C. D.; Han, Sung-Hwan

2006-11-01

We investigate an environmentally friendly aqueous solution system for rutile TiO2 violet color nanocrystalline thin films growth on ITO substrate at room temperature. Film shows considerable absorption in visible region with excitonic maxima at 434 nm. X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), selected area electron diffraction (SAED), UV-vis, water surface contact angle and energy dispersive X-ray analysis (EDX) techniques in addition to actual photo-image that shows purely rutile phase of TiO2 with violet color, super-hydrophilic and densely packed nanometer-sized spherical grains of approximate diameter 3.15 ± 0.4 nm, characterize the films. Band gap energy of 4.61 eV for direct transition was obtained for the rutile TiO2 films. Film surface shows super-hydrophilic behavior, as exhibited water contact angle was 7°. Strong visible absorption (not due to chlorine) leaves future challenge to use these films in extremely thin absorber (ETA) solar cells.

Facile synthesis of hollow Co3O4 microspheres and its use as a rapid responsive CL sensor of combustible gases.

PubMed

Teng, Fei; Yao, Wenqing; Zheng, Youfei; Ma, Yutao; Xu, Tongguang; Gao, Guizhi; Liang, Shuhui; Teng, Yang; Zhu, Yongfa

2008-09-15

The hollow Co(3)O(4) microspheres (HCMs) were prepared by the carbonaceous templates, which did not need the surface pretreatment. The chemiluminescence (CL) and catalytic properties for CO oxidation over these hollow samples were evaluated. The samples were characterized by scanning electron microscopy (SEM), energy disperse spectra (EDS), transmission electron microscopy (TEM), selected area electron diffraction (ED), X-ray diffraction (XRD), temperature-programmed desorption (TPD) and N(2) adsorption. The influences of filter' band length, flow rate of gas, test temperature, and particle structure on CL intensities were mainly investigated. It was found that compared with the solid Co(3)O(4) particles (SCPs), HCMs had a stronger CL intensity, which was ascribed to its hollow structure; and that CL properties of the catalysts were well correlated with their reaction activities. Moreover, HCMs were used to fabricate a highly sensitive gas detector, which is a rapid and effective method for the selection of catalysts or the detection of environmental deleterious gases.

Properties of Rolled AZ31 Magnesium Alloy Sheet Fabricated by Continuous Variable Cross-Section Direct Extrusion

NASA Astrophysics Data System (ADS)

Liu, Yang; Li, Feng; Li, Xue Wen; Shi, Wen Yong

2018-03-01

Rolling is currently a widely used method for manufacturing and processing high-performance magnesium alloy sheets and has received widespread attention in recent years. Here, we combined continuous variable cross-section direct extrusion (CVCDE) and rolling processes. The microstructure and mechanical properties of the resulting sheets rolled at different temperatures from CVCDE extrudate were investigated by optical microscopy, scanning electron microscope, transmission electron microscopy and electron backscatter diffraction. The results showed that a fine-grained microstructure was present with an average grain size of 3.62 μm in sheets rolled from CVCDE extrudate at 623 K. Dynamic recrystallization and a large strain were induced by the multi-pass rolling, which resulted in grain refinement. In the 573-673 K range, the yield strength, tensile strength and elongation initially increased and then declined as the CVCDE temperature increased. The above results provide an important scientific basis of processing, manufacturing and the active control on microstructure and property for high-performance magnesium alloy sheet.

Nature and evolution of incommensurate charge order in manganites visualized with cryogenic scanning transmission electron microscopy.

PubMed

El Baggari, Ismail; Savitzky, Benjamin H; Admasu, Alemayehu S; Kim, Jaewook; Cheong, Sang-Wook; Hovden, Robert; Kourkoutis, Lena F

2018-02-13

Incommensurate charge order in hole-doped oxides is intertwined with exotic phenomena such as colossal magnetoresistance, high-temperature superconductivity, and electronic nematicity. Here, we map, at atomic resolution, the nature of incommensurate charge-lattice order in a manganite using scanning transmission electron microscopy at room temperature and cryogenic temperature ([Formula: see text]93 K). In diffraction, the ordering wave vector changes upon cooling, a behavior typically associated with incommensurate order. However, using real space measurements, we discover that the ordered state forms lattice-locked regions over a few wavelengths interspersed with phase defects and changing periodicity. The cations undergo picometer-scale ([Formula: see text]6 pm to 11 pm) transverse displacements, suggesting that charge-lattice coupling is strong. We further unearth phase inhomogeneity in the periodic lattice displacements at room temperature, and emergent phase coherence at 93 K. Such local phase variations govern the long-range correlations of the charge-ordered state and locally change the periodicity of the modulations, resulting in wave vector shifts in reciprocal space. These atomically resolved observations underscore the importance of lattice coupling and phase inhomogeneity, and provide a microscopic explanation for putative "incommensurate" order in hole-doped oxides. Copyright © 2018 the Author(s). Published by PNAS.

Thermometry of Silicon Nanoparticles

NASA Astrophysics Data System (ADS)

Mecklenburg, Matthew; Zutter, Brian; Regan, B. C.

2018-01-01

Current thermometry techniques lack the spatial resolution required to see the temperature gradients in typical, highly scaled modern transistors. As a step toward addressing this problem, we measure the temperature dependence of the volume plasmon energy in silicon nanoparticles from room temperature to 1250 °C , using a chip-style heating sample holder in a scanning transmission electron microscope (STEM) equipped with electron energy loss spectroscopy (EELS). The plasmon energy changes as expected for an electron gas subject to the thermal expansion of silicon. Reversing this reasoning, we find that measurements of the plasmon energy provide an independent measure of the nanoparticle temperature consistent with that of the heater chip's macroscopic, dual-function heater-and-thermometer to within the 5% accuracy of the thermometer's calibration. Thus, silicon has the potential to provide its own high-spatial-resolution thermometric readout signal via measurements of its volume plasmon energy. Furthermore, nanoparticles can, in general, serve as convenient nanothermometers for in situ electron-microscopy experiments.

Method to determine thermal profiles of nanoscale circuitry

DOEpatents

Zettl, Alexander K; Begtrup, Gavi E

2013-04-30

A platform that can measure the thermal profiles of devices with nanoscale resolution has been developed. The system measures the local temperature by using an array of nanoscale thermometers. This process can be observed in real time using a high resolution imagining technique such as electron microscopy. The platform can operate at extremely high temperatures.

Abnormal cubic-tetragonal phase transition of barium strontium titanate nanoparticles studied by in situ Raman spectroscopy and transmission electron microscopy heating experiments

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhang, Yin; Chen, Chen; Gao, Ran

2015-11-02

Phase stability of the ferroelectric materials at high temperature is extremely important to their device performance. Ba{sub x}Sr{sub 1−x}TiO{sub 3} (BST) nanoparticles with different Sr contents (x = 1, 0.91, 0.65, 0.4, and 0) are prepared by a facile hydrothermal method. Using Raman spectroscopy and transmission electron microscopy (TEM) analyses under in situ heating conditions (up to 300 °C), the phase transitions of BST nanoparticles between 25 °C and 280 °C are comprehensively investigated. The original Curie temperature of BST nanoparticles decreases abruptly with the increase in Sr content, which is more obvious than in the bulk or film material. Besides, an abnormal phase transitionmore » from cubic to tetragonal structure is observed from BST nanoparticles and the transition temperature rises along with the increase in Sr content. Direct TEM evidences including a slight lattice distortion have been provided. Differently, BaTiO{sub 3} nanoparticles remained in the tetragonal phase during the above temperature ranges.« less

Room-temperature ferromagnetic Cr-doped Ge/GeOx core-shell nanowires.

PubMed

Katkar, Amar S; Gupta, Shobhnath P; Seikh, Md Motin; Chen, Lih-Juann; Walke, Pravin S

2018-06-08

The Cr-doped tunable thickness core-shell Ge/GeO x nanowires (NWs) were synthesized and characterized using x-ray diffraction, field-emission scanning electron microscopy, transmission electron microscopy, energy-dispersive x-ray spectroscopy, x-ray photoelectron spectroscopy and magnetization studies. The shell thickness increases with the increase in synthesis temperature. The presence of metallic Cr and Cr 3+ in core-shell structure was confirmed from XPS study. The magnetic property is highly sensitive to the core-shell thickness and intriguing room temperature ferromagnetism is realized only in core-shell NWs. The magnetization decreases with an increase in shell thickness and practically ceases to exist when there is no core. These NWs show remarkably high Curie temperature (T C  > 300 K) with the dominating values of its magnetic remanence (M R ) and coercivity (H C ) compared to germanium dilute magnetic semiconductor nanomaterials. We believe that our finding on these Cr-doped Ge/GeO X core-shell NWs has the potential to be used as a hard magnet for future spintronic devices, owing to their higher characteristic values of ferromagnetic ordering.

Stability of colloidal silver nanoparticles trapped in lipid bilayer: effect of lecithin concentration and applied temperature.

PubMed

Barani, Hossein; Montazer, Majid; Braun, Hans-Georg; Dutschk, Victoria

2014-12-01

The use of silver nanoparticle on various substrates has been widespread because of its good antibacterial properties that directly depend on the stability of the silver nanoparticles in a colloidal suspension. In this study, the colloidal solutions of the silver nanoparticles were synthesised by a simple and safe method by using lecithin as a stabilising agent and their stability was examined at various temperatures. The effect of the lecithin concentrations on the stability of the synthesised silver nanoparticles was examined from 25 to 80°C at 5°C intervals, by recording the changes in the UV-vis absorption spectra, the hydrodynamic diameter and the light scattering intensity of the silver nanoparticles. In addition, the morphology of the synthesised silver nanoparticles was investigated with the low-voltage scanning electron microscopy and transmission electron microscopy. The results indicated that increasing temperature caused different changes in the size of the stabilised and the unstabilised silver nanoparticles. The size of the stabilised silver nanoparticles reduced from 38 to 36 nm during increasing temperature, which confirmed good stability.

Effects of Cryogenic Temperature on Fracture Toughness of Core-Shell Rubber (CSR) Toughened Epoxy Nanocomposites

NASA Technical Reports Server (NTRS)

Wang, J.; Cannon, S. A.; Magee, D.; Schneider, J. A.

2008-01-01

This study investigated the effects of core-shell rubber (CSR) nanoparticles on the mechanical properties and fracture toughness of an epoxy resin at ambient and liquid nitrogen (LN2) temperatures. Varying amounts of Kane Ace MX130 toughening agent were added to a commercially available EPON 862/Epikure W epoxy resin. Elastic modulus was calculated using quasi-static tensile data. Fracture toughness was evaluated by the resulting breaking energy measured in Charpy impact tests conducted on an instrumented drop tower. The size and distribution of the CSR nanoparticles were characterized using Transmission Electron Microscopy (TEM) and Small Angle X-ray Scattering (SAXS). Scanning Electron Microscopy (SEM) was used to study the fracture surface morphology. The addition of the CSR nanoparticles increased the breaking energy with negligible change in elastic modulus and ultimate tensile stress (UTS). At ambient temperature the breaking energy increased with increasing additions of the CSR nanoparticles, while at LN2 temperatures, it reached a maximum at 5 wt% CSR concentration. KEY WORDS: liquid nitrogen (LN2) properties, fracture toughness, core-shell rubber (CSR).

Scanning Electron Microscopy-Energy-Dispersive X-Ray (SEM/EDX): A Rapid Diagnostic Tool to Aid the Identification of Burnt Bone and Contested Cremains.

PubMed

Ellingham, Sarah T D; Thompson, Tim J U; Islam, Meez

2018-03-01

This study investigates the use of Scanning electron microscopy-energy-dispersive X-ray (SEM-EDX) as a diagnostic tool for the determination of the osseous origin of samples subjected to different temperatures. Sheep (Ovis aries) ribs of two experimental groups (fleshed and defleshed) were burned at temperatures of between 100°C and 1100°C in 100°C increments and subsequently analyzed with the SEM-EDX to determine the atomic percentage of present elements. Three-factor ANOVA analysis showed that neither the exposure temperature, nor whether the burning occurred with or without soft tissue present had any significant influence on the bone's overall elemental makeup (p > 0.05). The Ca/P ratio remained in the osseous typical range of between 1.6 and 2.58 in all analyzed samples. This demonstrates that even faced with high temperatures, the overall gross elemental content and atomic percentage of elements in bone remain stable, creating a unique "fingerprint" for osseous material, even after exposure to extreme conditions. © 2017 American Academy of Forensic Sciences.

Room-temperature ferromagnetic Cr-doped Ge/GeOx core–shell nanowires

NASA Astrophysics Data System (ADS)

Katkar, Amar S.; Gupta, Shobhnath P.; Motin Seikh, Md; Chen, Lih-Juann; Walke, Pravin S.

2018-06-01

The Cr-doped tunable thickness core–shell Ge/GeOx nanowires (NWs) were synthesized and characterized using x-ray diffraction, field-emission scanning electron microscopy, transmission electron microscopy, energy-dispersive x-ray spectroscopy, x-ray photoelectron spectroscopy and magnetization studies. The shell thickness increases with the increase in synthesis temperature. The presence of metallic Cr and Cr3+ in core–shell structure was confirmed from XPS study. The magnetic property is highly sensitive to the core–shell thickness and intriguing room temperature ferromagnetism is realized only in core–shell NWs. The magnetization decreases with an increase in shell thickness and practically ceases to exist when there is no core. These NWs show remarkably high Curie temperature (TC > 300 K) with the dominating values of its magnetic remanence (MR) and coercivity (HC) compared to germanium dilute magnetic semiconductor nanomaterials. We believe that our finding on these Cr-doped Ge/GeOX core–shell NWs has the potential to be used as a hard magnet for future spintronic devices, owing to their higher characteristic values of ferromagnetic ordering.

Cathodoluminescence of stacking fault bound excitons for local probing of the exciton diffusion length in single GaN nanowires

DOE Office of Scientific and Technical Information (OSTI.GOV)

Nogues, Gilles, E-mail: gilles.nogues@neel.cnrs.fr; Den Hertog, Martien; Inst. NEEL, CNRS, F-38042 Grenoble

We perform correlated studies of individual GaN nanowires in scanning electron microscopy combined to low temperature cathodoluminescence, microphotoluminescence, and scanning transmission electron microscopy. We show that some nanowires exhibit well localized regions emitting light at the energy of a stacking fault bound exciton (3.42 eV) and are able to observe the presence of a single stacking fault in these regions. Precise measurements of the cathodoluminescence signal in the vicinity of the stacking fault give access to the exciton diffusion length near this location.

Direct correlations of structural and optical properties of three-dimensional GaN/InGaN core/shell micro-light emitting diodes

NASA Astrophysics Data System (ADS)

Sadat Mohajerani, Matin; Müller, Marcus; Hartmann, Jana; Zhou, Hao; Wehmann, Hergo-H.; Veit, Peter; Bertram, Frank; Christen, Jürgen; Waag, Andreas

2016-05-01

Three-dimensional (3D) InGaN/GaN quantum-well (QW) core-shell light emitting diodes (LEDs) are a promising candidate for the future solid state lighting. In this contribution, we study direct correlations of structural and optical properties of the core-shell LEDs using highly spatially-resolved cathodoluminescence spectroscopy (CL) in combination with scanning electron microscopy (SEM) and scanning transmission electron microscopy (STEM). Temperature-dependent resonant photoluminescence (PL) spectroscopy has been performed to understand recombination mechanisms and to estimate the internal quantum efficiency (IQE).

Collective Modes and Structural Modulation in Ni-Mn-Ga(Co) Martensite Thin Films Probed by Femtosecond Spectroscopy and Scanning Tunneling Microscopy.

PubMed

Schubert, M; Schaefer, H; Mayer, J; Laptev, A; Hettich, M; Merklein, M; He, C; Rummel, C; Ristow, O; Großmann, M; Luo, Y; Gusev, V; Samwer, K; Fonin, M; Dekorsy, T; Demsar, J

2015-08-14

The origin of the martensitic transition in the magnetic shape memory alloy Ni-Mn-Ga has been widely discussed. While several studies suggest it is electronically driven, the adaptive martensite model reproduced the peculiar nonharmonic lattice modulation. We used femtosecond spectroscopy to probe the temperature and doping dependence of collective modes, and scanning tunneling microscopy revealed the corresponding static modulations. We show that the martensitic phase can be described by a complex charge-density wave tuned by magnetic ordering and strong electron-lattice coupling.

Collective Modes and Structural Modulation in Ni-Mn-Ga(Co) Martensite Thin Films Probed by Femtosecond Spectroscopy and Scanning Tunneling Microscopy

NASA Astrophysics Data System (ADS)

Schubert, M.; Schaefer, H.; Mayer, J.; Laptev, A.; Hettich, M.; Merklein, M.; He, C.; Rummel, C.; Ristow, O.; Großmann, M.; Luo, Y.; Gusev, V.; Samwer, K.; Fonin, M.; Dekorsy, T.; Demsar, J.

2015-08-01

The origin of the martensitic transition in the magnetic shape memory alloy Ni-Mn-Ga has been widely discussed. While several studies suggest it is electronically driven, the adaptive martensite model reproduced the peculiar nonharmonic lattice modulation. We used femtosecond spectroscopy to probe the temperature and doping dependence of collective modes, and scanning tunneling microscopy revealed the corresponding static modulations. We show that the martensitic phase can be described by a complex charge-density wave tuned by magnetic ordering and strong electron-lattice coupling.

Improvement of critical current density in thallium-based (Tl,Bi)Sr{sub 1.6}Ba{sub 0.4}Ca{sub 2}Cu{sub 3}O{sub x} superconductors

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ren, Z.F.; Wang, C.A.; Wang, J.H.

1994-12-31

Epitaxial (Tl,Bi)Sr{sub 1.6}Ba{sub 0.4}Ca{sub 2}Cu{sub 3}O{sub x} (Tl,Bi)-1223 thin films on (100) single crystal LaAlO{sub 3} substrates were synthesized by a two-step procedure. Phase development, microstructure, and relationships between film and substrate were studied by X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). Resistance versus temperature, zero-field-cooled and field-cooled magnetization, and transport critical current density (J{sub c}) were measured. The zero-resistance temperature was 105-111 K. J{sub c} at 77 K and zero field was > 2 x 10{sup 6} A/cm{sup 2}. The films exhibited good flux pinning properties.

Microfluidic reactor synthesis and photocatalytic behavior of Cu@Cu2O nanocomposite

NASA Astrophysics Data System (ADS)

Xu, Lei; Srinivasakannan, C.; Peng, Jinhui; Yan, Mi; Zhang, Di; Zhang, Libo

2015-03-01

The Cu@Cu2O nanocomposites were synthesized by solution-phase synthesis of Cu nanoparticles in microfluidic reactor at room temperature, followed by controlling the oxidation process. The size, morphology, elemental compositions, and the chemical composition on the surface of Cu@Cu2O nanocomposite were characterized by transmission electron microscopy (TEM), scanning electron microscopy (SEM), X-ray diffraction (XRD), and X-ray photoelectron spectroscopy (XPS). Experimental results demonstrated that the surface of the Cu nanoparticles was oxidized to Cu2O which serves as the shell of nanoparticle. The amount of Cu2O can be controlled by varying the drying temperature. Additionally the binary Cu@Cu2O nanocomposite along with H2O2 exhibited its potential as an excellent photocatalyst for degradation of methylene blue (MB) under UV irradiation.

Ultrasound with low intensity assisted the synthesis of nanocrystalline TiO2 without calcination.

PubMed

Ghows, Narjes; Entezari, Mohamad H

2010-06-01

A novel method has been developed for the preparation of nano-sized TiO(2) with anatase phase. Nanoparticles with diameter about 6 nm were prepared at a relatively low temperature (75 degrees C) and short time. The synthesis was carried out by the hydrolysis of titanium tetra-isopropoxide (TTIP) in the presence of water, ethanol, and dispersant under ultrasonic irradiation (500 kHz) at low intensity. The results show that variables such as water/ethanol ratio, irradiation time, and temperature have a great influence on the particle size and crystalline phases of TiO(2) nanoparticles. Characterization of the product was carried out by different techniques such as powder X-ray diffraction (XRD), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HRTEM) and UV-vis spectroscopy. (c) 2010 Elsevier B.V. All rights reserved.

Synthesis of porous nanocrystalline NiO with hexagonal sheet-like morphology by homogeneous precipitation method

NASA Astrophysics Data System (ADS)

Sharma, Ravi Kant; Ghose, Ranjana

2015-04-01

Porous nanocrystalline NiO has been synthesized by a simple homogeneous precipitation method in short time at low calcination temperature without using any surfactant, chelating or gelating agents. The porous nanocrystalline NiO with a hexagonal sheet-like morphology were obtained by calcination of Ni(OH)2 nanoflakes at 500 °C. The calcination temperature strongly influences the morphology, crystallite size, specific surface area, pore volume and optical band gap of the samples. The samples were characterized using powder X-ray diffraction, thermal gravimetric analysis, FT-IR spectroscopy, UV-Visible diffuse reflectance spectroscopy, surface area measurements, field emission scanning electron microscopy coupled with energy dispersive X-ray analysis and transmission electron microscopy. The chemical activity of the samples was tested by catalytic reduction of 4-nitrophenol with NaBH4.

Carbon Coated α-Fe2O3 Photoanode Synthesized by a Facile Anodic Electrodeposition for Highly Efficient Water Oxidation

NASA Astrophysics Data System (ADS)

Zhang, Honglei; Li, Longzhu; Liu, Changhai; Wang, Wenchang; Liang, Penghua; Mitsuzak, Naotoshi; Chen, Zhidong

2018-05-01

This work provides a facile anodic electrodeposition method for synthesizing carbon coated α-Fe2O3 photoanode followed by annealing treatment with argon atmosphere. Compared with bare hematite photoanode, the carbon coated α-Fe2O3 photoanodes annealed at lower temperature (Fe2O3/C-L) and higher temperature (Fe2O3/C-H) have higher photocurrent density as 0.3 and 0.5 mA cm-2 (at 1.23 V vs. RHE), respectively. The excellent PEC performance is attributed to the synergistic reaction of carbon and vacancy oxygen. The morphology and properties of the sample were characterized with scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectroscopy, UV-Vis spectra, X-ray diffractometry, X-ray photoelectron spectra, and photoelectrical measurements.

Studying Pulsed Laser Deposition conditions for Ni/C-based multi-layers

NASA Astrophysics Data System (ADS)

Bollmann, Tjeerd R. J.

2018-04-01

Nickel carbon based multi-layers are a viable route towards future hard X-ray and soft γ-ray focusing telescopes. Here, we study the Pulsed Laser Deposition growth conditions of such bilayers by Reflective High Energy Electron Diffraction, X-ray Reflectivity and Diffraction, Atomic Force Microscopy, X-ray Photoelectron Spectroscopy and cross-sectional Transmission Electron Microscopy analysis, with emphasis on optimization of process pressure and substrate temperature during growth. The thin multi-layers are grown on a treated SiO substrate resulting in Ni and C layers with surface roughnesses (RMS) of ≤0.2 nm. Small droplets resulting during melting of the targets surface increase the roughness, however, and cannot be avoided. The sequential process at temperatures beyond 300 °C results into intermixing between the two layers, being destructive for the reflectivity of the multi-layer.

ZnO nanomaterials based surface acoustic wave ethanol gas sensor.

PubMed

Wu, Y; Li, X; Liu, J H; He, Y N; Yu, L M; Liu, W H

2012-08-01

ZnO nanomaterials based surface acoustic wave (SAW) gas sensor has been investigated in ethanol environment at room temperature. The ZnO nanomaterials have been prepared through thermal evaporation of high-purity zinc powder. The as-prepared ZnO nanomaterials have been characterized with scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X-ray Diffraction (XRD) techniques. The results indicate that the obtained ZnO nanomaterials, including many types of nanostructures such as nanobelts, nanorods, nanowires as well as nanosheets, are wurtzite with hexagonal structure and well-crystallized. The SAW sensor coated with the nanostructured ZnO materials has been tested in ethanol gas of various concentrations at room temperature. A network analyzer is used to monitor the change of the insertion loss of the SAW sensor when exposed to ethanol gas. The insertion loss of the SAW sensor varies significantly with the change of ethanol concentration. The experimental results manifest that the ZnO nanomaterials based SAW ethanol gas sensor exhibits excellent sensitivity and good short-term reproducibility at room temperature.

Growth process optimization of ZnO thin film using atomic layer deposition

NASA Astrophysics Data System (ADS)

Weng, Binbin; Wang, Jingyu; Larson, Preston; Liu, Yingtao

2016-12-01

The work reports experimental studies of ZnO thin films grown on Si(100) wafers using a customized thermal atomic layer deposition. The impact of growth parameters including H2O/DiethylZinc (DEZn) dose ratio, background pressure, and temperature are investigated. The imaging results of scanning electron microscopy and atomic force microscopy reveal that the dose ratio is critical to the surface morphology. To achieve high uniformity, the H2O dose amount needs to be at least twice that of DEZn per each cycle. If the background pressure drops below 400 mTorr, a large amount of nanoflower-like ZnO grains would emerge and increase surface roughness significantly. In addition, the growth temperature range between 200 °C and 250 °C is found to be the optimal growth window. And the crystal structures and orientations are also strongly correlated to the temperature as proved by electron back-scattering diffraction and x-ray diffraction results.

Synthesis and characterization of hybrid nanocomposites as highly-efficient conducting CH4 gas sensor.

PubMed

Aldalbahi, Ali; Feng, Peter; Alhokbany, Norah; Al-Farraj, Eida; Alshehri, Saad M; Ahamad, Tansir

2017-02-15

Functionalized (MWCNTs-COOH), non-functionalized multiwalled carbon nanotubes (MWCNTs) and polyaniline (PANI) based conducting nanocomposites (PANI/polymer/MWCNTs and PANI/polymer/MWCNTs-COOH) have been prepared in polymer matrix. The prepared nanocomposites were characterized via FTIR, TGA, Raman spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X-ray diffraction (XRD). It was observed that the prepared conducting nanocomposites show excellent sensing performances toward CH 4 at room temperature and both the response and recovery time were recorded at around 5s, respectively, at the room. The PANI/polymer/MWCNTs based detector had quicker/shorter response time (<1s), as well as higher sensitivity (3.1%) than that of the PANI/polymer/MWCNTs-COOH based detector. This was attributed to nonconductive -COOH that results in a poor sensitivity of PANI/polymer/MWCNTs-COOH-based prototype. The PANI/polymer/MWCNTs-COOH nanocomposites show almost 10 time higher sensitivity at higher temperature (60°C) than that at room temperature. Copyright © 2016. Published by Elsevier B.V.

Heteroepitaxial growth of Ge films on (100) GaAs by pyrolysis of digermane

NASA Astrophysics Data System (ADS)

Eres, Djula; Lowndes, Douglas H.; Tischler, J. Z.; Sharp, J. W.; Geohegan, D. B.; Pennycook, S. J.

1989-08-01

Pyrolysis of high-purity digermane (Ge2 H6 ) has been used to grow epitaxial Ge films of high crystalline quality on (100) GaAs substrates in a low-pressure environment. X-ray double-crystal diffractometry shows that fully commensurate, coherently strained epitaxial Ge films can be grown on (100) GaAs at digermane partial pressures of 0.05-40 mTorr for substrate temperatures of 380-600 °C. Amorphous films also were deposited. Information about the crystalline films surface morphology, growth mode, and microstructure was obtained from scanning electron microscopy, cross-section transmission electron microscopy, and in situ reflectivity measurements. The amorphous-to-crystalline transition temperature and the morphology of the crystalline films were both found to depend on deposition conditions (primarily the incidence rate of Ge-bearing species and the substrate temperature). Epitaxial growth rates using digermane were found to be about two orders of magnitude higher than rates using germane (GeH4 ) under similar experimental conditions.

Synthesis of Carbon Nanotubes and Nanospheres from Coconut Fibre and the Role of Synthesis Temperature on Their Growth

NASA Astrophysics Data System (ADS)

Adewumi, Gloria A.; Inambao, Freddie; Eloka-Eboka, Andrew; Revaprasadu, Neerish

2018-07-01

Carbon nanotubes (CNT) and carbon nanospheres were successfully synthesized from coconut fibre-activated carbon. The biomass was first carbonized then physically activated, followed by treatment using ethanol vapor at 700°C to 1100°C at 100°C intervals. The effect of synthesis temperature on the formation of the nanomaterials was studied using scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive x-ray spectrometry, x-ray diffraction (XRD), Fourier transform infrared microscopy (FTIR) and thermogravimetric analysis. SEM analysis revealed that nanospheres were formed at higher temperatures of 1000°C and 1100°C, while lower temperatures of 800°C and 900°C favored the growth of CNT. At 700°C, however, no tubes or spheres were formed. TEM and FTIR were used to observe spectral features, such as the peak positions, intensity and bandwidth, which are linked to some structural properties of the samples investigated. All these observations provided facts on the nanosphere and nanotube dimensions, vibrational modes and the degree of purity of the obtained samples. The TEM results show spheres of diameter in the range 50 nm to 250 nm while the tubes had diameters between 50 nm to 100 nm. XRD analysis reveals the materials synthesized are amorphous in nature with a hexagonal graphite structure.

Synthesis of Carbon Nanotubes and Nanospheres from Coconut Fibre and the Role of Synthesis Temperature on Their Growth

NASA Astrophysics Data System (ADS)

Adewumi, Gloria A.; Inambao, Freddie; Eloka-Eboka, Andrew; Revaprasadu, Neerish

2018-04-01

Carbon nanotubes (CNT) and carbon nanospheres were successfully synthesized from coconut fibre-activated carbon. The biomass was first carbonized then physically activated, followed by treatment using ethanol vapor at 700°C to 1100°C at 100°C intervals. The effect of synthesis temperature on the formation of the nanomaterials was studied using scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive x-ray spectrometry, x-ray diffraction (XRD), Fourier transform infrared microscopy (FTIR) and thermogravimetric analysis. SEM analysis revealed that nanospheres were formed at higher temperatures of 1000°C and 1100°C, while lower temperatures of 800°C and 900°C favored the growth of CNT. At 700°C, however, no tubes or spheres were formed. TEM and FTIR were used to observe spectral features, such as the peak positions, intensity and bandwidth, which are linked to some structural properties of the samples investigated. All these observations provided facts on the nanosphere and nanotube dimensions, vibrational modes and the degree of purity of the obtained samples. The TEM results show spheres of diameter in the range 50 nm to 250 nm while the tubes had diameters between 50 nm to 100 nm. XRD analysis reveals the materials synthesized are amorphous in nature with a hexagonal graphite structure.

Size and surface effects on the magnetism of magnetite and maghemite nanoparticles

DOE Office of Scientific and Technical Information (OSTI.GOV)

Nikiforov, V. N., E-mail: pppnvn@yandex.ru; Ignatenko, A. N.; Irkhin, V. Yu.

2017-02-15

The size effects of magnetite and maghemite nanoparticles on their magnetic properties (magnetic moment, Curie temperature, blocking temperature, etc.) have been investigated. Magnetic separation and centrifugation of an aqueous solution of nanoparticles were used for their separation into fractions; their sizes were measured by atomic force microscopy, dynamic light scattering, and electron microscopy. A change in the size leads to a change in the Curie temperature and magnetic moment per formula unit. Both native nanoparticles and those covered with a bioresorbable layer have been considered. The magnetic properties have been calculated by the Monte Carlo method for the classical Heisenbergmore » model with various bulk and surface magnetic moments.« less

Effect of solution treatment on microstructure and properties of duplex stainless steel

NASA Astrophysics Data System (ADS)

Wang, X. Y.; Luo, J. M.; Huang, L. Q.; Wang, H. B.; Ma, C. W.

2017-09-01

The influence of solution treatment on microstructure and properties of 2205 duplex stainless steel (DSS) was studied. The microstructure, precipitates and corrosion resisting property were observed and analyzed by means of optical microscopy (OM), scanning electron microscopy (SEM) and electrochemical methods. The results showed that a large number of brittle σ-phase precipitates, which deteriorate the plasticity and corrosion resistance of the material, were easy to produce in the duplex stainless steel under the low temperature. The precipitation of σ-phase can be decreased and the plasticity and corrosion resistance can be improved by increasing solution temperature. In addition, the ferrite content increases with the increase of solution temperature, while less affected by cooling rate.

Dynamic recrystallization and grain boundary migration in B2 FeAl

NASA Technical Reports Server (NTRS)

Baker, I.; Gaydosh, D. J.

1987-01-01

Transmission electron microscopy and optical microscopy were used to examine polycrystalline specimens of the B2-structured alloy FeAl strained under tension to fracture at elevated temperature. Strain-induced grain boundary migration was observed above 900 K and dynamic recrystallization was found at 1000 K and 1100 K. Little evidence of dynamic recovery was evident but some networks were formed at 1100 K.

Size-dependent magnetic anisotropy of PEG coated Fe3O4 nanoparticles; comparing two magnetization methods

NASA Astrophysics Data System (ADS)

Nayek, C.; Manna, K.; Imam, A. A.; Alqasrawi, A. Y.; Obaidat, I. M.

2018-02-01

Understanding the size dependent magnetic anisotropy of iron oxide nanoparticles is essential for the successful application of these nanoparticles in several technological and medical fields. PEG-coated iron oxide (Fe3O4) nanoparticles with core diameters of 12 nm, 15 nm, and 16 nm were synthesized by the usual co-precipitation method. The morphology and structure of the nanoparticles were investigated using transmission electron microscopy (TEM), high resolution transmission electron microscopy (HRTEM), selected area electron diffraction (SAED), and X-ray diffraction (XRD). Magnetic measurements were conducted using a SQUID. The effective magnetic anisotropy was calculated using two methods from the magnetization measurements. In the first method the zero-field-cooled magnetization versus temperature measurements were used at several applied magnetic fields. In the second method we used the temperature-dependent coercivity curves obtained from the zero-field-cooled magnetization versus magnetic field hysteresis loops. The role of the applied magnetic field on the effective magnetic anisotropy, calculated form the zero-field-cooled magnetization versus temperature measurements, was revealed. The size dependence of the effective magnetic anisotropy constant Keff obtained by the two methods are compared and discussed.

Electrical characterization of HgTe nanowires using conductive atomic force microscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gundersen, P.; Department of Physics, Norwegian University of Science and Technology, NO-7491 Trondheim; Kongshaug, K. O.

Self-organized HgTe nanowires grown by molecular beam epitaxy (MBE) have been characterized using conductive atomic force microscopy. As HgTe will degrade or evaporate at normal baking temperatures for electron beam lithography (EBL) resists, an alternative method was developed. Using low temperature optical lithography processes, large Au contacts were deposited on a sample covered with randomly oriented, lateral HgTe nanowires. Nanowires partly covered by the large electrodes were identified with a scanning electron microscope and then localized in the atomic force microscope (AFM). The conductive tip of the AFM was then used as a movable electrode to measure current-voltage curves atmore » several locations on HgTe nanowires. The measurements revealed that polycrystalline nanowires had diffusive electron transport, with resistivities two orders of magnitude larger than that of an MBE-grown HgTe film. The difference can be explained by scattering at the rough surface walls and at the grain boundaries in the wires. The method can be a solution when EBL is not available or requires too high temperature, or when measurements at several positions along a wire are required.« less

Scanning electron microscopy of the surfaces of ion implanted SiC

NASA Astrophysics Data System (ADS)

Malherbe, Johan B.; van der Berg, N. G.; Kuhudzai, R. J.; Hlatshwayo, T. T.; Thabethe, T. T.; Odutemowo, O. S.; Theron, C. C.; Friedland, E.; Botha, A. J.; Wendler, E.

2015-07-01

This paper gives a brief review of radiation damage caused by particle (ions and neutrons) bombardment in SiC at different temperatures, and its annealing, with an expanded discussion on the effects occurring on the surface. The surface effects were observed using SEM (scanning electron microscopy) with an in-lens detector and EBSD (electron backscatter diffraction). Two substrates were used, viz. single crystalline 6H-SiC wafers and polycrystalline SiC, where the majority of the crystallites were 3C-SiC. The surface modification of the SiC samples by 360 keV ion bombardment was studied at temperatures below (i.e. room temperature), just at (i.e. 350 °C), or above (i.e. 600 °C) the critical temperature for amorphization of SiC. For bombardment at a temperature at about the critical temperature an extra step, viz. post-bombardment annealing, was needed to ascertain the microstructure of bombarded layer. Another aspect investigated was the effect of annealing of samples with an ion bombardment-induced amorphous layer on a 6H-SiC substrate. SEM could detect that this layer started to crystalize at 900 °C. The resulting topography exhibited a dependence on the ion species. EBSD showed that the crystallites forming in the amorphized layer were 3C-SiC and not 6H-SiC as the substrate. The investigations also pointed out the behaviour of the epitaxial regrowth of the amorphous layer from the 6H-SiC interface.

Localized to itinerant transition of f electrons in ordered Ce films on W(110)

NASA Astrophysics Data System (ADS)

Chen, Q. Y.; Feng, W.; Xie, D. H.; Lai, X. C.; Zhu, X. G.; Huang, L.

2018-04-01

A key issue to understand the driving force and underlying physics in the isostructural γ -α transition in Cerium is the character of the 4 f states, whether it is localized or itinerant. Here the surface topography and electronic structure of the well-ordered Ce metal films on a W(110) substrate were investigated by using scanning tunneling microscopy, angle-resolved photoemission spectroscopy and density functional theory, and single-site dynamical mean-field theory calculations. Three nearly flat f bands can be observed, and a weakly dispersive quasiparticle band near the Fermi level has been directly observed at low temperature, indicating the hybridization between f electrons and conduction electrons in the low-temperature α phase. The hybridization strength becomes weaker upon increasing temperature, and the f electrons become almost fully localized at 300 K in the high-temperature γ phase. The observed localized-to-itinerant transition of the f electrons with decreasing temperature gives direct experimental proof for the changes of the 4 f character in the isostructural γ -α phase transition. Our results suggest that the character of the f electrons plays a crucial role during the γ -α phase transition.

Nanostructure of and structural defects in a Mo2BC hard coating investigated by transmission electron microscopy and atom probe tomography

NASA Astrophysics Data System (ADS)

Gleich, Stephan; Fager, Hanna; Bolvardi, Hamid; Achenbach, Jan-Ole; Soler, Rafael; Pradeep, Konda Gokuldoss; Schneider, Jochen M.; Dehm, Gerhard; Scheu, Christina

2017-08-01

In this work, the nanostructure of a Mo2BC hard coating was determined by several transmission electron microscopy methods and correlated with the mechanical properties. The coating was deposited on a Si (100) wafer by bipolar pulsed direct current magnetron sputtering from a Mo2BC compound target in Ar at a substrate temperature of 630 °C. Transmission electron microscopy investigations revealed structural features at various length scales: bundles (30 nm to networks of several micrometers) consisting of columnar grains (˜10 nm in diameter), grain boundary regions with a less ordered atomic arrangement, and defects including disordered clusters (˜1.5 nm in diameter) as well as stacking faults within the grains. The most prominent defect with a volume fraction of ˜0.5% is the disordered clusters, which were investigated in detail by electron energy loss spectroscopy and atom probe tomography. The results provide conclusive evidence that Ar is incorporated into the Mo2BC film as disordered Ar-rich Mo-B-C clusters of approximately 1.5 nm in diameter. Hardness values of 28 ± 1 GPa were obtained by nanoindentation tests. The Young's modulus of the Mo2BC coating exhibits a value of 462 ± 9 GPa, which is consistent with ab initio calculations for crystalline and defect free Mo2BC and measurements of combinatorically deposited Mo2BC thin films at a substrate temperature of 900 °C. We conclude that a reduction of the substrate temperature of 270 °C has no significant influence on hardness and Young's modulus of the Mo2BC hard coating, even if its nanostructure exhibits defects.

Low-temperature synthesis of 2D MoS2 on a plastic substrate for a flexible gas sensor.

PubMed

Zhao, Yuxi; Song, Jeong-Gyu; Ryu, Gyeong Hee; Ko, Kyung Yong; Woo, Whang Je; Kim, Youngjun; Kim, Donghyun; Lim, Jun Hyung; Lee, Sunhee; Lee, Zonghoon; Park, Jusang; Kim, Hyungjun

2018-05-08

The efficient synthesis of two-dimensional molybdenum disulfide (2D MoS2) at low temperatures is essential for use in flexible devices. In this study, 2D MoS2 was grown directly at a low temperature of 200 °C on both hard (SiO2) and soft substrates (polyimide (PI)) using chemical vapor deposition (CVD) with Mo(CO)6 and H2S. We investigated the effect of the growth temperature and Mo concentration on the layered growth by Raman spectroscopy and microscopy. 2D MoS2 was grown by using low Mo concentration at a low temperature. Through optical microscopy, Raman spectroscopy, X-ray photoemission spectroscopy, photoluminescence, and transmission electron microscopy measurements, MoS2 produced by low-temperature CVD was determined to possess a layered structure with good uniformity, stoichiometry, and a controllable number of layers. Furthermore, we demonstrated the realization of a 2D MoS2-based flexible gas sensor on a PI substrate without any transfer processes, with competitive sensor performance and mechanical durability at room temperature. This fabrication process has potential for burgeoning flexible and wearable nanotechnology applications.

Effect of Nb on microstructure and yield strength of a high temperature tempered martensitic steel

NASA Astrophysics Data System (ADS)

Wang, Qian; Sun, Yu; Zhang, Chuanyou; Wang, Qingfeng; Zhang, Fucheng

2018-04-01

Martensitic steels based on a composition of 25CrMo47NbVTi with different concentrations of Nb (0.003%–0.060%) were quenched (Q) at 900 °C and tempered (T) at 700 °C to obtain oil country tubular goods (OCTG) with higher yield strength. The precipitation and microstructures were characterized and quantified by optical microscopy (OM), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and x-ray diffraction (XRD). The results show that the increased Nb content led to an enhanced overall precipitation, the rising solution-precipitation temperature, the increased mass or volume fraction of the Nb-containing precipitates, and the decreased average diameter of Nb-containing particles. With the enhanced precipitation of small sized Nb-containing particles, the austenite grain and corresponding martensitic packet and block were evidently refined. In addition, the dislocation density increased slightly with increasing Nb addition. The yield strength was experimentally measured and quantitatively estimated. The findings based on theoretical calculations indicated that as a consequence of intensified strengthening from grain boundaries, precipitates and dislocations, the yield strength was enhanced significantly by Nb addition.

Submerged Arc Stainless Steel Strip Cladding—Effect of Post-Weld Heat Treatment on Thermal Fatigue Resistance

NASA Astrophysics Data System (ADS)

Kuo, I. C.; Chou, C. P.; Tseng, C. F.; Lee, I. K.

2009-03-01

Two types of martensitic stainless steel strips, PFB-132 and PFB-131S, were deposited on SS41 carbon steel substrate by a three-pass submerged arc cladding process. The effects of post-weld heat treatment (PWHT) on thermal fatigue resistance and hardness were evaluated by thermal fatigue and hardness testing, respectively. The weld metal microstructure was investigated by utilizing optical microscopy, scanning electron microscopy (SEM) equipped with energy dispersive X-ray spectroscopy (EDS) and transmission electron microscopy (TEM). Results showed that, by increasing the PWHT temperature, hardness decreased but there was a simultaneous improvement in weldment thermal fatigue resistance. During tempering, carbide, such as (Fe, Cr)23C6, precipitated in the weld metals and molybdenum appeared to promote (Fe, Cr, Mo)23C6 formation. The precipitates of (Fe, Cr, Mo)23C6 revealed a face-centered cubic (FCC) structure with fine grains distributed in the microstructure, thereby effectively increasing thermal fatigue resistance. However, by adding nickel, the AC1 temperature decreased, causing a negative effect on thermal fatigue resistance.

Delaminated graphene at silicon carbide facets: atomic scale imaging and spectroscopy.

PubMed

Nicotra, Giuseppe; Ramasse, Quentin M; Deretzis, Ioannis; La Magna, Antonino; Spinella, Corrado; Giannazzo, Filippo

2013-04-23

Atomic-resolution structural and spectroscopic characterization techniques (scanning transmission electron microscopy and electron energy loss spectroscopy) are combined with nanoscale electrical measurements (conductive atomic force microscopy) to study at the atomic scale the properties of graphene grown epitaxially through the controlled graphitization of a hexagonal SiC(0001) substrate by high temperature annealing. This growth technique is known to result in a pronounced electron-doping (∼10(13) cm(-2)) of graphene, which is thought to originate from an interface carbon buffer layer strongly bound to the substrate. The scanning transmission electron microscopy analysis, carried out at an energy below the knock-on threshold for carbon to ensure no damage is imparted to the film by the electron beam, demonstrates that the buffer layer present on the planar SiC(0001) face delaminates from it on the (112n) facets of SiC surface steps. In addition, electron energy loss spectroscopy reveals that the delaminated layer has a similar electronic configuration to purely sp2-hybridized graphene. These observations are used to explain the local increase of the graphene sheet resistance measured around the surface steps by conductive atomic force microscopy, which we suggest is due to significantly lower substrate-induced doping and a resonant scattering mechanism at the step regions. A first-principles-calibrated theoretical model is proposed to explain the structural instability of the buffer layer on the SiC facets and the resulting delamination.

New and little known feather mites (Acari)

USDA-ARS?s Scientific Manuscript database

Feather mites (Acari: Astigmata) were analyzed with low temperature scanning electron microscopy (LT-SEM), including the description of three new species: Plicatalloptes atrichogynus sp. nov. (Analgoidea: Alloptidae) from the Neotropical cormorant Phalacrocorax brasilianus (Gmelin, 1789) (Pelecanifo...

Growth, Structural, Electronic, and Magnetic Characterization of GaN, CrN, Fe Islands on CrN, and Fe/CrN Bilayer Thin Films

NASA Astrophysics Data System (ADS)

Alam, Khan

As a part of my Ph.D research, initially I was involved in construction and calibration of an ultra-high vacuum thin film facility, and later on I studied structural, electronic, and magnetic properties of GaN, CrN, Fe/CrN bilayers, and Fe islands on CrN thin films. All of these films were grown by molecular beam epitaxy and characterized with a variety of state-of-the-art techniques including variable temperature reflection high energy electron diffraction, low temperature scanning tunneling microscopy and spectroscopy, variable temperature vibrating sample magnetometry, variable temperature neutron diffraction and reflectometry, variable temperature x-ray diffraction, x-ray reflectometry, Rutherford backscattering, Auger electron spectroscopy, and cross-sectional tunneling electron microscopy. The experimental results are furthermore understood by comparing with numerical calculations using generalized gradient approximation, local density approximation with Hubbard correction, Refl1D, and data analysis and visual environment program. In my first research project, I studied Ga gas adatoms on GaN surfaces. We discovered frozen-out gallium gas adatoms on atomically smooth c(6x12) GaN(0001¯) surface using low temperature scanning tunneling microscopy. We identified adsorption sites of the Ga adatoms on c(6x12) reconstructed surface. Their bonding is determined by measuring low unoccupied molecular orbital level. Absorption sites of the Ga gas adatoms on centered 6x12 are identified, and their asymmetric absorption on the chiral domains is investigated. In second project, I investigated magneto-structural phase transition in chromium nitride (CrN) thin films. The CrN thin films are grown by molecular beam epitaxy. Structural and magnetic transition are studied using variable temperature reflection high energy electron diffraction and variable temperature neutron diffraction. We observed a structural phase transition at the surface at 277+/-2 K, and a sharp, first-order magnetic phase transition from paramagnetic (room temperature) to antiferromagnetic (low temperature) at 280+/-3 K. Our experiments suggest that the structural transition in CrN thin films occur in out-of-plane direction, and epitaxial constraints suppress the in-plane transition; therefore, the low temperature crystal structure of CrN is tetragonal. This new model explains our structural and magnetic data at low temperatures, but it is different than the previously published orthorhombic model. In third project, I studied exchange bias and exchange spring effect in MBE grown Fe/CrN bilayer thin films. We grew Fe/CrN bilayer thin films on MgO(001) substrate by molecular beam epitaxy, and studied them using variable temperature vibrating sample magnetometry, polarized neutron reflectometry, x-ray reflectivity, and cross-sectional transmission electron microscopy. We observed exchange bias and exchange spring effect in all bilayer thin films. We studied the relationship of exchange bias, blocking temperature, and coercivity with Fe and CrN layers thicknesses. We used polarized neutron beam reflectometry to see if spins at Fe/CrN interface are pinned. We found a thin ferromagnetically ordered CrN layer at the interface. In my final project, I studied growth of submonolayer Fe islands on CrN thin films. These films are prepared in two stages: first, a CrN layer is grown by MBE and then a submonolayer Fe is deposited at room temperature from a carefully degassed e-beam evaporator. The films are studied at liquid helium temperature using low temperature scanning tunneling microscopy and spectroscopy. Islands are seen in STM images, after the Fe deposition, at the edges as well as at the center of atomically flat CrN terraces. However, numerical calculations performed by our collaborator Ponce-P'erez from Benem'erita Universidad Aut'onoma de Puebla show that the Fe islands are energetically unstable on the surface. The Fe atoms substitute Cr atoms in the surface layer and the Cr atoms comes out and form islands. In order to find out elemental composition of the islands, we attempted to map local density of state by measuring differential conductance spectra as a function of bias voltage using LT-STS. We observed three characteristically different spectra; one in the CrN substrate and two in the islands. The CrN substrate curve has a "U" shape near Fermi level and a peak at ≈ 105 mV. The islands spectra show Kondo-like resonances at Fermi level; some islands produce a peak whereas others produce a dip the dI/dV curves near Fermi level. Further investigations are needed to determine the origin of the peak and dip in the island curves, as well as to find the composition of the islands.

A low energy electron microscopy study of the initial growth, structure, and thermal stability of 4,4'-biphenyldicarboxylic acid domains on Cu(001)

NASA Astrophysics Data System (ADS)

Khokhar, Fawad S.; van Gastel, Raoul; Schwarz, Daniel; Zandvliet, Harold J. W.; Poelsema, Bene

2011-09-01

The growth of 4,4'-biphenyldicarboxylic acid (BDA) on Cu(001) has been studied using low energy electron microscopy and selective area low energy electron diffraction. The emergence of large islands and hydrogen bonding to perpendicularly oriented, adjacent molecules is confirmed. The two benzene rings of adsorbed BDA are twisted along the molecular axis. Unconventional growth of the domains, followed by a second nucleation stage, is observed at room temperature. This unanticipated feature is attributed to the accumulation of stress in the islands. Ostwald ripening in the films and the decay of BDA domains at 448 K exhibits features that are consistent with diffusion limited behavior.

Features of plastic deformation and fracture of dispersion-strengthened V–Cr–Zr–W alloy depending on temperature of tension

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ditenberg, Ivan A.; Grinyaev, Konstantin V.; Tyumentsev, Alexander N.

2015-10-27

Influence of tension temperature on features of plastic deformation and fracture of V–4.23Cr–1.69Zr–7.56W alloy was investigated by scanning and transmission electron microscopy. It is shown that temperature increase leads to activation of the recovery processes, which manifests in the coarsening of microstructure elements, reducing the dislocation density, relaxation of continuous misorientations.

Surface alloying in Sn/Au(111) at elevated temperature

NASA Astrophysics Data System (ADS)

Sadhukhan, Pampa; Singh, Vipin Kumar; Rai, Abhishek; Bhattacharya, Kuntala; Barman, Sudipta Roy

2018-04-01

On the basis of x-ray photoelectron spectroscopy, we show that when Sn is deposited on Au(111) single crystal surface at a substrate temperature TS=373 K, surface alloying occurs with the formation of AuSn phase. The evolution of the surface structure and the surface morphology has been studied by low energy electron diffraction and scanning tunneling microscopy, respectively as a function of Sn coverage and substrate temperatures.

Room temperature ferrimagnetism and ferroelectricity in strained, thin films of BiFe 0.5Mn 0.5O 3

DOE PAGES

Choi, Eun -Mi; Fix, Thomas; Kursumovic, Ahmed; ...

2014-10-14

In this study, highly strained films of BiFe 0.5Mn 0.5O 3 (BFMO) grown at very low rates by pulsed laser deposition were demonstrated to exhibit both ferrimagnetism and ferroelectricity at room temperature and above. Magnetization measurements demonstrated ferrimagnetism (T C ~ 600K), with a room temperature saturation moment (M S) of up to 90 emu/cc (~0.58μ B/f.u) on high quality (001) SrTiO 3. X-ray magnetic circular dichroism showed that the ferrimagnetism arose from antiferromagnetically coupled Fe 3+ and Mn 3+ . While scanning transmission electron microscope studies showed there was no long range ordering of Fe and Mn, the magneticmore » properties were found to be strongly dependent on the strain state in the films. The magnetism is explained to arise from one of three possible mechanisms with Bi polarization playing a key role. A signature of room temperature ferroelectricity in the films was measured by piezoresponse force microscopy and was confirmed using angular dark field scanning transmission electron microscopy. The demonstration of strain induced, high temperature multiferroism is a promising development for future spintronic and memory applications at room temperature and above.« less

Using real-time electron microscopy to explore the effects of transition-metal composition on the local thermal stability in charged Li xNi yMn zCo 1-y-zO 2 cathode materials

DOE PAGES

Hwang, Sooyeon; Kim, Seung Min; Bak, Seong -Min; ...

2015-05-08

In this study, we use in-situ transmission electron microcopy (TEM) to investigate the thermal decomposition that occurs at the surface of charged Li xNi yMn zCo 1-y-zO 2 (NMC) cathode materials of different composition (with y, z=0.8, 0.1 and 0.6, 0.2 and 0.4, 0.3), after they have been charged to their practical upper limit voltage (4.3V). By heating these materials inside the TEM, we are able to directly characterize near surface changes in both their electronic structure (using electron energy loss spectroscopy) and crystal structure and morphology (using electron diffraction and bright-field imaging). The most Ni-rich material (y, z =more » 0.8, 0.1) is found to be thermally unstable at significantly lower temperatures than the other compositions – this is manifested by changes in both the electronic structure and the onset of phase transitions at temperatures as low as 100°C. Electron energy loss spectroscopy indicates that the thermally induced reduction of Ni ions drives these changes, and that this is exacerbated by the presence of an additional redox reaction that occurs at 4.2V in the y, z = 0.8, 0.1 material. Exploration of individual particles shows that there are substantial variations in the onset temperatures and overall extent of these changes. Of the compositions studied, the composition of y, z = 0.6, 0.2 has the optimal combination of high energy density and reasonable thermal stability. The observations herein demonstrate that real time electron microscopy provide direct insight into the changes that occur in cathode materials with temperature, allowing optimization of different alloy concentrations to maximize overall performance.« less

Effect of Annealing Temperature on the Mechanical and Corrosion Behavior of a Newly Developed Novel Lean Duplex Stainless Steel.

PubMed

Guo, Yanjun; Hu, Jincheng; Li, Jin; Jiang, Laizhu; Liu, Tianwei; Wu, Yanping

2014-09-12

The effect of annealing temperature (1000-1150 °C) on the microstructure evolution, mechanical properties, and pitting corrosion behavior of a newly developed novel lean duplex stainless steel with 20.53Cr-3.45Mn-2.08Ni-0.17N-0.31Mo was studied by means of optical metallographic microscopy (OMM), scanning electron microscopy (SEM), magnetic force microscopy (MFM), scanning Kelvin probe force microscopy (SKPFM), energy dispersive X-ray spectroscopy (EDS), uniaxial tensile tests (UTT), and potentiostatic critical pitting temperature (CPT). The results showed that tensile and yield strength, as well as the pitting corrosion resistance, could be degraded with annealing temperature increasing from 1000 up to 1150 °C. Meanwhile, the elongation at break reached the maximum of 52.7% after annealing at 1050 °C due to the effect of martensite transformation induced plasticity (TRIP). The localized pitting attack preferentially occurred at ferrite phase, indicating that the ferrite phase had inferior pitting corrosion resistance as compared to the austenite phase. With increasing annealing temperature, the pitting resistance equivalent number (PREN) of ferrite phase dropped, while that of the austenite phase rose. Additionally, it was found that ferrite possessed a lower Volta potential than austenite phase. Moreover, the Volta potential difference between ferrite and austenite increased with the annealing temperature, which was well consistent with the difference of PREN.

Effect of Annealing Temperature on the Mechanical and Corrosion Behavior of a Newly Developed Novel Lean Duplex Stainless Steel

PubMed Central

Guo, Yanjun; Hu, Jincheng; Li, Jin; Jiang, Laizhu; Liu, Tianwei; Wu, Yanping

2014-01-01

The effect of annealing temperature (1000–1150 °C) on the microstructure evolution, mechanical properties, and pitting corrosion behavior of a newly developed novel lean duplex stainless steel with 20.53Cr-3.45Mn-2.08Ni-0.17N-0.31Mo was studied by means of optical metallographic microscopy (OMM), scanning electron microscopy (SEM), magnetic force microscopy (MFM), scanning Kelvin probe force microscopy (SKPFM), energy dispersive X-ray spectroscopy (EDS), uniaxial tensile tests (UTT), and potentiostatic critical pitting temperature (CPT). The results showed that tensile and yield strength, as well as the pitting corrosion resistance, could be degraded with annealing temperature increasing from 1000 up to 1150 °C. Meanwhile, the elongation at break reached the maximum of 52.7% after annealing at 1050 °C due to the effect of martensite transformation induced plasticity (TRIP). The localized pitting attack preferentially occurred at ferrite phase, indicating that the ferrite phase had inferior pitting corrosion resistance as compared to the austenite phase. With increasing annealing temperature, the pitting resistance equivalent number (PREN) of ferrite phase dropped, while that of the austenite phase rose. Additionally, it was found that ferrite possessed a lower Volta potential than austenite phase. Moreover, the Volta potential difference between ferrite and austenite increased with the annealing temperature, which was well consistent with the difference of PREN. PMID:28788201

A simple method for environmental cell depressurization for use with an electron microscope.

PubMed

Ogawa, Naoki; Mizokawa, Ryo; Saito, Minoru; Ishikawa, Akira

2017-12-01

With the aid of the environmental cell (EC) in electron microscopy, hydrated specimens have been observed at high resolutions that optical microscopy cannot attain. Due to the ultra-high vacuum conditions of the inner column of the electron microscope, the EC requires sealing films that are sufficiently thin to allow electron transmission and that are sufficiently tough to withstand the pressure difference between the inside and outside of the EC. However, most hydrated specimens can be observed at low vacuum because the saturated vapor pressure of water is known to be 0.02 atm at room temperature. These concepts have been used in the differential pumping system, but it is complicated and relatively expensive. In this work, we propose a simple method for depressurization of the EC using a 'balloon structure' and demonstrate the theoretical benefits and practical improvement for specimen observations in low-vacuum conditions. © The Author 2017. Published by Oxford University Press on behalf of The Japanese Society of Microscopy. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

Cryogenic coherent X-ray diffraction imaging of biological samples at SACLA: a correlative approach with cryo-electron and light microscopy.

PubMed

Takayama, Yuki; Yonekura, Koji

2016-03-01

Coherent X-ray diffraction imaging at cryogenic temperature (cryo-CXDI) allows the analysis of internal structures of unstained, non-crystalline, whole biological samples in micrometre to sub-micrometre dimensions. Targets include cells and cell organelles. This approach involves preparing frozen-hydrated samples under controlled humidity, transferring the samples to a cryo-stage inside a vacuum chamber of a diffractometer, and then exposing the samples to coherent X-rays. Since 2012, cryo-coherent diffraction imaging (CDI) experiments have been carried out with the X-ray free-electron laser (XFEL) at the SPring-8 Ångstrom Compact free-electron LAser (SACLA) facility in Japan. Complementary use of cryo-electron microscopy and/or light microscopy is highly beneficial for both pre-checking samples and studying the integrity or nature of the sample. This article reports the authors' experience in cryo-XFEL-CDI of biological cells and organelles at SACLA, and describes an attempt towards reliable and higher-resolution reconstructions, including signal enhancement with strong scatterers and Patterson-search phasing.

Effect of LID (Registered) processing on the microstructure and mechanical properties of Ti-6Al-4V and Ti-6Al-2Sn-4Zr-2Mo titanium foil-gauge materials

NASA Technical Reports Server (NTRS)

Balckburn, Linda B.

1987-01-01

A study was undertaken to determine the mechanical properties and microstructures resulting from Liquid Interface Diffusion (LID -Registered) processing of foil-gauge specimens of Ti-6Al-4V and Ti-6Al-2Sn-4Zr-2Mo coated with varying amounts of LID material. In addition, the effects of various elevated temperature exposures on the concentration profiles of the LID alloying elements were investigated, using specimens with a narrow strip of LID material applied to the surface. Room and elevated temperature tensile properties were determined for both coated and uncoated specimens. Optical microscopy was used to examine alloy microstructures, and scanning electron microscopy to examine fracture surface morphologies. The chemical concentration profiles of the strip-coated specimens were determined with an electron microprobe.

Novel preparation of highly photocatalytically active copper chromite nanostructured material via a simple hydrothermal route

PubMed Central

Beshkar, Farshad; Zinatloo-Ajabshir, Sahar; Bagheri, Samira; Salavati-Niasari, Masoud

2017-01-01

Highly photocatalytically active copper chromite nanostructured material were prepared via a novel simple hydrothermal reaction between [Cu(en)2(H2O)2]Cl2 and [Cr(en)3]Cl3.3H2O at low temperature, without adding any pH regulator or external capping agent. The as-synthesized nanostructured copper chromite was analyzed by transmission electron microscopy (TEM), UV–vis diffuse reflectance spectroscopy, energy dispersive X-ray microanalysis (EDX), scanning electron microscopy (SEM), X-ray diffraction (XRD) and Fourier transform infrared (FT-IR) spectroscopy. Results of the morphological investigation of the as-synthesized products illustrate that the shape and size of the copper chromite depended on the surfactant sort, reaction duration and temperature. Moreover, the photocatalytic behavior of as-obtained copper chromite was evaluated by photodegradation of acid blue 92 (anionic dye) as water pollutant. PMID:28582420

Promising features of low-temperature grown Ge nanostructures on Si(001) substrates

NASA Astrophysics Data System (ADS)

Wang, Ze; Wang, Shuguang; Yin, Yefei; Liu, Tao; Lin, Dongdong; Li, De-hui; Yang, Xinju; Jiang, Zuimin; Zhong, Zhenyang

2017-03-01

High-quality Ge nanostructures are obtained by molecular beam epitaxy of Ge on Si(001) substrates at 200 °C and ex situ annealing at 400 °C. Their structural properties are comprehensively characterized by atomic force microscopy, transmission electron microscopy and Raman spectroscopy. It is disclosed that they are almost defect free except for some defects at the Ge/Si interface and in the subsequent Si capping layer. The misfit strain in the nanostructure is substantially relaxed. Dramatically strong photoluminescence (PL) from the Ge nanostructures is observed. Detailed analyses on the power- and temperature-dependent PL spectra, together with a self-consistent calculation, indicate the confinement and the high quantum efficiency of excitons within the Ge nanostructures. Our results demonstrate that the Ge nanostructures obtained via the present feasible route may have great potential in optoelectronic devices for monolithic optical-electronic integration circuits.

Evidence against a charge density wave on Bi(111)

DOE PAGES

Kim, T. K.; Wells, J.; Kirkegaard, C.; ...

2005-08-18

The Bi(111) surface was studied by scanning tunneling microscopy (STM), transmission electron microscopy (TEM) and angle-resolved photoemission (ARPES) in order to verify the existence of a recently proposed surface charge density wave (CDW). The STM and TEM results to not support a CDW scenario at low temperatures. Thus the quasiparticle interference pattern observed in STM confirms the spin-orbit split character of the surface states which prevents the formation of a CDW, even in the case of good nesting. The dispersion of the electronic states observed with ARPES agrees well with earlier findings. In particular, the Fermi contour of the electronmore » pocket at the centre of the surface Brillouin zone is found to have a hexagonal shape. However, no gap opening or other signatures of a CDW phase transition can be found in the temperature-dependent data.« less

Transmission electron microscopy study of the formation of epitaxial CoSi2/Si (111) by a room-temperature codeposition technique

NASA Technical Reports Server (NTRS)

D'Anterroches, Cecile; Yakupoglu, H. Nejat; Lin, T. L.; Fathauer, R. W.; Grunthaner, P. J.

1988-01-01

Co and Si have been codeposited on Si (111) substrates near room temperature in a stoichiometric 1:2 ratio in a molecular beam epitaxy system. Annealing of these deposits yields high-quality single-crystal CoSi2 layers. Transmission electron microscopy has been used to examine as-deposited layers and layers annealed at 300, 500, and 600 C. Single-crystal epitaxial grains of CoSi2 embedded in a matrix of amorphous Co/Si are observed in as-deposited samples, while the layer is predominantly single-crystal, inhomogeneously strained CoSi2 at 300 C. At 600 C, a homogeneously strained single-crystal layer with a high density of pinholes is observed. In contrast to other solid phase epitaxy techniques used to grow CoSi2 on Si (111), no intermediate silicide phases are observed prior to the formation of CoSi2.

Tungsten-Doped TiO2 Nanolayers with Improved CO2 Gas Sensing Properties for Environmental Applications

NASA Astrophysics Data System (ADS)

Saberi, Maliheh; Ashkarran, Ali Akbar

Tungsten-doped TiO2 gas sensors were successfully synthesized using sol-gel process and spin coating technique. The fabricated sensor was characterized by field emission scanning electron microscopy (FE-SEM), ultraviolet visible (UV-Vis) spectroscopy, transmission electron microscopy (TEM), X-Ray diffraction (XRD) and Fourier transform infrared (FTIR) spectroscopy. Gas sensing properties of pristine and tungsten-doped TiO2 nanolayers (NLs) were probed by detection of CO2 gas. A series of experiments were conducted in order to find the optimum operating temperature of the prepared sensors and also the optimum value of tungsten concentration in TiO2 matrix. It was found that introducing tungsten into the TiO2 matrix enhanced the gas sensing performance. The maximum response was found to be (1.37) for 0.001g tungsten-doped TiO2 NLs at 200∘C as an optimum operating temperature.

Facile synthesis of Ni/NiO@GO nanocomposites and its enhanced dielectric constant

NASA Astrophysics Data System (ADS)

Sarkar, S.; Giri, N.; Mondal, A.; Ray, R.

2018-05-01

Ni/NiO embedded Graphene Oxide (GO): Ni/NiO@GO is synthesized by citric acid assisted Pechini-type method. Structural and morphological characterizations are performed by X-ray powdered diffraction (XRD), field emission scanning electron microscopy (FESEM) and tunneling electron microscopy (TEM). Defects in GO sheets are probed by RAMAN spectroscopy. The temperature variation of dielectric constant (ɛR) and dielectric loss (tan δ) are investigated in the temperature range 300 - 400 K. Decoration of GO with Ni/NiO nanoparticles enhances its ɛR by˜55 times. Moreover, its dielectric constant measured at 5 MHz is found to be˜430 times to that of Ni/NiO along with the reduction of dielectric loss by a factor˜0.5. The enhanced dielectric constant makes the composite Ni/NiO@GO a potential candidate for using in ecologically friendly energy storage devices.

Joining of Silicon Carbide Through the Diffusion Bonding Approach

NASA Technical Reports Server (NTRS)

Halbig, Michael .; Singh, Mrityunjay

2009-01-01

In order for ceramics to be fully utilized as components for high-temperature and structural applications, joining and integration methods are needed. Such methods will allow for the fabrication the complex shapes and also allow for insertion of the ceramic component into a system that may have different adjacent materials. Monolithic silicon carbide (SiC) is a ceramic material of focus due to its high temperature strength and stability. Titanium foils were used as an interlayer to form diffusion bonds between chemical vapor deposited (CVD) SiC ceramics with the aid of hot pressing. The influence of such variables as interlayer thickness and processing time were investigated to see which conditions contributed to bonds that were well adhered and crack free. Optical microscopy, scanning electron microscopy, and electron microprobe analysis were used to characterize the bonds and to identify the reaction formed phases.

Nanoparticles of nickel oxide: growth and organization on zinc-substituted anionic clay matrix by one-pot route at room temperature

NASA Astrophysics Data System (ADS)

Carja, Gabriela; Nakajima, Akira; Dranca, Cristian; Okada, Kiyoshi

2010-10-01

A room temperature nanocarving strategy is developed for the fabrication of nanoparticles of nickel oxide on zinc-substituted anionic clay matrix (Ni/ZnLDH). It is based on the growth and organization of nanoparticles of nickel oxide which occur during the structural reconstruction of the layered structure of the anionic clay in NiSO4 aqueous solution. No organic compounds are used during the fabrication. The described material was characterized by X-ray diffraction (XRD), IR spectroscopy (FTIR), transmission electron microscopy (TEM), field-emission scanning electron microscopy (FESEM), energy dispersive X-ray (EDX) spectroscopy, and X-ray photoelectron spectroscopy (XPS). Results show that the nickel-clay nanoarchitecture consists of small nanoparticles of nickel oxide (average size 7 nm) deposited on the larger nanoparticles (average size 90 nm) of zinc-substituted clay. The optical properties of the new nickel-zinc formulation are studied by UV-Vis.

Preparation and characterization of novel carbon dioxide adsorbents based on polyethylenimine-modified Halloysite nanotubes.

PubMed

Cai, Haohao; Bao, Feng; Gao, Jie; Chen, Tao; Wang, Si; Ma, Rui

2015-01-01

New nano-sized carbon dioxide (CO2) adsorbents based on Halloysite nanotubes impregnated with polyethylenimine (PEI) were designed and synthesized, which were excellent adsorbents for the capture of CO2 at room temperature and had relatively high CO2 adsorption capacity. The prepared adsorbents were characterized by various techniques such as Fourier transform infrared spectrometry, gel permeation chromatography, dynamic light scattering, thermogravimetry, thermogravimetry-Fourier transform-infrared spectrometry, scanning electron microscopy and transmission electron microscopy. The adsorption characteristics and capacity were studied at room temperature, the highest CO2 adsorption capacity of 156.6 mg/g-PEI was obtained and the optimal adsorption capacity can reach a maximum value of 54.8 mg/g-adsorbent. The experiment indicated that this kind of adsorbent has a high stability at 80°C and PEI-impregnated adsorbents showed good reversibility and stability during cyclic adsorption-regeneration tests.

Removal combined with reduction of hexavalent chromium from aqueous solution by Fe-ethylene glycol complex microspheres

NASA Astrophysics Data System (ADS)

Zhang, Yong-Xing; Jia, Yong

2016-12-01

Three-dimensional Fe-ethylene glycol (Fe-EG) complex microspheres were synthesized by a facile hydrothermal method, and were characterized by field emission scanning electron microscopy and transmission electron microscopy. The adsorption as well as reduction properties of the obtained Fe-EG complex microspheres towards Cr(VI) ions were studied. The experiment data of adsorption kinetic and isotherm were fitted by nonlinear regression approach. In neutral condition, the maximum adsorption capacity was 49.78 mg g-1 at room temperature, and was increased with the increasing of temperature. Thermodynamic parameters including the Gibbs free energy, standard enthalpy and standard entropy revealed that adsorption of Cr(VI) was a feasible, spontaneous and endothermic process. Spectroscopic analysis revealed the adsorption of Cr(VI) was a physical adsorption process. The adsorbed CrO42- ions were partly reduced to Cr(OH)3 by Fe(II) ions and the organic groups in the Fe-EG complex.

Probing local work function of electron emitting Si-nanofacets

NASA Astrophysics Data System (ADS)

Basu, Tanmoy; Som, Tapobrata

2017-10-01

Large area, Si-nanofacets are synthesized by obliquely incident low energy Ar+-ion-beam bombardment at room temperature (RT). The field emission properties of such nanofacets are studied based on current-voltage measurements and the Fowler-Nordheim equation. Low turn-on field with relatively high current density is obtained due to the shape and an overall rough morphology. We demonstrate a tunable field emission property from the silicon nanofacets by varying the ion exposure time. Atomic force microscopy (AFM) in conjunction with Kelvin probe force microscopy (KPFM) measurements provide the information on the aspect ratio and confirms the presence of native oxide layer near the apexes of the facets, respectively. The inhomogeneous oxidation leads to an increase in the local work function at the apexes of the facets, restricting the electron emission from the same. Due to its room temperature fabrication, the present method is of great significance to the low-cost vacuum field emission devices fabrication.

Characterization of stress corrosion cracks in Ni-based weld alloys 52, 52M and 152 grown in high-temperature water

DOE Office of Scientific and Technical Information (OSTI.GOV)

Xie, Yi; Wu, Yaqiao; Burns, Jatuporn

Ni-based weld alloys 52, 52M and 152 are extensively used in repair and mitigation of primary water stress corrosion cracking (SCC) in nuclear power plants. In the present study, a series of microstructure and microchemistry at the SCC tips of these alloys were examined with scanning electron microscopy (SEM), electron backscatter diffraction (EBSD), transmission electron microscopy (TEM), energy-dispersive X-ray spectroscopy (EDS), scanning transmission electron microscopy (STEM) and energy filtered transmission electron microscopy (EFTEM). The specimens have similar chemical compositions and testing conditions. Intergranular (IG) and transgranular (TG) SCC was observed in all of them. The cracks were filled with nickel-oxidesmore » and partial precipitations of chrome carbides (CrCs), niobium carbides (NbCs), titanium nitrides (TiNs) and silicon carbides (SiCs), while iron (Fe) was largely dissolved into the solution. However, the crack densities, lengths and distributions were different for all three specimens. - Highlights: • Microstructure and microchemistry at the SCC tips of Ni-based weld alloys 52, 52M and 152 were examined. • The crack densities, lengths and distributions were found to be different for different alloys. • IGSCC and TGSCC were observed on alloy 52, only TGSCC was observed on alloy 52M and 152. • The cracks were filled by Ni-oxides and precipitated CrCs, NbCs, TiNs and SiCs.« less

Viscosity of the liquid Al-6Mg-1Mn-0.2Sc-0.1Zr alloy

NASA Astrophysics Data System (ADS)

Reznik, P. L.; Chikova, O. A.; Tsepelev, V. S.

2017-07-01

The microstructure and the phase composition of as-cast Al-Mg-Mn-Sc-Zr alloy samples are studied by electron microscopy and electron-probe microanalysis. The processes of solidification and melting of this alloy are described. The temperature dependence of the kinematic viscosity of the Al-Mg-Mn-Sc-Zr melts is studied during heating and subsequent cooling of the samples. The measurement results are used to determine the temperature at which inherited microheterogeneities in the melts are destroyed irreversibly.

High temperature irradiation induced creep in Ag nanopillars measured via in situ transmission electron microscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jawaharram, Gowtham Sriram; Price, Patrick M.; Barr, Christopher M.

Irradiation induced creep (IIC) rates are measured in compression on Ag nanopillar (square) beams in the sink-limited regime. The IIC rate increases linearly with stress at lower stresses, i.e. below ≈2/3 the high temperature yield stress and parabolically with pillar width, L, for L less than ≈300 nm. Here, the data are obtained by combining in situ transmission electron imaging with simultaneous ion irradiation, laser heating, and nanopillar compression. Results in the larger width regime are consistent with prior literature.

High temperature irradiation induced creep in Ag nanopillars measured via in situ transmission electron microscopy

DOE PAGES

Jawaharram, Gowtham Sriram; Price, Patrick M.; Barr, Christopher M.; ...

2018-01-30

Irradiation induced creep (IIC) rates are measured in compression on Ag nanopillar (square) beams in the sink-limited regime. The IIC rate increases linearly with stress at lower stresses, i.e. below ≈2/3 the high temperature yield stress and parabolically with pillar width, L, for L less than ≈300 nm. Here, the data are obtained by combining in situ transmission electron imaging with simultaneous ion irradiation, laser heating, and nanopillar compression. Results in the larger width regime are consistent with prior literature.

Influence of Temperature on Corrosion Behavior of 2A02 Al Alloy in Marine Atmospheric Environments

PubMed Central

Cao, Min; Liu, Li; Fan, Lei; Yu, Zhongfen; Li, Ying; Oguzie, Emeka E.; Wang, Fuhui

2018-01-01

The corrosion behavior of 2A02 Al alloy under 4 mg/cm2 NaCl deposition at different temperatures (from 30 to 80 °C) has been studied. This corrosion behavior was researched using mass-gain, scanning electron microscopy-SEM, laser scanning confocal microscopy-LSCM, X-ray photoelectron spectroscopy-XPS and other techniques. The results showed and revealed that the corrosion was maximal at 60 °C after 200 h of exposure. The increase of temperature not only affected the solubility of oxygen gas in the thin film, but also promoted the transport of ions (such as Cl−), and the formation of protective AlO(OH), which further affects the corrosion speed. PMID:29401690

Direct imaging of coexisting ordered and frustrated sublattices in artificial ferromagnetic quasicrystals

DOE PAGES

Farmer, B.; Bhat, V. S.; Balk, A.; ...

2016-04-25

Here, we have used scanning electron microscopy with polarization analysis and photoemission electron microscopy to image the two-dimensional magnetization of permalloy films patterned into Penrose P2 tilings (P2T). The interplay of exchange interactions in asymmetrically coordinated vertices and short-range dipole interactions among connected film segments stabilize magnetically ordered, spatially distinct sublattices that coexist with frustrated sublattices at room temperature. Numerical simulations that include long-range dipole interactions between sublattices agree with images of as-grown P2T samples and predict a magnetically ordered ground state for a two-dimensional quasicrystal lattice of classical Ising spins.

Micelle-assisted fabrication of necklace-shaped assembly of inorganic fullerene-like molybdenum disulfide nanospheres

NASA Astrophysics Data System (ADS)

Xiong, Yujie; Xie, Yi; Li, Zhengquan; Li, Xiaoxu; Zhang, Rong

2003-11-01

The fabrication of necklace-shaped assembly of inorganic fullerene-like molybdenum disulfide nanospheres via a micelle-assisted route is reported, in which necklace-shaped assembly of amorphous MoS 3 nanospheres is driven by the aggregation transformation of surfactants at low temperatures and then is transformed to the assembly of target fullerene-like MoS 2 by annealing. This nanostructure is a type of oriented assembly of inorganic fullerene-like structures, which is confirmed by the transmission electron microscopy and high-resolution transmission electron microscopy analysis. The optical absorption property is investigated to show their inorganic fullerene-like structure and uniform shape.

One-Pot Silver Nanoring Synthesis

NASA Astrophysics Data System (ADS)

Drogat, Nicolas; Granet, Robert; Sol, Vincent; Krausz, Pierre

2010-03-01

Silver colloidal nanorings have been synthesized by reducing silver ions with NaBH4 in trisodium citrate buffers. pH increase, by addition of NaOH, was used to speed up reduction reaction. The UV-vis absorption spectra of resulting silver nanorings showed two peaks accounting for transverse and longitudinal surface plasmon resonance, at ≈400 nm, and between 600 and 700 nm, respectively. The shapes of these silver nanoparticles (nanorings) depended on AgNO3/NaBH4 ratio, pH and reaction temperature. Particles were analysed by transmission electron microscopy, scanning electron microscopy and X-ray diffraction. A reaction pathway is proposed to explain silver nanoring formation.

One-pot silver nanoring synthesis.

PubMed

Drogat, Nicolas; Granet, Robert; Sol, Vincent; Krausz, Pierre

2009-12-16

Silver colloidal nanorings have been synthesized by reducing silver ions with NaBH4 in trisodium citrate buffers. pH increase, by addition of NaOH, was used to speed up reduction reaction. The UV-vis absorption spectra of resulting silver nanorings showed two peaks accounting for transverse and longitudinal surface plasmon resonance, at ≈400 nm, and between 600 and 700 nm, respectively. The shapes of these silver nanoparticles (nanorings) depended on AgNO3/NaBH4 ratio, pH and reaction temperature. Particles were analysed by transmission electron microscopy, scanning electron microscopy and X-ray diffraction. A reaction pathway is proposed to explain silver nanoring formation.

One-Pot Silver Nanoring Synthesis

PubMed Central

2010-01-01

Silver colloidal nanorings have been synthesized by reducing silver ions with NaBH4 in trisodium citrate buffers. pH increase, by addition of NaOH, was used to speed up reduction reaction. The UV–vis absorption spectra of resulting silver nanorings showed two peaks accounting for transverse and longitudinal surface plasmon resonance, at ≈400 nm, and between 600 and 700 nm, respectively. The shapes of these silver nanoparticles (nanorings) depended on AgNO3/NaBH4 ratio, pH and reaction temperature. Particles were analysed by transmission electron microscopy, scanning electron microscopy and X-ray diffraction. A reaction pathway is proposed to explain silver nanoring formation. PMID:20672109

Electroperturbation of human stratum corneum fine structure by high voltage pulses: a freeze-fracture electron microscopy and differential thermal analysis study.

PubMed

Jadoul, A; Tanojo, H; Préat, V; Bouwstra, J A; Spies, F; Boddé, H E

1998-08-01

Application of high voltage pulses (HVP) to the skin has been shown to promote the transdermal drug delivery by a mechanism involving skin electroporation. The aim of this study was to detect potential changes in lipid phase and ultrastructure induced in human stratum corneum by various HVP protocols, using differential thermal analysis and freeze-fracture electron microscopy. Due to the time involved between the moment the electric field is switched off and the analysis, only "secondary" phenomena rather than primary events could be observed. A decrease in enthalpies for the phase transitions observed at 70 degrees C and 85 degrees C was detected by differential thermal analysis after HVP treatment. No changes in transition temperature could be seen. The freeze-fracture electron microscopy study revealed a dramatic perturbation of the lamellar ordering of the intercellular lipid after application of HVP. Most of the planes displayed rough surfaces. The lipid lamellae exhibited rounded off steps or a vanished stepwise order. There was no evidence for perturbation of the corneocytes content. In conclusion, the freeze-fracture electron microscopy and differential thermal analysis studies suggest that HVP application induces a general perturbation of the stratum corneum lipid ultrastructure.

Viewing Integrated-Circuit Interconnections By SEM

NASA Technical Reports Server (NTRS)

Lawton, Russel A.; Gauldin, Robert E.; Ruiz, Ronald P.

1990-01-01

Back-scattering of energetic electrons reveals hidden metal layers. Experiment shows that with suitable operating adjustments, scanning electron microscopy (SEM) used to look for defects in aluminum interconnections in integrated circuits. Enables monitoring, in situ, of changes in defects caused by changes in temperature. Gives truer picture of defects, as etching can change stress field of metal-and-passivation pattern, causing changes in defects.

Chemical synthesis of oriented ferromagnetic LaSr-2 × 4 manganese oxide molecular sieve nanowires

DOE Office of Scientific and Technical Information (OSTI.GOV)

Carretero-Genevrier, Adrián; Gazquez, Jaume; Magen, Cesar

2012-04-25

Here we report a chemical solution based method using nanoporous track-etched polymer templates for producing long and oriented LaSr-2 × 4 manganese oxide molecular sieve nanowires. Scanning transmission electron microscopy and electron energy loss spectroscopy analyses show that the nanowires are ferromagnetic at room temperature, single crystalline, epitaxially grown and self-aligned.

Inducing fluorescence of uranyl acetate as a dual-purpose contrast agent for correlative light-electron microscopy with nanometre precision.

PubMed

Tuijtel, Maarten W; Mulder, Aat A; Posthuma, Clara C; van der Hoeven, Barbara; Koster, Abraham J; Bárcena, Montserrat; Faas, Frank G A; Sharp, Thomas H

2017-09-05

Correlative light-electron microscopy (CLEM) combines the high spatial resolution of transmission electron microscopy (TEM) with the capability of fluorescence light microscopy (FLM) to locate rare or transient cellular events within a large field of view. CLEM is therefore a powerful technique to study cellular processes. Aligning images derived from both imaging modalities is a prerequisite to correlate the two microscopy data sets, and poor alignment can limit interpretability of the data. Here, we describe how uranyl acetate, a commonly-used contrast agent for TEM, can be induced to fluoresce brightly at cryogenic temperatures (-195 °C) and imaged by cryoFLM using standard filter sets. This dual-purpose contrast agent can be used as a general tool for CLEM, whereby the equivalent staining allows direct correlation between fluorescence and TEM images. We demonstrate the potential of this approach by performing multi-colour CLEM of cells containing equine arteritis virus proteins tagged with either green- or red-fluorescent protein, and achieve high-precision localization of virus-induced intracellular membrane modifications. Using uranyl acetate as a dual-purpose contrast agent, we achieve an image alignment precision of ~30 nm, twice as accurate as when using fiducial beads, which will be essential for combining TEM with the evolving field of super-resolution light microscopy.

A Fast Response Ammonia Sensor Based on Coaxial PPy-PAN Nanofiber Yarn.

PubMed

Liu, Penghong; Wu, Shaohua; Zhang, Yue; Zhang, Hongnan; Qin, Xiaohong

2016-06-23

Highly orientated polypyrrole (PPy)-coated polyacrylonitrile (PAN) (PPy-PAN) nanofiber yarn was prepared with an electrospinning technique and in-situ chemical polymerization. The morphology and chemical structure of PPy-PAN nanofiber yarn was characterized by scanning electron microscopy (SEM), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), and fourier transform infrared spectroscopy (FTIR), which indicated that the PPy as the shell layer was homogeneously and uniformly polymerized on the surface of PAN nanofiber. The effects of different concentration of doping acid on the responses of PPy-PAN nanofiber yarn sensor were investigated. The electrical responses of the gas sensor based on the PPy-PAN nanofiber yarn to ammonia were investigated at room temperature. The nanoyarn sensor composed of uniaxially aligned PPy-PAN nanofibers with a one-dimensional structure exhibited a transient response, and the response time was less than 1 s. The excellent sensing properties mentioned above give rise to good potential application prospects in the field of ammonia sensor.

4D imaging of transient structures and morphologies in ultrafast electron microscopy.

PubMed

Barwick, Brett; Park, Hyun Soon; Kwon, Oh-Hoon; Baskin, J Spencer; Zewail, Ahmed H

2008-11-21

With advances in spatial resolution reaching the atomic scale, two-dimensional (2D) and 3D imaging in electron microscopy has become an essential methodology in various fields of study. Here, we report 4D imaging, with in situ spatiotemporal resolutions, in ultrafast electron microscopy (UEM). The ability to capture selected-area-image dynamics with pixel resolution and to control the time separation between pulses for temporal cooling of the specimen made possible studies of fleeting structures and morphologies. We demonstrate the potential for applications with two examples, gold and graphite. For gold, after thermally induced stress, we determined the atomic structural expansion, the nonthermal lattice temperature, and the ultrafast transients of warping/bulging. In contrast, in graphite, striking coherent transients of the structure were observed in both image and diffraction, directly measuring, on the nanoscale, the longitudinal resonance period governed by Young's elastic modulus. The success of these studies demonstrates the promise of UEM in real-space imaging of dynamics.

Momentum microscopy of ? single crystals with detailed surface characterisation

NASA Astrophysics Data System (ADS)

Ellguth, M.; Tusche, C.; Iga, F.; Suga, S.

2016-11-01

We report the in situ preparation of surfaces of the proposed topological Kondo insulator SmB? by controlled cycles of Ar ion sputtering and annealing. The procedure provides a reproducible way for the preparation of Sm- or B-rich surface terminations by low (?1080 ?C) or high (?1200 ?C) temperature annealing. The surface quality and termination were checked by low energy electron diffraction and Auger electron spectroscopy. Photoemission studies were carried out using momentum microscopy and two laboratory light sources providing polarised radiation with an energy of 6 eV (fourth harmonic of a pulsed Ti:Sapphire laser) and unpolarised radiation with an energy of 21.2 eV (He-I line of a gas discharge lamp). Full dispersions of electronic states in a wide two-dimensional momentum space were obtained by momentum microscopy from the in situ prepared Sm-terminated surface. The shape of the Fermi surface is discussed based on the sections through the bulk Brillouin zone sampled by the different photon energies.

Magnetic resonance force microscopy of paramagnetic electron spins at millikelvin temperatures.

PubMed

Vinante, A; Wijts, G; Usenko, O; Schinkelshoek, L; Oosterkamp, T H

2011-12-06

Magnetic resonance force microscopy (MRFM) is a powerful technique to detect a small number of spins that relies on force detection by an ultrasoft magnetically tipped cantilever and selective magnetic resonance manipulation of the spins. MRFM would greatly benefit from ultralow temperature operation, because of lower thermomechanical noise and increased thermal spin polarization. Here we demonstrate MRFM operation at temperatures as low as 30 mK, thanks to a recently developed superconducting quantum interference device (SQUID)-based cantilever detection technique, which avoids cantilever overheating. In our experiment, we detect dangling bond paramagnetic centres on a silicon surface down to millikelvin temperatures. Fluctuations of such defects are supposedly linked to 1/f magnetic noise and decoherence in SQUIDs, as well as in several superconducting and single spin qubits. We find evidence that spin diffusion has a key role in the low-temperature spin dynamics.

Report on the Installation and Preparedness of a Protochips Fusion in-situ Heating Holder for TEM

DOE Office of Scientific and Technical Information (OSTI.GOV)

Edmondson, Philip D.

2017-03-01

This brief report documents the procurement and installation of a Protochips Fusion (formerly Aduro) high-temperature, high stability transmission electron microscopy (TEM) specimen holder that allows for the high spatial resolution characterization of material specimens at high temperature in situ of an electron microscope. This specimen holder was specifically procured for use with The FEI Talos F200X Scanning/Transmission Electron Microscope (STEM) in Oak Ridge National Laboratory’s (ORNL’s) Low Activation Materials Development and Analysis (LAMDA) Laboratory. The Protochips Fusion holder will enable high-resolution structural and chemical analysis of irradiated materials at high temperature, becoming a unique capability worldwide, and would encourage high-qualitymore » in situ experiments to be conducted on irradiated materials.« less

Ab initio structure determination of nanocrystals of organic pharmaceutical compounds by electron diffraction at room temperature using a Timepix quantum area direct electron detector

DOE Office of Scientific and Technical Information (OSTI.GOV)

Genderen, E. van; Clabbers, M. T. B.; Center for Cellular Imaging and NanoAnalytics

A specialized quantum area detector for electron diffraction studies makes it possible to solve the structure of small organic compound nanocrystals in non-cryo conditions by direct methods. Until recently, structure determination by transmission electron microscopy of beam-sensitive three-dimensional nanocrystals required electron diffraction tomography data collection at liquid-nitrogen temperature, in order to reduce radiation damage. Here it is shown that the novel Timepix detector combines a high dynamic range with a very high signal-to-noise ratio and single-electron sensitivity, enabling ab initio phasing of beam-sensitive organic compounds. Low-dose electron diffraction data (∼0.013 e{sup −} Å{sup −2} s{sup −1}) were collected at roommore » temperature with the rotation method. It was ascertained that the data were of sufficient quality for structure solution using direct methods using software developed for X-ray crystallography (XDS, SHELX) and for electron crystallography (ADT3D/PETS, SIR2014)« less

Metallic interconnects for SOFC: Characterisation of corrosion resistance and conductivity evaluation at operating temperature of differently coated alloys

NASA Astrophysics Data System (ADS)

Fontana, S.; Amendola, R.; Chevalier, S.; Piccardo, P.; Caboche, G.; Viviani, M.; Molins, R.; Sennour, M.

One of challenges in improving the performance and cost-effectiveness of solid oxide fuel cells (SOFCs) is the development of suitable interconnect materials. Recent researches have enabled to decrease the operating temperature of the SOFC from 1000 to 800 °C. Chromia forming alloys are then among the best candidates for interconnects. However, low electronic conductivity and volatility of chromium oxide scale need to be solved to improve interconnect performances. In the field of high temperature oxidation of metals, it is well known that the addition of reactive element into alloys or as thin film coatings, improves their oxidation resistance at high temperature. The elements of beginning of the lanthanide group and yttrium are the most efficient. The goal of this study is to make reactive element oxides (La 2O 3, Nd 2O 3 and Y 2O 3) coatings by metal organic chemical vapour deposition (MOCVD) on Crofer 22 APU, AL 453 and Haynes 230 in order to form perovskite oxides which present a good conductivity at high temperature. The coatings were analysed after 100 h ageing at 800 °C in air under atmospheric pressure by scanning electron microscopy (SEM), energy dispersive X-ray (EDX) analyses, X-ray diffraction (XRD) and transmission electron microscopy (TEM) analyses. Area-specific resistance (ASR) was measured in air for the same times and temperature, using a sandwich technique with Pt paste for electrical contacts between surfaces. The ASR values for the best coating were estimated to be limited to 0.035 Ω cm 2, even after 40,000 h use.

Characterization of Micro-arc Oxidation Coatings on 6N01 Aluminum Alloy Under Different Electrolyte Temperature Control Modes

NASA Astrophysics Data System (ADS)

Wang, Xuefei; Zhu, Zongtao; Li, Yuanxing; Chen, Hui

2018-03-01

The micro-arc oxidation coatings of 6N01 aluminum alloy produced under different control modes of the electrolyte temperature are discussed in detail. Compared to those coated by a thermostatically controlled treatment, the coatings had different surface characterizations when they were coated without controlling the electrolyte temperature, particularly after treatment involving boiling electrolytes. Scanning electron microscopy and confocal laser scanning microscopy were used to observe the morphology of the coatings. Energy-dispersive spectrometry and x-ray diffractometer were used to characterize their elemental and crystalline phase compositions. The results indicate that the treatment without a controlled electrolyte temperature ultimately led to a thicker and rougher film with a respectably thick inner barrier film, a lower content of γ-Al2O3 and better corrosion resistance.

Effect of Boron and Titanium Addition on the Hot Ductility of Low-Carbon Nb-Containing Steel

NASA Astrophysics Data System (ADS)

Liu, Wei-Jian; Li, Jing; Shi, Cheng-Bin; Huo, Xiang-Dong

2015-12-01

The effect of boron and titanium addition on the hot ductility of Nb-containing steel was investigated using hot tensile tests. The fracture surface and the quenched longitudinal microstructure were examined by optical microscopy (OM), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The results showed that both steel samples had the similar change from 1,100°C to 700°C. The hot ductility of Nb-containing steel with boron and titanium addition was higher than the steel without boron and titanium in the temperature range of 900-750°C. Because the formation of intergranular ferrite was inhibited by solute boron segregating on the grain boundary, the formation of TiN changed the distribution of Nb- and boron-containing precipitates and improved the amount of intragranular ferrite.

Optical and electrical properties of Cu-based all oxide semi-transparent photodetector

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kim, Hong-Sik; Patel, Malkeshkumar; Yadav, Pankaj

2016-09-05

Zero-bias operating Cu oxide-based photodetector was achieved by using large-scale available sputtering method. Cu oxide (Cu{sub 2}O or CuO) was used as p-type transparent layer to form a heterojunction by contacting n-type ZnO layer. All metal-oxide materials were employed to realize transparent device at room temperature and showed a high transparency (>75% at 600 nm) with excellent photoresponses. The structural, morphological, optical, and electrical properties of Cu oxides of CuO and Cu{sub 2}O are evaluated in depth by UV-visible spectrometer, X-ray diffraction, scanning electron microscopy, atomic force microscopy, Kelvin probe force microscopy, and Hall measurements. We may suggest a route ofmore » high-functional Cu oxide-based photoelectric devices for the applications in flexible and transparent electronics.« less

Catalyst–substrate interaction and growth delay in vapor–liquid–solid nanowire growth

NASA Astrophysics Data System (ADS)

Kolíbal, Miroslav; Pejchal, Tomáš; Musálek, Tomáš; Šikola, Tomáš

2018-05-01

Understanding of the initial stage of nanowire growth on a bulk substrate is crucial for the rational design of nanowire building blocks in future electronic and optoelectronic devices. Here, we provide in situ scanning electron microscopy and Auger microscopy analysis of the initial stage of Au-catalyzed Ge nanowire growth on different substrates. Real-time microscopy imaging and elementally resolved spectroscopy clearly show that the catalyst dissolves the underlying substrate if held above a certain temperature. If the substrate dissolution is blocked (or in the case of heteroepitaxy) the catalyst needs to be filled with nanowire material from the external supply, which significantly increases the initial growth delay. The experiments presented here reveal the important role of the substrate in metal-catalyzed nanowire growth and pave the way for different growth delay mitigation strategies.

Catalyst-substrate interaction and growth delay in vapor-liquid-solid nanowire growth.

PubMed

Kolíbal, Miroslav; Pejchal, Tomáš; Musálek, Tomáš; Šikola, Tomáš

2018-05-18

Understanding of the initial stage of nanowire growth on a bulk substrate is crucial for the rational design of nanowire building blocks in future electronic and optoelectronic devices. Here, we provide in situ scanning electron microscopy and Auger microscopy analysis of the initial stage of Au-catalyzed Ge nanowire growth on different substrates. Real-time microscopy imaging and elementally resolved spectroscopy clearly show that the catalyst dissolves the underlying substrate if held above a certain temperature. If the substrate dissolution is blocked (or in the case of heteroepitaxy) the catalyst needs to be filled with nanowire material from the external supply, which significantly increases the initial growth delay. The experiments presented here reveal the important role of the substrate in metal-catalyzed nanowire growth and pave the way for different growth delay mitigation strategies.

Low dimensional CH3NH3PbBr3 cubes for persistent luminescence: Energy variation of electron excitation

NASA Astrophysics Data System (ADS)

Besral, N.; Paul, T.; Thakur, S.; Sarkar, S.; Sardar, K.; Chanda, K.; Das, A.; Chattopadhyay, K. K.

2018-04-01

The impact of varying electron beam voltage upon room temperature CL (cathodoluminescence) properties of crystalline organic-inorganic lead halide perovskite CH3NH3PbBr3 (Methylammonium lead tribromide) microcubes have been studied. CH3NH3PbBr3 microcubes were synthesized at room temperature by a very straight forward wet chemical route. After preliminary characterizations like XRD (X-ray diffraction), FESEM (Field emission scanning electron microscopy), UV-Vis spectroscopy, CL study at three different beam voltages i.e. 5 kV, 10 kV and 15 kV respectively was performed at room temperature. Prominent emission signals were obtained with emission peaks at 2.190 eV (FWHM 0.120 eV), 2.222 eV (FWHM 0.108 eV) and 2.242 eV (FWHM 0.095 eV) for electron beam voltages 5 kV, 10 kV and 15 kV respectively.

Cu incorporated amorphous diamond like carbon (DLC) composites: An efficient electron field emitter over a wide range of temperature

NASA Astrophysics Data System (ADS)

Ahmed, Sk Faruque; Alam, Md Shahbaz; Mukherjee, Nillohit

2018-03-01

The effect of temperature on the electron field emission properties of copper incorporated amorphous diamond like carbon (a-Cu:DLC) thin films have been reported. The a-Cu:DLC thin films have been deposited on indium tin oxide (ITO) coated glass and silicon substrate by the radio frequency sputtering process. The chemical composition of the films was investigated using X-ray photoelectron spectroscopy and the micro structure was established using high resolution transmission electron microscopy. The sp2 and sp3 bonding ratio in the a-Cu:DLC have been analyzed by the Fourier transformed infrared spectroscopy studies. The material showed excellent electron field emission properties; which was optimized by varying the copper atomic percentage and temperature of the films. It was found that the threshold field and effective emission barrier were reduced significantly by copper incorporation as well as temperature and a detailed explanation towards emission mechanism has been provided.

Investigating local degradation and thermal stability of charged nickel-based cathode materials through real-time electron microscopy.

PubMed

Hwang, Sooyeon; Kim, Seung Min; Bak, Seong-Min; Cho, Byung-Won; Chung, Kyung Yoon; Lee, Jeong Yong; Chang, Wonyoung; Stach, Eric A

2014-09-10

In this work, we take advantage of in situ transmission electron microscopy (TEM) to investigate thermally induced decomposition of the surface of Li(x)Ni(0.8)Co(0.15)Al(0.05)O2 (NCA) cathode materials that have been subjected to different states of charge (SOC). While uncharged NCA is stable up to 400 °C, significant changes occur in charged NCA with increasing temperature. These include the development of surface porosity and changes in the oxygen K-edge electron energy loss spectra, with pre-edge peaks shifting to higher energy losses. These changes are closely related to O2 gas released from the structure, as well as to phase changes of NCA from the layered structure to the disordered spinel structure, and finally to the rock-salt structure. Although the temperatures where these changes initiate depend strongly on the state of charge, there also exist significant variations among particles with the same state of charge. Notably, when NCA is charged to x = 0.33 (the charge state that is the practical upper limit voltage in most applications), the surfaces of some particles undergo morphological and oxygen K-edge changes even at temperatures below 100 °C, a temperature that electronic devices containing lithium ion batteries (LIB) can possibly see during normal operation. Those particles that experience these changes are likely to be extremely unstable and may trigger thermal runaway at much lower temperatures than would be usually expected. These results demonstrate that in situ heating experiments are a unique tool not only to study the general thermal behavior of cathode materials but also to explore particle-to-particle variations, which are sometimes of critical importance in understanding the performance of the overall system.

Thermal stability of intermetallic phases in Fe-rich Fe-Cr-Ni-Mo alloys

DOE PAGES

Yang, Ying; Tan, Lizhen; Busby, Jeremy T.

2015-06-12

Understanding the stability of precipitate phases in the Fe-rich Fe-Cr-Ni-Mo alloys is critical to the alloy design and application of Mo-containing Austenitic steels. Coupled with thermodynamic modeling, stability of the chi and Laves phases in two Fe-Cr-Ni-Mo alloys were investigated at 1000, 850 and 700 °C for different annealing time. The morphologies, compositions and crystal structures of the matrix and precipitate phases were carefully examined by Scanning Electron Microscopy, Electron Probe Microanalysis, X-ray diffraction and Transmission Electron Microscopy. The two key findings resulted from this work. One is that the chi phase is stable at high temperature and transformed intomore » the Laves phase at low temperature. The other is that both the chi and Laves phases have large solubilites of Cr, Mo and Ni, among which the Mo solubility has a major role on the relative stability of the precipitate phases. The developed thermodynamic models were then applied to evaluating the Mo effect on the stability of precipitate phases in AISI 316 and NF709 alloys.« less

Room temperature synthesis of silver nanowires from tabular silver bromide crystals in the presence of gelatin

NASA Astrophysics Data System (ADS)

Liu, Suwen; Wehmschulte, Rudolf J.; Lian, Guoda; Burba, Christopher M.

2006-03-01

Long silver nanowires were synthesized at room temperature by a simple and fast process derived from the development of photographic films. A film consisting of an emulsion of tabular silver bromide grains in gelatin was treated with a photographic developer (4-(methylamino)phenol sulfate (metol), citric acid) in the presence of additional aqueous silver nitrate. The silver nanowires have lengths of more than 50 μm, some even more than 100 μm, and average diameters of about 80 nm. Approximately, 70% of the metallic silver formed in the reduction consists of silver nanowires. Selected area electron diffraction (SAED) results indicate that the silver nanowires grow along the [111] direction. It was found that the presence of gelatin, tabular silver bromide crystals and silver ions in solution are essential for the formation of the silver nanowires. The nanowires appear to originate from the edges of the silver bromide crystals. They were characterized by transmission electron microscopy (TEM), SAED, scanning electron microscopy (SEM), and powder X-ray diffraction (XRD).

Room temperature synthesis of silver nanowires from tabular silver bromide crystals in the presence of gelatin

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liu Suwen; Wehmschulte, Rudolf J.; Lian Guoda

2006-03-15

Long silver nanowires were synthesized at room temperature by a simple and fast process derived from the development of photographic films. A film consisting of an emulsion of tabular silver bromide grains in gelatin was treated with a photographic developer (4-(methylamino)phenol sulfate (metol), citric acid) in the presence of additional aqueous silver nitrate. The silver nanowires have lengths of more than 50 {mu}m, some even more than 100 {mu}m, and average diameters of about 80 nm. Approximately, 70% of the metallic silver formed in the reduction consists of silver nanowires. Selected area electron diffraction (SAED) results indicate that the silvermore » nanowires grow along the [111] direction. It was found that the presence of gelatin, tabular silver bromide crystals and silver ions in solution are essential for the formation of the silver nanowires. The nanowires appear to originate from the edges of the silver bromide crystals. They were characterized by transmission electron microscopy (TEM), SAED, scanning electron microscopy (SEM), and powder X-ray diffraction (XRD)« less

Investigation on the storage of benzotriazole corrosion inhibitor in TiO2 nanotube

NASA Astrophysics Data System (ADS)

Nguyen, Thi Dieu Hang; Tiep Nong, Thanh; Quang Nguyen, Van; Quyen Nguyen, The; Le, Quang Trung

2018-06-01

The present paper describes different methods for storing the benzotriazole (BTA) corrosion inhibitor in the titanium dioxide nanotubes (TNT) as nanocontainers. Three methods were used, including the vacuum impregnation at ambient temperature, the vacuum impregnation at cooling temperature () and the rotary vacuum evaporation. TNT, BTA and BTA/TNT products were characterized using scanning electron microscopy (SEM), transmission electron microscopy (TEM), Brunauer-Emmett-Teller (BET) surface area, differential scanning calorimetry (DSC), thermogravimetric analysis (TGA) and Fourier transform infrared (FT-IR) spectroscopy. nanotube powder was synthesized by hydrothermal treatment from the inexpensive spherical commercial precursor. The results obtained from SEM, TEM images and BET values showed the successful synthesis of TNT with a homogeneous morphology of nano size tubes and a large specific surface . The existence of BTA in TNT was demonstrated. The BTA/TNT obtained via the rotary vacuum evaporation contained a very significant amount of BTA (66.6 weight %) but BTA existed mostly outside the nanotubes. Two processes of vacuum impregnation at ambient temperature and vacuum impregnation at cooling temperature revealed that there was about 8 weight % BTA stored in BTA/TNT product and BTA was present mostly inside the nanotubes.

Temperature and pH effect on reduction of graphene oxides in aqueous solution

NASA Astrophysics Data System (ADS)

Tai, Guoan; Zeng, Tian; Li, Hongxiang; Liu, Jinsong; Kong, Jizhou; Lv, Fuyong

2014-09-01

Reduced graphene oxides (RGOs) have usually been obtained by hydrazine reduction, but hydrazine-related compounds are corrosive, highly flammable and very hazardous, and the obtained RGOs heavily aggregated. Here we investigated extensively the effect of temperature and pH value on the structure of RGOs in hydrothermal environments without any reducing agents. The attenuated total reflectance Fourier transform infrared (ATR-FTIR) spectra showed that reduction rate of GOs remarkably increased with the temperature from 100 to 180 °C and with pH value from 3 to 10. Field emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM) exhibited the structural transition of the RGOs. Energy-dispersive x-ray analysis (EDX) showed the reduction degree of the RGO samples quantitatively. The results demonstrate that the GOs can be reduced controllably by a hydrothermal reduction process at pH value of 10 at 140 °C, and the large-scale RGOs are cut into small nanosheets with size from several to a few tens of nanometers with increasing temperature and duration. This study provides a feasible approach to controllably reduce GO with different nanostructures such as porous structures and quantum dots for applications in optoelectronics and biomedicals.

All zinc-blende GaAs/(Ga,Mn)As core-shell nanowires with ferromagnetic ordering.

PubMed

Yu, Xuezhe; Wang, Hailong; Pan, Dong; Zhao, Jianhua; Misuraca, Jennifer; von Molnár, Stephan; Xiong, Peng

2013-04-10

Combining self-catalyzed vapor-liquid-solid growth of GaAs nanowires and low-temperature molecular-beam epitaxy of (Ga,Mn)As, we successfully synthesized all zinc-blende (ZB) GaAs/(Ga,Mn)As core-shell nanowires on Si(111) substrates. The ZB GaAs nanowire cores are first fabricated at high temperature by utilizing the Ga droplets as the catalyst and controlling the triple phase line nucleation, then the (Ga,Mn)As shells are epitaxially grown on the side facets of the GaAs core at low temperature. The growth window for the pure phase GaAs/(Ga,Mn)As core-shell nanowires is found to be very narrow. Both high-resolution transmission electron microscopy and scanning electron microscopy observations confirm that all-ZB GaAs/(Ga,Mn)As core-shell nanowires with smooth side surface are obtained when the Mn concentration is not more than 2% and the growth temperature is 245 °C or below. Magnetic measurements with different applied field directions provide strong evidence for ferromagnetic ordering in the all-ZB GaAs/(Ga,Mn)As nanowires. The hybrid nanowires offer an attractive platform to explore spin transport and device concepts in fully epitaxial all-semiconductor nanospintronic structures.

Synthesis and thermal stability of W/WS{sub 2} inorganic fullerene-like nanoparticles with core-shell structure

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chang Lianxia; Yang Haibin; Fu Wuyou

W/WS{sub 2} inorganic fullerene-like (IF) nanoparticles with core-shell structure are synthesized by the reaction of tungsten nanospheres and sulfur at relatively low temperatures (380-600 deg. C) under hydrogen atmosphere, in which tungsten nanospheres were prepared by wire electrical explosion method. Images of transmission electron microscopy and high-resolution transmission electron microscopy show that the composite particles are of core-shell structure with spherical shape and the shell thickness is about 10 nm. X-ray powder diffraction results indicate that the interlayer spacing of IF-WS{sub 2} shell decreases and approaches that of 2H-WS{sub 2} with increasing annealing temperatures, representing an expansion of 3.3-1.6%. Amore » mechanism of IF-WS{sub 2} formation via sulfur diffusion into fullerene nanoparticles is discussed. Thermal analysis shows that the nanoparticles obtained at different temperatures exhibit similar thermal stability and the onset temperature of oxidization is about 410 deg. C. Encapsulating hard tungsten core into IF-WS{sub 2} and the spherical shape of the core-shell structures may enhance their performance in tribological applications.« less

TEM/STEM study of Zircaloy-2 with protective FeAl(Cr) layers under simulated BWR environment and high-temperature steam exposure

NASA Astrophysics Data System (ADS)

Park, Donghee; Mouche, Peter A.; Zhong, Weicheng; Mandapaka, Kiran K.; Was, Gary S.; Heuser, Brent J.

2018-04-01

FeAl(Cr) thin-film depositions on Zircaloy-2 were studied using transmission electron microscopy (TEM) and scanning transmission electron microscopy (STEM) with respect to oxidation behavior under simulated boiling water reactor (BWR) conditions and high-temperature steam. Columnar grains of FeAl with Cr in solid solution were formed on Zircaloy-2 coupons using magnetron sputtering. NiFe2O4 precipitates on the surface of the FeAl(Cr) coatings were observed after the sample was exposed to the simulated BWR environment. High-temperature steam exposure resulted in grain growth and consumption of the FeAl(Cr) layer, but no delamination at the interface. Outward Al diffusion from the FeAl(Cr) layer occurred during high-temperature steam exposure (700 °C for 3.6 h) to form a 100-nm-thick alumina oxide layer, which was effective in mitigating oxidation of the Zircaloy-2 coupons. Zr intermetallic precipitates formed near the FeAl(Cr) layer due to the inward diffusion of Fe and Al. The counterflow of vacancies in response to the Al and Fe diffusion led to porosity within the FeAl(Cr) layer.

Scanning-electron-microscopy observations and mechanical characteristics of ion-beam-sputtered surgical implant alloys

NASA Technical Reports Server (NTRS)

Weigand, A. J.; Meyer, M. L.; Ling, J. S.

1977-01-01

An electron bombardment ion thruster was used as an ion source to sputter the surfaces of orthopedic prosthetic metals. Scanning electron microscopy photomicrographs were made of each ion beam textured surface. The effect of ion texturing an implant surface on its bond to bone cement was investigated. A Co-Cr-W alloy and surgical stainless steel were used as representative hard tissue implant materials to determine effects of ion texturing on bulk mechanical properties. Work was done to determine the effect of substrate temperature on the development of an ion textured surface microstructure. Results indicate that the ultimate strength of the bulk materials is unchanged by ion texturing and that the microstructure will develop more rapidly if the substrate is heated prior to ion texturing.

Characterization of Low Firing Temperature Ceramic Glaze Using Phuket MSW and Soda Lime Cullet

NASA Astrophysics Data System (ADS)

Ketboonruang, P.; Jinawat, S.; Kashima, D. P.; Wasanapiarnpong, T.; Sujaridworakun, P.; Buggakuptav, W.; Traipol, N.; Jiemsirilers, S.

2011-10-01

The normal firing temperature of ceramic products is around 1200 °C. In order to reduce firing temperature, industrial wastes were utilized in ceramic glaze. Phuket municipal solid waste (MSW), soda lime cullet, and borax were used as raw materials for low firing temperature glazes. The glaze compositions were designed using a triaxial diagram. Stoneware ceramic body was glazed then fired at 1000 and 1150 °C for 15 minutes. Morphology and phase composition of glazes were analyzed by Scanning electron microscopy (SEM-EDS) and X-ray diffraction (XRD). Thermal expansion compatibility of Stoneware body and glazes were investigated using a dilatometer. Melting behaviour of selected glaze was analyzed by heating stage microscopy. Phuket MSW and Soda lime glass cullet can be used in high percentage as major raw materials for low firing temperature ceramic glaze that show good texture and vitrified at lower firing temperature without using any commercial ceramic frits. The firing temperature can be reduced up to 150 °C in this study.

Effect of Temperature on Nucleation of Nanocrystalline Indium Tin Oxide Synthesized by Electron-Beam Evaporation

NASA Astrophysics Data System (ADS)

Shen, Yan; Zhao, Yujun; Shen, Jianxing; Xu, Xiangang

2017-07-01

Indium tin oxide (ITO) has been widely applied as a transparent conductive layer and optical window in light-emitting diodes, solar cells, and touch screens. In this paper, crystalline nano-sized ITO dendrites are obtained using an electron-beam evaporation technique. The surface morphology of the obtained ITO was studied for substrate temperatures of 25°C, 130°C, 180°C, and 300°C. Nano-sized crystalline dendrites were synthesized only at a substrate temperature of 300°C. The dendrites had a cubic structure, confirmed by the results of x-ray diffraction and transmission electron microscopy. The growth mechanism of the nano-crystalline dendrites could be explained by a vapor-liquid-solid (VLS) growth model. The catalysts of the VLS process were indium and tin droplets, confirmed by varying the substrate temperature, which further influenced the nucleation of the ITO dendrites.

Low-temperature growth and photoluminescence property of ZnS nanoribbons.

PubMed

Zhang, Zengxing; Wang, Jianxiong; Yuan, Huajun; Gao, Yan; Liu, Dongfang; Song, Li; Xiang, Yanjuan; Zhao, Xiaowei; Liu, Lifeng; Luo, Shudong; Dou, Xinyuan; Mou, Shicheng; Zhou, Weiya; Xie, Sishen

2005-10-06

At a low temperature of 450 degrees C, ZnS nanoribbons have been synthesized on Si and KCl substrates by a simple chemical vapor deposition (CVD) method with a two-temperature-zone furnace. Zinc and sulfur powders are used as sources in the different temperature zones. X-ray diffraction (XRD), selected area electron diffraction (SEAD), and transmission electron microscopy (TEM) analysis show that the ZnS nanoribbons are the wurtzite structure, and there are two types-single-crystal and bicrystal nanoribbons. Photoluminescence (PL) spectrum shows that the spectrum mainly includes two parts: a purple emission band centering at about 390 nm and a blue emission band centering at about 445 nm with a weak green shoulder around 510 nm.

Energy Storage of Polyarylene Ether Nitriles at High Temperature

NASA Astrophysics Data System (ADS)

Tang, Xiaohe; You, Yong; Mao, Hua; Li, Kui; Wei, Renbo; Liu, Xiaobo

2018-03-01

Polyarylene ether nitrile (PEN) was synthesized and used as film capacitors for energy storage at high temperature. Scanning electron microscopy observation indicated that the films of PEN have pinholes at nanoscales which restricted the energy storage properties of the material. The pinhole shadowing effect through which the energy storage properties of PEN were effectively improved to be 2.3 J/cm3 was observed by using the overlapped film of PEN. The high glass transition temperature (T g) of PEN was as high as 216 °C and PEN film showed stable dielectric constant, breakdown strength and energy storage density before the T g. The PEN films will be a potential candidate as high performance electronic storage materials used at high temperature.

Interpretation of transport measurements in ZnO-thin films

NASA Astrophysics Data System (ADS)

Petukhov, Vladimir; Stoemenos, John; Rothman, Johan; Bakin, Andrey; Waag, Andreas

2011-01-01

In order to interpret results of temperature dependent Hall measurements in heteroepitaxial ZnO-thin films, we adopted a multilayer conductivity model considering carrier-transport through the interfacial layer with degenerate electron gas as well as the upper part of ZnO layers with lower conductivity. This model was applied to the temperature dependence of the carrier concentration and mobility measured by Hall effect in a ZnO-layer grown on c-sapphire with conventional high-temperature MgO and low-temperature ZnO buffer. We also compared our results with the results of maximum entropy mobility-spectrum analysis (MEMSA). The formation of the highly conductive interfacial layer was explained by analysis of transmission electron microscopy (TEM) images taken from similar layers.

The synergy of corrosion and fretting wear process on Inconel 690 in the high temperature high pressure water environment

NASA Astrophysics Data System (ADS)

Wang, Zihao; Xu, Jian; Li, Jie; Xin, Long; Lu, Yonghao; Shoji, Tetsuo; Takeda, Yoichi; Otsuka, Yuichi; Mutoh, Yoshiharu

2018-04-01

The synergistic effect of corrosion and fretting process of the steam generator (SG) tube was investigated by using a self-designed high temperature test rig in this paper. The experiments were performed at 100°C , 200°C and 288°C , respectively. The fretting corrosion damage was studied by optical microscopy (OM), scanning electron microscope (SEM), energy dispersive spectrometer (EDS), Raman spectroscopy and auger electron spectroscopy (AES). The results demonstrated that the corrosion process in high temperature high pressure (HTHP) water environment had a distinct interaction with the fretting process of Inconel 690. With the increment of temperature, the damage mechanism changed from a simple mechanical process to a mechanochemical process.

CdO-based nanostructures as novel CO2 gas sensors

NASA Astrophysics Data System (ADS)

Krishnakumar, T.; Jayaprakash, R.; Prakash, T.; Sathyaraj, D.; Donato, N.; Licoccia, S.; Latino, M.; Stassi, A.; Neri, G.

2011-08-01

Crystalline Cd(OH)2/CdCO3 nanowires, having lengths in the range from 0.3 up to several microns and 5-30 nm in diameter, were synthesized by a microwave-assisted wet chemical route and used as a precursor to obtain CdO nanostructures after a suitable thermal treatment in air. The morphology and microstructure of the as-synthesized and annealed materials have been investigated by scanning electron microscopy, transmission electron microscopy, x-ray diffraction and thermogravimetry-differential scanning calorimetry. The change in morphology and electrical properties with temperature has revealed a wire-to-rod transformation along with a decreases of electrical resistance. Annealed samples were printed on a ceramic substrate with interdigitated contacts to fabricate resistive solid state sensors. Gas sensing properties were explored by monitoring CO2 in synthetic air in the concentration range 0.2-5 v/v% (2000-50 000 ppm). The effect of annealing temperature, working temperature and CO2 concentration on sensing properties (sensitivity, response/recovery time and stability) were investigated. The results obtained demonstrate that CdO-based thick films have good potential as novel CO2 sensors for practical applications.

Effects of Core-Shell Rubber (CSR) Nanoparticles on the Cryogenic Fracture Toughness of CSR Modified Epoxy

NASA Technical Reports Server (NTRS)

Wang, Jun; Magee, Daniel; Schneider, Judy; Cannon, Seth

2009-01-01

This study investigated the effects of core-shell rubber (CSR) nanoparticles on the mechanical properties and fracture toughness of an epoxy resin at ambient and liquid nitrogen (LN2) temperatures. Varying amounts of Kane Ace(Registered TradeMark) MX130 and Kane Ace(Registered TradeMark) MX960 toughening agent were added to a commercially available EPON 862/Epikure W epoxy resin. Elastic modulus was calculated using quasi-static tensile data. Fracture toughness was evaluated by the resulting breaking energy measured in Charpy impact tests conducted on an instrumented drop tower. The size and distribution of the CSR nanoparticles were characterized using Transmission Electron Microscopy (TEM) and Small Angle X-ray Scattering (SAXS). Scanning Electron Microscopy (SEM) was used to study the fracture surface morphology. The addition of the CSR nanoparticles increased the breaking energy with negligible change in elastic modulus and ultimate tensile stress (UTS). At ambient temperature the breaking energy increased with increasing additions of the CSR nanoparticles up to 13.8wt%, while at LN2 temperatures, it reached a plateau at much lower CSR concentration.

MOCVD of aluminium oxide films using aluminium β-diketonates as precursors

NASA Astrophysics Data System (ADS)

Devi, A.; Shivashankar, S. A.; Samuelson, A. G.

2002-06-01

Deposition of Al203 coatings by CVD is of importance because they are often used as abrading material in cemented carbide cutting tools. The conventionally used CVD process for Al203 involves the corrosive reactant AICl3. In this paper, we report on the thermal characterisation of the metalorganic precursors namely aluminium tris-tetramethyl-heptanedionate [ Al(thd)3] and aluminium tris-acetylacetonate [ Al(acac)3] and their application to the CVD of Al203 films. Crystalline A1203 films were deposited by MOCVD at low temperatures by the pyrolysis of Al(thd)3 and AI(acac)3. The films were deposited on a TiN-coated tungsten carbide (TiN/WC) and Si(100) substrates in the temperature range 500-1100 °C. The as-deposited films were characterised by x-ray diffraction, optical microscopy, scanning and transmission electron microscopy, Auger electron spectroscopy. The observed crystallinity of films grown at low temperatures, their microstructure, and composition may be interpreted in terms of a growth process that involves the melting of the metalorganic precursor on the hot growth surface.

IF-WS{sub 2} nanoparticles size design and synthesis via chemical reduction

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ghoreishi, S.M., E-mail: ghoreshi@cc.iut.ac.ir; Meshkat, S.S.; Dadkhah, A.A.

2010-05-15

An innovative synthesis of inorganic fullerene-like disulfide tungsten (IF-WS{sub 2}) nanoparticles was developed using a chemical reduction reaction in a horizontal quartz reactor. In this process, first tungsten trisulfide (WS{sub 3}) was formed via a chemical reaction of tetra thiotungstate ammonium ((NH{sub 4}){sub 2}WS{sub 4}), polyethylene glycol (PEG), and hydrochloric acid (HCl) at ambient temperature and pressure. Subsequently, WS{sub 3} was reacted with hydrogen (H{sub 2}) at high temperature (1173-1373 K) in a quartz tube. The produced WS{sub 2} nanoparticles were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray (EDAX), and transmission electron microscopy (TEM). Themore » characterization results indicated that the high-purity (100%) IF-WS{sub 2} nanoparticles were produced. Moreover, addition of surfactant (PEG) and higher operating temperature (1173-1373 K) decreased the particles agglomeration, and consequently led to the reduction of average diameter of WS{sub 2} particles in the range of 50-78 nm. The developed method is simple, environmentally compatible, and cost-effective in contrast to the conventional techniques.« less

The role of annealing temperature and bio template (egg white) on the structural, morphological and magnetic properties of manganese substituted MFe2O4 (M=Zn, Cu, Ni, Co) nanoparticles

NASA Astrophysics Data System (ADS)

Ranjith Kumar, E.; Jayaprakash, R.; Kumar, Sanjay

2014-02-01

Manganese substituted ferrites (ZnFe2O4, CuFe2O4, NiFe2O4 and CoFe2O4) have been prepared in the bio template medium by using a simple evaporation method. The annealing temperature plays an important position on changing particle size and morphology of the mixed ferrite nanoparticles were found out by X-ray diffraction, transmission electron microscopy and scanning electron microscopy methods. The role of manganese substitution in the mixed ferrite nanoparticles were also analyzed for different annealing temperature. The substitution of Mn also creates a vital change in magnetic properties which is studied by using vibrating sample magnetometer (VSM). These spinel ferrites are decomposed to α-Fe2O3 after annealing above 550 °C in air. However, α-Fe2O3 phase was slowly vanished after ferrites annealing above 900 °C. The effect of this secondary phase on the structural change and magnetic properties of the mixed ferrite nanoparticles is discussed.

Polyaniline-Cadmium Ferrite Nanostructured Composite for Room-Temperature Liquefied Petroleum Gas Sensing

NASA Astrophysics Data System (ADS)

Kotresh, S.; Ravikiran, Y. T.; Tiwari, S. K.; Vijaya Kumari, S. C.

2017-08-01

We introduce polyaniline-cadmium ferrite (PANI-CdFe2O4) nanostructured composite as a room-temperature-operable liquefied petroleum gas (LPG) sensor. The structure of PANI and the composite prepared by chemical polymerization was characterized by Fourier-transform infrared (FT-IR) spectroscopy, x-ray diffraction (XRD) analysis, and field-emission scanning electron microscopy. Comparative XRD and FT-IR analysis confirmed CdFe2O4 embedded in PANI matrix with mutual interfacial interaction. The nanostructure of the composite was confirmed by transmission electron microscopy. A simple LPG sensor operable at room temperature, exclusively based on spin-coated PANI-CdFe2O4 nanocomposite, was fabricated with maximum sensing response of 50.83% at 1000 ppm LPG. The response and recovery time of the sensor were 50 s and 110 s, respectively, and it was stable over a period of 1 month with slight degradation of 4%. The sensing mechanism is discussed on the basis of the p- n heterojunction barrier formed at the interface of PANI and CdFe2O4.

Micro- and nano-scale characterization to study the thermal degradation of cement-based materials

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lim, Seungmin, E-mail: lim76@illinois.edu; Mondal, Paramita

2014-06-01

The degradation of hydration products of cement is known to cause changes in the micro- and nano-structure, which ultimately drive thermo-mechanical degradation of cement-based composite materials at elevated temperatures. However, a detailed characterization of these changes is still incomplete. This paper presents results of an extensive experimental study carried out to investigate micro- and nano-structural changes that occur due to exposure of cement paste to high temperatures. Following heat treatment of cement paste up to 1000 °C, damage states were studied by compressive strength test, thermogravimetric analysis (TGA), scanning electron microscopy (SEM) atomic force microscopy (AFM) and AFM image analysis.more » Using experimental results and research from existing literature, new degradation processes that drive the loss of mechanical properties of cement paste are proposed. The development of micro-cracks at the interface between unhydrated cement particles and paste matrix, a change in C–S–H nano-structure and shrinkage of C–S–H, are considered as important factors that cause the thermal degradation of cement paste. - Highlights: • The thermal degradation of hydration products of cement is characterized at micro- and nano-scale using scanning electron microscopy (SEM) and atomic force microscopy (AFM). • The interface between unhydrated cement particles and the paste matrix is considered the origin of micro-cracks. • When cement paste is exposed to temperatures above 300 ºC, the nano-structure of C-S-H becomes a more loosely packed globular structure, which could be indicative of C-S-H shrinkage.« less

Insight in the 3D morphology of silica-based nanotubes using electron microscopy.

PubMed

Dennenwaldt, Teresa; Wisnet, Andreas; Sedlmaier, Stefan J; Döblinger, Markus; Schnick, Wolfgang; Scheu, Christina

2016-11-01

Amorphous silica-based nanotubes (SBNTs) were synthesized from phosphoryl triamide, OP(NH 2 ) 3 , thiophosphoryl triamide, SP(NH 2 ) 3 , and silicon tetrachloride, SiCl 4 , at different temperatures and with varying amount of the starting material SiCl 4 using a recently developed template-free synthesis approach. Diameter and length of the SBNTs are tunable by varying the synthesis parameters. The 3D mesocrystals of the SBNTs were analyzed with focused ion beam sectioning and electron tomography in the transmission electron microscope showing the hollow tubular structure of the SBNTs. The reconstruction of a small SBNT assembly was achieved from a high-angle annular-dark field scanning transmission electron microscopy tilt series containing only thirteen images allowing analyzing beam sensitive material without altering the structure. The reconstruction revealed that the individual nanotubes are forming an interconnected array with an open channel structure. Copyright © 2016 Elsevier Ltd. All rights reserved.

A selective ultrahigh responding high temperature ethanol sensor using TiO2 nanoparticles.

PubMed

Arafat, M M; Haseeb, A S M A; Akbar, Sheikh A

2014-07-28

In this research work, the sensitivity of TiO2 nanoparticles towards C2H5OH, H2 and CH4 gases was investigated. The morphology and phase content of the particles was preserved during sensing tests by prior heat treatment of the samples at temperatures as high as 750 °C and 1000 °C. Field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM) and X-ray diffraction (XRD) analysis were employed to characterize the size, morphology and phase content of the particles. For sensor fabrication, a film of TiO2 was printed on a Au interdigitated alumina substrate. The sensing temperature was varied from 450 °C to 650 °C with varying concentrations of target gases. Results show that the sensor has ultrahigh response towards ethanol (C2H5OH) compared to hydrogen (H2) and methane (CH4). The optimum sensing temperature was found to be 600 °C. The response and recovery times of the sensor are 3 min and 15 min, respectively, for 20 ppm C2H5OH at the optimum operating temperature of 600 °C. It is proposed that the catalytic action of TiO2 with C2H5OH is the reason for the ultrahigh response of the sensor.

Effect of alloy composition on high-temperature bending fatigue strength of ferritic stainless steels

NASA Astrophysics Data System (ADS)

Ahn, Yong-Sik; Song, Jeon-Young

2011-12-01

Exhaust manifolds are subjected to an environment in which heating and cooling cycles occur due to the running pattern of automotive engines. This temperature profile results in the repeated bending stress of exhaust pipes. Therefore, among high-temperature characteristics, the bending fatigue strength is an important factor that affects the lifespan of exhaust manifolds. Here, we report on the effect of the alloy composition, namely the weight fraction of the elements Cr, Mo, Nb, and Ti, on the high-temperature bending fatigue strength of the ferritic stainless steel used in exhaust manifolds. Little difference in the tensile strength and bending fatigue strength of the different composition steels was observed below 600 °C, with the exception of the low-Cr steel. However, steels with high Cr, Mo, or Nb fractions showed considerably larger bending fatigue strength at temperatures of 800 °C. After heating, the precipitates from the specimens were extracted electrolytically and analyzed using scanning electron microscopy energy dispersive spectrometry and transmission electron microscopy. Alloying with Cr and Mo was found to increase the bending fatigue strength due to the substitutional solid solution effect, while alloying with Nb enhanced the strength by forming fine intermetallic compounds, including NbC and Fe2Nb.

The Influence of Sintering Temperature on the Microstructure and Thermoelectric Properties of n-Type Bi2Te3- x Se x Nanomaterials

NASA Astrophysics Data System (ADS)

Du, Y.; Cai, K. F.; Li, H.; An, B. J.

2011-05-01

Pure Bi2Te3 and Bi2Se3 nanopowders were hydrothermally synthesized, and n-type Bi2Te3- x Se x bulk samples were prepared by hot pressing a mixture of Bi2Te3 and Bi2Se3 nanopowders at 623 K, 648 K or 673 K and 80 MPa in vacuum. The phase composition of the powders and bulk samples were characterized by x-ray diffraction. The morphology of the powders was examined by transmission electron microscopy. The microstructure and composition of the bulk samples were characterized by field-emission scanning electron microscopy and energy-dispersive x-ray spectroscopy, respectively. The density of the samples increased with sintering temperature. The samples were somewhat oxidized, and the amount of oxide (Bi2TeO5) present increased with sintering temperature. The samples consisted of sheet-like grains with a thickness less than 100 nm. Seebeck coefficient, electrical conductivity, and thermal conductivity of the samples were measured from room temperature up to 573 K. Throughout the temperature range investigated, the sample sintered at 623 K had a higher power factor than the samples sintered at 648 K or 673 K.

A Selective Ultrahigh Responding High Temperature Ethanol Sensor Using TiO2 Nanoparticles

PubMed Central

Arafat, M. M.; Haseeb, A. S. M. A.; Akbar, Sheikh A.

2014-01-01

In this research work, the sensitivity of TiO2 nanoparticles towards C2H5OH, H2 and CH4 gases was investigated. The morphology and phase content of the particles was preserved during sensing tests by prior heat treatment of the samples at temperatures as high as 750 °C and 1000 °C. Field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM) and X-ray diffraction (XRD) analysis were employed to characterize the size, morphology and phase content of the particles. For sensor fabrication, a film of TiO2 was printed on a Au interdigitated alumina substrate. The sensing temperature was varied from 450 °C to 650 °C with varying concentrations of target gases. Results show that the sensor has ultrahigh response towards ethanol (C2H5OH) compared to hydrogen (H2) and methane (CH4). The optimum sensing temperature was found to be 600 °C. The response and recovery times of the sensor are 3 min and 15 min, respectively, for 20 ppm C2H5OH at the optimum operating temperature of 600 °C. It is proposed that the catalytic action of TiO2 with C2H5OH is the reason for the ultrahigh response of the sensor. PMID:25072346

Study of thermal-field emission properties and investigation of temperature dependent noise in the field emission current from vertical carbon nanotube emitters

NASA Astrophysics Data System (ADS)

Kolekar, Sadhu; Patole, S. P.; Patil, Sumati; Yoo, J. B.; Dharmadhikari, C. V.

2017-10-01

We have investigated temperature dependent field electron emission characteristics of vertical carbon nanotubes (CNTs). The generalized expression for electron emission from well-defined cathode surface is given by Millikan and Lauritsen [1] for the combination of temperature and electric field effect. The same expression has been used to explain the electron emission characteristics from vertical CNT emitters. Furthermore, this has been applied to explain the electron emission for different temperatures ranging from room temperature to 1500 K. The real-time field electron emission images at room temperature and 1500 K are recorded by using Charge Coupled Device (CCD) in order to understand the effect of temperature on distribution of electron emission spots and ring like structures in Field Emission Microscope (FEM) image. The FEM images could be used to calculate the total number of emitters per cm2 for electron emission. The calculated number of emitters per cm2 from FEM image is typically, 4.5 × 107 and the actual number emitters per cm2 present as per Atomic Force Microscopy (AFM) data is 1.2 × 1012. The measured Current-Voltage (I-V) characteristics exhibit non linear Folwer-Nordheim (F-N) type behavior. The fluctuations in the emission current were recorded at different temperatures and Fast Fourier transformed into temperature dependent power spectral density. The latter was found to obey power law relation S(f) = A(Iδ/fξ), where δ and ξ are temperature dependent current and frequency exponents respectively.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sicupira, Felipe Lucas; Sandim, Maria José R.; Sandim, Hugo R.Z.

The good performance of supermartensitic stainless steels is strongly dependent on the volume fraction of retained austenite at room temperature. The present work investigates the effect of secondary tempering temperatures on this phase transformation and quantifies the amount of retained austenite by X-ray diffraction and saturation magnetization. The steel samples were tempered for 1 h within a temperature range of 600–800 °C. The microstructure was characterized using scanning electron microscopy and electron backscatter diffraction. Results show that the amount of retained austenite decreased with increasing secondary tempering temperature in both quantification methods. - Highlights: • The phase transformation during secondarymore » tempering temperatures was observed. • Phases were quantified by X-ray diffraction and DC-saturation magnetization. • More retained austenite forms with increasing secondary tempering temperature. • The retained austenite is mainly located at the grain and lath boundaries.« less

Scanning tunneling microscopy study of low temperature silicon epitaxy on hydrogen/silicon(001) and phosphine adsorption on silicon(111)-7x7

NASA Astrophysics Data System (ADS)

Ji, Jeong-Young

A three-chamber ultra-high-vacuum (UHV) system with preparation, scanning tunneling microscopy (STM), and chemical vapor deposition (CVD) chambers was designed and built. Here, one can perform surface preparation, STM e-beam lithography, precursor gas dosing, ion sputtering, silicon epitaxy, and various measurements such as reflection high energy electron diffraction (RHEED), low energy electron diffraction (LEED), and Auger electron spectroscopy (AES). Processes performed in the ultra-clean preparation and gas-filled CVD chambers can be monitored by transferring the samples back to the STM chamber to take topographical images. Si deposition on H-terminated Si(001)-2x1 surfaces at temperatures 300--530 K was studied by scanning tunneling microscopy. Hydrogen apparently hinders Si adatom diffusion and enhances surface roughening. Post-growth annealing transfers the top layer atoms downward to fill in vacancies in the lower layer, restoring the crystallinity of the thin film. Hydrogen is shown to remain on the growth front up to at least 10 ML. Si deposition onto the H/Si(001)-3x1 surface at 530 K suggests that dihydride units further suppress Si adatom diffusion and increase surface roughness. PH3 adsorption on Si(111)-7x7 was studied for various exposures between 0.3--60 L at room temperature by means of the scanning-tunneling-microscopy (STM). PH3-, PH2-, H-reacted, and unreacted adatoms can be identified by analyzing STM images at different sample biases. Most of PH3 adsorbs dissociatively on the surface at initial exposure, generating H and PH2 adsorption sites, followed by molecular adsorption of PH3. Rest atoms are more reactive than the adatoms and PH 2-reacted rest atom sites are also observed in STM images. Statistical analysis shows that center adatoms are more reactive than corner adatoms and the saturation P coverage is ˜0.22 ML. Finally, 900 K annealing of a PH 3 dosed surface results in a disordered, partially P-covered surface and PH3 dosing at 900 K forms the same surface reconstruction as a P2-adsorbed surface at similar temperature.

The Formation, Transport Properties and Microstructure of 45 Degrees (001) Tilt Grain Boundaries in Yttrium BARIUM(2) COPPER(3) OXYGEN(7-X) Thin Films

NASA Astrophysics Data System (ADS)

Vuchic, Boris Vukan

1995-01-01

Most high angle grain boundaries in high-T _{c} superconductors exhibit weak link behavior. The Josephson-like properties of these grain boundaries can be used for many device applications such as superconducting quantum interference devices (SQUIDs). The structure-property relationship of different types of 45 ^circ (001) YBa_2 Cu_3O_{7-x} thin film grain boundary junctions are examined to study their weak link nature. A technique, termed sputter-induced epitaxy, is developed to form 45^circ (001) tilt grain boundaries in YBa_2Cu _3O_{7-x} thin films on (100) MgO substrates. A low voltage ion bombardment pre-growth substrate treatment is used to modify the epitaxial orientation relationship between the thin film and the substrate in selected regions. By modifying the orientation of the thin film, grain boundary junctions can be placed in any configuration on the substrate. A variety of pre-growth sputtering conditions in conjunction with atomic force microscopy and Rutherford backscatter spectrometry are used to determine the role of the ions in modifying the substrate surface. Sputter-induced epitaxy is extended to a multilayer MgO/LaAlO_3 substrate, allowing integration of the sputter -induced epitaxy junctions into multilayer structures. The low temperature transport properties of the sputter-induced epitaxy junctions and a set of bi-epitaxial grain boundaries are studied. Individual grain boundaries are isolated and characterized for resistance vs. temperature, current vs. voltage as a function of temperature and magnetic field behavior. Resistive and superconducting grain boundaries are compared. Microstructural analysis is performed using scanning electron microscopy, transmission electron microscopy and high resolution electron microscopy (HREM). Marked differences are observed in the microstructure of resistive and superconducting grain boundaries. HREM studies suggest the importance of the local atomic scale structure of the grain boundary in transport properties. A phenomenological grain boundary model is proposed to describe the structure -property relationship of the boundaries.

Understanding local degradation of cycled Ni-rich cathode materials at high operating temperature for Li-ion batteries

NASA Astrophysics Data System (ADS)

Hwang, Sooyeon; Kim, Dong Hyun; Chung, Kyung Yoon; Chang, Wonyoung

2014-09-01

We utilize transmission electron microscopy in conjunction with electron energy loss spectroscopy to investigate local degradation that occurs in LixNi0.8Co0.15Al0.05O2 cathode materials (NCA) after 30 cycles with cutoff voltages of 4.3 V and 4.8 V at 55 °C. NCA has a homogeneous crystallographic structure before electrochemical reactions; however, we observed that 30 cycles of charge/discharge reactions induced inhomogeneity in the crystallographic and electronic structures and also introduced porosity particularly at surface area. These changes were more noticeable in samples cycled with higher cutoff voltage of 4.8 V. Effect of operating temperature was further examined by comparing electronic structures of oxygen of the NCA particles cycled at both room temperature and 55 °C. The working temperature has a greater impact on the NCA cathode materials at a cutoff voltage of 4.3 V that is the practical the upper limit voltage in most applications, while a cutoff voltage of 4.8 V is high enough to cause surface degradation even at room temperature.

Effects of aging treatment on the microstructure and superelasticity of columnar-grained Cu71Al18Mn11 shape memory alloy

NASA Astrophysics Data System (ADS)

Liu, Ji-li; Huang, Hai-you; Xie, Jian-xin

2016-10-01

The effect of aging treatment on the superelasticity and martensitic transformation critical stress in columnar-grained Cu71Al18Mn11 shape memory alloy (SMA) at the temperature ranging from 250°C to 400°C was investigated. The microstructure evolution during the aging treatment was characterized by optical microscopy, scanning electron microscopy, transmission electron microscopy, and X-ray diffraction. The results show that the plate-like bainite precipitates distribute homogeneously within austenitic grains and at grain boundaries. The volume fraction of bainite increases with the increase in aging temperature and aging time, which substantially improves the martensitic transformation critical stress of the alloy, whereas the bainite only slightly affects the superelasticity. This behavior is attributed to a coherent relationship between the bainite and the austenite, as well as to the bainite and the martensite exhibiting the same crystal structure. The variations of the martensitic transformation critical stress and the superelasticity of columnar-grained Cu71Al18Mn11 SMA with aging temperature and aging time are described by the Austin-Rickett equation, where the activation energy of bainite precipitation is 77.2 kJ·mol-1. Finally, a columnar-grained Cu71Al18Mn11 SMA with both excellent superelasticity (5%-9%) and high martensitic transformation critical stress (443-677 MPa) is obtained through the application of the appropriate aging treatments.

In situ synthesis of semiconducting single-walled carbon nanotubes by modified arc discharging method

NASA Astrophysics Data System (ADS)

Zhao, Tingkai; Ji, Xianglin; Jin, Wenbo; Yang, Wenbo; Zhao, Xing; Dang, Alei; Li, Hao; Li, Tiehu

2017-02-01

Semiconducting single-walled carbon nanotubes (s-SWCNTs) were in situ synthesized by a temperature-controlled arc discharging furnace with DC electric field using Co-Ni alloy powder as catalyst in helium gas. The microstructures of s-SWCNTs were characterized using high-resolution transmission electron microscopy, electron diffraction, and Raman spectrometry apparatus. The experimental results indicated that the best voltage value in DC electric field is 54 V, and the environmental temperature of the reaction chamber is 600 °C. The mean diameter of s-SWCNTs was estimated about 1.3 nm. The chiral vector ( n, m) of s-SWCNTs was calculated to be (10, 10) type according to the electron diffraction patterns.

Ultrathin NiGe films prepared via catalytic solid-vapor reaction of Ni with GeH(4).

PubMed

Peter, Antony P; Opsomer, Karl; Adelmann, Christoph; Schaekers, Marc; Meersschaut, Johan; Richard, Olivier; Vaesen, Inge; Moussa, Alain; Franquet, Alexis; Zsolt, Tokei; Van Elshocht, Sven

2013-10-09

A low-temperature (225-300 °C) solid-vapor reaction process is reported for the synthesis of ultrathin NiGe films (∼6-23 nm) on 300 mm Si wafers covered with thermal oxide. The films were prepared via catalytic chemical vapor reaction of germane (GeH4) gas with physical vapor deposited (PVD) Ni films of different thickness (2-10 nm). The process optimization by investigating GeH4 partial pressure, reaction temperature, and time shows that low resistive, stoichiometric, and phase pure NiGe films can be formed within a broad window. NiGe films crystallized in an orthorhombic structure and were found to exhibit a smooth morphology with homogeneous composition as evidenced by glancing angle X-ray diffraction (GIXRD), scanning electron microscopy (SEM), atomic force microscopy (AFM), and Rutherford back-scattering (RBS) analysis. Transmission electron microscopy (TEM) analysis shows that the NiGe layers exhibit a good adhesion without voids and a sharp interface on the thermal oxide. The NiGe films were found to be morphologically and structurally stable up to 500 °C and exhibit a resistivity value of 29 μΩ cm for 10 nm NiGe films.

Effect of the sample annealing temperature and sample crystallographic orientation on the charge kinetics of MgO single crystals subjected to keV electron irradiation.

PubMed

Boughariou, A; Damamme, G; Kallel, A

2015-04-01

This paper focuses on the effect of sample annealing temperature and crystallographic orientation on the secondary electron yield of MgO during charging by a defocused electron beam irradiation. The experimental results show that there are two regimes during the charging process that are better identified by plotting the logarithm of the secondary electron emission yield, lnσ, as function of the total trapped charge in the material QT. The impact of the annealing temperature and crystallographic orientation on the evolution of lnσ is presented here. The slope of the asymptotic regime of the curve lnσ as function of QT, expressed in cm(2) per trapped charge, is probably linked to the elementary cross section of electron-hole recombination, σhole, which controls the trapping evolution in the reach of the stationary flow regime. © 2014 The Authors Journal of Microscopy © 2014 Royal Microscopical Society.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Salili, S.M.; School of Metallurgy and Materials Engineering, College of Engineering, University of Tehran, Tehran; Ataie, A., E-mail: aataie@ut.ac.ir

This research aimed to synthesize nanostructured strontium-doped lanthanum manganite, La{sub 0.8}Sr{sub 0.2}MnO{sub 3} (LSMO), with its Curie temperature (T{sub c}) adjusted to the therapeutic range, through a mechanothermal route. In order to investigate the effect of heat treatment temperature and duration on the resulting crystallite size, morphology, magnetic behavior and Curie temperature, the starting powder mixture was milled in a planetary ball mill before being subsequently heat treated at distinct temperatures for different time lengths. The composition, morphology, and magnetic behavior were characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high resolution transmission electron microscopymore » (HRTEM), selected area electron diffraction (SAED) and vibrating sample magnetometer (VSM). In addition, magnetic properties were further investigated using an alternating current (AC) susceptometer and thermo-magnetic analyzer. 20 h of milling produced a crystallite size reduction leading to a decrease in the heat treatment temperature of LSMO synthesis to 800 °C. Moreover, SEM analysis has shown the morphology of a strong agglomeration of fine nanoparticles. HRTEM showed clear lattice fringes of high crystallinity. The mean crystallite and particle size of 20-hour milled sample heat treated at 1100 °C for 10 h are relatively 69 and 100 nm, respectively. The VSM data at room temperature, indicated a paramagnetic behavior for samples heat treated at 800 °C. However, by increasing heat treatment temperature to 1100 °C, LSMO indicates a ferromagnetic behavior with well-adjusted Curie temperature of 320 K, suitable for hyperthermia applications. Also, reentrant spin glass (RSG) behavior has been found in heat treated samples. The particles are coated with (3-aminopropyl) triethoxysilane (APTES) for biocompatibility purposes; Fourier transform infrared spectroscopy (FTIR) and thermo-gravimetric analysis (TGA) are used for further confirmation of APTES coating. - Highlights: • La{sub 0.8}Sr{sub 0.2}MnO{sub 3} nanoparticles were synthesized via a mechanothermal route. • We report a significant reduction in the heat treatment temperature. • The Curie temperature was tuned within the therapeutic range. • The particles were coated with (3-aminopropyl) triethoxysilane for biocompatibility purposes.« less

Temperature Induced Voltage Offset Drifts in Silicon Carbide Pressure Sensors

NASA Technical Reports Server (NTRS)

Okojie, Robert S.; Lukco, Dorothy; Nguyen, Vu; Savrun, Ender

2012-01-01

We report the reduction of transient drifts in the zero pressure offset voltage in silicon carbide (SiC) pressure sensors when operating at 600 C. The previously observed maximum drift of +/- 10 mV of the reference offset voltage at 600 C was reduced to within +/- 5 mV. The offset voltage drifts and bridge resistance changes over time at test temperature are explained in terms of the microstructure and phase changes occurring within the contact metallization, as analyzed by Auger electron spectroscopy and field emission scanning electron microscopy. The results have helped to identify the upper temperature reliable operational limit of this particular metallization scheme to be 605 C.

Virtual scanning tunneling microscopy: A local spectroscopic probe of two-dimensional electron systems

NASA Astrophysics Data System (ADS)

Sciambi, A.; Pelliccione, M.; Bank, S. R.; Gossard, A. C.; Goldhaber-Gordon, D.

2010-09-01

We propose a probe technique capable of performing local low-temperature spectroscopy on a two-dimensional electron system (2DES) in a semiconductor heterostructure. Motivated by predicted spatially-structured electron phases, the probe uses a charged metal tip to induce electrons to tunnel locally, directly below the tip, from a "probe" 2DES to a "subject" 2DES of interest. We test this concept with large-area (nonscanning) tunneling measurements, and predict a high spatial resolution and spectroscopic capability, with minimal influence on the physics in the subject 2DES.

Structure Evolution and Distributions of Grain-Boundary Misorientainons in Submicrocrystalline Molybdenum Irradiated with a Pulsed Electron Beam

NASA Astrophysics Data System (ADS)

Stepanova, E. N.; Grabovetskaya, G. P.; Teresov, A. D.; Mishin, I. P.

2018-05-01

Using the methods of electron backscatter diffraction, electron microscopy and X-ray diffraction analysis, it is demonstrated that irradiation of the surface of a submicrocrystalline molybdenum specimen with a pulsed electron beam in a non-melt regime results in the formation of a gradient structure in its bulk. The irradiation temperature is shown to affect the density of defects, the value of stress, and the distributions of grain-boundary misorientations in the surface and bulk of the submicrocrystalline molybdenum specimens.

Pulsed-Plasma Physical Vapor Deposition Approach Toward the Facile Synthesis of Multilayer and Monolayer Graphene for Anticoagulation Applications.

PubMed

Vijayaraghavan, Rajani K; Gaman, Cezar; Jose, Bincy; McCoy, Anthony P; Cafolla, Tony; McNally, Patrick J; Daniels, Stephen

2016-02-01

We demonstrate the growth of multilayer and single-layer graphene on copper foil using bipolar pulsed direct current (DC) magnetron sputtering of a graphite target in pure argon atmosphere. Single-layer graphene (SG) and few-layer graphene (FLG) films are deposited at temperatures ranging from 700 °C to 920 °C within <30 min. We find that the deposition and post-deposition annealing temperatures influence the layer thickness and quality of the graphene films formed. The films were characterized using atomic force microscopy (AFM), scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), and optical transmission spectroscopy techniques. Based on the above studies, a diffusion-controlled mechanism was proposed for the graphene growth. A single-step whole blood assay was used to investigate the anticoagulant activity of graphene surfaces. Platelet adhesion, activation, and morphological changes on the graphene/glass surfaces, compared to bare glass, were analyzed using fluorescence microscopy and SEM techniques. We have found significant suppression of the platelet adhesion, activation, and aggregation on the graphene-covered surfaces, compared to the bare glass, indicating the anticoagulant activity of the deposited graphene films. Our production technique represents an industrially relevant method for the growth of SG and FLG for various applications including the biomedical field.

Ordered arrays of multiferroic epitaxial nanostructures.

PubMed

Vrejoiu, Ionela; Morelli, Alessio; Biggemann, Daniel; Pippel, Eckhard

2011-01-01

Epitaxial heterostructures combining ferroelectric (FE) and ferromagnetic (FiM) oxides are a possible route to explore coupling mechanisms between the two independent order parameters, polarization and magnetization of the component phases. We report on the fabrication and properties of arrays of hybrid epitaxial nanostructures of FiM NiFe(2)O(4) (NFO) and FE PbZr(0.52)Ti(0.48)O(3) or PbZr(0.2)Ti(0.8)O(3), with large range order and lateral dimensions from 200 nm to 1 micron. The structures were fabricated by pulsed-laser deposition. High resolution transmission electron microscopy and high angle annular dark-field scanning transmission electron microscopy were employed to investigate the microstructure and the epitaxial growth of the structures. Room temperature ferroelectric and ferrimagnetic domains of the heterostructures were imaged by piezoresponse force microscopy (PFM) and magnetic force microscopy (MFM), respectively. PFM and MFM investigations proved that the hybrid epitaxial nanostructures show ferroelectric and magnetic order at room temperature. Dielectric effects occurring after repeated switching of the polarization in large planar capacitors, comprising ferrimagnetic NiFe2O4 dots embedded in ferroelectric PbZr0.52Ti0.48O3 matrix, were studied. These hybrid multiferroic structures with clean and well defined epitaxial interfaces hold promise for reliable investigations of magnetoelectric coupling between the ferrimagnetic / magnetostrictive and ferroelectric / piezoelectric phases.

Low temperature molten-salt synthesis of nanocrystalline cubic Sr{sub 2}SbMnO{sub 6}

DOE Office of Scientific and Technical Information (OSTI.GOV)

Baral, Antara; Varma, K.B.R., E-mail: kbrvarma@mrc.iisc.ernet.i

2009-12-15

Sr{sub 2}SbMnO{sub 6} (SSM) powders were successfully synthesized at reasonably low temperatures via molten-salt synthesis (MSS) method using eutectic composition of 0.635 Li{sub 2}SO{sub 4}-0.365 Na{sub 2}SO{sub 4} (flux). High-temperature cubic phase SSM was stabilized at room temperature by calcining the as-synthesized powders at 900 deg. C/10 h. The phase formation and morphology of these powders were characterized via X-ray powder diffraction and scanning electron microscopy, respectively. The SSM phase formation associated with {approx}60 nm sized crystallites was also confirmed by transmission electron microscopy. The activation energy associated with the particle growth was found to be 95+-5 kJ mol{sup -1}.more » The dielectric constant of the tetragonal phase of the ceramic (fabricated using this cubic phase powder) with and without the flux (sulphates) has been monitored as a function of frequency (100 Hz-1 MHz) at room temperature. Internal barrier layer capacitance (IBLC) model was invoked to rationalize the dielectric properties. - Graphical abstract: The as synthesized powders of Sr{sub 2}SbMnO{sub 6} calcined at 900 deg. C/10 h yielded a cubic phase ({approx}60 nm sized crystallites). Centrosymmetric tetragonal (I4/mcm) phase was obtained by increasing the calcination temperature to 1000 deg. C. Display Omitted« less

Ultrafast studies of coexisting electronic order in cuprate superconductors

NASA Astrophysics Data System (ADS)

Hinton, James; Thewalt, Eric; Alpichshev, Zhanybek; Sternbach, Aaron; McLeod, Alex; Ji, L.; Veit, Mike; Dorrow, Chelsey; Koralek, Jake; Xhao, Xudong; Barisic, Neven; Kemper, Alexander; Gedik, Nuh; Greven, Martin; Basov, Dimitri; Orenstein, Joe

The cuprate family of high temperature superconductors displays a variety of electronic phases which emerge when charge carriers are added to the antiferromagnetic parent compound. These electronic phases are characterized by subtle differences in the low energy electronic excitations. Ultrafast time-resolved reflectivity (TRR) provides an ideal tool for investigating the cuprate phase diagram, as small changes in the electronic structure can produce significant contrast in the non-equilibrium reflectivity. Here we present TRR measurements of cuprate superconductors, focusing on the model single-layer cuprate HgBa2CuO4+δ. We observe a cusp-like feature in the quasiparticle lifetime near the superconducting transition temperature Tc. This feature can be understood using a model of coherently-mixed charge-density wave and superconducting pairing. We propose extending this technique to the nanoscale using ultrafast scattering scanning near-field microscopy (u-SNOM). This will allow us to explore how these electronic phases coexist and compete in real-space.

Electron paramagnetic resonance, scanning electron microscopy with energy dispersion X-ray spectrometry, X-ray powder diffraction, and NMR characterization of iron-rich fired clays.

PubMed

Presciutti, Federica; Capitani, Donatella; Sgamellotti, Antonio; Brunetti, Brunetto Giovanni; Costantino, Ferdinando; Viel, Stéphane; Segre, Annalaura

2005-12-01

The aim of this study is to clarify the structure of an iron-rich clay and the structural changes involved in the firing process as a preliminary step to get information on ancient ceramic technology. To this purpose, illite-rich clay samples fired at different temperatures were characterized using a multitechnique approach, i.e., by electron paramagnetic resonance, scanning electron microscopy with electron dispersion X-ray spectrometry, X-ray powder diffraction, magic angle spinning and multiple quantum magic angle spinning NMR. During firing, four main reaction processes occur: dehydration, dehydroxylation, structural breakdown, and recrystallization. When the results are combined from all characterization methods, the following conclusions could be obtained. Interlayer H2O is located close to aluminum in octahedral sites and is driven off at temperatures lower than 600 degrees C. Between 600 and 700 degrees C dehydroxylation occurs whereas, between 800 and 900 degrees C, the aluminum in octahedral sites disappears, due to the breakdown of the illite structure, and all iron present is oxidized to Fe3+. In samples fired at 1000 and 1100 degrees C iron clustering was observed as well as large single crystals of iron with the occurrence of ferro- or ferrimagnetic effects. Below 900 degrees C the aluminum in octahedral sites presents a continuous distribution of chemical shift, suggesting the presence of slightly distorted sites. Finally, over the whole temperature range, the presence of at least two tetrahedral aluminum sites was revealed, characterized by different values of the quadrupolar coupling constant.

Formation of ZnS nanostructures by a simple way of thermal evaporation

NASA Astrophysics Data System (ADS)

Yuan, H. J.; Xie, S. S.; Liu, D. F.; Yan, X. Q.; Zhou, Z. P.; Ci, L. J.; Wang, J. X.; Gao, Y.; Song, L.; Liu, L. F.; Zhou, W. Y.; Wang, G.

2003-11-01

The mass synthesis of ZnS nanobelts, nanowires, and nanoparticles has been achieved by a simple method of thermal evaporation of ZnS powders onto silicon substrates in the presence of Au catalyst. The temperature of the substrates and the concentration of ZnS vapor were the critical experimental parameters for the formation of different morphologies of ZnS nanostructures. Scanning electron microscopy and transmission electron microscopy show that the diameters of as-prepared nanowires were 30-70 nm. The UV emission at 374 nm is probably related to the exciton emission, while the mechanism of blue emission at 443 nm is probably mainly due to the presence of various surface states.

Effects of Polyethylene Glycol and Citric Acid on Preparation and Hydrodechlorination Activity of Molybdenum Phosphide

NASA Astrophysics Data System (ADS)

Liu, Xiaomeng; Lu, Shaoxiang; Xu, Hanghui; Ren, Lili

2018-07-01

Molybdenum phosphide (MoP), modified by polyethylene glycol (PEG) and citric acid (CA), exhibited 2 to 3 times superior activity than the MoP modified by CA alone. And the optimal activity temperature was reduced from 500 to 450oC. The catalyst was fully characterized by a variety of techniques including X-ray diffraction (XRD), N2 adsorption-desorption isotherm, scanning electron microscopy (SEM), transmission electron microscopy (TEM). The results showed that the addition of PEG and CA increased the surface area of MoP and decreased the particle size of MoP. Furthermore, the reaction mechanism also has been discussed by combining the activity data and characterization results.

Synthesis of highly nanoporous YBO3 architecture via a co-precipitation approach and tunable luminescent properties.

PubMed

Liu, Lili; Zhang, Xianwen; Chaudhuri, Jharna

2015-01-01

We present a simple co-precipitation method to prepare highly nanoporous YBO(3) architecture using NaBO(3) ·  4H(2)O as a boric source and 600°C as the annealing temperature. The reaction was carried out under an aqueous condition without any organic solvent, surfactant, or catalysts. The prepared samples were characterized by powder X-ray diffraction (PXRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The photoluminescence of doped-nanoporous YBO(3):Eu(3+) was further investigated. It is expected that highly nanoporous YBO(3) architecture can be an ideal candidate for applications in catalysis, adsorption, and optoelectronic devices. © Wiley Periodicals, Inc.

Influence of annealing temperature on Raman and photoluminescence spectra of electron beam evaporated TiO₂ thin films.

PubMed

Vishwas, M; Narasimha Rao, K; Chakradhar, R P S

2012-12-01

Titanium dioxide (TiO(2)) thin films were deposited on fused quartz substrates by electron beam evaporation method at room temperature. The films were annealed at different temperatures in ambient air. The surface morphology/roughness at different annealing temperatures were analyzed by atomic force microscopy (AFM). The crystallinity of the film has improved with the increase of annealing temperature. The effect of annealing temperature on optical, photoluminescence and Raman spectra of TiO(2) films were investigated. The refractive index of TiO(2) films were studied by envelope method and reflectance spectra and it is observed that the refractive index of the films was high. The photoluminescence intensity corresponding to green emission was enhanced with increase of annealing temperature. The peaks in Raman spectra depicts that the TiO(2) film is of anatase phase after annealing at 300°C and higher. The films show high refractive index, good optical quality and photoluminescence characteristics suggest that possible usage in opto-electronic and optical coating applications. Copyright © 2012 Elsevier B.V. All rights reserved.

The matrices of unequilibrated ordinary chondrites - Implications for the origin and history of chondrites

NASA Technical Reports Server (NTRS)

Huss, G. R.; Keil, K.; Taylor, G. J.

1981-01-01

The matrices of 16 unequilibrated chondrites were examined by optical microscopy, an electron microprobe, and a scanning electron microscope. The fine-grained, opaque, silicate matrix of type 3 unequilibrated chondrites was compositionally, mineralogically, and texturally different from the chondrules and their fragments; it may be the low temperature condensate proposed by Larimer and Anders (1967, 1970). Each meteorite has been metamorphosed by a combination of processes including thermal metamorphism and the passage of shock waves; the appearance of each chondrite results from the temperature and pressure conditions which formed it, and subsequent metamorphic alterations.

Visualizing the mesothoracic spiracles in a bark beetle: The coffee berry borer, Hypothenemus hampei

USDA-ARS?s Scientific Manuscript database

In a low-temperature scanning electron microscopy study aimed at determining whether the coffee berry borer (Hypothenemus hampei (Ferrari); Coleoptera: Curculionidae: Scolytinae) possesses mycangia, we fortuitously detected the mesothoracic spiracles, which are usually concealed. The mesothoracic s...

Configuration-specific electronic structure of strongly interacting interfaces: TiOPc on Cu(110)

NASA Astrophysics Data System (ADS)

Maughan, Bret; Zahl, Percy; Sutter, Peter; Monti, Oliver L. A.

2017-12-01

We use low-temperature scanning tunneling microscopy in combination with angle-resolved ultraviolet and two-photon photoemission spectroscopy to investigate the interfacial electronic structure of titanyl phthalocyanine (TiOPc) on Cu(110). We show that the presence of two unique molecular adsorption configurations is crucial for a molecular-level analysis of the hybridized interfacial electronic structure. Specifically, thermally induced self-assembly exposes marked adsorbate-configuration-specific contributions to the interfacial electronic structure. The results of this work demonstrate an avenue towards understanding and controlling interfacial electronic structure in chemisorbed films even for the case of complex film structure.

Ultrasonic and metallographic studies on AISI 4140 steel exposed to hydrogen at high pressure and temperature

NASA Astrophysics Data System (ADS)

Oruganti, Malavika

This thesis conducts an investigation to study the effects of hydrogen exposure at high temperature and pressure on the behavior of AISI 4140 steel. Piezoelectric ultrasonic technique was primarily used to evaluate surface longitudinal wave velocity and defect geometry variations, as related to time after exposure to hydrogen at high temperature and pressure. Critically refracted longitudinal wave technique was used for the former and pulse-echo technique for the latter. Optical microscopy and scanning electron microscopy were used to correlate the ultrasonic results with the microstructure of the steel and to provide better insight into the steel behavior. The results of the investigation indicate that frequency analysis of the defect echo, determined using the pulse-echo technique at regular intervals of time, appears to be a promising tool for monitoring defect growth induced by a high temperature and high pressure hydrogen-related attack.

Growth of tungsten oxide nanostructures by chemical solution deposition

NASA Astrophysics Data System (ADS)

Jin, L. H.; Bai, Y.; Li, C. S.; Wang, Y.; Feng, J. Q.; Lei, L.; Zhao, G. Y.; Zhang, P. X.

2018-05-01

Tungsten oxide nanostructures were fabricated on LaAlO3 (00l) substrates by a simple chemical solution deposition. The decomposition behavior and phase formation of ammonium tungstate precursor were characterized by thermal analysis and X-ray diffraction. Moreover, the morphology and chemical state of nanostructures were analyzed by scanning electron microscopy, atomic force microscopy and X-ray photoelectron spectra. The effects of crystallization temperature on the formation of nanodots and nanowires were investigated. The results indicated that the change of nanostructures had close relationship with the crystallization temperature during the chemical solution deposition process. Under higher crystallization temperature, the square-like dots transformed into the dome-like nanodots and nanowires. Moreover high density well-ordered nanodots could be obtained on the substrate with the further increase of crystallization temperature. It also suggested that this simple chemical solution process could be used to adjust the nanostructures of tungsten oxide compounds on substrate.

Fabrication of Al/Mg/Al Composites via Accumulative Roll Bonding and Their Mechanical Properties

PubMed Central

Nie, Jinfeng; Liu, Mingxing; Wang, Fang; Zhao, Yonghao; Li, Yusheng; Cao, Yang; Zhu, Yuntian

2016-01-01

Al(1060)/Mg(AZ31)/Al(1060) multilayered composite was successfully produced using an accumulative roll bonding (ARB) process for up to four cycles at an elevated temperature (400 °C). The microstructure evolution of the composites and the bonding characteristics at the interfaces between Al and Mg layers with increasing ARB cycles were characterized through optical microscopy, field emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM). It was found that the grains of Al and Mg layers were significantly refined and Al3Mg2 and Al12 Mg17 intermetallic compound layers formed at the Al/Mg bonding interfaces. The strength increased gradually and the ultimate tensile strength (UTS) reached a maximum value of about 240 MPa at the third pass. Furthermore, the strengthening mechanism of the composite was analyzed based on the fracture morphologies. PMID:28774072

Low-Cycle Fatigue Properties of P92 Ferritic-Martensitic Steel at Elevated Temperature

NASA Astrophysics Data System (ADS)

Zhang, Zhen; Hu, ZhengFei; Schmauder, Siegfried; Mlikota, Marijo; Fan, KangLe

2016-04-01

The low-cycle fatigue behavior of P92 ferritic-martensitic steel and the corresponding microstructure evolution at 873 K has been extensively studied. The test results of fatigue lifetime are consistent with the Coffin-Manson relationship over a range of controlled total strain amplitudes from 0.15 to 0.6%. The influence of strain amplitude on the fatigue crack initiation and growth has been observed using optical microscopy and scanning electron microscopy. The formation mechanism of secondary cracks is established according to the observation of fracture after fatigue process and there is an intrinsic relationship between striation spacing, current crack length, and strain amplitude. Transmission electron microscopy has been employed to investigate the microstructure evolution after fatigue process. It indicates the interaction between carbides and dislocations together with the formation of cell structure inhibits the cyclic softening. The low-angle sub-boundary elimination in the martensite is mainly caused by the cyclic stress.

High-temperature frictional wear behavior of MCrAlY-based coatings deposited by atmosphere plasma spraying

NASA Astrophysics Data System (ADS)

Tao, Chong; Wang, Lei; Song, Xiu

2017-02-01

Al2O3-Cr2O3/NiCoCrAlYTa coatings were prepared via atmosphere plasma spraying (APS). The microstructure and phase composition of the coatings were analyzed by X-ray diffraction (XRD), scanning electron microscopy (SEM), laser confocal scanning microscopy (LSCM), and transmission electron microscopy (TEM). The dry frictional wear behavior of the coatings at 500°C in static air was investigated and compared with that of 0Cr25Ni20 steel. The results show that the coatings comprise the slatted layers of oxide phases, unmelted particles, and pores. The hot abrasive resistance of the coatings is enhanced compared to that of 0Cr25Ni20, and their mass loss is approximately one-fifteenth that of 0Cr25Ni20 steel. The main wear failure mechanisms of the coatings are abrasive wear, fatigue wear, and adhesive wear.

Room-Temperature Multiferroics and Thermal Conductivity of 0.85BiFe1-2xTixMgxO3-0.15CaTiO3 Epitaxial Thin Films (x = 0.1 and 0.2).

PubMed

Zhang, Ji; Sun, Wei; Zhao, Jiangtao; Sun, Lei; Li, Lei; Yan, Xue-Jun; Wang, Ke; Gu, Zheng-Bin; Luo, Zhen-Lin; Chen, Yanbin; Yuan, Guo-Liang; Lu, Ming-Hui; Zhang, Shan-Tao

2017-08-02

Thin films of 0.85BiFe 1-2x Ti x Mg x O 3 -0.15CaTiO 3 (x = 0.1 and 0.2, abbreviated to C-1 and C-2, respectively) have been fabricated on (001) SrTiO 3 substrate with and without a conductive La 0.7 Sr 0.3 MnO 3 buffer layer. The X-ray θ-2θ and ϕ scans, atomic force microscopy, and cross-sectional transmission electron microscopy confirm the (001) epitaxial nature of the thin films with very high growth quality. Both the C-1 and C-2 thin films show well-shaped magnetization-magnetic field hysteresis at room temperature, with enhanced switchable magnetization values of 145.3 and 42.5 emu/cm 3 , respectively. The polarization-electric loops and piezoresponse force microscopy measurements confirm the room-temperature ferroelectric nature of both films. However, the C-1 films illustrate a relatively weak ferroelectric behavior and the poled states are easy to relax, whereas the C-2 films show a relatively better ferroelectric behavior with stable poled states. More interestingly, the room-temperature thermal conductivity of C-1 and C-2 films are measured to be 1.10 and 0.77 W/(m·K), respectively. These self-consistent multiferroic properties and thermal conductivities are discussed by considering the composition-dependent content and migration of Fe-induced electrons and/or charged point defects. This study not only provides multifunctional materials with excellent room-temperature magnetic, ferroelectric, and thermal conductivity properties but may also stimulate further work to develop BiFeO 3 -based materials with unusual multifunctional properties.

Preparation of meta-stable phases of barium titanate by Sol-hydrothermal method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Selvaraj, Mahalakshmi; Department of Material Science, School of Chemistry, Madurai Kamaraj University, Tamilnadu Madurai-625 021; Venkatachalapathy, V.

2015-11-15

Two low-cost chemical methods of sol–gel and the hydrothermal process have been strategically combined to fabricate barium titanate (BaTiO{sub 3}) nanopowders. This method was tested for various synthesis temperatures (100 °C to 250 °C) employing barium dichloride (BaCl{sub 2}) and titanium tetrachloride (TiCl{sub 4}) as precursors and sodium hydroxide (NaOH) as mineralizer for synthesis of BaTiO{sub 3} nanopowders. The as-prepared BaTiO{sub 3} powders were investigated for structural characteristics using x-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The overall analysis indicates that the hydrothermal conditions create a gentle environment to promote the formation of crystalline phasemore » directly from amorphous phase at the very low processing temperatures investigated. XRD analysis showed phase transitions from cubic - tetragonal - orthorhombic - rhombohedral with increasing synthesis temperature and calculated grain sizes were 34 – 38 nm (using the Scherrer formula). SEM and TEM analysis verified that the BaTiO{sub 3} nanopowders synthesized by this method were spherical in shape and about 114 - 170 nm in size. The particle distribution in both SEM and TEM shows that as the reaction temperature increases from 100 °C to 250 °C, the particles agglomerate. Selective area electron diffraction (SAED) shows that the particles are crystalline in nature. The study shows that choosing suitable precursor and optimizing pressure and temperature; different meta-stable (ferroelectric) phases of undoped BaTiO{sub 3} nanopowders can be stabilized by the sol-hydrothermal method.« less

Facile preparation of dendritic Ag-Pd bimetallic nanostructures on the surface of Cu foil for application as a SERS-substrate

NASA Astrophysics Data System (ADS)

Yi, Zao; Tan, Xiulan; Niu, Gao; Xu, Xibin; Li, Xibo; Ye, Xin; Luo, Jiangshan; Luo, Binchi; Wu, Weidong; Tang, Yongjian; Yi, Yougen

2012-05-01

Dendritic Ag-Pd bimetallic nanostructures have been synthesized on the surface of Cu foil via a multi-stage galvanic replacement reaction (MGRR) of Ag dendrites in a Na2PdCl4 solution. After five stages of replacement reaction, one obtained structures with protruding Ag-Pd flakes; these will mature into many porous structures with a few Ag atoms that are left over dendrites. The dendritic Ag-Pd bimetallic nanostructures were characterized by transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), field emission scanning electron microscopy (FESEM), energy-dispersive X-ray (EDX), selected area electron diffraction (SAED) and X-ray photoelectron spectroscopy (XPS). The morphology of the products strongly depended on the stage of galvanic replacement reaction and reaction temperature. The morphology and composition-dependent surface-enhanced Raman scattering (SERS) of the as-synthesized Ag-Pd bimetallic nanostructures were investigated. The effectiveness of these dendritic Ag-Pd bimetallic nanostructures on the surface of Cu foil as substrates toward SERS detection was evaluated by using rhodamine 6G (R6G) as a probe molecule. The results indicate that as-synthesized dendritic Ag-Pd bimetallic nanostructures are good candidates for SERS spectroscopy.

Effect of screw threading dislocations and inverse domain boundaries in GaN on the shape of reciprocal-space maps.

PubMed

Barchuk, Mykhailo; Motylenko, Mykhaylo; Lukin, Gleb; Pätzold, Olf; Rafaja, David

2017-04-01

The microstructure of polar GaN layers, grown by upgraded high-temperature vapour phase epitaxy on [001]-oriented sapphire substrates, was studied by means of high-resolution X-ray diffraction and transmission electron microscopy. Systematic differences between reciprocal-space maps measured by X-ray diffraction and those which were simulated for different densities of threading dislocations revealed that threading dislocations are not the only microstructure defect in these GaN layers. Conventional dark-field transmission electron microscopy and convergent-beam electron diffraction detected vertical inversion domains as an additional microstructure feature. On a series of polar GaN layers with different proportions of threading dislocations and inversion domain boundaries, this contribution illustrates the capability and limitations of coplanar reciprocal-space mapping by X-ray diffraction to distinguish between these microstructure features.

Stable tetragonal phase and magnetic properties of Fe-doped HfO2 nanoparticles

NASA Astrophysics Data System (ADS)

Sales, T. S. N.; Cavalcante, F. H. M.; Bosch-Santos, B.; Pereira, L. F. D.; Cabrera-Pasca, G. A.; Freitas, R. S.; Saxena, R. N.; Carbonari, A. W.

2017-05-01

In this paper, the effect in structural and magnetic properties of iron doping with concentration of 20% in hafnium dioxide (HfO2) nanoparticles is investigated. HfO2 is a wide band gap oxide with great potential to be used as high-permittivity gate dielectrics, which can be improved by doping. Nanoparticle samples were prepared by sol-gel chemical method and had their structure, morphology, and magnetic properties, respectively, investigated by X-ray diffraction (XRD), transmission electron microscopy (TEM) and scanning electron microscopy (SEM) with electron back scattering diffraction (EBSD), and magnetization measurements. TEM and SEM results show size distribution of particles in the range from 30 nm to 40 nm with small dispersion. Magnetization measurements show the blocking temperature at around 90 K with a strong paramagnetic contribution. XRD results show a major tetragonal phase (94%).

On the growth mechanisms of polar (100) surfaces of ceria on copper (100)

NASA Astrophysics Data System (ADS)

Hackl, Johanna; Duchoň, Tomáš; Gottlob, Daniel M.; Cramm, Stefan; Veltruská, Kateřina; Matolín, Vladimír; Nemšák, Slavomír; Schneider, Claus M.

2018-05-01

We present a study of temperature dependent growth of nano-sized ceria islands on a Cu (100) substrate. Low-energy electron microscopy, micro-electron diffraction, X-ray absorption spectroscopy, and photoemission electron microscopy are used to determine the morphology, shape, chemical state, and crystal structure of the grown islands. Utilizing real-time observation capabilities, we reveal a three-way interaction between the ceria, substrate, and local oxygen chemical potential. The interaction manifests in the reorientation of terrace boundaries on the Cu (100) substrate, characteristic of the transition between oxidized and metallic surface. The reorientation is initiated at nucleation sites of ceria islands, whose growth direction is influenced by the proximity of the terrace boundaries. The grown ceria islands were identified as fully stoichiometric CeO2 (100) surfaces with a (2 × 2) reconstruction.

Sensing Properties of a Novel Temperature Sensor Based on Field Assisted Thermal Emission.

PubMed

Pan, Zhigang; Zhang, Yong; Cheng, Zhenzhen; Tong, Jiaming; Chen, Qiyu; Zhang, Jianpeng; Zhang, Jiaxiang; Li, Xin; Li, Yunjia

2017-02-27

The existing temperature sensors using carbon nanotubes (CNTs) are limited by low sensitivity, complicated processes, or dependence on microscopy to observe the experimental results. Here we report the fabrication and successful testing of an ionization temperature sensor featuring non-self-sustaining discharge. The sharp tips of nanotubes generate high electric fields at relatively low voltages, lowering the work function of electrons emitted by CNTs, and thereby enabling the safe operation of such sensors. Due to the temperature effect on the electron emission of CNTs, the collecting current exhibited an exponential increase with temperature rising from 20 °C to 100 °C. Additionally, a higher temperature coefficient of 0.04 K -1 was obtained at 24 V voltage applied on the extracting electrode, higher than the values of other reported CNT-based temperature sensors. The triple-electrode ionization temperature sensor is easy to fabricate and converts the temperature change directly into an electrical signal. It shows a high temperature coefficient and good application potential.

Sensing Properties of a Novel Temperature Sensor Based on Field Assisted Thermal Emission

PubMed Central

Pan, Zhigang; Zhang, Yong; Cheng, Zhenzhen; Tong, Jiaming; Chen, Qiyu; Zhang, Jianpeng; Zhang, Jiaxiang; Li, Xin; Li, Yunjia

2017-01-01

The existing temperature sensors using carbon nanotubes (CNTs) are limited by low sensitivity, complicated processes, or dependence on microscopy to observe the experimental results. Here we report the fabrication and successful testing of an ionization temperature sensor featuring non-self-sustaining discharge. The sharp tips of nanotubes generate high electric fields at relatively low voltages, lowering the work function of electrons emitted by CNTs, and thereby enabling the safe operation of such sensors. Due to the temperature effect on the electron emission of CNTs, the collecting current exhibited an exponential increase with temperature rising from 20 °C to 100 °C. Additionally, a higher temperature coefficient of 0.04 K−1 was obtained at 24 V voltage applied on the extracting electrode, higher than the values of other reported CNT-based temperature sensors. The triple-electrode ionization temperature sensor is easy to fabricate and converts the temperature change directly into an electrical signal. It shows a high temperature coefficient and good application potential. PMID:28264427

Thermal stability and reduction of iron oxide nanowires at moderate temperatures.

PubMed

Paolone, Annalisa; Angelucci, Marco; Panero, Stefania; Betti, Maria Grazia; Mariani, Carlo

2014-01-01

The thermal stability of iron oxide nanowires, which were obtained with a hard template method and are promising elements of Li-ion based batteries, has been investigated by means of thermogravimetry, infrared and photoemission spectroscopy measurements. The chemical state of the nanowires is typical of the Fe2O3 phase and the stoichiometry changes towards a Fe3O4 phase by annealing above 440 K. The shape and morphology of the nanowires is not modified by moderate thermal treatment, as imaged by scanning electron microscopy. This complementary spectroscopy-microscopy study allows to assess the temperature limits of these Fe2O3 nanowires during operation, malfunctioning or abuse in advanced Li-ion based batteries.

Concept for room temperature single-spin tunneling force microscopy with atomic spatial resolution

NASA Astrophysics Data System (ADS)

Payne, Adam

A study of a force detected single-spin magnetic resonance measurement concept with atomic spatial resolution is presented. The method is based upon electrostatic force detection of spin-selection rule controlled single electron tunneling between two electrically isolated paramagnetic states. Single-spin magnetic resonance detection is possible by measuring the force detected tunneling charge noise on and off spin resonance. Simulation results of this charge noise, based upon physical models of the tunneling and spin physics, are directly compared to measured atomic force microscopy (AFM) system noise. The results show that the approach could provide single-spin measurement of electrically isolated defect states with atomic spatial resolution at room temperature.

Microstructures responsible for the invar and permalloy effects in Fe-Ni alloys

NASA Astrophysics Data System (ADS)

Ustinovshchikov, Yu. I.; Shabanova, I. N.; Lomova, N. V.

2015-05-01

The experimental studies of Fe68Ni32 and Fe23Ni77 alloys by transmission electron microscopy and X-ray electron spectroscopy show that the ordering-separation phase transition in these alloys occurs in a temperature range near 600°C. At temperatures higher than the transition temperature, the ordering energy of the alloy is positive, and the structures contain clusters enriched in one of the components. After heat treatment at the temperatures where the invar effect in the Fe68Ni32 alloy is maximal, a modulated microstructure forms. Below the transition temperature, the ordering energy is negative, which provides a tendency to formation of chemical compounds. After aging at these temperatures (where the Fe23Ni77 alloy exhibits high permalloy properties), highly dispersed completely coherent particles of the FeNi3 phase with structure L12 precipitate in a solid solution.

In vitro corrosion resistance of plasma source ion nitrided austenitic stainless steels.

PubMed

Le, M K; Zhu, X M

2001-04-01

Plasma source ion nitriding has emerged as a low-temperature, low-pressure nitriding approach for low-energy implanting nitrogen ions and then diffusing them into steel and alloy. In this work, a single high nitrogen face-centered-cubic (f.c.c.) phase (gammaN) formed on the 1Cr18Ni9Ti and AISI 316L austenitic stainless steels with a high nitrogen concentration of about 32 at % was characterized using Auger electron spectroscopy, electron probe microanalysis, glancing angle X-ray diffraction, and transmission electron microscopy. The corrosion resistance of the gammaN-phase layer was studied by the electrochemical cyclic polarization measurement in Ringer's solutions buffered to pH from 3.5 to 7.2 at a temperature of 37 degrees C. No pitting corrosion in the Ringer's solutions with pH = 7.2 and 5.5 was detected for the gammaN-phase layers on the two stainless steels. The high pitting potential for the gammaN-phase layers is higher, about 500 and 600 mV, above that of the two original stainless steels, respectively, in the Ringer's solution with pH = 3.5. The corroded surface morphologies of the gammaN-phase layers observed by scanning electron microscopy are consistent with the results of the electrochemical polarization measurement.

Simultaneous First-Order Valence and Oxygen Vacancy Order/Disorder Transitions in (Pr 0.85 Y 0.15 ) 0.7 Ca 0.3 CoO 3-δ via Analytical Transmission Electron Microscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gulec, Ahmet; Phelan, Daniel; Leighton, Chris

Perovskite cobaltites have been studied for years as some of the few solids to exhibit thermally driven spin-state crossovers. The unanticipated first-order spin and electronic transitions recently discovered in Pr-based cobaltites are notably different from these conventional crossovers, and are understood in terms of a unique valence transition. In essence, the Pr valence is thought to spontaneously shift from 3+ toward 4+ on cooling, driving subsequent transitions in Co valence and electronic/magnetic properties. Here, we apply temperature-dependent transmission electron microscopy and spectroscopy to study this phenomenon, for the first time with atomic spatial resolution, in the prototypical (Pr 0.85Y 0.15)(0.70)more » Ca 0.30CoO 3-δ. In addition to the direct spectroscopic observation of charge transfer between Pr and Co at the 165 K transition (on both the Pr and O edges), we also find a simultaneous order/disorder transition associated with O vacancies. Remarkably, the first-order valence change drives a transition between ordered and random O vacancies, at constant O vacancy density, demonstrating reversible crystallization of such vacancies even at cryogenic temperatures.« less

Microstructural evolution and magnetic properties of ultrafine solute-atom particles formed in a Cu75-Ni20-Fe5 alloy on isothermal annealing

NASA Astrophysics Data System (ADS)

Kim, Jun-Seop; Takeda, Mahoto; Bae, Dong-Sik

2016-12-01

Microstructural features strongly affect magnetism in nano-granular magnetic materials. In the present work we have investigated the relationship between the magnetic properties and the self-organized microstructure formed in a Cu75-Ni20-Fe5 alloy comprising ferromagnetic elements and copper atoms. High resolution transmission electron microscopy (HRTEM) observations showed that on isothermal annealing at 873 K, nano-scale solute (Fe,Ni)-rich clusters initially formed with a random distribution in the Cu-rich matrix. Superconducting quantum interference device (SQUID) measurements revealed that these ultrafine solute clusters exhibited super-spinglass and superparamagnetic states. On further isothermal annealing the precipitates evolved to cubic or rectangular ferromagnetic particles and aligned along the <100> directions of the copper-rich matrix. Electron energy-band calculations based on the first-principle Korringa-Kohn-Rostocker (KKR) method were also implemented to investigate both the electronic structure and the magnetic properties of the alloy. Inputting compositions obtained experimentally by scanning transmission electron microscopy-electron dispersive X-ray spectroscopy (STEM-EDS) analysis, the KKR calculation confirmed that ferromagnetic precipitates (of moment 1.07μB per atom) formed after annealing for 2 × 104 min. Magneto-thermogravimetric (MTG) analysis determined with high sensitivity the Curie temperatures and magnetic susceptibility above room temperature of samples containing nano-scale ferromagnetic particles.

Correlating electronic transport to atomic structures in self-assembled quantum wires.

PubMed

Qin, Shengyong; Kim, Tae-Hwan; Zhang, Yanning; Ouyang, Wenjie; Weitering, Hanno H; Shih, Chih-Kang; Baddorf, Arthur P; Wu, Ruqian; Li, An-Ping

2012-02-08

Quantum wires, as a smallest electronic conductor, are expected to be a fundamental component in all quantum architectures. The electronic conductance in quantum wires, however, is often dictated by structural instabilities and electron localization at the atomic scale. Here we report on the evolutions of electronic transport as a function of temperature and interwire coupling as the quantum wires of GdSi(2) are self-assembled on Si(100) wire-by-wire. The correlation between structure, electronic properties, and electronic transport are examined by combining nanotransport measurements, scanning tunneling microscopy, and density functional theory calculations. A metal-insulator transition is revealed in isolated nanowires, while a robust metallic state is obtained in wire bundles at low temperature. The atomic defects lead to electron localizations in isolated nanowire, and interwire coupling stabilizes the structure and promotes the metallic states in wire bundles. This illustrates how the conductance nature of a one-dimensional system can be dramatically modified by the environmental change on the atomic scale. © 2012 American Chemical Society

Preparation of nickel oxide thin films at different annealing temperature by sol-gel spin coating method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Abdullah, M. A. R., E-mail: ameerridhwan89@gmail.com; Mamat, M. H., E-mail: hafiz-030@yahoo.com; Ismail, A. S., E-mail: kyrin-samaxi@yahoo.com

2016-07-06

Preparation of NiO thin films at different annealing temperature by sol-gel method was conducted to synthesize the quality of the surface thin films. The effects of annealing temperature on the surface topology were systematically investigated. Our studies confirmed that the surface roughness of the thin films was increased whenever annealing temperature was increase. NiO thin films morphology structure analysis was confirmed by field emission scanning electron microscope. Surface roughness of the thin films was investigated by atomic force microscopy.

A study on the stability and green synthesis of silver nanoparticles using Ziziphora tenuior (Zt) extract at room temperature.

PubMed

Sadeghi, Babak; Gholamhoseinpoor, F

2015-01-05

Biomolecules present in plant extracts can be used to reduce metal ions to nanoparticles in a single-step green synthesis process. This biogenic reduction of metal ion to base metal is quite rapid, readily conducted at room temperature and pressure, and easily scaled up. Mediated Synthesis by plant extracts is environmentally benign. The involved reducing agents include the various water soluble plant metabolites (e.g. alkaloids, phenolic compounds, terpenoids) and co-enzymes. Silver (Ag) nanoparticles have the particular focus of plant-based syntheses. Extracts of a diverse range of Ziziphora tenuior (Zt) have been successfully used in making nanoparticles. The aim of this study was to investigate the antioxidant properties of this plant and its ability to synthesize silver nanoparticles. Z.tenuior leaves were used to prepare the aqueous extract for this study. Silver nanoparticles were characterized with different techniques such as UV-vis spectroscopy, Fourier transform infrared (FT-IR) spectroscopy, X-ray diffraction (XRD), Scanning electron microscopy (SEM), and transmission electron microscopy (TEM). Transmission electron microscopy experiments showed that these nanoparticles are spherical and uniformly distributed and its size is from 8 to 40 nm. FT-IR spectroscopy revealed that silver nanoparticles were functionalized with biomolecules that have primary amine group (NH₂), carbonyl group, -OH groups and other stabilizing functional groups. X-ray diffraction pattern showed high purity and face centered cubic structure of silver nanoparticles with size of 38 nm. In addition to plant extracts, live plants can be used for the synthesis. Here were view the methods of making nanoparticles using plant extracts. The scanning electron microscopy (SEM) implies the right of forming silver nanoparticles. The results of TEM, SEM, FT-IR, UV-VIS and XRD confirm that the leaves extract of Zt can synthesis silver nanoparticles. Copyright © 2014 Elsevier B.V. All rights reserved.

Fabrication and characterization of poly(L-lactic acid) gels induced by fibrous complex crystallization with solvents

DOE Office of Scientific and Technical Information (OSTI.GOV)

Matsuda, Yasuhiro; Fukatsu, Akinobu; Wang, Yangyang

2014-01-01

Complex crystal induced gelation of poly(L-lactic acid) (PLLA) solutions was studied for a series of solvents, including N,N-dimethylformamide (DMF). By cooling the solutions prepared at elevated temperatures, PLLA gels were produced in solvents that induced complex crystals ( -crystals) with PLLA. Fibrous structure of PLLA in the gel with DMF was observed by polarizing optical microscopy, field emission electron microscopy, and atomic force microscopy. Upon heating, the crystal form of PLLA in the DMF gel changed from -crystal to a-crystal, the major crystal form in common untreated PLLA films, but the morphology and high elastic modulus of the gel remainedmore » until the a-crystal dissolved at higher temperature. In addition, a solvent exchanging method was developed, which allowed PLLA gels to be prepared in other useful solvents that do not induce -crystals without losing the morphology and mechanical properties.« less

Graphene on silicon dioxide via carbon ion implantation in copper with PMMA-free transfer

NASA Astrophysics Data System (ADS)

Lehnert, Jan; Spemann, Daniel; Hamza Hatahet, M.; Mändl, Stephan; Mensing, Michael; Finzel, Annemarie; Varga, Aron; Rauschenbach, Bernd

2017-06-01

In this work, a synthesis method for the growth of low-defect large-area graphene using carbon ion beam implantation into metallic Cu foils is presented. The Cu foils (1 cm2 in size) were pre-annealed in a vacuum at 950 °C for 2 h, implanted with 35 keV carbon ions at room temperature, and subsequently annealed at 850 °C for 2 h to form graphene layers with the layer number controlled by the implantation fluence. The graphene was then transferred to SiO2/Si substrates by a PMMA-free wet chemical etching process. The obtained regions of monolayer graphene are of ˜900 μm size. Raman spectroscopy, atomic force microscopy, scanning electron microscopy, and optical microscopy performed at room temperature demonstrated a good quality and homogeneity of the graphene layers, especially for monolayer graphene.

Growth of diamond by RF plasma-assisted chemical vapor deposition

NASA Technical Reports Server (NTRS)

Meyer, Duane E.; Ianno, Natale J.; Woollam, John A.; Swartzlander, A. B.; Nelson, A. J.

1988-01-01

A system has been designed and constructed to produce diamond particles by inductively coupled radio-frequency, plasma-assisted chemical vapor deposition. This is a low-pressure, low-temperature process used in an attempt to deposit diamond on substrates of glass, quartz, silicon, nickel, and boron nitride. Several deposition parameters have been varied including substrate temperature, gas concentration, gas pressure, total gas flow rate, RF input power, and deposition time. Analytical methods employed to determine composition and structure of the deposits include scanning electron microscopy, absorption spectroscopy, scanning Auger microprobe spectroscopy, and Raman spectroscopy. Analysis indicates that particles having a thin graphite surface, as well as diamond particles with no surface coatings, have been deposited. Deposits on quartz have exhibited optical bandgaps as high as 4.5 eV. Scanning electron microscopy analysis shows that particles are deposited on a pedestal which Auger spectroscopy indicates to be graphite. This is a phenomenon that has not been previously reported in the literature.

The effect of calcination on multi-walled carbon nanotubes produced by dc-arc discharge.

PubMed

Pillai, Sreejarani K; Augustyn, Willem G; Rossouw, Margaretha H; McCrindle, Robert I

2008-07-01

Multi-walled carbon nanotubes were synthesized by dc-arc discharge in helium atmosphere and the effect of calcination at different temperatures ranging from 300-600 degrees C was studied in detail. The degree of degradation to the structural integrity of the multi-walled carbon nanotubes during the thermal process was studied by Raman spectroscopy, Scanning electron microscopy and High resolution transmission electron microscopy. The thermal behaviour of the as prepared and calcined samples was investigated by thermogravimetric analysis. Calcination in air at 400 degrees C for 2 hours was found to be an efficient and simple method to eliminate carbonaceous impurities from the nanotube bundles with minimal damage to the tube walls and length. The impurities were oxidized at a faster rate when compared to the nanotubes and gave good yield of about 50%. The nanotubes were observed to be damaged at temperature higher than 450 degrees C. The results show that this method is less destructive when compared liquid phase oxidation with 5 M HNO3.

Behavior of oxide film at the interface between particles in sintered Al powders by pulse electric-current sintering

NASA Astrophysics Data System (ADS)

Xie, Guoqiang; Ohashi, Osamu; Song, Minghui; Furuya, Kazuo; Noda, Tetsuji

2003-03-01

The microstructure of the bonding interfaces between particles in aluminum (Al) powder sintered specimens by the pulse electric-current sintering (PECS) process was observed, using conventional transmission electron microscopy (CTEM) and high-resolution transmission electron microscopy (HRTEM). The behavior of oxide film at the interface between Al particles and its effect on properties of the sintered specimens were investigated. The results showed there were two kinds of bonding interfaces in the sintered specimens, namely, the direct metal/metal bonding and the metal/oxide film layer/metal bonding interface. By increasing the fraction of the direct metal/metal bonding interfaces, the tensile strength of the sintered specimens increased, and the electrical resistivity decreased. By increasing the loading pressure at higher sintering temperatures or increasing the sintering temperature under loading pressure, the breakdown of oxide film was promoted. The broken oxide film debris was dispersed in aluminum metal near the bonding interfaces between particles.

Nitridation of porous GaAs by an ECR ammonia plasma

NASA Astrophysics Data System (ADS)

Naddaf, M.; Hullavarad, S. S.; Ganesan, V.; Bhoraskar, S. V.

2006-02-01

The effect of surface porosity of GaAs on the nature of growth of GaN, by use of plasma nitridation of GaAs, has been investigated. Porous GaAs samples were prepared by anodic etching of n-type (110) GaAs wafers in HCl solution. Nitridation of porous GaAs samples were carried out by using an electron-cyclotron resonance-induced ammonia plasma. The formation of mixed phases of GaN was investigated using the grazing angle x-ray diffraction method. A remarkable improvement in the intensity of photoluminescence (PL) compared with that of GaN synthesized by direct nitriding of GaAs surface has been observed. The PL intensity of nitrided porous GaAs at the temperature of 380 °C was found to be about two orders of magnitude higher as compared with the directly nitrided GaAs at the temperature of 500 °C. The changes in the morphology of nitrided porous GaAs have been investigated using both scanning electron microscopy and atomic force microscopy.

Observation of stable Néel skyrmions in cobalt/palladium multilayers with Lorentz transmission electron microscopy

DOE PAGES

Pollard, Shawn D.; Garlow, Joseph A.; Yu, Jiawei; ...

2017-03-10

Néel skyrmions are of high interest due to their potential applications in a variety of spintronic devices, currently accessible in ultrathin heavy metal/ferromagnetic bilayers and multilayers with a strong Dzyaloshinskii–Moriya interaction. Here in this paper we report on the direct imaging of chiral spin structures including skyrmions in an exchange-coupled cobalt/palladium multilayer at room temperature with Lorentz transmission electron microscopy, a high-resolution technique previously suggested to exhibit no Néel skyrmion contrast. Phase retrieval methods allow us to map the internal spin structure of the skyrmion core, identifying a 25 nm central region of uniform magnetization followed by a larger regionmore » characterized by rotation from in- to out-of-plane. The formation and resolution of the internal spin structure of room temperature skyrmions without a stabilizing out-of-plane field in thick magnetic multilayers opens up a new set of tools and materials to study the physics and device applications associated with chiral ordering and skyrmions.« less

Simple fabrication process for 2D ZnO nanowalls and their potential application as a methane sensor.

PubMed

Chen, Tse-Pu; Chang, Sheng-Po; Hung, Fei-Yi; Chang, Shoou-Jinn; Hu, Zhan-Shuo; Chen, Kuan-Jen

2013-03-20

Two-dimensional (2D) ZnO nanowalls were prepared on a glass substrate by a low-temperature thermal evaporation method, in which the fabrication process did not use a metal catalyst or the pre-deposition of a ZnO seed layer on the substrate. The nanowalls were characterized for their surface morphology, and the structural and optical properties were investigated using scanning electron microscopy (SEM), X-ray diffraction (XRD), transmission electron microscopy (TEM), and photoluminescence (PL). The fabricated ZnO nanowalls have many advantages, such as low growth temperature and good crystal quality, while being fast, low cost, and easy to fabricate. Methane sensor measurements of the ZnO nanowalls show a high sensitivity to methane gas, and rapid response and recovery times. These unique characteristics are attributed to the high surface-to-volume ratio of the ZnO nanowalls. Thus, the ZnO nanowall methane sensor is a potential gas sensor candidate owing to its good performance.

Preparation and characterization of polyol assisted ultrafine Cu-Ni-Mg-Ca mixed ferrite via co-precipitation method

NASA Astrophysics Data System (ADS)

Boobalan, T.; Pavithradevi, S.; Suriyanarayanan, N.; Manivel Raja, M.; Ranjith Kumar, E.

2017-04-01

Nanocrystalline spinel ferrite of composition Cu0.2Ni0.2Mg0.2Ca0.4Fe2O4 is synthesized by wet hydroxyl co-precipitation method in ethylene glycol as chelating agent and sodium hydroxide as precipitator at pH 8. Ethylene glycol is utilized as the medium which serves as the dissolvable and in addition a complexing specialist. The synthesized particles are annealed at various temperatures. Thermogravimetric investigation affirms that at 280 °C ethylene glycol is dissipated totally and stable phase arrangement happens over 680 °C. FTIR spectra of as synthesized and annealed at 1050 °C recorded between 400 cm-1 and 4000 cm-1. Structural characterizations of all the samples are carried out by X-ray diffraction (XRD) technique. Transmission electron microscopy (TEM) and scanning electron microscopy (SEM) affirm that the particles are spherical and cubic shape with the crystallite size of 12 nm to 32 nm. Magnetic measurements are performed utilizing vibrating sample magnetometer at room temperature.

Surface Nanocrystallization and Amorphization of Dual-Phase TC11 Titanium Alloys under Laser Induced Ultrahigh Strain-Rate Plastic Deformation

PubMed Central

Luo, Sihai; Zhou, Liucheng; Wang, Xuede; Cao, Xin; Nie, Xiangfan

2018-01-01

As an innovative surface technology for ultrahigh strain-rate plastic deformation, laser shock peening (LSP) was applied to the dual-phase TC11 titanium alloy to fabricate an amorphous and nanocrystalline surface layer at room temperature. X-ray diffraction, transmission electron microscopy, and high-resolution transmission electron microscopy (HRTEM) were used to investigate the microstructural evolution, and the deformation mechanism was discussed. The results showed that a surface nanostructured surface layer was synthesized after LSP treatment with adequate laser parameters. Simultaneously, the behavior of dislocations was also studied for different laser parameters. The rapid slipping, accumulation, annihilation, and rearrangement of dislocations under the laser-induced shock waves contributed greatly to the surface nanocrystallization. In addition, a 10 nm-thick amorphous structure layer was found through HRTEM in the top surface and the formation mechanism was attributed to the local temperature rising to the melting point, followed by its subsequent fast cooling. PMID:29642379

Copper nanowire-graphene core-shell nanostructure for highly stable transparent conducting electrodes.

PubMed

Ahn, Yumi; Jeong, Youngjun; Lee, Donghwa; Lee, Youngu

2015-03-24

A copper nanowire-graphene (CuNW-G) core-shell nanostructure was successfully synthesized using a low-temperature plasma-enhanced chemical vapor deposition process at temperatures as low as 400 °C for the first time. The CuNW-G core-shell nanostructure was systematically characterized by scanning electron microscopy, transmission electron microscopy, X-ray diffraction, Raman, and X-ray photoelectron spectroscopy measurements. A transparent conducting electrode (TCE) based on the CuNW-G core-shell nanostructure exhibited excellent optical and electrical properties compared to a conventional indium tin oxide TCE. Moreover, it showed remarkable thermal oxidation and chemical stability because of the tight encapsulation of the CuNW with gas-impermeable graphene shells. The potential suitability of CuNW-G TCE was demonstrated by fabricating bulk heterojunction polymer solar cells. We anticipate that the CuNW-G core-shell nanostructure can be used as an alternative to conventional TCE materials for emerging optoelectronic devices such as flexible solar cells, displays, and touch panels.

Surface Nanocrystallization and Amorphization of Dual-Phase TC11 Titanium Alloys under Laser Induced Ultrahigh Strain-Rate Plastic Deformation.

PubMed

Luo, Sihai; Zhou, Liucheng; Wang, Xuede; Cao, Xin; Nie, Xiangfan; He, Weifeng

2018-04-06

As an innovative surface technology for ultrahigh strain-rate plastic deformation, laser shock peening (LSP) was applied to the dual-phase TC11 titanium alloy to fabricate an amorphous and nanocrystalline surface layer at room temperature. X-ray diffraction, transmission electron microscopy, and high-resolution transmission electron microscopy (HRTEM) were used to investigate the microstructural evolution, and the deformation mechanism was discussed. The results showed that a surface nanostructured surface layer was synthesized after LSP treatment with adequate laser parameters. Simultaneously, the behavior of dislocations was also studied for different laser parameters. The rapid slipping, accumulation, annihilation, and rearrangement of dislocations under the laser-induced shock waves contributed greatly to the surface nanocrystallization. In addition, a 10 nm-thick amorphous structure layer was found through HRTEM in the top surface and the formation mechanism was attributed to the local temperature rising to the melting point, followed by its subsequent fast cooling.

Study of the Reactive-element Effect in Oxidation of Fe-cr Alloys Using Transverse Section Analytical Electron Microscopy

NASA Technical Reports Server (NTRS)

King, W. E.; Ethridge, E. C.

1985-01-01

The role of trace additions of reactive elements like Y, Ce, Th, or Hf to Cr bearing alloys was studied by applying a new developed technique of transverse section analytical electron microscopy. This reactive-element effect improves the high temperature oxidation resistance of alloys by strongly reducing the high temperature oxidation rate and enhancing the adhesion of the oxide scale, however, the mechanisms for this important effect remain largely unknown. It is indicated that the presence of yttrium affects the oxidation of Fe-Cr-Y alloys in at least two ways. The reactive element alters the growth mechanism of the oxide scale as evidenced by the marked influence of the reactive element on the oxide scale microstructure. The present results also suggest that reactive-element intermetallic compounds, which internally oxidize in the metal during oxidation, act as sinks for excess vacancies thus inhibiting vacancy condensation at the scale-metal interface and possibly enhancing scale adhesion.

The application of in situ analytical transmission electron microscopy to the study of preferential intergranular oxidation in Alloy 600.

PubMed

Burke, M G; Bertali, G; Prestat, E; Scenini, F; Haigh, S J

2017-05-01

In situ analytical transmission electron microscopy (TEM) can provide a unique perspective on dynamic reactions in a variety of environments, including liquids and gases. In this study, in situ analytical TEM techniques have been applied to examine the localised oxidation reactions that occur in a Ni-Cr-Fe alloy, Alloy 600, using a gas environmental cell at elevated temperatures. The initial stages of preferential intergranular oxidation, shown to be an important precursor phenomenon for intergranular stress corrosion cracking in pressurized water reactors (PWRs), have been successfully identified using the in situ approach. Furthermore, the detailed observations correspond to the ex situ results obtained from bulk specimens tested in hydrogenated steam and in high temperature PWR primary water. The excellent agreement between the in situ and ex situ oxidation studies demonstrates that this approach can be used to investigate the initial stages of preferential intergranular oxidation relevant to nuclear power systems. Copyright © 2016 Elsevier B.V. All rights reserved.

Scanning electron microscopy of heat treated TiO2 nanotubes arrays obtained by anodic oxidation

NASA Astrophysics Data System (ADS)

Naranjo, D. I.; García-Vergara, S. J.; Blanco, S.

2017-12-01

Scanning electron microscopy was used to investigate the anatase-rutile transformation of self-organized TiO2 nanotubes obtained on titanium foil by anodizing and subsequent heat treatment. The anodizing was carried out at 20V in an 1% v/v HF acid and ethylene glycol:water (50:50) electrolyte at room temperature. The anodized samples were initially pre-heat treated at 450°C for 4 hours to modify the amorphous structure of TiO2 nanotubes into anatase structure. Then, the samples were heated between 600 to 800°C for different times, in order to promote the transformation to rutile structure. The formation of TiO2 nanotubes is evident by SEM images. Notably, when the samples are treated at high temperature, the formation of rutile crystals starts to become evident at the nanotubes located on the originally grain boundaries of the titanium. Thus, the anatase - rutile transformation has a close relationship with the microstructure of the titanium, more exactly with grain boundaries.

Heat pipe fatigue test specimen: Metallurgical evaluation

NASA Technical Reports Server (NTRS)

Walak, Steven E.; Cronin, Michael J.; Grobstein, Toni

1992-01-01

An innovative creep/fatigue test was run to simulate the temperature, mechanical load, and sodium corrosion conditions expected in a heat pipe designed to supply thermal energy to a Stirling cycle power converter. A sodium-charged Inconel 718 heat pipe with a Nickel 200 screen wick was operated for 1090 hr at temperatures between 950 K (1250 F) and 1050 K (1430 F) while being subjected to creep and fatigue loads in a servo-hydraulic testing machine. After testing, the heat pipe was sectioned and examined using optical microscopy, scanning electron microscopy, and electron microprobe analysis with wavelength dispersive x-ray spectroscopy. The analysis concentrated on evaluating topographic, microstructural, and chemical changes in the sodium exposed surfaces of the heat pipe wall and wick. Surface changes in the evaporator, condenser, and adiabatic sections of the heat pipe were examined in an effort to correlate the changes with the expected sodium environment in the heat pipe. This report describes the setup, operating conditions, and analytical results of the sodium heat pipe fatigue test.

Electrochemical performance of a thermally rearranged polybenzoxazole nanocomposite membrane as a separator for lithium-ion batteries at elevated temperature

NASA Astrophysics Data System (ADS)

Lee, Moon Joo; Hwang, Jun-Ki; Kim, Ji Hoon; Lim, Hyung-Seok; Sun, Yang-Kook; Suh, Kyung-Do; Lee, Young Moo

2016-02-01

Shape-tunable hydroxyl copolyimide (HPI) nanoparticles are fabricated by a re-precipitation method and are coated onto electrospun HPI membranes, followed by heat treatment to prepare thermally rearranged polybenzoxazole (TR-PBO) composite membranes. The morphology of HPI nanoparticles consisted of sphere and sea-squirt structures, which is controlled by changing the concentration of the stabilizer. The morphological characteristics of TR-PBO nanoparticles convert from HPI nanoparticles by heat treatment and their composite membranes is confirmed by scanning electron microscopy (SEM), transmission electron microscopy (TEM), infrared spectroscopy (ATR-IR), thermogravimetric analysis (TGA) analysis, and contact angle measurements. TGA and DSC measurements confirm the excellent thermal stability compared to Celgard, a commercial PP separator for lithium-ion batteries (LIBs). Further, TR-PBO nano-composite membranes used in coin-cell type LIBs as a separator show excellent high power density performance as compared to Celgard. This is due to the fact that sea-squirt structured nanoparticles have better electrochemical properties than sphere structured nanoparticles at high temperature.

Synthesis of highly-monodisperse spherical titania particles with diameters in the submicron range.

PubMed

Tanaka, Shunsuke; Nogami, Daisuke; Tsuda, Natsuki; Miyake, Yoshikazu

2009-06-15

Monodisperse titania spheres with particle diameters in the range 380-960 nm were successfully synthesized by hydrolysis and condensation of titanium tetraisopropoxide. The preparation was performed using ammonia or dodecylamine (DDA) as a catalyst in methanol/acetonitrile co-solvent at room temperature. The samples were characterized by powder X-ray diffraction, scanning electron microscopy, transmission electron microscopy, dynamic light scattering, and nitrogen sorption measurement. The use of DDA was effective for the synthesis of monodisperse titania spheres with low coefficient of variation. When the titania spherical particles with coefficient of variation less than 4% were obtained, the colloidal crystallization easily occurred simply by centrifugation. The monodispersity was maintained even after crystallization of the particles by high temperature annealing. The titania particles prepared using DDA had mesopores near the surface of the spheres, providing high pore accessibility to the sphere from the surface-air interface. The particle size uniformity and photocatalytic reactivity of the titania prepared using DDA were higher than those of the titania prepared using ammonia.

Self-assembled growth of MnSi~1.7 nanowires with a single orientation and a large aspect ratio on Si(110) surfaces

PubMed Central

2013-01-01

MnSi~1.7 nanowires (NWs) with a single orientation and a large aspect ratio have been formed on a Si(110) surface with the molecular beam epitaxy method by a delicate control of growth parameters, such as temperature, deposition rate, and deposition time. Scanning tunneling microscopy (STM) was employed to study the influence of these parameters on the growth of NWs. The supply of free Si atoms per unit time during the silicide reaction plays a critical role in the growth kinetics of the NWs. High growth temperature and low deposition rate are favorable for the formation of NWs with a large aspect ratio. The orientation relationship between the NWs and the reconstruction rows of the Si(110) surface suggests that the NWs grow along the 11¯0 direction of the silicon substrate. High-resolution STM and backscattered electron scanning electron microscopy images indicate that the NWs are composed of MnSi~1.7. PMID:23339353

Purification Procedures for Single-Wall Carbon Nanotubes

NASA Technical Reports Server (NTRS)

Gorelik, Olga P.; Nikolaev, Pavel; Arepalli, Sivaram

2001-01-01

This report summarizes the comparison of a variety of procedures used to purify carbon nanotubes. Carbon nanotube material is produced by the arc process and laser oven process. Most of the procedures are tested using laser-grown, single-wall nanotube (SWNT) material. The material is characterized at each step of the purification procedures by using different techniques including scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), transmission electron microscopy (TEM), Raman, X-ray diffractometry (XRD), thermogravimetric analysis (TGA), nuclear magnetic resonance (NMR), and high-performance liquid chromatography (HPLC). The identified impurities are amorphous and graphitic carbon, catalyst particle aggregates, fullerenes, and hydrocarbons. Solvent extraction and low-temperature annealing are used to reduce the amount of volatile hydrocarbons and dissolve fullerenes. Metal catalysts and amorphous as well as graphitic carbon are oxidized by reflux in acids including HCl, HNO3 and HF and other oxidizers such as H2O2. High-temperature annealing in vacuum and in inert atmosphere helps to improve the quality of SWNTs by increasing crystallinity and reducing intercalation.

An Electron Microscopy Study of Graphite Growth in Nodular Cast Irons

NASA Astrophysics Data System (ADS)

Laffont, L.; Jday, R.; Lacaze, J.

2018-04-01

Growth of graphite during solidification and high-temperature solid-state transformation has been investigated in samples cut out from a thin-wall casting which solidified partly in the stable (iron-graphite) and partly in the metastable (iron-cementite) systems. Transmission electron microscopy has been used to characterize graphite nodules in as-cast state and in samples having been fully graphitized at various temperatures in the austenite field. Nodules in the as-cast material show a twofold structure characterized by an inner zone where graphite is disoriented and an outer zone where it is well crystallized. In heat-treated samples, graphite nodules consist of well-crystallized sectors radiating from the nucleus. These observations suggest that the disoriented zone appears because of mechanical deformation when the liquid contracts during its solidification in the metastable system. During heat-treatment, the graphite in this zone recrystallizes. In turn, it can be concluded that nodular graphite growth mechanism is the same during solidification and solid-state transformation.

Simple Fabrication Process for 2D ZnO Nanowalls and Their Potential Application as a Methane Sensor

PubMed Central

Chen, Tse-Pu; Chang, Sheng-Po; Hung, Fei-Yi; Chang, Shoou-Jinn; Hu, Zhan-Shuo; Chen, Kuan-Jen

2013-01-01

Two-dimensional (2D) ZnO nanowalls were prepared on a glass substrate by a low-temperature thermal evaporation method, in which the fabrication process did not use a metal catalyst or the pre-deposition of a ZnO seed layer on the substrate. The nanowalls were characterized for their surface morphology, and the structural and optical properties were investigated using scanning electron microscopy (SEM), X-ray diffraction (XRD), transmission electron microscopy (TEM), and photoluminescence (PL). The fabricated ZnO nanowalls have many advantages, such as low growth temperature and good crystal quality, while being fast, low cost, and easy to fabricate. Methane sensor measurements of the ZnO nanowalls show a high sensitivity to methane gas, and rapid response and recovery times. These unique characteristics are attributed to the high surface-to-volume ratio of the ZnO nanowalls. Thus, the ZnO nanowall methane sensor is a potential gas sensor candidate owing to its good performance. PMID:23519350

Pore Breathing of Metal-Organic Frameworks by Environmental Transmission Electron Microscopy.

PubMed

Parent, Lucas R; Pham, C Huy; Patterson, Joseph P; Denny, Michael S; Cohen, Seth M; Gianneschi, Nathan C; Paesani, Francesco

2017-10-11

Metal-organic frameworks (MOFs) have emerged as a versatile platform for the rational design of multifunctional materials, combining large specific surface areas with flexible, periodic frameworks that can undergo reversible structural transitions, or "breathing", upon temperature and pressure changes, and through gas adsorption/desorption processes. Although MOF breathing can be inferred from the analysis of adsorption isotherms, direct observation of the structural transitions has been lacking, and the underlying processes of framework reorganization in individual MOF nanocrystals is largely unknown. In this study, we describe the characterization and elucidation of these processes through the combination of in situ environmental transmission electron microscopy (ETEM) and computer simulations. This combined approach enables the direct monitoring of the breathing behavior of individual MIL-53(Cr) nanocrystals upon reversible water adsorption and temperature changes. The ability to characterize structural changes in single nanocrystals and extract lattice level information through in silico correlation provides fundamental insights into the relationship between pore size/shape and host-guest interactions.

A parametric study of single-wall carbon nanotube growth by laser ablation

NASA Technical Reports Server (NTRS)

Arepalli, Sivaram; Holmes, William A.; Nikolaev, Pavel; Hadjiev, Victor G.; Scott, Carl D.

2004-01-01

Results of a parametric study of carbon nanotube production by the double-pulse laser oven process are presented. The effect of various operating parameters on the production of single-wall carbon nanotubes (SWCNTs) is estimated by characterizing the nanotube material using analytical techniques, including scanning electron microscopy, transmission electron microscopy, thermo gravimetric analysis and Raman spectroscopy. The study included changing the sequence of the laser pulses, laser energy, pulse separation, type of buffer gas used, operating pressure, flow rate, inner tube diameter, as well as its material, and oven temperature. It was found that the material quality and quantity improve with deviation from normal operation parameters such as laser energy density higher than 1.5 J/cm2, pressure lower than 67 kPa, and flow rates higher than 100 sccm. Use of helium produced mainly small diameter tubes and a lower yield. The diameter of SWCNTs decreases with decreasing oven temperature and lower flow rates.

Synthesis and characterization of Ce, Cu co-doped ZnS nanoparticles

NASA Astrophysics Data System (ADS)

Harish, G. S.; Sreedhara Reddy, P.

2015-09-01

Ce, Cu co-doped ZnS nanoparticles were prepared at room temperature using a chemical co-precipitation method. The prepared nanoparticles were characterized by X- ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive analysis of X-rays (EDAX), diffuse reflectance spectroscopy (DRS), photoluminescence (PL) and high resolution Raman spectroscopic techniques. Transmission electron microscopy (TEM) and X-ray diffraction studies showed that the diameter of the particles was around 2-3 nm. Broadened XRD peaks revealed the formation of nanoparticles with a face centered cubic (fcc) structure. DRS studies confirmed that the band gap increased with an increase in the dopant concentration. The Raman spectra of undoped and Ce, Cu ions co-doped ZnS nanoparticles showed longitudinal optical mode and transverse optical mode. Compared with the Raman modes (276 and 351 cm-1) of undoped ZnS nanoparticles, the Raman modes of Ce, Cu co- doped ZnS nanoparticles were slightly shifted towards lower frequency. PL spectra of the samples showed remarkable enhancement in the intensity upon doping.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chen, Limiao, E-mail: chenlimiao@csu.edu.cn; Jing, Qifeng; Chen, Jun

Silver nanostructures with dendritic, flower-like and irregular morphologies were controllably deposited on a silicon substrate in an aqueous hydrogen fluoride solution at room temperature. The morphology of the Ag nanostructures changed from dendritic to urchin-like, flowerlike and pinecone-like with increasing the concentration of polyvinyl pyrrolidone (MW = 55,000) from 2 to 10 mM. The Ag nanostructures were characterized by transmission electron microscopy, high-resolution transmission electron microscopy, scanning electron microscopy, energy-dispersive X-ray, and X-ray diffraction. Through a series of time-dependent morphological evolution studies, the growth processes of Ag nanostructures have been systematically investigated and the corresponding growth mechanisms have been discussed.more » In addition, the morphology-dependent surface-enhanced Raman scattering of as-synthesized Ag nanostructures were investigated. The results indicated that flower-like Ag nanostructure had the highest activity than the other Ag nanostructures for Rhodamine 6G probe molecules. Highlights: • A simple method was developed to prepare dendritic and flower-like Ag nanostructures. • The flower-like Ag nanoparticles exhibit highest SERS activity. • The SERS substrate based on flower-like Ag particles can be used to detect melamine.« less

Magnetic properties and transmission electron microscopy studies of Ni nanoparticles encapsulated in carbon nanocages and carbon nanotubes

DOE Office of Scientific and Technical Information (OSTI.GOV)

He Chunnian; Zhao Naiqin; Shi Chunsheng

2008-08-04

Three types of carbon nanomaterials, including bamboo-shaped carbon nanotubes with Ni encapsulated and hollow and Ni catalytic particles filled carbon nanocages, have been prepared by methane catalytic decomposition at a relatively low temperature. Transmission electron microscopy observations showed that fascinating fullerene-like Ni-C (graphitic) core-shell nanostructures predominated. Detailed examination of high-resolution transmission electron microscopy showed that the walls of bamboo-shaped carbon nanotubes with quasi-cone catalytic particles encapsulated consisted of oblique graphene planes with respect to the tube axis. The Ni particles encapsulated in the carbon nanocages were larger than that encapsulated in carbon nanotubes, but the diameters of the cores ofmore » hollow carbon nanocages were less than that of Ni particles encapsulated in carbon nanotubes, suggesting that the sizes of catalyst particles played an important role during carbon nanomaterial growth. The magnetic properties of the carbon nanomaterials were measured, which showed relatively large coercive force (H{sub c} = 138.4 O{sub e}) and good ferromagnetism (M{sub r}/M{sub s} = 0.325)« less

Formation and anisotropic magnetoresistance of Co/Pt nano-contacts through aluminum oxide barrier

NASA Astrophysics Data System (ADS)

Al-Mahdawi, Muftah; Sahashi, Masashi

2014-01-01

We report on the observation of anisotropic magnetoresistance (AMR) in vertical asymmetric nano-contacts (NCs) made through AlOx nano-oxide layer (NOL) formed by ion-assisted oxidation method in the film stack of Co/AlOx-NOL/Pt. Analysis of NC formation was based on in situ conductive atomic force microscopy and transmission electron microscopy. Depending on the purity of NCs from Al contamination, we observed up to 29% AMR ratio at room temperature.

Driving force of stacking-fault formation in SiC p-i-n diodes.

PubMed

Ha, S; Skowronski, M; Sumakeris, J J; Paisley, M J; Das, M K

2004-04-30

The driving force of stacking-fault expansion in SiC p-i-n diodes was investigated using optical emission microscopy and transmission electron microscopy. The stacking-fault expansion and properties of the partial dislocations were inconsistent with any stress as the driving force. A thermodynamic free energy difference between the perfect and a faulted structure is suggested as a plausible driving force in the tested diodes, indicating that hexagonal polytypes of silicon carbide are metastable at room temperature.

Confocal Raman and electronic microscopy studies on the topotactic conversion of calcium carbonate from Pomacea lineate shells into hydroxyapatite bioceramic materials in phosphate media.

PubMed

dePaula, S M; Huila, M F G; Araki, K; Toma, H E

2010-12-01

Conversion of Pomacea lineate shells into hydroxyapatite (HA) bioceramic materials was investigated by their in vitro treatment with phosphate solutions, at room temperature. Confocal Raman microscopy revealed that the conversion proceeds at distinct rates through the nacreous or periostracum sides of the shell. The conversion can be accelerated using powdered samples, yielding biocompatible materials of great interest in biomedicine. Copyright © 2010 Elsevier Ltd. All rights reserved.

Template confined synthesis of amorphous carbon nanotubes and its confocal Raman microscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Maity, Supratim; Roychowdhury, Tuhin; Chattopadhyay, Kalyan Kumar, E-mail: kalyan-chattopadhyay@yahoo.com

2014-04-24

Amorphous carbon nanotubes (aCNTs) were synthesized by AAO (anodic aluminum oxide) template at a temperature 500 °C in nitrogen atmosphere using the citric acid as a carbon source without the help of any catalyst particles. Morphological analysis of the as prepared samples was carried out by field emission scanning electron microscopy (FESEM). Confocal Raman imaging has been studied and an attempt has been made to find out the graphitic (sp{sup 2}) and disordered phase of the CNTs.

Surface microstructure and high temperature corrosion resistance of arc-sprayed FeCrAl coating irradiated by high current pulsed electron beam

NASA Astrophysics Data System (ADS)

Hao, Shengzhi; Zhao, Limin; He, Dongyun

2013-10-01

The surface microstructure of arc-sprayed FeCrAl coating irradiated by high current pulsed electron beam (HCPEB) with long pulse duration of 200 μs was characterized by using optical microscopy, scanning electron microscopy and X-ray diffractometry. The distribution of chemical composition in modified surface layer was measured with electron probe micro-analyzer. The high temperature corrosion resistance of FeCrAl coating was tested in a saturated Na2SO4 and K2SO4 solution at 650 °C. After HCPEB irradiation, the coarse surface of arc-sprayed coating was changed as discrete bulged nodules with smooth and compact appearance. When using low energy density of 20 J/cm2, the surface modified layer was continuous entirely with an average melting depth of ˜30 μm. In the surface remelted layer, Fe and Cr elements gave a uniform distribution, while Al and O elements agglomerated particularly at the concave part between nodule structures to form α-Al2O3 phase. After high temperature corrosion tests, the FeCrAl coating treated with HCPEB of 20 J/cm2 remained a glossy surface with weight increment of ˜51 mg/cm2, decreased by 20% as compared to the initial sample. With the increasing energy density of HCPEB irradiation, the integrity of surface modified layer got segmented due to the formation of larger bulged nodules and cracks at the concave parts. For the HCPEB irradiation of 40 J/cm2, the high temperature corrosion resistance of FeCrAl coating was deteriorated drastically.

Correlation-driven insulator-metal transition in near-ideal vanadium dioxide films

DOE PAGES

Gray, A. X.; Jeong, J.; Aetukuri, N. P.; ...

2016-03-18

We use polarization- and temperature-dependent x-ray absorption spectroscopy, in combination with photoelectron microscopy, x-ray diffraction, and electronic transport measurements, to study the driving force behind the insulator-metal transition in VO 2. We show that both the collapse of the insulating gap and the concomitant change in crystal symmetry in homogeneously strained single-crystalline VO 2 films are preceded by the purely electronic softening of Coulomb correlations within V-V singlet dimers. Furthermore, this process starts 7 K (±0.3 K) below the transition temperature, as conventionally defined by electronic transport and x-ray diffraction measurements, and sets the energy scale for driving the near-room-temperaturemore » insulator-metal transition in this technologically promising material.« less

Positron annihilation study of the interfacial defects in ZnO nanocrystals: Correlation with ferromagnetism

NASA Astrophysics Data System (ADS)

Wang, Dong; Chen, Z. Q.; Wang, D. D.; Qi, N.; Gong, J.; Cao, C. Y.; Tang, Z.

2010-01-01

High purity ZnO nanopowders were pressed into pellets and annealed in air between 100 and 1200 °C. The crystal quality and grain size of the ZnO nanocrystals were investigated by x-ray diffraction 2θ scans. Annealing induces an increase in the grain size from 25 to 165 nm with temperature increasing from 400 to 1200 °C. Scanning electron microscopy and high-resolution transmission electron microscopy observations also confirm the grain growth during annealing. Positron annihilation measurements reveal vacancy defects including Zn vacancies, vacancy clusters, and voids in the grain boundary region. The voids show an easy recovery after annealing at 100-700 °C. However, Zn vacancies and vacancy clusters observed by positrons remain unchanged after annealing at temperatures below 500 °C and begin to recover at higher temperatures. After annealing at temperatures higher than 1000 °C, no positron trapping by the interfacial defects can be observed. Raman spectroscopy studies confirm the recovery of lattice disorder after annealing. Hysteresis loops are observed for the 100 and 400 °C annealed samples, which indicate ferromagnetism in ZnO nanocrystals. However, the ferromagnetism disappears after annealing above 700 °C, suggesting that it might originate from the surface defects such as Zn vacancies.

Polymer deformation and filling modes during microembossing

NASA Astrophysics Data System (ADS)

Rowland, Harry D.; King, William P.

2004-12-01

This work investigates the initial stages of polymer deformation during hot embossing micro-manufacturing at processing temperatures near the glass transition temperature (Tg) of polymer films having sufficient thickness such that polymer flow is not supply limited. Several stages of polymer flow can be observed by employing stamp geometries of various widths and varying imprint conditions of time and temperature to modulate polymer viscosity. Experiments investigate conditions affecting cavity filling phenomena, including apparent polymer viscosity. Stamps with periodic ridges of height and width 4 µm and periodicity 30, 50 and 100 µm emboss trenches into polymethyl methacrylate films at Tg - 10 °C < Temboss < Tg + 20 °C. Imprint parameters of time, temperature and load are correlated with replicated polymer shape, height and imprinted area. Polymer replicates are measured by atomic force microscopy and inspected by scanning electron microscopy. Cavity size and the temperature dependence of polymer viscosity significantly influence the nature of polymer deformation in hot embossing micro-manufacturing and must be accounted for in rational process design.

Injectable and body temperature sensitive hydrogels based on chitosan and hyaluronic acid for pH sensitive drug release.

PubMed

Zhang, Wei; Jin, Xin; Li, Heng; Zhang, Run-Run; Wu, Cheng-Wei

2018-04-15

Hydrogels based on chitosan/hyaluronic acid/β-sodium glycerophosphate demonstrate injectability, body temperature sensitivity, pH sensitive drug release and adhesion to cancer cell. The drug (doxorubicin) loaded hydrogel precursor solutions are injectable and turn to hydrogels when the temperature is increased to body temperature. The acidic condition (pH 4.00) can trigger the release of drug and the cancer cell (Hela) can adhere to the surface of the hydrogels, which will be beneficial for tumor site-specific administration of drug. The mechanical strength, the gelation temperature, and the drug release behavior can be tuned by varying hyaluronic acid content. The mechanisms were characterized using dynamic mechanical analysis, Fourier transform infrared spectroscopy, scanning electron microscopy and fluorescence microscopy. The carboxyl group in hyaluronic acid can form the hydrogen bondings with the protonated amine in chitosan, which promotes the increase of mechanical strength of the hydrogels and depresses the initial burst release of drug from the hydrogel. Copyright © 2018 Elsevier Ltd. All rights reserved.

Sol-gel NiFe2O4 nanoparticles: Effect of the silica coating

NASA Astrophysics Data System (ADS)

Larumbe, S.; Pérez-Landazábal, J. I.; Pastor, J. M.; Gómez-Polo, C.

2012-05-01

NiFe2O4 and NiFe2O4-SiO2 nanoparticles were synthesized by a sol-gel method using citric acid as fuel, giving rise its combustion to the crystallization of the spinel phase. Different synthesis conditions were analyzed with the aim of obtaining stoichiometric NiFe2O4 nanoparticles. The spinel structure in the calcined nanoparticles (400 °C, 2 h) was evaluated by x-ray diffraction. Their nanometer size (mean diameters around 10-15 nm) was confirmed through electron microscopy (field emission scanning electron microscopy and transmission electron microscopy). Rietveld refinement indicates the existence of a small percentage of NiO and Fe3O4 phases and a certain degree of structural disorder. The main effect of the silica coating is to enhance the disorder effects and prevent the crystalline growth after post-annealing treatments. Due to the small particle size, the nanoparticles display characteristic superparamagnetic behaviour and surface effects associated to a spin-glass like state: i.e., reduction in the saturation magnetization values and splitting of the zero field cooled (ZFC)-field cooled (FC) high field magnetization curves. The fitting of the field dependence of the ZFC-FC irreversibility temperatures to the Almeida—Thouless equation confirms the spin-glass nature of the detected magnetic phenomena. Exchange bias effects (shifts in the FC hysteresis loops) detected below the estimated freezing temperature support the spin-glass nature of the spin disorder effects.

Investigation of the microstructure of metallic droplets on Ga(AsBi)/GaAs

NASA Astrophysics Data System (ADS)

Sterzer, E.; Knaub, N.; Ludewig, P.; Straubinger, R.; Beyer, A.; Volz, K.

2014-12-01

Low Bi content GaAs is a promising material for new optical devices with less heat production. The growth of such devices by metal organic vapor phase epitaxy faces several challenges. This paper summarizes results of the formation of metallic droplets during the epitaxial growth of Ga(AsBi) using all-liquid group III and V precursors. The samples that are grown, investigated by atomic force microscopy and scanning electron microscopy, show a different metal droplet distribution over the surface depending on the growth temperature and the V/III ratio of the precursors. Investigations with energy dispersive X-ray analysis and selective etching prove the appearance of phase separated Ga-Bi and pure Bi droplets at growth temperatures between 375 °C and 425 °C, which is explainable by the phase diagram of Ga-Bi. Since the pure Bi droplets show a preferred orientation on the surface after cool-down, transmission electron microscopy measurements were done by using the dark field imaging mode in addition to electron diffraction and high resolution imaging. These experiments show the single crystalline structure of the Bi droplets. The comparison of experimental diffraction patterns with image simulation shows a preferred alignment of Bi {10-1} lattice planes parallel to GaAs {202} lattice planes with the formation of a coincidence lattice. Thus it is possible to derive a model of how the Bi droplets evolve on the GaAs surface.

Realization of improved metallization-Ti/Al/Ti/W/Au ohmic contacts to n-GaN for high temperature application

NASA Astrophysics Data System (ADS)

Motayed, A.; Davydov, A. V.; Boettinger, W. J.; Josell, D.; Shapiro, A. J.; Levin, I.; Zheleva, T.; Harris, G. L.

2005-05-01

Tungsten metal layer was used for the first time as an effective diffusion barrier for the standard Ti/Al/Ti/Au ohmic metallization scheme to obtain thermally stable ohmic contact suitable for high temperature applications. Comparative studies were performed on three distinct metallization schemes: 1) standard GaN/Ti/Al/Ti/Au, 2) GaN/Ti/Al/W/Au, and 3) GaN/Ti/Al/Ti/W/Au. For the GaN with doping level of 5 × 1017 cm-3, the lowest specific contact resistance for the Ti/Al/Ti/W/Au metallization scheme annealed in argon at 750 °C for 30 sec was 5 × 10-6 .cm2, which is comparable to the standard Ti/Al/Ti/Au scheme. X-ray diffractions (XRD), auger electron spectroscopy (AES) depth profiling, field-emission scanning electron microscopy (FE-SEM), atomic force microscopy (AFM), and cross-sectional transmission electron microscopy (TEM) revealed that the Ti/Al/Ti/W/Au metallization has superior morphology and microstructural properties compared to standard Ti/Al/Ti/Au metallizations. Remarkably, this metallization was able to withstand thermal aging at 500 °C for 50 hrs with only marginal morphological and electrical deterioration. These studies revealed that the utilization of a compound diffusion barrier stack, as in the Ti/Al/Ti/W/Au metallization, yields electrically, structurally, and morphologically superior metallizations with exceptional thermal stability.

Solidification Sequence of Spray-Formed Steels

NASA Astrophysics Data System (ADS)

Zepon, Guilherme; Ellendt, Nils; Uhlenwinkel, Volker; Bolfarini, Claudemiro

2016-02-01

Solidification in spray-forming is still an open discussion in the atomization and deposition area. This paper proposes a solidification model based on the equilibrium solidification path of alloys. The main assumptions of the model are that the deposition zone temperature must be above the alloy's solidus temperature and that the equilibrium liquid fraction at this temperature is reached, which involves partial remelting and/or redissolution of completely solidified droplets. When the deposition zone is cooled, solidification of the remaining liquid takes place under near equilibrium conditions. Scanning electron microscopy (SEM) and optical microscopy (OM) were used to analyze the microstructures of two different spray-formed steel grades: (1) boron modified supermartensitic stainless steel (SMSS) and (2) D2 tool steel. The microstructures were analyzed to determine the sequence of phase formation during solidification. In both cases, the solidification model proposed was validated.

Co3O4/CoP composite hollow polyhedron: A superior catalyst with dramatic efficiency and stability for the room temperature reduction of 4-nitrophenol

NASA Astrophysics Data System (ADS)

Liu, Xing; Li, Xiangqing; Qin, Lixia; Mu, Jin; Kang, Shi-Zhao

2018-03-01

In the present work, Co3O4/CoP composite hollow polyhedrons were prepared and characterized with X-ray diffraction, scanning electron microscopy, transmission electron microscopy, X-ray photoelectron spectroscopy and N2 adsorption-desorption isotherms. Then, the catalytic activity of the as-prepared Co3O4/CoP hollow polyhedrons was evaluated for the borohydride-assisted reduction of 4-nitrophenol at room temperature. The results indicate that the as-prepared Co3O4/CoP hollow polyhedrons are an efficient recyclable catalyst for the reduction of 4-nitrophenol. When the 4-nitrophenol initial concentration is 1.0 × 10-4 mol L-1 (100 mL), almost 100% 4-nitrophenol can be reduced within 3 min in the presence of the Co3O4/CoP hollow polyhedrons. The apparent rate constant of the 4-nitrophenol reduction is 1.61 min-1 at room temperature, and the activity factor is about 5.37 × 104 mL min-1 g-1, which is almost two times higher than that over Ag nanoparticles. Finally, the catalytic mechanism was preliminarily discussed. It is found that CoP plays an important role in the catalytic process. Here, CoP serves as active sites, which leads to efficient formation of hydrogen atoms from BH4- and fast electron transfer.

Structure, Surface Morphology, and Optical and Electronic Properties of Annealed SnS Thin Films Obtained by CBD

NASA Astrophysics Data System (ADS)

Reghima, Meriem; Akkari, Anis; Guasch, Cathy; Turki-Kamoun, Najoua

2014-09-01

SnS thin films were initially coated onto Pyrex substrates by the chemical bath deposition (CBD) method and annealed at various temperatures ranging from 200°C to 600°C for 30 min in nitrogen gas. X-ray diffraction (XRD) analysis revealed that a structural transition from face-centered cubic to orthorhombic occurs when the annealing temperature is over 500°C. The surface morphology of all thin layers was investigated by means of scanning electron microscopy and atomic force microscopy. The elemental composition of Sn and S, as measured by energy dispersive spectroscopy, is near the stoichiometric ratio. Optical properties studied by means of transmission and reflection measurements show an increase in the absorption coefficient with increasing annealing temperatures. The band gap energy is close to 1.5 eV, which corresponds to the optimum for photovoltaic applications. Last, the thermally stimulated current measurements show that the electrically active traps located in the band gap disappear after annealing at 500°C. These results suggest that, once again, annealing as a post-deposition treatment may be useful for improving the physical properties of the SnS layers included in photovoltaic applications. Moreover, the thermo-stimulated current method may be of practical relevance to explore the electronic properties of more conventional industrial methods, such as sputtering and chemical vapor deposition.

Observation of defect-induced Photoresponse and charge carrier transport in single GeSe2 nanobelt devices

NASA Astrophysics Data System (ADS)

Mukherjee, Bablu; Tok, Eng Soon; Haur Sow, Chorng

2013-03-01

Single crystal GeSe2 nanobelts were grown using chemical vapor deposition techniques. Morphology of the nanostructures was characterized using scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffractometry (XRD) and Raman spectroscopy. Electronic transport properties, impedance spectroscopy, photoconductive characteristics and temperature-dependent electrical resistivity measurements were carried out on individual GeSe2 nanobelt devices. The photosensitivity of single GeSe2 nanobelt (NB) devices was examined with two different excitation wavelengths of laser beams with photon energies above band gap and at sub-band gap of the NB. A maximum photoconductive gain 106 % was achieved at a wavelength of 808 nm. The magnitude of the photocurrent and response time of the individual GeSe2 NB device indicate that the photoresponse could be attributed to the presence of isolated mid band gap defect levels. Temperature dependent photocurrent measurements indicate the rough estimation of the energy levels for the defect states. Localized photostudy shows that the large photoresponse of the device primarily occurs at the metal-NB contact regions. Department of Physics, 2 Science Drive 3, National University of Singapore (NUS), Singapore 117542

Parametric Study of Solder Flux Hygroscopicity: Impact of Weak Organic Acids on Water Layer Formation and Corrosion of Electronics

NASA Astrophysics Data System (ADS)

Piotrowska, Kamila; Ud Din, Rameez; Grumsen, Flemming Bjerg; Jellesen, Morten Stendahl; Ambat, Rajan

2018-07-01

The presence of solder flux residues on the printed circuit board assembly surface is an important factor contributing to humidity-related reliability issues that affect device lifetime. This investigation focuses on understanding the hygroscopic nature of typical wave solder flux activators—weak organic acids—under varied temperature conditions. In situ x-ray diffraction measurements assessed the effect of high temperature on the crystal structure of organic activators. The hygroscopicity studies were carried out under relative humidity (RH) levels varying from 30% to ˜ 99% and at temperatures 25°C, 40°C, and 60°C. Water absorption levels were determined using the gravimetric method, and the influence on reliability was assessed using electrochemical impedance and leak current measurements performed on the surface insulation resistance comb patterns. The corrosion studies were correlated with the hygroscopicity results and solubility data. Corrosion morphology was analysed using the optical microscopy and scanning electron microscopy. The results show that the hygroscopic nature of typical solder flux residue depends on its chemical structure and temperature. An increase of temperature shifts the critical RH level for water vapour absorption towards lower RH range, accelerating the formation of a conductive electrolyte and the occurrence of ion transport-induced electrochemical migration. The overall ranking of flux activators with the increasing order of aggressivity is: palmitic < suberic < adipic < succinic < glutaric < dl-malic acid.

Synthesis of stable TiO2 nanotubes: effect of hydrothermal treatment, acid washing and annealing temperature.

PubMed

López Zavala, Miguel Ángel; Lozano Morales, Samuel Alejandro; Ávila-Santos, Manuel

2017-11-01

Effect of hydrothermal treatment, acid washing and annealing temperature on the structure and morphology of TiO 2 nanotubes during the formation process was assessed. X-ray diffraction, scanning electron microscopy (SEM), transmission electron microscopy (TEM) and energy dispersive X-ray spectroscopy analysis were conducted to describe the formation and characterization of the structure and morphology of nanotubes. Hydrothermal treatment of TiO 2 precursor nanoparticles and acid washing are fundamental to form and define the nanotubes structure. Hydrothermal treatment causes a change in the crystallinity of the precursor nanoparticles from anatase phase to a monoclinic phase, which characterizes the TiO 2 nanosheets structure. The acid washing promotes the formation of high purity nanotubes due to Na + is exchanged from the titanate structure to the hydrochloric acid (HCl) solution. The annealing temperature affects the dimensions, structure and the morphology of the nanotubes. Annealing temperatures in the range of 400 °C and 600 °C are optimum to maintain a highly stable tubular morphology of nanotubes. Additionally, nanotubes conserve the physicochemical properties of the precursor Degussa P25 nanoparticles. Temperatures greater than 600 °C alter the morphology of nanotubes from tubular to an irregular structure of nanoparticles, which are bigger than those of the precursor material, i.e., the crystallinity turn from anatase phase to rutile phase inducing the collapse of the nanotubes.

Parametric Study of Solder Flux Hygroscopicity: Impact of Weak Organic Acids on Water Layer Formation and Corrosion of Electronics

NASA Astrophysics Data System (ADS)

Piotrowska, Kamila; Ud Din, Rameez; Grumsen, Flemming Bjerg; Jellesen, Morten Stendahl; Ambat, Rajan

2018-04-01

The presence of solder flux residues on the printed circuit board assembly surface is an important factor contributing to humidity-related reliability issues that affect device lifetime. This investigation focuses on understanding the hygroscopic nature of typical wave solder flux activators—weak organic acids—under varied temperature conditions. In situ x-ray diffraction measurements assessed the effect of high temperature on the crystal structure of organic activators. The hygroscopicity studies were carried out under relative humidity (RH) levels varying from 30% to ˜ 99% and at temperatures 25°C, 40°C, and 60°C. Water absorption levels were determined using the gravimetric method, and the influence on reliability was assessed using electrochemical impedance and leak current measurements performed on the surface insulation resistance comb patterns. The corrosion studies were correlated with the hygroscopicity results and solubility data. Corrosion morphology was analysed using the optical microscopy and scanning electron microscopy. The results show that the hygroscopic nature of typical solder flux residue depends on its chemical structure and temperature. An increase of temperature shifts the critical RH level for water vapour absorption towards lower RH range, accelerating the formation of a conductive electrolyte and the occurrence of ion transport-induced electrochemical migration. The overall ranking of flux activators with the increasing order of aggressivity is: palmitic < suberic < adipic < succinic < glutaric < uc(dl)-malic acid.

Electric property measurement of free-standing SrTiO3 nanoparticles assembled by dielectrophoresis

NASA Astrophysics Data System (ADS)

Budiman, Faisal; Kotooka, Takumi; Horibe, Yoichi; Eguchi, Masanori; Tanaka, Hirofumi

2018-06-01

Free-standing strontium titanate (SrTiO3/STO) nanoparticles (NPs) were synthesized by the sol–gel method. X-ray diffractometry revealed that the required minimum annealing temperature to synthesize pure and highly crystalline STO NPs was 500 °C. Moreover, morphological observation by field emission scanning electron microscopy showed that the STO NPs have a spherical structure and their size depended on annealing condition. Electrical properties were measured using a low-temperature probing system. Here, an electrode was fabricated by electron beam lithography and the synthesized STO NPs were aligned at the electrodes by dielectrophoresis. The conductance of a sample was proportional to temperature. Two conduction mechanisms originating from hopping and tunneling appeared in the Arrhenius plot.

SRB seawater corrosion project

NASA Technical Reports Server (NTRS)

Bozack, M. J.

1991-01-01

The corrosion behavior of 2219 aluminum when exposed to seawater was characterized. Controlled corrosion experiments at three different temperatures (30, 60 and 100 C) and two different environments (seawater and 3.5 percent salt solution) were designed to elucidate the initial stages in the corrosion process. It was found that 2219 aluminum is an active catalytic surface for growth of Al2O3, NaCl, and MgO. Formation of Al2O3 is favored at lower temperatures, while MgO is favored at higher temperatures. Visible corrosion products are formed within 30 minutes after seawater exposure. Corrosion characteristics in 3.5 percent salt solution are different than corrosion in seawater. Techniques utilized were: (1) scanning electron microscopy, (2) energy dispersive x-ray spectroscopy, and (3) Auger electron spectroscopy.

The Structure, Function and Evolution of a Novel Form of Fluid-feeding Apparatus for Microbivory

USDA-ARS?s Scientific Manuscript database

Low temperature scanning electron microscopy (LT-SEM) has revealed anatomical details suggesting that Osperalycus and Gordialycus (Acariformes: Nematalycidae) have an unusual feeding apparatus that appears to be specialized for feeding on the fluid contents of small microorganisms (diameter '5 µm). ...

Electroluminescence of hot electrons in AlGaN/GaN high-electron-mobility transistors under radio frequency operation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Brazzini, Tommaso, E-mail: tommaso.brazzini@bristol.ac.uk; Sun, Huarui; Uren, Michael J.

2015-05-25

Hot electrons in AlGaN/GaN high electron mobility transistors are studied during radio frequency (RF) and DC operation by means of electroluminescence (EL) microscopy and spectroscopy. The measured EL intensity is decreased under RF operation compared to DC at the same average current, indicating a lower hot electron density. This is explained by averaging the DC EL intensity over the measured load line used in RF measurements, giving reasonable agreement. In addition, the hot electron temperature is lower by up to 15% under RF compared to DC, again at least partially explainable by the weighted averaging along the specific load line.more » However, peak electron temperature under RF occurs at high V{sub DS} and low I{sub DS} where EL is insignificant suggesting that any wear-out differences between RF and DC stress of the devices will depend on the balance between hot-carrier and field driven degradation mechanisms.« less

Porous Ni-Mn oxide nanosheets in situ formed on nickel foam as 3D hierarchical monolith de-NOx catalysts

NASA Astrophysics Data System (ADS)

Cai, Sixiang; Zhang, Dengsong; Shi, Liyi; Xu, Jing; Zhang, Lei; Huang, Lei; Li, Hongrui; Zhang, Jianping

2014-06-01

In this work, we successfully in situ decorated nickel foam with porous Ni-Mn oxide nanosheets (3DH-NM/NF) as 3D hierarchical monolith de-NOx catalysts via a simple hydrothermal reaction and calcination process. The catalysts were carefully examined by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, elemental mapping, X-ray photoelectron spectroscopy, H2 temperature-programmed reduction and NH3 temperature-programmed desorption measurements. The results indicated that the nanosheets are composed of a Ni6Mn1O8 spinel and the metal species are uniformly dispersed in bi-metal oxides. As a result, the strong synergistic effects between the Mn and Ni species have been observed. The active oxygen species, reducible species and acidity are enhanced by the in situ formation of the nanosheets on the surface of nickel foam. These desirable features of 3DH-NM/NF catalysts bring about the excellent de-NOx performance. Moreover, the 3DH-NM/NF catalysts also present good stability and H2O resistance. Based on these favorable properties, 3DH-NM/NF could be considered as a promising candidate for the monolith de-NOx catalysts.In this work, we successfully in situ decorated nickel foam with porous Ni-Mn oxide nanosheets (3DH-NM/NF) as 3D hierarchical monolith de-NOx catalysts via a simple hydrothermal reaction and calcination process. The catalysts were carefully examined by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, elemental mapping, X-ray photoelectron spectroscopy, H2 temperature-programmed reduction and NH3 temperature-programmed desorption measurements. The results indicated that the nanosheets are composed of a Ni6Mn1O8 spinel and the metal species are uniformly dispersed in bi-metal oxides. As a result, the strong synergistic effects between the Mn and Ni species have been observed. The active oxygen species, reducible species and acidity are enhanced by the in situ formation of the nanosheets on the surface of nickel foam. These desirable features of 3DH-NM/NF catalysts bring about the excellent de-NOx performance. Moreover, the 3DH-NM/NF catalysts also present good stability and H2O resistance. Based on these favorable properties, 3DH-NM/NF could be considered as a promising candidate for the monolith de-NOx catalysts. Electronic supplementary information (ESI) available: Experimental details and catalytic performance of the NM/cordierite catalysts, SEM image and EDX analysis of the NF and 3DH-N/NF catalysts, N2 selectivity and catalytic performance under different gas hourly space velocities of the 3DH-NM/NF catalysts. See DOI: 10.1039/c4nr00475b

Nb-Base FS-85 Alloy as a Candidate Structural Material for Space Reactor Applications: Effects of Thermal Aging

NASA Astrophysics Data System (ADS)

Leonard, Keith J.; Busby, Jeremy T.; Hoelzer, David T.; Zinkle, Steven J.

2009-04-01

The proposed uses of fission reactors for manned or deep space missions have typically relied on the potential use of refractory metal alloys as structural materials. Throughout the history of these programs, a leading candidate has been Nb-1Zr, due to its good fabrication and welding characteristics. However, the less-than-optimal creep resistance of this alloy has encouraged interest in the more complex FS-85 (Nb-28Ta-10W-1Zr) alloy. Despite this interest, only a relatively small database exists for the properties of FS-85. Database gaps include the potential microstructural instabilities that can lead to mechanical property degradation. In this work, changes in the microstructure and mechanical properties of FS-85 were investigated following 1100 hours of thermal aging at 1098, 1248, and 1398 K. The changes in electrical resistivity, hardness, and tensile properties between the as-annealed and aged materials are compared. Evaluation of the microstructural changes was performed through optical microscopy (OM), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The development of intragranular and grain-boundary precipitation of Zr-rich compounds as a function of aging temperature was followed. Brittle tensile behavior was measured in the material aged at 1248 K, while ductile behavior occurred in samples aged above and below this temperature. The effect of temperature on the under- and overaging of the grain-boundary particles is believed to have contributed to the mechanical property behavior of the aged materials.

n-type dopants in (001) β-Ga2O3 grown on (001) β-Ga2O3 substrates by plasma-assisted molecular beam epitaxy

NASA Astrophysics Data System (ADS)

Han, Sang-Heon; Mauze, Akhil; Ahmadi, Elaheh; Mates, Tom; Oshima, Yuichi; Speck, James S.

2018-04-01

Ge and Sn as n-type dopants in (001) β-Ga2O3 films were investigated using plasma-assisted molecular beam epitaxy. The Ge concentration showed a strong dependence on the growth temperature, whereas the Sn concentration remains independent of the growth temperature. The maximum growth temperature at which a wide range of Ge concentrations (from 1017 to 1020 cm-3) could be achieved was 675 °C while the same range of Sn concentration could be achieved at growth temperature of 750 °C. Atomic force microscopy results revealed that higher growth temperature shows better surface morphology. Therefore, our study reveals a tradeoff between higher Ge doping concentration and high quality surface morphology on (001) β-Ga2O3 films grown by plasma-assisted molecular beam epitaxy. The Ge doped films had an electron mobility of 26.3 cm2 V-1 s-1 at the electron concentration of 6.7 × 1017 cm-3 whereas the Sn doped films had an electron mobility of 25.3 cm2 V-1 s-1 at the electron concentration of 1.1 × 1018 cm-3.

Graphene nanoplate-MnO2 composites for supercapacitors: a controllable oxidation approach.

PubMed

Huang, Huajie; Wang, Xin

2011-08-01

Graphene nanoplate-MnO(2) composites have been synthesized by oxidising part of the carbon atoms in the framework of graphene nanoplates at ambient temperature. The composites were characterized by means of X-ray diffraction (XRD), Raman spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS) and cyclic voltammetry (CV). It was found that the oxidation extent of the carbon atoms in the graphene framework in these composites was dependent on the reaction time, which also influenced their microstructure, morphology and electrochemical properties. Compared with MnO(2) nanolamellas, the nanocomposite prepared with a reaction time of 3 h reveals better electrochemical properties as a supercapacitor electrode material. This journal is © The Royal Society of Chemistry 2011

Comparison of dislocation content measured with transmission electron microscopy and micro-Laue diffraction based streak analysis

DOE PAGES

Zhang, C.; Balachandran, S.; Eisenlohr, P.; ...

2017-10-04

The subsurface dislocation content in a Ti-5Al-2.5Sn (wt%) uniaxial tension sample deformed at ambient temperature was characterized by peak streak analysis of micro-Laue diffraction patterns collected non-destructively by differential aperture X-raymicroscopy, and with focused ion beam transmission electron microscopy of material in the same volume. This comparison reveals that micro-Laue diffraction streak analysis based on an edge dislocation assumption can accurately identify the dominant dislocation slip system history (Burgers vector and plane observed by TEM), despite the fact that dislocations have predominantly screw character. As a result, other dislocations identified by TEM were not convincingly discernible from the peak streakmore » analysis.« less

Spinel lithium manganese oxide nanoparticles: unique molten salt synthesis strategy and excellent electrochemical performances.

PubMed

Wang, Xiong; Zhu, Juanjuan; Liu, Yingjie

2009-11-01

As a promising candidate cathode material, spinel lithium manganese oxide nanoparticles were successfully synthesized through a novel molten salt synthesis route at relatively low temperature, using manganese dioxide nanowires as precursor. A variety of techniques were applied to characterize the spinel nanomaterial, including X-ray diffraction, transmission electron microscopy, field-emission scanning electron microscopy, and X-ray photoelectron spectroscopy. The average particle size of the resulting spinel nanoparticles was about 80 nm with narrow distribution. As cathode material for rechargeable lithium ion battery, the electrochemical properties were investigated. All the results show that the electrochemical performances of the homogeneous spinel nanoparticles were improved, which might be ascribed to large specific surface area, fairly narrow size distribution, and the unique synthesis strategy.

Autonomous Filling of Grain-Boundary Cavities during Creep Loading in Fe-Mo Alloys

NASA Astrophysics Data System (ADS)

Zhang, S.; Fang, H.; Gramsma, M. E.; Kwakernaak, C.; Sloof, W. G.; Tichelaar, F. D.; Kuzmina, M.; Herbig, M.; Raabe, D.; Brück, E.; van der Zwaag, S.; van Dijk, N. H.

2016-10-01

We have investigated the autonomous repair of creep damage by site-selective precipitation in a binary Fe-Mo alloy (6.2 wt pct Mo) during constant-stress creep tests at temperatures of 813 K, 823 K, and 838 K (540 °C, 550 °C, and 565 °C). Scanning electron microscopy studies on the morphology of the creep-failed samples reveal irregularly formed deposits that show a close spatial correlation with the creep cavities, indicating the filling of creep cavities at grain boundaries by precipitation of the Fe2Mo Laves phase. Complementary transmission electron microscopy and atom probe tomography have been used to characterize the precipitation mechanism and the segregation at grain boundaries in detail.

Structural and morphological study of chemically synthesized CdSe thin films

NASA Astrophysics Data System (ADS)

Agrawal, P.; Singh, Randhir; Sharma, Jeewan; Sachdeva, M.; Singh, Anupinder; Bhargava, A.

2018-05-01

Nanocrystalline CdSe thin films were prepared by Chemical Bath Deposition (CBD) method using potassium nitrilo-triacetic acid cadmium complex and sodium selenosulphite. The as deposited films were red in color, uniform and well adherent to the glass substrate. These films were strongly dependent on the deposition parameters such as bath composition, deposition temperature and time. Films were annealed at 350 °C for four hours. The morphological, structural and optical properties were studied using X-ray diffraction (XRD), UV-VIS spectrophotometer measurements, scanning electron microscopy and atomic force microscopy. The XRD analysis confirmed that films are predominantly in hexagonal phase. Scanning electron micrograph shows that the grains are uniformly spread all over the film and each grain contains many nanocrystals with spherical shapes.

Formation of Nanodimensional 3C-SiC Structures from Rice Husks

NASA Astrophysics Data System (ADS)

Gorzkowski, E. P.; Qadri, S. B.; Rath, B. B.; Goswami, R.; Caldwell, J. D.

2013-05-01

We have demonstrated that large quantities of β-SiC nanostructures can be obtained from rice husk agricultural waste by using controlled conditions in a thermogravimetric setup. This simple and inexpensive method of producing these structures on a large scale is critical for applications in nanoelectronics, nanosensors, and biotechnology. The temperature and atmosphere are two critical elements in forming either α-cristobalite (SiO2) or β-SiC. Using different characterization methods (x-ray diffraction, scanning electron microscopy, transmission electron microscopy, and Raman spectroscopy), we have shown that pyrolysis of rice husks in argon atmosphere at 1375°C results in simultaneous formation of carbon nanotubes, β-SiC nanowires/nanorods, and β-SiC powder.

Structural and optical properties of glancing angle deposited TiO2 nanowires array.

PubMed

Chinnamuthu, P; Mondal, A; Singh, N K; Dhar, J C; Das, S K; Chattopadhyay, K K

2012-08-01

TiO2 nanowires (NWs) have been synthesized by glancing angle deposition technique using e-beam evaporator. The average length 490 nm and diameter 80 nm of NWs were examined by field emission-scanning electron microscopy. Transmission electron microscopy emphasized that the NWs were widely dispersed at the top. X-ray diffraction has been carried out on the TiO2 thin film (TF) and NW array. A small blue shift of 0.03 eV was observed in Photoluminescence (PL) main band emission for TiO2 NW as compared to TiO2 TF. The high temperature annealing at 980 degrees C partially removed the oxygen vacancy from the sample, which was investigated by PL and optical absorption measurements.

Transmission Electron Microscopy (TEM) Study of the Oxide Layers Formed on Fe-12Cr-4Al Ferritic Alloy in an Oxygenated Pb-Bi Environment at 800°C

NASA Astrophysics Data System (ADS)

Popovic, M. P.; Yang, Y.; Bolind, A. M.; Ozdol, V. B.; Olmsted, D. L.; Asta, M.; Hosemann, P.

2018-06-01

Liquid lead-bismuth eutectic (LBE) can serve as a heat transfer fluid for advanced nuclear applications as well as concentrated solar power but poses corrosion challenges for the structural materials at elevated temperatures. Oxide passivation of the surfaces of these materials during exposure to liquid LBE can inhibit such material degradation. In this study, transmission electron microscopy of oxides formed on Fe-Cr-Al alloy during exposure to low-oxygenated LBE at 800°C has been performed. A complex structure of the oxide film has been revealed, consisting of a homogeneous inner layer of mostly Al2O3 and a heterogeneous outer layer.

Comparison of dislocation content measured with transmission electron microscopy and micro-Laue diffraction based streak analysis

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhang, C.; Balachandran, S.; Eisenlohr, P.

The subsurface dislocation content in a Ti-5Al-2.5Sn (wt%) uniaxial tension sample deformed at ambient temperature was characterized by peak streak analysis of micro-Laue diffraction patterns collected non-destructively by differential aperture X-raymicroscopy, and with focused ion beam transmission electron microscopy of material in the same volume. This comparison reveals that micro-Laue diffraction streak analysis based on an edge dislocation assumption can accurately identify the dominant dislocation slip system history (Burgers vector and plane observed by TEM), despite the fact that dislocations have predominantly screw character. As a result, other dislocations identified by TEM were not convincingly discernible from the peak streakmore » analysis.« less

Synthesis of gold nanoflowers using deep eutectic solvent with high surface enhanced Raman scattering properties

NASA Astrophysics Data System (ADS)

Aghakhani Mahyari, Farzaneh; Tohidi, Maryam; Safavi, Afsaneh

2016-09-01

A facile, seed-less and one-pot method was developed for synthesis of gold nanoflowers with multiple tips through reduction of HAuCl4 with deep eutectic solvent at room temperature. This solvent is eco-friendly, low-cost, non-toxic and biodegradable and can act as both reducing and shape-controlling agent. In this protocol, highly branched and stable gold nanoflowers were obtained without using any capping agent. The obtained products were characterized by different techniques including, field emission scanning electron microscopy, transmission electron microscopy, x-ray diffraction and UV-vis spectroscopy. The as-prepared gold nanoflowers exhibit efficient surface-enhanced Raman scattering (SERS) properties which can be used as excellent substrates for SERS.

An electron microscopy examination of primary recrystallization in TD-nickel.

NASA Technical Reports Server (NTRS)

Petrovic, J. J.; Ebert, L. J.

1972-01-01

Primary recrystallization in TD-nickel 1 in. bar has previously been regarded as the process by which the initial fine grain structure is converted to a coarse grain size (increases in grain size by 500 times) under suitable deformation and annealing conditions. This process is dependent on deformation mode. While it occurs readily after rolling transverse to the bar axis and annealing (800 C), it is completely inhibited by longitudinal rolling and swaging deformations, even for very high (1320 C) annealing temperatures. A transmission electron microscopy examination of deformation and annealing substructures indicates that primary recrystallization in TD-nickel 1 in. bar actually occurs on the sub-light optical level, to produce a grain structure similar in size to the initial fine grained state.

Germanium photodetectors fabricated on 300 mm silicon wafers for near-infrared focal plane arrays

NASA Astrophysics Data System (ADS)

Zeller, John W.; Rouse, Caitlin; Efstathiadis, Harry; Dhar, Nibir K.; Wijewarnasuriya, Priyalal; Sood, Ashok K.

2017-09-01

SiGe p-i-n photodetectors have been fabricated on 300 mm (12") diameter silicon (Si) wafers utilizing high throughput, large-area complementary metal-oxide semiconductor (CMOS) technologies. These Ge photodetectors are designed to operate in room temperature environments without cooling, and thus have potential size and cost advantages over conventional cooled infrared detectors. The two-step fabrication process for the p-i-n photodetector devices, designed to minimize the formation of defects and threading dislocations, involves low temperature epitaxial growth of a thin p+ (boron) Ge seed/buffer layer, followed by higher temperature deposition of a thicker Ge intrinsic layer. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) demonstrated uniform layer compositions with well defined layer interfaces and reduced dislocation density. Time-of-flight secondary ion mass spectroscopy (TOF-SIMS) was likewise employed to analyze the doping levels of the p+ and n+ layers. Current-voltage (I-V) measurements demonstrated that these SiGe photodetectors, when exposed to incident visible-NIR radiation, exhibited dark currents down below 1 μA and significant enhancement in photocurrent at -1 V. The zero-bias photocurrent was also relatively high, showing a minimal drop compared to that at -1 V bias.

Acetylene Gas-Sensing Properties of Layer-by-Layer Self-Assembled Ag-Decorated Tin Dioxide/Graphene Nanocomposite Film

PubMed Central

Jiang, Chuanxing; Yin, Nailiang; Yao, Yao; Shaymurat, Talgar; Zhou, Xiaoyan

2017-01-01

This paper demonstrates an acetylene gas sensor based on an Ag-decorated tin dioxide/reduced graphene oxide (Ag–SnO2/rGO) nanocomposite film, prepared by layer-by-layer (LbL) self-assembly technology. The as-prepared Ag–SnO2/rGO nanocomposite was characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and Raman spectrum. The acetylene sensing properties were investigated using different working temperatures and gas concentrations. An optimal temperature of 90 °C was determined, and the Ag–SnO2/rGO nanocomposite sensor exhibited excellent sensing behaviors towards acetylene, in terms of response, repeatability, stability and response/recovery characteristics, which were superior to the pure SnO2 and SnO2/rGO film sensors. The sensing mechanism of the Ag–SnO2/rGO sensor was attributed to the synergistic effect of the ternary nanomaterials, and the heterojunctions created at the interfaces between SnO2 and rGO. This work indicates that the Ag–SnO2/rGO nanocomposite is a good candidate for constructing a low-temperature acetylene sensor. PMID:28927021

Modification of the Stress-Strain Curve for High-Strength Line Pipe Steel

NASA Astrophysics Data System (ADS)

Jonsson, Katherine

2013-01-01

This thesis presents work performed to improve the work hardening behaviour of an X80 microalloyed steel through various Interrupted Thermal Treatments (ITT). The aim of this work was to determine the relationships between thermal history, microstructure and mechanical properties through both qualitative and quantitative measures. Prior to the ITT experiments, a continuous cooling transformation (CCT) diagram was constructed under no-strain conditions to identify the transformation temperatures and products that are achievable in X80 steel. The thermal treatments were applied using a Gleeble thermal-mechanical simulator to generate a variety of microstructures in various fractions and morphologies. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were used to investigate and quantify the microstructures in terms of phase fraction and grain size. The ITT experiments successfully generated microstructures comprised of ferrite, bainitic ferrite, martensite and martensite-austenite (M-A) without the addition of strain. The effect of cooling rates, interrupt temperature, re-heat temperature and hold times were investigated and the mechanical performance was correlated with the quantified microstructures. Although the ITT experiments did not improve the strength relative to a continuously cooled sample, the work hardening coefficient was increased as a result of the interrupted thermal treatments.

Phase decomposition of γ-U (bcc) in U-10 wt% Mo fuel alloy during hot isostatic pressing of monolithic fuel plate

NASA Astrophysics Data System (ADS)

Park, Y.; Eriksson, N.; Newell, R.; Keiser, D. D.; Sohn, Y. H.

2016-11-01

Eutectoid decomposition of γ-phase (cI2) into α-phase (oC4) and γ‧-phase (tI6) during the hot isostatic pressing (HIP) of the U-10 wt% Mo (U10Mo) alloy was investigated using monolithic fuel plate samples consisting of U10Mo fuel alloy, Zr diffusion barrier and AA6061 cladding. The decomposition of the γ-phase was observed because the HIP process is carried out near the eutectoid temperature, 555 °C. Initially, a cellular structure, consisting of γ‧-phase surrounded by α-phase, developed from the destabilization of the γ-phase. The cellular structure further developed into an alternating lamellar structure of α- and γ‧-phases. Using scanning electron microscopy and transmission electron microscopy, qualitative and quantitative microstructural analyses were carried out to identify the phase constituents, and elucidate the microstructural development based on time-temperature-transformation diagram of the U10Mo alloy. The destabilization of γ -phase into α- and γ‧-phases would be minimized when HIP process was carried out with rapid ramping/cooling rate and dwell temperature higher than 560 °C.

Microstructural analysis of 800H steel exposed at test operation in HTHL by using FIB-SEM and HRTEM techniques

NASA Astrophysics Data System (ADS)

Marušáková, Daniela; Bublíková, Petra; Berka, Jan; Vávrovcová, Zuzana; Burda, Jaroslav

2017-09-01

To understand the degradation process of metal materials which are used in power engineering, appropriate evaluation procedure is necessary to ensure. In that order, the degradation of alloy 800H during the first period of test operation in High Temperature Helium Loop (HTHL) was tested. Experiment was carried out in atmosphere of pure technical helium with purity 4.6 containing only residual concentration of moisture up to 300 vppm. Parameters during the operation test were not constant, process was interrupted several times. The maximum temperature on specimens during this period was 750 °C, average temperature was 460 °C, gas pressure ranged from 3 to 6 MPa and gas flow from 3 to 9 gs-1. Total duration of the test was 264 h. After the exposure the degradation of specimens was investigated by Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM). Using the technique of Focused Ion Beam (FIB) integrated within SEM the transparent samples with quality surface parameters were obtained for TEM analysis. FIB technique in combination with High Resolution TEM ensured the guaranteed methodology of exposed sample preparation and precise description of changes in this kind of material.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Song, Gian; Sun, Zhiqian; Li, Lin

There have been numerous efforts to develop creep-resistant materials strengthened by incoherent particles at high temperatures and stresses in response to future energy needs for steam turbines in thermal-power plants. However, the microstructural instability of the incoherent-particle-strengthened ferritic steels limits their application to temperatures below 900 K. Here, we report a novel ferritic alloy with the excellent creep resistance enhanced by coherent hierarchical precipitates, using the integrated experimental (transmission-electron microscopy/scanning-transmission-electron microscopy, in-situ neutron diffraction, and atom-probe tomography) and theoretical (crystal-plasticity finite-element modeling) approaches. This alloy is strengthened by nano-scaled L21-Ni2TiAl (Heusler phase)-based precipitates, which themselves contain coherent nano-scaled B2 zones.more » These coherent hierarchical precipitates are uniformly distributed within the Fe matrix. Our hierarchical structure material exhibits the superior creep resistance at 973 K in terms of the minimal creep rate, which is four orders of magnitude lower than that of conventional ferritic steels. These results provide a new alloy-design strategy using the novel concept of hierarchical precipitates and the fundamental science for developing creep-resistant ferritic alloys. Finally, the present research will broaden the applications of ferritic alloys to higher temperatures.« less

A Study of the Oxidation Behaviour of Pile Grade A (PGA) Nuclear Graphite Using Thermogravimetric Analysis (TGA), Scanning Electron Microscopy (SEM) and X-Ray Tomography (XRT).

PubMed

Payne, Liam; Heard, Peter J; Scott, Thomas B

2015-01-01

Pile grade A (PGA) graphite was used as a material for moderating and reflecting neutrons in the UK's first generation Magnox nuclear power reactors. As all but one of these reactors are now shut down there is a need to understand the residual state of the material prior to decommissioning of the cores, in particular the location and concentration of key radio-contaminants such as 14C. The oxidation behaviour of unirradiated PGA graphite was studied, in the temperature range 600-1050°C, in air and nitrogen using thermogravimetric analysis, scanning electron microscopy and X-ray tomography to investigate the possibility of using thermal degradation techniques to examine 14C distribution within irradiated material. The thermal decomposition of PGA graphite was observed to follow the three oxidation regimes historically identified by previous workers with limited, uniform oxidation at temperatures below 600°C and substantial, external oxidation at higher temperatures. This work demonstrates that the different oxidation regimes of PGA graphite could be developed into a methodology to characterise the distribution and concentration of 14C in irradiated graphite by thermal treatment.

A Study of the Oxidation Behaviour of Pile Grade A (PGA) Nuclear Graphite Using Thermogravimetric Analysis (TGA), Scanning Electron Microscopy (SEM) and X-Ray Tomography (XRT)

PubMed Central

Payne, Liam; Heard, Peter J.; Scott, Thomas B.

2015-01-01

Pile grade A (PGA) graphite was used as a material for moderating and reflecting neutrons in the UK’s first generation Magnox nuclear power reactors. As all but one of these reactors are now shut down there is a need to understand the residual state of the material prior to decommissioning of the cores, in particular the location and concentration of key radio-contaminants such as 14C. The oxidation behaviour of unirradiated PGA graphite was studied, in the temperature range 600–1050°C, in air and nitrogen using thermogravimetric analysis, scanning electron microscopy and X-ray tomography to investigate the possibility of using thermal degradation techniques to examine 14C distribution within irradiated material. The thermal decomposition of PGA graphite was observed to follow the three oxidation regimes historically identified by previous workers with limited, uniform oxidation at temperatures below 600°C and substantial, external oxidation at higher temperatures. This work demonstrates that the different oxidation regimes of PGA graphite could be developed into a methodology to characterise the distribution and concentration of 14C in irradiated graphite by thermal treatment. PMID:26575374

Magnetic response of hybrid ferromagnetic and antiferromagnetic core-shell nanostructures

NASA Astrophysics Data System (ADS)

Khan, U.; Li, W. J.; Adeela, N.; Irfan, M.; Javed, K.; Wan, C. H.; Riaz, S.; Han, X. F.

2016-03-01

The synthesis of FeTiO3-Ni(Ni80Fe20) core-shell nanostructures by a two-step method (sol-gel and DC electrodeposition) has been demonstrated. XRD analysis confirms the rhombohedral crystal structure of FeTiO3(FTO) with space group R3&cmb.macr;. Transmission electron microscopy clearly depicts better morphology of nanostructures with shell thicknesses of ~25 nm. Room temperature magnetic measurements showed significant enhancement of magnetic anisotropy for the permalloy (Ni80Fe20)-FTO over Ni-FTO core-shell nanostructures. Low temperature magnetic measurements of permalloy-FeTiO3 core-shell structure indicated a strong exchange bias mechanism with magnetic coercivity below the antiferromagnetic Neel temperature (TN = 59 K). The exchange bias is attributed to the alignment of magnetic moments in the antiferromagnetic material at low temperature. Our scheme opens a path towards optimum automotive systems and wireless communications wherein broader bandwidths and smaller sizes are required.The synthesis of FeTiO3-Ni(Ni80Fe20) core-shell nanostructures by a two-step method (sol-gel and DC electrodeposition) has been demonstrated. XRD analysis confirms the rhombohedral crystal structure of FeTiO3(FTO) with space group R3&cmb.macr;. Transmission electron microscopy clearly depicts better morphology of nanostructures with shell thicknesses of ~25 nm. Room temperature magnetic measurements showed significant enhancement of magnetic anisotropy for the permalloy (Ni80Fe20)-FTO over Ni-FTO core-shell nanostructures. Low temperature magnetic measurements of permalloy-FeTiO3 core-shell structure indicated a strong exchange bias mechanism with magnetic coercivity below the antiferromagnetic Neel temperature (TN = 59 K). The exchange bias is attributed to the alignment of magnetic moments in the antiferromagnetic material at low temperature. Our scheme opens a path towards optimum automotive systems and wireless communications wherein broader bandwidths and smaller sizes are required. Electronic supplementary information (ESI) available. See DOI: 10.1039/c5nr07946b

Optical spectroscopy and microscopy of radiation-induced light-emitting point defects in lithium fluoride crystals and films

NASA Astrophysics Data System (ADS)

Montereali, R. M.; Bonfigli, F.; Menchini, F.; Vincenti, M. A.

2012-08-01

Broad-band light-emitting radiation-induced F2 and F3+ electronic point defects, which are stable and laser-active at room temperature in lithium fluoride crystals and films, are used in dosimeters, tuneable color-center lasers, broad-band miniaturized light sources and novel radiation imaging detectors. A brief review of their photoemission properties is presented, and their behavior at liquid nitrogen temperatures is discussed. Some experimental data from optical spectroscopy and fluorescence microscopy of these radiation-induced point defects in LiF crystals and thin films are used to obtain information about the coloration curves, the efficiency of point defect formation, the effects of photo-bleaching processes, etc. Control of the local formation, stabilization, and transformation of radiation-induced light-emitting defect centers is crucial for the development of optically active micro-components and nanostructures. Some of the advantages of low temperature measurements for novel confocal laser scanning fluorescence microscopy techniques, widely used for spatial mapping of these point defects through the optical reading of their visible photoluminescence, are highlighted.

Electron microscopy study of antioxidant interaction with bacterial cells

NASA Astrophysics Data System (ADS)

Plotnikov, Oleg P.; Novikova, Olga V.; Konnov, Nikolai P.; Korsukov, Vladimir N.; Gunkin, Ivan F.; Volkov, Uryi P.

2000-10-01

To maintain native microorganisms genotype and phenotype features a lyophylization technique is widely used. However in this case cells are affected by influences of vacuum and low temperature that cause a part of the cells population to be destruction. Another factor reduced microorganisms vitality is formation of reactive oxygen forms that damage certain biological targets (such as DNA, membranes etc.) Recently to raise microorganism's resistance against adverse condition natural and synthetic antioxidants are used. Antioxidant- are antagonists of free radicals. Introduction of antioxidants in protective medium for lyophylization increase bacteria storage life about 2,0-4,8 fold in comparison with reference samples. In the article the main results of our investigation of antioxidants interaction with microorganism cells is described. As bacteria cells we use vaccine strain yersinia pestis EV, that were grown for 48 h at 28 degree(s)C on the Hottinger agar (pH 7,2). Antioxidants are inserted on the agar surface in specimen under test. To investigate a localization of antioxidants for electron microscopy investigation, thallium organic antioxidants were used. The thallium organic compounds have an antioxidant features if thallium is in low concentration (about 1(mu) g/ml). The localization of the thallium organic antioxidants on bacteria Y. pestis EV is visible in electron microscopy images, thallium being heavy metal with high electron density. The negatively stained bacteria and bacteria thin sections with thallium organic compounds were investigated by means of transmission electron microscopy. The localization of the thallium organic compounds is clearly visible in electron micrographs as small dark spots with size about 10-80nm. Probably mechanisms of interaction of antioxidants with bacteria cells are discussed.

Ultrafast structural and electronic dynamics of the metallic phase in a layered manganite

PubMed Central

Piazza, L.; Ma, C.; Yang, H. X.; Mann, A.; Zhu, Y.; Li, J. Q.; Carbone, F.

2013-01-01

The transition between different states in manganites can be driven by various external stimuli. Controlling these transitions with light opens the possibility to investigate the microscopic path through which they evolve. We performed femtosecond (fs) transmission electron microscopy on a bi-layered manganite to study its response to ultrafast photoexcitation. We show that a photoinduced temperature jump launches a pressure wave that provokes coherent oscillations of the lattice parameters, detected via ultrafast electron diffraction. Their impact on the electronic structure are monitored via ultrafast electron energy loss spectroscopy, revealing the dynamics of the different orbitals in response to specific structural distortions. PMID:26913564

Atomic bonding effects in annular dark field scanning transmission electron microscopy. I. Computational predictions

DOE Office of Scientific and Technical Information (OSTI.GOV)

Odlyzko, Michael L.; Mkhoyan, K. Andre, E-mail: mkhoyan@umn.edu; Himmetoglu, Burak

2016-07-15

Annular dark field scanning transmission electron microscopy (ADF-STEM) image simulations were performed for zone-axis-oriented light-element single crystals, using a multislice method adapted to include charge redistribution due to chemical bonding. Examination of these image simulations alongside calculations of the propagation of the focused electron probe reveal that the evolution of the probe intensity with thickness exhibits significant sensitivity to interatomic charge transfer, accounting for observed thickness-dependent bonding sensitivity of contrast in all ADF-STEM imaging conditions. Because changes in image contrast relative to conventional neutral atom simulations scale directly with the net interatomic charge transfer, the strongest effects are seen inmore » crystals with highly polar bonding, while no effects are seen for nonpolar bonding. Although the bonding dependence of ADF-STEM image contrast varies with detector geometry, imaging parameters, and material temperature, these simulations predict the bonding effects to be experimentally measureable.« less

Characterization of the α phase nucleation in a two-phase metastable β titanium alloy

NASA Astrophysics Data System (ADS)

Lenain, A.; Clément, N.; Jacques, P. J.; Véron, M.

2005-12-01

Beta titanium alloys are increasingly the best choice for automotive and aerospace applications due to their high performance-to-density ratio. Among these alloys, the TIMETAL Ti-LCB is already used in the automotive industry because it presents excellent mechanical properties and a lower cost compared with other Ti alloys. The current study deals with the characterization of the nucleation and growth of the α phase in several thermomechanical processes, because the distribution and size of the α phase strongly influence the mechanical properties of the resulting microstructures. Several heat treatments were conducted after either cold rolling or annealing. The resulting microstructures were characterized by scanning electron microscopy, transmission electron microscopy, x-ray diffraction, or electron backscatter diffraction. It was observed that the morphology and the volume fraction of the α phase are strongly dependent on the holding temperature, on the heating or cooling rate, and on the β grain size.

Influence of the adsorption geometry of PTCDA on Ag(111) on the tip-molecule forces in non-contact atomic force microscopy.

PubMed

Langewisch, Gernot; Falter, Jens; Schirmeisen, André; Fuchs, Harald

2014-01-01

Perylene-3,4,9,10-tetracarboxylic dianhydride (PTCDA) adsorbed on a metal surface is a prototypical organic-anorganic interface. In the past, scanning tunneling microscopy and scanning tunneling spectroscopy studies of PTCDA adsorbed on Ag(111) have revealed differences in the electronic structure of the molecules depending on their adsorption geometry. In the work presented here, high-resolution 3D force spectroscopy measurements at cryogenic temperatures were performed on a surface area that contained a complete PTCDA unit cell with the two possible geometries. At small tip-molecule separations, deviations in the tip-sample forces were found between the two molecule orientations. These deviations can be explained by a different electron density in both cases. This result demonstrates the capability of 3D force spectroscopy to detect even small effects in the electronic properties of organic adsorbates.

Room Temperature Gas Sensing Properties of Sn-Substituted Nickel Ferrite (NiFe2O4) Thin Film Sensors Prepared by Chemical Co-Precipitation Method

NASA Astrophysics Data System (ADS)

Manikandan, V.; Li, Xiaogan; Mane, R. S.; Chandrasekaran, J.

2018-04-01

Tin (Sn) substituted nickel ferrite (NiFe2O4) thin film sensors were prepared by a simple chemical co-precipitation method, which initially characterized their structure and surface morphology with the help of x-ray diffraction and scanning electron microscopy. Surface morphology of the sensing films reveals particles stick together with nearer particles and this formation leads to a large specific area as a large specific area is very useful for easy adsorption of gas molecules. Transmission electron microscopy and selected area electron diffraction pattern images confirm particle size and nanocrystallnity as due to formation of circular rings. Fourier transform infrared analysis has supported the presence of functional groups. The 3.69 eV optical band gap of the film was found which enabled better gas sensing. Gas sensors demonstrate better response and recovery characteristics, and the maximum response was 68.43%.

Molecular beam epitaxy growth of high electron mobility InAs/AlSb deep quantum well structure

NASA Astrophysics Data System (ADS)

Wang, Juan; Wang, Guo-Wei; Xu, Ying-Qiang; Xing, Jun-Liang; Xiang, Wei; Tang, Bao; Zhu, Yan; Ren, Zheng-Wei; He, Zhen-Hong; Niu, Zhi-Chuan

2013-07-01

InAs/AlSb deep quantum well (QW) structures with high electron mobility were grown by molecular beam epitaxy (MBE) on semi-insulating GaAs substrates. AlSb and Al0.75Ga0.25Sb buffer layers were grown to accommodate the lattice mismatch (7%) between the InAs/AlSb QW active region and GaAs substrate. Transmission electron microscopy shows abrupt interface and atomic force microscopy measurements display smooth surface morphology. Growth conditions of AlSb and Al0.75Ga0.25Sb buffer were optimized. Al0.75Ga0.25Sb is better than AlSb as a buffer layer as indicated. The sample with optimal Al0.75Ga0.25Sb buffer layer shows a smooth surface morphology with root-mean-square roughness of 6.67 Å. The electron mobility has reached as high as 27 000 cm2/Vs with a sheet density of 4.54 × 1011/cm2 at room temperature.

Patterned low temperature copper-rich deposits using inkjet printing

NASA Astrophysics Data System (ADS)

Rozenberg, Gregor G.; Bresler, Eric; Speakman, Stuart P.; Jeynes, Chris; Steinke, Joachim H. G.

2002-12-01

A PZT piezoelectric ceramic research drop-on-demand inkjet print head operating in bend mode was used as a means of delivering a copper precursor, vinyltrimethylsilane copper (+1) hexafluoroacetylacetonate, in a controlled and placement accurate fashion. The reagent disproportionates at low temperature (<200 °C), to deposit copper on glass. These deposits are shown to be more than 90% copper by weight by electron probe microanalysis and microbeam Rutherford backscattering spectroscopy. Microscopy shows a deposit diameter and three-dimensional profile that suggests a complex deposition and conversion mechanism. Our findings represent an important step towards the manufacture of electronic devices by entirely nonlithographic means.

In situ investigation of the mobility of small gold clusters on cleaved MgO surfaces

NASA Technical Reports Server (NTRS)

Metois, J. J.; Heinemann, K.; Poppa, H.

1976-01-01

The mobility of small clusters of gold (about 10 A in diameter) on electron-beam-cleaved MgO surfaces was studied by in situ transmission electron microscopy under controlled vacuum and temperature conditions. During the first 10 min following a deposition at room temperature, over 10 per cent of the crystallites moved over short distances (about 20 A) discontinuously, with a velocity greater than 150 A/sec. Eighty per cent of the mobility events were characterized by the avoidance of proximity of other crystallites, and this was tentatively explained as the result of repulsive elastic forces between the interacting crystallites.

Room Temperature Ferromagnetic Mn:Ge(001).

PubMed

Lungu, George Adrian; Stoflea, Laura Elena; Tanase, Liviu Cristian; Bucur, Ioana Cristina; Răduţoiu, Nicoleta; Vasiliu, Florin; Mercioniu, Ionel; Kuncser, Victor; Teodorescu, Cristian-Mihail

2013-12-27

We report the synthesis of a room temperature ferromagnetic Mn-Ge system obtained by simple deposition of manganese on Ge(001), heated at relatively high temperature (starting with 250 °C). The samples were characterized by low energy electron diffraction (LEED), scanning tunneling microscopy (STM), high resolution transmission electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS), superconducting quantum interference device (SQUID), and magneto-optical Kerr effect (MOKE). Samples deposited at relatively elevated temperature (350 °C) exhibited the formation of ~5-8 nm diameter Mn₅Ge₃ and Mn 11 Ge₈ agglomerates by HRTEM, while XPS identified at least two Mn-containing phases: the agglomerates, together with a Ge-rich MnGe ~2.5 phase, or manganese diluted into the Ge(001) crystal. LEED revealed the persistence of long range order after a relatively high amount of Mn (100 nm) deposited on the single crystal substrate. STM probed the existence of dimer rows on the surface, slightly elongated as compared with Ge-Ge dimers on Ge(001). The films exhibited a clear ferromagnetism at room temperature, opening the possibility of forming a magnetic phase behind a nearly ideally terminated Ge surface, which could find applications in integration of magnetic functionalities on semiconductor bases. SQUID probed the co-existence of a superparamagnetic phase, with one phase which may be attributed to a diluted magnetic semiconductor. The hypothesis that the room temperature ferromagnetic phase might be the one with manganese diluted into the Ge crystal is formulated and discussed.

Room Temperature Ferromagnetic Mn:Ge(001)

PubMed Central

Lungu, George Adrian; Stoflea, Laura Elena; Tanase, Liviu Cristian; Bucur, Ioana Cristina; Răduţoiu, Nicoleta; Vasiliu, Florin; Mercioniu, Ionel; Kuncser, Victor; Teodorescu, Cristian-Mihail

2014-01-01

We report the synthesis of a room temperature ferromagnetic Mn-Ge system obtained by simple deposition of manganese on Ge(001), heated at relatively high temperature (starting with 250 °C). The samples were characterized by low energy electron diffraction (LEED), scanning tunneling microscopy (STM), high resolution transmission electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS), superconducting quantum interference device (SQUID), and magneto-optical Kerr effect (MOKE). Samples deposited at relatively elevated temperature (350 °C) exhibited the formation of ~5–8 nm diameter Mn5Ge3 and Mn11Ge8 agglomerates by HRTEM, while XPS identified at least two Mn-containing phases: the agglomerates, together with a Ge-rich MnGe~2.5 phase, or manganese diluted into the Ge(001) crystal. LEED revealed the persistence of long range order after a relatively high amount of Mn (100 nm) deposited on the single crystal substrate. STM probed the existence of dimer rows on the surface, slightly elongated as compared with Ge–Ge dimers on Ge(001). The films exhibited a clear ferromagnetism at room temperature, opening the possibility of forming a magnetic phase behind a nearly ideally terminated Ge surface, which could find applications in integration of magnetic functionalities on semiconductor bases. SQUID probed the co-existence of a superparamagnetic phase, with one phase which may be attributed to a diluted magnetic semiconductor. The hypothesis that the room temperature ferromagnetic phase might be the one with manganese diluted into the Ge crystal is formulated and discussed. PMID:28788444

Infrared nanoscopy down to liquid helium temperatures

NASA Astrophysics Data System (ADS)

Lang, Denny; Döring, Jonathan; Nörenberg, Tobias; Butykai, Ádám; Kézsmárki, István; Schneider, Harald; Winnerl, Stephan; Helm, Manfred; Kehr, Susanne C.; Eng, Lukas M.

2018-03-01

We introduce a scattering-type scanning near-field infrared microscope (s-SNIM) for the local scale near-field sample analysis and spectroscopy from room temperature down to liquid helium (LHe) temperature. The extension of s-SNIM down to T = 5 K is in particular crucial for low-temperature phase transitions, e.g., for the examination of superconductors, as well as low energy excitations. The low temperature (LT) s-SNIM performance is tested with CO2-IR excitation at T = 7 K using a bare Au reference and a structured Si/SiO2-sample. Furthermore, we quantify the impact of local laser heating under the s-SNIM tip apex by monitoring the light-induced ferroelectric-to-paraelectric phase transition of the skyrmion-hosting multiferroic material GaV4S8 at Tc = 42 K. We apply LT s-SNIM to study the spectral response of GaV4S8 and its lateral domain structure in the ferroelectric phase by the mid-IR to THz free-electron laser-light source FELBE at the Helmholtz-Zentrum Dresden-Rossendorf, Germany. Notably, our s-SNIM is based on a non-contact atomic force microscope (AFM) and thus can be complemented in situ by various other AFM techniques, such as topography profiling, piezo-response force microscopy (PFM), and/or Kelvin-probe force microscopy (KPFM). The combination of these methods supports the comprehensive study of the mutual interplay in the topographic, electronic, and optical properties of surfaces from room temperature down to 5 K.

Exploring the Electrical Conductivity of Cytochrome P450 by Nano-Electrode and Conductive Atomic Force Microscopy

NASA Astrophysics Data System (ADS)

Li, Debin; Gu, Jianhua; Chye, Yewhee; Lederman, David; Kabulski, Jarod; Gannett, Peter; Tracy, Timothy

2006-03-01

There is a growing interest in measuring the conductivity of electron-transfer proteins. The cytochrome P450 (CP450) enzymes represent an important class of heme-containing enzymes. Immobilizing CP450 enzymes on a surface can be used for studying a single enzyme with respect to electron transfer. The spin state of the heme iron can change upon binding of a substrate. In our experiment, CP450 (diameter ˜ 5 nm) has been bonded to a metal surface. Nano-electrodes (gap < 10 nm) were fabricated by defining a bridge via e-beam lithography and then breaking the junction by electromigration at low temperatures. We have examined the electronic properties of CP450 by itself and after binding CP450 with flurbiprofen. The room temperature I-V conductivity is reminiscent to cyclic voltammetry measurements, indicating the presence of strong ionic transfer. At lower temperatures (100 K) the I-V characteristics indicate electronic transport dominated by tunneling processes. The conductive AFM is an additional method used to examine the enzyme's electronic properties. The results from two methods will be discussed..

Effects of a Ta interlayer on the phase transition of TiSi2 on Si(111)

NASA Astrophysics Data System (ADS)

Jeon, Hyeongtag; Jung, Bokhee; Kim, Young Do; Yang, Woochul; Nemanich, R. J.

2000-09-01

This study examines the effects of a thin Ta interlayer on the formation of TiSi2 on Si(111) substrate. The Ta interlayer was introduced by depositing Ta and Ti films sequentially on an atomically clean Si(111) substrate in an ultrahigh vacuum (UHV) system. Samples of 100 Å Ti with 5 and 10 Å Ta interlayers were compared to similar structures without an interlayer. After deposition, the substrates were annealed for 10 min, in situ, at temperatures between 500 and 750 °C in 50 °C increments. The TiSi2 formation with and without the Ta interlayer was analyzed with an X-ray diffractometer, Auger electron spectroscopy (AES), Scanning electron microscopy (SEM), transmission electron microscopy (TEM), and a four-point probe. The AES analysis data showed a 1:2 ratio of Ti:Si in the Ti-silicide layer and indicated that the Ta layer remained at the interface between TiSi2 and the Si(111) substrate. The C 49-C 54 TiSi2 phase transition temperature was lowered by ˜200 °C. The C 49-C 54 TiSi2 phase transition temperature was 550 °C for the samples with a Ta interlayer and was 750 °C for the samples with no Ta interlayer. The sheet resistance of the Ta interlayered Ti silicide showed lower values of resistivity at low temperatures which indicated the change in phase transition temperature. The C 54 TiSi2 displayed different crystal orientation when the Ta interlayer was employed. The SEM and TEM micrographs showed that the TiSi2 with a Ta interlayer significantly suppressed the tendency to islanding and surface agglomeration.

Effect of T6 heat treatment on the microstructural and mechanical properties of Al-Si-Cu-Mg alloys

NASA Astrophysics Data System (ADS)

Patel, Dhruv; Davda, Chintan; Solanki, P. S.; Keshvani, M. J.

2016-05-01

In this communication, it is aimed to optimize the conditions for T6 heat treatment of permanent die cast Al-Si-Cu-Mg alloys. Various solutionizing temperatures, aging treatments and soaking times were used to improve / modify the mechanical properties of presently studied alloys. Formation mechanism of the particles was understood by carrying out optical microscopy and energy dispersive X-ray (EDX) spectroscopy measurements. Spherical particles of alloys were studied for their microstructural properties using scanning electron microscopy (SEM). Microhardness test was performed to investigate their mechanical properties. Dependence of cluster formation and microhardness of the alloys on the adequate solutionizing temperature, aging treatment and soaking time has been discussed in detail.

Preliminary Results on Thermal Shock Behavior of CuZnAl Shape Memory Alloy Using a Solar Concentrator as Heating Source

NASA Astrophysics Data System (ADS)

Tudora, C.; Abrudeanu, M.; Stanciu, S.; Anghel, D.; Plaiaşu, G. A.; Rizea, V.; Ştirbu, I.; Cimpoeşu, N.

2018-06-01

It is highly accepted that martensitic transformation can be induced by temperature variation and by stress solicitation. Using a solar concentrator, we manage to increase the material surface temperature (till 573 respectively 873 K) in very short periods of time in order to analyze the material behavior under thermal shocks. The heating/cooling process was registered and analyzed during the experiments. Material surface was analyzed before and after thermal shocks by microstructure point of view using scanning electron microscopy (SEM) and atomic force microscopy (AFM). The experiments follow the material behavior during fast heating and propose the possibility of activating smart materials using the sun heat for aerospace applications.

Temperature Driven Topological Switch in 1T'-MoTe2 and Strain Induced Nematicity in NaFeAs

NASA Astrophysics Data System (ADS)

Berger, Ayelet Denise Notis

Quasiparticle interference (QPI) is a powerful technique within Scanning Tunneling Microscopy (STM) that is used to probe the electronic bandstructure of materials. This thesis presents two examples using QPI to measure the bandstructure in materials with exotic electronic states that can be tuned via outside parameters (temperature and strain). In Part I of the thesis, we discuss the temperature dependence of Fermi Arcs in 1T'-MoTe 2, and then in Part II, the strain dependent nematic state in NaFeAs. The recent discovery of Weyl semimetals has introduced a new family of materials with topologically protected electronic properties and potential applications due to their anomalous transport effects. Even more useful is a Weyl semimetal that can be turned "on" and "off," switching between a topological and trivial state. One possible material is MoTe2, which undergoes a phase transition at 240K. This thesis consists of experiments using Scanning Tunneling Microscopy (STM) and Spectroscopy (STS) at different temperatures to visualize changes in the electronic bandstructure of MoTe2 across the topological phase transition. We show that a signature of topologically protected Fermi Arcs is present at low temperatures but disappears at room temperature, in the trivial phase. We include an in-depth discussion of how to account for thermal effects when comparing these two types of measurements. In Part II, we discuss strain induced nematicity in NaFeAs, an iron pnictide. Nematic fluctuations and spin correlations play an important role in the phase diagram of the iron pnictides, a family of unconventional superconductors. Illuminating the mechanism behind this symmetry breaking is key to understanding the superconducting state. Previous work has shown that nematicity in the iron pnictides responds strongly to applied strain [1, 2]. In this thesis, I present results from a new experimental technique, elasto-scanning tunneling microscopy (E-STM), which combines in situ strain and atomic resolution STM/STS. For the first time, we are able to observe the effects of strain on nematicity at the local level. We perform E-STM measurements in both the spin density wave phase and the tetragonal phase of NaFeAs and measure a distinct response in each. We successfully use strain to manipulate domain boundaries in the spin density wave state and we find the intensity of nematic fluctuations is coupled to strain in NaFeAs in the tetragonal phase.

Physical and chemical properties of biobased plastic resins containing chicken feather fibers

USDA-ARS?s Scientific Manuscript database

This study was conducted to (a) characterize bioplastic pellets containing feather fibers (pellets) by low temperature-scanning electron microscopy and X-Ray diffraction analysis, (b) evaluate growth and flowering of Begonia boliviensis A. DC. ‘Bonfire’ when grown in medium amended with pellets, and...

Biophysical characteristics of Adelges tsugae feeding sites on six hemlock (Tsuga) species and a hybrid: implications for resistance

USDA-ARS?s Scientific Manuscript database

Characteristics of the plant surface significantly affect host-plant selection by phytophagous insects. Surface morphology of six hemlock species (Tsuga spp.) and a hybrid was investigated using low-temperature scanning electron microscopy. Observations focused on trichome presence and placement a...

Electron Microscopy of Intracellular Protozoa

DTIC Science & Technology

1988-12-20

LR Gold resin containing 0.75% (w/v) benzoin methyl ether as an ultraviolet initiator and left overnight in fresh resin. The samples were finally...ethanol at progressively lower temperatures between OC and -20°C, and infiltrated with LR Gold resin containing 0.5% w/w benzoin methyl ether as an

TEM studies of plasma nitrided austenitic stainless steel.

PubMed

Stróz, D; Psoda, M

2010-03-01

Cross-sectional transmission electron microscopy and X-ray phase analysis were used to study the structure of a layer formed during nitriding the AISI 316L stainless steel at temperature 440 degrees C. It was found that the applied treatment led to the formation of 6-microm-thick layer of the S-phase. There is no evidence of CrN precipitation. The X-ray diffraction experiments proved that the occurred austenite lattice expansion - due to nitrogen atoms - depended on the crystallographic direction. The cross-sectional transmission electron microscopy studies showed that the layer consisted of a single cubic phase that contained a lot of defects such as dislocations, stacking faults, slip bands and twins. The high-resolution electron microscopy observations were applied to study the defect formation due to the nitriding process. It was shown that the presence of great number of stacking faults leads to formation of nanotwins. Weak, forbidden {100} reflections were still another characteristic feature of the S-phase. These were not detected in the X-ray spectra of the phase. Basing on the high-resolution electron microscopy studies it can be suggested that the short-range ordering of the nitrogen atoms in the octahedral sites inside the f.c.c. matrix lattice takes place and gives rise to appearance of these spots. It is suggested that the cubic lattice undergoes not only expansion but also slight rombohedral distortion that explains differences in the lattice expansion for different crystallographic directions.

Superconductivity in sputtered CuMO6S8

NASA Technical Reports Server (NTRS)

Alterovitz, S.; Woollam, J. A.; Kammerdiner, L.; Luo, H. L.; Martin, C.

1977-01-01

Samples were prepared by melting the metals, followed by annealing to various temperatures. The result was a structurally weak material. Sputtered films on sapphire substrates were prepared and studied. The substrates give the films mechanical strength and permit easy attachment of electrical leads. Materials were characterized by X-ray diffraction, electron microscopy, electrical resistance vs. temperature, and critical current measurements. Some of the results on CuMo6S8 are presented.

Magnesium Nanoparticles for Hydrogen Storage: Structure, Kinetics and Thermodynamics

NASA Astrophysics Data System (ADS)

Pasquini, L.; Brighi, M.; Montone, A.; Vittori Antisari, M.; Dam, B.; Palmisano, V.; Bonetti, E.

2012-08-01

Magnesium nanoparticles coated by a native oxide shell and decorated by palladium clusters were synthesized by the inert gas condensation technique. The kinetics and thermodynamics of hydrogen sorption were investigated by Sieverts measurements at high temperature and by optical hydrogenography close to ambient temperature. The structure and morphology of the nanoparticles were studied by electron microscopy and X-ray diffraction both in the as-prepared state and after hydrogen sorption cycles.

Temperature effect on the growth of Au-free InAs and InAs/GaSb heterostructure nanowires on Si substrate by MOCVD

NASA Astrophysics Data System (ADS)

Kakkerla, Ramesh Kumar; Anandan, Deepak; Hsiao, Chih-Jen; Yu, Hung Wei; Singh, Sankalp Kumar; Chang, Edward Yi

2018-05-01

We demonstrate the growth of vertically aligned Au-free InAs and InAs/GaSb heterostructure nanowires on Si (1 1 1) substrate by Metal Organic Chemical Vapor Deposition (MOCVD). The effect of growth temperature on the morphology and growth rate of the InAs and InAs/GaSb heterostructure nanowires (NWs) is investigated. Control over diameter and length of the InAs NWs and the GaSb shell thickness was achieved by using growth temperature. As the GaSb growth temperature increase, GaSb radial growth rate increases due to the increase in alkyl decomposition at the substrate surface. Diffusivity of the adatoms increases as the GaSb growth temperature increase which results in tapered GaSb shell growth. Scanning Electron Microscope (SEM) and Transmission Electron Microscope (TEM) measurements revealed that the morphology and shell thickness can be tuned by the growth temperature. Electron microscopy also shows the formation of GaSb both in radial and axial directions outside the InAs NW core can be controlled by the growth temperature. This study demonstrates the control over InAs NWs growth and the GaSb shell thickness can be achieved through proper growth temperature control, such technique is essential for the growth of nanowire for future nano electronic devices, such as Tunnel FET.

Electron-beam-irradiation-induced crystallization of amorphous solid phase change materials

NASA Astrophysics Data System (ADS)

Zhou, Dong; Wu, Liangcai; Wen, Lin; Ma, Liya; Zhang, Xingyao; Li, Yudong; Guo, Qi; Song, Zhitang

2018-04-01

The electron-beam-irradiation-induced crystallization of phase change materials in a nano sized area was studied by in situ transmission electron microscopy and selected area electron diffraction. Amorphous phase change materials changed to a polycrystalline state after being irradiated with a 200 kV electron beam for a long time. The results indicate that the crystallization temperature strongly depends on the difference in the heteronuclear bond enthalpy of the phase change materials. The selected area electron diffraction patterns reveal that Ge2Sb2Te5 is a nucleation-dominated material, when Si2Sb2Te3 and Ti0.5Sb2Te3 are growth-dominated materials.

Microwave Synthesized ZnO Nanorod Arrays for UV Sensors: A Seed Layer Annealing Temperature Study.

PubMed

Pimentel, Ana; Ferreira, Sofia Henriques; Nunes, Daniela; Calmeiro, Tomas; Martins, Rodrigo; Fortunato, Elvira

2016-04-20

The present work reports the influence of zinc oxide (ZnO) seed layer annealing temperature on structural, optical and electrical properties of ZnO nanorod arrays, synthesized by hydrothermal method assisted by microwave radiation, to be used as UV sensors. The ZnO seed layer was produced using the spin-coating method and several annealing temperatures, ranging from 100 to 500 °C, have been tested. X-ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscopy (AFM) and spectrophotometry measurements have been used to investigate the structure, morphology, and optical properties variations of the produced ZnO nanorod arrays regarding the seed layer annealing temperatures employed. After the growth of ZnO nanorod arrays, the whole structure was tested as UV sensors, showing an increase in the sensitivity with the increase of seed layer annealing temperature. The UV sensor response of ZnO nanorod arrays produced with the seed layer annealed temperature of 500 °C was 50 times superior to the ones produced with a seed layer annealed at 100 °C.

Microwave Synthesized ZnO Nanorod Arrays for UV Sensors: A Seed Layer Annealing Temperature Study

PubMed Central

Pimentel, Ana; Ferreira, Sofia Henriques; Nunes, Daniela; Calmeiro, Tomas; Martins, Rodrigo; Fortunato, Elvira

2016-01-01

The present work reports the influence of zinc oxide (ZnO) seed layer annealing temperature on structural, optical and electrical properties of ZnO nanorod arrays, synthesized by hydrothermal method assisted by microwave radiation, to be used as UV sensors. The ZnO seed layer was produced using the spin-coating method and several annealing temperatures, ranging from 100 to 500 °C, have been tested. X-ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscopy (AFM) and spectrophotometry measurements have been used to investigate the structure, morphology, and optical properties variations of the produced ZnO nanorod arrays regarding the seed layer annealing temperatures employed. After the growth of ZnO nanorod arrays, the whole structure was tested as UV sensors, showing an increase in the sensitivity with the increase of seed layer annealing temperature. The UV sensor response of ZnO nanorod arrays produced with the seed layer annealed temperature of 500 °C was 50 times superior to the ones produced with a seed layer annealed at 100 °C. PMID:28773423

Phase behaviors of binary mixtures composed of electron-rich and electron-poor triphenylene discotic liquid crystals

NASA Astrophysics Data System (ADS)

An, Lingling; Jing, Min; Xiao, Bo; Bai, Xiao-Yan; Zeng, Qing-Dao; Zhao, Ke-Qing

2016-09-01

Disk-like liquid crystals (DLCs) can self-assemble to ordered columnar mesophases and are intriguing one-dimensional organic semiconductors with high charge carrier mobility. To improve their applicable property of mesomorphic temperature ranges, we exploit the binary mixtures of electronic donor-acceptor DLC materials. The electron-rich 2,3,6,7,10,11-hexakis(alkoxy)triphenylenes (C4, C6, C8, C10, C12) and an electron-deficient tetrapentyl triphenylene-2,3,6,10-tetracarboxylate have been prepared and their binary mixtures have been investigated. The mesomorphism of the 1:1 (molar ratio) mixtures has been characterized by polarizing optical microscopy (POM), differential scanning calorimetry (DSC), and small angel x-ray scattering (SAXS). The self-assembled monolayer structure of a discogen on a solid-liquid interface has been imaged by the high resolution scanning tunneling microscopy (STM). The match of peripheral chain length has important influence on the mesomorphism of the binary mixtures. Project supported by the National Natural Science Foundation of China (Grant Nos. 51273133 and 51443004).

Determination of the five parameter grain boundary character distribution of nanocrystalline alpha-zirconium thin films using transmission electron microscopy

DOE PAGES

Ghamarian, I.; Samani, P.; Rohrer, G. S.; ...

2017-03-24

Grain boundary engineering and other fundamental materials science problems (e.g., phase transformations and physical properties) require an improvement in the understanding of the type and population of grain boundaries in a given system – yet, databases are limited in number and spare in detail, including for hcp crystals such as zirconium. One way to rapidly obtain databases to analyze is to use small-grained materials and high spatial resolution orientation microscopy techniques, such as ASTAR™/precession electron diffraction. To demonstrate this, a study of grain boundary character distributions was conducted for α-zirconium deposited at room temperature on fused silica substrates using physicalmore » vapor deposition. The orientation maps of the nanocrystalline thin films were acquired by the ASTARα/precession electron diffraction technique, a new transmission electron microscope based orientation microscopy method. The reconstructed grain boundaries were classified as pure tilt, pure twist, 180°-twist and 180°-tilt grain boundaries based on the distribution of grain boundary planes with respect to the angle/axis of misorientation associated with grain boundaries. The results of the current study were compared to the results of a similar study on α-titanium and the molecular dynamics results of grain boundary energy for α-titanium.« less

Structural and electrical properties of conducting diamond nanowires.

PubMed

Sankaran, Kamatchi Jothiramalingam; Lin, Yen-Fu; Jian, Wen-Bin; Chen, Huang-Chin; Panda, Kalpataru; Sundaravel, Balakrishnan; Dong, Chung-Li; Tai, Nyan-Hwa; Lin, I-Nan

2013-02-01

Conducting diamond nanowires (DNWs) films have been synthesized by N₂-based microwave plasma enhanced chemical vapor deposition. The incorporation of nitrogen into DNWs films is examined by C 1s X-ray photoemission spectroscopy and morphology of DNWs is discerned using field-emission scanning electron microscopy and transmission electron microscopy (TEM). The electron diffraction pattern, the visible-Raman spectroscopy, and the near-edge X-ray absorption fine structure spectroscopy display the coexistence of sp³ diamond and sp² graphitic phases in DNWs films. In addition, the microstructure investigation, carried out by high-resolution TEM with Fourier transformed pattern, indicates diamond grains and graphitic grain boundaries on surface of DNWs. The same result is confirmed by scanning tunneling microscopy and scanning tunneling spectroscopy (STS). Furthermore, the STS spectra of current-voltage curves discover a high tunneling current at the position near the graphitic grain boundaries. These highly conducting regimes of grain boundaries form effective electron paths and its transport mechanism is explained by the three-dimensional (3D) Mott's variable range hopping in a wide temperature from 300 to 20 K. Interestingly, this specific feature of high conducting grain boundaries of DNWs demonstrates a high efficiency in field emission and pave a way to the next generation of high-definition flat panel displays or plasma devices.

Direct synthesis of ultrafine tetragonal BaTiO3 nanoparticles at room temperature

PubMed Central

2011-01-01

A large quantity of ultrafine tetragonal barium titanate (BaTiO3) nanoparticles is directly synthesized at room temperature. The crystalline form and grain size are checked by both X-ray diffraction and transmission electron microscopy. The results revealed that the perovskite nanoparticles as fine as 7 nm have been synthesized. The phase transition of the as-prepared nanoparticles is investigated by the temperature-dependent Raman spectrum and shows the similar tendency to that of bulk BaTiO3 materials. It is confirmed that the nanoparticles have tetragonal phase at room temperature. PMID:21781339

Apparent critical thickness versus temperature for InAs quantum dot growth on GaAs(001)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Patella, F.; Arciprete, F.; Fanfoni, M.

2006-04-17

We studied the temperature dependence of the two-dimensional to three-dimensional growth transition in InAs/GaAs(001) heteroepitaxy by means of reflection high energy electron diffraction and atomic force microscopy. The observed shift of the transition to higher InAs deposition times, at temperatures above 500 deg. C, is not a change of critical thickness for islanding, which instead, is constant in the 450-560 deg. C range. Consequently, In-Ga intermixing and surface and interface strain have a negligible dependence on temperature in this range.

Effects of the Tempering and High-Pressure Torsion Temperatures on Microstructure of Ferritic/Martensitic Steel Grade 91

PubMed Central

Ganeev, Artur; Nikitina, Marina; Sitdikov, Vil; Islamgaliev, Rinat; Hoffman, Andrew; Wen, Haiming

2018-01-01

Grade 91 (9Cr-1Mo) steel was subjected to various heat treatments and then to high-pressure torsion (HPT) at different temperatures. Its microstructure was studied using transmission electron microscopy (TEM) and X-ray diffraction (XRD). Effects of the tempering temperature and the HPT temperature on the microstructural features and microhardness in the ultrafine-grained (UFG) Grade 91 steel were researched. The study of the UFG structure formation takes into account two different microstructures observed: before HPT in both samples containing martensite and in fully ferritic samples. PMID:29671761

Tribological behavior and self-healing functionality of TiNbCN-Ag coatings in wide temperature range

NASA Astrophysics Data System (ADS)

Bondarev, A. V.; Kiryukhantsev-Korneev, Ph. V.; Levashov, E. A.; Shtansky, D. V.

2017-02-01

Ag- and Nb-doped TiCN coatings with about 2 at.% of Nb and Ag contents varied between 4.0 and 15.1 at.% were designed as promising materials for tribological applications in a wide temperature range. We report on the structure, mechanical, and tribological properties of TiNbCN-Ag coatings fabricated by simultaneous co-sputtering of TiC0.5 + 10%Nb2C and Ag targets in comparison with those of Ag-free coating. The tribological characteristics were evaluated during constant-temperature tests both at room temperature and 300 °C, as well as during dynamic temperature ramp tests in the range of 25-700 °C. The coating structure and elemental composition were studied by means of X-ray diffraction, scanning and transmission electron microscopy, and glow discharge optical emission spectroscopy. The coating microstructures and elemental compositions inside wear tracks, as well as the wear products, were examined by scanning electron microscopy, energy-dispersive spectroscopy, and Raman spectroscopy. We demonstrate that simultaneous alloying with Nb and Ag permits to overcome the main drawbacks of TiCN coatings such as their relatively high values of friction coefficient at elevated temperatures and low oxidation resistance. It is shown that a relatively high amount of Ag (15 at.%) is required to provide enhanced tribological behavior in a wide temperature range of 25-700 °C. In addition, the prepared Ag-doped coatings demonstrated active oxidation protection and self-healing functionality due to the segregation of Ag metallic particles in damage areas such as cracks, pin-holes, or oxidation sites.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ovcharov, A. V.; Karateev, I. A.; Mikhutkin, A. A.

The surface microstructure of Ni–W alloy tapes, which are used as substrates to form films of high-temperature superconductors and photovoltaic devices, has been studied. Several samples of a Ni{sub 95}W{sub 5} tape (Evico) annealed under different conditions were analyzed using scanning electron microscopy, energy-dispersive X-ray microanalysis, electron diffraction, and electron energy-loss spectroscopy. NiWO{sub 4} precipitates are found on the surface of annealed samples. The growth of precipitates at a temperature of 950°C is accompanied by the formation of pores on the surface or under an oxide film. Depressions with a wedge-shaped profile are found at the grain boundaries. Annealing inmore » a reducing atmosphere using a specially prepared chamber allows one to form a surface free of nickel tungstate precipitates.« less

The control of ice crystal growth and effect on porous structure of konjac glucomannan-based aerogels.

PubMed

Ni, Xuewen; Ke, Fan; Xiao, Man; Wu, Kao; Kuang, Ying; Corke, Harold; Jiang, Fatang

2016-11-01

Konjac glucomannan (KGM)-based aerogels were prepared using a combination of sol-gel and freeze-drying methods. Preparation conditions were chosen to control ice crystal growth and aerogel structure formation. The ice crystals formed during pre-freezing were observed by low temperature polarizing microscopy, and images of aerogel pores were obtained by scanning electron microscopy. The size of ice crystals were calculated and size distribution maps were drawn, and similarly for aerogel pores. Results showed that ice crystal growth and aerogel pore sizes may be controlled by varying pre-freezing temperatures, KGM concentration and glyceryl monostearate concentration. The impact of pre-freezing temperatures on ice crystal growth was explained as combining ice crystal growth rate with nucleation rate, while the impacts of KGM and glyceryl monostearate concentration on ice crystal growth were interpreted based on their influences on sol network structure. Copyright © 2016 Elsevier B.V. All rights reserved.

Evolution of Near-Surface Internal and External Oxide Morphology During High-Temperature Selective Oxidation of Steels

NASA Astrophysics Data System (ADS)

Story, Mary E.; Webler, Bryan A.

2018-05-01

In this work we examine some observations made using high-temperature confocal scanning laser microscopy (HT-CSLM) during selective oxidation experiments. A plain carbon steel and advanced high-strength steel (AHSS) were selectively oxidized at high temperature (850-900°C) in either low oxygen or water vapor atmospheres. Surface evolution, including thermal grooving along grain boundaries and oxide growth, was viewed in situ during heating. Experiments investigated the influence of the microstructure and oxidizing atmosphere on selective oxidation behavior. Sequences of CSLM still frames collected during the experiment were processed with ImageJ to obtain histograms that showed a general darkening trend indicative of oxidation over time with all samples. Additional ex situ scanning electron microscopy and energy dispersive spectroscopy analysis supported in situ observations. Distinct oxidation behavior was observed for each case. Segregation, grain orientation, and extent of internal oxidation were all found to strongly influence surface evolution.

High-temperature ultrasonic characterization of the mechanical and microstructural behavior of a fibrous composite with a magnesium lithium aluminum silicate glass-ceramic matrix

DOE Office of Scientific and Technical Information (OSTI.GOV)

Cutard, T.; Huger, M.; Fargeot, D.

The mechanical behavior and the microstructural modifications of a SiC-fiber-reinforced magnesium lithium aluminum silicate glass-ceramic (SiC/MASL) have been characterized by ultrasonic measurement of uniaxial Young`s modulus at high temperature. Under vacuum, long isothermal agings in the 750--1,000 C temperature range have shown matrix modifications in terms of crystallization of residual glassy phases, and of phase transformations in the Li{sub 2}O-Al{sub 2}O{sub 3}-SiO{sub 2} system. In air, long isothermal agings performed under the same conditions have led to the same matrix transformations but in competition with oxidation mechanisms of the carbon fiber-matrix interphase. All of these matrix and/or interface transformations havemore » been confirmed by X-ray diffraction analysis, scanning electron microscopy, scanning acoustic microscopy, and microindentation tests.« less

Influence of interface layer on optical properties of sub-20 nm-thick TiO2 films

NASA Astrophysics Data System (ADS)

Shi, Yue-Jie; Zhang, Rong-Jun; Li, Da-Hai; Zhan, Yi-Qiang; Lu, Hong-Liang; Jiang, An-Quan; Chen, Xin; Liu, Juan; Zheng, Yu-Xiang; Wang, Song-You; Chen, Liang-Yao

2018-02-01

The sub-20 nm ultrathin titanium dioxide (TiO2) films with tunable thickness were deposited on Si substrates by atomic layer deposition (ALD). The structural and optical properties were acquired by transmission electron microscopy, atomic force microscopy and spectroscopic ellipsometry. Afterwards, a constructive and effective method of analyzing interfaces by applying two different optical models consisting of air/TiO2/Ti x Si y O2/Si and air/effective TiO2 layer/Si, respectively, was proposed to investigate the influence of interface layer (IL) on the analysis of optical constants and the determination of band gap of TiO2 ultrathin films. It was found that two factors including optical constants and changing components of the nonstoichiometric IL could contribute to the extent of the influence. Furthermore, the investigated TiO2 ultrathin films of 600 ALD cycles were selected and then annealed at the temperature range of 400-900 °C by rapid thermal annealing. Thicker IL and phase transition cause the variation of optical properties of TiO2 films after annealing and a shorter electron relaxation time reveals the strengthened electron-electron and electron-phonon interactions in the TiO2 ultrathin films at high temperature. The as-obtained results in this paper will play a role in other studies of high dielectric constants materials grown on Si substrates and in the applications of next generation metal-oxide-semiconductor devices.

Control of Wigner localization and electron cavity effects in near-field emission spectra of In(Ga)P/GaInP quantum-dot structures

NASA Astrophysics Data System (ADS)

Mintairov, A. M.; Kapaldo, J.; Merz, J. L.; Rouvimov, S.; Lebedev, D. V.; Kalyuzhnyy, N. A.; Mintairov, S. A.; Belyaev, K. G.; Rakhlin, M. V.; Toropov, A. A.; Brunkov, P. N.; Vlasov, A. S.; Zadiranov, Yu. M.; Blundell, S. A.; Mozharov, A. M.; Mukhin, I.; Yakimov, M.; Oktyabrsky, S.; Shelaev, A. V.; Bykov, V. A.

2018-05-01

Structural and emission properties of few-electron In(Ga)P/GaInP quantum dots (QDs) representing natural Wigner molecules (WM) and whispering gallery mode (WGM) electron (e ) cavities have been investigated. QD structures were grown using self-organized metal-organic vapor phase epitaxy and deposition from ˜3 to 7 monolayers of InP at 700 °C. Using atomic force microscopy, transmission electron microscopy, near-field scanning optical microscopy (NSOM), and μ -photoluminescence (μ -PL) spectra we obtained In(Ga)P/GaInP QDs having lateral size 80-180 nm, height 5-30 nm, Ga content 0.0-0.4, density 2 -10 μm-2 , and electron population up to 20 and demonstrated control of their density and size distribution. Using high-spatial-resolution low-temperature PL spectra, NSOM imaging, and calculations of charge density distributions we observed Wigner localization and e -cavity effects for a series of dots having quantum confinement ℏ ω0=0.5 -6 meV . We used these data together with time-resolved PL measurements to clarify the effect of Coulomb interaction and WM formation on emission spectra of few-electron QDs. We present direct observation of 2 e , 6 e , and 9 e WMs; 2 e and 4 e WGMs; and Fabry-Perot e modes and establish conditions of e -WGM-cavity formation in these QDs.

Precipitation in Ni-Si during electron and ion irradiation

NASA Astrophysics Data System (ADS)

Lucas, G. E.; Zama, T.; Ishino, S.

1986-11-01

This study was undertaken to further investigate how the nature of the irradiation condition affects precipitation in a dilute Ni-Si system. Transmission electron microscopy (TEM) discs of a solution annealed Ni alloy containing 5 at% Si were irradiated with 400 keV Ar + ions, 200 keV He + ions and 1 MeV electrons at average displacement rates in the range 2 × 10 -5dpa/s to 2 × 10 -3dpa/s at temperatures in the range 25°C to 450°C. Samples irradiated with electrons were observed in situ in an HVEM, while ion irradiated specimens were examined in a TEM after irradiation. Precipitation of Ni 3Si was detected by the appearance of superlattice spots in the electron diffraction patterns. It was found that as the mass of the irradiating species increased, the lower bound temperature at which Ni 3Si precipitation was first observed increased. For electron irradiation, the lower bound temperature at 2 × 10 -3dpa/s was ˜125°C, whereas for 400 keV Ar + irradiation at a similar average displacement rate the lower boundary was approximately 325°C. This suggests that cascade disordering competes with radiation induced solute segregation.

Effect of deposition pressure on the microstructure and thermoelectric properties of epitaxial ScN(001) thin films sputtered onto MgO(001) substrates

DOE PAGES

Burmistrova, Polina V.; Zakharov, Dmitri N.; Favaloro, Tela; ...

2015-03-14

Four epitaxial ScN(001) thin films were successfully deposited on MgO(001) substrates by dc reactive magnetron sputtering at 2, 5, 10, and 20 mTorr in an Ar/N2 ambient atmosphere at 650 °C. The microstructure of the resultant films was analyzed by x-ray diffraction, scanning electron microscopy, and transmission electron microscopy. Electrical resistivity, electron mobility and concentration were measured using the room temperature Hall technique, and temperature dependent in-plain measurements of the thermoelectric properties of the ScN thin films were performed. The surface morphology and film crystallinity significantly degrade with increasing deposition pressure. The ScN thin film deposited at 20 mTorr exhibitsmore » the presence of <221> oriented secondary grains resulting in decreased electric properties and a low thermoelectric power factor of 0.5 W/m-K² at 800 K. ScN thin films grown at 5 and 10 mTorr are single crystalline, yielding the power factor of approximately 2.5 W/m-K² at 800 K. The deposition performed at 2 mTorr produces the highest quality ScN thin film with the electron mobility of 98 cm² V⁻¹ s⁻¹ and the power factor of 3.3 W/m-K² at 800 K.« less

Modified Graphene with SnO2 Nanocomposites Using Thermal Decomposition Method and Sensing Behavior Towards NO2 Gas

NASA Astrophysics Data System (ADS)

Sharma, Vikram

2017-11-01

This is the first time the graphene sample has been functionalized with metal oxide nanoparticles by thermal decomposition process. In this paper, graphene has been synthesized from natural resources using flower petals as carbon feedstock by thermal exfoliation technique at temperatures 1300 °C and the synthesis of graphene-tin oxide (SnO2) nanocomposites has been done using chemical treatment followed by thermal decomposition method. The response versus time condition has been investigated for the fabricated sample. The electrical resistance w.r.t. temperature could be explained by the thermal generation of electron-hole pairs and carrier scattering by acoustic phonons. The structural, morphological and chemical composition studies of the nanocomposites were carried out by the Raman spectroscopy, x-ray diffraction spectroscopy, scanning electron microscopy (SEM), x-ray photoelectron spectroscopy and high-resolution transmission electron microscopy (HRTEM). The evidence of good-quality graphene is obtained from Raman spectroscopy studies. The SEM and HRTEM images have shown that SnO2 nanoparticles are well distributed in the multilayer electron transparent graphene films. The sensor response was found to lie between 8.25 and 9.36% at 500 ppm of nitrogen dioxide, and also resistance recovered quickly without any application of heat. We believe such chemical treatment of graphene could potentially be used to manufacture a new generation of low-power nano-NO2 sensors.

Growth temperature optimization of GaAs-based In0.83Ga0.17As on InxAl1-xAs buffers

NASA Astrophysics Data System (ADS)

Chen, X. Y.; Gu, Y.; Zhang, Y. G.; Ma, Y. J.; Du, B.; Zhang, J.; Ji, W. Y.; Shi, Y. H.; Zhu, Y.

2018-04-01

Improved quality of gas source molecular beam epitaxy grown In0.83Ga0.17As layer on GaAs substrate was achieved by adopting a two-step InxAl1-xAs metamorphic buffer at different temperatures. With a high-temperature In0.83Al0.17As template following a low-temperature composition continuously graded InxAl1-xAs (x = 0.05-0.86) buffer, better structural, optical and electrical properties of succeeding In0.83Ga0.17As were confirmed by atomic force microscopy, photoluminescence and Hall-effect measurements. Cross-sectional transmission electron microscopy revealed significant effect of the two-step temperature grown InAlAs buffer layers on the inhibition of threading dislocations due to the deposition of high density nuclei on GaAs substrate at the low growth temperature. The limited reduction for the dark current of GaAs-based In0.83Ga0.17As photodetectors on the two-step temperature grown InxAl1-xAs buffer layers was ascribed to the contribution of impurities caused by the low growth temperature of InAlAs buffers.

Chitosan-phosphotungstic acid complex as membranes for low temperature H2-O2 fuel cell

NASA Astrophysics Data System (ADS)

Santamaria, M.; Pecoraro, C. M.; Di Quarto, F.; Bocchetta, P.

2015-02-01

Free-standing Chitosan/phosphotungstic acid polyelectrolyte membranes were prepared by an easy and fast in-situ ionotropic gelation process performed at room temperature. Scanning electron microscopy was employed to study their morphological features and their thickness as a function of the chitosan concentration. The membrane was tested as proton conductor in low temperature H2-O2 fuel cell allowing to get peak power densities up to 350 mW cm-2. Electrochemical impedance measurements allowed to estimate a polyelectrolyte conductivity of 18 mS cm-1.

Mechanical Behavior of Sapphire Reinforced Alumina Matrix Composites at Elevated Temperatures

NASA Technical Reports Server (NTRS)

Jaskowiak, Martha H.; Eldridge, Jeffrey I.; Setlock, John A.; Gyekenyesi, John Z.

1997-01-01

Zirconia coated sapphire reinforced alumina matrix composites have been tested both after heat treatment to 1400 C and at temperatures ranging from 800 C to 1200 C in. air. Interfacial shear stress has also been measured with fiber pushout tests performed in air at room temperature, 800 C and 1OOO C. Matrix crack spacing was measured for the tensile tested composites and used to estimate interfacial shear stress up to 1200 C. Electron microscopy was used to determine the source of fiber fracture and to study interfacial failure within the composite.

The room-temperature synthesis of anisotropic CdHgTe quantum dot alloys: a "molecular welding" effect.

PubMed

Taniguchi, Shohei; Green, Mark; Lim, Teck

2011-03-16

The room-temperature chemical transformation of spherical CdTe nanoparticles into anisotropic alloyed CdHgTe particles using mercury bromide in a toluene/methanol system at room temperature has been investigated. The resulting materials readily dissolved in toluene and exhibited a significant red-shift in the optical properties toward the infrared region. Structural transformations were observed, with electron microscopy showing that the CdTe nanoparticles were chemically attached ('welded') to other CdTe nanoparticles, creating highly complex anisotropic heterostructures which also incorporated mercury.

Temperature dependence of spin-orbit torques in W/CoFeB bilayers

DOE Office of Scientific and Technical Information (OSTI.GOV)

Skowroński, Witold, E-mail: skowron@agh.edu.pl; Cecot, Monika; Kanak, Jarosław

We report on the temperature variation of spin-orbit torques in perpendicularly magnetized W/CoFeB bilayers. Harmonic Hall voltage measurements in perpendicularly magnetized CoFeB reveal increased longitudinal and transverse effective magnetic field components at low temperatures. The damping-like spin-orbit torque reaches an efficiency of 0.55 at 19 K. Scanning transmission electron microscopy and X-ray reflectivity measurements indicate that considerable interface mixing between W and CoFeB may be responsible for strong spin-orbit interactions.

New developments in electron microscopy for serial image acquisition of neuronal profiles.

PubMed

Kubota, Yoshiyuki

2015-02-01

Recent developments in electron microscopy largely automate the continuous acquisition of serial electron micrographs (EMGs), previously achieved by laborious manual serial ultrathin sectioning using an ultramicrotome and ultrastructural image capture process with transmission electron microscopy. The new systems cut thin sections and capture serial EMGs automatically, allowing for acquisition of large data sets in a reasonably short time. The new methods are focused ion beam/scanning electron microscopy, ultramicrotome/serial block-face scanning electron microscopy, automated tape-collection ultramicrotome/scanning electron microscopy and transmission electron microscope camera array. In this review, their positive and negative aspects are discussed. © The Author 2015. Published by Oxford University Press on behalf of The Japanese Society of Microscopy. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

Copper vapor-assisted growth of hexagonal graphene domains on silica islands

DOE Office of Scientific and Technical Information (OSTI.GOV)

Li, Jun; Que, Yande; Jiang, Lili

2016-07-11

Silica (SiO{sub 2}) islands with a dendritic structure were prepared on polycrystalline copper foil, using silane (SiH{sub 4}) as a precursor, by annealing at high temperature. Assisted by copper vapor from bare sections of the foil, single-layer hexagonal graphene domains were grown directly on the SiO{sub 2} islands by chemical vapor deposition. Scanning electron microscopy, atomic force microscopy, Raman spectra, and X-ray photoelectron spectroscopy confirm that hexagonal graphene domains, each measuring several microns, were synthesized on the silica islands.

The substitution of aluminum for cobalt in nanostructured bainitic steels

NASA Astrophysics Data System (ADS)

Yang, Jing; Qiu, Hui; Xu, Pudong; Yu, Hui; Wang, Yuchen

2018-06-01

Two kinds of new steels are designed, in which the only difference is the use of the alloy element aluminum instead of cobalt. The effect of cobalt and aluminum addition on the microstructure and mechanical properties of high-carbon nanostructured bainitic steels was studied. The microstructure and mechanical properties achieved by a low temperature au tempering treatment were investigated by optical microscopy, X-ray diffraction, scanning and transmission electron microscopy and hardness, tension, impact tests. The experimental results show that better mechanical properties were achieved in the high-carbon Al-contained steel.

Size-selective breaking of the core-shell structure of gallium nanoparticles.

PubMed

Catalán Gómez, Sergio; Redondo-Cubero, Andres; Palomares Simon, Francisco Javier; Vazquez Burgos, Luis; Nogales, Emilio; Nucciarelli, Flavio; Mendez, Bianchi; Gordillo, Nuria; Pau, Jose Luis

2018-06-11

Core-shell gallium nanoparticles (Ga NPs) have recently been proposed as an ultraviolet plasmonic material for different applications but only at room temperature. Here, the thermal stability as a function of the size of the NPs is reported over a wide range of temperatures. We analyse the chemical and structural properties of the oxide shell by x-ray photoelectron spectroscopy and atomic force microscopy. We demonstrate the inverse dependence of the shell breaking temperature with the size of the NPs. Spectroscopic ellipsometry is used for tracking the rupture and its mechanism is systematically investigated by scanning electron microscopy, grazing incidence x-ray diffraction and cathodoluminescence. Taking advantage of the thermal stability of the NPs, we perform complete oxidations that lead to homogenous gallium oxide NPs. Thus, this study set the physical limits of Ga NPs to last at high temperatures, and opens up the possibility to achieve totally oxidized NPs while keeping their sphericity. © 2018 IOP Publishing Ltd.

Temperature-triggered micellization of block copolymers on an ionic liquid surface.

PubMed

Lu, Haiyun; Akgun, Bulent; Wei, Xinyu; Li, Le; Satija, Sushil K; Russell, Thomas P

2011-10-18

In situ neutron reflectivity was used to study thermally induced structural changes of the lamellae-forming polystyrene-block-poly(2-vinylpyridine) (PS-b-P2VP) block copolymer thin films floating on the surface of an ionic liquid (IL). The IL, 1-butyl-3-methylimidazolium trifluoromethanesulfonate, is a nonsolvent for PS and a temperature-tunable solvent for P2VP, and, as such, micellization can be induced at the air-IL interface by changing the temperature. Transmission electron microscopy and scanning force microscopy were used to investigate the resultant morphologies of the micellar films. It was found that highly ordered nanostructures consisting of spherical micelles with a PS core surrounded by a P2VP corona were produced. In addition, bilayer films of PS homopolymer on top of a PS-b-P2VP layer also underwent micellization with increasing temperature but the micellization was strongly dependent on the thickness of the PS and PS-b-P2VP layers. © 2011 American Chemical Society

Temperature tunable micellization of polystyrene-block-poly(2-vinylpyridine) at Si-ionic liquid interface.

PubMed

Lu, Haiyun; Lee, Dong Hyun; Russell, Thomas P

2010-11-16

Highly ordered and stable micelles formed from both symmetric and asymmetric block copolymers of polystyrene-block-poly(2-vinylpyridine) (PS-b-P2VP) at the Si-ionic liquid (IL) interface have been investigated by scanning force microscopy (SFM) and transmission electron microscopy (TEM). The 1-butyl-3-methylimidazolium trifluoromethanesulfonate IL, a selective and temperature-tunable solvent for the P2VP block, was used and gave rise to block copolymer micelles having different morphologies that strongly depended on the annealing temperature. The effects of film thickness, molecular weight of block copolymers, and experimental conditions, such as preannealing, rinsing, and substrate properties, on the morphologies of block copolymer micelles were also studied. In addition, spherical micelles consisting of PS core and P2VP shell could also be obtained by core-corona inversion by annealing the as-coated micellar film in the IL at high temperatures. The possible mechanism for micelle formation is discussed.

Scanning Probe Microscopies and Their Applications Towards the Study of Superconductors

NASA Astrophysics Data System (ADS)

Helfrich, Jennifer Ann

1995-11-01

The invention of the scanning tunneling microscope (STM) in 1982 made it possible to study surfaces and structures at resolutions previously believed unattainable. Adapting the STM for low temperatures makes it possible to study superconductors with new methods and to obtain valuable information. This thesis describes a novel low temperature STM (LTSTM) that was designed and built at Northwestern University for the purpose of studying superconductors in the mixed state. At low temperatures, this LTSTM has a scan range an order of magnitude larger than other LTSTM's designed elsewhere. It is capable of low temperature imaging and obtaining dI/dV vs. V curves. A detailed study of magnetic force microscopy (MFM) probes is also presented. The fields and forces between probe and surface were computer modeled. These results are compared with results from electron holographs of MFM probes. The final section of the thesis describes an a.c. susceptibility measurement on a UPt_3 sphere. Results are presented and discussed.

Mn-doped Ge self-assembled quantum dots via dewetting of thin films

NASA Astrophysics Data System (ADS)

Aouassa, Mansour; Jadli, Imen; Bandyopadhyay, Anup; Kim, Sung Kyu; Karaman, Ibrahim; Lee, Jeong Yong

2017-03-01

In this study, we demonstrate an original elaboration route for producing a Mn-doped Ge self-assembled quantum dots on SiO2 thin layer for MOS structure. These magnetic quantum dots are elaborated using dewetting phenomenon at solid state by Ultra-High Vacuum (UHV) annealing at high temperature of an amorphous Ge:Mn (Mn: 40%) nanolayer deposed at very low temperature by high-precision Solid Source Molecular Beam Epitaxy on SiO2 thin film. The size of quantum dots is controlled with nanometer scale precision by varying the nominal thickness of amorphous film initially deposed. The magnetic properties of the quantum-dots layer have been investigated by superconducting quantum interference device (SQUID) magnetometry. Atomic force microscopy (AFM), x-ray energy dispersive spectroscopy (XEDS) and transmission electron microscopy (TEM) were used to examine the nanostructure of these materials. Obtained results indicate that GeMn QDs are crystalline, monodisperse and exhibit a ferromagnetic behavior with a Curie temperature (TC) above room temperature. They could be integrated into spintronic technology.

Direct writing of room temperature and zero field skyrmion lattices by a scanning local magnetic field

NASA Astrophysics Data System (ADS)

Zhang, Senfu; Zhang, Junwei; Zhang, Qiang; Barton, Craig; Neu, Volker; Zhao, Yuelei; Hou, Zhipeng; Wen, Yan; Gong, Chen; Kazakova, Olga; Wang, Wenhong; Peng, Yong; Garanin, Dmitry A.; Chudnovsky, Eugene M.; Zhang, Xixiang

2018-03-01

Magnetic skyrmions are topologically protected nanoscale spin textures exhibiting fascinating physical behaviors. Recent observations of room temperature skyrmions in sputtered multilayer films are an important step towards their use in ultra-low power devices. Such practical applications prefer skyrmions to be stable at zero magnetic fields and room temperature. Here, we report the creation of skyrmion lattices in Pt/Co/Ta multilayers by a scanning local field using magnetic force microscopy tips. We also show that those newly created skyrmion lattices are stable at both room temperature and zero fields. Lorentz transmission electron microscopy measurements reveal that the skyrmions in our films are of Néel-type. To gain a deeper understanding of the mechanism behind the creation of a skyrmion lattice by the scanning of local fields, we perform micromagnetic simulations and find the experimental results to be in agreement with our simulation data. This study opens another avenue for the creation of skyrmion lattices in thin films.

Enhanced stress corrosion cracking resistance and electrical conductivity of a T761 treated Al-Zn-Mg-Cu alloy thin plate

NASA Astrophysics Data System (ADS)

Chen, Xu; Zhai, Sudan; Gao, Di; Liu, Ye; Xu, Jing; Liu, Yang

2018-01-01

The stress corrosion cracking (SCC) behavior, electrical conductivity and mechanical properties of an Al-Zn-Mg-Cu alloy pre-stretched thin plate for wing skin were researched in this paper. The microstructures and SCC fracture surfaces of the alloy treated at different conditions were characterized by transmission electron microscopy, optical microscopy and scanning electron microscopy. Results indicated that with the increasing of aging temperature, the electrical conductivity and the elongation increased greatly, while the strength decreased gradually which were closely associated with the type and morphology of the precipitates. Compared with the T6 treated alloy, the SCC resistance of the T761 treated Al-Zn-Mg-Cu alloy was improved greatly. The SCC behavior of the T6 treated alloy was dominated by anodic dissolution theory, whereas the hydrogen induced cracking controlled the fracture behavior of the T761 treated alloy which was influenced by the morphology of grain boundary precipitates in this investigated alloy.

Correlation between molten vanadium salts and the structural degradation of HK-type steel superheater tubes

NASA Astrophysics Data System (ADS)

de Carvalho Nunes, Frederico; de Almeida, Luiz Henrique; Ribeiro, André Freitas

2006-12-01

HK steels are among the most used heat-resistant cast stainless steels, being corrosion-resistant and showing good mechanical properties at high service temperatures. These steels are widely used in reformer furnaces and as superheater tubes. During service, combustion gases leaving the burners come in contact with these tubes, resulting in corrosive attack and a large weight loss occurs due to the presence of vanadium, which forms low melting point salts, removing the protective oxide layer. In this work the external surface of a tube with dramatic wall thickness reduction was analyzed using light microscopy, scanning electron microscopy, and transmission electron microscopy. The identification of the phases was achieved by energy dispersive spectroscopy (EDS) analyses. The results showed oxides arising from the external surface. In this oxidized region vanadium compounds inside chromium carbide particles were also observed, due to inward vanadium diffusion during corrosion attack. A chemical reaction was proposed to explain the presence of vanadium in the metal microstructure.

Spatial Complexity Due to Bulk Electronic Liquid Crystals in Superconducting Dy-Bi2212

NASA Astrophysics Data System (ADS)

Carlson, Erica; Phillabaum, Benjamin; Dahmen, Karin

2012-02-01

Surface probes such as scanning tunneling microscopy (STM) have detected complex electronic patterns at the nanoscale in many high temperature superconductors. In cuprates, the pattern formation is associated with the pseudogap phase, a precursor to the high temperature superconducting state. Rotational symmetry breaking of the host crystal (i.e. from C4 to C2) in the form of electronic nematicity has recently been proposed as a unifying theme of the pseudogap phase [Lawler Nature 2010]. However, the fundamental physics governing the nanoscale pattern formation has not yet been identified. Here we use universal cluster properties extracted from STM studies of cuprate superconductors to identify the funda- mental physics controlling the complex pattern formation. We find that due to a delicate balance between disorder, interactions, and material anisotropy, the rotational symmetry breaking is fractal in nature, and that the electronic liquid crystal extends throughout the bulk of the material.

In Situ Microstructural Control and Mechanical Testing Inside the Transmission Electron Microscope at Elevated Temperatures

NASA Astrophysics Data System (ADS)

Wang, Baoming; Haque, M. A.

2015-08-01

With atomic-scale imaging and analytical capabilities such as electron diffraction and energy-loss spectroscopy, the transmission electron microscope has allowed access to the internal microstructure of materials like no other microscopy. It has been mostly a passive or post-mortem analysis tool, but that trend is changing with in situ straining, heating and electrical biasing. In this study, we design and demonstrate a multi-functional microchip that integrates actuators, sensors, heaters and electrodes with freestanding electron transparent specimens. In addition to mechanical testing at elevated temperatures, the chip can actively control microstructures (grain growth and phase change) of the specimen material. Using nano-crystalline aluminum, nickel and zirconium as specimen materials, we demonstrate these novel capabilities inside the microscope. Our approach of active microstructural control and quantitative testing with real-time visualization can influence mechanistic modeling by providing direct and accurate evidence of the fundamental mechanisms behind materials behavior.

Accurate calibration for the quantification of the Al content in AlGaN epitaxial layers by energy-dispersive X-ray spectroscopy in a Transmission Electron Microscope

NASA Astrophysics Data System (ADS)

Amari, H.; Lari, L.; Zhang, H. Y.; Geelhaar, L.; Chèze, C.; Kappers, M. J.; McAleese, C.; Humphreys, C. J.; Walther, T.

2011-11-01

Since the band structure of group III- nitrides presents a direct electronic transition with a band-gap energy covering the range from 3.4 eV for (GaN) to 6.2 eV (for AlN) at room temperature as well as a high thermal conductivity, aluminium gallium nitride (AlGaN) is a strong candidate for high-power and high-temperature electronic devices and short-wavelength (visible and ultraviolet) optoelectronic devices. We report here a study by energy-filtered transmission electron microscopy (EFTEM) and energy-dispersive X-ray spectroscopy (EDXS) of the micro structure and elemental distribution in different aluminium gallium nitride epitaxial layers grown by different research groups. A calibration procedure is out-lined that yields the Al content from EDXS to within ~1 at % precision.

Electronic properties of two inequivalent surfaces in MoTe2 studied by quasi-particle interference

NASA Astrophysics Data System (ADS)

Iaia, Davide; Shichao, Yan; Madhavan, Vidya

MoTe2 has received renewed interest due to its topological properties. At a temperature below 250 K, MoTe2 is a type II Weyl semimetal hosting three-dimensional (3D) linearly dispersing states with well defined chirality. Nodes in this 3D dispersion are called Weyl points. Weyl points of opposite chirality are expected to be connected by topologically protected Fermi arcs. In this talk we discuss low temperature scanning tunneling microscopy studies of the electronic structure of MoTe2. The electronic properties are studied using quasi-particle interference technique which allows us to resolve Fermi arcs features and to clearly distinguish between two inequivalent MoTe2 surfaces. Our results provide important contributions to further our understanding of the electronic properties of this new and exotic class of materials. National Science Foundation (NSF).

Fabrication of a temperature-responsive and recyclable MoS2 nanocatalyst through composting with poly (N-isopropylacrylamide)

NASA Astrophysics Data System (ADS)

Liu, Yan; Chen, Pengpeng; Nie, Wangyan; Zhou, Yifeng

2018-04-01

A temperature-responsive, recyclable nanocatalyst was fabricated by composting the exfoliated molybdenum disulfide (MoS2) nanosheets with poly (N-isopropylacry lamide) (PNIPAM). The structure and morphology of MoS2/PNIPAM nanocatalyst was fully characterized by Fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), Thermogravimetry analysis (TGA), Scanning electron microscope (SEM) and Transmission electron microscopy (TEM). The temperature-responsive properties of the MoS2/PNIPAM nanocatalyst were confirmed by Dynamic Light Scattering (DLS) and Ultraviolet-visible ((UV-vis)) absorption spectroscopy. The catalytic activities of the MoS2/PNIPAM nanocatalyst were studied using the reduction reaction of 4-nitrophenol (4-NP) to 4-aminophenol (4-AP) as the model reaction. Results showed that the catalytic activity of the MoS2/PNIPAM nanocatalyst could be regulated by temperature. Furthermore, when the temperature went higher than the low critical solution temperature (LCST) of PNIPAM, the MoS2/PNIPAM nanocatalyst tended to aggregated to form bulk materials from homogeneous suspension.

The low-temperature method for study of coniferous tissues in the environmental scanning electron microscope.

PubMed

Neděla, Vilém; Tihlaříková, Eva; Hřib, Jiří

2015-01-01

The use of non-standard low-temperature conditions in environmental scanning electron microscopy might be promising for the observation of coniferous tissues in their native state. This study is aimed to analyse and evaluate the method based on the principle of low-temperature sample stabilization. We demonstrate that the upper mucous layer is sublimed and a microstructure of the sample surface can be observed with higher resolution at lower gas pressure conditions, thanks to a low-temperature method. An influence of the low-temperature method on sample stability was also studied. The results indicate that high-moisture conditions are not suitable for this method and often cause the collapse of samples. The potential improvement of stability to beam damage has been demonstrated by long-time observation at different operation parameters. We finally show high applicability of the low-temperature method on different types of conifers and Oxalis acetosella. © 2014 Wiley Periodicals, Inc.

Scanning tunneling microscopy and spectroscopy studies of the heavy-electron superconductor TlNi2Se2

NASA Astrophysics Data System (ADS)

Wilfert, Stefan; Schmitt, Martin; Schmidt, Henrik; Mauerer, Tobias; Sessi, Paolo; Wang, Hangdong; Mao, Qianhui; Fang, Minghu; Bode, Matthias

2018-01-01

We report on the structural and superconducting electronic properties of the heavy-electron superconductor TlNi2Se2 . By using a variable-temperature scanning tunneling microscopy (VT-STM) the coexistence of (√{2 }×√{2 }) R 45∘ and (2 ×1 ) surface reconstructions is observed. Similar to earlier observations on the "122" family of Fe-based superconductors, we find that their respective surface fraction strongly depends on the temperature during cleavage, the measurement temperature, and the sample's history. Cleaving at low temperature predominantly results in the (√{2 }×√{2 }) R 45∘ -reconstructed surface. A detailed analysis of the (√{2 }×√{2 }) R 45∘ -reconstructed domains identifies (2 ×1 ) -ordered dimers, tertramers, and higher order even multimers as domain walls. Higher cleaving temperatures and the warming of low-temperature-cleaved samples increases the relative weight of the (2 ×1 ) surface reconstruction. By slowly increasing the sample temperature Ts inside the VT-STM we find that the (√{2 }×√{2 }) R 45∘ surface reconstructions transforms into the (2 ×1 ) structure at Ts=123 K. We identify the polar nature of the TlNi2Se2 (001) surface as the most probable driving mechanism of the two reconstructions, as both lead to a charge density ρ =0.5 e- , thereby avoiding divergent electrostatic potentials and the resulting "polar catastrophe." Low-temperature scanning tunneling spectroscopy (STS) performed with normal metal and superconducting probe tips shows a superconducting gap which is best fit with an isotropic s wave. We could not detect any correlation between the local surface reconstruction, suggesting that the superconductivity is predominantly governed by TlNi2Se2 bulk properties. Correspondingly, temperature- and field-dependent data reveal that both the critical temperature and critical magnetic field are in good agreement with bulk values obtained earlier from transport measurements. In the superconducting state the formation of an Abrikosov lattice is observed without any zero bias anomaly at the vortex core.

Selective Growth of Metallic and Semiconducting Single Walled Carbon Nanotubes on Textured Silicon.

PubMed

Jang, Mira; Lee, Jongtaek; Park, Teahee; Lee, Junyoung; Yang, Jonghee; Yi, Whikun

2016-03-01

We fabricated the etched Si substrate having the pyramidal pattern size from 0.5 to 4.2 μm by changing the texturing process parameters, i.e., KOH concentration, etching time, and temperature. Single walled carbon nanotubes (SWNTs) were then synthesized on the etched Si substrates with different pyramidal pattern by chemical vapor deposition. We investigated the optical and electronic properties of SWNT film grown on the etched Si substrates of different morphology by using scanning electron microscopy, Raman spectroscopy and conducting probe atomic force microscopy. We confirmed that the morphology of substrate strongly affected the selective growth of the SWNT film. Semiconducting SWNTs were formed on larger pyramidal sized Si wafer with higher ratio compared with SWNTs on smaller pyramidal sized Si.

To study the effect of doping concentration of silver on structural and optical properties of cadmium oxide (CdO) nanostructure

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kumar, Rajesh, E-mail: rkkaushik06@gmail.com; Dept. of Physics, Vaish College of Engineering, Rohtak-124001, Haryana; Sharma, Ashwani

The present work deals with study of structural and optical properties of Silver (Ag) doped Cadmium oxide (CdO) nanostructured synthesized by Chemical Co-precipitation Techniques followed by calcinations at small temperature. The doping concentrations were changing from 0.1 to 10 at% respectively. Structural analysis study of these calcined materials is carried out by X-ray diffraction (XRD), Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM). The optical properties of calcined samples were investigating by Fourier transformation infrared (FTIR)spectroscopy, UV-Visible Spectroscopy (UV-Vis). The structural properties analysis results revels that crystallite size are in the range of nano region and TEM results aremore » quite in accordance with XRD results.« less

Synthesis and photocatalytic properties of TiO{sub 2} nanostructures

DOE Office of Scientific and Technical Information (OSTI.GOV)

Xia, X.H.; Liang, Y.; Wang, Z.

2008-08-04

TiO{sub 2} particles, rods, flowers and sheets were prepared by hydrothermal method via adjusting the temperature, the pressure and the concentration of TiCl{sub 4}. The as-prepared TiO{sub 2} powders were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), UV-vis diffuse reflectance spectra and N{sub 2} adsorption-desorption measurements. It was found that pressure is the most important factor influencing the morphology of TiO{sub 2}. The photocatalytic activity of the products was evaluated by the photodegradation of aqueous brilliant red X-3B solution under UV light. Among the as-prepared nanostructures, the flower-like TiO{sub 2}more » exhibited the highest photocatalytic activity.« less

Synthesis of silver nanoparticles using reducing agents obtained from natural sources (Rumex hymenosepalus extracts)

PubMed Central

2013-01-01

We have synthesized silver nanoparticles from silver nitrate solutions using extracts of Rumex hymenosepalus, a plant widely found in a large region in North America, as reducing agent. This plant is known to be rich in antioxidant molecules which we use as reducing agents. Silver nanoparticles grow in a single-step method, at room temperature, and with no addition of external energy. The nanoparticles have been characterized by ultraviolet-visible spectroscopy and transmission electron microscopy, as a function of the ratio of silver ions to reducing agent molecules. The nanoparticle diameters are in the range of 2 to 40 nm. High-resolution transmission electron microscopy and fast Fourier transform analysis show that two kinds of crystal structures are obtained: face-centered cubic and hexagonal. PMID:23841946

Direct synthesis of few-layer graphene supported platinum nanocatalyst for methanol oxidation

NASA Astrophysics Data System (ADS)

Tan, Hong; Ma, Xiaohui; Sheng, Leimei; An, Kang; Yu, Liming; Zhao, Hongbin; Xu, Jiaqiang; Ren, Wei; Zhao, Xinluo

2014-11-01

High-crystalline few-layer graphene supported Pt nanoparticles have been synthesized by arc discharge evaporation of carbon electrodes containing Pt element. A high-temperature treatment under hydrogen atmosphere has been carried out to obtain a new type of Pt/graphene catalyst for methanol oxidation in direct methanol fuel cell. The morphology and structure characterizations of as-grown few-layer graphene supported Pt nanoparticles and Pt/graphene catalysts have been studied by Raman spectroscopy, scanning electron microscopy with energy-dispersive spectroscopy, and high-resolution transmission electron microscopy. Cyclic voltammograms and chronoamperometric curves show that our present Pt/graphene catalysts have larger current density for methanol oxidation, higher tolerance to carbon monoxide poisoning, and better stability during the operating procedure, compared to commercial Pt/C catalysts.

Atmospheric pressure chemical vapor deposition: an alternative route to large-scale MoS2 and WS2 inorganic fullerene-like nanostructures and nanoflowers.

PubMed

Li, Xiao-Lin; Ge, Jian-Ping; Li, Ya-Dong

2004-11-19

Large-scale MoS2 and WS2 inorganic fullerene-like (IF) nanostructures (onionlike nanoparticles, nanotubes) and elegant three-dimensional nanoflowers (NF) have been selectively prepared through an atmospheric pressure chemical vapor deposition (APCVD) process with the reaction of chlorides and sulfur. The morphologies were controlled by adjusting the deposition position, the deposition temperature, and the flux of the carrier gas. All of the nanostructures have been characterized by X-ray powder diffraction (XRD), transmission electron microscopy (TEM), and scanning electron microscopy (SEM). A reaction mechanism is proposed based on the experimental results. The surface area of MoS2 IF nanoparticles and the field-emission effect of as-prepared WS2 nanoflowers is reported.

Nanotubes, nanobelts, nanowires, and nanorods of silicon carbide from the wheat husks

DOE Office of Scientific and Technical Information (OSTI.GOV)

Qadri, S. B.; Rath, B. B.; Gorzkowski, E. P.

2015-09-14

Nanotubes, nanowires, nanobelts, and nanorods of SiC were synthesized from the thermal treatment of wheat husks at temperatures in excess of 1450 °C. From the analysis based on x-ray diffraction, Raman spectroscopy, scanning electron microscopy, and transmission electron microscopy, it has been found that the processed samples of wheat husk consisted of 2H and 3C polytypes of SiC exhibiting the nanostructure shapes. These nanostructures of silicon carbide formed from wheat husks are of technological importance for designing advance composites, applications in biotechnology, and electro-optics. The thermodynamics of the formation of SiC is discussed in terms of the rapid solid state reactionmore » between hydrocarbons and silica on the molecular scale, which is inherently present in the wheat husks.« less

Nanotubes, nanobelts, nanowires, and nanorods of silicon carbide from the wheat husks

NASA Astrophysics Data System (ADS)

Qadri, S. B.; Rath, B. B.; Gorzkowski, E. P.; Feng, J.; Qadri, S. N.; Caldwell, J. D.

2015-09-01

Nanotubes, nanowires, nanobelts, and nanorods of SiC were synthesized from the thermal treatment of wheat husks at temperatures in excess of 1450 °C. From the analysis based on x-ray diffraction, Raman spectroscopy, scanning electron microscopy, and transmission electron microscopy, it has been found that the processed samples of wheat husk consisted of 2H and 3C polytypes of SiC exhibiting the nanostructure shapes. These nanostructures of silicon carbide formed from wheat husks are of technological importance for designing advance composites, applications in biotechnology, and electro-optics. The thermodynamics of the formation of SiC is discussed in terms of the rapid solid state reaction between hydrocarbons and silica on the molecular scale, which is inherently present in the wheat husks.

The Application of Electron Microscopy Techniques to the Space Shuttle Columbia Accident Investigation

NASA Technical Reports Server (NTRS)

Shah, Sandeep; Jerman, Greg

2005-01-01

The Space Shuttle Columbia was returning from a 16-day research mission, STS- 107, with nominal system performance prior to the beginning of the entry interface into earth's upper atmosphere. Approximately one minute and twenty four seconds into the peak heating region of the entry interface, an off-nominal temperature rise was observed in the left main landing gear brake line. Nearly seven minutes later, all contact was lost with Columbia. Debris was observed periodically exiting the Shuttle's flight path throughout the reentry profile over California, Nevada, and New Mexico, until its final breakup over Texas. During the subsequent investigation, electron microscopy techniques were crucial in revealing the location of the fatal damage that resulted in the loss of Columbia and her crew.

Antibacterial Activity of Electrochemically Synthesized Colloidal Silver Nanoparticles Against Hospital-Acquired Infections

NASA Astrophysics Data System (ADS)

Thuc, Dao Tri; Huy, Tran Quang; Hoang, Luc Huy; Hoang, Tran Huy; Le, Anh-Tuan; Anh, Dang Duc

2017-06-01

This study evaluated the antibacterial activity of electrochemically synthesized colloidal silver nanoparticles (AgNPs) against hospital-acquired infections. Colloidal AgNPs were synthesized via a single process using bulk silver bars, bi-distilled water, trisodium citrate, and direct current voltage at room temperature. Colloidal AgNPs were characterized by transmission electron microscopy, field-emission scanning electron microscopy, and energy-dispersive x-ray analyses. The antibacterial activity of colloidal AgNPs against four bacterial strains isolated from clinical samples, including methicillin-resistant Staphylococcus aureus, Escherichia coli O157:H7, multidrug-resistant Pseudomonas aeruginosa, and carbapenem-resistant Klebsiella pneumonia, was evaluated by disc diffusion, minimum inhibitory concentration (MIC), and ultrathin sectioning electron microscopy. The results showed that the prepared AgNPs were 19.7 ± 4.3 nm in size, quasi-spherical, and of high purity. Zones of inhibition approximately 6-10 mm in diameter were found, corresponding to AgNPs concentrations of 50 μg/mL to 100 μg/mL. The MIC results revealed that the antibacterial activity of the prepared AgNPs was strongly dependent on the concentration and strain of the tested bacteria.

Automated 100-Position Specimen Loader and Image Acquisition System for Transmission Electron Microscopy

PubMed Central

Lefman, Jonathan; Morrison, Robert; Subramaniam, Sriram

2007-01-01

We report the development of a novel, multi-specimen imaging system for high-throughput transmission electron microscopy. Our cartridge-based loading system, called the “Gatling”, permits the sequential examination of as many as 100 specimens in the microscope for room temperature electron microscopy using mechanisms for rapid and automated specimen exchange. The software for the operation of the Gatling and automated data acquisition has been implemented in an updated version of our in-house program AutoEM. In the current implementation of the system, the time required to deliver 95 specimens into the microscope and collect overview images from each is about 13 hours. Regions of interest are identified from a low magnification atlas generation from each specimen and an unlimited number of higher magnifications images can be subsequently acquired from these regions using fully automated data acquisition procedures that can be controlled from a remote interface. We anticipate that the availability of the Gatling will greatly accelerate the speed of data acquisition for a variety of applications in biology, materials science and nanotechnology that require rapid screening and image analysis of multiple specimens. PMID:17240161

The effect of reaction temperature on the room temperature ferromagnetic property of sol-gel derived tin oxide nanocrystal

NASA Astrophysics Data System (ADS)

Sakthiraj, K.; Hema, M.; Balachandra Kumar, K.

2018-06-01

In the present study, nanocrystalline tin oxide materials were prepared using sol-gel method with different reaction temperatures (25 °C, 50 °C, 75 °C & 90 °C) and the relation between the room temperature ferromagnetic property of the sample with processing temperature has been analysed. The X-ray diffraction pattern and infrared absorption spectra of the as-prepared samples confirm the purity of the samples. Transmission electron microscopy images visualize the particle size variation with respect to reaction temperature. The photoluminescence spectra of the samples demonstrate that luminescence process in materials is originated due to the electron transition mediated by defect centres. The room temperature ferromagnetic property is observed in all the samples with different amount, which was confirmed using vibrating sample magnetometer measurements. The saturation magnetization value of the as-prepared samples is increased with increasing the reaction temperature. From the photoluminescence & magnetic measurements we accomplished that, more amount of surface defects like oxygen vacancy and tin interstitial are created due to the increase in reaction temperature and it controls the ferromagnetic property of the samples.

Spectroellipsometric studies of sol-gel derived Sr0.6Ba0.4Nb2O6 films

NASA Astrophysics Data System (ADS)

Ho, Melanie M. T.; Tang, T. B.; Mak, C. L.; Pang, G. K. H.; Chan, K. Y.; Wong, K. H.

2006-10-01

Sr0.6Ba0.4Nb2O6 (SBN) films have been fabricated on (001)Si substrates by a sol-gel technique. The annealing process was carried out in air at various temperatures ranging from 200to700°C. Studies using x-ray diffractometry, high resolution transmission electron microscopy, and scanning electron microscopy showed that polycrystalline films, with a grain size of about 100nm, were obtained only for annealing temperatures ⩾600°C. The optical properties of these sol-gel derived SBN films were studied by spectroscopic ellipsometry (SE). In the analysis of the measured SE spectra, a triple-layer Lorentz model has been developed and used to deduce the optical properties of the SBN films. Our systematic SE measurements revealed that the refractive indices of the SBN films increase with the annealing temperature. This increase is more pronounced at around the crystallization temperature, i.e., between 500 and 600°C. The extinction coefficients of the films also exhibit a similar trend, showing a zero value for amorphous films and larger values for films annealed at above 600°C. Our results demonstrate that while crystallization helps to raise the refractive index of the film due to film densification, it also promotes scattering by grain boundary, resulting in a larger extinction coefficient.

Dielectric properties of (CuO, CaO2, and BaO)y/CuTl-1223 composites

NASA Astrophysics Data System (ADS)

Mumtaz, M.; Kamran, M.; Nadeem, K.; Jabbar, Abdul; Khan, Nawazish A.; Saleem, Abida; Tajammul Hussain, S.; Kamran, M.

2013-07-01

We synthesized (CuO, CaO2, and BaO)y/Cu0.5Tl0.5Ba2Ca2Cu3O10-δ (y = 0, 5%, 10%, 15%) composites by solid-state reaction and characterized them by x-ray diffraction, scanning electron microscopy, dc-resistivity, and Fourier transform infrared spectroscopy. Frequency and temperature dependent dielectric properties, such as real and imaginary parts of the dielectric constant, dielectric loss, and ac-conductivity of these composites were studied by capacitance and conductance measurements as a function of frequency (10 kHz to 10 MHz) and temperature (78 to 300 K). X-ray diffraction analysis reveals that the characteristic behavior of the superconductor phase and the structure of Cu0.5Tl0.5Ba2Ca2Cu3O10-δ are nearly undisturbed by doping with nanoparticles. Scanning electron microscopy images show the improvement in the intergranular linking between the superconducting grains occurring with increasing nanoparticle concentration. Microcracks are healed up with these nanoparticles, and superconducting volume fraction is also increased. Dielectric properties of these composites strongly depend on the frequency and temperature. Zero resistivity critical temperature and dielectric properties show opposite trends with the addition of nanoparticles to the Cu0.5Tl0.5Ba2Ca2Cu3O10-δ superconductor matrix.

Low temperature neutron irradiation effects on microstructure and tensile properties of molybdenum

DOE Office of Scientific and Technical Information (OSTI.GOV)

Li, Meimei; Eldrup, M.; Byun, Thak Sang

2008-01-01

Polycrystalline molybdenum was irradiated in the hydraulic tube facility at the High Flux Isotope Reactor to doses ranging from 7.2 x 10{sup -5} to 0.28 dpa at {approx} 80 C. As-irradiated microstructure was characterized by room-temperature electrical resistivity measurements, transmission electron microscopy (TEM) and positron annihilation spectroscopy (PAS). Tensile tests were carried out between -50 and 100 C over the strain rate range 1 x 10{sup -5} to 1 x 10{sup -2} s{sup -1}. Fractography was performed by scanning electron microscopy (SEM), and the deformation microstructure was examined by TEM after tensile testing. Irradiation-induced defects became visible by TEM atmore » {approx}0.001 dpa. Both their density and mean size increased with increasing dose. Submicroscopic three-dimensional cavities were detected by PAS even at {approx}0.0001 dpa. The cavity density increased with increasing dose, while their mean size and size distribution was relatively insensitive to neutron dose. It is suggested that the formation of visible dislocation loops was predominantly a nucleation and growth process, while in-cascade vacancy clustering may be significant in Mo. Neutron irradiation reduced the temperature and strain rate dependence of the yield stress, leading to radiation softening in Mo at lower doses. Irradiation had practically no influence on the magnitude and the temperature and strain rate dependence of the plastic instability stress.« less

Co- and Ce/Co-coated ferritic stainless steel as interconnect material for Intermediate Temperature Solid Oxide Fuel Cells

NASA Astrophysics Data System (ADS)

Falk-Windisch, Hannes; Claquesin, Julien; Sattari, Mohammad; Svensson, Jan-Erik; Froitzheim, Jan

2017-03-01

Chromium species volatilization, oxide scale growth, and electrical scale resistance were studied at 650 and 750 °C for thin metallic Co- and Ce/Co-coated steels intended to be utilized as the interconnect material in Intermediate Temperature Solid Oxide Fuel Cells (IT-SOFC). Mass gain was recorded to follow oxidation kinetics, chromium evaporation was measured using the denuder technique and Area Specific Resistance (ASR) measurements were carried out on 500 h pre-exposed samples. The microstructure of thermally grown oxide scales was characterized using Scanning Electron Microscopy (SEM), Scanning Transmission Electron Microscopy (STEM), and Energy Dispersive X-Ray Analysis (EDX). The findings of this study show that a decrease in temperature not only leads to thinner oxide scales and less Cr vaporization but also to a significant change in the chemical composition of the oxide scale. Very low ASR values (below 10 mΩ cm2) were measured for both Co- and Ce/Co-coated steel at 650 and 750 °C, indicating that the observed change in the chemical composition of the Co spinel does not have any noticeable influence on the ASR. Instead it is suggested that the Cr2O3 scale is expected to be the main contributor to the ASR, even at temperatures as low as 650 °C.

Investigation of temperature, catalyst thickness and substrate effects in In2O3 nanostructures

NASA Astrophysics Data System (ADS)

Tuzluca, Fatma Nur; Yesilbag, Yasar Ozkan; Ertugrul, Mehmet

2017-12-01

This study successfully synthesized In2O3 nanotowers (NTs), nanowires (NWs), nanochains (NChs) and nanocrystals (NCs) on n-type Si(100) and quartz substrates at temperature of 900-1000 °C by using Au catalysts via the Chemical Vapor Deposition (CVD) technique. The analyses of experimental results revealed that In2O3 nanostructures (NSs) grew in different morphologies due to variable parameters, such as temperature, thickness of catalyst and substrate type. This was because these In2O3 NSs were formed by both the Vapor-Liquid-Solid (VLS) and the Vapor-Solid (VS) growth mechanisms. For instance, In2O3 NTs and NChs were formed by the VLS growth mechanism; In2O3 NCs were formed by the VS growth mechanism and In2O3 NWs were formed by both the VLS and VS growth mechanisms. Morphology and crystal structures were identified through X-Ray Diffraction (XRD), High Resolution Transmission Electron Microscopy (HRTEM), Field Emission Scanning Electron Microscopy (FESEM) and Energy Dispersive X-Ray Spectroscopy (EDS). Moreover, photoluminescence (PL) peaks of In2O3 NSs were measured to be 367 nm, 470 nm, and 630 nm at room temperature (RT). These measurement results indicated that structural, morphological, compositional and optical properties of synthesized In2O3 NSs correlated with growth parameters.

Cu assisted stabilization and nucleation of L1 2 precipitates in Al 0.3 CuFeCrNi 2 fcc-based high entropy alloy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gwalani, B.; Choudhuri, D.; Soni, V.

2017-05-01

A detailed investigation of precipitation of the ordered L12 (γ’) phase in a Al0.3CrCuFeNi2 high entropy alloy (HEA), more generally referred to as a complex concentrated alloy (CCA), reveals the role of copper (Cu) on stabilization and precipitation of the ordered L12 ( γ’) phase. Detailed characterization via coupling of scanning and transmission electron microscopy, and atom probe tomography revealed novel insights into Cu clustering within the face-centered cubic matrix of this HEA, leading to heterogeneous nucleation sites for the γ’ precipitates. The subsequent partitioning of Cu into the γ’ precipitates indicates their stabilization is due to Cu addition. Themore » γ’ order-disorder transition temperature was determined to be ~930 _C in this alloy, based on synchrotron diffraction experiments, involving in situ annealing. The growth and high temperature stability of the γ’ precipitates was also confirmed via systematic scanning electron microscopy investigations of samples annealed at temperatures in the range of 700-900 oC. The role of Cu revealed by this study can be employed in the design of precipitation strengthened HEAs, as well as in a more general sense applied to other types of superalloys, with the objective of potentially enhancing their mechanical properties at room and elevated temperatures« less

Synthesis and characterization of InNbO₄ nanopowder for gas sensors.

PubMed

Balamurugan, C; Vijayakumar, E; Subramania, A

2012-01-15

Indium niobate (InNbO(4)) nanopowder was prepared by a comparatively low temperature niobium citrate complex process. The prepared InNbO(4) was characterized by thermal analysis, X-ray diffraction analysis (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive X-ray spectroscopy, diffuse reflectance spectroscopy (DRS), and impedance studies. It revealed that the well crystalline monoclinic InNbO(4) nanopowder was obtained at the calcination temperature of 600°C. The average particle diameter was 22nm. The optical band gap was found to be 2.66eV. The temperature dependent conductivity obeyed Arrhenius relation. The activation energy of the conductivity process was calculated to be 0.43eV. The gas sensing behaviour of the prepared InNbO(4) was studied by measuring the change in resistance of the sensor material as a function of various concentrations of the test gases such as liquid petroleum gas (LPG), ammonia (NH(3)) and ethanol (C(2)H(5)OH) at their optimized operating temperature. InNbO(4) had a better sensitivity to LPG (0.97) and NH(3) (0.70) gas than ethanol (0.46). The sensor responses of InNbO(4) as a function of gas concentrations and with recovery time were also studied in detail. Copyright © 2011 Elsevier B.V. All rights reserved.

TEM preparation methods and influence of radiation damage on the beam sensitive CaCO3 shell of Emiliania huxleyi.

PubMed

Hoffmann, Ramona; Wochnik, Angela S; Betzler, Sophia B; Matich, Sonja; Griesshaber, Erika; Schmahl, Wolfgang W; Scheu, Christina

2014-07-01

The ultrastructure of biologically formed calcium carbonate crystals like the shell of Emiliania huxleyi depends on the environmental conditions such as pH value, temperature and salinity. Therefore, they can be used as indicator for climate changes. However, for this a detailed understanding of their crystal structure and chemical composition is required. High resolution methods like transmission electron microscopy can provide those information on the nanoscale, given that sufficiently thin samples can be prepared. In our study, we developed sample preparation techniques for cross-section and plan-view investigations and studied the sample stability under electron bombardment. In addition to the biological material (Emiliania huxleyi) we also prepared mineralogical samples (Iceland spar) for comparison. High resolution transmission electron microscopy imaging, electron diffraction and electron energy-loss spectroscopy studies revealed that all prepared samples are relatively stable under electron bombardment at an acceleration voltage of 300 kV when using a parallel illumination. Above an accumulated dose of ∼10(5) e/nm2 the material--independent whether its origin is biological or geological--transformed to poly-crystalline calcium oxide. Copyright © 2014 Elsevier Ltd. All rights reserved.

Catalysts based on PdO_ZrO2 in the hydrodechlorination reaction of chlorobenzene

NASA Astrophysics Data System (ADS)

Otroshchenko, T. P.; Turakulova, A. O.; Lokteva, E. S.; Golubina, E. V.; Lunin, V. V.

2015-07-01

The possibility of using mixed oxides of palladium and zirconium obtained with biotemplates (cellulose and wood pulp) as the precursor of catalysts for the hydrodechlorination of chlorobenzene is analyzed. The properties of the samples are studied by means of scanning electron microscopy (SEM), transmission electron microscopy (TEM), the Brunauer-Emmet-Teller (BET) method, and temperature-programmed reduction (TPR). They are then compared to the properties of a supported analogue. The biomorphic precursors are characterized by high porosity and include micropores, mesopores, and macropores; the results from TPR reveal the presence in the precursors of several forms of PdO that differ by reduction temperature. It is shown that the distribution of palladium in the catalysts obtained by reducing the precursors with hydrogen depends on the method used in synthesizing the precursor. It is shown that the studied catalysts ensure 100% conversion of chlorobenzene at temperatures of 100 to 250°C. It is established that cyclohexane is the principal product in the presence of the supported catalyst across the range of temperatures, while cyclohexane and benzene are detected among the products in the presence of biomorphous samples at temperatures above 130°C. The effect the presence of an admixture of alkaline and alkaline-earth metals in the catalyst has on the selectivity of the process is noted. It is established that the catalysts operate in a stable manner for at least 27 h of use under experimental conditions.

Studies of silicon quantum dots prepared at different substrate temperatures

NASA Astrophysics Data System (ADS)

Al-Agel, Faisal A.; Suleiman, Jamal; Khan, Shamshad A.

2017-03-01

In this research work, we have synthesized silicon quantum dots at different substrate temperatures 193, 153 and 123 K at a fixed working pressure 5 Torr. of Argon gas. The structural studies of these silicon quantum dots have been undertaken using X-ray diffraction, Field Emission Scanning Electron Microscopy (FESEM) and High Resolution Transmission Electron Microscopy (HRTEM). The optical and electrical properties have been studied using UV-visible spectroscopy, Fourier transform infrared (FTIR) spectroscopy, Fluorescence spectroscopy and I-V measurement system. X-ray diffraction pattern of Si quantum dots prepared at different temperatures show the amorphous nature except for the quantum dots synthesized at 193 K which shows polycrystalline nature. FESEM images of samples suggest that the size of quantum dots varies from 2 to 8 nm. On the basis of UV-visible spectroscopy measurements, a direct band gap has been observed for Si quantum dots. FTIR spectra suggest that as-grown Si quantum dots are partially oxidized which is due exposure of as-prepared samples to air after taking out from the chamber. PL spectra of the synthesized silicon quantum dots show an intense peak at 444 nm, which may be attributed to the formation of Si quantum dots. Temperature dependence of dc conductivity suggests that the dc conductivity enhances exponentially by raising the temperature. On the basis above properties i.e. direct band gap, high absorption coefficient and high conductivity, these silicon quantum dots will be useful for the fabrication of solar cells.

Room-temperature CO Thermoelectric Gas Sensor based on Au/Co3O4 Catalyst Tablet.

PubMed

Sun, L; Luan, W L; Wang, T C; Su, W X; Zhang, L X

2017-02-17

A carbon monoxide (CO) thermoelectric (TE) gas sensor was fabricated by affixing a Au/Co 3 O 4 catalyst tablet on a TE film layer. The Au/Co 3 O 4 catalyst tablet was prepared by a co-precipitation and tablet compression method and its possible catalytic mechanism was discussed by means of x-ray diffraction, field emission scanning electron microscopy, high resolution transmission electron microscopy, x-ray photoelectron spectroscopy, temperature-programmed reduction of hydrogen, Fourier transform infrared spectroscopy and Brunauer-Emmett-Teller analysis. The optimal catalyst, with a Au content of 10 wt%, was obtained at a calcination temperature between 200 and 300 °C. The small size of the Au nanoparticles, high specific surface, the existence of Co 3+ and water-derived species contributed to  high catalytic activity. Based on the optimal Au/Co 3 O 4 catalyst tablet, the CO TE gas sensor worked at room temperature and showed a response voltage signal (ΔV) of 23 mV, high selectivity among hydrogen and methane, high stability, and a fast response time of 106 s for 30 000 ppm CO/air. In addition, a CO concentration in the range of 5000-30 000 ppm could obviously be detected and exhibited a linear relationship with ΔV. The CO TE gas sensor provides a promising option for the detection of CO gas at room temperature.

Parametric Study on the Tensile Properties of Ni-Based Alloy for a VHTR

NASA Astrophysics Data System (ADS)

Kim, Dong-Jin; Jung, Su Jin; Mun, Byung Hak; Kim, Sung Woo; Lim, Yun Soo

2015-01-01

A very high-temperature reactor (VHTR) has been studied among generation IV nuclear power plants owing to its many advantages such as high-electric efficiency and massive hydrogen production. The material used for the heat exchanger should sustain structural integrity for its life even though the material is exposed to a harsh environment at 1223 K (950 °C) in an impure helium coolant. Therefore, an enhancement of the material performance at high temperature gives a margin in determining the operating temperature and life time. This work is an effort to find an optimum combination of alloying elements and processing parameters to improve the material performance. The tensile property and microstructure for nickel-based alloys fabricated in a laboratory were evaluated as a function of the heat treatment, cold working, and grain boundary strengthener using a tension test at 1223 K (950 °C), scanning electron microscopy, and transmission electron microscopy. Elongation to rupture was increased by additional heat treatment and cold working, followed by additional heat treatment in the temperature range from 1293 K to 1383 K (1020 °C to 1110 °C) implying that the intergranular carbide contributes to grain boundary strengthening. The temperature at which the grain boundary is improved by carbide decoration was higher for a cold-worked specimen, which was described by the difference in carbide stability and carbide formation kinetics between no cold-worked and cold-worked specimens. Zr and Hf played a scavenging effect of harmful elements causing an increase in ductility.

Effect of annealing on Curie temperature and phase transition in La{sub 0.55}Sr{sub 0.08}Mn{sub 0.37}O{sub 3} epitaxial films grown on SrTiO{sub 3} (100) substrates by reactive radio frequency magnetron sputtering

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ichinose, T.

2016-08-15

Mn-poor LaSrMnO{sub 3} (LSMO) epitaxial films were grown on SrTiO{sub 3} (100) substrates by radio frequency magnetron sputtering in an argon and oxygen gas mix, and then the samples were annealed in air at various temperatures (T{sub a}). 2 theta-chi X-ray diffraction mapping, nano-beam diffraction analysis through transmission electron microscopy, and electron back scatter diffraction through scanning electron microscopy revealed that the crystal symmetry of the LSMO films changed from monoclinic/orthorhombic to rhombohedral on annealing in air. Curie temperature (T{sub C}) of the LSMO films was found to increase with increasing T{sub a}, and become higher than the room temperaturemore » at T{sub a} ≥ 861 °C, indicating that the cause of these changes was the filling of oxygen and the transition of the crystal symmetry into rhombohedral. - Highlights: •Mn-poor LSMO changed from monoclinic/orthorhombic to rhombohedral by oxygen supply. •Mn-poor LSMO was increased T{sub C} by changed crystal symmetry, and it showed T{sub C} above RT. •Annealed in air effectively supplied O{sub 2} more than O{sub 2} gas during sputtering •EBSD is useful to evaluate crystal symmetry of complex oxide film from the substrate.« less

Pronounced pre-martensitic anomaly in the magnetization on Ni2MnGa thin films

NASA Astrophysics Data System (ADS)

Neckel, I. T.; Müller, C.; Nobrega, K. Z.; Dartora, C. A.; Schreiner, W. H.; Mosca, D. H.

2018-05-01

We have prepared [110]-textured Ni2MnGa thin films exhibiting an unusual pre-martensitic transition accompanied by an extremely large magnetization change. The thin films were grown by molecular beam epitaxy directly on epi-ready GaAs(111)B. Crystalline structure was investigated in situ by reflection high-energy electron diffraction (RHEED) and ex situ by x-ray diffraction (XRD) and transmission electron microscopy (TEM). The results show that the film exhibits cubic crystalline structure (L2 1) at room temperature with lattice parameter a = 5.88 Å which undergoes martensitic transition. Magnetic characterization shows ferromagnetic behavior at room temperature with Curie temperature higher than room temperature. Martensitic transformation occurs at TM ∼ 185 K. A phenomenological model based on Landau theory of phase transformation was developed to explain the anomalous pre-martensitic transition at ∼285 K.

Low Temperature Synthesis of Cobalt-Chromium Carbide Nanoparticles-Doped Carbon Nanofibers.

PubMed

Yousef, Ayman; Brooks, Robert M; Abutaleb, Ahmed; Al-Deyab, Salem S; El-Newehy, Mohamed H

2018-04-01

Electrospinning has been used to synthesize cobalt-chromium carbide nanoparticles (NPs)-doped carbon nanofibers (CNFs) (Composite). Electrospun mat comprising of cobalt acetate, chromium acetate and poly(vinyl alcohol) (PVA) has been carbonized at low temperature (850 °C) for 3 h under argon atmosphere to produce the introduced composite. The process was achieved at low temperature due to the presence of cobalt as an activator. Field emission scanning electron microscope (FE-SEM), X-ray diffractometry (XRD), and transmission electron microscopy (TEM) equipped with EDX techniques were used to determine the products characteristics. The results indicated the formation of pure cobalt (Co), Cr7C3 NPs and crystalline CNFs. The Co and Cr7C3 NPs were covered with CNFs. Overall, the proposed NFs open new avenue to prepare different metals-metal carbides-carbon NFs at low temperature and short reaction time.

Antibacterial characteristics of thermal plasma spray system.

PubMed

Goudarzi, M; Saviz, Sh; Ghoranneviss, M; Salar Elahi, A

2018-03-15

The objective of this study is to investigate antibacterial characteristics of a thermal plasma spray system. For this purpose, copper powder was coated on a handmade atmospheric plasma spraying system made by the stainless steel 316 substrate, which is preheated at different temperatures before spraying. A number of deposition characteristics such as antibacterial characteristics, adhesion strength and hardness of coating, was investigated. All of the spray parameters are fixed except the substrate temperature. The chemical composition was analyzed by X-ray diffraction (XRD). A scanning electron microscopy (SEM) and back scattering electron microscopy (BSE) were used to show the coating microstructure, its thickness and also the powder micrograph. The energy dispersive X-ray spectroscopy (EDX) was used to analyze the coating particles. Hardness of the deposition was examined by Vickers tester (HV0.1). Its adhesion strength was declared by cross cut tester (TQC). In addition, the percentage of bactericidal coating was evidenced with Staphylococcus aurous and Escherichia coli bacteria. Study results show that as the substrates temperature increases, the number of splats in the shape of pancake increases, the greatness and percentage of the deposition porosity both decrease. The increment of the substrate temperature leads to more oxidation and makes thicker dendrites on the splat. The enhancement of the substrate temperature also enlarges thickness and efficiency of coating. The interesting results are that antibacterial properties of coatings against the Escherichia coli are more than Staphylococcus aurous bacteria. However the bactericidal percentage of the coatings against Staphylococcus aurous and Escherichia coli bacteria roughly does not change with increasing the substrate temperature. Furthermore, by increment of the substrate temperature, coatings with both high adhesion and hardness are obtained. Accordingly, the temperature of substrate can be an important parameter for progressing mechanical properties of the antiseptic deposition.

Fire Events and Soil Thermometry: The Applications of Clay Chemistry for Tracing Temperature Changes in Soils and Sediments Below Surface Fires

NASA Astrophysics Data System (ADS)

Watson, E.; Werts, S. P.; Gelabert, M.

2016-12-01

Fires in the natural environment affect the physical, chemical, and biological properties of soils. However, fires may also alter the mineralogy of the geologic material in which it comes in contact. Previous experiments on high temperature alteration of clays indicate that dehydration, oxidation, and hydroxylation in clay minerals can occur progressively in that order at increasing temperatures up to 500°C. It is also well known that wildfire events can heat soils to these temperature ranges several centimeters deep. In this experiment, alterations in clay chemistry were used as a tool to investigate fire intensity along with the changing morphology of clay minerals. For data collection, small camp fires were set in York County, SC and temperatures were recorded using a datalogger system to 5 cm deep during the fire event. Control samples were taken adjacent to the fires to compare the changing morphology of the minerals when heated. Powder x-ray diffraction and scanning electron microscopy were used to identify the clay mineralogy. The clay from soil samples was identified as hydrous kaolinite, anhydrous kaolinite, and varying types of goethite. To observe the dehydration, oxidation, and hydroxylation of clay minerals, scanning electron microscopy with emission dispersive spectroscopy was used to identify the O/cation ratios present, which would indicate changes in the oxidation state of the clay minerals. By mapping the changes in O/cation ratios with temperature in silicates, we are able to trace the temperature of the sediments during fire events. This research suggests it may be possible to utilize these geochemical trends to aid in soil and sediment temperature investigations in both archeological and modern soil and surface process investigations.

Synthesis of Nanocrystalline CaWO4 as Low-Temperature Co-fired Ceramic Material: Processing, Structural and Physical Properties

NASA Astrophysics Data System (ADS)

Vidya, S.; Solomon, Sam; Thomas, J. K.

2013-01-01

Nanocrystalline scheelite CaWO4, a promising material for low-temperature co-fired ceramic (LTCC) applications, has been successfully synthesized through a single-step autoignition combustion route. Structural analysis of the sample was performed by powder x-ray diffraction (XRD), Fourier-transform infrared spectroscopy, and Raman spectroscopy. The XRD analysis revealed that the as-prepared sample was single phase with scheelite tetragonal structure. The basic optical properties and optical constants of the CaWO4 nanopowder were studied using ultraviolet (UV)-visible absorption spectroscopy, which showed that the material was a wide-bandgap semiconductor with bandgap of 4.7 eV at room temperature. The sample showed poor transmittance in the ultraviolet region but maximum transmission in the visible/near-infrared regions. The photoluminescence spectra recorded at different temperatures showed intense emission in the green region. The particle size estimated from transmission electron microscopy was 23 nm. The feasibility of CaWO4 for LTCC applications was studied from its sintering behavior. The sample was sintered at a relatively low temperature of 810°C to high density, without using any sintering aid. The surface morphology of the sintered sample was analyzed by scanning electron microscopy. The dielectric constant and loss factor of the sample measured at 5 MHz were found to be 10.50 and 1.56 × 10-3 at room temperature. The temperature coefficient of the dielectric constant was -88.71 ppm/°C. The experimental results obtained in this work demonstrate the potential of nano-CaWO4 as a low-temperature co-fired ceramic as well as an excellent luminescent material.

Trachymolgus purpureus sp. nov., an armored snout mite (Acari: Bdellidae) from the Ozark highlands: morphology, development, and key to Trachymolgus Berlese

USDA-ARS?s Scientific Manuscript database

Trachymolgus purpureus Fisher & Dowling sp. nov. is described from the Ozark highlands of North America. A diversity of imaging techniques are used to illustrate the species including field emission low-temperature scanning electron microscopy (FE-LTSEM), stereomicrography, compound light micrograph...

Magnetic properties evolution of the CoxFe3-xO4/SiO2 system due to advanced thermal treatment at 700 °C and 1000 °C

NASA Astrophysics Data System (ADS)

Dippong, Thomas; Levei, Erika Andrea; Tanaselia, Claudiu; Gabor, Mihai; Nasui, Mircea; Barbu Tudoran, Lucian; Borodi, Gheorghe

2016-07-01

The CoxFe3-xO4 (x=0.5-2.5) system embedded in the silica matrix was synthesised by sol-gel method using cobalt nitrate, iron nitrate, 1.4-butanediol and tetraethyl orthosilicate. Five different Co/Fe molar ratios in the presence of diol and one without diol were used for the synthesis. The obtained gels were subjected to thermal treatment at 700 °C and 1000 °C. The oxide species formed in the silica matrix, the optimum temperature for the CoFe2O4 phase formation, the evolution of nanocrystallites size and magnetic properties with the calcination temperature were studied. The formed oxide species were studied using X-ray diffraction, Fourier transformed infrared spectrometry, the Co/Fe molar ratio was confirmed using inductively coupled plasma optical emission spectrometry, the nanocrystallites size, shape and clustering was identified by transmission electron microscopy and scanning electron microscopy, while the formation of magnetic phases was investigated by hysteresis and magnetization derivatives measurements.

A Comparative Study of Chemically and Biologically Synthesized MgO Nanomaterial for Liquefied Petroleum Gas Detection

NASA Astrophysics Data System (ADS)

Thirupathi, Rampelly; Solleti, Goutham; Sreekanth, Tirumala; Sadasivuni, Kishor Kumar; Venkateswara Rao, Kalagadda

2018-03-01

The exceptional chemical and physical properties of nanostructured materials are extremely suitable for designing new and enhanced sensing devices, particularly gas sensors and biosensors. The present work describes the synthesis of magnesium oxide (MgO) nanoparticles through two methods: a green synthesis using aloe vera plant extract and a chemical method using a glycine-based solution combustion route. In a single step, the extracted organic molecules from aloe vera plants were used to reduce metal ions by the green method. MgO nanoparticles were coated onto the interdigital electrode using the drop-drying method. The dynamic gas-sensing characteristics were measured for liquefied petroleum gas (LPG) at different concentrations and various temperatures. The MgO nanoparticles were characterized by using x-ray diffraction, field emission scanning electron microscopy, and high-resolution transmission electron microscopy to determine the size and structure of the particles. The product's functional properties were analyzed by Fourier transform-infrared spectroscopy and UV-visible spectroscopy. We found that the LPG sensing behavior of biologically synthesized MgO registers excellent sensitivity at various operating temperatures.

Microwave-assisted hydrothermal synthesis of marigold-like ZnIn2S4 microspheres and their visible light photocatalytic activity

NASA Astrophysics Data System (ADS)

Chen, Zhixin; Li, Danzhen; Xiao, Guangcan; He, Yunhui; Xu, Yi-Jun

2012-02-01

Marigold-like ZnIn2S4 microspheres were synthesized by a microwave-assisted hydrothermal method with the temperature ranging from 80 to 195 °C. X-ray diffraction, X-ray photoelectron spectroscopy, nitrogen sorption analysis, UV-visible spectroscopy, scanning electron microscopy and transmission electron microscopy were used to characterize the products. It was found that the crystallographic structure and optical property of the products synthesized at different temperatures were almost the same. The degradation of methyl orange (MO) under the visible light irradiation has been used as a probe reaction to investigate the photocatalytic activity of as-prepared ZnIn2S4, which shows that the ZnIn2S4 sample synthesized at 195 °C shows the best photocatalytic activity for MO degradation. In addition, the photocatalytic activities of all the samples prepared by the microwave-assisted hydrothermal method are better than those prepared by a normal hydrothermal method, which could be attributed to the formation of more defect sites during the microwave-assisted hydrothermal treatment.

A Comparative Study of Chemically and Biologically Synthesized MgO Nanomaterial for Liquefied Petroleum Gas Detection

NASA Astrophysics Data System (ADS)

Thirupathi, Rampelly; Solleti, Goutham; Sreekanth, Tirumala; Sadasivuni, Kishor Kumar; Venkateswara Rao, Kalagadda

2018-07-01

The exceptional chemical and physical properties of nanostructured materials are extremely suitable for designing new and enhanced sensing devices, particularly gas sensors and biosensors. The present work describes the synthesis of magnesium oxide (MgO) nanoparticles through two methods: a green synthesis using aloe vera plant extract and a chemical method using a glycine-based solution combustion route. In a single step, the extracted organic molecules from aloe vera plants were used to reduce metal ions by the green method. MgO nanoparticles were coated onto the interdigital electrode using the drop-drying method. The dynamic gas-sensing characteristics were measured for liquefied petroleum gas (LPG) at different concentrations and various temperatures. The MgO nanoparticles were characterized by using x-ray diffraction, field emission scanning electron microscopy, and high-resolution transmission electron microscopy to determine the size and structure of the particles. The product's functional properties were analyzed by Fourier transform-infrared spectroscopy and UV-visible spectroscopy. We found that the LPG sensing behavior of biologically synthesized MgO registers excellent sensitivity at various operating temperatures.

High-purity Cu nanocrystal synthesis by a dynamic decomposition method.

PubMed

Jian, Xian; Cao, Yu; Chen, Guozhang; Wang, Chao; Tang, Hui; Yin, Liangjun; Luan, Chunhong; Liang, Yinglin; Jiang, Jing; Wu, Sixin; Zeng, Qing; Wang, Fei; Zhang, Chengui

2014-12-01

Cu nanocrystals are applied extensively in several fields, particularly in the microelectron, sensor, and catalysis. The catalytic behavior of Cu nanocrystals depends mainly on the structure and particle size. In this work, formation of high-purity Cu nanocrystals is studied using a common chemical vapor deposition precursor of cupric tartrate. This process is investigated through a combined experimental and computational approach. The decomposition kinetics is researched via differential scanning calorimetry and thermogravimetric analysis using Flynn-Wall-Ozawa, Kissinger, and Starink methods. The growth was found to be influenced by the factors of reaction temperature, protective gas, and time. And microstructural and thermal characterizations were performed by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, and differential scanning calorimetry. Decomposition of cupric tartrate at different temperatures was simulated by density functional theory calculations under the generalized gradient approximation. High crystalline Cu nanocrystals without floccules were obtained from thermal decomposition of cupric tartrate at 271°C for 8 h under Ar. This general approach paves a way to controllable synthesis of Cu nanocrystals with high purity.

High-purity Cu nanocrystal synthesis by a dynamic decomposition method

NASA Astrophysics Data System (ADS)

Jian, Xian; Cao, Yu; Chen, Guozhang; Wang, Chao; Tang, Hui; Yin, Liangjun; Luan, Chunhong; Liang, Yinglin; Jiang, Jing; Wu, Sixin; Zeng, Qing; Wang, Fei; Zhang, Chengui

2014-12-01

Cu nanocrystals are applied extensively in several fields, particularly in the microelectron, sensor, and catalysis. The catalytic behavior of Cu nanocrystals depends mainly on the structure and particle size. In this work, formation of high-purity Cu nanocrystals is studied using a common chemical vapor deposition precursor of cupric tartrate. This process is investigated through a combined experimental and computational approach. The decomposition kinetics is researched via differential scanning calorimetry and thermogravimetric analysis using Flynn-Wall-Ozawa, Kissinger, and Starink methods. The growth was found to be influenced by the factors of reaction temperature, protective gas, and time. And microstructural and thermal characterizations were performed by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, and differential scanning calorimetry. Decomposition of cupric tartrate at different temperatures was simulated by density functional theory calculations under the generalized gradient approximation. High crystalline Cu nanocrystals without floccules were obtained from thermal decomposition of cupric tartrate at 271°C for 8 h under Ar. This general approach paves a way to controllable synthesis of Cu nanocrystals with high purity.

A study of early corrosion behaviors of FeCrAl alloys in liquid lead-bismuth eutectic environments

NASA Astrophysics Data System (ADS)

Lim, Jun; Nam, Hyo On; Hwang, Il Soon; Kim, Ji Hyun

2010-12-01

Lead and lead-bismuth eutectic (LBE) alloy have been increasingly receiving attention as heavy liquid metal coolants (HLMC) for future nuclear energy systems. The compatibility of structural materials and components with lead-bismuth eutectic liquid at high temperature is one of key issues for the commercialization of lead fast reactors. In the present study, the corrosion behaviors of iron-based alumina-forming alloys (Kanthal-AF®, PM2000, MA956) were investigated by exposing to stagnant LBE environments at 500 °C and 550 °C for up to 500 h. After exposures, the thickness and chemistry of the oxide layer on the specimens were analyzed by scanning electron microscopy, scanning transmission electron microscopy and energy dispersive X-ray spectroscopy. As a result, the oxide characteristics and the corrosion resistance were compared. In this study, it was shown that the corrosion resistance of FeCrAl ODS steels (PM2000, MA956) are superior to that of FeCrAl ferritic steel (Kanthal-AF®) in higher temperature LBE.