Effects of alcohol solvents on anatase TiO2 nanocrystals prepared by microwave-assisted solvothermal method

NASA Astrophysics Data System (ADS)

Wu, Yu-Chun; Tai, Yu-Chuen

2013-06-01

The effects of solvents on the anatase crystallite size prepared by sol-gel microwave-assisted solvothermal method were investigated in this study. Eight different alcohol solvents classified into two groups, i.e. primary and secondary/ternary alcohols, were used as reaction media and the effects of solvent properties, such as dielectric constant, boiling point, and internal pressure during the solvothermal process, on the crystallite size and shape were analyzed. According to the experimental results, selecting the solvent type allowed not only the alteration of the crystallite size but also the crystallite shape without the need of any additives. The boiling point of solvent was determined as the major factor influencing the crystallite size. Among the solvents with similar boiling points, the solvent with a higher carbon number produced the smaller crystallite size because of steric hindrance effect. In addition, the carboxyl groups dissociated from the alcohol solvent can play a role as a structural capping agent to retard the anatase crystal growth along the [001] direction and led to a rectangular crystallite shape with preferred development in {001} facets. On the other hand, the alcoholysis reaction was found easily occurred between the primary alcohol and isopropoxide that effectively limited the hydrolysis and condensation processes but also suppressed the structural capping effect. Therefore, the anatase crystals prepared in the primary alcohols became exceptionally small and showed spherical shape. Finally, the anatase crystals prepared using isopropanol demonstrated the highest photocatalytic activity due to its evident preferred crystallization in the {001} facets.

Size distribution of magnetic iron oxide nanoparticles using Warren-Averbach XRD analysis

NASA Astrophysics Data System (ADS)

Mahadevan, S.; Behera, S. P.; Gnanaprakash, G.; Jayakumar, T.; Philip, J.; Rao, B. P. C.

2012-07-01

We use the Fourier transform based Warren-Averbach (WA) analysis to separate the contributions of X-ray diffraction (XRD) profile broadening due to crystallite size and microstrain for magnetic iron oxide nanoparticles. The profile shape of the column length distribution, obtained from WA analysis, is used to analyze the shape of the magnetic iron oxide nanoparticles. From the column length distribution, the crystallite size and its distribution are estimated for these nanoparticles which are compared with size distribution obtained from dynamic light scattering measurements. The crystallite size and size distribution of crystallites obtained from WA analysis are explained based on the experimental parameters employed in preparation of these magnetic iron oxide nanoparticles. The variation of volume weighted diameter (Dv, from WA analysis) with saturation magnetization (Ms) fits well to a core shell model wherein it is known that Ms=Mbulk(1-6g/Dv) with Mbulk as bulk magnetization of iron oxide and g as magnetic shell disorder thickness.

Further Improvement of the RITS Code for Pulsed Neutron Bragg-edge Transmission Imaging

NASA Astrophysics Data System (ADS)

Sato, H.; Watanabe, K.; Kiyokawa, K.; Kiyanagi, R.; Hara, K. Y.; Kamiyama, T.; Furusaka, M.; Shinohara, T.; Kiyanagi, Y.

The RITS code is a unique and powerful tool for a whole Bragg-edge transmission spectrum fitting analysis. However, it has had two major problems. Therefore, we have proposed methods to overcome these problems. The first issue is the difference in the crystallite size values between the diffraction and the Bragg-edge analyses. We found the reason was a different definition of the crystal structure factor. It affects the crystallite size because the crystallite size is deduced from the primary extinction effect which depends on the crystal structure factor. As a result of algorithm change, crystallite sizes obtained by RITS drastically approached to crystallite sizes obtained by Rietveld analyses of diffraction data; from 155% to 110%. The second issue is correction of the effect of background neutrons scattered from a specimen. Through neutron transport simulation studies, we found that the background components consist of forward Bragg scattering, double backward Bragg scattering, and thermal diffuse scattering. RITS with the background correction function which was developed through the simulation studies could well reconstruct various simulated and experimental transmission spectra, but refined crystalline microstructural parameters were often distorted. Finally, it was recommended to reduce the background by improving experimental conditions.

Controlling morphology and crystallite size of Cu(In{sub 0.7}Ga{sub 0.3})Se{sub 2} nano-crystals synthesized using a heating-up method

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

Hsu, Wei-Hsiang; Hsiang, Hsing-I, E-mail: hsingi@mail.ncku.edu.tw; Chia, Chih-Ta

2013-12-15

CuIn{sub 0.7}Ga{sub 0.3}Se{sub 2}(CIGS) nano-crystals were successfully synthesized via a heating-up process. The non-coordinating solvent (1-octadecene) and selenium/cations ratio effects on the crystalline phase and crystallite size of CIGS nano-crystallites were investigated. It was observed that the CIGS nano-crystallite morphology changed from sheet into spherical shape as the amount of 1-octadecene addition was increased. CIGS nano-crystals were obtained in 9–20 nm sizes as the selenium/cations ratio increased. These results suggest that the monomer reactivity in the solution can be adjusted by changing the solvent type and selenium/cations ratio, hence affecting the crystallite size and distribution. - Graphical abstract: CuIn{sub 0.7}Ga{submore » 0.3}Se{sub 2}(CIGS) nano-crystals were successfully synthesized via a heating-up process in this study. The super-saturation in the solution can be adjusted by changing the OLA/ODE ratio and selenium/cation ratio.« less

The effect of confinement on the crystalline microstructure of polymer: fullerene bulk heterojunctions

DOE PAGES

Ashraf, A.; Dissanayake, D. M. N. M.; Eisaman, M. D.

2015-07-01

We investigate the effect of confinement on the coherence length and the crystalline microstructure of the polymer component of polymer: fullerene bulk heterojunction thin films using grazing incidence wide angle x-ray scattering. We find that the polymer crystallite size decreases and the alignment of the molecules along the surface normal increases, as the thin-film thickness is reduced from 920nm to < 20nm and approaches the thin-film confinement regime. Furthermore, we find that the polymer crystallite size near the surface (air interface) is lower than the crystallite size in the bulk or the bottom (substrate interface) of bulk heterojunction films thickermore » than the confinement regime. Variation in polymer crystallite size can cause changes in charge carrier mobility and recombination rates, which in turn affect the performance of bulk heterojunction thin film devices such as photovoltaics and photodetectors« less

Synthetic control of manganese birnessite: Impact of crystallite size on Li, Na, and Mg based electrochemistry

DOE PAGES

Yin, Jiefu; Takeuchi, Esther S.; Takeuchi, Kenneth J.; ...

2016-08-12

We demonstrated the synthesis and characterization of Mg-birnessite (Mg xMnO 2) with different crystallite sizes, prepared though low temperature precipitation and ion exchange. The influence of crystallite size on electrochemical performance of Mg-birnessite was studied for the first time, where material with smaller crystallite size was demonstrated to have enhanced capacity and rate capability in Li ion, Na ion, and Mg ion based electrolytes. Cation diffusion using GITT type testing demonstrated the ion diffusion coefficient of Mg 2+ was ~10× lower compared with Li + and Na +. This work illustrates that tuning of inorganic materials properties can lead tomore » significant enhancement of electrochemical performance in lithium, sodium as well as magnesium based batteries for materials such as Mg-birnessite and provides a deliberate approach to improve electrochemical performance.« less

Role of stacking disorder in ice nucleation

NASA Astrophysics Data System (ADS)

Lupi, Laura; Hudait, Arpa; Peters, Baron; Grünwald, Michael; Gotchy Mullen, Ryan; Nguyen, Andrew H.; Molinero, Valeria

2017-11-01

The freezing of water affects the processes that determine Earth’s climate. Therefore, accurate weather and climate forecasts hinge on good predictions of ice nucleation rates. Such rate predictions are based on extrapolations using classical nucleation theory, which assumes that the structure of nanometre-sized ice crystallites corresponds to that of hexagonal ice, the thermodynamically stable form of bulk ice. However, simulations with various water models find that ice nucleated and grown under atmospheric temperatures is at all sizes stacking-disordered, consisting of random sequences of cubic and hexagonal ice layers. This implies that stacking-disordered ice crystallites either are more stable than hexagonal ice crystallites or form because of non-equilibrium dynamical effects. Both scenarios challenge central tenets of classical nucleation theory. Here we use rare-event sampling and free energy calculations with the mW water model to show that the entropy of mixing cubic and hexagonal layers makes stacking-disordered ice the stable phase for crystallites up to a size of at least 100,000 molecules. We find that stacking-disordered critical crystallites at 230 kelvin are about 14 kilojoules per mole of crystallite more stable than hexagonal crystallites, making their ice nucleation rates more than three orders of magnitude higher than predicted by classical nucleation theory. This effect on nucleation rates is temperature dependent, being the most pronounced at the warmest conditions, and should affect the modelling of cloud formation and ice particle numbers, which are very sensitive to the temperature dependence of ice nucleation rates. We conclude that classical nucleation theory needs to be corrected to include the dependence of the crystallization driving force on the size of the ice crystallite when interpreting and extrapolating ice nucleation rates from experimental laboratory conditions to the temperatures that occur in clouds.

Role of stacking disorder in ice nucleation.

PubMed

Lupi, Laura; Hudait, Arpa; Peters, Baron; Grünwald, Michael; Gotchy Mullen, Ryan; Nguyen, Andrew H; Molinero, Valeria

2017-11-08

The freezing of water affects the processes that determine Earth's climate. Therefore, accurate weather and climate forecasts hinge on good predictions of ice nucleation rates. Such rate predictions are based on extrapolations using classical nucleation theory, which assumes that the structure of nanometre-sized ice crystallites corresponds to that of hexagonal ice, the thermodynamically stable form of bulk ice. However, simulations with various water models find that ice nucleated and grown under atmospheric temperatures is at all sizes stacking-disordered, consisting of random sequences of cubic and hexagonal ice layers. This implies that stacking-disordered ice crystallites either are more stable than hexagonal ice crystallites or form because of non-equilibrium dynamical effects. Both scenarios challenge central tenets of classical nucleation theory. Here we use rare-event sampling and free energy calculations with the mW water model to show that the entropy of mixing cubic and hexagonal layers makes stacking-disordered ice the stable phase for crystallites up to a size of at least 100,000 molecules. We find that stacking-disordered critical crystallites at 230 kelvin are about 14 kilojoules per mole of crystallite more stable than hexagonal crystallites, making their ice nucleation rates more than three orders of magnitude higher than predicted by classical nucleation theory. This effect on nucleation rates is temperature dependent, being the most pronounced at the warmest conditions, and should affect the modelling of cloud formation and ice particle numbers, which are very sensitive to the temperature dependence of ice nucleation rates. We conclude that classical nucleation theory needs to be corrected to include the dependence of the crystallization driving force on the size of the ice crystallite when interpreting and extrapolating ice nucleation rates from experimental laboratory conditions to the temperatures that occur in clouds.

Size-induced variations in bulk/surface structures and their impact on photoluminescence properties of GdVO4:Eu3+ nanoparticles.

PubMed

Yang, Liusai; Li, Liping; Zhao, Minglei; Li, Guangshe

2012-07-28

This work explores the size-induced lattice modification and its relevance to photoluminescence properties of tetragonal zircon-type GdVO(4):Eu(3+) nanostructures. GdVO(4):Eu(3+) nanoparticles with crystallite sizes ranging from 14.4 to 24.7 nm were synthesized by a hydrothermal method using sodium citrate as a capping agent. Regardless of the reaction temperatures, all samples retained an ellipsoidal-like morphology. Nevertheless, as the crystallite size reduces, there appears a tensile strain and lattice distortion, which is accompanied by a lattice expansion and a decreased symmetry of structural units. These lattice modifications could be associated with the changes in the interior chemical bonding due to the interactions of surface defect dipoles that have imposed an increased negative pressure with crystallite size reduction. Furthermore, crystallite size reduction also led to a significant increase in the amounts of surface hydroxyl groups and citric species, as well as the concentration of the surface Eu(3+) ions. When Eu(3+) was taken as a structural probe, it was found that the asymmetric ratio (I(02)/I(01)) of Eu(3+) gradually declined to show a remarkable decrease in color chromaticity as crystallite size reduces, which could be interpreted as due to the change of local environments of Eu(3+) ions from the interior to the surface of the nanoparticles.

Phase Composition, Crystallite Size and Physical Properties of B2O3-added Forsterite Nano-ceramics

NASA Astrophysics Data System (ADS)

Pratapa, S.; Chairunnisa, A.; Nurbaiti, U.; Handoko, W. D.

2018-05-01

This study was aimed to know the effect of B2O3 addition on the phase composition, crystallite size and dielectric properties of forsterite (Mg2SiO4) nano-ceramics. It utilized a purified silica sand from Tanah Laut, South Kalimantan as the source of (amorphous) silica and a magnesium oxide (MgO) powder. They were thoroughly mixed and milled prior to calcination. The addition of 1, 2, 3, and 4 wt% B2O3 to the calcined powder was done before uniaxial pressing and then sintering at 950 °C for 4 h. The phase composition and forsterite crystallite size, the microstructure and the dielectric constant of the sintered samples were characterized using X-ray diffractometer (XRD), Scanning Electron Microscope (SEM) and Vector Network Analyzer (VNA), respectively. Results showed that all samples contained forsterite, periclase (MgO) and proto enstatite (MgSiO3) with different weight fractions and forsterite crystallite size. In general, the weight fraction and crystallite size of forsterite increased with increasing B2O3 addition. The weight fraction and crystallite size of forsterite in the 4%-added sample reached 99% wt and 164 nm. Furthermore, the SEM images showed that the average grain size became slightly larger and the ceramics also became slightly denser as more B2O3 was added. The results are in accordance with density measurements using the Archimedes method which showed that the 4% ceramic exhibited 1.845 g/cm3 apparent density, while the 1% ceramic 1.681 g/cm3. We also found that the higher the density, the higher the average dielectric constant, i.e. it was 4.6 for the 1%-added sample and 6.4 for the 4%-added sample.

Near-infrared emission from mesoporous crystalline germanium

NASA Astrophysics Data System (ADS)

Boucherif, Abderraouf; Korinek, Andreas; Aimez, Vincent; Arès, Richard

2014-10-01

Mesoporous crystalline germanium was fabricated by bipolar electrochemical etching of Ge wafer in HF-based electrolyte. It yields uniform mesoporous germanium layers composed of high density of crystallites with an average size 5-7 nm. Subsequent extended chemical etching allows tuning of crystallites size while preserving the same chemical composition. This highly controllable nanostructure exhibits photoluminescence emission above the bulk Ge bandgap, in the near-infrared range (1095-1360nm) with strong evidence of quantum confinement within the crystallites.

Synthesis of Copper Birnessite, Cu xMnO y·nH 2O with Crystallite Size Control: Impact of Crystallite Size on Electrochemistry

DOE PAGES

Li, Yue Ru; Marschilok, Amy C.; Takeuchi, Esther S.; ...

2015-11-24

This report describes the first detailed electrochemical examination of a series of copper birnessite samples under lithium-based battery conditions, allowing a structure/function analysis of the electrochemistry and related material properties. To obtain the series of copper birnessite samples, a novel synthetic approach for the preparation of copper birnessite, Cu xMnO y·nH 2O is reported. The copper content (x) in Cu xMnO y·nH 2O, 0.28 >= x >= 0.20, was inversely proportional to crystallite size, which ranged from 12 to 19 nm. The electrochemistry under lithium-based battery conditions showed that the higher copper content (x = 0.28) and small crystallite sizemore » (similar to 12 nm) sample delivered similar to 194 mAh/g, about 20% higher capacity than the low copper content (x = 0.22) and larger crystallite size (similar to 19 nm) material. In addition, Cu xMnO y·nH 2O displays quasi-reversible electrochemistry in magnesium based electrolytes, indicating that copper birnessite could be a candidate for future application in magnesium-ion batteries.« less

Correlations between Crystallite Size, Shape, Surface, and Infrared Spectra Using the Ti-C System

NASA Astrophysics Data System (ADS)

Kimura, Y.; Ikegami, A.; Kurumada, M.; Kamitsuji, K.; Kaito, C.

2004-06-01

TiC crystallites less than 10 nm in size showed an absorption feature at 14.3 μm. This 14.3 μm absorption was rarely seen in specimens ranging from bulk material to grains of 50 nm in size. The 14.3 μm feature was weakened as a result of the growth of TiC crystallites by heat treatment. When the carbide grains were covered with a carbon layer, the absorption peaks were considerably weakened, i.e., the absorption intensity depended on the grain surface state. A possible explanation is that the effects of size and shape on the spectra depend on the surface anisotropy.

Influence of crystallite size on the magnetic and heat generation properties of La0.77Sr0.23MnO3 nanoparticles for hyperthermia applications

NASA Astrophysics Data System (ADS)

Das, Harinarayan; Inukai, Akihiro; Debnath, Nipa; Kawaguchi, Takahiko; Sakamoto, Naonori; Hoque, Sheikh Manjura; Aono, Hiromichi; Shinozaki, Kazuo; Suzuki, Hisao; Wakiya, Naoki

2018-01-01

In this paper, we report a detailed study of magnetic properties and AC magnetic heat generation characteristics of La0.77Sr0.23MnO3 (LSMO) nanoparticles to investigate appropriate crystallite size with a view to the proper application of self-controlled magnetic hyperthermia treatments of cancer. A series of nanocrystalline LSMO manganite was synthesized through the chemical route called as "polymerized complex method" and then subsequently annealed at the different temperature from 600 to 1400 °C to obtain various crystallite size. Phase formation and crystal structure of the prepared powder were determined by the powder X-ray diffraction (XRD) using Rietveld analysis. The XRD patterns reveal that all powder samples are a single phase rhombohedral perovskite-like structure with R 3 bar c space group. The mean crystallite size of prepared particles varied from 19 to 243.8 nm with the increase of the annealing temperature starting from 600 to 1400 °C. The field emission scanning electron microscopy (FE-SEM) analysis shows the surface morphology with a strong agglomeration of fine nanoparticles. The Magnetic study reveals that these nanoparticles exhibit ferromagnetic nature with different value of magnetization, coercivity, Curie temperature which is strongly dependent on their crystallite size. The maximum saturation temperature (TS = 66 °C) under AC magnetic field (H = 1.77 kA/m, f = 370 kHz) was found for the crystallite size of 39.5 nm due to its pure single domain phase. Such LSMO nanoparticles, having the higher heating rate, can be used in magnetically induced hyperthermia cancer treatment.

Modeling of the Structure of Disordered Metallic Alloys and Its Transformation Under Thermal Forcing

NASA Astrophysics Data System (ADS)

Cress, Ryan Paul

The morphology of disordered binary metallic alloys is investigated. The structure of disordered binary metallic alloys is modeled as a randomly close packed (RCP) assembly of atoms. It was observed through a 2-D binary hard sphere experiment that RCP structure can be modeled as a mixture of nano-crystallites and glassy matter. We define the degree of crystallinity as the fraction of atoms contained in nano-crystallites in an RCP medium. Nano-crystallites by size in a crystallite size distribution were determined experimentally to define the morphology of the RCP medium. Both the degree of crystallinity and the crystallite size distribution have been found to be determined by the composition of a given binary mixture. A 2-D Monte Carlo simulation was developed in order to replicate the RCP structure observed in the experiment which is then extended to cases of arbitrary composition. Crystallites were assumed to be spherical with isotropic cross sections. The number of atoms in an individual crystallite in 2-D is simply transformed into the number of atoms in 3-D; we then obtain the crystallite size distribution in 3-D. This experiment accounts for the contribution from the repulsive core of the inter-atomic potential. The attractive part of the potential is recovered by constructing spherical nano-crystallites of a given radius from a crystalline specimen of each given alloy. A structural model of a disordered alloy is thus obtained. With the basic structure of the RCP medium defined, the response to heating would be in the form of changes to the crystallite size distribution. This was first investigated in a hard sphere mechanical oven experiment. The experimental setup consists of a 2-D cell which is driven by two independent stepper motors. The motors drive a binary RCP bed of spheres on a slightly tilted plane according to a chaotic algorithmm. The motors are driven at four different speed settings. The RCP medium was analyzed using a sequence of digital images taken of the beds. The bursts of images provide a Gaussian distribution of particle speeds in x and y directions thus giving rise to the notion of "temperature." This temperature scales with the motor speed settings. The measured average degree of crystallinity is found to decrease as the effective temperature was raised suggesting that nano-crystallites dissociate under thermal forcing. The evolution of a specimen's structure is calculated rigorously by means of the law of mass action formalism. A system of thermal dissociation reaction equations is written out for the set of nano-crystallites according to the 3-D crystallite size distribution. The equilibrium treatment is justified because the energy differences between metastable RCP structures fall within kT. Thermal dissociation of one surface atom at a time is assumed because the energy cost in dissociation of a surface atom on a nano-crystallite is significantly less than that of a multi atom cluster. The full set of reaction equations cover all possible dissociation steps, which may amount to several thousand for a disordered alloy specimen. The primary determining factor in each of these dissociation equations is the dissociation potential or the amount of attractive energy needed to remove a surface atom on a nano-crystallite of a given size. The attractive potential between atoms is calculated using a Lennard-Jones potential between a pair of atoms for which quantum chemistry calculations exist in the literature. All interactions impinged on the surface atom by all other atoms in a crystallite are summed. As the nano-crystallites dissociate due to heating, the structure of the alloy changes, and this leads to modifications of alloy's transport properties. The model is found to predict the melting temperature of various disordered binary alloys as well as refractory metals in good agreement with known data. The structure model for disordered binary alloys gives an excellent characterization of the alloy morphology. It therefore provides fruitful avenues for making predictions about how thermophysical properties of disordered binary alloys change as the alloy temperature is raised by heating.

X-ray peak profile analysis of zinc oxide nanoparticles formed by simple precipitation method

NASA Astrophysics Data System (ADS)

Pelicano, Christian Mark; Rapadas, Nick Joaquin; Magdaluyo, Eduardo

2017-12-01

Zinc oxide (ZnO) nanoparticles were successfully synthesized by a simple precipitation method using zinc acetate and tetramethylammonium hydroxide. The synthesized ZnO nanoparticles were characterized by X-ray Diffraction analysis (XRD) and Transmission Electron Microscopy (TEM). The XRD result revealed a hexagonal wurtzite structure for the ZnO nanoparticles. The TEM image showed spherical nanoparticles with an average crystallite size of 6.70 nm. For x-ray peak analysis, Williamson-Hall (W-H) and Size-Strain Plot (SSP) methods were applied to examine the effects of crystallite size and lattice strain on the peak broadening of the ZnO nanoparticles. Based on the calculations, the estimated crystallite sizes and lattice strains obtained are in good agreement with each other.

Method of controlling crystallite size in nuclear-reactor fuels

DOEpatents

Lloyd, Milton H.; Collins, Jack L.; Shell, Sam E.

1985-01-01

Improved spherules for making enhanced forms of nuclear-reactor fuels are prepared by internal gelation procedures within a sol-gel operation and are accomplished by first boiling the concentrated HMTA-urea feed solution before engaging in the spherule-forming operation thereby effectively controlling crystallite size in the product spherules.

THE EFFECT OF SATELLITE LINES FROM THE X-RAY SOURCE ON X-RAY DIFFRACTION PEAKS

EPA Science Inventory

The article discusses the development of a method for relating reactivity to crystallite size and strain parameters obtained by the Warren-Averbach technique. EPA has been using crystallite size and strain data obtained from x-ray diffraction (XRD) peak profile analysis to predic...

Method of controlling crystallite size in nuclear-reactor fuels

DOEpatents

Lloyd, M.H.; Collins, J.L.; Shell, S.E.

Improved spherules for making enhanced forms of nuclear-reactor fuels are prepared by internal gelation procedures within a sol-gel operation and are accomplished by first boiling the concentrated HMTA-urea feed solution before engaging in the spherule-forming operation thereby effectively controlling crystallite size in the product spherules.

Nucleation and Early Stages of Layer-by-Layer Growth of Metal Organic Frameworks on Surfaces

PubMed Central

2015-01-01

High resolution atomic force microscopy (AFM) is used to resolve the evolution of crystallites of a metal organic framework (HKUST-1) grown on Au(111) using a liquid-phase layer-by-layer methodology. The nucleation and faceting of individual crystallites is followed by repeatedly imaging the same submicron region after each cycle of growth and we find that the growing surface is terminated by {111} facets leading to the formation of pyramidal nanostructures for [100] oriented crystallites, and triangular [111] islands with typical lateral dimensions of tens of nanometres. AFM images reveal that crystallites can grow by 5–10 layers in each cycle. The growth rate depends on crystallographic orientation and the morphology of the gold substrate, and we demonstrate that under these conditions the growth is nanocrystalline with a morphology determined by the minimum energy surface. PMID:26709359

Effect of calcination temperature on phase transformation and crystallite size of copper oxide (CuO) powders

NASA Astrophysics Data System (ADS)

Ratnawulan, Fauzi, Ahmad; AE, Sukma Hayati

2017-08-01

Copper oxide powder was prepared from Copper iron from South Solok, Indonesia. The samples was dried and calcined for an hour at temperatures of 145°C, 300°C,850°C, 1000°C. Phase transformation and crystallite size of the calcined powders have been investigated as a function of calcination temperature by room-temperature X-ray diffraction (XRD). It was seen that the tenorite, CuO was successfully obtained. With increasing calcining temperature, CuO transformed from malachite Cu2(CO3)(OH)2 to tenorite phase (CuO) and crystallite size of prepared samples increased from 36 nm to 76 nm.

Structure and magnetic properties of mechanically alloyed Co and Co-Ni

NASA Astrophysics Data System (ADS)

Guessasma, S.; Fenineche, N.

The influence of milling process on magnetic properties of Co and Co-Ni materials is studied. Coercivity, squareness ratio and crystallite size of mechanically alloyed Co-Ni material were related to milling time. For Co material, coercivity, cubic phase ratio and crystallite size were related to milling energy considering the vial and plateau rotation velocities. An artificial neural network (ANN) combining the parameters for both materials is used to predict magnetic and structure results versus milling conditions. Predicted results showed that milling energy is mostly dependent on the ratio vial to plateau rotation velocities and that milling times larger than 40 h do not add significant change to both structure and magnetic responses. Magnetic parameters were correlated to crystallite size and the D 6 law was only valid for small sizes.

Magnetic and critical properties of Pr0.6Sr0.4MnO3 nanocrystals prepared by a combination of the solid state reaction and the mechanical ball milling methods

NASA Astrophysics Data System (ADS)

Dung, Nguyen Thi; Linh, Dinh Chi; Huyen Yen, Pham Duc; Yu, Seong Cho; Van Dang, Nguyen; Dang Thanh, Tran

2018-06-01

Influence of the crystallite size on the magnetic and critical properties of nanocrystals has been investigated. The results show that Curie temperature and magnetization slightly decrease with decreasing average crystallite size . Based on the mean-field theory and the magnetic-field dependences of magnetization at different temperatures , we pointed out that the ferromagnetic-paramagnetic phase transition in the samples undergoes the second-order phase transition with the critical exponents (, , and ) close to those of the mean-field theory. However, there is a small deviation from those expected for the mean-field theory of the values of , and obtained for the samples. It means that short-range ferromagnetic interactions appear in the smaller particles. In other words, nanocrystals become more magnetically inhomogeneous with smaller crystallite sizes that could be explained by the presence of surface-related effects, lattice strain and distortions, which lead the strength of ferromagnetic interaction is decreased in the small crystallite sizes.

Microstructural Evolution of Nanocrystalline ZrO2 in a Fe Matrix During High-Temperature Exposure

NASA Astrophysics Data System (ADS)

Raghavendra, K. G.; Dasgupta, Arup; Athreya, C. N.; Jayasankar, K.; Saroja, S.; Subramanya Sarma, V.

2018-06-01

The current study examines the evolution of nanocrystallites of ZrO2 with time and temperature in a Fe-ZrO2 composite. The crystallite sizes were determined through X-ray peak broadening analysis by the Williamson-Hall method together with dark field transmission electron microscopy. The ZrO2 crystallites were found to be stable and retained their sizes at 973 K and 1073 K for hold durations up to 600 minutes. On the other hand, the crystallites were seen to grow at 1173 K and reached up to 200 nm for a hold time of 600 minutes. The Ostwald ripening model was adopted to understand crystallite growth while a dislocation-driven pipe diffusion was adopted for understanding the kinetics of grain growth. The activation energy of grain growth was calculated as 379 kJ mol-1. The modeled and experimentally calculated size evolutions with time and temperature were shown to be in good agreement with each other. A detailed discussion on the kinetics and activation energy of grain growth of ZrO2 crystallites in a Fe matrix is presented in this manuscript.

Study of the resonant frequencies of silicon microcantilevers coated with vanadium dioxide films during the insulator-to-metal transition

NASA Astrophysics Data System (ADS)

Rúa, Armando; Fernández, Félix E.; Hines, Melissa A.; Sepúlveda, Nelson

2010-03-01

Vanadium dioxide (VO2) thin films were grown on silicon microcantilevers and companion test substrates by pulsed laser deposition followed by in situ annealing in an oxidizing atmosphere, with annealing times used to control crystallite sizes. Annealing times of 18 min produced VO2 films with average crystallite sizes of ˜10 nm or less, while those annealed for 35 min had crystallites of average size ˜90 nm, comparable to sample thickness. X-ray diffraction and x-ray photoelectron spectroscopy studies of the samples showed that films with crystallite sizes ˜40 nm or greater consisted of substoichiometric VO2 in its monoclinic phase, with preferential orientation with (011) planes parallel to the sample surface, while finer structured samples had a substantially similar composition, but showed no clear evidence of preferential orientation and were probably partially amorphous. Forced vibration experiments were performed with the cantilevers as they were thermally cycled through the VO2 insulator-to-metal transition (IMT). Very large reversible changes in the resonant frequencies of up to 5% (3.6 kHz) as well as hysteretic behavior were observed, which depend strongly on film crystallite size. The average value of Young's modulus for VO2 films with crystallite sizes of ˜90 nm was estimated from the mechanical resonance data at room temperature to be ˜120 GPa, but the large tensile stresses which develop between film and substrate through the IMT impede a similar determination for the VO2 tetragonal phase, since the commonly used relationships for cantilever frequencies derived from elasticity theory are not applicable for strongly curved composite beams. The results presented show that VO2 thin films can be useful in novel microscale and nanoscale electromechanical resonators in which effective stiffness can be tuned thermally or optically. This response can provide additional functionality to VO2—based devices which take advantage of other property changes through the IMT.

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

Apaydin, Ramazan Oguzhan; Ebin, Burcak; Gurmen, Sebahattin

Copper-Nickel (CuNi) nanostructured alloy particles were produced by Ultrasonic Spray Pyrolysis and Hydrogen Reduction Method (USP-HR) from high purity copper and nickel nitrate aqueous solutions. The effect of the precursor solution in the range of 0.1 and 0.5 mol/L on the morphology and crystallite size of CuNi nanoparticles were investigated under 2 h running time, 700 °C operating temperature and 0.5 L/min H{sub 2} flow rate. Particle size, morphology, composition and crystallite structure were characterized by Scanning Electron Microscopy (SEM), Energy Dispersive Spectroscopy (EDS) and X-Ray Diffraction (XRD). Particle characterization studies show that nanostructured alloy particles have cubic crystal structuremore » and they are in submicron size range with spherical morphology. The crystallite sizes of the particles calculated with Scherrer formula are 40 and 34 nm and average particles sizes observed from the SEM images are 300 and 510 nm for each experiment respectively.« less

THE CHARACTERIZATION OF A SOLID SORBENT WITH CRYSTALLITE SIZE AND STRAIN DATA FROM X-RAY DIFFRACTION LINE BROADENING

EPA Science Inventory

The paper gives results of the characterization of a solid sorbent with crystallite size and strain data from x-ray diffraction line broadening, as part of an EPA investigation of the injection of dry Ca(OH)2 into coal-fired electric power plant burners for the control of SO2 emi...

Thin Film Research. Volume 1

DTIC Science & Technology

1985-05-30

Order (FECO) ......... 23 3. X -Ray Diffraction ............................... 26 4. Transmission Electron Microscopy (TEM) ............... 26 5...remained amorphous after bombardment, as evidenced by X - ray diffraction, and showed no other changes. 0 (2) For Sb203, the crystallite size was reduced...main effect on MgF2 was the reduction in crystallite size. The films were too thir. for meaningful x - ray diffraction analysis. Durability and

Effect of sample moisture content on XRD-estimated cellulose crystallinity index and crystallite size

Treesearch

Umesh P. Agarwal; Sally A. Ralph; Carlos Baez; Richard S. Reiner; Steve P. Verrill

2017-01-01

Although X-ray diffraction (XRD) has been the most widely used technique to investigate crystallinity index (CrI) and crystallite size (L200) of cellulose materials, there are not many studies that have taken into account the role of sample moisture on these measurements. The present investigation focuses on a variety of celluloses and cellulose...

Crystallite Size-Lattice Strain Estimation and Optical Properties of Mn0.5Zn0.5Fe2O4 Nanoparticles

NASA Astrophysics Data System (ADS)

Indrayana, I. P. T.; Suharyadi, E.

2018-04-01

In the present work, we performed William-Hall plot using uniform deformation model (UDM) to estimate the crystallite size and lattice strain of Mn0.5Zn0.5Fe2O4 with various calcination temperature. The calculated crystallite sizes are 25.86 nm, 29.55 nm and 24.97 nm for nanoparticles which were calcined at a temperature of 600°C, 800°C and 1000°C, consecutively. The strain of nanoparticles has value in the order of 10-3. Controlling the calcination temperature will facilitate a change in crystallinity of nanoparticles and influence their crystallite size and strain of the crystal lattice. The optical band gap energy of samples nanoparticles is in a range of 1.09 eV – 3.30 eV. Increasing calcination temperature increased the direct and indirect band gap energy. The Urbach energy was found to increase with increased of gap energy. These results demonstrated that higher structural and optical properties of Mn0.5Zn0.5Fe2O4 can be obtained from a higher calcination temperature.

Synthesis of antimony-doped tin oxide (ATO) nanoparticles by the nitrate-citrate combustion method

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

Zhang Jianrong; Gao Lian

2004-12-02

Antimony-doped tin oxide (ATO) nanoparticles having rutile structure have been synthesized by the combustion method using citric acid (CA) as fuel and nitrate as an oxidant, the metal sources were granulated tin and Sb{sub 2}O{sub 3}. The influence of citric acid (fuel) to metal ratio on the average crystallite size, specific surface area and morphology of the nanoparticles has been investigated. X-ray diffraction showed the tin ions were reduced to elemental tin during combustion reaction. The average ATO crystallite size increased with the increase of citric acid (fuel). Powder morphology and the comparison of crystallite size and grain size showsmore » that the degree of agglomeration of the powder decreased with an increase of the ratio. The highest specific surface area was 37.5 m{sup 2}/g when the citric acid to tin ratio was about 6.« less

Effect of the CTAB concentration on the upconversion emission of ZrO 2:Er 3+ nanocrystals

NASA Astrophysics Data System (ADS)

López-Luke, T.; De la Rosa, E.; Sólis, D.; Salas, P.; Angeles-Chavez, C.; Montoya, A.; Díaz-Torres, L. A.; Bribiesca, S.

2006-10-01

Upconversion emission of ZrO 2:Er 3+ (0.2 mol%) nanophosphor were studied as function of surfactant concentration after excitation at 968 nm. The strong green emission was produced by the transition 2H 11/2 + 4S 3/2 → 4I 15/2 and was explained in terms of cooperative energy transfer between neighboring ions. The upconverted signal was enhanced but the fluorescence decay time was reduced as either the surfactant concentration increases or the annealing time reduces. Experimental results show that surfactant concentration controls the particle size and morphology while annealing time control the phase composition and crystallite size. The highest intensity was obtained for a sample composed of a mixture of tetragonal (33 wt.%) and monoclinic (67 wt.%) phase with crystallite size of 31 and 59 nm, respectively. This result suggests that tetragonal crystalline structure and small crystallite size are more favorable for the upconversion emission.

Comparative study of Ni and Cu doped ZnO nanoparticles: Structural and optical properties

NASA Astrophysics Data System (ADS)

Thakur, Shaveta; Thakur, Samita; Sharma, Jyoti; Kumar, Sanjay

2018-05-01

Nanoparticles of undoped and doped (0.1 M Ni2+ and Cu2+) ZnO are synthesized using chemical precipitation method. The crystallite size, morphology, chemical bonding and optical properties of as prepared nanoparticles are determined by X-ray diffraction (XRD), Scanning electron microscopy (SEM), Fourier transform infrared (FTIR) spectroscopy and UV-visible spectra. XRD analysis shows that the prepared samples are single phase and have hexagonal wurtzite structure. The crystallite size of the doped and undoped nanoparticles is determined using Scherrer method. The crystallite size is found to be increased with concentration of nickel and copper. All stretching and vibrational bands are observed at their specific positions through FTIR. The increase in band gap can be attributed to the different chemical nature of dopant and host cation.

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

Fitriana, Karina Nur, E-mail: nurfitriana.karina@gmail.com; Hafizah, Mas Ayu Elita, E-mail: kemasayu@yahoo.com; Manaf, Azwar, E-mail: azwar@ui.ac.id

Synthesis of single phased SrO.6Fe{sub 2-x}Mn{sub x/2}Ti{sub x/2}O{sub 3} (x = 0.0; 0.5; and 1.0) nanoparticles has been prepared through mechanical alloying, assisted with the ultrasonic destruction process. Monocrystalline particles were obtained when x = 0 treated with ultrasonic destruction at 55 μm of transducer amplitude. Average particle size and crystallite size were reduced significantly from 723 nm to ∼87 nm for x = 0. The particle size was not significantly reduced when x = 0.5 and x = 1 was changed. On the other hand, substitution of Ti elements on some of Fe elements expectedly had a major effectmore » on reducing particle size. This was proven by larger size on both particle and crystallite size at x = 1 rather than x = 0.5, with comparison respectively 2:1 (in nm). In addition, a higher transducer power was required for modifying Strontium Hexaferrite (SHF) with more Ti elements and a bigger size of pre-ultrasonic destructed sample. It is concluded that the amplitude of the transducer in ultrasonic destruction process and the element of ionic substitution affects both average particle size and crystallite size of SHF.« less

Hierarchically 3D assembled strontium titanate nanomaterials for water splitting application

NASA Astrophysics Data System (ADS)

Moniruddin, Md; Afroz, Khurshida; Shabdan, Yerkin; Bizri, Baraa; Nuraje, Nurxat

2017-10-01

Water splitting is an important technique to store solar energy in the simple form of chemical energy, such as hydrogen. Strontium titanate (SrTiO3) is one of the most promising photocatalysts to produce hydrogen gas from water splitting. In this research, an electrospinning technique in combination with sol-gel method was developed to synthesize 3D porous SrTiO3 nanostructures. Different crystallite sizes of SrTiO3-nanofibers (STO-NFs) were produced by varying the synthesis parameters including precursor concentration and calcination temperature. The synthesized nanofibers were characterized using DSC, TGA, XRD, SEM, and TEM. The crystallite size of STO-NFs decreases with increasing precursor concentration (3.03-15.78 vol.%) and gradually increases as the calcination temperature increases within the range of 600-800 °C. The photocatalytic activity of different STO-NFs (based on crystallite size) was also evaluated by the amount of H2 production from water splitting under UV irradiation. The H2 evolution study demonstrated that the photocatalytic activity of the STO-NFs strongly depends on the crystallite size of the nanofibers, precursor concentration, and calcination temperature. The H2 production rate increases with increasing crystallite size and temperature, whereas it decreases with increasing precursor concentration. The photocatalytic performance of the STO-NFs was also compared with the commercial SrTiO3 nanoparticles (STO-NPs) after Pt addition as a cocatalyst, where the synthesized nanofibers showed 2 times higher H2 production rate (1.14 mmol/g-h) than that of the nanoparticles. This synthesis technique provides a good example to produce other inorganic photocatalytic 3D porous structure materials.

Ex-Situ Synthesis of Polyvinyl alcohol(PVA)-coated Fe3O4 Nanoparticles by Coprecipitation-Ultrasonication Method

NASA Astrophysics Data System (ADS)

Riva'i, Imam; Oktavia Wulandari, Ika; Sulistyarti, Hermin; Sabarudin, Akhmad

2018-01-01

In this study, the synthesis of Fe3O4 nanoparticles was done with surface modification using PVA with coprecipitation-ultrasonication method. Time variations and PVA concentrations were added to determine the effect on crystallite size and lattice parameters on the synthesis of Fe3O4-PVA nanoparticles. Fe3O4 characterization was done using X-Ray Diffraction (XRD) and Fourier Transform Infrared Spectroscopy (FTIR) instruments. FTIR was employed to determine PVA coating on the surface of Fe3O4 nanoparticles. The crystallite size and lattice parameters were analyzed using XRD. From the FTIR data, it is known that the interaction between PVA and Fe3O4 nanoparticles is characterized by Fe-O-C group at 1100 cm-1 region which is characteristic of Fe3O4-PVA nanoparticles, C-H groups of PVA in the range of 2950 cm-1 wave number, C-C of PVA regions of wave number 1405 cm-1, Fe3O4 and Fe3O4-PVA samples are in the range of 565 cm-1. In addition, the variation of ultrasonication time and the addition of PVA concentration have an effect on the crystallite size change and the lattice parameter observed from the XRD data. The use of ultrasonication time will affect the size of the crystallite become smaller and the grating lattice parameters obtained are wider. The effect of addition of PVA showed that higher concentration of PVA resulted in smaller crystallite size and larger lattice parameters. These results indicated that ultrasonication time and addition of PVA concentration greatly affect the characteristics of nanoparticles.

Effect of current density during electrodeposition on microstructure and hardness of textured Cu coating in the application of antimicrobial Al touch surface.

PubMed

Augustin, Arun; Huilgol, Prashant; Udupa, K Rajendra; Bhat K, Udaya

2016-10-01

Copper is a well proven antimicrobial material which can be used in the form of a coating on the touch surfaces. Those coating can offer a good service as touch surface for very long time if only they possess good mechanical properties like scratch resistance and microhardness. In the present work the above mentioned mechanical properties were determined on the electrodeposited copper thin film; deposited on double zincated aluminium. During deposition, current density was varied from 2Adm(-2) to 10Adm(-2), to produce crystallite size in the range of 33.5nm to 66nm. The crystallite size was calculated from the X-ray peak broadening (Scherrer׳s formula) which were later confirmed by TEM micrographs. The scratch hardness and microhardness of the coating were measured and correlated with the crystallite size in the copper coating. Both characteristic values were found to increase with the reduction in crystallite size. Reduced crystallite size (Hall-Petch effect) and preferred growth of copper films along (111) plane play a significant role on the increase in the hardness of the coating. Further, TEM analysis reveals the presence of nano-twins in the film deposited at higher current density, which contributed to a large extent to the sharp increase of coating hardness compared to the mechanism of Hall-Petch effect. The antimicrobial ability of the coated sample has been evaluated against Escherichia coli bacteria and which is compared with that of commercially available bulk copper using the colony count method. 94% of E. coli cells were died after six hours of exposure to the copper coated surface. The morphology of the copper treated cells was studied using SEM. Copyright © 2016 Elsevier Ltd. All rights reserved.

Effects of crystallite size on the structure and magnetism of ferrihydrite

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

Wang, Xiaoming; Zhu, Mengqiang; Koopal, Luuk K.

2015-12-15

The structure and magnetic properties of nano-sized (1.6 to 4.4 nm) ferrihydrite samples are systematically investigated through a combination of X-ray diffraction (XRD), X-ray pair distribution function (PDF), X-ray absorption spectroscopy (XAS) and magnetic analyses. The XRD, PDF and Fe K-edge XAS data of the ferrihydrite samples are all fitted well with the Michel ferrihydrite model, indicating similar local-, medium- and long-range ordered structures. PDF and XAS fitting results indicate that, with increasing crystallite size, the average coordination numbers of Fe–Fe and the unit cell parameter c increase, while Fe2 and Fe3 vacancies and the unit cell parameter a decrease.more » Mössbauer results indicate that the surface layer is relatively disordered, which might have been caused by the random distribution of Fe vacancies. These results support Hiemstra's surface-depletion model in terms of the location of disorder and the variations of Fe2 and Fe3 occupancies with size. Magnetic data indicate that the ferrihydrite samples show antiferromagnetism superimposed with a ferromagnetic-like moment at lower temperatures (100 K and 10 K), but ferrihydrite is paramagnetic at room temperature. In addition, both the magnetization and coercivity decrease with increasing ferrihydrite crystallite size due to strong surface effects in fine-grained ferrihydrites. Smaller ferrihydrite samples show less magnetic hyperfine splitting and a lower unblocking temperature (T B) than larger samples. The dependence of magnetic properties on grain size for nano-sized ferrihydrite provides a practical way to determine the crystallite size of ferrihydrite quantitatively in natural environments or artificial systems.« less

Developpement d'un modele thermodynamique pour les cristallites de coke: Application aux systems carbone-hydrogene et carbone-soufre

NASA Astrophysics Data System (ADS)

Ouzilleau, Philippe

Carbon materials are essential components of multiple key industrial processes. One example of such a process is the production of aluminum using the Hall-Heroult process. It is well known that important quantities of carbon materials are regularily consumed by the operation of the Hall-Heroult process. In recent years, the increased impurity content of industrial carbon materials motivated the development of a better understanding for the high temperature behavior of these specific materials. The most common forms of carbon materials used in the industry are cokes. Cokes are carbon materials which, following heat treatment, present a crystalline structure similar to that observed in graphite. However, the observed crystallite size of cokes is usually much smaller than the one observed in graphite. For this reason, the chemical and thermodynamic properties of the ordered phase of cokes (i.e. coke crystallites) are very different than those of graphite (although coke crystallites of infinite size would possess properties almost identical to graphite). Coke crystallites consist of hexagonal planes of carbon atoms stacked one above the other. This particular aspect causes strong anisotropic properties in coke crystallites. No thermodynamic model was found for the production of a reliable correlation between the effect of crystallite size and chemical composition for the predictive calculations of the thermodynamic properties (and phase equilibriums) of coke crystallites. It is also difficult to produce predictive calculations that can be compared to experimental results using such a thermodynamic model. The goal of the present work is to propose a thermodynamic model designed to solve this problem. The present model is based on the well-defined geometrical properties of coke cristallites. This geometry allows the development of mathematical equations for the calculation of the mass balances of the crystallite (using a simplified geometry) using only the commonly used cristallite size parameters La (diameter of the crystallite) and Lc (height of the crystallite). The use of the Compound Energy Formalism is necessary to establish the methodology of the present model. Globally, the planar structure of the crystallites is divided into three sublattices on which individual chemical species are assumed to mix randomly. Appropriate thermodynamic paths are used to define the relative enthalpies and absolute entropies of these chemical species. The relative enthalpy and absolute entropy of the coke crystallites are derived for various values of La in the carbon/hydrogen and carbon/sulfur chemical systems. For the carbon/hydrogen system, the model parameters are based on the known values for the entropy of formation of simple hydrogenous organic compounds in the gaseous phase and known carbon/hydrogen bond enthalpies. Also, additional enthalpic properties of coke crystallites and graphitic structures are required for the definition of the thermodynamic paths (for example, the enthalpy associated with the delocalization of one electron in graphitic structures). Results for the carbon/hydrogen system are compared to experiments concerning the dehydrogenation of various cokes. A very satisfying agreement is obtained between the dehydrogenation curves predictively calculated by the model and the reported experimental results (obtained using slow heating rates). Most of the hydrogen content of coke crystallites (this content does not inclue the hydrogen in the condensed volatile matter phase) is predicted to leave the crystalline structure for temperatures between 1100 and 1300 K. Also, experimental measurements of the Gibbs energy of coke relative to graphite are reported. These measurements were obtained using a solid state electrochemical technique. A stabiliy of approximately 900 J g-1, relative to graphite, is reported for temperatures between 950 and 1250 K and for a crystallite size La of ˜10 nm. This value is in excellent agreement with the present thermodynamic model. Finally, an open discussion is made on the possible existance of a degraphitization behavior for coke crystallites heat treated above 2585 K. For the carbon/sulfur system, a modeling approach similar to the one developed for the carbon/hydrogen system is used. Approximately 75% of the model parameters of the carbon/hydrogen and carbon/sulfur systems are common to the two models. Predictive desulfurization curves using the current thermodynamic model are presented for temperatures above 1500 K. A very good agreement is obtained between the model calculations and the reported experimental data. Most of the sulfur content of coke crystallites is predicted to leave the crystallites for temperatures between 1600 and 1850 K. This temperature range is very similar to the puffing temperatures typically found during the desulfurization of petrochemical cokes. The good precision of the model for both studied systems (carbon/sulfur and carbon/hydrogen) combined with the transferability of the model parameters between the carbon/hydrogen and carbon/sulfur systems tend to validate the global approach developed so far.

Native Cellulose: Structure, Characterization and Thermal Properties

PubMed Central

Poletto, Matheus; Ornaghi Júnior, Heitor L.; Zattera, Ademir J.

2014-01-01

In this work, the relationship between cellulose crystallinity, the influence of extractive content on lignocellulosic fiber degradation, the correlation between chemical composition and the physical properties of ten types of natural fibers were investigated by FTIR spectroscopy, X-ray diffraction and thermogravimetry techniques. The results showed that higher extractive contents associated with lower crystallinity and lower cellulose crystallite size can accelerate the degradation process and reduce the thermal stability of the lignocellulosic fibers studied. On the other hand, the thermal decomposition of natural fibers is shifted to higher temperatures with increasing the cellulose crystallinity and crystallite size. These results indicated that the cellulose crystallite size affects the thermal degradation temperature of natural fibers. This study showed that through the methods used, previous information about the structure and properties of lignocellulosic fibers can be obtained before use in composite formulations. PMID:28788179

Magnetic properties of M0.3Fe2.7O4 (M = Fe, Zn and Mn) ferrites nanoparticles

NASA Astrophysics Data System (ADS)

Modaresi, Nahid; Afzalzadeh, Reza; Aslibeiki, Bagher; Kameli, Parviz

2018-06-01

In the present article a comparative study on the structural and magnetic properties of nano-sized M0.3Fe0.7Fe2O4 (M = Fe, Zn and Mn) ferrites have been reported. The X-ray diffraction (XRD) patterns show that the crystallite size depends on the cation distribution. The Rietveld refinement of XRD patterns using MAUD software determines the distribution of cations and unit cell dimensions. The magnetic measurements show that the maximum and minimum value of saturation magnetization is obtained for Zn and Mn doped samples, respectively. The peak temperature of AC magnetic susceptibility of Zn and Fe doped samples below 300 K shows the superparamagnetic behavior in these samples at room temperature. the AC susceptibility results confirm the presence of strong interactions between the nanoparticles which leads to a superspin glass state in the samples at low temperatures.

Polymorphism influences singlet fission rates in tetracene thin films

DOE PAGES

Arias, Dylan H.; Ryerson, Joseph L.; Cook, Jasper D.; ...

2015-11-06

Here, we report the effect of crystal structure and crystallite grain size on singlet fission (SF) in polycrystalline tetracene, one of the most widely studied SF and organic semiconductor materials. SF has been comprehensively studied in one polymoprh (Tc I), but not in the other, less stable polymorph (Tc II). Using carefully controlled thermal evaporation deposition conditions and high sensitivity ultrafast transient absorption spectroscopy, we found that for large crystallite size samples, SF in nearly pure Tc II films is significantly faster than SF in Tc I films. We also discovered that crystallite size has a minimal impact on themore » SF rate in Tc II films, but a significant influence in Tc I films. Large crystallites exhibit SF times of 125 ps and 22 ps in Tc I and Tc II, respectively, whereas small crystallites have SF times of 31 ps and 33 ps. Our results demonstrate first, that attention must be paid to polymorphism in obtaining a self-consistent rate picture for SF in tetracene and second, that control of polymorphism can play a significant role towards achieving a mechanistic understanding of SF in polycrystalline systems. In this latter context we show that conventional theory based on non-covalent tetracene couplings is insufficient, thus highlighting the need for models that capture the delocalized and highly mobile nature of excited states in elucidating the full photophysical picture.« less

Demagnetizing fields of crystallites and a method for measuring the thermodynamic fields of quasi-single-crystal and polycrystalline thin YBa{sub 2}Cu{sub 3}O{sub 7-x} disks

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

Rostami, Kh. R.

The role of the demagnetizing fields of crystallites in HTSC samples is studied. An increase in the crystallite size is shown to suppress the intra-and intercrystalline critical currents of the sample in lower fields. The demagnetizing fields of crystallites are shown to be one of the main causes of the fact that the Bean model is invalid for HTSC samples. A method is proposed to measure the thermodynamic field of a superconductor; this method allows the first thermodynamic critical magnetic fields of the sample and its crystallites and 'subcrystallites' to be measured with a high accuracy. The first thermodynamic criticalmore » magnetic fields are used to estimate the critical current density J{sub c} of the sample, crystallites, and subcrystallites.« less

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

Garcia-Mateo, Carlos, E-mail: cgm@cenim.csic.es

Since the major strengthening mechanisms in nanocrystalline bainitic steels arise from the exceptionally small size of the bainitc ferrite plate, accurate determination of this parameter is fundamental for quantitative relating the microstructure to the mechanical properties. In this work, the thickness of the bainitic ferrite subunits obtained by different bainitic heat treatments was determined in two steels, with carbon contents of 0.3 and 0.7 wt.%, from SEM and TEM micrographs. As these measurements were made on 2D images taken from random sections, the method includes some stereological correction factors to obtain accurate information. Finally, the determined thicknesses of bainitic ferritemore » plates were compared with the crystallite size calculated from the analysis of X-ray diffraction peak broadening. Although in some case the values obtained for crystallite size and plate thickness can be similar, this study confirms that indeed they are two different parameters. - Highlights: •Bainitic microstructure in a nanostructured and sub-micron steel •Bainitic ferrite plate thickness measured by SEM and TEM •Crystallite size determined by X-ray analysis.« less

Study on the corrosion properties of nanocrystalline nickel electrodepositied by reverse pulse current

NASA Astrophysics Data System (ADS)

Cheng, Wen; Ge, Wen; Yang, Qian; Qu, Xinxin

2013-07-01

Nanocrystalline nickel coatings were produced by the method of reverse pulse electrodepositing on the surface of steel sheets. The crystallite size of nanocrystalline nickel coatings was determined by X-ray diffraction (XRD). The effect of saccharin concentration on the crystallite size of the coatings was studied. The average crystallite sizes were diminished as a result of increasing saccharin concentration. CHI660C electrochemical workstation was used to determine the Tafel polarization curves and electrochemical impedance spectroscopy (EIS) of the coatings. The value of corrosion potential, natural corrosion current density, polarizaiton resistance and impedance was calculated, the results suggested that smaller grain size led to higher polarization resistance. EIS gave the charge transfer resistance Rct and pore resistance Rpo variation trend from beginning to 30 min. Scanning electron microscopy (SEM) examination showed the surface morphology of the nickel coatings after the neutral salt spray (NSS) test or bathing in 10% HCl. The images indicated that the corrosion behavior of nanocrystalline nickel coatings was pitting corrosion, the mechanism was also discussed.

Elucidation of structural, vibrational and dielectric properties of transition metal (Co2+) doped spinel Mg-Zn chromites

NASA Astrophysics Data System (ADS)

Choudhary, Pankaj; Varshney, Dinesh

2018-05-01

Co2+ doped Mg-Zn spinel chromite compositions Mg0.5Zn0.5-xCoxCr2O4 (0.0 ≤ x ≤ 0.5) have been synthesized by the high-temperature solid state method. Synchrotron and X-ray diffraction (XRD) studies show single-phase crystalline nature. The structural analysis is validated by Rietveld refinement confirms the cubic structure with space group Fd3m. Crystallite size is estimated from Synchrotron XRD which was found to be 30-34 nm. Energy dispersive analysis confirms stoichiometric Mg0.5Zn0.5-xCoxCr2O4 composition. Average crystallite size distribution is estimated from imaging software (Image - J) of SEM is in the range of 100-250 nm. Raman spectroscopy reveals four active phonon modes, and a pronounced red shift is due to enhanced Co2+ concentration. Increased Co2+ concentration in Mg-Zn chromites shows a prominent narrowing of band gap from 3.46 to 2.97 eV. The dielectric response is attributed to the interfacial polarization, and the electrical modulus study supports non-Debye type of dielectric relaxation. Ohmic junctions (minimum potential drop) at electrode interface are active at lower levels of doping (x < 0.2) give rise to a low-frequency semicircle as evidenced from the complex impedance analysis. The low dielectric loss and high ac conductivity of Co2+ doped Mg-Zn spinel chromites are suitable for power transformer applications at high frequencies.

Magnesium-ion battery-relevant electrochemistry of MgMn 2O 4: crystallite size effects and the notable role of electrolyte water content

DOE PAGES

Yin, Jiefu; Brady, Alexander B.; Takeuchi, Esther S.; ...

2017-03-06

MgMn 2O 4 nanoparticles with crystallite sizes of 11 (MMO-1) and 31 nm (MMO-2) were synthesized and their magnesium-ion battery-relevant electrochemistry was investigated. Here, MMO-1 delivered an initial capacity of 220 mA h g –1 (678 mW h g –1). Electrolyte water content had a profound effect on cycle retention.

Structural properties and gas sensing behavior of sol-gel grown nanostructured zinc oxide

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

Rajyaguru, Bhargav; Gadani, Keval; Kansara, S. B.

2016-05-06

In this communication, we report the results of the studies on structural properties and gas sensing behavior of nanostructured ZnO grown using acetone precursor based modified sol-gel technique. Final product of ZnO was sintered at different temperatures to vary the crystallite size while their structural properties have been studied using X-ray diffraction (XRD) measurement performed at room temperature. XRD results suggest the single phasic nature of all the samples and crystallite size increases from 11.53 to 20.96 nm with increase in sintering temperature. Gas sensing behavior has been studied for acetone gas which indicates that lower sintered samples are moremore » capable to sense the acetone gas and related mechanism has been discussed in the light of crystallite size, crystal boundary density, defect mechanism and possible chemical reaction between gas traces and various oxygen species.« less

Hydrothermal synthesis and magnetic properties of Mn doped ZnS nanoparticles

NASA Astrophysics Data System (ADS)

Rashad, M. M.; Rayan, D. A.; El-Barawy, K.

2010-01-01

Nanocrystallite Mn doped Zn1-XS (X = 0 to 0.4) powders have been synthesized through a hydrothermal route. The effect of the hydrothermal temperature and Mn2+ ions substitution on the crystal structure, crystallite size, microstructure and magnetic properties were investigated using (XRD), (SEM) and (VSM). The results revealed that wurtzite zinc sulfide phase was formed using thiourea as a sulfur source at temperature 150- 200oC for 24 h. The crystallite size was (7.9-15.1 nm) was obtained at the same conditions. The doping of Mn2+ ions decreased the crystallite size of the formed ZnS wurtzite phase was in the range between 7.9 and 3.8 nm. SEM micrographs showed that the produced ZnS and Mn doped ZnS particles were appeared as spherical shape. The magnetic properties were improved by substitution of Mn2+ ions up to 0.2.

Control of crystallite and particle size in the synthesis of layered double hydroxides: Macromolecular insights and a complementary modeling tool.

PubMed

Galvão, Tiago L P; Neves, Cristina S; Caetano, Ana P F; Maia, Frederico; Mata, Diogo; Malheiro, Eliana; Ferreira, Maria J; Bastos, Alexandre C; Salak, Andrei N; Gomes, José R B; Tedim, João; Ferreira, Mário G S

2016-04-15

Zinc-aluminum layered double hydroxides with nitrate intercalated (Zn(n)Al-NO3, n=Zn/Al) is an intermediate material for the intercalation of different functional molecules used in a wide range of industrial applications. The synthesis of Zn(2)Al-NO3 was investigated considering the time and temperature of hydrothermal treatment. By examining the crystallite size in two different directions, hydrodynamic particle size, morphology, crystal structure and chemical species in solution, it was possible to understand the crystallization and dissolution processes involved in the mechanisms of crystallite and particle growth. In addition, hydrogeochemical modeling rendered insights on the speciation of different metal cations in solution. Therefore, this tool can be a promising solution to model and optimize the synthesis of layered double hydroxide-based materials for industrial applications. Copyright © 2016 Elsevier Inc. All rights reserved.

Efficient perovskite light-emitting diodes featuring nanometre-sized crystallites

NASA Astrophysics Data System (ADS)

Xiao, Zhengguo; Kerner, Ross A.; Zhao, Lianfeng; Tran, Nhu L.; Lee, Kyung Min; Koh, Tae-Wook; Scholes, Gregory D.; Rand, Barry P.

2017-01-01

Organic-inorganic hybrid perovskite materials are emerging as highly attractive semiconductors for use in optoelectronics. In addition to their use in photovoltaics, perovskites are promising for realizing light-emitting diodes (LEDs) due to their high colour purity, low non-radiative recombination rates and tunable bandgap. Here, we report highly efficient perovskite LEDs enabled through the formation of self-assembled, nanometre-sized crystallites. Large-group ammonium halides added to the perovskite precursor solution act as a surfactant that dramatically constrains the growth of 3D perovskite grains during film forming, producing crystallites with dimensions as small as 10 nm and film roughness of less than 1 nm. Coating these nanometre-sized perovskite grains with longer-chain organic cations yields highly efficient emitters, resulting in LEDs that operate with external quantum efficiencies of 10.4% for the methylammonium lead iodide system and 9.3% for the methylammonium lead bromide system, with significantly improved shelf and operational stability.

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.

Crystal growth in zinc borosilicate glasses

NASA Astrophysics Data System (ADS)

Kullberg, Ana T. G.; Lopes, Andreia A. S.; Veiga, João P. B.; Monteiro, Regina C. C.

2017-01-01

Glass samples with a molar composition (64+x)ZnO-(16-x)B2O3-20SiO2, where x=0 or 1, were successfully synthesized using a melt-quenching technique. Based on differential thermal analysis data, the produced glass samples were submitted to controlled heat-treatments at selected temperatures (610, 615 and 620 °C) during various times ranging from 8 to 30 h. The crystallization of willemite (Zn2SiO4) within the glass matrix was confirmed by means of X-ray diffraction (XRD) and scanning electron microscopy (SEM). Under specific heat-treatment conditions, transparent nanocomposite glass-ceramics were obtained, as confirmed by UV-vis spectroscopy. The influence of temperature, holding time and glass composition on crystal growth was investigated. The mean crystallite size was determined by image analysis on SEM micrographs. The results indicated an increase on the crystallite size and density with time and temperature. The change of crystallite size with time for the heat-treatments at 615 and 620 °C depended on the glass composition. Under fixed heat-treatment conditions, the crystallite density was comparatively higher for the glass composition with higher ZnO content.

Structure and mechanical properties of foils made of nanocrystalline beryllium

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

Zhigalina, O. M., E-mail: zhigal@ns.crys.ras.ru; Semenov, A. A.; Zabrodin, A. V.

2016-07-15

The phase composition and structural features of (45–90)-μm-thick foils obtained from nanocrystalline beryllium during multistep thermomechanical treatment have been established using electron microscopy, electron diffraction, electron backscattering diffraction, and energy-dispersive analysis. This treatment is shown to lead to the formation of a structure with micrometer- and submicrometer-sized grains. The minimum average size of beryllium grains is 352 nm. The inclusions of beryllium oxide (BeO) of different modifications with tetragonal (sp. gr. P4{sub 2}/mnm) and hexagonal (sp. gr. P6{sub 3}/mmc) lattices are partly ground during deformation to a size smaller than 100 nm and are located along beryllium grain boundaries inmore » their volume, significantly hindering migration during treatment. The revealed structural features of foils with submicrometer-sized crystallites provide the thermal stability of their structural state. Beryllium with this structure is a promising material for X-ray instrument engineering and for the production of ultrathin (less than 10 μm) vacuum-dense foils with very high physicomechanical characteristics.« less

Reciprocal-space mapping of epitaxic thin films with crystallite size and shape polydispersity.

PubMed

Boulle, A; Conchon, F; Guinebretière, R

2006-01-01

A development is presented that allows the simulation of reciprocal-space maps (RSMs) of epitaxic thin films exhibiting fluctuations in the size and shape of the crystalline domains over which diffraction is coherent (crystallites). Three different crystallite shapes are studied, namely parallelepipeds, trigonal prisms and hexagonal prisms. For each shape, two cases are considered. Firstly, the overall size is allowed to vary but with a fixed thickness/width ratio. Secondly, the thickness and width are allowed to vary independently. The calculations are performed assuming three different size probability density functions: the normal distribution, the lognormal distribution and a general histogram distribution. In all cases considered, the computation of the RSM only requires a two-dimensional Fourier integral and the integrand has a simple analytical expression, i.e. there is no significant increase in computing times by taking size and shape fluctuations into account. The approach presented is compatible with most lattice disorder models (dislocations, inclusions, mosaicity, ...) and allows a straightforward account of the instrumental resolution. The applicability of the model is illustrated with the case of an yttria-stabilized zirconia film grown on sapphire.

Synthesis and characterization of nanocrystalline mesoporous zirconia using supercritical drying.

PubMed

Tyagi, Beena; Sidhpuria, Kalpesh; Shaik, Basha; Jasra, Raksh Vir

2006-06-01

Synthesis of nano-crystalline zirconia aerogel was done by sol-gel technique and supercritical drying using n-propanol solvent at and above supercritical temperature (235-280 degrees C) and pressure (48-52 bar) of n-propanol. Zirconia xerogel samples have also been prepared by conventional thermal drying method to compare with the super critically dried samples. Crystalline phase, crystallite size, surface area, pore volume, and pore size distribution were determined for all the samples in detail to understand the effect of gel drying methods on these properties. Supercritical drying of zirconia gel was observed to give thermally stable, nano-crystalline, tetragonal zirconia aerogels having high specific surface area and porosity with narrow and uniform pore size distribution as compared to thermally dried zirconia. With supercritical drying, zirconia samples show the formation of only mesopores whereas in thermally dried samples, substantial amount of micropores are observed along with mesopores. The samples prepared using supercritical drying yield nano-crystalline zirconia with smaller crystallite size (4-6 nm) as compared to higher crystallite size (13-20 nm) observed with thermally dried zirconia.

Synthesis and structural characterization of transition metal doped MgO: Mg0.95Mn0.01TM0.04O (TM = Co, Ni, Cu)

NASA Astrophysics Data System (ADS)

Islam, Ishtihadah; Khandy, Shakeel Ahmad; Hafiz, Aurangzeb Khurram

2018-05-01

In the present work, preparation and characterization of transition metal doped MgO: Zn0.94Mn0.01TM0.05O (TM = Co, Ni and Cu) nano-particles have been reported. Transition metal doped samples of MgO were synthesized by Sol gel auto combustion method. Structural characterisation from XRD and SEM show the formation of single-phase primary particles, nearly of spherical shaped nano-crystallites. The crystallite size was found to be 78.2, 67.02, 78.11 and 64 nm for pure, Co, Cu and Ni doped MgMnO nano-particles, respectively. Hence, the average crystallite size increases monotonously from Co to Cu doping.

Effect of X-ray Line Spectra Profile Fitting with Pearson VII, Pseudo-Voigt and Generalized Fermi Functions on Asphalt Binder Aromaticity and Crystallite Parameters

NASA Astrophysics Data System (ADS)

Gebresellasie, K.; Shirokoff, J.; Lewis, J. C.

2012-12-01

X-ray line spectra profile fitting using Pearson VII, pseudo-Voigt and generalized Fermi functions was performed on asphalt binders prior to the calculation of aromaticity and crystallite size parameters. The effects of these functions on the results are presented and discussed in terms of the peak profile fit parameters, the uncertainties in calculated values that can arise owing to peak shape, peak features in the pattern and crystallite size according to the asphalt models (Yen, modified Yen or Yen-Mullins) and theories. Interpretation of these results is important in terms of evaluating the performance of asphalt binders widely used in the application of transportation systems (roads, highways, airports).

Molecular dynamics modeling of PPTA crystallite mechanical properties in the presence of defects

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

Mercer, Brian; Zywicz, Edward; Papadopoulos, Panayiotis

Here, the mechanical properties of PPTA crystallites, the fundamental building blocks of aramid polymer fibers such as Kevlar® and Twaron®, are studied here using molecular dynamics simulations. The ReaxFF interatomic potential is employed to study crystallite failure via covalent and hydrogen bond rupture in constant strain-rate tensile loading simulations. Emphasis is placed on analyzing how chain-end defects in the crystallite influence its mechanical response and fracture strength. Chain-end defects are found to affect the behavior of nearby chains in a region of the PPTA crystallite that is small relative to the typical crystallite size in manufactured aramid fibers. The centralmore » Csingle bondN bond along the backbone chain is identified as the weakest in the PPTA polymer chain backbone in dynamic strain-to-failure simulations of the crystallite. It is found that clustering of chain-ends leads to reduced crystallite strength and crystallite failure via hydrogen bond rupture and chain sliding, whereas randomly scattered defects impact the strength less and failure is by covalent bond rupture and chain scission. The axial crystallite modulus increases with increasing chain length and is independent of chain-end defect locations. On the basis of these findings, a theoretical model is proposed to predict the axial modulus as a function of chain length.« less

Molecular dynamics modeling of PPTA crystallite mechanical properties in the presence of defects

DOE PAGES

Mercer, Brian; Zywicz, Edward; Papadopoulos, Panayiotis

2017-03-11

Here, the mechanical properties of PPTA crystallites, the fundamental building blocks of aramid polymer fibers such as Kevlar® and Twaron®, are studied here using molecular dynamics simulations. The ReaxFF interatomic potential is employed to study crystallite failure via covalent and hydrogen bond rupture in constant strain-rate tensile loading simulations. Emphasis is placed on analyzing how chain-end defects in the crystallite influence its mechanical response and fracture strength. Chain-end defects are found to affect the behavior of nearby chains in a region of the PPTA crystallite that is small relative to the typical crystallite size in manufactured aramid fibers. The centralmore » Csingle bondN bond along the backbone chain is identified as the weakest in the PPTA polymer chain backbone in dynamic strain-to-failure simulations of the crystallite. It is found that clustering of chain-ends leads to reduced crystallite strength and crystallite failure via hydrogen bond rupture and chain sliding, whereas randomly scattered defects impact the strength less and failure is by covalent bond rupture and chain scission. The axial crystallite modulus increases with increasing chain length and is independent of chain-end defect locations. On the basis of these findings, a theoretical model is proposed to predict the axial modulus as a function of chain length.« less

Neodymium cobalt oxide as a chemical sensor

NASA Astrophysics Data System (ADS)

Abdel-Latif, I. A.; Rahman, Mohammed M.; Khan, Sher Bahadar

2018-03-01

Chemical sensing and electrical transport properties of neodymium coblate, NdCoO3, was investigated in this work. It was prepared by using co-precipitation method. Pure neodymium chloride and cobalt chloride were mixing in the presence of sodium hydroxide and the obtained co-precipitated powder was calcined at 850 and 1000 °C. The synthesized composites, as-grown (NdCoO3-I), calcined at 850 °C (NdCoO3-II), and calcined at 1000 °C (NdCoO3-III) were studied in details in terms of their morphological and structural properties. The X-ray analysis confirmed that the synthesized products are well crystalline possessing single phase orthorhombic crystal system of space group Pbnm(62). The crystallite size of NdCoO3-I, NdCoO3-II, and NdCoO3-III is 22, 111, and 338 nm, respectively which reflect that crystallite size is increasing with increase in firing temperature. The DC resistivity was measured as a function of temperature in the temperature range from room temperature up to 200 °C. All NdCoO3 are semiconductor in this range of temperature but showed different activation energy which strongly depends on the crystallite size of the products. The activation energy decreased with increase in crystallite size, 0.798, 0.414 and 0.371 eV for NdCoO3-I, NdCoO3-II, and NdCoO3-III, respectively. Thus resistivity increases with increase in crystallite size of NdCoO3. All NdCoO3 products were tested as chemical sensor for acetone by electrochemical approaches and showed excellent sensitivity. Among the NdCoO3 samples, NdCoO3-III showed the highest sensitivity (3.4722 μAcm-2 mM-1) compared to other compositions and gradually decreased to 3.2407 μAcm-2 mM-1 with decreasing the crystallite size of NdCoO3-II. It is also observed that the sensitivity drastically decreased to 0.76253 μAcm-2 mM-1 in the case of NdCoO3-I. It is introduced an efficient route for the detection of environmental unsafe chemicals by electrochemical approach for the safety of healthcare and environmental fields in broad scales.

Impact of crystalline defects and size on X-ray line broadening: A phenomenological approach for tetragonal SnO{sub 2} nanocrystals

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

Muhammed Shafi, P.; Chandra Bose, A., E-mail: acbose@nitt.edu

2015-05-15

Nanocrystalline tin oxide (SnO{sub 2}) powders with different grain size were prepared by chemical precipitation method. The reaction was carried out by varying the period of hydrolysis and the as-prepared samples were annealed at different temperatures. The samples were characterized using X-ray powder diffractometer and transmission electron microscopy. The microstrain and crystallite size were calculated for all the samples by using Williamson-Hall (W-H) models namely, isotropic strain model (ISM), anisotropic strain model (ASM) and uniform deformation energy density model (UDEDM). The morphology and particle size were determined using TEM micrographs. The directional dependant young’s modulus was modified as an equationmore » relating elastic compliances (s{sub ij}) and Miller indices of the lattice plane (hkl) for tetragonal crystal system and also the equation for elastic compliance in terms of stiffness constants was derived. The changes in crystallite size and microstrain due to lattice defects were observed while varying the hydrolysis time and the annealing temperature. The dependence of crystallite size on lattice strain was studied. The results were correlated with the available studies on electrical properties using impedance spectroscopy.« less

Synthesis of strontium substituted barium titanate nanoparticles by mechanical alloying and high power ultrasonication destruction

NASA Astrophysics Data System (ADS)

Yustanti, Erlina; Hafizah, Mas Ayu Elita; Manaf, Azwar

2016-04-01

This paper reports the particle and crystallite size characterizations of mechanically alloyed Ba(1-x)SrxTiO3 (BST) with x = 0.3 and 0.7 prepared with the assistance of a high-power sonicator. Analytical grade BaCO3, TiO2 and SrCO3 precursors with a purity of greater than 99 wt.% were mixed and milled using a planetary ball mill to a powder weight ratio of 10:1. Powders obtained after 20 hours of milling time were then sintered at 1200°C for 4 hours to form crystalline powders.These powders were further treated ultrasonically under a fixed 6.7 gr/l particle concentration in demineralized water for 1, 3, 5, 7 hours and a fixed ultrasonic irradiation time of 1 hour to the dispersion of 6.7; 20; 33.3 gr/l concentrations. As to the results of crystallite size characterization, it is demonstrated that the mean crystallite size of BST with x = 0.3 and 0.7 undergo a slight change after the first 1 hour irradiation time and then remain almost unchanged. This was in contrary to the particle size in which the mean particle size of BST with x = 0.3 increased from 765 nm to 1405 nm after 7 hours irradiation time, while that of x = 0.7 increased from 505 nm to 1298 nm after 3 hours and then reduced back to the initial size after 7 hours ultra sonication time. The increase in particle size was due to large of cohesive forces among fine particles. It is also demonstrated that the concentration of particles in a dispersion with anionic surfactant do not effective to reduce the particle sizes ultrasonically. Nanoparticles with the mean size respectively 40 and 10 times larger than their respective crystallite size were successfully obtained respectively in x = 0.3 and x = 0.7.

Synthesis of strontium substituted barium titanate nanoparticles by mechanical alloying and high power ultrasonication destruction

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

Yustanti, Erlina, E-mail: erlina.yustanti@ui.ac.id; Department of Metallurgy, Faculty of Engineering University of Sultan AgengTirtayasa Jl. Jenderal Sudirman KM 03 Cilegon-Banten 65134; Hafizah, Mas Ayu Elita, E-mail: kemasayu@yahoo.com

2016-04-19

This paper reports the particle and crystallite size characterizations of mechanically alloyed Ba{sub (1-x)}Sr{sub x}TiO{sub 3} (BST) with x = 0.3 and 0.7 prepared with the assistance of a high-power sonicator. Analytical grade BaCO{sub 3}, TiO{sub 2} and SrCO{sub 3} precursors with a purity of greater than 99 wt.% were mixed and milled using a planetary ball mill to a powder weight ratio of 10:1. Powders obtained after 20 hours of milling time were then sintered at 1200°C for 4 hours to form crystalline powders.These powders were further treated ultrasonically under a fixed 6.7 gr/l particle concentration in demineralized watermore » for 1, 3, 5, 7 hours and a fixed ultrasonic irradiation time of 1 hour to the dispersion of 6.7; 20; 33.3 gr/l concentrations. As to the results of crystallite size characterization, it is demonstrated that the mean crystallite size of BST with x = 0.3 and 0.7 undergo a slight change after the first 1 hour irradiation time and then remain almost unchanged. This was in contrary to the particle size in which the mean particle size of BST with x = 0.3 increased from 765 nm to 1405 nm after 7 hours irradiation time, while that of x = 0.7 increased from 505 nm to 1298 nm after 3 hours and then reduced back to the initial size after 7 hours ultra sonication time. The increase in particle size was due to large of cohesive forces among fine particles. It is also demonstrated that the concentration of particles in a dispersion with anionic surfactant do not effective to reduce the particle sizes ultrasonically. Nanoparticles with the mean size respectively 40 and 10 times larger than their respective crystallite size were successfully obtained respectively in x = 0.3 and x = 0.7.« less

Crystallinity of the epitaxial heterojunction of C60 on single crystal pentacene

NASA Astrophysics Data System (ADS)

Tsuruta, Ryohei; Mizuno, Yuta; Hosokai, Takuya; Koganezawa, Tomoyuki; Ishii, Hisao; Nakayama, Yasuo

2017-06-01

The structure of pn heterojunctions is an important subject in the field of organic semiconductor devices. In this work, the crystallinity of an epitaxial pn heterojunction of C60 on single crystal pentacene is investigated by non-contact mode atomic force microscopy and high-resolution grazing incidence x-ray diffraction. Analysis shows that the C60 molecules assemble into grains consisting of single crystallites on the pentacene single crystal surface. The in-plane mean crystallite size exceeds 0.1 μm, which is at least five time larger than the size of crystallites deposited onto polycrystalline pentacene thin films grown on SiO2. The results indicate that improvement in the crystal quality of the underlying molecular substrate leads to drastic promotion of the crystallinity at the organic semiconductor heterojunction.

Anomalous behavior of B{sub 1g} mode in highly transparent anatase nano-crystalline Nb-doped Titanium Dioxide (NTO) thin films

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

Gautam, Subodh K., E-mail: subodhkgtm@gmail.com, E-mail: fouran@gmail.com; Ojha, S.; Singh, Fouran, E-mail: subodhkgtm@gmail.com, E-mail: fouran@gmail.com

2015-12-15

The effect of Niobium doping and size of crystallites on highly transparent nano-crystalline Niobium doped Titanium Dioxide (NTO) thin films with stable anatase phase are reported. The Nb doping concentration is varied within the solubility limit in TiO{sub 2} lattice. Films were annealed in controlled environment for improving the crystallinity and size of crystallites. Elemental and thickness analysis were carried out using Rutherford backscattering spectrometry and cross sectional field emission scanning electron microscopy. Structural characteristics reveal a substitutional incorporation of Nb{sup +5} in the TiO{sub 2} lattice which inhibits the anatase crystallites growth with increasing the doping percentage. The micro-Ramanmore » (MR) spectra of films with small size crystallites shows stiffening of about 4 cm{sup −1} for the E{sub g(1)} mode and is ascribed to phonon confinement and non-stoichiometry. In contrast, B{sub 1g} mode exhibits a large anomalous softening of 20 cm{sup −1} with asymmetrical broadening; which was not reported for the case of pure TiO{sub 2} crystallites. This anomalous behaviour is explained by contraction of the apical Ti-O bonds at the surface upon substitutional Nb{sup 5+} doping induced reduction of Ti{sup 4+} ions also known as hetero-coordination effect. The proposed hypotheses is manifested through studying the electronic structure and phonon dynamics by performing the near edge x-ray absorption fine structure (NEXAFS) and temperature dependent MR down to liquid nitrogen temperature on pure and 2.5 at.% doped NTO films, respectively.« less

Protein-free formation of bone-like apatite: New insights into the key role of carbonation

PubMed Central

Deymier, Alix C.; Nair, Arun K.; Depalle, Baptiste; Qin, Zhao; Arcot, Kashyap; Drouet, Christophe; Yoder, Claude H.; Buehler, Markus J.; Thomopoulos, Stavros; Genin, Guy M.; Pasteris, Jill D.

2017-01-01

The nanometer-sized plate-like morphology of bone mineral is necessary for proper bone mechanics and physiology. However, mechanisms regulating the morphology of these mineral nanocrystals remain unclear. The dominant hypothesis attributes the size and shape regulation to organic-mineral interactions. Here, we present data supporting the hypothesis that physicochemical effects of carbonate integration within the apatite lattice control the morphology, size, and mechanics of bioapatite mineral crystals. Carbonated apatites synthesized in the absence of organic molecules presented plate-like morphologies and nanoscale crystallite dimensions. Experimentally-determined crystallite size, lattice spacing, solubility and atomic order were modified by carbonate concentration. Molecular dynamics (MD) simulations and density functional theory (DFT) calculations predicted changes in surface energy and elastic moduli with carbonate concentration. Combining these results with a scaling law predicted the experimentally observed scaling of size and energetics with carbonate concentration. The experiments and models describe a clear mechanism by which crystal dimensions are controlled by carbonate substitution. Furthermore, the results demonstrate that carbonate substitution is sufficient to drive the formation of bone-like crystallites. This new understanding points to pathways for biomimetic synthesis of novel, nanostructured biomaterials. PMID:28279923

On the Nature of Disorder in Solid 4He

NASA Astrophysics Data System (ADS)

Krainyukova, N. V.

2010-02-01

We apply a modified Debye approach to calculate the Gibbs free energy for different structural phases and crystallite sizes in 4He. Atoms are assumed to interact via the Aziz potential. We have found that some intermediate (between hcp and bcc) phase predicted previously is more favorable than hcp at low temperatures and for small sizes. We show that it can exist in a wide pressure range up to 60 bar in 4He for crystallite sizes about 3,000 atoms. For larger sizes (10,000 atoms or more) this phase becomes unfavorable. In multidomain structures the intermediate phase competes with hcp and metastable fcc that can be a reason for disorder in solid 4He.

Strain and grain size of TiO2 nanoparticles from TEM, Raman spectroscopy and XRD: The revisiting of the Williamson-Hall plot method

NASA Astrophysics Data System (ADS)

Kibasomba, Pierre M.; Dhlamini, Simon; Maaza, Malik; Liu, Chuan-Pu; Rashad, Mohamed M.; Rayan, Diaa A.; Mwakikunga, Bonex W.

2018-06-01

The Williamson-Hall (W-H) equation, which has been used to obtain relative crystallite sizes and strains between samples since 1962, is revisited. A modified W-H equation is derived which takes into account the Scherrer equation, first published in 1918, (which traditionally gives more absolute crystallite size prediction) and strain prediction from Raman spectra. It is found that W-H crystallite sizes are on average 2.11 ± 0.01 times smaller than the sizes from Scherrer equation. Furthermore the strain from the W-H plots when compared to strain obtained from Raman spectral red-shifts yield factors whose values depend on the phases in the materials - whether anatase, rutile or brookite. Two main phases are identified in the annealing temperatures (350 °C-700 °C) chosen herein - anatase and brookite. A transition temperature of 550 °C has been found for nano-TiO2 to irreversibly transform from brookite to anatase by plotting the Raman peak shifts against the annealing temperatures. The W-H underestimation on the strain in the brookite phase gives W-H/Raman factor of 3.10 ± 0.05 whereas for the anatase phase, one gets 2.46 ± 0.03. The new βtot2cos2θ-sinθ plot and when fitted with a polynomial yield less strain but much better matching with experimental TEM crystallite sizes and the agglomerates than both the traditional Williamson-Hall and the Scherrer methods. There is greater improvement in the model when linearized - that is the βtotcos2θ-sinθ plot rather than the βtot2cos2θ-sinθ plot.

XRD analysis of undoped and Fe doped TiO{sub 2} nanoparticles by Williamson Hall method

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

Bharti, Bandna; Barman, P. B.; Kumar, Rajesh, E-mail: rajesh.kumar@juit.ac.in

2015-08-28

Undoped and Fe doped titanium dioxide (TiO{sub 2}) nanoparticles were synthesized by sol-gel method at room temperature. The synthesized samples were annealed at 500°C. For structural analysis, the prepared samples were characterized by X-ray diffraction (XRD). The crystallite size of TiO{sub 2} and Fe doped TiO{sub 2} nanoparticles were calculated by Scherer’s formula, and was found to be 15 nm and 11 nm, respectively. Reduction in crystallite size of TiO{sub 2} with Fe doping was observed. The anatase phase of Fe-doped TiO{sub 2} nanoparticles was also confirmed by X-ray diffraction. By using Williamson-Hall method, lattice strain and crystallite size weremore » also calculated. Williamson–Hall plot indicates the presence of compressive strain for TiO{sub 2} and tensile strain for Fe-TiO{sub 2} nanoparticles annealed at 500°C.« less

Influence of the hydrothermal temperature and pH on the crystallinity of a sputtered hydroxyapatite film

NASA Astrophysics Data System (ADS)

Ozeki, K.; Aoki, H.; Masuzawa, T.

2010-09-01

Hydroxyapatite (HA) was coated onto titanium substrates using radio frequency sputtering, and the sputtered films were crystallized under hydrothermal conditions at 110-170 °C at pH values of 7.0 and 9.5. The crystallite size, the remnant film thickness, and the surface morphology of the films were observed using X-ray diffraction, energy dispersive X-ray spectroscopy, and scanning electron microscopy, respectively. The crystallite size increased with the process temperature, and reached 123.6 nm (pH 9.5 and 170 °C) after 24 h. All of the crystallite sizes of the film treated at pH 9.5 were higher than those treated at pH 7.0 at each process temperature. The film treated at pH 9.5 retained more than 90% of the initial film thickness at any process temperature. The ratio of the film treated at pH 7.0 did not reached 90% at less than 150 °C, and tended to increase with the process temperature.

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

Pratapa, S.; Susanti, L.; Insany, Y. A. S.

Simple coprecipitation method has been used to produce nanoparticles of MgO (magnesia), MgO{center_dot}Al{sub 2}O{sub 3}(spinel), Y{sub 2}O{sub 3}(yttria) and Fe{sub 3}O{sub 4}(ferrite). The raw materials were, in respective, magnesium powder, magnesium and aluminium powders, ytrria powder, and natural sand. The coprecipitation included the use of suitable acid and base to dissolve the powders or sand and to produce precipitates, as well as the use of water to wash and purify the precipitates, and drying at relatively low temperatures, namely lower than 100 deg. C, followed by heating at 450 deg. C, 750 deg. C, 600 deg. C and 200 deg.more » C to produce magnesia, spinel, yttria and ferrite nanopowders, respectively. X-ray diffractometry was used to characterise the purity and nanocrystallinity of the final powders. It was found qualitatively that the powders were of high purity. Further line-broadening analysis using single-line and Rietveld-based softwares was performed to reveal the nanocrystallinity of the powders. Different line breadth values were found for the powders, indicating different crystallite sizes. It was also found that, particularly for spinel and yttria, the diffraction peaks exhibited 'longer' tails, indicating broader crystallite size distribution. The average crystallite size for the powders ranged from 3 to 70 nm. The results could then be used as 'fingerprints' for nanocrystallinity using x-ray diffractometry. The XRD crystallite sizes for yttria and ferrite nanocrystals are in fair agreement with their counterparts from electron microscopy observation.« less

Effect of Cu2+ substitution on the structural, optical and magnetic behaviour ofchemically derived manganese ferrite nanoparticles

NASA Astrophysics Data System (ADS)

Vasuki, G.; Balu, T.

2018-06-01

Mixed spinel copper manganese ferrite (CuXMn1‑XFe2O4, X = 0, 0.25, 0.5, 0.75, 1) nanoparticles were synthesized by chemical co-precipitation technique. From the powder x-ray diffraction analysis the lattice constant, volume of unit cell, x-ray density, hopping lengths, crystallite size, surface area, dislocation density and microstrain were calculated. The substitution of Cu2+ ions shows a considerable reduction in the crystallite size of manganese ferrite from 34 nm to 22 nm. Further a linear fit of Williamson-Hall plot has been drawn to determine the microstrain and crystallite size. The crystallite size and morphology were further observed through high resolution transmission electron microscope and scanning electron microscope. The diffraction rings observed from selected area electron diffraction pattern exhibits the crystalline nature of all the samples. The energy dispersive x-ray analysis shows the composition of all the elements incorporated in the synthesized nanomaterials. FTIR studies reveal the absorption peaks that correspond to the metal-oxygen vibrations in the tetrahedral and octahedral sites. From the UV–vis absorption spectra the band gap energy, refractive index and optical dielectric constant were determined. Magnetic studies carried out using vibrating sample magnetometer shows interesting behaviour in the variation of magnetisation and coercivity. Peculiar magnetic behaviour is observed when Cu2+ ions are substituted in manganese ferrites. All the synthesized materials have very low value of squareness ratio which attributes to the superparamagnetic behaviour.

Synthesis and characterization of nanocrystalline LaMnO3 modified BaTiO3 ferroelectric ceramics prepared by chemical route

NASA Astrophysics Data System (ADS)

Dhak, Prasanta; Adak, Mrinal Kanti; Dhak, Debasis

2016-02-01

Nanocrystalline Ba1-3xTi1-3xLa2xMn4xO3, [x = 0.006, 0.008, 0.01 and 0.05] (abbreviated hereafter as BTLM) by chemical route. The phase formation and purity were checked by X-ray diffraction (XRD) study and transmission electron microscopy (TEM). The grain morphology after sintering was studied by scanning electron microscopy (SEM). The crystallite sizes range from 21 nm to 30 nm, while the particle size ranges between 27 nm and 38 nm. The grain size 212 nm and grain density 96.8% were found to be maximum for BTLM x = 0.05 and x = 0.01, respectively. The temperature dependence of dielectric constants was found to be more diffused and the peak value of the dielectric constant was decreased and more flat with the increase of the substituent concentration. The tangent loss was found to be decreased and reached to the minimum value of 0.032 for BTLM x = 0.05. The remnant polarization Pr, was 10 μC/cm2 for BTLM x = 0.01.

Structural and electromagnetic properties of NiAlxFe2-xO4/SiO2 nanocomposite films deposited using a sol-gel spin-coating method

NASA Astrophysics Data System (ADS)

Wang, Li; Li, Xuejian; Li, Ji; Liu, Mei; Xu, Shichong; Li, Haibo

2017-12-01

NiAlxFe2-xO4/SiO2 (0 ≤ x ≤ 1.0) nanocomposite films deposited on Si(1 0 0) substrates were prepared by a sol-gel spin-coating method. The influences of Al3+ content and annealing temperature on the structural and electromagnetic properties of the nanocomposite films were investigated. The results indicated that NiAlxFe2-xO4 in the nanocomposite films crystallized after annealing at 1073 K and above. When the doping content x increased from 0 to 1.0, the lattice constants and the average crystallite sizes of the NiAlxFe2-xO4 nanoparticles decreased. The saturation magnetization and coercivity of the films were inversely proportional to the Al3+ content. The maximum value of saturation magnetization (361.6 emu/cm3) and the minimum value of coercivity (18.6 kA/m) were obtained for x of 0.2. When the annealing temperature increased from 1073 to 1473 K, the lattice constant and the average crystallite size of the NiAl0.2Fe1.8O4 nanoparticles increased from 0.8322 to 0.8349 nm and 4 to 28 nm, respectively, and the saturation magnetization and coercivity of the films increased from 214.8 to 464.5 emu/cm3 and 8.2 to 26.9 kA/m, respectively. Moreover, the DC resistivity of the films increased with increasing Al3+ content and annealing temperature.

Nanostructure investigation of magnetic nanomaterial Ni{sub 0.5}Zn{sub 0.3}Cu{sub 0.2}Fe{sub 2}O{sub 4} synthesized by sol-gel method

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

Pransisco, Prengki, E-mail: prengkipransisco@gmail.com; Badan Lingkungan Hidup Derah Kabupaten Empat Lawang South of Sumatera; Shafie, Afza, E-mail: afza@petronas.com.my

2015-07-22

Magnetic nanomaterial Ni{sub 0.5}Zn{sub 0.3}Cu{sub 0.2}Fe{sub 2}O{sub 4} was successfully prepared by using sol-gel method. Heat treatment on material is always giving defect on properties of material. This paper investigates the effect of heat treatment on nanostructure of magnetic nanomaterial Ni{sub 0.5}Zn{sub 0.3}Cu{sub 0.2}Fe{sub 2}O{sub 4}. According to thermo gravimetric analysis (TGA) that after 600°C there is no more weight loss detected and it was decided as minimum calcination temperature. Intensity, crystallite size, structure, lattice parameter and d-spacing of the material were investigated by using X-ray diffraction (XRD). High resolution transmission electron microscope (HRTEM) was used to examine nanostructure, nanosize,more » shape and distribution particle of magnetic material Ni{sub 0.5}Zn{sub 0.3}Cu{sub 0.2}Fe{sub 2}O{sub 4} and variable pressure field emission scanning electron microscope (VP-FESEM) was used to investigate the surface morphology and topography of the material. The XRD result shows single-phase cubic spinel structure with average crystallite size in the range of 25.6-95.9 nm, the value of the intensity of the material was increased with increasing temperature, and followed by lattice parameter was increased with increasing calcination temperature, value of d-spacing was relatively decreased with accompanied increasing temperature. From HRTEM result the distribution of particles was tend to be agglomerates with particle size of 7.8-17.68 nm. VP-FESEM result shows that grain size of the material increases with increasing calcination temperature and the surface morphology shows that the material is in hexagonal shape and it was also proved by mapping result which showing the presence each of constituents inside the compound.« less

Preparation and Characterization of Chitosan-coated Fe3O4 Nanoparticles using Ex-Situ Co-Precipitation Method and Tripolyphosphate/Sulphate as Dual Crosslinkers

NASA Astrophysics Data System (ADS)

Wulandari, Ika O.; Mardila, Vita T.; Santjojo, D. J. Djoko H.; Sabarudin, Akhmad

2018-01-01

The unique properties of nanomaterial provide great opportunities to develop in several fields. Several types of nanoparticles have been proven beneficial for biomedical and therapeutic agent development. Particularly for clinical use, nanoparticles must be biocompatible and non-toxic. Iron oxide nanoparticles consist of either magnetite (Fe3O4) or maghemite (γ-Fe2O3) was eligible to use for in vivo application including targeting drug delivery. Due to their distinct properties, these nanoparticles could be directed to the specific target under external magnetic field. However, nanoparticles have a tendency to form agglomeration. Therefore, surface modification was required to reduce the agglomeration. In this study, nanoparticles of Fe3O4 were produced and coated by biomaterial (chitosan) using ex-situ co-precipitation method. Nanoparticles of Fe3O4 were synthesized by adding ammonia water into iron ferric and ferrous solution. Synthesis process of Fe3O4 was conducted prior to adding chitosan. Chitosan was then cross-linked by a combination of tripolyphosphate/sulphate. The different composition ratio and crosslinking time provide the different physical and magnetic characteristics of nanoparticles. Particle and crystallite size was determined by using Scanning Electron Microscopy (SEM) and X-Ray Diffraction (XRD) respectively, whereas magnetic characteristic was determined by Electron Spin Resonance (ESR). The results showed that the ratio enhancement between chitosan: Fe3O4 increase the particle size, while decreased the crystallite size. Morphology and particle size were influenced by the ratio of crosslinkers. It was found that the higher tripolyphosphate content was contributed to the small size and more spherical morphology. In addition, the influence of crosslinking time toward crystallite size was determined by altering stirring time. The longer duration of crosslinking time, provide the larger crystallite size of chitosan-Fe3O4. There was an interesting correlation between particle size and amount of Fe3O4 phase with ESR curve.

Structural changes during milling of aluminum oxide powders

NASA Technical Reports Server (NTRS)

Ziepler, G.

1984-01-01

The mechanical activation of four fused corundum powders and a calcined Al2O3 powder was studied. The milled powders were characterized by their structural properties, crystallite size, and lattice distortions. Structural changes during milling, detected by X-ray line broadening analysis, gave information about the enhanced activity of the powders caused by the lattice distortions and by the decreasing crystallite size during milling. The structural changes during milling, under the same milling conditions, can be quite different for the same ceramic material, but with different characteristics in the as received state.

Growth, characterization and estimation of lattice strain and size in CdS nanoparticles: X-ray peak profile analysis

NASA Astrophysics Data System (ADS)

Solanki, Rekha Garg; Rajaram, Poolla; Bajpai, P. K.

2018-05-01

This work is based on the growth, characterization and estimation of lattice strain and crystallite size in CdS nanoparticles by X-ray peak profile analysis. The CdS nanoparticles were synthesized by a non-aqueous solvothermal method and were characterized by powder X-ray diffraction (XRD), transmission electron microscopy (TEM), Raman and UV-visible spectroscopy. XRD confirms that the CdS nanoparticles have the hexagonal structure. The Williamson-Hall (W-H) method was used to study the X-ray peak profile analysis. The strain-size plot (SSP) was used to study the individual contributions of crystallite size and lattice strain from the X-rays peaks. The physical parameters such as strain, stress and energy density values were calculated using various models namely, isotropic strain model, anisotropic strain model and uniform deformation energy density model. The particle size was estimated from the TEM images to be in the range of 20-40 nm. The Raman spectrum shows the characteristic optical 1LO and 2LO vibrational modes of CdS. UV-visible absorption studies show that the band gap of the CdS nanoparticles is 2.48 eV. The results show that the crystallite size estimated from Scherrer's formula, W-H plots, SSP and the particle size calculated by TEM images are approximately similar.

Kinetic and microstructural study of titanium nitride deposited by laser chemical vapor deposition

NASA Astrophysics Data System (ADS)

Egland, Keith Maynard

Titanium nitride (TiN) films were deposited onto Ti-6Al-4V substrates by laser chemical vapor deposition using a cw COsb2 laser and TiClsb4,\\ Nsb2, and Hsb2 reactant gases. In-situ laser induced fluorescence (LIF) and multi-wavelength pyrometry determined relative titanium gas phase atomic number density and deposition temperature, respectively. Deposited films were yellow to gold in color. Transmission electron microscopy on one sample revealed a face-centered cubic structure with a lattice parameter (0.4237 nm) expected for TiN. Auger electron spectroscopy found substoichiometric compositions with a N/Ti ratio between 0.7 and 0.9. Variables decreasing grain size (lower temperature, higher TiClsb4 input) decreased the N/Ti ratio. Higher Nsb2 input increased stoichiometry, while larger Hsb2 input decreased stoichiometry. The deposit substoichiometry is believed to be caused by diffusion of nitrogen through TiN grain boundaries to the titanium alloy substrate. The morphology starts as a dense polycrystalline structure evolving into a columnar structure having facets or nodules at the surface with crystallite sizes ranging from 10-1000 nm. TiClsb4 input had a inverse correlation with crystallite size, while Nsb2:Hsb2 ratio had minimal effect; the crystallite size (G) varied exponentially with temperature (T) for a given irradiation time, i.e., G = C exp (-28000/T), with constant C reflecting substrate roughness and gas composition. Microhardness tests revealed substrate contributions; nevertheless, films appeared to have a minimum hardness of 2000 Hsbv. The deposition apparent activation energy was calculated as 122 ± 9 kJ/mole using growth rates measured by film height and 117 ± 23 kJ/mole using growth rates measured by LIF signals. This puts the process in the surface kinetic growth regime over the temperature range 1370-1610 K. Above Nsb2 and Hsb2 levels of 1.25% and below TiClsb4 input of 4.5%, the growth rate has a half-order dependence on nitrogen and a linear dependence on hydrogen and is approximated by$r = {{kPsb{TiClsb4}Psb{Hsb2}Psbsp{Nsb2}{1/2}exp≤ft({{-}Esb{a}/ {RT}right)}/{1 + Psb{Ar}}}}.Since nitrogen positively affects growth rate (when added to a TiClsb4+Hsb2 mixture), stepwise reduction of TiClsb4 to Ti by hydrogen does not occur. NHsb{x} complexes are clearly involved in the growth mechanism; a likely combination of rate determining steps is the formation of NH and the initial reduction of TiClsb4$ by hydrogen.

Structure and properties of carbon black particles

NASA Astrophysics Data System (ADS)

Xu, Wei

Structure and properties of carbon black particles were investigated using atomic force microscopy, gas adsorption, Raman spectroscopy, and X-ray diffraction. Supplementary information was obtained using TEM and neutron scattering. The AFM imaging of carbon black aggregates provided qualitative visual information on their morphology, complementary to that obtained by 3-D modeling based on TEM images. Our studies showed that carbon black aggregates were relatively flat. The surface of all untreated carbon black particles was found to be rough and its fractal dimension was 2.2. Heating reduced the roughness and fractal dimension for all samples heat treated at above 1300 K to 2.0. Once the samples were heat treated rapid cooling did not affect the surface roughness. However, rapid cooling reduced crystallite sizes, and different Raman spectra were obtained for carbon blacks of various history of heat treatment. By analyzing the Raman spectra we determined the crystallite sizes and identified amorphous carbon. The concentration of amorphous carbon depends on hydrogen content. Once hydrogen was liberated at increased temperature, the concentration of amorphous carbon was reduced and crystallites started to grow. Properties of carbon blacks at high pressure were also studied. Hydrostatic pressure did not affect the size of the crystallites in carbon black particles. The pressure induced shift in Raman frequency of the graphitic component was a result of increased intermolecular forces and not smaller crystallites. Two methods of determining the fractal dimension, the FHH model and the yardstick technique based on the BET theory were used in the literature. Our study proved that the FHH model is sensitive to numerous assumptions and leads to wrong conclusions. On the other hand the yardstick method gave correct results, which agreed with the AFM results.

The effect of milling time and sintering temperature on Mn, Ti substituted barium hexaferrite nanoparticle

NASA Astrophysics Data System (ADS)

Yustanti, Erlina; Manaf, Azwar

2018-04-01

Barium hexaferrite (BaO.6Fe2O3/BaFe12O19) is a permanent magnetic material and microwave absorbing material. The value of microwave absorption can be increased through the engineering of the material structure, while the reduction of crystallite and particle size up to nanometer results device performance improvement to be superior. In this research, the structural engineering through mechanical alloying and crystallite size reduction through high power ultrasonic irradiation will be explained. Mixing and alloying of Sigma Aldrich BaCO3, Fe2O3, MnCO3, TiO2 p.a 99% precursor material used ball mill with powder ratio of vial at 1:10. Mechanical alloying for 60 hours at 160 rpm produced amorphous material. The process of the crystalline embryo nucleation for 4 hours produced multicrystalline material at a sinter temperature of 1100°C. Phase analysis of the mechanical alloying result using x-ray diffractometer was confirmed either the formation of BaO.6Fe2-xMnx/2Tix/2O3 (x=0.5) single phase. Multicrystalline powder of BaO.6Fe2-xMnx/2Tix/2O3 (x=0.5) was obtained through 20 hours hand grinding and re-milling to bulk sample. Crystallite size reduction in the analysis was conducted through particle density variation in ultrasonic reactor and variation of the increase in ultrasonic time. Increase in milling time up to 60 hours produced fragmenting so that particle size reduction from 18.8 µm to 0.9 µm was occurred. The 12-h ultrasonic irradiation at a frequency of 20 kHz amplitude of 60 µm produced a crystallite-size reduction up to 18 nm at a 10 g/L particle density.

Fabrication and characterization of nano-Y2O3 and Al2O3 dispersed W-Ni alloys by mechanical alloying and pressureless conventional sintering

NASA Astrophysics Data System (ADS)

Talekar, V. R.; Patra, A.; Karak, S. K.

2018-03-01

Nano Y2O3 and Al2O3 dispersed W-Ni alloys with nominal composition of W89Ni10 (Y2O3)1 (alloy A), W89Ni10 (Al2O3)1 (alloy B) were mechanically alloyed for 10 h followed by compaction at 0.5 GPa pressure with 5 min of dwell time and conventional sintering at 1400°C with 2 h soaking time in Ar atmosphere with Ar flow rate of 100 ml/min. The microstructure of milled and sintered alloy was investigated using X-ray Diffraction (XRD), Scanning electron Microscopy (SEM), Energy dispersive spectroscopy (EDS) and Elemental mapping. Minimum crystallite size of 31.9 nm and maximum lattice strain, dislocation density of 0.23%, 9.12(1016/m2) respectively was found in alloy A at 10 h of milling. Uneven and coarse particles at 0 h of milling converted to elongated flake shape at 10 h of milling. Bimodal (fine and coarse) particle size distribution is revealed in both the alloys and minimum particle size of 0.69 μm is achieved in 10 h milled alloy A. Evidences of formation of intermetallic phases like Y2WO6, Y6WO12 and Y10W2O21 in sintered alloy A and Al2(WO4)3, NiAl10O16, NiAl2O4 and AlWO4 in sintered alloy B were revealed by XRD pattern and SEM micrograph. Minimum grain size of 1.50 μm was recorded in sintered alloy A. Both faceted and spherical W matrix is evident in both the alloys which suggests occurrence of both solid phase and liquid phase sintering. Maximum % relative sintered density and hardness of 85.29% and 5.13 GPa respectively was found in alloy A. Wear study at 20N force at 25 rpm for 15 min on ball on plate wear tester revealed that minimum wear depth (48.99 μm) and wear track width (272 μm) was found for alloy A as compared to alloy B.

Line profile analysis of ODS steels Fe20Cr5AlTiY milled powders at different Y2O3 concentrations

NASA Astrophysics Data System (ADS)

Afandi, A.; Nisa, R.; Thosin, K. A. Z.

2017-04-01

Mechanical properties of material are largely dictated by constituent microstructure parameters such as dislocation density, lattice microstrain, crystallite size and its distribution. To develop ultra-fine grain alloys such as Oxide Dispersion Strengthened (ODS) alloys, mechanical alloying is crucial step to introduce crystal defects, and refining the crystallite size. In this research the ODS sample powders were mechanically alloyed with different Y2O3 concentration respectively of 0.5, 1, 3, and 5 wt%. MA process was conducted with High Energy Milling (HEM) with the ball to powder ratio of 15:1. The vial and the ball were made of alumina, and the milling condition is set 200 r.p.m constant. The ODS powders were investigated by X-Ray Diffractions (XRD), Bragg-Brentano setup of SmartLab Rigaku with 40 KV, and 30 mA, step size using 0.02°, with scanning speed of 4°min-1. Line Profile Analysis (LPA) of classical Williamson-Hall was carried out, with the aim to investigate the different crystallite size, and microstrain due to the selection of the full wide at half maximum (FWHM) and integral breadth.

Electronic and structural properties of micro-and nanometre-sized crystalline copper monoxide ceramics investigated by positron annihilation

NASA Astrophysics Data System (ADS)

Druzhkov, A. P.; Gizhevskii, B. A.; Arbuzov, V. L.; Kozlov, E. A.; Shalnov, K. V.; Naumov, S. V.; Perminov, D. A.

2002-09-01

Electronic and structural properties of copper monoxide (CuO) sintered as a common ceramic and nanoceramic are studied by positron annihilation spectroscopy. A CuO nanoceramic with crystallite size ranging from 15 to 90 nm was prepared from a common one by shock-wave loading. It is found that the momentum distribution of valence electrons in CuO is shifted, as compared with metallic copper, towards higher momentum values. This result is related to the effect of the Cu 3d-O 2p hybridization in the Cu-O ionic covalent bond formation. It is found that open volumes, identified mainly as small agglomerates of oxygen vacancies, appear at the nanoceramic crystallite interfaces. The degree of the Cu-O bond covalency decreases locally at the crystallite interfaces because of an oxygen deficit. The nanocrystalline state in CuO is shown to be thermally stable up to 700 K.

Effect of synthesis conditions on the nanopowder properties of Ce{sub 0.9}Zr{sub 0.1}O{sub 2}

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

Zimicz, M.G.; Fabregas, I.O.; Lamas, D.G.

Graphical abstract: . The synthesis of nanocrystalline Ce{sub 0.9}Zr{sub 0.1}O{sub 2} powders via the gel-combustion method, using different fuels, and following either stoichiometric or non-stoichiometric pH-controlled routes is investigated. Research highlights: {yields} All samples exhibited the fluorite-type crystal structure, nanometric average crystallite size and negligible carbon content. {yields} Synthesis conditions strongly affect the average crystallite size, the degree of agglomeration, the specific surface area and the pore volume. {yields} Our results indicate that, by controlling the synthesis conditions it is possible to obtain solids with custom-made morphological properties. -- Abstract: In this work, the synthesis of nanocrystalline Ce{sub 0.9}Zr{sub 0.1}O{submore » 2} powders via the gel-combustion method, using different fuels, and following either stoichiometric or non-stoichiometric pH-controlled routes is investigated. The objective is to evaluate the effect of synthesis conditions on the textural and morphological properties, and the crystal structure of the synthesized materials. The solids were characterized by nitrogen physisorption, Scanning Electron Microscopy (SEM), X-ray powder diffraction (XPD), and Carbon-Hydrogen-Nitrogen Elemental Analysis (CHN). All the powders exhibited nanometric crystallite size, fluorite-type structure and negligible carbon content. Synthesis conditions strongly affect the average crystallite size, the degree of agglomeration, the specific surface area and the pore volume. Our results indicate that, by controlling the synthesis conditions it is possible to obtain solids with custom-made morphological properties.« less

Crystallographic Analysis of a Japanese Sword by using Bragg Edge Transmission Spectroscopy

NASA Astrophysics Data System (ADS)

Shiota, Yoshinori; Hasemi, Hiroyuki; Kiyanagi, Yoshiaki

Neutron imaging using a pulsed neutron source can give crystallographic information over wide area of a sample by analysing position dependent transmission spectra. With the use of a Bragg edge imaging method we non-destructively obtained crystallographic information of a Japanese sword, signed by Bishu Osafune Norimitsu, in order to know position dependent crystallographic characteristics and to check usefulness of the method for the Japanese sword investigation. Strong texture appeared on the back side. On the other hand in the middle area almost isotropic feature appeared and edge side showed feature between them. Rather isotropic area in the centre area gradually reduced from the grip side to the tip side. The crystallite size was smaller near the edge and became larger towards the back side. The smaller crystallite size will be due to quenching around the edge and this trend disappeared in the grip (nakago) area. The larger crystallite size will be due to strong hammering. Coarse grains were also observed directly as transmission images with the use of a high spatial resolution detector. The spatial distribution of the grains was not uniform but the reason have not been understood. Furthermore, a white area around a tip area was proved to be a void by looking at the Brag edge transmission spectra. This void may be formed during forging process of two kinds of steel. It is suggested that consideration on differences in the texture and the crystallite size depending on position will give information to clarify the manufacturing process, and Bragg edge analysis will be a profitable tool for research of Japanese sword.

Pulsed supercritical synthesis of anatase TiO₂ nanoparticles in a water-isopropanol mixture studied by in situ powder X-ray diffraction.

PubMed

Rostgaard Eltzholtz, Jakob; Tyrsted, Christoffer; Ørnsbjerg Jensen, Kirsten Marie; Bremholm, Martin; Christensen, Mogens; Becker-Christensen, Jacob; Brummerstedt Iversen, Bo

2013-03-21

A new step in supercritical nanoparticle synthesis, the pulsed supercritical synthesis reactor, is investigated in situ using synchrotron powder X-ray diffraction (PXRD) to understand the formation of nanoparticles in real time. This eliminates the common problem of transferring information gained during in situ studies to subsequent laboratory reactor conditions. As a proof of principle, anatase titania nanoparticles were synthesized in a 50/50 mixture of water and isopropanol near and above the critical point of water (P = 250 bar, T = 300, 350, 400, 450, 500 and 550 °C). The evolution of the reaction product was followed by sequentially recording PXRD patterns with a time resolution of less than two seconds. The crystallite size of titania is found to depend on both temperature and residence time, and increasing either parameter leads to larger crystallites. A simple adjustment of either temperature or residence time provides a direct method for gram scale production of anatase nanoparticles of average crystallite sizes between 7 and 35 nm, thus giving the option of synthesizing tailor-made nanoparticles. Modeling of the in situ growth curves using an Avrami growth model gave an activation energy of 66(19) kJ mol(-1) for the initial crystallization. The in situ PXRD data also provide direct information about the size dependent macrostrain in the nanoparticles and with decreasing crystallite size the unit cell contracts, especially along the c-direction. This agrees well with previous ex situ results obtained for hydrothermal synthesis of titania nanoparticles.

Dislocation, crystallite size distribution and lattice strain of magnesium oxide nanoparticles

NASA Astrophysics Data System (ADS)

Sutapa, I. W.; Wahid Wahab, Abdul; Taba, P.; Nafie, N. L.

2018-03-01

The oxide of magnesium nanoparticles synthesized using sol-gel method and analysis of the structural properties was conducted. The functional groups of nanoparticles has been analysed by Fourier Transform Infrared Spectroscopy (FT-IR). Dislocations, average size of crystal, strain, stress, the energy density of crystal, crystallite size distribution and morphologies of the crystals were determined based on X-ray diffraction profile analysis. The morphological of the crystal was analysed based on the image resulted from SEM analysis. The crystallite size distribution was calculated with the contention that the particle size has a normal logarithmic form. The most orientations of crystal were determined based on the textural crystal from diffraction data of X-ray diffraction profile analysis. FT-IR results showed the stretching vibration mode of the Mg-O-Mg in the range of 400.11-525 cm-1 as a broad band. The average size crystal of nanoparticles resulted is 9.21 mm with dislocation value of crystal is 0.012 nm-2. The strains, stress, the energy density of crystal are 1.5 x 10-4 37.31 MPa; 0.72 MPa respectively. The highest texture coefficient value of the crystal is 0.98. This result is supported by morphological analysis using SEM which shows most of the regular cubic-shaped crystals. The synthesis method is suitable for simple and cost-effective synthesis model of MgO nanoparticles.

Influence of solution deposition rate on properties of V2O5 thin films deposited by spray pyrolysis technique

NASA Astrophysics Data System (ADS)

Abd-Alghafour, N. M.; Ahmed, Naser M.; Hassan, Zai; Mohammad, Sabah M.

2016-07-01

Vanadium oxide (V2O5) thin films were deposited on glass substrates by using a cost-efficient spray pyrolysis technique. The films were grown at 350° through thermal decomposition of VCl3 in deionized water with different solution spray rates. The high resolution X-ray diffraction results revealed the formation of nanocrystalline films having orthorhombic structures with preferential orientation along (101) direction. The spray rate influenced the surface morphology and crystallite size of the films. The crystallite size was found to increase whereas the micro-strain was decreased by increasing the spray deposition rates. The increase in crystallite size and decrease in the macrostrain resulted in an improvement in the films' crystallinity. The UV-Visible spectroscopy analysis indicated that the average transmittance of all films lies in the range 75-80 %. The band gap of V2O5 film was decreased from 2.65 to 2.46 eV with increase of the spray deposition rate from 5 ml/min to 10 ml/min. first, second, and third level headings (first level heading).

Fabrication of hydroxyapatite and TiO 2 nanorods on microarc-oxidized titanium surface using hydrothermal treatment

NASA Astrophysics Data System (ADS)

Song, Ho-Jun; Kim, Ji-Woo; Kook, Min-Suk; Moon, Won-Jin; Park, Yeong-Joon

2010-09-01

AC-type microarc oxidation (MAO) and hydrothermal treatment techniques were used to enhance the bioactivity of commercially pure titanium (CP-Ti). The porous TiO 2 layer fabricated by the MAO treatment had a dominant anatase structure and contained Ca and P ions. The MAO-treated specimens were treated hydrothermally to form HAp crystallites on the titanium oxide layer in an alkaline aqueous solution (OH-solution) or phosphorous-containing alkaline solution (POH-solution). A small number of micro-sized hydroxyapatite (HAp) crystallites and a thin layer composed of nano-sized HAps were formed on the Ti-MAO-OH group treated hydrothermally in an OH-solution, whereas a large number of micro-sized HAp crystallites and dense anatase TiO 2 nanorods were formed on the Ti-MAO-POH group treated hydrothermally in a POH-solution. The layer of bone-like apatite that formed on the surface of the POH-treated sample after soaking in a modified simulated body fluid was thicker than that on the OH-treated samples.

Chemical spray pyrolyzed kesterite Cu2ZnSnS4 (CZTS) thin films

NASA Astrophysics Data System (ADS)

Khalate, S. A.; Kate, R. S.; Deokate, R. J.

2018-04-01

Pure kesterite phase thin films of Cu2ZnSnS4 (CZTS) were synthesized at different substrate temperatures using sulphate precursors by spray pyrolysis method. The significance of synthesis temperature on the structural, morphological and optical properties has been studied. The X-ray analysis assured that synthesized CZTS thin films showing pure kesterite phase. The value of crystallite size was found maximum at the substrate temperature 400 °C. At the same temperature, microstructural properties such as dislocation density, micro-strain and stacking fault probability were found minimum. The morphological examination designates the development of porous and uniform CZTS thin films. The synthesized CZTS thin films illustrate excellent optical absorption (105 cm-1) in the visible band and the optical band gap varies in the range of 1.489 eV to 1.499 eV.

One-Pot Process in Scalable Bath for Water-Dispersed ZnS Nanocrystals with the Tailored Size

DOE PAGES

Jung, Hyunsung; Phelps, Tommy J.; Rondinone, Adam J.; ...

2017-05-01

Well-dispersed ZnS nanocrystals with tailored size in aqueous solutions were synthesized by employing cysteine-sulfur (Cys-S) complexes with low molecular weight in a scalable anoxic vessel. High yield production of water-dispersed ZnS nanocrystals on a 10-L scale was demonstrated in an aqueous solution process. The average crystallite size of ZnS was controlled by changing the ratio of the cysteine to sulfide in the applied Cys-S complexes. A decrease in the crystallite size of ZnS likely resulted in both the blue shift of peak positions and the relative variation of peak intensities in the photoluminescence properties. In addition, the pH-dependent stability againstmore » aggregation of ZnS nanocrystals was investigated to reduce agglomeration.« less

Electron-Beam Deposition of Superconducting Molybdenum Thin Films for the Development of Mo/Au TES X-Ray Microcalorimeter

NASA Technical Reports Server (NTRS)

Finkbeiner, Fred Michael; Adams, Joseph S.; Bandler, Simon R.; Betancour-Martinez, Gabriele L.; Brown, Ari David; Chang, Meng-Ping; Chervenak, James A.; Chiao, Meng P.; Datesman, Aaron; Eckart, Megan E.;

Grain size effect on activation energy in spinel CoFe{sub 2}O{sub 4} ceramic

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

Supriya, Sweety, E-mail: sweety@iitp.ac.in; Kumar, Sunil; Kar, Manoranjan

2016-05-23

Cobalt ferrite of different average crystallites (from nanocrystallite to micro crystallites) has been prepared by the Sol-Gel Method. The X-ray diffraction (XRD) analysis confirms the cubic spinel phase with no trace of impurity phases. The effect of annealing temperature on micro structure and electric transport properties as a function of frequency and temperature has been studied. It is observed that the electric impedance and conductivity are strongly dependent on grain size. The impedance spectroscopic study is employed to understand the electrical transport properties of cobalt ferrite.

Tunable conductivity in mesoporous germanium

NASA Astrophysics Data System (ADS)

Beattie, Meghan N.; Bioud, Youcef A.; Hobson, David G.; Boucherif, Abderraouf; Valdivia, Christopher E.; Drouin, Dominique; Arès, Richard; Hinzer, Karin

2018-05-01

Germanium-based nanostructures have attracted increasing attention due to favourable electrical and optical properties, which are tunable on the nanoscale. High densities of germanium nanocrystals are synthesized via electrochemical etching, making porous germanium an appealing nanostructured material for a variety of applications. In this work, we have demonstrated highly tunable electrical conductivity in mesoporous germanium layers by conducting a systematic study varying crystallite size using thermal annealing, with experimental conductivities ranging from 0.6 to 33 (×10‑3) Ω‑1 cm‑1. The conductivity of as-prepared mesoporous germanium with 70% porosity and crystallite size between 4 and 10 nm is shown to be ∼0.9 × 10‑3 Ω‑1 cm‑1, 5 orders of magnitude smaller than that of bulk p-type germanium. Thermal annealing for 10 min at 400 °C further reduced the conductivity; however, annealing at 450 °C caused a morphological transformation from columnar crystallites to interconnecting granular crystallites and an increase in conductivity by two orders of magnitude relative to as-prepared mesoporous germanium caused by reduced influence of surface states. We developed an electrostatic model relating the carrier concentration and mobility of p-type mesoporous germanium to the nanoscale morphology. Correlation within an order of magnitude was found between modelled and experimental conductivities, limited by variation in sample uniformity and uncertainty in void size and fraction after annealing. Furthermore, theoretical results suggest that mesoporous germanium conductivity could be tuned over four orders of magnitude, leading to optimized hybrid devices.

Deconvolution of Composition and Crystallite Size of Silver Hollandite Nanorods: Influence on Electrochemistry

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

Durham, Jessica L.; Huang, Jianping; Zhang, Bingjie

In this paper, silver hollandite (Ag 1.4Mn 8O 16) has been synthesized by an aqueous, low-temperature co-precipitation technique to afford silver hollandite with distinct crystallite sizes (10 and 15 nm, identified as S-Ag 1.4Mn 8O 16 and L-Ag 1.4Mn 8O 16, respectively) and equivalent silver content (x), allowing for the deconvolution of electrochemical effects related to crystallite size and silver content. The as-prepared silver hollandite materials were confirmed to be structurally analogous. Notably, TEM imaging reveals a high degree of bundling of S-Ag 1.4Mn 8O 16 nanorods compared to L-Ag 1.4Mn 8O 16 which facilitates more intimate connection of themore » S-Ag 1.4Mn 8O 16 material with enhanced interparticle contact. The electrochemical behavior and lithium diffusion properties were investigated by galvanostatic cycling, CV, electrochemical impedance, pulsed-discharge experiments, and ex-situ XAS analysis of cycled cathodes. Lithium based electrochemical cells containing S-Ag 1.4Mn 8O 16 delivered a capacity 15X higher than L-Ag 1.4Mn 8O 16 on cycle 1. Ex-situ XAS demonstrated structural change for S-Ag 1.4Mn 8O 16 and formation of Ag 0 on insertion of 3.8 Li + intercalation. However, the samples of L-Ag 1.4Mn 8O 16 were lithiated by a more limited 0.25 molar equivalents, where no significant structural changes were observed. Finally, the findings affirm crystallite size significantly impacts electrochemistry independent of cation occupancy of the α-MnO 2 type structure.« less

Deconvolution of Composition and Crystallite Size of Silver Hollandite Nanorods: Influence on Electrochemistry

DOE PAGES

Durham, Jessica L.; Huang, Jianping; Zhang, Bingjie; ...

2017-12-16

In this paper, silver hollandite (Ag 1.4Mn 8O 16) has been synthesized by an aqueous, low-temperature co-precipitation technique to afford silver hollandite with distinct crystallite sizes (10 and 15 nm, identified as S-Ag 1.4Mn 8O 16 and L-Ag 1.4Mn 8O 16, respectively) and equivalent silver content (x), allowing for the deconvolution of electrochemical effects related to crystallite size and silver content. The as-prepared silver hollandite materials were confirmed to be structurally analogous. Notably, TEM imaging reveals a high degree of bundling of S-Ag 1.4Mn 8O 16 nanorods compared to L-Ag 1.4Mn 8O 16 which facilitates more intimate connection of themore » S-Ag 1.4Mn 8O 16 material with enhanced interparticle contact. The electrochemical behavior and lithium diffusion properties were investigated by galvanostatic cycling, CV, electrochemical impedance, pulsed-discharge experiments, and ex-situ XAS analysis of cycled cathodes. Lithium based electrochemical cells containing S-Ag 1.4Mn 8O 16 delivered a capacity 15X higher than L-Ag 1.4Mn 8O 16 on cycle 1. Ex-situ XAS demonstrated structural change for S-Ag 1.4Mn 8O 16 and formation of Ag 0 on insertion of 3.8 Li + intercalation. However, the samples of L-Ag 1.4Mn 8O 16 were lithiated by a more limited 0.25 molar equivalents, where no significant structural changes were observed. Finally, the findings affirm crystallite size significantly impacts electrochemistry independent of cation occupancy of the α-MnO 2 type structure.« less

X-ray line profile analysis of BaTiO3 thin film prepared by sol-gel deposition

NASA Astrophysics Data System (ADS)

Ooi, Zeen Vee; Saif, Ala'eddin A.; Wahab, Yufridin; Jamal, Zul Azhar Zahid

2017-04-01

Barium titanate (BaTiO3) thin film was prepared using sol-gel method and spun-coated on SiO2/Si substrate. The phase and crystallinity of the synthesized film were identified using X-ray diffractometer (XRD), which scanned at the range of 20° to 60°. The phase and lattice parameters of the fabricated film were extracted from the recorded XRD patterns using lattice geometry equations. The crystallite size and lattice strain were determined using X-ray line profile analysis (XLPA) with various approaches. The Scherrer equation was applied to the perovskite peaks of the film to explore the size contribution on the peak broadening. Meanwhile, the Williamson-Hall and size-strain plot (SSP) methods were used to review two main independent contributions, i.e. crystallite sizes and lattice strain, on the X-ray line broadening. From the analysis, it is found that Scherrer method gives smallest crystallite size value by ignoring the strain-induced broadening effect. On the other hand, Williamson-Hall and SSP graphs revealed the existence of the lattice strain within the film, which contributes to the broadening in the Bragg peak. The results that analyzed via both techniques show a linear trend with all data points fitted. However, result obtained from SSP method gives better settlement due to the best fit of the data.

Crystallization of dicalcium phosphate dihydrate with presence of glutamic acid and arginine at 37 °C.

PubMed

Li, Chengfeng; Ge, Xiaolu; Li, Guochang; Bai, Jiahai; Ding, Rui

2014-08-01

The formations of non-metabolic stones, bones and teeth were seriously related to the morphology, size and surface reactivity of dicalcium phosphate dihydrate (DCPD). Herein, a facile biomimetic mineralization method with presence of glutamic acid and arginine was employed to fabricate DCPD with well-defined morphology and adjustable crystallite size. In reaction solution containing more arginine, crystallization of DCPD occurred with faster rate of nucleation and higher density of stacked layers due to the generation of more OH(-) ions after hydrolysis of arginine at 37 °C. With addition of fluorescein or acetone, the consumption of OH(-) ions or desolvation reaction of Ca(2+) ions was modulated, which resulted in the fabrication of DCPD with adjustable crystallite sizes and densities of stacked layers. In comparison with fluorescein-loading DCPD, dicalcium phosphate anhydrate was prepared with enhanced photoluminescence properties due to the reduction of self-quenching effect and regular arrangement of encapsulated fluorescein molecules. With addition of more acetone, DCPD was prepared with smaller crystallite size via antisolvent crystallization. The simulated process with addition of amino acids under 37 °C would shed light on the dynamic process of biomineralization for calcium phosphate compounds. Copyright © 2014 Elsevier B.V. All rights reserved.

Synthesis and characterization of a mixed phase of anatase TiO2 and TiO2(B) by low pressure chemical vapour deposition (LPCVD) for high photocatalytic activity

NASA Astrophysics Data System (ADS)

Chimupala, Y.; Hyett, G.; Simpson, R.; Brydson, R.

2014-06-01

This project is concerned with enhancing photocatalytic activity by preparing a mixed phase of nano-sized TiO2. TiO2 thin films were synthesized by using Low Pressure Chemical Vapour Deposition (LPCVD). Titanium isopropoxide and N2 gas were used as the precursor and carrier gas respectively. The effects of reaction temperature, carrier gas flow rate and deposited area were studied. TiO2 thin films with nano-sized TiO2 particles were obtained under suitable conditions and SEM, TEM, powder XRD and Raman spectroscopy were employed to characterize the phase and physical appearance of synthesized materials. Preliminary results show that a dual phase (TiO2(B) and anatase) thin film nanopowder was successfully prepared by LPCVD with needle- and polygonal plate-shape crystallites respectively. This thin film deposit produced a preferred orientation of TiO2(B) needles in the [001] direction of average crystallite size 50-80 nm in length and 5-10 nm in width, whilst the crystallite size of anatase polygonal-plates was around 200 nm. The optimal LPCVD condition for preparing this mixed phase of TiO2 was 600°C with a 1 mL/s N2 flow rate.

A study of inter-crystallite spaces in some polycrystalline inorganic systems using positron annihilation lifetime spectroscopy

NASA Astrophysics Data System (ADS)

Shantarovich, V. P.; Suzuki, T.; Ito, Y.; Kondo, K.; Gustov, V. W.; Melikhov, I. V.; Berdonosov, S. S.; Ivanov, L. N.; Yu, R. S.

2007-02-01

Positron annihilation lifetime spectroscopy (PALS) was used for calculation of number density and effective sizes of free volume holes (inter-crystallite spaces) in polycrystal CaSO 4, CaCO 3 (vaterit) and Ca 10(PO 4) 6(OH) 2 (apatite). The effect of substitution of two-valence Ca(II) for three-valence Eu(III) on annihilation characteristics of apatite, studied together with the data on thermo-stimulated luminescence (TSL) and low-temperature sorption of gas (N 2), helped to elucidate mechanism of positronium atom (Ps) localization in the free volume holes and perform corresponding calculations. It came out that PALS is more sensitive to inter-crystallite sites (10 16 cm -3) in polycrystallites than to the free volume holes in polymer glasses (10 19 cm -3). This is due to higher mobility of the precursor of localized Ps in crystallites.

The crystallization of tough thermoplastic resins in the presence of carbon fibers

NASA Technical Reports Server (NTRS)

Theil, Michael H.

1988-01-01

The presence of carbon fibers increased the crystallization rates of both PEEK and PPS thermoplastic polymers. The effect was most pronounced at higher crystallization temperatures. Isothermal crystallization rates were analyzed by applying classical phenomenological nucleation theory. Unusually high values of the so-called Avrami exponent were found for neat PEEK. Isothermal crystallization of PEEK and PPS polymers produced crystalline samples having a wide variety of melting temperatures. The melting as observed by differential scanning calorimetry occurred as dual endotherms which were called primary (higher temperature) and secondary melting peaks. Each primary peak accounted for most of the crystallinity present. The secondary peaks represented the melting of crystallites formed later than those attributable to the primary endotherms. The presence of carbon fibers increased the thermal stability of both PEEK and PPS crystallites as manifested by higher temperatures for the primary melting peaks. This may be attributable to increased crystallite size, greater crystallite perfection, and/or favorable modification of the crystallite interface. Over the range studied, crystallization temperature strongly influenced the positions of the secondary peaks but not the primary peaks.

High temperature stability of anatase in titania-alumina semiconductors with enhanced photodegradation of 2, 4-dichlorophenoxyacetic acid.

PubMed

López-Granada, G; Barceinas-Sánchez, J D O; López, R; Gómez, R

2013-12-15

The incorporation of aluminum acetylacetonate as alumina source during the gelation of titanium alkoxide reduces the nucleation sites for the formation of large rutile crystals on temperatures ranging from 400 to 800°C. As a result, the aggregation of anatase crystals is prevented at high temperature. A relationship among the specific surface area, pore size, energy band gap, crystalline structure and crystallite size as the most relevant parameters are evaluated and discussed. According to the results for the photocatalytic degradation of 2,4-dichlorophenoxyacetic acid, the specific surface area, pore size, Eg band gap are not determinant in the photocatalytic properties. It was found that the anatase crystallite size is the mores important parameter affecting the degradation efficiency. Copyright © 2013 Elsevier B.V. All rights reserved.

Size-dependent elastic/inelastic behavior of enamel over millimeter and nanometer length scales.

PubMed

Ang, Siang Fung; Bortel, Emely L; Swain, Michael V; Klocke, Arndt; Schneider, Gerold A

2010-03-01

The microstructure of enamel like most biological tissues has a hierarchical structure which determines their mechanical behavior. However, current studies of the mechanical behavior of enamel lack a systematic investigation of these hierarchical length scales. In this study, we performed macroscopic uni-axial compression tests and the spherical indentation with different indenter radii to probe enamel's elastic/inelastic transition over four hierarchical length scales, namely: 'bulk enamel' (mm), 'multiple-rod' (10's microm), 'intra-rod' (100's nm with multiple crystallites) and finally 'single-crystallite' (10's nm with an area of approximately one hydroxyapatite crystallite). The enamel's elastic/inelastic transitions were observed at 0.4-17 GPa depending on the length scale and were compared with the values of synthetic hydroxyapatite crystallites. The elastic limit of a material is important as it provides insights into the deformability of the material before fracture. At the smallest investigated length scale (contact radius approximately 20 nm), elastic limit is followed by plastic deformation. At the largest investigated length scale (contact size approximately 2 mm), only elastic then micro-crack induced response was observed. A map of elastic/inelastic regions of enamel from millimeter to nanometer length scale is presented. Possible underlying mechanisms are also discussed. (c) 2009 Elsevier Ltd. All rights reserved.

Optical properties of La{sub 2}CuO{sub 4} and La{sub 2-x}Ca{sub x}CuO{sub 4} crystallites in UV-vis-NIR region synthesized by sol-gel process

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

Li Yifeng; Huang Jianfeng, E-mail: hjfnpu@163.com; Cao Liyun

2012-02-15

La{sub 2}CuO{sub 4} and La{sub 2-x}Ca{sub x}CuO{sub 4} crystallites were prepared via a simple sol-gel process. The as-prepared La{sub 2}CuO{sub 4} and La{sub 2} {sub -x}Ca{sub x}CuO{sub 4} crystallites were characterized by X-ray diffraction, transmission electron microscope and UV-vis-NIR spectra. Results show that the grain size of La{sub 2}CuO{sub 4} crystallites increases with the increase of heat treatment temperature from 600 Degree-Sign C to 800 Degree-Sign C. Optical properties show that La{sub 2}CuO{sub 4} crystallites have broad absorption both in the UV-vis region and in the NIR region. The band gap of the as-prepared crystallites decreases from 1.367 eV tomore » 1.284 eV with the increase of calcination temperature from 600 Degree-Sign C to 800 Degree-Sign C. In the series of La{sub 2-x}Ca{sub x}CuO{sub 4} compounds (x = 0.05, 0.08, 0.10, 0.12, 0.15 and 0.20), all of the samples exhibit an orthogonal crystal structure and the solubility limit of Ca{sup 2+} in La{sub 2}CuO{sub 4} is within the range of x = 0.12-0.15. In the whole UV-vis-NIR region, La{sub 2-x}Ca{sub x}CuO{sub 4} crystallites exhibit a broad absorption and the corresponding band gap first increases and then decreases with increasing of Ca{sup 2+} content. - Highlights: Black-Right-Pointing-Pointer The optical band gap can be tuned by adjusting the grain size and Ca{sup 2+} content. Black-Right-Pointing-Pointer La{sub 2}CuO{sub 4} crystallites exhibit a broad absorption band both in the UV-vis region and in the NIR region. Black-Right-Pointing-Pointer The band gap increases from 1.284 eV to 1.319 eV with the decrease of heat treatment temperature. Black-Right-Pointing-Pointer In the whole UV-vis-NIR region, the La{sub 2-x}Ca{sub x}CuO{sub 4} crystallites displayed a broad absorption. Black-Right-Pointing-Pointer The band gap of La{sub 2-x}Ca{sub x}CuO{sub 4} increases linearly with doping level when 0 {<=} x {<=} 0.12.« less

Effect of solvent on the synthesis of SnO{sub 2} nanoparticles

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

Kumar, Virender; Singh, Karamjit; Singh, Kulwinder

Tin oxide (SnO{sub 2}) nanoparticles have been synthesized by co-precipitation method. The synthesized nanoparticles have been characterized by X-ray diffraction (XRD) and Ultraviolet-Visible spectroscopy (UV-VIS). XRD analysis confirmed the formation of single phase of SnO{sub 2} nanoparticles. It has been found that solvents played important role in controlling the crystallite size of SnO{sub 2} nanoparticles. The XRD analysis showed well crystallized tetragonal SnO{sub 2} nanoparticles. The crystallite size of SnO{sub 2} nanoparticles varies with the solvent. Tauc plot showed that optical band gap was also tailored by controlling the solvent during synthesis.

Size Fluctuations of Near Critical Nuclei and Gibbs Free Energy for Nucleation of BDA on Cu(001)

NASA Astrophysics Data System (ADS)

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

2012-07-01

We present a low-energy electron microscopy study of nucleation and growth of BDA on Cu(001) at low supersaturation. At sufficiently high coverage, a dilute BDA phase coexists with c(8×8) crystallites. The real-time microscopic information allows a direct visualization of near-critical nuclei, determination of the supersaturation and the line tension of the crystallites, and, thus, derivation of the Gibbs free energy for nucleation. The resulting critical nucleus size nicely agrees with the measured value. Nuclei up to 4-6 times larger still decay with finite probability, urging reconsideration of the classic perception of a critical nucleus.

Size fluctuations of near critical nuclei and Gibbs free energy for nucleation of BDA on Cu(001).

PubMed

Schwarz, Daniel; van Gastel, Raoul; Zandvliet, Harold J W; Poelsema, Bene

2012-07-06

We present a low-energy electron microscopy study of nucleation and growth of BDA on Cu(001) at low supersaturation. At sufficiently high coverage, a dilute BDA phase coexists with c(8×8) crystallites. The real-time microscopic information allows a direct visualization of near-critical nuclei, determination of the supersaturation and the line tension of the crystallites, and, thus, derivation of the Gibbs free energy for nucleation. The resulting critical nucleus size nicely agrees with the measured value. Nuclei up to 4-6 times larger still decay with finite probability, urging reconsideration of the classic perception of a critical nucleus.

Tailoring nanocrystalline diamond film properties

DOEpatents

Gruen, Dieter M [Downers Grove, IL; McCauley, Thomas G [Somerville, MA; Zhou, Dan [Orlando, FL; Krauss, Alan R [Naperville, IL

2003-07-15

A method for controlling the crystallite size and growth rate of plasma-deposited diamond films. A plasma is established at a pressure in excess of about 55 Torr with controlled concentrations of hydrogen up to about 98% by volume, of unsubstituted hydrocarbons up to about 3% by volume and an inert gas of one or more of the noble gases and nitrogen up to about 98% by volume. The volume ratio of inert gas to hydrogen is preferably maintained at greater than about 4, to deposit a diamond film on a suitable substrate. The diamond film is deposited with a predetermined crystallite size and at a predetermined growth rate.

Influence of solution deposition rate on properties of V{sub 2}O{sub 5} thin films deposited by spray pyrolysis technique

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

Abd–Alghafour, N. M., E-mail: na2013bil@gmail.com; Ahmed, Naser M.; Hassan, Zai

Vanadium oxide (V{sub 2}O{sub 5}) thin films were deposited on glass substrates by using a cost-efficient spray pyrolysis technique. The films were grown at 350° through thermal decomposition of VCl{sub 3} in deionized water with different solution spray rates. The high resolution X-ray diffraction results revealed the formation of nanocrystalline films having orthorhombic structures with preferential orientation along (101) direction. The spray rate influenced the surface morphology and crystallite size of the films. The crystallite size was found to increase whereas the micro-strain was decreased by increasing the spray deposition rates. The increase in crystallite size and decrease in themore » macrostrain resulted in an improvement in the films’ crystallinity. The UV-Visible spectroscopy analysis indicated that the average transmittance of all films lies in the range 75-80 %. The band gap of V{sub 2}O{sub 5} film was decreased from 2.65 to 2.46 eV with increase of the spray deposition rate from 5 ml/min to 10 ml/min. first, second, and third level headings (first level heading).« less

Study of structural and magnetic properties of melt spun Nd2Fe13.6Zr0.4B ingot and ribbon

NASA Astrophysics Data System (ADS)

Amin, Muhammad; Siddiqi, Saadat A.; Ashfaq, Ahmad; Saleem, Murtaza; Ramay, Shahid M.; Mahmood, Asif; Al-Zaghayer, Yousef S.

2015-12-01

Nd2Fe13.6Zr0.4B hard magnetic material were prepared using arc-melting technique on a water-cooled copper hearth kept under argon gas atmosphere. The prepared samples, Nd2Fe13.6Zr0.4B ingot and ribbon are characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM) for crystal structure determination and morphological studies, respectively. The magnetic properties of the samples have been explored using vibrating sample magnetometer (VSM). The lattice constants slightly increased due to the difference in the ionic radii of Fe and that of Zr. The bulk density decreased due to smaller molar weight and low density of Zr as compared to that of Fe. Ingot sample shows almost single crystalline phase with larger crystallite sizes whereas ribbon sample shows a mixture of amorphous and crystalline phases with smaller crystallite sizes. The crystallinity of the material was highly affected with high thermal treatments. Magnetic measurements show noticeable variation in magnetic behavior with the change in crystallite size. The sample prepared in ingot type shows soft while ribbon shows hard magnetic behavior.

Effects of solution concentration and capping agents on the properties of potassium titanyl phosphate noparticles synthesized using a co-precipitation method

NASA Astrophysics Data System (ADS)

Gharibshahian, E.; Jafar Tafershi, M.; Fazli, M.

2018-05-01

In this study, KTiOPO4 (KTP) nanoparticles were synthesized using a co-precipitation method. The effects of the solution concentration (M) and capping agents, such as PVA, oxalic acid, glycine, triethanolamine, and L-alanine, on the structural, microstructural, and optical properties of the products were investigated using X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, ultraviolet-visible spectroscopy, field emission scanning electron microscopy, and transmission electron microscopy. Decreasing the solution concentration decreased the crystallite size from 53.07 nm (for M = 2) to 39.42 nm (for M = 0.5). After applying different capping agents to the sample at the optimum concentration (M = 0.5), the crystallite size decreased again and grains as small as 10.61 nm were obtained. XRD and FTIR analyses indicated the formation of KTP nanoparticles with an orthorhombic structure in all of the samples. The optical band gap increased as the crystallite size decreased. Different morphological patterns such as spherical, needle shaped, polyhedron, and tablet forms were observed in the nanoparticles, which were correlated with the effects of the capping agents employed.

Synthesis of nanocrystalline Ni/Ce-YSZ powder via a polymerization route

NASA Astrophysics Data System (ADS)

Abolghasemi, Z.; Tamizifar, M.; Arzani, K.; Nemati, A.; Khanfekr, A.; Bolandi, M.

2013-08-01

Pechini process was used for preparation of three kinds of nanocrystalline powders of yttria-stabilized zirconia (YSZ): doped with 1.5 mol% nickel oxide, doped with 15 mol% ceria, and doped with 1.5 mol% nickel oxide plus 15 mol% ceria. Zirconium chloride, yttrium nitrate, cerium nitrate, nickel nitrate, citric acid and ethylene glycol were polymerized at 80 °C to produce a gel. XRD, SEM and TEM analyses were used to investigate the crystalline phases and microstructures of obtained compounds. The results of XRD revealed the formation of nanocrystalline powder at 900 °C. Morphology of the powder calcined at 900 °C, examined with a scanning electron microscope, showed that the presence of nickel and cerium inhibited the grain growth in the system. The average crystallite size of the material doped with nickel oxide (9.33 nm) was bigger than the one doped with cerium oxide (9.29 nm), while the YSZ doping with the two oxides simultaneously promoted the grain growth with crystallite size of 11.37 nm. Yttria-stabilized zirconia powder with a mean crystallite size of 9.997 nm was prepared successfully by this method.

Precipitation-Induced Changes in Microstrain and Its Relation with Hardness and Tempering Parameter in 17-4 PH Stainless Steel

NASA Astrophysics Data System (ADS)

Mahadevan, S.; Manojkumar, R.; Jayakumar, T.; Das, C. R.; Rao, B. P. C.

2016-06-01

17-4 PH (precipitation hardening) stainless steel is a soft martensitic stainless steel strengthened by aging at appropriate temperature for sufficient duration. Precipitation of copper particles in the martensitic matrix during aging causes coherency strains which improves the mechanical properties, namely hardness and strength of the matrix. The contributions to X-ray diffraction (XRD) profile broadening due to coherency strains caused by precipitation and crystallite size changes due to aging are separated and quantified using the modified Williamson-Hall approach. The estimated normalized mean square strain and crystallite size are used to explain the observed changes in hardness. Microstructural changes observed in secondary electron images are in qualitative agreement with crystallite size changes estimated from XRD profile analysis. The precipitation kinetics in the age-hardening regime and overaged regime are studied from hardness changes and they follow the Avrami kinetics and Wilson's model, respectively. In overaged condition, the hardness changes are linearly correlated to the tempering parameter (also known as Larson-Miller parameter). Similar linear variation is observed between the normalized mean square strain (determined from XRD line profile analysis) and the tempering parameter, in the incoherent regime which is beyond peak microstrain conditions.

Surface spins disorder in uncoated and SiO2 coated maghemite nanoparticles

NASA Astrophysics Data System (ADS)

Zeb, F.; Nadeem, K.; Shah, S. Kamran Ali; Kamran, M.; Gul, I. Hussain; Ali, L.

2017-05-01

We studied the surface spins disorder in uncoated and silica (SiO2) coated maghemite (γ-Fe2O3) nanoparticles using temperature and time dependent magnetization. The average crystallite size for SiO2 coated and uncoated nanoparticles was about 12 and 29 nm, respectively. Scanning electron microscopy (SEM) showed that the nanoparticles are spherical in shape and well separated. Temperature scans of zero field cooled (ZFC)/field cooled (FC) magnetization measurements showed lower average blocking temperature (TB) for SiO2 coated maghemite nanoparticles as compared to uncoated nanoparticles. The saturation magnetization (Ms) of SiO2 coated maghemite nanoparticles was also lower than the uncoated nanoparticles and is attributed to smaller average crystallite size of SiO2 coated nanoparticles. For saturation magnetization vs. temperature data, Bloch's law (M(T)= M(0).(1- BTb)) was fitted well for both uncoated and SiO2 coated nanoparticles and yields: B =3×10-7 K-b, b=2.22 and B=0.0127 K-b, b=0.57 for uncoated and SiO2 coated nanoparticles, respectively. Higher value of B for SiO2 coated nanoparticles depicts decrease in exchange coupling due to enhanced surface spins disorder (broken surface bonds) as compared to uncoated nanoparticles. The Bloch's exponent b was decreased for SiO2 coated nanoparticles which is due to their smaller average crystallite size or finite size effects. Furthermore, a sharp increase of coercivity at low temperatures (<25 K) was observed for SiO2 coated nanoparticles which is also due to contribution of increased surface anisotropy or frozen surface spins in these smaller nanoparticles. The FC magnetic relaxation data was fitted to stretched exponential law which revealed slower magnetic relaxation for SiO2 coated nanoparticles. All these measurements revealed smaller average crystallite size and enhanced surface spins disorder in SiO2 coated nanoparticles than in uncoated γ-Fe2O3 nanoparticles.

Investigation of the optoelectronic behavior of Pb-doped CdO nanostructures

NASA Astrophysics Data System (ADS)

Eskandari, Abdollah; Jamali-Sheini, Farid; Cheraghizade, Mohsen; Yousefi, Ramin

2018-03-01

Un- and lead (Pb)-doped cadmium oxide (CdO) semiconductor nanostructures were synthesized by a sonochemical method to study their physical properties. The obtained X-ray diffraction (XRD) patterns indicated cubic CdO crystalline structures for all samples and showed that the crystallite size of CdO increases with Pb addition. Scanning electron microscopy (SEM) images of the nanostructures illustrated agglomerated oak-like particles for the Pb-doped CdO nanostructures. Furthermore, optical studies suggested that the emission band gap energy of the CdO nanostructures lies in the range of 2.27-2.38 eV and crystalline defects increase by incorporation of Pb atoms in the CdO crystalline lattice. In addition, electrical experiments declared that the n-type electrical nature of the un- and Pb-doped CdO nanostructures and the minimum of Pb atoms lead to a high carrier concentration.

Structural and optical properties of hydrazine hydrate capped cadmium sulphide nanoparticles

NASA Astrophysics Data System (ADS)

Solanki, Rekha Garg; Rajaram, P.

2018-05-01

Semiconductor nanoparticles have received considerable interest due to their size-dependent optical properties. CdS is an important semiconductor material widely used in low cost photovoltaic devices, light-emitting diodes and biological imaging. The nanoparticles of CdS were prepared by a simple chemical precipitation method in aqueous medium. The reaction was carried out at room temperature. The cadmium sulphide nanoparticles were characterized using X-ray powder diffraction (XRD) and UV-visible spectroscopy. The lattice strain, crystallite size and dislocation density were calculated using the Williamson-Hall (W-H) method. The band gap was obtained from the UV-Visible spectra of CdS nanoparticles. The band gap of CdS nanoparticles is around 2.68 eV and the crystallite size is around 5.8 nm.

Structural and optical properties of Ni-doped CdS thin films prepared by chemical bath deposition method

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

Premarani, R.; Saravanakumar, S., E-mail: sarophy84@gmail.com; Chandramohan, R.

2015-06-24

The structural and optical behavior of undoped Cadmiun Sulphide (CdS) and Ni-doped CdS thinfilms prepared by Chemical Bath Deposition (CBD) technique is reported. The crystallite sizes of the thinfilms have been characterized by X-ray diffraction pattern (XRD). The particle sizes increase with the increase of Ni content in the CdS thinfilms. Scanning Electron Microscope (SEM) results indicated that CdS thinfilms is made up of aggregate of spherical-like particles. The composition was estimated by Energy Dispersive Analysis of X-ray (EDX) and reported. Spectroscopic studies revealed considerable improvement in transmission and the band gap of the films changes with addition of Nimore » dopant that is associated with variation in crystallite sizes in the nano regime.« less

Determination of Microstructural Parameters of Nanocrystalline Hydroxyapatite Prepared by Mechanical Alloying Method

NASA Astrophysics Data System (ADS)

Joughehdoust, Sedigheh; Manafi, Sahebali

2011-12-01

Hydroxyapatite [HA, Ca10(PO4)6(OH)2] is chemically similar to the mineral component of bones and hard tissues. HA can support bone ingrowth and osseointegration when used in orthopaedic, dental and maxillofacial applications. In this research, HA nanostructure was synthesized by mechanical alloying method. Phase development, particle size and morphology of HA were investigated by X-ray diffraction (XRD) pattern, zetasizer instrument, scanning electron microscopy (SEM), respectively. XRD pattern has been used to determination of the microstructural parameters (crystallite size, lattice parameters and crystallinity percent) by Williamson-Hall equation, Nelson-Riley method and calculating the areas under the peaks, respectively. The crystallite size and particle size of HA powders were in nanometric scales. SEM images showed that some parts of HA particles have agglomerates. The ratio of lattice parameters of synthetic hydroxyapatite (c/a = 0.73) was determined in this study is the same as natural hydroxyapatite structure.

Phase and crystallite size analysis of (Ti1-xMox)C-(Ni,Cr) cermet obtained by mechanical alloying

NASA Astrophysics Data System (ADS)

Suryana, Anis, Muhammad; Manaf, Azwar

2018-04-01

In this paper, we report the phase and crystallite size analysis of (Ti1-xMox)C-(Ni,Cr) with x = 0-0.5 cermet obtained by mechanical alloying of Ti, Mo, Ni, Cr and C elemental powders using a high-energy shaker ball mill under wet condition for 10 hours. The process used toluene as process control agent and the ball to mass ratio was 10:1. The mechanically milled powder was then consolidated and subsequently heated at a temperature 850°C for 2 hours under an argon flow to prevent oxidation. The product was characterized by X-ray diffraction (XRD) and scanning electron microscope equipped with energy dispersive analyzer. Results shown that, by the selection of appropriate condition during the mechanical alloying process, a metastable Ti-Ni-Cr-C powders could be obtained. The powder then allowed the in situ synthesis of TiC-(Ni,Cr) cermet which took place during exposure time at a high temperature that applied in reactive sintering step. Addition to molybdenum has caused shifting the TiC XRD peaks to a slightly higher angle which indicated that molybdenum dissolved in TiC phase. The crystallite size distribution of TiC is discussed in the report, which showing that the mean size decreased with the addition of molybdenum.

Influence of the crystallinity of a sputtered hydroxyapatite film on its osteocompatibility.

PubMed

Ozeki, K; Goto, T; Aoki, H; Masuzawa, T

2015-01-01

Hydroxyapatite (HA) was coated onto titanium substrates using radio frequency sputtering, and the sputtered films were crystallized using a hydrothermal treatment at 120°C and 170°C to evaluate the influence of the crystallinity of the HA film on its osteocompatibility. The crystallite size and surface morphology of the films were observed using X-ray diffraction (XRD) and scanning electron microscopy (SEM), respectively. The alkaline phosphatase (ALP) expression, osteocalin (OCN) expression and bone formation of osteoblast cells on the films were measured to evaluate the osteocompatibility of the film.The crystallite size increased as the hydrothermal temperature increased, and the crystallite sizes of the film treated at 120°C and 170°C were 82.2±12.3 nm and 124.7±13.3 nm, respectively. Globular particles were observed in the hydrothermally treated film using SEM. The size of the particles on the film increased as the hydrothermal temperature increased, and the width of the particles on the film treated at 120°C and 170°C were approximately 120-190 nm and 300-500 nm, respectively. In the osteoblast cell culture experiments, the ALP expression, OCN expression and bone formation area on the films treated at 120°C were higher than those treated for films treated at 170°C.

Carbon nanoscroll-silk crystallite hybrid structures with controllable hydration and mechanical properties.

PubMed

Cheng, Yuan; Koh, Leng-Duei; Wang, Fan; Li, Dechang; Ji, Baohua; Yeo, Jingjie; Guan, Guijian; Han, Ming-Yong; Zhang, Yong-Wei

2017-07-06

Hybrid structures of nanomaterials (e.g. tubes, scrolls, threads, cages) and biomaterials (e.g. proteins) hold tremendous potential for applications as drug carriers, biosensors, tissue scaffolds, cancer therapeutic agents, etc. However, in many cases, the interacting forces at the nano-bio interfaces and their roles in controlling the structures and dynamics of nano-bio-hybrid systems are very complicated but poorly understood. In this study, we investigate the structure and mechanical behavior of a protein-based hybrid structure, i.e., a carbon nanoscroll (CNS)-silk crystallite with a hydration level controllable by an interlayer interaction in CNS. Our findings demonstrate that CNS with a reduced core size not only shields the crystallite from a weakening effect of water, but also markedly strengthens the crystallite. Besides water shielding, the enhanced strength arises from an enhanced interaction between the crystallite and CNS due to the enhanced interlayer interaction in CNS. In addition, the interfacial strength for pulling the crystallite out of the CNS-silk structure is found to be dependent on both the interlayer interaction energy in CNS as well as the sequence of protein at the CNS-silk interface. The present study is of significant value in designing drugs or protein delivery vehicles for biomedical applications, and serves as a general guide in designing novel devices based on rolled-up configurations of two-dimensional (2D) materials.

Scanning electron microscopy of clays and clay minerals

USGS Publications Warehouse

Bohor, B.F.; Hughes, R.E.

1971-01-01

The scanning electron microscope (SEM) proves to be ideally suited for studying the configuration, texture, and fabric of clay samples. Growth mechanics of crystalline units—interpenetration and interlocking of crystallites, crystal habits, twinning, helical growth, and topotaxis—also are uniquely revealed by the SEM.Authigenic kaolins make up the bulk of the examples because their larger crystallite size, better crystallinity, and open texture make them more suited to examination by the SEM than most other clay mineral types.

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

Blackstone, R.; Graham, L.W.

The dimensional changes observed in a range of graphitic materials following irradiation at 600, 900, and 1200 deg C are reported. The results are discussed in the light of current models for irradiation damage in graphite and it is concluded that for conventional materials the dimensional behaviour can be related to the material properties. Further confirmation of the extreme dependence of the dimensional changes on the crystallite size has been obtained. The way in which the rate of dimensional change varies with temperature is compatible with this effect being caused by vacancy loss at crystallite boundaries. For a given crystallitemore » size there appears to be a breakaway temperature above which the rate of dimensional change accelerates rapidly. (auth)« less

Preparation and evaluation of advanced electrocatalysts for phosphoric acid fuel cells

NASA Technical Reports Server (NTRS)

Stonehart, P.; Baris, J.; Hochmuth, J.; Pagliaro, P.

1981-01-01

A number of electrocatalyst combinations were prepared and characterized. These electrocatalysts were formulated to contain platinum combined with transition metal carbide forming elements (W, Mo, V) for cathodes and platinum combined with palladium for anodes. High resolution electron microscopy was used to determine the crystallite size and dispersion of platinum-palladium alloy electrocatalysts in order to provide analytical support for the electrochemical determinations of the particle dispersions. An equation was derived which correlates palladium crystallite size with electrochemical hydrogen adsorption. Based on comparisons of electrocatalyst performances in the presence of pure hydrogen and hydrogen containing carbon monoxide, it was shown that the apparent poisoning of the electrocatalyst by carbon monoxide is influenced by the electrode structure.

Expected values and variances of Bragg peak intensities measured in a nanocrystalline powder diffraction experiment

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

Öztürk, Hande; Noyan, I. Cevdet

A rigorous study of sampling and intensity statistics applicable for a powder diffraction experiment as a function of crystallite size is presented. Our analysis yields approximate equations for the expected value, variance and standard deviations for both the number of diffracting grains and the corresponding diffracted intensity for a given Bragg peak. The classical formalism published in 1948 by Alexander, Klug & Kummer [J. Appl. Phys.(1948),19, 742–753] appears as a special case, limited to large crystallite sizes, here. It is observed that both the Lorentz probability expression and the statistics equations used in the classical formalism are inapplicable for nanocrystallinemore » powder samples.« less

Expected values and variances of Bragg peak intensities measured in a nanocrystalline powder diffraction experiment

DOE PAGES

Öztürk, Hande; Noyan, I. Cevdet

2017-08-24

A rigorous study of sampling and intensity statistics applicable for a powder diffraction experiment as a function of crystallite size is presented. Our analysis yields approximate equations for the expected value, variance and standard deviations for both the number of diffracting grains and the corresponding diffracted intensity for a given Bragg peak. The classical formalism published in 1948 by Alexander, Klug & Kummer [J. Appl. Phys.(1948),19, 742–753] appears as a special case, limited to large crystallite sizes, here. It is observed that both the Lorentz probability expression and the statistics equations used in the classical formalism are inapplicable for nanocrystallinemore » powder samples.« less

Zinc-Containing Restorations Create Amorphous Biogenic Apatite at the Carious Dentin Interface: A X-Ray Diffraction (XRD) Crystal Lattice Analysis.

PubMed

Toledano, Manuel; Aguilera, Fátima S; López-López, Modesto T; Osorio, Estrella; Toledano-Osorio, Manuel; Osorio, Raquel

2016-10-01

The aim of this research was to assess the ability of amalgam restorations to induce amorphous mineral precipitation at the caries-affected dentin substrate. Sound and caries-affected dentin surfaces were subjected to both Zn-free and Zn-containing dental amalgam restorations. Specimens were submitted to thermocycling (100,000 cycles/5°C-55°C, 3 months). Dentin surfaces were studied by atomic force microscopy (nanoroughness), X-ray diffraction, field emission scanning electron microscopy, and energy-dispersive analysis, for physical and morphological surface characterization. Zn-containing amalgam placement reduced crystallinity, crystallite size, and grain size of calcium phosphate crystallites at the dentin surface. Both microstrain and nanoroughness were augmented in caries-affected dentin restored with Zn-containing amalgams. Caries-affected dentin showed the shortest mineral crystallites (11.04 nm), when Zn-containing amalgams were used for restorations, probably leading to a decrease of mechanical properties which might favor crack propagation and deformation. Sound dentin restored with Zn-free amalgams exhibited a substantial increase in length of grain particles (12.44 nm) embedded into dentin crystallites. Zn-containing amalgam placement creates dentin mineralization and the resultant mineral was amorphous in nature. Amorphous calcium phosphate provides a local ion-rich environment, which is considered favorable for in situ generation of prenucleation clusters, promotong further dentin remineralization.

Estimation of lattice strain in nanocrystalline RuO2 by Williamson-Hall and size-strain plot methods

NASA Astrophysics Data System (ADS)

Sivakami, R.; Dhanuskodi, S.; Karvembu, R.

2016-01-01

RuO2 nanoparticles (RuO2 NPs) have been successfully synthesized by the hydrothermal method. Structure and the particle size have been determined by X-ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscopy (AFM) and transmission electron microscopy (TEM). UV-Vis spectra reveal that the optical band gap of RuO2 nanoparticles is red shifted from 3.95 to 3.55 eV. BET measurements show a high specific surface area (SSA) of 118-133 m2/g and pore diameter (10-25 nm) has been estimated by Barret-Joyner-Halenda (BJH) method. The crystallite size and lattice strain in the samples have been investigated by Williamson-Hall (W-H) analysis assuming uniform deformation, deformation stress and deformation energy density, and the size-strain plot method. All other relevant physical parameters including stress, strain and energy density have been calculated. The average crystallite size and the lattice strain evaluated from XRD measurements are in good agreement with the results of TEM.

Influences of Co doping on the structural and optical properties of ZnO nanostructured

NASA Astrophysics Data System (ADS)

Majeed Khan, M. A.; Wasi Khan, M.; Alhoshan, Mansour; Alsalhi, M. S.; Aldwayyan, A. S.

2010-07-01

Pure and Co-doped ZnO nanostructured samples have been synthesized by a chemical route. We have studied the structural and optical properties of the samples by using X-ray diffraction (XRD), field-emission scanning electron microscopy (FESEM), field-emission transmission electron microscope (FETEM), energy-dispersive X-ray (EDX) analysis and UV-VIS spectroscopy. The XRD patterns show that all the samples are hexagonal wurtzite structures. Changes in crystallite size due to mechanical activation were also determined from X-ray measurements. These results were correlated with changes in particle size followed by SEM and TEM. The average crystallite sizes obtained from XRD were between 20 to 25 nm. The TEM images showed the average particle size of undoped ZnO nanostructure was about 20 nm whereas the smallest average grain size at 3% Co was about 15 nm. Optical parameters such as absorption coefficient ( α), energy band gap ( E g ), the refractive index ( n), and dielectric constants ( σ) have been determined using different methods.

Effect of nanostructure on thermoelectric properties of La0.7Sr0.3MnO3 in 300–600 K temperature range

NASA Astrophysics Data System (ADS)

Singh, Saurabh; Srivastav, Simant Kumar; Patel, Ashutosh; Chatterjee, Ratnamala; Pandey, Sudhir K.

2018-05-01

In oxide materials, nanostructuring effect has been found a very promising approach for the enhancement of figure-of-merit, ZT. In the present work, we have synthesized La0.7Sr0.3MnO3 (LSMO) compound using sol-gel method and samples of crystallite size of ∼20, ∼41, and ∼49 nm were obtained by giving different heat treatment. Seebeck coefficient (α), electrical resistivity (ρ), and thermal conductivity (κ) measurements were carried out in 300–600 K temperature range. The systematic change in the values of α from ∼‑19 μV/K to ∼‑24 μV/K and drastic reduction in the values of κ from ∼0.88 W/mK to ∼0.23 W/mK are observed as crystallite size is reduced from 49 nm to 20 nm at ∼600 K. Also, fall in the values of ρ in the paramagnetic (PM) insulator phase (400–600 K) are effectively responsible for the increasing trend in the values of ZT at high temperature. For the crystallite size of 41 nm, the value of ZT at 600 K was found to be ∼0.017.

The formation of titanium dioxide crystallite nanoparticles during activation of PAN nanofibers containing titanium isopropoxide

NASA Astrophysics Data System (ADS)

Mehrpouya, Fahimeh; Tavanai, Hossein; Morshed, Mohammad; Ghiaci, Mehran

2012-08-01

Activated carbon (AC) can act as an important carrier for TiO2 nanoparticles. TiO2 nanoparticle can be fabricated by the hydrolysis and condensation of titanium alkoxides like titanium isopropoxide. This study showed that the formation of titanium dioxide crystallite nanoparticle during activation of PAN nanofibers containing titanium isopropoxide leads to the formation of mainly anatase crystal TiO2 nanoparticle in AC nanofibers, with a good dispersion in both the longitude and cross section of nanofibers. The TiO2 crystallite size lies in the range of 7.3-11.3 nm. The dispersion of TiO2 nanoparticles in the matrix of AC nanofibers is far superior to the direct mixing of TiO2 nanoparticles in the original electrospinning solution.

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

Ravikumar, Patta; Kisan, Bhagaban; Perumal, A., E-mail: perumal@iitg.ernet.in

We report systematic investigations of structural, vibrational, resonance and magnetic properties of nanoscale NiO powders prepared by ball milling process under different milling speeds for 30 hours of milling. Structural properties revealed that both pure NiO and as-milled NiO powders exhibit face centered cubic structure, but average crystallite size decreases to around 11 nm along with significant increase in strain with increasing milling speed. Vibrational properties show the enhancement in the intensity of one-phonon longitudinal optical (LO) band and disappearance of two-magnon band due to size reduction. In addition, two-phonon LO band exhibits red shift due to size-induced phonon confinementmore » effect and surface relaxation. Pure NiO powder exhibit antiferromagnetic nature, which transforms into induced ferromagnetic after size reduction. The average magnetization at room temperature increases with decreasing the crystallite size and a maximum moment of 0.016 μ{sub B}/f.u. at 12 kOe applied field and coercivity of 170 Oe were obtained for 30 hours milled NiO powders at 600 rotation per minute milling speed. The change in the magnetic properties is also supported by the vibrational properties. Thermomagnetization measurements at high temperature reveal a well-defined magnetic phase transition at high temperature (T{sub C}) around 780 K due to induced ferromagnetic phase. Electron paramagnetic resonance (EPR) studies reveal a good agreement between the EPR results and magnetic properties. The observed results are described on the basis of crystallite size variation, defect density, large strain, oxidation/reduction of Ni and interaction between uncompensated surfaces and particle core with lattice expansion. The obtained results suggest that nanoscale NiO powders with high T{sub C} and moderate magnetic moment at room temperature with cubic structure would be useful to expedite for spintronic devices.« less

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

Frølich, S.; Leemreize, H.; Jakus, A.

A model sample consisting of two different hydroxyapatite (hAp) powders was used as a bone phantom to investigate the extent to which X-ray diffraction tomography could map differences in hAp lattice constants and crystallite size. The diffraction data were collected at beamline 1-ID, the Advanced Photon Source, using monochromatic 65 keV X-radiation, a 25 × 25 µm pinhole beam and translation/rotation data collection. The diffraction pattern was reconstructed for each volume element (voxel) in the sample, and Rietveld refinement was used to determine the hAp lattice constants. The crystallite size for each voxel was also determined from the 00.2 hApmore » diffraction peak width. The results clearly show that differences between hAp powders could be measured with diffraction tomography.« less

Matrix Structure Evolution and Nanoreinforcement Distribution in Mechanically Milled and Spark Plasma Sintered Al-SiC Nanocomposites.

PubMed

Saheb, Nouari; Aliyu, Ismaila Kayode; Hassan, Syed Fida; Al-Aqeeli, Nasser

2014-09-19

Development of homogenous metal matrix nanocomposites with uniform distribution of nanoreinforcement, preserved matrix nanostructure features, and improved properties, was possible by means of innovative processing techniques. In this work, Al-SiC nanocomposites were synthesized by mechanical milling and consolidated through spark plasma sintering. Field Emission Scanning Electron Microscope (FE-SEM) with Energy Dispersive X-ray Spectroscopy (EDS) facility was used for the characterization of the extent of SiC particles' distribution in the mechanically milled powders and spark plasma sintered samples. The change of the matrix crystallite size and lattice strain during milling and sintering was followed through X-ray diffraction (XRD). The density and hardness of the developed materials were evaluated as function of SiC content at fixed sintering conditions using a densimeter and a digital microhardness tester, respectively. It was found that milling for 24 h led to uniform distribution of SiC nanoreinforcement, reduced particle size and crystallite size of the aluminum matrix, and increased lattice strain. The presence and amount of SiC reinforcement enhanced the milling effect. The uniform distribution of SiC achieved by mechanical milling was maintained in sintered samples. Sintering led to the increase in the crystallite size of the aluminum matrix; however, it remained less than 100 nm in the composite containing 10 wt.% SiC. Density and hardness of sintered nanocomposites were reported and compared with those published in the literature.

A bioactive coating with submicron-sized titania crystallites fabricated by induction heating of titanium after tensile deformations.

PubMed

Li, Ning-Bo; Xu, Wen-Hua; Xiao, Gui-Yong; Zhao, Jun-Han; Lu, Yu-Peng

2017-11-01

Thermal oxidation technology was widely investigated as one of effective surface modification method for improving the bioactivity and biocompatibility of titanium and its alloys. In this work, the induction heat oxidization method, a fast, efficient, economical and environmental protective technology, was applied to prepare the submicron-morphological oxide coating with variable rutile TiO 2 equiaxed crystallites on the surface of pure Ti substrates after cold-drawing with 10-20% deformations. The results showed the plastic-deformed Ti cylinders recrystallized during induction heating treatment (IHT) for 10-20s which resulted in evolution of microstructures as well as slight improvement of microhardness. The surface characteristics of TiO 2 crystallites in oxidation layers were determined by the microstructural evolutions of Ti substrate in terms of the nucleation and growth of TiO 2 crystallites. Specially, the oxidized surface with 50-75nm roughness and more uniform and finer equiaxed oxide grains remarkablely improved the apatite deposition after bioactive evaluation in 1.5 × SBF for 7 days. This work provided a potential method to create controlled bioactive oxide coatings with submicro-/nano-scaled TiO 2 crystallites on titanium substrate in terms of the role of metallographic microstructure in the formation process of titanium oxides. Copyright © 2017 Elsevier Ltd. All rights reserved.

Rietveld analysis of the effect of annealing atmosphere on phase evolution of nanocrystalline TiO2 powders.

PubMed

Salari, M; Rezaee, M; Chidembo, A T; Konstantinov, K; Liu, H K

2012-06-01

The structural evolution of nanocrystalline TiO2 was studied by X-ray diffraction (XRD) and the Rietveld refinement method (RRM). TiO2 powders were prepared by the sol-gel technique. Post annealing of as-synthesized powders in the temperature range from 500 degrees C to 800 degrees C under air and argon atmospheres led to the formation of TiO2 nanoparticles with mean crystallite size in the range of 37-165 nm, based on the Rietveld refinement results. It was found that the phase structure, composition, and crystallite size of the resulting particles were dependent on not only the annealing temperature, but also the annealing atmosphere. Rietveld refinement of the XRD data showed that annealing the powders under argon atmosphere promoted the polymorphic phase transformation from anatase to rutile. Field emission scanning electron microscopy (FESEM) was employed to investigate the morphology and size of the annealed powders.

Tailoring of Boehmite-Derived Aluminosilicate Aerogel Structure and Properties: Influence of Ti Addition

NASA Technical Reports Server (NTRS)

Hurwitz, Frances I.; Guo, Haiquan; Sheets, Erik J.; Miller, Derek R.; Newlin, Katy N.

2010-01-01

Aluminosilicate aerogels offer potential for extremely low thermal conductivities at temperatures greater than 900 C, beyond where silica aerogels reach their upper temperature limits. Aerogels have been synthesized at various Al:Si ratios, including mullite compositions, using Boehmite (AlOOH) as the Al source, and tetraethoxy orthosilicate as the Si precursor. The Boehmite-derived aerogels are found to form by a self-assembly process of AlOOH crystallites, with Si-O groups on the surface of an alumina skeleton. Morphology, surface area and pore size varies with the crystallite size of the starting Boehmite powder, as well as with synthesis parameters. Ternary systems, including Al-Si-Ti aerogels incorporating a soluble Ti precursor, are possible with careful control of pH. The addition of Ti influences sol viscosity, gelation time pore structure and pore size distribution, as well as phase formation on heat treatment.

Ambient aging of rhenium filaments used in thermal ionization mass spectrometry: Growth of oxo-rhenium crystallites and anti-aging strategies.

PubMed

Mannion, Joseph M; Wellons, Matthew S; Shick, Charles R; Fugate, Glenn A; Powell, Brian A; Husson, Scott M

2017-01-01

Degassing is a common preparation technique for rhenium filaments used for thermal ionization mass spectrometric analysis of actinides, including plutonium. Although optimization studies regarding degassing conditions have been reported, little work has been done to characterize filament aging after degassing. In this study, the effects of filament aging after degassing were explored to determine a "shelf-life" for degassed rhenium filaments, and methods to limit filament aging were investigated. Zone-refined rhenium filaments were degassed by resistance heating under high vacuum before exposure to ambient atmosphere for up to 2 months. After degassing the nucleation and preferential growth of oxo-rhenium crystallites on the surface of polycrystalline rhenium filaments was observed by atomic force microscopy and scanning electron microscopy (SEM). Compositional analysis of the crystallites was conducted using SEM-Raman spectroscopy and SEM energy dispersive X-ray spectroscopy, and grain orientation at the metal surface was investigated by electron back-scatter diffraction mapping. Spectra collected by SEM-Raman suggest crystallites are composed primarily of perrhenic acid. The relative extent of growth and crystallite morphology were found to be grain dependent and affected by the dissolution of carbon into filaments during annealing (often referred to as carbonization or carburization). Crystallites were observed to nucleate in region specific modes and grow over time through transfer of material from the surface. Factors most likely to affect the rates of crystallite growth include rhenium substrate properties such as grain size, orientation, levels of dissolved carbon, and relative abundance of defect sites; as well as environmental factors such as length of exposure to oxygen and relative humidity. Thin (∼180 nm) hydrophobic films of poly(vinylbenzyl chloride) were found to slow the growth of oxo-rhenium crystallites on the filament surfaces and may serve as an alternative carbon source for filament carburization.

Structural, morphological, and optical properties of tin(IV) oxide nanoparticles synthesized using Camellia sinensis extract: a green approach

NASA Astrophysics Data System (ADS)

Selvakumari, J. Celina; Ahila, M.; Malligavathy, M.; Padiyan, D. Pathinettam

2017-09-01

Tin oxide (SnO2) nanoparticles were cost-effectively synthesized using nontoxic chemicals and green tea ( Camellia sinensis) extract via a green synthesis method. The structural properties of the obtained nanoparticles were studied using X-ray diffraction, which indicated that the crystallite size was less than 20 nm. The particle size and morphology of the nanoparticles were analyzed using scanning electron microscopy and transmission electron microscopy. The morphological analysis revealed agglomerated spherical nanoparticles with sizes varying from 5 to 30 nm. The optical properties of the nanoparticles' band gap were characterized using diffuse reflectance spectroscopy. The band gap was found to decrease with increasing annealing temperature. The O vacancy defects were analyzed using photoluminescence spectroscopy. The increase in the crystallite size, decreasing band gap, and the increasing intensities of the UV and visible emission peaks indicated that the green-synthesized SnO2 may play future important roles in catalysis and optoelectronic devices.

Enriched adhesion of talc/ZnO nanocomposites on cotton fabric assisted by aloe-vera for bio-medical application

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

Selvakumar, D.; Yogamalar, N. R.; Jayavel, R., E-mail: rjvel@annauniv.edu

Synthesis and characterization of talc/ZnO nanocomposites with the assistance of aloe-vera are investigated by structural and morphological studies. The crystal structure and the phase analysis of ZnO and talc are characterized and confirmed by X-ray diffraction (XRD) analysis. The average crystallite size estimation from the Scherrer formula and the particle size analysis clearly predicts that the size of the ZnO declines when aloe-vera is used as a capping molecule in comparison to the commercially available ZnO. The reduced crystallite size of ZnO renders a stable cohesion with the talc composition and the presence of distinct functional group pyridines/ammonia in themore » synthesized nanocomposites enriches the good adhesion between the as-synthesized material and cotton fabric. The adhesion and homogeneous distribution of talc/ZnO nanocomposites on the cotton fabric are inferred from the scanning electron microscopy (SEM) results. The basic studies and characterizations would pave way for futuristic bio-medical application.« less

Enriched adhesion of talc/ZnO nanocomposites on cotton fabric assisted by aloe-vera for bio-medical application

NASA Astrophysics Data System (ADS)

Selvakumar, D.; Thenammai, A. N.; Yogamalar, N. R.; Hemamalini, R.; Jayavel, R.

2015-06-01

Synthesis and characterization of talc/ZnO nanocomposites with the assistance of aloe-vera are investigated by structural and morphological studies. The crystal structure and the phase analysis of ZnO and talc are characterized and confirmed by X-ray diffraction (XRD) analysis. The average crystallite size estimation from the Scherrer formula and the particle size analysis clearly predicts that the size of the ZnO declines when aloe-vera is used as a capping molecule in comparison to the commercially available ZnO. The reduced crystallite size of ZnO renders a stable cohesion with the talc composition and the presence of distinct functional group pyridines/ammonia in the synthesized nanocomposites enriches the good adhesion between the as-synthesized material and cotton fabric. The adhesion and homogeneous distribution of talc/ZnO nanocomposites on the cotton fabric are inferred from the scanning electron microscopy (SEM) results. The basic studies and characterizations would pave way for futuristic bio-medical application.

Structural and Morphological Evaluation of Nano-Sized MoSi2 Powder Produced by Mechanical Milling

NASA Astrophysics Data System (ADS)

Sameezadeh, Mahmood; Farhangi, Hassan; Emamy, Masoud

Nano-sized intermetallic powders have received great attention owing to their property advantages over conventional micro-sized counterparts. In the present study nano-sized MoSi2 powder has been produced successfully from commercially available MoSi2 (3 μm) by a mechanical milling process carried out for a period of 100 hours. The effects of milling time on size and morphology of the powders were studied by SEM and TEM and image analyzing system. The results indicate that the as-received micrometric powder with a wide size distribution of irregular shaped morphology changes to a narrow size distribution of nearly equiaxed particles with the progress of attrition milling up to 100 h, reaching an average particle size of 71 nm. Structural evolution of milled samples was characterized by XRD to determine the crystallite size and lattice microstrain using Williamson-Hall method. According to the results, the crystallite size of the powders decreases continuously down to 23 nm with increasing milling time up to 100 h and this size refinement is more rapid at the early stages of the milling process. On the other hand, the lattice strain increases considerably with milling up to 65 h and further milling causes no significant changes of lattice strain.

Dielectric relaxation behavior and impedance studies of Cu2+ ion doped Mg - Zn spinel nanoferrites

NASA Astrophysics Data System (ADS)

Choudhary, Pankaj; Varshney, Dinesh

2018-03-01

Cu2+ substituted Mg - Zn nanoferrites is synthesized by low temperature fired sol gel auto combustion method. The spinel nature of nanoferrites was confirmed by lab x-ray technique. Williamson - Hall (W-H) analysis estimate the average crystallite size (22.25-29.19 ± 3 nm) and micro strain induced Mg0.5Zn0.5-xCuxFe2O4 (0.0 ≤ x ≤ 0.5). Raman scattering measurements confirm presence of four active phonon modes. Red shift is observed with enhanced Cu concentration. Dielectric parameters exhibit a non - monotonous dispersion with Cu concentration and interpreted with the support of hopping mechanism and Maxwell-Wagner type of interfacial polarization. The ac conductivity of nanoferrites increases with raising the frequency. Complex electrical modulus reveals a non - Debye type of dielectric relaxation present in nanoferrites. Reactive impedance (Z″) detected an anomalous behavior and is related with resonance effect. Complex impedance demonstrates one semicircle corresponding to the intergrain (grain boundary) resistance and also explains conducting nature of nanoferrites. For x = 0.2, a large semicircle is observed revealing the ohmic nature (minimum potential drop at electrode surface). Dielectric properties were improved for nanoferrites with x = 0.2 and is due to high dielectric constant, conductivity and minimum loss value (∼0.009) at 1 MHz.

Nanophase cobalt, nickel and zinc ferrites: synchrotron XAS study on the crystallite size dependence of metal distribution.

PubMed

Nordhei, Camilla; Ramstad, Astrid Lund; Nicholson, David G

2008-02-21

Nanophase cobalt, nickel and zinc ferrites, in which the crystallites are in the size range 4-25 nm, were synthesised by coprecipitation and subsequent annealing. X-Ray absorption spectroscopy using synchrotron radiation (supported by X-ray powder diffraction) was used to study the effects of particle size on the distributions of the metal atoms over the tetrahedral and octahedral sites of the spinel structure. Deviations from the bulk structure were found which are attributed to the significant influence of the surface on very small particles. Like the bulk material, nickel ferrite is an inverse spinel in the nanoregime, although the population of metals on the octahedral sites increases with decreasing particle size. Cobalt ferrite and zinc ferrite take the inverse and normal forms of the spinel structure respectively, but within the nanoregime both systems show similar trends in being partially inverted. Further, in zinc ferrite, unlike the normal bulk structure, the nanophase system involves mixed coordinations of zinc(ii) and iron(iii) consistent with increasing partial inversion with size.

Estimation of lattice strain in nanocrystalline RuO2 by Williamson-Hall and size-strain plot methods.

PubMed

Sivakami, R; Dhanuskodi, S; Karvembu, R

2016-01-05

RuO2 nanoparticles (RuO2 NPs) have been successfully synthesized by the hydrothermal method. Structure and the particle size have been determined by X-ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscopy (AFM) and transmission electron microscopy (TEM). UV-Vis spectra reveal that the optical band gap of RuO2 nanoparticles is red shifted from 3.95 to 3.55eV. BET measurements show a high specific surface area (SSA) of 118-133m(2)/g and pore diameter (10-25nm) has been estimated by Barret-Joyner-Halenda (BJH) method. The crystallite size and lattice strain in the samples have been investigated by Williamson-Hall (W-H) analysis assuming uniform deformation, deformation stress and deformation energy density, and the size-strain plot method. All other relevant physical parameters including stress, strain and energy density have been calculated. The average crystallite size and the lattice strain evaluated from XRD measurements are in good agreement with the results of TEM. Copyright © 2015 Elsevier B.V. All rights reserved.

In situ SAXS study on size changes of platinum nanoparticles with temperature

NASA Astrophysics Data System (ADS)

Wang, W.; Chen, X.; Cai, Q.; Mo, G.; Jiang, L. S.; Zhang, K.; Chen, Z. J.; Wu, Z. H.; Pan, W.

2008-09-01

Poly(vinylpyrrolidone) (PVP)-coated platinum (Pt) nanoparticles were prepared in methanol-water reduction method. In situ small-angle X-ray scattering (SAXS) and X-ray diffraction (XRD) techniques were used to probe the size change of particles and crystallites with temperature. Tangent-by-tangent (TBT) method of SAXS data analysis was improved and used to get the particle size distribution (PSD) from SAXS intensity. Scherrer’s equation was used to derive the crystallite size from XRD pattern. Combining SAXS and XRD results, a step-like characteristic of the Pt nanoparticle growth has been found. Three stages (diffusion, aggregation, and agglomeration) can be used to describe the growth of the Pt nanoparticles and nanocrystallites. Aggregation was found to be the main growth mode of the Pt nanoparticles during heating. The maximum growth rates of Pt nanoparticles and Pt nanocrystallites, as well as the maximum aggregation degree of Pt nanocrystallites were found, respectively, at 250 °C, 350 °C and 300 °C. These results are helpful to understanding the growth mode of nanoparticles, as well as controlling the nanoparticle size.

STRUCTURAL, SURFACE MORPHOLOGICAL AND MAGNETIC STUDIES OF Zn1-xFexS (x=0.00-0.10) DILUTED MAGNETIC SEMICONDUCTORS GROWN BY CO-PRECIPITATION METHOD

NASA Astrophysics Data System (ADS)

Hassan, M.; Ghazanfar, M.; Arooj, N.; Riaz, S.; Hussain, S. Sajjad; Naseem, S.

We have fabricated Zn1-xFexS (x=0.00, 0.02, 0.04, 0.06, 0.08 and 0.10) diluted magnetic semiconductors using co-precipitation method. X-ray diffraction patterns depict that Zn1-xFexS appears as a dominant phase with cubic zinc blende structure and nanoscale crystallite size. In addition, a secondary phase of rhombohedral ZnS also appears; however, no additional phase arises that primarily belongs to Fe dopant. Using Debye-Scherrer relation, the crystallite size is found to be in the range of 20-27nm, which is in good agreement with the crystallite size calculated using the Williamson-Hall (WH) plot method. The appearance of secondary phase provoked to study the residual strain using Stokes-Wilson equation, which is nearly consistent to that observed using WH plot method. The surface morphology, revealed using scanning electron microscopy, depicts non-uniform surface structure with a variety of grains and void dimensions. Hysteresis loops measured for Zn1-xFexS at room temperature (RT) illustrate a paramagnetic behavior at higher fields; however, small ferromagnetic behavior is evident due to the small openings of the measured hysteresis loops around the origin. The measured RT ferromagnetism reveals the potential spintronic device applications of the studied diluted magnetic semiconductors.

Method and article of manufacture corresponding to a composite comprised of ultra nonacrystalline diamond, metal, and other nanocarbons useful for thermoelectric and other applications

DOEpatents

Gruen, Dieter M.

2010-05-18

One provides (101) disperse ultra-nanocrystalline diamond powder material that comprises a plurality of substantially ordered crystallites that are each sized no larger than about 10 nanometers. One then reacts (102) these crystallites with a metallic component. The resultant nanowire is then able to exhibit a desired increase with respect to its ability to conduct electricity while also substantially preserving the thermal conductivity behavior of the disperse ultra-nanocrystalline diamond powder material. The reaction process can comprise combining (201) the crystallites with one or more metal salts in an aqueous solution and then heating (203) that aqueous solution to remove the water. This heating can occur in a reducing atmosphere (comprising, for example, hydrogen and/or methane) to also reduce the salt to metal.

Shear induced orientation of edible fat and chocolate crystals

NASA Astrophysics Data System (ADS)

Mazzanti, Gianfranco; Welch, Sarah E.; Marangoni, Alejandro G.; Sirota, Eric B.; Idziak, Stefan H. J.

2003-03-01

Shear-induced orientation of fat crystallites was observed during crystallization of cocoa butter, milk fat, stripped milk fat and palm oil. This universal effect was observed in systems crystallized under high shear. The minor polar components naturally present in milk fat were found to decrease the shear-induced orientation effect in this system. The competition between Brownian and shear forces, described by the Peclet number, determines the crystallite orientation. The critical radius size, from the Gibbs-Thomson equation, provides a tool to understand the effect of shear at the onset stages of crystallization.

Synthesis and Characterization of Some Alkaline-Earth-Oxide Nanoparticles

NASA Astrophysics Data System (ADS)

Singh, Jitendra Pal; Lim, Weon Cheol; Won, Sung Ok; Song, Jonghan; Chae, Keun Hwa

2018-04-01

The present work reports the synthesis of MgO and CaO nanoparticles by using the sol-gel autocombustion method. The annealing of the precursor at 1200 °C was observed to lead the formation of MgO nanoparticles having average crystallite size of 31 nm. Annealing the precursor at same temperature produced materials having a CaO phase with a minor impure phase of calcium carbonate ( 3%). The crystallite size corresponding to the CaO phase was 38 nm. A change of thermal history in the precursor was observed not to result in an improvement of the CaO phase. The change of thermal history in the precursor gave rise to mixed phases of CaCO3 and Ca(OH)2 rather than the phase of CaO. Further, annealing at 1200 °C for 12 h resulted in the formation of the CaO phase along with almost 1 - 5% of calcium hydroxide as an impurity phase. X-ray absorption spectroscopic measurements carried out on these materials revealed that the local electronic/atomic structure of these oxides was not only affected by the impurity phases but also influenced by the carbaneous impurities attached to the crystallites.

Effect of Mg2+ on acidic calcium phosphate phases grown by electrodeposition

NASA Astrophysics Data System (ADS)

Correia, Matheus Bento; Júnior, José Pedro Gualberto; Macedo, Michelle Cardinale S. S.; Resende, Cristiane Xavier; dos Santos, Euler Araujo

2017-10-01

In this work, the effect of Mg2+ ions on the electrodeposition of dicalcium phosphate dihydrate (DCPD), octacalcium phosphate (OCP) and calcium-deficient hydroxyapatite (CDHA) crystals on a commercially pure titanium (cp-Ti) substrate was evaluated. We demonstrated that Mg2+ ions could change the morphology of the coatings by inhibiting the growth rate of the OCP and CDHA crystals and diminishing the crystallite size of DCPD. The inhibition effect on OCP and CDHA was most likely due to a surface adsorption mechanism since no evidence of a doping process was observed using Rietveld refinement and electron diffraction analyses. Conversely, the presence of Mg2+ ions generated a favorable condition for the nucleation of a new Mg2+-rich DCPD crystal population, presenting smaller crystallite sizes.

Raman validity for crystallite size La determination on reticulated vitreous carbon with different graphitization index

NASA Astrophysics Data System (ADS)

Baldan, M. R.; Almeida, E. C.; Azevedo, A. F.; Gonçalves, E. S.; Rezende, M. C.; Ferreira, N. G.

2007-11-01

The graphitization index provided by X-ray diffraction (XRD) and Raman spectrometry for reticulated vitreous carbon (RVC) substrates, carbonized at different heat treatment temperatures (HTT), is investigated. A systematic study of the dependence between the disorder-induced D and G Raman bands is presented. The crystallite size La was obtained for both X-ray diffraction and Raman spectrometry techniques. Particularly, the validity for La determination, from Raman spectra, is pointed out comparing the commonly used formula based on peaks amplitude ratio ( ID/ IG) and the recent proposed equation that uses the integrated intensities of D and G bands. The results discrepancy is discussed taken into account the strong contribution of the line broadening presented in carbon materials heat treated below 2000 °C.

Characterization of synthetic nanocrystalline mackinawite: crystal structure, particle size, and specific surface area

PubMed Central

Jeong, Hoon Y.; Lee, Jun H.; Hayes, Kim F.

2010-01-01

Iron sulfide was synthesized by reacting aqueous solutions of sodium sulfide and ferrous chloride for 3 days. By X-ray powder diffraction (XRPD), the resultant phase was determined to be primarily nanocrystalline mackinawite (space group: P4/nmm) with unit cell parameters a = b = 3.67 Å and c = 5.20 Å. Iron K-edge XAS analysis also indicated the dominance of mackinawite. Lattice expansion of synthetic mackinawite was observed along the c-axis relative to well-crystalline mackinawite. Compared with relatively short-aged phase, the mackinawite prepared here was composed of larger crystallites with less elongated lattice spacings. The direct observation of lattice fringes by HR-TEM verified the applicability of Bragg diffraction in determining the lattice parameters of nanocrystalline mackinawite from XRPD patterns. Estimated particle size and external specific surface area (SSAext) of nanocrystalline mackinawite varied significantly with the methods used. The use of Scherrer equation for measuring crystallite size based on XRPD patterns is limited by uncertainty of the Scherrer constant (K) due to the presence of polydisperse particles. The presence of polycrystalline particles may also lead to inaccurate particle size estimation by Scherrer equation, given that crystallite and particle sizes are not equivalent. The TEM observation yielded the smallest SSAext of 103 m2/g. This measurement was not representative of dispersed particles due to particle aggregation from drying during sample preparation. In contrast, EGME method and PCS measurement yielded higher SSAext (276–345 m2/g by EGME and 424 ± 130 m2/g by PCS). These were in reasonable agreement with those previously measured by the methods insensitive to particle aggregation. PMID:21085620

Synthesis of nanometer-size inorganic materials for the examination of particle size effects on heterogeneous catalysis

NASA Astrophysics Data System (ADS)

Emerson, Sean Christian

The effect of acoustic and hydrodynamic cavitation on the precipitation of inorganic catalytic materials, specifically titania supported gold, was investigated. The overall objective was to understand the fundamental factors involved in synthesizing nanometer-size catalytic materials in the 1--10 nm range in a cavitating field. Materials with grain sizes in this range have been associated with enhanced catalytic activity compared to larger grain size materials. A new chemical approach was used to produce titania supported gold by co-precipitation with higher gold yields compared to other synthesis methods. Using this approach, it was determined that acoustic cavitation was unable to influence the gold mean crystallite size compared to non-sonicated catalysts. However, gold concentration on the catalysts was found to be very important for CO oxidation activity. By decreasing the gold concentration from a weight loading of 0.50% down to approximately 0.05%, the rate of reaction per mole of gold was found to increase by a factor of 19. Hydrodynamic cavitation at low pressures (6.9--48 bar) was determined to have no effect on gold crystallite size at a fixed gold content for the same precipitation technique used in the acoustic cavitation studies. By changing the chemistry of the precipitation system, however, it was found that a synergy existed between the dilution of the gold precursor solution, the orifice diameter, and the reducing agent addition rate. Individually, these factors were found to have little effect and only their interaction allowed gold grain size control in the range of 8--80 nm. Further modification of the system chemistry and the use of hydrodynamic cavitation at pressures in excess of 690 bar allowed the systematic control of gold crystallite size in the range of 2--9 nm for catalysts containing 2.27 +/- 0.17% gold. In addition, it was shown that the enhanced mixing due to cavitation led to larger gold yields compared to classical syntheses. The control of gold grain size was gained at the loss of CO activity, which was attributed to the formation of non-removable sodium titanate species. The increased mixing associated with cavitation contributed to the activity loss by partially burying the gold and incorporating more of the sodium titanate species into the catalysts. This work produced the first evidence of hydrodynamic cavitation influencing the gold crystallite size on titania supported gold catalysts and is the only study reporting the control of grain size by simple mechanical adjustment of the experimental parameters. Despite the low activity observed due to sodium titanate, the methodology of adjusting the chemistry of a precipitating system could be used to eliminate such species. The approach of modifying the chemical precipitation kinetics relative to the dynamics of cavitation offers a general scheme for future research on cavitational processing effects.

Size dependent polaronic conduction in hematite

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

Sharma, Monika; Banday, Azeem; Murugavel, Sevi

2016-05-23

Lithium Ion Batteries have been attracted as the major renewable energy source for all portable electronic devices because of its advantages like superior energy density, high theoretical capacity, high specific energy, stable cycling and less memory effects. Recently, α-Fe{sub 2}O{sub 3} has been considered as a potential anode material due to high specific capacity, low cost, high abundance and environmental benignity. We have synthesized α-Fe{sub 2}O{sub 3} with various sizes by using the ball milling and sol-gel procedure. Here, we report the dc conductivity measurement for the crystallite size ranging from 15 nm to 50 nm. It has been observedmore » that the enhancement in the polaronic conductivity nearly two orders in magnitude while reducing the crystallite size from bulk into nano scale level. The enhancement in the conductivity is due to the augmented to compressive strain developed in the material which leads to pronounced decrease in the hopping length of polarons. Thus, nanocrystaline α-Fe{sub 2}O{sub 3} may be a better alternative anode material for lithium ion batteries than earlier reported systems.« less

Variation of Strontium (Sr) in the Ferroelectric Material Barium Strontium Titanate (Ba1-xSrxTiO3) by Co precipitation Method

NASA Astrophysics Data System (ADS)

Subarwanti, Y.; Safitri, R. D.; Supriyanto, A.; Iriani, Y.; Jamaludin, A.

2017-02-01

Barium Strontium Titanate (BST) have been made with variation strontium (Sr) 10%, 30% and 50% by co-precipitation method. This study aims to determine influence addition Sr against the crystal structure, crystallite size, lattice parameter, grain size and dielectric constant. Samples have been made by co-precipitation method and then the samples were sintered by furnace at 1100°C with holding time 4 hours. Characterization of BST use X-Ray Diffraction instrument, Scanning Electron Microscopy and Resistance Capacitance Inductance (RCL meter). Based on result obtained, the larger Sr content cause the diffraction angle shift to the right (the greater) and crystallinity increasing. But, the value of dielectric constant, crystallite size and grain size decreasing with additional Sr content. Measurement of dielectric constant (K) performed in the frequency range 1 kHz to 100 kHz and the highest value at Sr content 0.1 i.e. 258.35. The addition of Sr content 30% and 50% change the crystal structure from tetragonal to cubic which has paraelectric phase.

Improved magnetic and electrical properties of Cu doped Fe-Ni invar alloys synthesized by chemical reduction technique

NASA Astrophysics Data System (ADS)

Ahmad, Sajjad; Ziya, Amer Bashir; Ashiq, Muhammad Naeem; Ibrahim, Ather; Atiq, Shabbar; Ahmad, Naseeb; Shakeel, Muhammad; Khan, Muhammad Azhar

2016-12-01

Fe-Ni-Cu invar alloys of various compositions (Fe65Ni35-xCux, x=0, 0.2, 0.6, 1, 1.4 and 1.8) were synthesized via chemical reduction route. These alloys were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and vibrating sample magnetometry (VSM) techniques. The XRD analysis revealed the formation of face centered cubic (fcc) structure. The lattice parameter and the crystallite size of the investigated alloys were calculated and the line broadening indicated the nano-crystallites size of alloy powder. The particle size was estimated from SEM and it decreases by the incorporation of Cu and found to be in the range of 24-40 nm. The addition of Cu in these alloys appreciably enhances the saturation magnetization and it increases from 99 to 123 emu/g. Electrical conductivity has been improved with Cu addition. The thermal conductivity was calculated using the Wiedemann-Franz law.

Effect of oxidizer to fuel molar ratio on particle size and DC conductivity of CeO{sub 2} nanoparticles

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

Harish, B. M.; Rajeeva, M. P.; Naveen, C. S.

2016-05-06

Cerium oxide nanoparticles were synthesized by solution combustion method with varying the oxidizer (cerium nitrate hexa hydrate) to fuel (Glycine) molar ratio. The prepared samples were characterized by UV-visible spectrometer, X-ray diffractometer (XRD), Scanning electron microscope (SEM) and Energy dispersive X-Ray analysis (EDAX). XRD pattern reveals the formation of cubic fluorite structure of CeO{sub 2}. It was observed that finest crystallites were found at extreme fuel-deficient condition and it is good enough to produce favorable powder characteristics. The average crystallite size was found to be 14.46 nm to 21.57 nm. The temperature dependent dc conductivity was carried out using Keithleymore » source meter between the temperature range from 300 K to 573 K. From this study it was found that the conductivity increases with increase of temperature due to semiconducting behavior of CeO{sub 2} and it decreases with particle size due to increase in the energy band gap.« less

Self-composite comprised of nanocrystalline diamond and a non-diamond component useful for thermoelectric applications

DOEpatents

Gruen, Dieter M.

2012-09-04

One provides nanocrystalline diamond material that comprises a plurality of substantially ordered diamond crystallites that are sized no larger than about 10 nanometers. One then disposes a non-diamond component within the nanocrystalline diamond material. By one approach this non-diamond component comprises an electrical conductor that is formed at the grain boundaries that separate the diamond crystallites from one another. The resultant nanowire is then able to exhibit a desired increase with respect to its ability to conduct electricity while also preserving the thermal conductivity behavior of the nanocrystalline diamond material.

Self-composite comprised of nanocrystalline diamond and a non-diamond component useful for thermoelectric applications

DOEpatents

Gruen, Dieter M [Downers Grove, IL

2009-08-11

One provides nanocrystalline diamond material that comprises a plurality of substantially ordered diamond crystallites that are sized no larger than about 10 nanometers. One then disposes a non-diamond component within the nanocrystalline diamond material. By one approach this non-diamond component comprises an electrical conductor that is formed at the grain boundaries that separate the diamond crystallites from one another. The resultant nanowire is then able to exhibit a desired increase with respect to its ability to conduct electricity while also preserving the thermal conductivity behavior of the nanocrystalline diamond material.

Effect of fluorine doping on highly transparent conductive spray deposited nanocrystalline tin oxide thin films

NASA Astrophysics Data System (ADS)

Moholkar, A. V.; Pawar, S. M.; Rajpure, K. Y.; Bhosale, C. H.; Kim, J. H.

2009-09-01

The undoped and fluorine doped thin films are synthesized by using cost-effective spray pyrolysis technique. The dependence of optical, structural and electrical properties of SnO 2 films, on the concentration of fluorine is reported. Optical absorption, X-ray diffraction, scanning electron microscope (SEM) and Hall effect studies have been performed on SnO 2:F (FTO) films coated on glass substrates. The film thickness varies from 800 to 1572 nm. X-ray diffraction pattern reveals the presence of cassiterite structure with (2 0 0) preferential orientation for FTO films. The crystallite size varies from 35 to 66 nm. SEM and AFM study reveals the surface of FTO to be made of nanocrystalline particles. The electrical study reveals that the films are degenerate and exhibit n-type electrical conductivity. The 20 wt% F doped film has a minimum resistivity of 3.8 × 10 -4 Ω cm, carrier density of 24.9 × 10 20 cm -3 and mobility of 6.59 cm 2 V -1 s -1. The sprayed FTO film having minimum resistance of 3.42 Ω/cm 2, highest figure of merit of 6.18 × 10 -2 Ω -1 at 550 nm and 96% IR reflectivity suggest, these films are useful as conducting layers in electrochromic and photovoltaic devices and also as the passive counter electrode.

Empirical test of an illite/muscovite 40Ar/39Ar thermochronometer

NASA Astrophysics Data System (ADS)

Verdel, C.; van der Pluijm, B. A.; Niemi, N. A.; Hall, C. M.

2010-12-01

Minerals which both preserve age information and indicate metamorphic conditions are particularly useful in thermochronology. Variations in sub-greenschist facies metamorphism have traditionally been quantified in terms of the illite to muscovite transition, a transformation which involves the growth of crystallites of increasing thickness at higher metamorphic temperatures. Thickness variations may influence Ar retention within these K-rich minerals, both in nature and during neutron irradiation. Along a transect in the southwestern US from the Grand Canyon to Death Valley, metamorphic conditions of a stratigraphic interval (the Middle Cambrian Bright Angel Shale and laterally equivalent Carrara Fm.) range from zeolite facies in the east to greenschist facies in the west, as determined by estimating illite crystallite thickness with X-ray diffraction. 40Ar/39Ar step-heating experiments were conducted on illite/muscovite-rich, micron to submicron grain sizes of these shales that were encapsulated in quartz tubes prior to irradiation. The proportion of 39Ar expelled during irradiation decreases in these samples as both crystallite thickness and grain size increases. Spectra from the least metamorphosed samples (diagenetic zone) are staircase-shaped and reach maximum ages that appear to reflect the age of detrital muscovite. Spectra from the highest grade samples (epizone) display partial plateaus and yield much younger maximum ages. Based on these findings we conclude that Ar can escape from illite via two processes: loss from low retention sites on crystallite edges and c-axis perpendicular volume diffusion. Based on our empirical data, the closure temperature of illite appears to lie at or near the anchizone-epizone bounday, or roughly 200-300 °C. Illite/muscovite thickness and 40Ar/39Ar data may therefore be useful for studies of detrital muscovite geochronology in very low grade shales and as a thermochronometer for higher grade pelites.

Influence of metal work function and incorporation of Sr atom on WO3 thin films for MIS and MIM structured SBDs

NASA Astrophysics Data System (ADS)

Marnadu, R.; Chandrasekaran, J.; Raja, M.; Balaji, M.; Maruthamuthu, S.; Balraju, P.

2018-07-01

In this work, two different structure of Cu/Sr-WO3/p-Si metal-insulator-semiconductor (MIS) and Cu/Sr-WO3/FTO metal-insulator-metal (MIM) Schottky barrier diodes (SBDs) fabricated with an insulating layer of pure tungsten trioxide (WO3) and Sr-WO3 thin films have been reported. The Sr-WO3 layer was coated separately, with different concentrations (0, 4, 8 and 12 wt %) of strontium (Sr) via jet nebulizer spray pyrolysis technique (JNSP) on the p-type silica wafer (p-Si) and fluorine doped tin oxide (FTO) substrates which are been optimized at 400 °C. The XRD analysis reveals the multiphase crystalline structures for 12 wt % of Sr-WO3 film with higher average crystallite size. FE-SEM images show the randomly oriented sub-microsized slab and seashell like structures. Higher surface roughness with improved grain size for 12 wt % of Sr-WO3 film. The presence of W, O and Sr atoms was confirmed by EDX spectra. In optical studies, Maximum absorption with minimum optical band gap was observed for 12 wt % of Sr-WO3 composite film. There was a linear increase in the electrical conductivity of the films with higher wt. % of Sr. Evidently the activation energy decreased with Sr concentration which is in accordance with the bandgap values. The fitting results of the measured I-V, reveal that MIS (SBDs) under illumination condition have minimum ideality factor (n = 2.39) and maximum barrier height (Φb = 0.57) values for higher concentration (12 wt %) of Sr film compared to MIM SBDs.

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

Tahir, Dahlang, E-mail: dtahir@fmipa.unhas.ac.id; Bakri, Fahrul; Liong, Syarifuddin

We have studied the molecular properties, structural properties, and chemical composition of composites by Fourier transform infrared (FTIR) spectroscopy, X-ray diffraction (XRD) spectroscopy, and X-ray fluorescence (XRF) spectroscopy, respectively. FTIR spectra shows absorption band of hydroxyl group (-OH), methyl group (-CH{sub 3}) and aromatic group (C-C). The absorption band for aromatic group (C-C) shows the formation of carbonaceous in composites. XRF shows chemical composition of composites, which the main chemicals are SO{sub 3}, Cl, and ZnO. The loss on ignition value (LOI) of activated charcoal indicates high carbonaceous matter. The crystallite size for diffraction pattern from hydrogel polymer is aboutmore » 17 nm and for activated charcoal are about 19 nm. The crystallite size of the polymer is lower than that of activated charcoal, which make possible of the particle from filler in contact with each other to form continuous conducting polymer through polymer matrix.« less

Morphological and XPS study of ball milled Fe1-xAlx (0.3≤x≤0.6) alloys

NASA Astrophysics Data System (ADS)

Rajan, Sandeep; Kumar, Anil; Vyas, Anupam; Brajpuriya, Ranjeet

2018-05-01

The paper presents mechanical and XPS study of ball milled Fe1-xAlx (0.3≤x≤0.6) alloys. The author prepared the solid solution of Fe(Al) with different composition of Al by using mechanical alloying (MA) technique. The MA process induces a progressive dissolution of Al into Fe, resulted in the formation of an extended Fe(Al) solid solution with the bcc structure after 5 hr of milling. The SEM Images shows that the initial shape of particles disappeared completely, and their structure became a mixture of small and large angular-shaped crystallites with different sizes. The TEM micrograph also confirms the reduction in crystallite size and alloy formation. XPS study shows the shift in the binding energy position of both Fe and Al Peaks provide strong evidence of Fe(Al) phase formation after milling.

Microstructural changes in CdSe-coated ZnO nanowires evaluated by in situ annealing in transmission electron microscopy and x-ray diffraction

NASA Astrophysics Data System (ADS)

Majidi, Hasti; Winkler, Christopher R.; Taheri, Mitra L.; Baxter, Jason B.

2012-07-01

We report on the crystallite growth and phase change of electrodeposited CdSe coatings on ZnO nanowires during annealing. Both in situ transmission electron microscopy (TEM) and x-ray diffraction (XRD) reveal that the nanocrystal size increases from ˜3 to ˜10 nm upon annealing at 350 °C for 1 h and then to more than 30 nm during another 1 h at 400 °C, exhibiting two distinct growth regimes. Nanocrystal growth occurs together with a structural change from zinc blende to wurtzite. The structural transition begins at 350 °C, which results in the formation of stacking faults. Increased crystallite size, comparable to the coating thickness, can improve charge separation in extremely thin absorber solar cells. We demonstrate a nearly two-fold improvement in power conversion efficiency upon annealing.

Synthesis and characterization of nanocrystalline Co-Fe-Nb-Ta-B alloy

NASA Astrophysics Data System (ADS)

Raanaei, Hossein; Fakhraee, Morteza

2017-09-01

In this research work, structural and magnetic evolution of Co57Fe13Nb8Ta4B18 alloy, during mechanical alloying process, have been investigated by using, X-ray diffraction, scanning electron microscopy, transmission electron microscopy, electron dispersive X-ray spectroscopy, differential thermal analysis and also vibrating sample magnetometer. It is observed that at 120 milling time, the crystallite size reaches to about 7.8 nm. Structural analyses show that, the solid solution of the initial powder mixture occurs at160 h milling time. The coercivity behavior demonstrates a rise, up to 70 h followed by decreasing tendency up to final stage of milling process. Thermal analysis of 160 h milling time sample reveals two endothermic peaks. The characterization of annealed milled sample for 160 h milling time at 427 °C shows crystallite size growth accompanied by increasing in saturation magnetization.

IN SITU Deposition of Fe-TiC Nanocomposite on Steel by Laser Cladding

NASA Astrophysics Data System (ADS)

Razavi, Mansour; Rahimipour, Mohammad Reza; Ganji, Mojdeh; Ganjali, Mansoreh; Gangali, Monireh

The possibility of deposition of Fe-TiC nanocomposite on the surface of carbon steel substrate with the laser coating method had been investigated. Mechanical milling was used for the preparation of raw materials. The mixture of milled powders was used as a coating material on the substrate steel surface and a CO2 laser was used in continuous mode for coating. Microstructural studies were performed by scanning electron microscopy. Determinations of produced phases, crystallite size and mean strain have been done by X-ray diffraction. The hardness and wear resistance of coated samples were measured. The results showed that the in situ formation of Fe-TiC nanocomposite coating using laser method is possible. This coating has been successfully used to improve the hardness and wear resistance of the substrate so that the hardness increased by about six times. Coated iron and titanium carbide crystallite sizes were in the nanometer scale.

Scaling effects in sodium zirconium silicate phosphate (Na 1+ xZr 2Si xP 3- xO 12) ion-conducting thin films

DOE PAGES

Ihlefeld, Jon F.; Gurniak, Emily; Jones, Brad H.; ...

2016-05-04

Preparation of sodium zirconium silicate phosphate (NaSICon), Na 1+xZr 2Si xP 3–xO 12 (0.25 ≤ x ≤ 1.0), thin films has been investigated via a chemical solution approach on platinized silicon substrates. Increasing the silicon content resulted in a reduction in the crystallite size and a reduction in the measured ionic conductivity. Processing temperature was also found to affect microstructure and ionic conductivity with higher processing temperatures resulting in larger crystallite sizes and higher ionic conductivities. The highest room temperature sodium ion conductivity was measured for an x = 0.25 composition at 2.3 × 10 –5 S/cm. In conclusion, themore » decreasing ionic conductivity trends with increasing silicon content and decreasing processing temperature are consistent with grain boundary and defect scattering of conducting ions.« less

Defect structure in electrodeposited nanocrystalline Ni layers with different Mo concentrations

NASA Astrophysics Data System (ADS)

Kapoor, Garima; Péter, László; Fekete, Éva; Gubicza, Jenő

2018-05-01

The effect of molybdenum (Mo) alloying on the lattice defect structure in electrodeposited nanocrystalline nickel (Ni) films was studied. The electrodeposited layers were prepared on copper substrate at room temperature, with a constant current density and pH value. The chemical composition of these layers was determined by EDS. In addition, X-ray diffraction line profile analysis was carried out to study the microstructural parameters such as the crystallite size, the dislocation density and the stacking fault probability. It was found that the higher Mo content yielded more than one order of magnitude larger dislocation density while the crystallite size was only slightly smaller. In addition, the twin boundary formation activity during deposition increased with increasing Mo concentration. The results obtained on electrodeposited layers were compared with previous research carried out on bulk nanocrystalline Ni-Mo materials with similar compositions but processed by severe plastic deformation.

Raman analysis of an impacted α-GeO2-H2O mixture

NASA Astrophysics Data System (ADS)

Rosales, Ivonne; Thions-Renero, Claude; Martinez, Erendira; Agulló-Rueda, Fernando; Bucio, Lauro; Orozco, Eligio

2012-09-01

Through a Raman analysis, we detected polymorphism at high pressure on mixtures of α-GeO2 microcrystalline powder and water under impact experiments with a single-stage gas gun. The Raman measurements taken from recovered samples show two vibrational modes associated with water-related species. After the impact, the size of the α-GeO2 crystallites was approximately 10 times higher showing molten zones and a lot of porous faces. Raman examination showed some unknown peaks possibly associated with other GeO2 polymorphs detected by X-ray diffraction experiments and perhaps stabilized in the porous of the α-GeO2 crystallites.

Structural and dielectric studies of Ce doped BaSnO3 perovskite nanostructures

NASA Astrophysics Data System (ADS)

Angel, S. Lilly; Deepa, K.; Rajamanickam, N.; Jayakumar, K.; Ramachandran, K.

2018-04-01

Undoped and Cerium (Ce) doped BaSnO3(BSO) nanostructures were synthesized by co-precipitation method. The cubic structure and perovskite phase were confirmed by X-ray diffraction (XRD). The crystallite size of BSO is 41nm and when Ce ion concentration is increased, the crystallite sizesdecreased. The nanocube, nanocuboids and nanorods are observed from SEM analysis. The purity of the undoped and doped samples are confirmed by EDS spectrum. For larger defects, wide band gap was obtained from UV-Vis and PL spectrum. The dielectric constants are increased at low frequencies when Ce impurities are introduced in the BSO matrix at Sn site.

Size dependent behavior of Fe 3O 4 crystals during electrochemical (de)lithiation: an in situ X-ray diffraction, ex situ X-ray absorption spectroscopy, transmission electron microscopy and theoretical investigation

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

Bock, David C.; Pelliccione, Christopher J.; Zhang, Wei

Here, the iron oxide magnetite, Fe 3O 4, is a promising conversion type lithium ion battery anode material due to its high natural abundance, low cost and high theoretical capacity. While the close packing of ions in the inverse spinel structure of Fe 3O 4 enables high energy density, it also limits the kinetics of lithium ion diffusion in the material. Nanosizing of Fe 3O 4 to reduce the diffusion path length is an effective strategy for overcoming this issue and results in improved rate capability. However, the impact of nanosizing on the multiple structural transformations that occur during themore » electrochemical (de)lithiation reaction in Fe 3O 4 is poorly understood. In this study, the influence of crystallite size on the lithiation-conversion mechanisms in Fe 3O 4 is investigated using complementary X-ray techniques along with transmission electron microscopy (TEM) and continuum level simulations on electrodes of two different Fe 3O 4 crystallite sizes. In situ X-ray diffraction (XRD) measurements were utilized to track the changes to the crystalline phases during (de)lithiation. X-ray absorption spectroscopy (XAS) measurements at multiple points during the (de)lithiation processes provided local electronic and atomic structural information. Tracking the crystalline and nanocrystalline phases during the first (de)lithiation provides experimental evidence that (1) the lithiation mechanism is non-uniform and dependent on crystallite size, where increased Li + diffusion length in larger crystals results in conversion to Fe 0 metal while insertion of Li + into spinel-Fe 3O 4 is still occurring, and (2) the disorder and size of the Fe metal domains formed when either material is fully lithiated impacts the homogeneity of the FeO phase formed during the subsequent delithiation.« less

Size dependent behavior of Fe 3O 4 crystals during electrochemical (de)lithiation: an in situ X-ray diffraction, ex situ X-ray absorption spectroscopy, transmission electron microscopy and theoretical investigation

DOE PAGES

Bock, David C.; Pelliccione, Christopher J.; Zhang, Wei; ...

2017-07-17

Here, the iron oxide magnetite, Fe 3O 4, is a promising conversion type lithium ion battery anode material due to its high natural abundance, low cost and high theoretical capacity. While the close packing of ions in the inverse spinel structure of Fe 3O 4 enables high energy density, it also limits the kinetics of lithium ion diffusion in the material. Nanosizing of Fe 3O 4 to reduce the diffusion path length is an effective strategy for overcoming this issue and results in improved rate capability. However, the impact of nanosizing on the multiple structural transformations that occur during themore » electrochemical (de)lithiation reaction in Fe 3O 4 is poorly understood. In this study, the influence of crystallite size on the lithiation-conversion mechanisms in Fe 3O 4 is investigated using complementary X-ray techniques along with transmission electron microscopy (TEM) and continuum level simulations on electrodes of two different Fe 3O 4 crystallite sizes. In situ X-ray diffraction (XRD) measurements were utilized to track the changes to the crystalline phases during (de)lithiation. X-ray absorption spectroscopy (XAS) measurements at multiple points during the (de)lithiation processes provided local electronic and atomic structural information. Tracking the crystalline and nanocrystalline phases during the first (de)lithiation provides experimental evidence that (1) the lithiation mechanism is non-uniform and dependent on crystallite size, where increased Li + diffusion length in larger crystals results in conversion to Fe 0 metal while insertion of Li + into spinel-Fe 3O 4 is still occurring, and (2) the disorder and size of the Fe metal domains formed when either material is fully lithiated impacts the homogeneity of the FeO phase formed during the subsequent delithiation.« less

High throughput, high resolution enzymatic lithography process: effect of crystallite size, moisture, and enzyme concentration.

PubMed

Mao, Zhantong; Ganesh, Manoj; Bucaro, Michael; Smolianski, Igor; Gross, Richard A; Lyons, Alan M

2014-12-08

By bringing enzymes into contact with predefined regions of a surface, a polymer film can be selectively degraded to form desired patterns that find a variety of applications in biotechnology and electronics. This so-called "enzymatic lithography" is an environmentally friendly process as it does not require actinic radiation or synthetic chemicals to develop the patterns. A significant challenge to using enzymatic lithography has been the need to restrict the mobility of the enzyme in order to maintain control of feature sizes. Previous approaches have resulted in low throughput and were limited to polymer films only a few nanometers thick. In this paper, we demonstrate an enzymatic lithography system based on Candida antartica lipase B (CALB) and poly(ε-caprolactone) (PCL) that can resolve fine-scale features, (<1 μm across) in thick (0.1-2.0 μm) polymer films. A Polymer Pen Lithography (PPL) tool was developed to deposit an aqueous solution of CALB onto a spin-cast PCL film. Immobilization of the enzyme on the polymer surface was monitored using fluorescence microscopy by labeling CALB with FITC. The crystallite size in the PCL films was systematically varied; small crystallites resulted in significantly faster etch rates (20 nm/min) and the ability to resolve smaller features (as fine as 1 μm). The effect of printing conditions and relative humidity during incubation is also presented. Patterns formed in the PCL film were transferred to an underlying copper foil demonstrating a "Green" approach to the fabrication of printed circuit boards.

Synthesis and structural characterization of nano-hydroxyapatite biomaterials prepared by microwave processing

NASA Astrophysics Data System (ADS)

Ramli, Rosmamuhamadani; Arawi, Ainaa Zafirah Omar; Talari, Mahesh Kumar; Mahat, Mohd Muzamir; Jais, Umi Sarah

2012-07-01

Synthetic hydroxyapatite, (HA, Ca10(PO4)6(OH)2), is an attractive and widely utilized bio-ceramic material for orthopedic and dental implants because of its close resemblance of native tooth and bone crystal structure. Synthetic HA exhibits excellent osteoconductive properties. Osteoconductivity means the ability to provide the appropriate scaffold or template for bone formation. Calcium phosphate biomaterials [(HA), tri-calcium phosphate (TCP) and biphasic calcium phosphate (HA/TCP)] with appropriate three-dimensional geometry are able to bind and concentrate endogenous bone morphogenetic proteins in circulation, and may become osteoinductive and can be effective carriers of bone cell seeds. This HA can be used in bio-implants as well as drug delivery application due to the unique properties of HA. Biomaterials synthesized from the natural species like mussel shells have additional benefits such as high purity, less expensive and high bio compatibility. In this project, HA-nanoparticles of different crystallite size were prepared by microwave synthesis of precursors. High purity CaO was extracted from the natural mussel shells for the synthesis of nano HA. Dried nano HA powders were analyzed using X-Ray Diffraction (XRD) technique for the determination of crystal structure and impurity content. Scanning Electron Microscopic (SEM) investigation was employed for the morphological investigation of nano HA powders. From the results obtained, it was concluded that by altering the irradiation time, nano HA powders of different crystallite sizes and morphologies could be produced. Crystallite sizes calculated from the XRD patterns are found to be in the range of 10-55 nm depending on the irradiation time.

The Effect of Crystallite Size and Texture on the Strength of MgGeO3 Post-Perovskite

NASA Astrophysics Data System (ADS)

Miyagi, Lowell

2011-06-01

In-situ radial synchrotron x-ray diffraction is used to measure lattice strain and lattice preferred orientation (texture) in MgGeO3 post-perovskite synthesized and deformed in the diamond anvil cell up to 135 GPa. Lattice strains are used to calculate differential stress supported by the sample and can provide a lower bounds estimate on yield strength. MgGeO3 post-perovskite synthesized from the enstatite phase exhibits a weak transformation texture of (100) planes at high angles to the direction of compression. In a sample with larger crystallites, pressure increase and deformation results in (001) lattice planes orienting nearly perpendicular to compression, consistent with dominant (001) slip. In another sample with smaller crystallites it is difficult to induce texture change, and differential stress is higher than in the sample with larger crystallites. When MgGeO3 post-perovskite is synthesized from the perovskite phase a different transformation texture of (001) planes at high angles to compression is observed. This sample is able to support large differential stress as the direction perpendicular to the (001) plane is a plastically hard orientation for MgGeO3 post-perovskite. This work was supported by the Carnegie DOE Alliance Center and a Bateman fellowship at Yale University.

Synthesis and characterization of nano-sized zirconia powder synthesized by single emulsion-assisted direct precipitation.

PubMed

Chandra, Navin; Singh, Deepesh Kumar; Sharma, Meenakshi; Upadhyay, Ravi Kant; Amritphale, S S; Sanghi, S K

2010-02-15

For the first time, single reverse microemulsion-assisted direct precipitation route has been successfully used to synthesize tetragonal zirconia nanoparticles in narrow size range. The synthesized powder was characterized using FT-IR, XRD and HRTEM techniques. The zirconia nanoparticles obtained were spherical in shape and has narrow particle size distribution in the range of 13-31nm and crystallite size in the range of 13-23nm. Copyright 2009 Elsevier Inc. All rights reserved.

Synthesis, characterization and magnetic properties of nanocrystalline FexNi80-xCo20 ternary alloys

NASA Astrophysics Data System (ADS)

Dalavi, Shankar B.; Theerthagiri, J.; Raja, M. Manivel; Panda, R. N.

2013-10-01

Fe-Ni-Co alloys of various compositions (FexNi80-xCo20,x=20-50) were synthesized by using a sodium borohydride reduction route. The phase purity and crystallite size was ascertained by using powder X-ray diffraction (XRD). The alloys crystallize in the face centered cubic (fcc) structure with lattice parameters, a=3.546-3.558 Å. The XRD line broadening indicates the fine particle nature of the materials. The estimated crystallite sizes were found to be 27.5, 27, 24, and 22.8 nm for x=20, 30, 40, and 50; alloys respectively. Scanning electron micrograph studies indicates particle sizes to be in the range of 83-60 nm for Fe-Ni-Co alloys. The values of saturation magnetization for FexNi80-xCo20 are found to be in the range of 54.3-41.2 emu/g and are significantly lower than the bulk values (175-180 emu/g). The coercivity decreases from 170 to 122 Oe with decrease in Fe content. The observed magnetic behavior has been explained on the basis of size, surface effects, spin canting and the presence of superparamagnetic fractions in the ultrafine materials.

Synthesis, Optical and Structural Properties of Copper Sulfide Nanocrystals from Single Molecule Precursors

PubMed Central

Ajibade, Peter A.; Botha, Nandipha L.

2017-01-01

We report the synthesis and structural studies of copper sulfide nanocrystals from copper (II) dithiocarbamate single molecule precursors. The precursors were thermolysed in hexadecylamine (HDA) to prepare HDA-capped CuS nanocrystals. The optical properties of the nanocrystals studied using UV–visible and photoluminescence spectroscopy showed absorption band edges at 287 nm that are blue shifted, and the photoluminescence spectra show emission curves that are red-shifted with respect to the absorption band edges. These shifts are as a result of the small crystallite sizes of the nanoparticles leading to quantum size effects. The structural studies were carried out using powder X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), and atomic force microscopy. The XRD patterns indicates that the CuS nanocrystals are in hexagonal covellite crystalline phases with estimated particles sizes of 17.3–18.6 nm. The TEM images showed particles with almost spherical or rod shapes, with average crystallite sizes of 3–9.8 nm. SEM images showed morphology with ball-like microspheres on the surfaces, and EDS spectra confirmed the presence of CuS nanoparticles. PMID:28336865

Study of mesoporous CdS-quantum-dot-sensitized TiO2 films by using X-ray photoelectron spectroscopy and AFM

PubMed Central

Wojcieszak, Robert; Raj, Gijo

2014-01-01

Summary CdS quantum dots were grown on mesoporous TiO2 films by successive ionic layer adsorption and reaction processes in order to obtain CdS particles of various sizes. AFM analysis shows that the growth of the CdS particles is a two-step process. The first step is the formation of new crystallites at each deposition cycle. In the next step the pre-deposited crystallites grow to form larger aggregates. Special attention is paid to the estimation of the CdS particle size by X-ray photoelectron spectroscopy (XPS). Among the classical methods of characterization the XPS model is described in detail. In order to make an attempt to validate the XPS model, the results are compared to those obtained from AFM analysis and to the evolution of the band gap energy of the CdS nanoparticles as obtained by UV–vis spectroscopy. The results showed that XPS technique is a powerful tool in the estimation of the CdS particle size. In conjunction with these results, a very good correlation has been found between the number of deposition cycles and the particle size. PMID:24605274

Structure and morphology evolution of silica-modified pseudoboehmite aerogels during heat treatment

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

Pakharukova, V.P., E-mail: verapakh@catalysis.ru; Novosibirsk State University, Pirogova Street 2, 630090 Novosibirsk; Research and Educational Center for Energy Efficient Catalysis, Novosibirsk State University, Novosibirsk 630090

Silica-modified pseudoboehmite aerogels (0, 10, 20 at% of Si) were prepared by sol–gel method followed by supercritical drying. The phase transformations, changes in structure and morphology upon calcination were thoroughly investigated by advanced X-Ray diffraction (XRD) techniques and high-resolution transmission electron microscopy (HRTEM). Obtained pseudoboehmite samples had specific nanostructure: ultrathin two-dimensional (2D) crystallites were loosely packed. The silica dopant drastically enhanced the crystallite anisotropy. Thus, the aerogel with Al:Si atomic ratio of 9:1 consisted of the pseudoboehmite nanosheets with thickness of one unit cell (average dimensions of 14.0×1.2×14.5 nm). The specific nanostructure caused remarkable features of experimental XRD patterns, includingmore » anisotropic peak broadening and appearance of forbidden reflection. Direct simulation of XRD patterns with using the Debye Scattering Equation allowed the size and morphology of pseudoboehmite crystallites to be determined. The silica addition strongly delayed formation of γ-alumina and further phase transformations upon calcinaton. Thermal stability of alumina was suggested to be affected by the particle morphology inherited from the pseudoboehmite precursor. - Graphical abstract: Pseudoboehmite samples had specific nanostructure: ultrathin two-dimensional (2D) crystallites were loosely packed. - Highlights: • Silica-doped boehmites were prepared by sol–gel method with supercritical drying. • Ultrathin two-dimensional crystallites of pseudoboehmite were obtained. • Changes in structure and morphology upon calcination were studied. • Simulation of XRD patterns was performed with use of the Debye Scattering Equation. • Thermal stability of alumina depended on morphology inherited from pseudoboehmite.« less

Fabrication of nano ZrO2 dispersed novel W79Ni10Ti5Nb5 alloy by mechanical alloying and pressureless sintering

NASA Astrophysics Data System (ADS)

Sahoo, R. R.; Patra, A.; Karak, S. K.

2017-02-01

A high energy planetary ball-mill was employed to synthesize tungsten (W) based alloy with nominal composition of W79Ni10Ti5Nb5(ZrO2)1 (in wt. %) for 20 h with chrome steel as grinding media, toluene as process control agent (PCA) along with compaction at 500 MPa pressure for 5 mins and sintering at 1500°C for 2 h using Ar atmosphere. X-ray diffraction (XRD), Scanning electron microscopy (SEM), Energy dispersive spectroscopy (EDS), elemental mapping and Transmission electron microscopy (TEM) was used to study the phase formation, microstructure of both milled powder and consolidated alloy. The crystallite size of W in W79Ni10Ti5Nb5(ZrO2)1 powder was 37 nm, 14.7 nm at 10 h and 20 h of milling respectively and lattice strain enhances to 0.54% at 20 h of milling. The crystallite size reduction is more at 10 h of milling and the rate drop beyond 10 to 20 h of milling. The intense improvement in dislocation density was evident upto 10 h of milling and the rate decreases between 10 to 20 h of milling. Increase in the lattice parameter of tungsten in W79Ni10Ti5Nb5(ZrO2)1 alloy upto 0.09% was observed at 10 h of milling owing to severe stress assisted deformation followed by contraction upto 0.07% at 20 h of milling due to formation of solid solution. The large spherical particles at 0 h of milling transformed to elongated shape at 10 h of milling and finer morphology at 20 h of milling. The average particle size reduced from 100 µm to 4.5 µm with the progress of milling from 0 to 20 h. Formation of fine polycrystallites of W was revealed by bright field TEM analysis and the observed crystallite size from TEM study was well supported by the evaluated crystallite size from XRD. XRD pattern and SEM micrograph of sintered alloy revealed the formation of NbNi, Ni3Ti intermetallic phases. Densification of 91.5% was attained in the 20 h milled and sintered alloy. Mechanical behaviour of the sintered product was evaluated by hardness and wear study. W79Ni10Ti5Nb5(ZrO2)1 alloy showed increase in hardness with decreasing load. The wear rate increases with increasing load due to higher abrasion effect at higher load.

Structural and magnetic properties of cobalt-doped iron oxide nanoparticles prepared by solution combustion method for biomedical applications.

PubMed

Venkatesan, Kaliyamoorthy; Rajan Babu, Dhanakotti; Kavya Bai, Mane Prabhu; Supriya, Ravi; Vidya, Radhakrishnan; Madeswaran, Saminathan; Anandan, Pandurangan; Arivanandhan, Mukannan; Hayakawa, Yasuhiro

2015-01-01

Cobalt-doped iron oxide nanoparticles were prepared by solution combustion technique. The structural and magnetic properties of the prepared samples were also investigated. The average crystallite size of cobalt ferrite (CoFe2O4) magnetic nanoparticle was calculated using Scherrer equation, and it was found to be 16±5 nm. The particle size was measured by transmission electron microscope. This value was found to match with the crystallite size calculated by Scherrer equation corresponding to the prominent intensity peak (311) of X-ray diffraction. The high-resolution transmission electron microscope image shows clear lattice fringes and high crystallinity of cobalt ferrite magnetic nanoparticles. The synthesized magnetic nanoparticles exhibited the saturation magnetization value of 47 emu/g and coercivity of 947 Oe. The anti-microbial activity of cobalt ferrite nanoparticles showed better results as an anti-bacterial agent. The affinity constant was determined for the nanoparticles, and the cytotoxicity studies were conducted for the cobalt ferrite nanoparticles at different concentrations and the results are discussed.

Leaf size and surface characteristics of Betula papyrifera exposed to elevated CO2 and O3.

PubMed

Riikonen, Johanna; Percy, Kevin E; Kivimäenpää, Minna; Kubiske, Mark E; Nelson, Neil D; Vapaavuori, Elina; Karnosky, David F

2010-04-01

Betula papyrifera trees were exposed to elevated concentrations of CO(2) (1.4 x ambient), O(3) (1.2 x ambient) or CO(2) + O(3) at the Aspen Free-air CO(2) Enrichment Experiment. The treatment effects on leaf surface characteristics were studied after nine years of tree exposure. CO(2) and O(3) increased epidermal cell size and reduced epidermal cell density but leaf size was not altered. Stomatal density remained unaffected, but stomatal index increased under elevated CO(2). Cuticular ridges and epicuticular wax crystallites were less evident under CO(2) and CO(2) + O(3). The increase in amorphous deposits, particularly under CO(2) + O(3,) was associated with the appearance of elongated plate crystallites in stomatal chambers. Increased proportions of alkyl esters resulted from increased esterification of fatty acids and alcohols under elevated CO(2) + O(3). The combination of elevated CO(2) and O(3) resulted in different responses than expected under exposure to CO(2) or O(3) alone. 2009 Elsevier Ltd. All rights reserved.

Pre-coalescence scaling of graphene island sizes

NASA Astrophysics Data System (ADS)

Das, Shantanu; Drucker, Jeff

2018-05-01

Graphene grown using cold-wall chemical vapor deposition on Cu surfaces follows a classical nucleation and growth mechanism. Following nucleation at the earliest growth stages, isolated crystallites grow, impinge, and coalesce to form a continuous layer. During the pre-coalescence growth regime, the size distributions of graphene crystallites exhibit scaling of the form N(s) = θ/⟨s⟩2 g(s/⟨s⟩), where s is the island area, θ is the graphene coverage, ⟨s⟩ is the average island area, N is the areal density, and g(x) is a scaling function. For graphene grown on Cu surfaces that have been annealed in a reducing Ar + H2 ambient, excellent data collapse onto a universal Avrami scaling function is observed irrespective of graphene coverage, surface roughness, or Cu grain size. This result is interpreted to indicate attachment-limited growth and desorption of diffusing C-containing species. Graphene grown on Cu surfaces that were annealed in a non-reducing environment exhibits a qualitatively different scaling function, indicating diffusion-limited growth with a lower attachment barrier combined with C detachment from the graphene edges.

Structural and magnetic properties of cobalt-doped iron oxide nanoparticles prepared by solution combustion method for biomedical applications

PubMed Central

Venkatesan, Kaliyamoorthy; Rajan Babu, Dhanakotti; Kavya Bai, Mane Prabhu; Supriya, Ravi; Vidya, Radhakrishnan; Madeswaran, Saminathan; Anandan, Pandurangan; Arivanandhan, Mukannan; Hayakawa, Yasuhiro

2015-01-01

Cobalt-doped iron oxide nanoparticles were prepared by solution combustion technique. The structural and magnetic properties of the prepared samples were also investigated. The average crystallite size of cobalt ferrite (CoFe2O4) magnetic nanoparticle was calculated using Scherrer equation, and it was found to be 16±5 nm. The particle size was measured by transmission electron microscope. This value was found to match with the crystallite size calculated by Scherrer equation corresponding to the prominent intensity peak (311) of X-ray diffraction. The high-resolution transmission electron microscope image shows clear lattice fringes and high crystallinity of cobalt ferrite magnetic nanoparticles. The synthesized magnetic nanoparticles exhibited the saturation magnetization value of 47 emu/g and coercivity of 947 Oe. The anti-microbial activity of cobalt ferrite nanoparticles showed better results as an anti-bacterial agent. The affinity constant was determined for the nanoparticles, and the cytotoxicity studies were conducted for the cobalt ferrite nanoparticles at different concentrations and the results are discussed. PMID:26491320

Microstress, strain, band gap tuning and photocatalytic properties of thermally annealed and Cu-doped ZnO nanoparticles

NASA Astrophysics Data System (ADS)

Prasad, Neena; V. M. M, Saipavitra; Swaminathan, Hariharan; Thangaraj, Pandiyarajan; Ramalinga Viswanathan, Mangalaraja; Balasubramanian, Karthikeyan

2016-06-01

ZnO nanoparticles and Cu-doped ZnO nanoparticles were prepared by co-precipitation method. Also, a part of the pure ZnO nanoparticles were annealed at 750 °C for 3, 6, and 9 h. X-ray diffraction studies were carried out and the lattice parameters, unit cell volume, interplanar spacing, and Young's modulus were calculated for all the samples, and also the crystallite size was found using the Scherrer method. X-ray peak broadening analysis was used to estimate the crystallite sizes and the strain using the Williamson-Hall (W-H) method and the size-strain plot (SSP) method. Stress and the energy density were calculated using the W-H method assuming different models such as uniform deformation model, uniform strain deformation model, uniform deformation energy density model, and the SSP method. Optical absorption properties of the samples were understood from their UV-visible spectra. Photocatalytic activities of ZnO and 5 % Cu-doped ZnO were observed by the degradation of methylene blue dye in aqueous medium under the irradiation of 20-W compact fluorescent lamp for an hour.

Microstructural characterization of high-manganese austenitic steels with different stacking fault energies

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

Sato, Shigeo, E-mail: s.sato@imr.tohoku.ac.jp; Kwon, Eui-Pyo; Imafuku, Muneyuki

Microstructures of tensile-deformed high-manganese austenitic steels exhibiting twinning-induced plasticity were analyzed by electron backscatter diffraction pattern observation and X-ray diffraction measurement to examine the influence of differences in their stacking fault energies on twinning activity during deformation. The steel specimen with the low stacking fault energy of 15 mJ/m{sup 2} had a microstructure with a high population of mechanical twins than the steel specimen with the high stacking fault energy (25 mJ/m{sup 2}). The <111> and <100> fibers developed along the tensile axis, and mechanical twinning occurred preferentially in the <111> fiber. The Schmid factors for slip and twinning deformationsmore » can explain the origin of higher twinning activity in the <111> fiber. However, the high stacking fault energy suppresses the twinning activity even in the <111> fiber. A line profile analysis based on the X-ray diffraction data revealed the relationship between the characteristics of the deformed microstructures and the stacking fault energies of the steel specimens. Although the variation in dislocation density with the tensile deformation is not affected by the stacking fault energies, the effect of the stacking fault energies on the crystallite size refinement becomes significant with a decrease in the stacking fault energies. Moreover, the stacking fault probability, which was estimated from a peak-shift analysis of the 111 and 200 diffractions, was high for the specimen with low stacking fault energy. Regardless of the difference in the stacking fault energies of the steel specimens, the refined crystallite size has a certain correlation with the stacking fault probability, indicating that whether the deformation-induced crystallite-size refinement occurs depends directly on the stacking fault probability rather than on the stacking fault energies in the present steel specimens. - Highlights: {yields} We studied effects of stacking fault energies on deformed microstructures of steels. {yields} Correlations between texture and occurrence of mechanical twinning are discussed. {yields} Evolutions of dislocations and crystallite are analyzed by line profile analysis.« less

Nanostructured TiO2 and ZnO prepared by using pressurized hot water and their eco-toxicological evaluation

NASA Astrophysics Data System (ADS)

Troppová, Ivana; Matějová, Lenka; Sezimová, Hana; Matěj, Zdeněk; Peikertová, Pavlína; Lang, Jaroslav

2017-06-01

The eco-toxicological effects of unconventionally prepared nanostructured TiO2 and ZnO were evaluated in this study, since both oxides are keenly investigated semiconductor photocatalysts in the last three decades. Unconventional processing by pressurized hot water was applied in order to crystallize oxide materials as an alternative to standard calcination. Acute biological toxicity of the synthesized oxides was evaluated using germination of Sinapis alba seed (ISO 11269-1) and growth of Lemna minor fronds (ISO 20079) and was compared to commercially available TiO2 Degussa P25. Toxicity results revealed that synthesized ZnO as well as TiO2 is toxic contrary to commercial TiO2 Degussa P25 which showled stimulation effect to L. minor and no toxicity to S. alba. ZnO was significantly more toxic than TiO2. The effect of crystallite size was considered, and it was revealed that small crystallite size and large surface area are not the toxicity-determining factors. Factors such as the rate of nanosized crystallites aggregation and concentration, shape and surface properties of TiO2 nanoparticles affect TiO2 toxicity to both plant species. Seriously, the dissolution of Ti4+ ions from TiO2 was also observed which may contribute to its toxicity. In case of ZnO, the dissolution of Zn2+ ions stays the main cause of its toxicity.

Origin of high carrier mobility and low residual stress in RF superimposed DC sputtered Al doped ZnO thin film for next generation flexible devices

NASA Astrophysics Data System (ADS)

Kumar, Naveen; Dubey, Ashish; Bahrami, Behzad; Venkatesan, S.; Qiao, Qiquan; Kumar, Mukesh

2018-04-01

In this work, the energy and flux of high energetic ions were controlled by RF superimposed DC sputtering process to increase the grain size and suppress grain boundary potential with minimum residual stress in Al doped ZnO (AZO) thin film. AZO thin films were deposited at different RF/(RF + DC) ratios by keeping total power same and were investigated for their electrical, optical, structural and nanoscale grain boundaries potential. All AZO thin film showed high crystallinity and orientation along (002) with peak shift as RF/(RF + DC) ratio increased from 0.0, pure DC, to 1.0, pure RF. This peak shift was correlated with high residual stress in as-grown thin film. AZO thin film grown at mixed RF/(RF + DC) of 0.75 showed high electron mobility, low residual stress and large crystallite size in comparison to other AZO thin films. The nanoscale grain boundary potential was mapped using Kelvin Probe Force Microscopy in all AZO thin film and it was observed that carrier mobility is controlled not only by grains size but also by grain boundary potential. The XPS analysis confirms the variation in oxygen vacancies and zinc interstitials which explain the origin of low grain boundaries potential and high carrier mobility in AZO thin film deposited at 0.75 RF/(RF + DC) ratio. This study proposes a new way to control the grain size and grain boundary potential to further tune the optoelectronic-mechanical properties of AZO thin films for next generation flexible and optoelectronic devices.

Detrital illite crystals identified from crystallite thickness measurements in siliciclastic sediments

USGS Publications Warehouse

Aldega, L.; Eberl, D.D.

2005-01-01

Illite crystals in siliciclastic sediments are heterogeneous assemblages of detrital material coming from various source rocks and, at paleotemperatures >70 ??C, of superimposed diagenetic modification in the parent sediment. We distinguished the relative proportions of 2M1 detrital illite and possible diagenetic 1Md + 1M illite by a combined analysis of crystal-size distribution and illite polytype quantification. We found that the proportions of 1Md + 1M and 2M1 illite could be determined from crystallite thickness measurements (BWA method, using the MudMaster program) by unmixing measured crystallite thickness distributions using theoretical and calculated log-normal and/or asymptotic distributions. The end-member components that we used to unmix the measured distributions were three asymptotic-shaped distributions (assumed to be the diagenetic component of the mixture, the 1Md + 1M polytypes) calculated using the Galoper program (Phase A was simulated using 500 crystals per cycle of nucleation and growth, Phase B = 333/cycle, and Phase C = 250/ cycle), and one theoretical log-normal distribution (Phase D, assumed to approximate the detrital 2M1 component of the mixture). In addition, quantitative polytype analysis was carried out using the RockJock software for comparison. The two techniques gave comparable results (r2 = 0.93), which indicates that the unmixing method permits one to calculate the proportion of illite polytypes and, therefore, the proportion of 2M1 detrital illite, from crystallite thickness measurements. The overall illite crystallite thicknesses in the samples were found to be a function of the relative proportions of thick 2M1 and thin 1Md + 1M illite. The percentage of illite layers in I-S mixed layers correlates with the mean crystallite thickness of the 1Md + 1M polytypes, indicating that these polytypes, rather than the 2M1 polytype, participate in I-S mixed layering.

Laser-Gyro Materials Studies

DTIC Science & Technology

1986-03-01

mean-square (rms) have been measured on fused quartz and Zerodur surfaces polished by manufacturers of ring- laser gyros. The measurements were made...Sizes and Percent Crystallinity of Laser Gyro Materials. Crystallite Crystallinity, Material size, :-100 A ±10 vol% Zerodur 800 79 Quartz 500 53...Based on t data presented in this rel ort, Cervit, Zerodur , and RLA 559,122 from Corning Glass Works have acceptable material properties for laser

Factors Influencing Ferrihydrite Crystallinity In Natural And Synthetic Systems

EPA Science Inventory

Recent investigations of the structure of the mineral ferrihydrite indicate that disparities in the number of peaks observed in powder x-ray diffraction patterns can be attributed to differences in crystallite size. This has lead to the conclusion that specimens previously refer...

A bottom-up building process of nanostructured La0.75Sr0.25Cr0.5Mn0.5O3-δ electrodes for symmetrical-solid oxide fuel cell: Synthesis, characterization and electrocatalytic testing

NASA Astrophysics Data System (ADS)

Chanquía, Corina M.; Montenegro-Hernández, Alejandra; Troiani, Horacio E.; Caneiro, Alberto

2014-01-01

Pure-phase La0.75Sr0.25Cr0.5Mn0.5O3-δ (LSCM) nanocrystallites have been successfully synthesized by the combustion method, employing glycine as fuel and complexing agent, and ammonium nitrate as combustion trigger. A detailed morphological and structural characterization is performed, by using of X-ray diffraction, N2 physisorption and electron microscopy. The LSCM material consists in interconnected nanocrystallites (∼30 nm) forming a sponge-like structure with meso and macropores, being its specific surface area around 10 m2 g-1. Crystalline structural analyses show that the LSCM nanopowder has trigonal/rhombohedral symmetry in the R-3c space group. By employing the spin coating technique and quick-stuck thermal treatments of the ink-electrolyte, electrodes with different crystallite size (95, 160 and 325 nm) are built onto both sides of the La0.8Sr0.2Ga0.8Mg0.2O3-δ-disk electrolyte. To test the influence of the electrode crystallite size on the electrocatalytic behavior of the symmetrical cells, electrochemical impedance spectroscopy measurements at 800 °C were performed. When the electrode crystallite size becomes smaller, the area specific resistance decreases from 3.6 to 1.31 Ω cm2 under 0.2O2-0.8Ar atmosphere, possibly due to the enlarging of the triple-phase boundary, while this value increases from 7.04 to 13.78 Ω cm2 under 0.17H2-0.03H2O-0.8Ar atmosphere, probably due to thermodynamic instability of the LSCM nanocrystallites.

Facile synthesis of both needle-like and spherical hydroxyapatite nanoparticles: effect of synthetic temperature and calcination on morphology, crystallite size and crystallinity.

PubMed

Wijesinghe, W P S L; Mantilaka, M M M G P G; Premalal, E V A; Herath, H M T U; Mahalingam, S; Edirisinghe, M; Rajapakse, R P V J; Rajapakse, R M G

2014-09-01

Synthetic hydroxyapatite (HA) nanoparticles, that mimic natural HA, are widely used as biocompatible coatings on prostheses to repair and substitute human bones. In this study, HA nanoparticles are prepared by precipitating them from a precursor solution containing calcium sucrate and ammonium dihydrogen orthophosphate, at a Ca/P mole ratio of 1.67:1, at temperatures, ranging from 10°C to 95°C. A set of products, prepared at different temperatures, is analyzed for their crystallinity, crystallite size, morphology, thermal stability and composition, by X-ray diffraction (XRD), scanning electron microscopy (SEM), thermogravimetric analysis (TGA) and Fourier transform infrared (FT-IR) spectroscopic techniques, while the other set is analyzed after calcining the respective products, soon after their synthesis, for 3h, at 700°C. The as-prepared products, after 2h of drying, without any calcination, are not crystalline, but they grow very slowly into needle-like morphologies, as they are ripened with time. The percentage crystallinity of the final products increases from 15% to 52%, with increasing the preparative temperature. The calcined samples always produce spherical nanoparticles of essentially the same diameter, between 90 nm and 100 nm, which does not change due to aging and preparative temperatures. Therefore, the same method can be utilized to synthesize both spherical and needle-like nanoparticles of hydroxyapatite, with well-defined sizes and shapes. The ability to use readily available cheap raw materials, for the synthesis of such well-defined crystallites of hydroxyapatite, is an added advantage of this method, which may be explored further for the scaling up of the procedures to suit to industrial scale synthesis of such hydroxyapatite nanoparticles. Copyright © 2014 Elsevier B.V. All rights reserved.

Synthesis of [Zn-Al-CO 3] layered double hydroxides by a coprecipitation method under steady-state conditions

NASA Astrophysics Data System (ADS)

Chang, Z.; Evans, D. G.; Duan, X.; Vial, C.; Ghanbaja, J.; Prevot, V.; de Roy, M.; Forano, C.

2005-09-01

A continuous co-precipitation method under steady-state conditions has been investigated for the preparation of nanometer-size layered double hydroxide (LDH) particles using Zn 2Al(OH) 6(CO 3) 0.5·2H 2O as a prototype. The objective was to shorten the preparation time by working without an aging step, using a short and controlled residence time in order to maintain a constant supersaturation level in the reactor and constant particle properties in the exit stream over time. The effects of varying the operating conditions on the structural and textural properties of the LDHs have been studied, including total cation concentration, solvent, residence time, pH and intercalation anion. The products have been characterized using ICP, XRD, FTIR, BET, SEM and TEM. The LDHs prepared by the continuous coprecipitation method have a poorer crystallinity and lower crystallite sizes than those synthesized by the conventional batch method. The results have shown that increasing either cation concentration or the fraction of monoethylene glycol (MEG) in MEG/H 2O mixtures up to 80% (v/v) affect salt solubility and supersaturation, which gives rise to smaller crystallites, larger surface areas and more amorphous compounds. This increase is however limited by the precipitation of zinc and aluminum hydroxides occurring around a total cation concentration of 3.0×10 -1 M in pure water and 3.0×10 -2 M in H 2O/EtOH mixtures. Crystallite size increases with residence time, suggesting a precipitation process controlled by growth. Finally, the continuous coprecipitation method under steady-state conditions has been shown to be a promising alternative to the traditional coprecipitation technique in either pure water or mixed H 2O/MEG solvents.

Nucleation and growth of single layer graphene on electrodeposited Cu by cold wall chemical vapor deposition

NASA Astrophysics Data System (ADS)

Das, Shantanu; Drucker, Jeff

2017-03-01

The nucleation density and average size of graphene crystallites grown using cold wall chemical vapor deposition (CVD) on 4 μm thick Cu films electrodeposited on W substrates can be tuned by varying growth parameters. Growth at a fixed substrate temperature of 1000 °C and total pressure of 700 Torr using Ar, H2 and CH4 mixtures enabled the contribution of total flow rate, CH4:H2 ratio and dilution of the CH4/H2 mixture by Ar to be identified. The largest variation in nucleation density was obtained by varying the CH4:H2 ratio. The observed morphological changes are analogous to those that would be expected if the deposition rate were varied at fixed substrate temperature for physical deposition using thermal evaporation. The graphene crystallite boundary morphology progresses from irregular/jagged through convex hexagonal to regular hexagonal as the effective C deposition rate decreases. This observation suggests that edge diffusion of C atoms along the crystallite boundaries, in addition to H2 etching, may contribute to shape evolution of the graphene crystallites. These results demonstrate that graphene grown using cold wall CVD follows a nucleation and growth mechanism similar to hot wall CVD. As a consequence, the vast knowledge base relevant to hot wall CVD may be exploited for graphene synthesis by the industrially preferable cold wall method.

Effect of the microstructure on electrical properties of high-purity germanium

NASA Astrophysics Data System (ADS)

Podkopaev, O. I.; Shimanskii, A. F.; Molotkovskaya, N. O.; Kulakovskaya, T. V.

2013-05-01

The interrelation between the electrical properties and the microstructure of high-purity germanium crystals has been revealed. The electrical conductivity of polycrystalline samples increases and the life-time of nonequilibrium charge carriers in them decreases with a decrease in the crystallite sizes.

Extraction of effective solid-liquid interfacial free energies for full 3D solid crystallites from equilibrium MD simulations

DOE PAGES

Zepeda-Ruiz, L. A.; Sadigh, B.; Chernov, A. A.; ...

2017-11-21

Molecular dynamics simulations of an embedded atom copper system in the NPH ensemble are used to study the e ective solid-liquid interfacial free energy of quasispherical solid crystals within a liquid. This is within the larger context of MD simulations of this system undergoing solidi cation, where single individually-prepared crystallites of di erent sizes grow until they reach a thermodynamically stable nal state. The resulting equilibrium shapes possess the full structural details expected for solids with weakly anisotropic surface free energies (in these cases, ~5 % radial attening and rounded [111] octahedral faces). The simplifying assumption of sphericity and perfectmore » isotropy leads to an e ective interfacial free energy as appearing in the Gibbs-Thomson equation, which we determine to be ~179 erg/cm 2, roughly independent of crystal size for radii in the 50 - 250 A range. This quantity may be used in atomistically-informed models of solidi cation kinetics for this system.« less

Catalyst support of mixed cerium zirconium titanium oxide, including use and method of making

DOEpatents

Willigan, Rhonda R [Manchester, CT; Vanderspurt, Thomas Henry [Glastonbury, CT; Tulyani, Sonia [Manchester, CT; Radhakrishnan, Rakesh [Vernon, CT; Opalka, Susanne Marie [Glastonbury, CT; Emerson, Sean C [Broad Brook, CT

2011-01-18

A durable catalyst support/catalyst is capable of extended water gas shift operation under conditions of high temperature, pressure, and sulfur levels. The support is a homogeneous, nanocrystalline, mixed metal oxide of at least three metals, the first being cerium, the second being Zr, and/or Hf, and the third importantly being Ti, the three metals comprising at least 80% of the metal constituents of the mixed metal oxide and the Ti being present in a range of 5% to 45% by metals-only atomic percent of the mixed metal oxide. The mixed metal oxide has an average crystallite size less than 6 nm and forms a skeletal structure with pores whose diameters are in the range of 4-9 nm and normally greater than the average crystallite size. The surface area of the skeletal structure per volume of the material of the structure is greater than about 240 m.sup.2/cm.sup.3. The method of making and use are also described.

Control of crystallite orientation and size in Fe and FeCo nanoneedles.

PubMed

Mendoza-Reséndez, Raquel; Luna, Carlos; Barriga-Castro, Enrique Diaz; Bonville, Pierre; Serna, Carlos J

2012-06-08

Uniform magnetic nanoneedles have been prepared by hydrogen reduction of elongated nanoarchitectures. These precursors are as-prepared or cobalt-coated aggregates of highly oriented haematite nanocrystals (∼5 nm). The final materials are flattened nanoneedles formed by chains of assembled Fe or FeCo single-domain nanocrystals. The microstructural properties of such nanoneedles were tailored using renewed and improved synthetic strategies. In this fashion, the needle elongation and composition, the crystallite size (from 15 up to 30 nm), the nanocrystal orientation (with the 〈110〉 or 〈001〉 directions roughly along the long axis of the nanoneedle) and their type of arrangement (single chains, frustrated double chains and double chains) were controlled by modifying the reduction time, the axial ratio of the precursor haematite and the presence of additional coatings of aluminum or yttrium compounds. The values of the coercivity H(C) found for these nanoneedles are compared with the values predicted by the chain of spheres model assuming a symmetric fanning mechanism for magnetization reversal.

The effect of temperature deposited on the performance of ZnO-CNT-graphite for supercapacitors

NASA Astrophysics Data System (ADS)

Darari, Alfin; Hakim, Istajib S.; Priyono; Subagio, Agus; Pardoyo; Subhan, Achmad

2017-07-01

Carbon nanotubes (CNTs), graphite are now widely studied as the electrodes of supercapacitor, owing to their high conductivity, large surface area, chemical stability, etc. A lot of research has been focused on Carbon/metal oxide nanocomposite electrode for Electrode supercapacitor because it will increase the total capacitance. In this research, ZnO nanoparticles were deposited onto substrate CNT:Graphite in different temperatures such as 300°, 350°, and 400°C. The characterization of the crystal size using X-Ray Diffraction (XRD) patterns showed ZnO material peak was detected a ZnO crystallite. The size of ZnO crystallite in 300°, 350°, and 400°C consecutively is 101.1; 103.4; and 116.7 nm. The test results are Electrochemical impedance spectrometry (EIS) high electrical conductivity values obtained on the composition of ZnO-CNT-graphite with a temperature of 350°C 4.6 (S/m); and (2) the highest value of capacitance in 300°C is 1.23 F/g.

Extraction of effective solid-liquid interfacial free energies for full 3D solid crystallites from equilibrium MD simulations

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

Zepeda-Ruiz, L. A.; Sadigh, B.; Chernov, A. A.

Molecular dynamics simulations of an embedded atom copper system in the NPH ensemble are used to study the e ective solid-liquid interfacial free energy of quasispherical solid crystals within a liquid. This is within the larger context of MD simulations of this system undergoing solidi cation, where single individually-prepared crystallites of di erent sizes grow until they reach a thermodynamically stable nal state. The resulting equilibrium shapes possess the full structural details expected for solids with weakly anisotropic surface free energies (in these cases, ~5 % radial attening and rounded [111] octahedral faces). The simplifying assumption of sphericity and perfectmore » isotropy leads to an e ective interfacial free energy as appearing in the Gibbs-Thomson equation, which we determine to be ~179 erg/cm 2, roughly independent of crystal size for radii in the 50 - 250 A range. This quantity may be used in atomistically-informed models of solidi cation kinetics for this system.« less

Metalorganic Chemical Vapor Deposition of Ruthenium-Doped Diamond like Carbon Films

NASA Technical Reports Server (NTRS)

Sunkara, M. K.; Ueno, M.; Lian, G.; Dickey, E. C.

2001-01-01

We investigated metalorganic precursor deposition using a Microwave Electron Cyclotron Resonance (ECR) plasma for depositing metal-doped diamondlike carbon films. Specifically, the deposition of ruthenium doped diamondlike carbon films was investigated using the decomposition of a novel ruthenium precursor, Bis(ethylcyclopentadienyl)-ruthenium (Ru(C5H4C2H5)2). The ruthenium precursor was introduced close to the substrate stage. The substrate was independently biased using an applied RF power. Films were characterized using Fourier Transform Infrared Spectroscopy (FTIR), Transmission Electron Microscopy (TEM) and Four Point Probe. The conductivity of the films deposited using ruthenium precursor showed strong dependency on the deposition parameters such as pressure. Ruthenium doped sample showed the presence of diamond crystallites with an average size of approx. 3 nm while un-doped diamondlike carbon sample showed the presence of diamond crystallites with an average size of 11 nm. TEM results showed that ruthenium was atomically dispersed within the amorphous carbon network in the films.

Synthesis, surface chemistry and pseudocapacitance mechanisms of VN nanocrystals derived by a simple two-step halide approach

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

Choi, Daiwon; Jampani, Prashanth H.; Jayakody, J. R. P.

Chloroamide precursors generated via a simple two-step ammonolysis reaction of transition metal chloride in the liquid phase at room temperature were heat treated in ammonia at moderate temperature to yield nano-sized VN crystallites. Grain growth inhibited by lowering the synthesis temperature (≈400°C) yielded agglomerated powders of spherical crystallites of cubic phase of VN with particle sizes as small as 6nm in diameter. X-ray diffraction, FTIR, mass spectroscopy (MS), and nuclear magnetic resonance (NMR) spectroscopy assessed the ammonolysis and nitridation reaction of the VCl 4-NH 3 system. X-ray Rietveld refinement, the BET technique and high-resolution transmission microscopy (HRTEM), energy dispersive x-raymore » (EDX) and thermogravimetric analysis (TGA) helped assess the crystallographic and microstructural nature of the VN nanocrystals. The surface chemistry and redox reaction leading to the gravimetric pseudo-capacitance value of (≈855 F/g) measured for the VN nanocrystals was determined and validated using FTIR, XPS and cyclic voltammetry analyses.« less

The impact of thermal treatment conditions on the formation of crystalline structure of Ce-Zr-oxide composite obtained by a modified sol-gel technique

NASA Astrophysics Data System (ADS)

Trusova, E. A.; Khrushcheva, A. A.; Shvorneva, L. I.

2012-02-01

We present the results of the modified sol-gel synthesis of ultrafine ceria-doped zirconia powder for medical ceramics (implants) and catalytic purposes (environmental catalysis and petrochemistry). Special attention has been paid to study the influence of thermal treatment on crystallite size and crystal lattice parameters of zirconia doped by ceria. Zirconyl chloride and cerium nitrate were used as metal sources, and tetraethylammonium hydroxide (TEAH) was used as a sol stabilizer at molar ratio TEAH/Σ (Ce + Zr) equal to 0.5. It was proved that zirconium and cerium practically completely were included in the obtained solid solutions, since their phase compositions fully correspond to initial quantities of cerium and zirconium in reaction mixture. It was shown that average crystallite size of the obtained powders did not exceed 75Å, and the powders were resistant to thermal treatment. It was established that stabilization of the crystal lattice of ZrO2 occurs through formation of a cubic ceria sublattice.

Nanocrystalline Iron-Ore-Based Catalysts for Fischer-Tropsch Synthesis.

PubMed

Yong, Seok; Park, Ji Chan; Lee, Ho-Tae; Yang, Jung-Il; Hong, SungJun; Jung, Heon; Chun, Dong Hyun

2016-02-01

Nanocrystalline iron ore particles were fabricated by a wet-milling process using an Ultra Apex Mill, after which they were used as raw materials of iron-based catalysts for low-temperature Fischer-Tropsch synthesis (FTS) below 280 degrees C, which usually requires catalysts with a high surface area, a large pore volume, and a small crystallite size. The wet-milling process using the Ultra Apex Mill effectively destroyed the initial crystallite structure of the natural iron ores of several tens to hundreds of nanometers in size, resulting in the generation of nanocrystalline iron ore particles with a high surface area and a large pore volume. The iron-ore-based catalysts prepared from the nanocrystalline iron ore particles effectively catalyzed the low-temperature FTS, displaying a high CO conversion (about 90%) and good C5+ hydrocarbon productivity (about 0.22 g/g(cat)(-h)). This demonstrates the feasibility of using the iron-ore-based catalysts as inexpensive and disposable catalysts for the low-temperature FTS.

Titanium dioxide nanoparticles: Impact of increasing ionic strength during synthesis, reflux, and hydrothermal aging

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

Isley, Sara L.; Jordan, David S.; Penn, R. Lee

2009-01-08

This work investigates the role of ionic strength during synthesis, reflux, and hydrothermal aging of sol-gel synthesized titanium dioxide. Research presented here uses X-ray diffraction data and Rietveld refinements to quantify anatase, brookite, and rutile phases as functions of synthetic and aging variables. In addition, the Scherrer equation is used to obtain average crystallite sizes for each phase quantified. Results presented in this work demonstrate that the most control over the sol-gel products can be obtained by modifying the pH during hydrolysis. In addition, while varying the ionic strength during reflux and hydrothermal aging can result in enhanced control overmore » the crystalline phase and crystallite size, the most control can be achieved by varying the ionic strength during synthesis. Finally, sol-gel synthesis at low pH (-0.6) and high-chloride concentration (3 M NaCl) produced a heterogeneous sample composed of nanocrystalline anatase (3.8 nm) and rutile (2.9 nm)« less

Manifestation of weak ferromagnetism and photocatalytic activity in bismuth ferrite nanoparticles

NASA Astrophysics Data System (ADS)

Sakar, M.; Balakumar, S.; Saravanan, P.; Jaisankar, S. N.

2013-02-01

Bismuth ferrite (BFO) nanoparticles were synthesized by auto-ignition technique with and without adding ignition fuel such as citric acid. The presence of citric acid in the reaction mixture yielded highly-magnetic BFO/γ-Fe2O3 nanocomposite. When this composite was annealed to 650°C, a single phase BFO was formed with average crystallite size of 50 nm and showed weak ferromagnetic behavior. Conversely, the phase pure BFO prepared without adding citric acid exhibited antiferromagnetism because of its larger crystallite size of around 70 nm. The visible-light driven photocatalytic activity of both the pure BFO and BFO/γ-Fe2O3 nanocomposite were examined by degrading methyl orange dye. The pure BFO showed a moderate photocatalytic activity; while BFO/γ-Fe2O3 nanocomposite showed enhanced activity. This could be probably due to the optimal band gap ratio between BFO and γ-Fe2O3 phases reduced the recombination of electron-hole pairs which aided in the enhancement of photocatalytic activity.

On the solid phase crystallization of In{sub 2}O{sub 3}:H transparent conductive oxide films prepared by atomic layer deposition

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

Macco, Bart; Verheijen, Marcel A.; Black, Lachlan E.

2016-08-28

Hydrogen-doped indium oxide (In{sub 2}O{sub 3}:H) has emerged as a highly transparent and conductive oxide, finding its application in a multitude of optoelectronic devices. Recently, we have reported on an atomic layer deposition (ALD) process to prepare high quality In{sub 2}O{sub 3}:H. This process consists of ALD of In{sub 2}O{sub 3}:H films at 100 °C, followed by a solid phase crystallization step at 150–200 °C. In this work, we report on a detailed electron microscopy study of this crystallization process which reveals new insights into the crucial aspects for achieving the large grain size and associated excellent properties of the material. Themore » key finding is that the best optoelectronic properties are obtained by preparing the films at the lowest possible temperature prior to post-deposition annealing. Electron microscopy imaging shows that such films are mostly amorphous, but feature a very low density of embedded crystallites. Upon post-deposition annealing, crystallization proceeds merely from isotropic crystal grain growth of these embedded crystallites rather than by the formation of additional crystallites. The relatively high hydrogen content of 4.2 at. % in these films is thought to cause the absence of additional nucleation, thereby rendering the final grain size and optoelectronic properties solely dependent on the density of embedded crystallites. The temperature-dependent grain growth rate has been determined, from which an activation energy of (1.39 ± 0.04) eV has been extracted. Finally, on the basis of the observed crystallization mechanism, a simple model to fully describe the crystallization process has been developed. This model has been validated with a numerical implementation thereof, which accurately predicts the observed temperature-dependent crystallization behaviour.« less

Adsorption of Pb2+ ions on novel ternary nanocomposite of tin, iron and titania

NASA Astrophysics Data System (ADS)

Rehman, Mahfooz ur; Rehman, Wajid; Waseem, Muhammad; Haq, Sirajul; Hussain Shah, Khizar; Kang, Peng

2018-02-01

In this study, ternary nanocomposite (TNC) was synthesized by microemulsion method by taking Sn, Ti and Fe in (1:1:1) molar ratio. The BET surface area and pore size were measured by nitrogen adsorption method. The morphological features of TNC like particle size, elemental percentage and crystallite size were studied by scanning electron microscopy (SEM), energy dispersive x-rays (EDX) and x-rays diffraction (XRD) respectively, whereas the surface functional groups were detected by Fourier Transform Infrared (FTIR) spectroscopy. The crystallite size was found to be 11 nm, calculated from FWHM of diffraction peak with relative intensity 100%. For the thermal stability of TNC, thermogravimetric analysis (TGA) was performed. Batch adsorption tests were used for the removal of Pb2+ ions from aqueous solutions. The maximum adsorption capacity in this study was found to be 79.56 mg g-1 at 40 °C which is promising than the values reported in the literature. Based on the regression coefficient (r 2), the adsorption data was found well fitted to the Langmuir as compared to Freundlich model. The exchange of a single proton with every Pb2+ ion was calculated. Thermodynamic parameters were indicative for the sorption process to be endothermic and spontaneous.

Synthesis of nanocrystalline zirconia by amorphous citrate route: structural and thermal (HTXRD) studies

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

Bhagwat, Mahesh; Ramaswamy, Veda

Nanocrystalline zirconia powder with a fairly narrow particle size distribution has been synthesized by the amorphous citrate route. The sample obtained has a high BET surface area of 89 m{sup 2} g{sup -1}. Rietveld refinement of the powder X-ray diffraction (XRD) profile of the zirconia sample confirms stabilization of zirconia in the tetragonal phase with around 8% monoclinic impurity. The data show the presence of both anionic as well as cationic vacancies in the lattice. Crystallite size determined from XRD is 8 nm and is in close agreement with the particle size determined by TEM. The in situ high temperature-X-raymore » diffraction (HTXRD) study revealed high thermal stability of the mixture till around 1023 K after which the transformation of tetragonal phase into the monoclinic phase has been seen as a function of temperature till 1473 K. This transformation is accompanied by an increase in the crystallite size of the sample from 8 to 55 nm. The thermal expansion coefficients are 9.14 x 10{sup -6} K{sup -1} along 'a'- and 15.8 x 10{sup -6} K{sup -1} along 'c'-axis. The lattice thermal expansion coefficient in the temperature range 298-1623 K is 34.6 x 10{sup -6} K{sup -1}.« less

Structure and morphology evolution of silica-modified pseudoboehmite aerogels during heat treatment

NASA Astrophysics Data System (ADS)

Pakharukova, V. P.; Shalygin, A. S.; Gerasimov, E. Yu.; Tsybulya, S. V.; Martyanov, O. N.

2016-01-01

Silica-modified pseudoboehmite aerogels (0, 10, 20 at% of Si) were prepared by sol-gel method followed by supercritical drying. The phase transformations, changes in structure and morphology upon calcination were thoroughly investigated by advanced X-Ray diffraction (XRD) techniques and high-resolution transmission electron microscopy (HRTEM). Obtained pseudoboehmite samples had specific nanostructure: ultrathin two-dimensional (2D) crystallites were loosely packed. The silica dopant drastically enhanced the crystallite anisotropy. Thus, the aerogel with Al:Si atomic ratio of 9:1 consisted of the pseudoboehmite nanosheets with thickness of one unit cell (average dimensions of 14.0×1.2×14.5 nm). The specific nanostructure caused remarkable features of experimental XRD patterns, including anisotropic peak broadening and appearance of forbidden reflection. Direct simulation of XRD patterns with using the Debye Scattering Equation allowed the size and morphology of pseudoboehmite crystallites to be determined. The silica addition strongly delayed formation of γ-alumina and further phase transformations upon calcinaton. Thermal stability of alumina was suggested to be affected by the particle morphology inherited from the pseudoboehmite precursor.

A thermal study on the structural changes of bimetallic ZrO2-modified TiO2 nanotubes synthesized using supercritical CO2.

PubMed

Lucky, R A; Charpentier, P A

2009-05-13

In this study the thermal behavior of bimetallic ZrO(2)-TiO(2) (10/90 mol/mol) nanotubes are discussed which were synthesized via a sol-gel process in supercritical carbon dioxide (scCO(2)). The effects of calcination temperature on the morphology, phase structure, mean crystallite size, specific surface area and pore volume of the nanotubes were investigated by using a variety of physiochemical techniques. We report that SEM and TEM images showed that the nanotubular structure was preserved at up to 800 degrees C calcination temperature. When exposed to higher temperatures (900-1000 degrees C) the ZrO(2)-TiO(2) tubes deformed and the crystallites fused together, forming larger crystallites, and a bimetallic ZrTiO(4) species was detected. These results were further examined using TGA, FTIR, XRD and HRTEM analysis. The BET textural properties demonstrated that the presence of a small amount of Zr in the TiO(2) matrix inhibited the grain growth, stabilized the anatase phase and increased the thermal stability.

Extent and relevance of stacking disorder in “ice Ic”

PubMed Central

Kuhs, Werner F.; Sippel, Christian; Falenty, Andrzej; Hansen, Thomas C.

2012-01-01

A solid water phase commonly known as “cubic ice” or “ice Ic” is frequently encountered in various transitions between the solid, liquid, and gaseous phases of the water substance. It may form, e.g., by water freezing or vapor deposition in the Earth’s atmosphere or in extraterrestrial environments, and plays a central role in various cryopreservation techniques; its formation is observed over a wide temperature range from about 120 K up to the melting point of ice. There was multiple and compelling evidence in the past that this phase is not truly cubic but composed of disordered cubic and hexagonal stacking sequences. The complexity of the stacking disorder, however, appears to have been largely overlooked in most of the literature. By analyzing neutron diffraction data with our stacking-disorder model, we show that correlations between next-nearest layers are clearly developed, leading to marked deviations from a simple random stacking in almost all investigated cases. We follow the evolution of the stacking disorder as a function of time and temperature at conditions relevant to atmospheric processes; a continuous transformation toward normal hexagonal ice is observed. We establish a quantitative link between the crystallite size established by diffraction and electron microscopic images of the material; the crystallite size evolves from several nanometers into the micrometer range with progressive annealing. The crystallites are isometric with markedly rough surfaces parallel to the stacking direction, which has implications for atmospheric sciences. PMID:23236184

Modeling of Amorphous Calcium Carbonate

NASA Astrophysics Data System (ADS)

Sinha, Sourabh; Rez, Peter

2011-10-01

Many species (e.g. sea urchin) form amorphous calcium carbonate (ACC) precursor phases that subsequently transform into crystalline CaCO3. It is certainly possible that ACC might have up to 10 wt% Mg and ˜3 wt% of water. The structure of ACC and mechanisms by which it transforms to crystalline phase are still unknown. Our goal here is to determine an atomic structure model that is consistent with diffraction and IR measurements of ACC. For this purpose a calcite supercell with 24 formula units (120 atoms) was constructed. Various configurations with 6 Mg atoms substituting for Ca (6 wt%) and 3-5 H2O molecules (2.25- 3.75 wt%) inserted in the spaces between Ca atoms, were relaxed using VASP. Most noticeable effects were the tilts of CO3 groups and distortion of Ca sub-lattice, especially in the case of water. The distributions of nearest Ca-Ca distance and CO3 tilts were extracted from those configurations. We also performed the same analysis starting with aragonite. Sampling from above distributions we built models for amorphous calcite/aragonite of size ˜1700 nm^3. We found that the induced distortions were not enough to generate a diffraction pattern typical of an amorphous material. Next we studied diffraction pattern of several nano-crystallites as recent studies suggest that amorphous calcite might be composed of nano- crystallites. We could then generate a diffraction pattern that appeared similar to that from ACC, for a nano-crystallite of size ˜2 nm^3.

Re-dispersion and film formation of GdVO4 :  Ln3+ (Ln3+ = Dy3+, Eu3+, Sm3+, Tm3+) nanoparticles: particle size and luminescence studies.

PubMed

Shanta Singh, N; Ningthoujam, R S; Phaomei, Ganngam; Singh, S Dorendrajit; Vinu, A; Vatsa, R K

2012-04-21

GdVO(4) : Ln(3+) (Ln(3+) = Dy(3+), Eu(3+), Sm(3+), Tm(3+)) nanoparticles are prepared by a simple chemical route at 140 °C. The crystallite size can be tuned by varying the pH of the reaction medium. Interestingly, the crystallite size is found to increase significantly when pH increases from 6 to 12. This is related to slower nucleation of the GdVO(4) formation with increase of VO(4)(3-) present in solution. The luminescence study shows an efficient energy transfer from vanadate absorption of GdVO(4) to Ln(3+) and thereby enhanced emissions are obtained. A possible reaction mechanism at different pH values is suggested in this study. As-prepared samples are well dispersed in ethanol, methanol and water, and can be incorporated into polymer films. Luminescence and its decay lifetime studies confirm the decrease in non-radiative transition probability with the increase of heat treatment temperature. Re-dispersed particles will be useful in potential applications of life science and the film will be useful in display devices.

Nanocrystalline (U0.5Ce0.5)O2±x solid solutions through citrate gel-combustion

NASA Astrophysics Data System (ADS)

Maji, D.; Ananthasivan, K.; Venkata Krishnan, R.; Balakrishnan, S.; Amirthapandian, S.; Joseph, Kitheri; Dasgupta, Arup

2018-04-01

Nanocrystalline powders of (U0.5Ce0.5)O2±x solid solutions were synthesized in bulk (100-200 g) through the citrate gel combustion. The fuel (citric acid) to oxidant (nitrate) mole ratio (R) was varied from 0.1 to 1.0. Two independent lots of the products obtained through the gel-combustion were calcined at 973 K in air and in a mixture of argon containing 8% H2 respectively. All these powders were characterized for their bulk density, X-ray crystallite size, specific surface area, size distribution of the particles, porosity as well as residual carbon. The morphology and microstructures of these powders were studied by using scanning electron microscopy (SEM) and transmission electron microscopy (TEM) respectively. Nanocrystalline single phase fluorite solid solutions having a typical crystallite size of about (7-15 nm) were obtained. These powders were highly porous comprising cuboidal flaky agglomerates. The combustion mixture with an 'R' value of 0.25 was found to undergo volume combustion and was found to yield a product that was distinctly different. The systematic investigation on synthesis and characterization of nanocrystalline UCeO2 is reported for the first time.

Mechanism of solid state amorphization of glucose upon milling.

PubMed

Dujardin, N; Willart, J F; Dudognon, E; Danède, F; Descamps, M

2013-02-07

Crystalline α-glucose is known to amorphize upon milling at -15 °C while it remains structurally invariant upon milling at room temperature. We have taken advantage of this behavior to compare the microstructural evolutions of the material in both conditions in order to identify the essential microstructural features which drive the amorphization process upon milling. The investigations have been performed by differential scanning calorimetry and by powder X-ray diffraction. The results indicate that two different amorphization mechanisms occur upon milling: an amorphization at the surface of crystallites due to the mechanical shocks and a spontaneous amorphization of the crystallites as they reach a critical size, which is close to 200 Å in the particular case of α-glucose.

50 CFR 648.83 - Multispecies minimum fish sizes.

Code of Federal Regulations, 2010 CFR

2010-10-01

... 50 Wildlife and Fisheries 8 2010-10-01 2010-10-01 false Multispecies minimum fish sizes. 648.83... Measures for the NE Multispecies and Monkfish Fisheries § 648.83 Multispecies minimum fish sizes. (a) Minimum fish sizes. (1) Minimum fish sizes for recreational vessels and charter/party vessels that are not...

Effect of High Strain-Rate Deformation and Aging Temperature on the Evolution of Structure, Microhardness, and Wear Resistance of Low-Alloyed Cu-Cr-Zr Alloy

NASA Astrophysics Data System (ADS)

Kheifets, A. E.; Khomskaya, I. V.; Korshunov, L. G.; Zel'dovich, V. I.; Frolova, N. Yu.

2018-04-01

The effect of the preliminary high strain-rate deformation, performed via the method of dynamic channel-angular pressing (DCAP), and subsequent annealings on the tribological properties of a dispersionhardened Cu-0.092 wt % Cr-0.086 wt % Zr alloy has been investigated. It has been shown that the surfacelayer material of the alloy with a submicrocrystalline (SMC) structure obtained by the DCAP method can be strengthened using severe plastic deformation by sliding friction at the expense of creating a nanocrystalline structure with crystallites of 15-60 nm in size. It has been shown that the SMC structure obtained by the high strain-rate DCAP deformation decreases the wear rate of the samples upon sliding friction by a factor of 1.4 compared to the initial coarse-grained state. The maximum values of the microhardness and minimum values of the coefficient of friction and shear strength have been obtained in the samples preliminarily subjected to DCAP and aging at 400°C. The attained level of microhardness is 3350 MPa, which exceeds the microhardness of the alloy in the initial coarse-grained state by five times.

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).

Effect of Annealing Temperature on Structural and Optical Properties of Sol-Gel-Derived ZnO Thin Films

NASA Astrophysics Data System (ADS)

Arif, Mohd.; Sanger, Amit; Vilarinho, Paula M.; Singh, Arun

2018-04-01

Nanocrystalline ZnO thin films were deposited on glass substrate via sol-gel dip-coating technique then annealed at 300°C, 400°C, and 500°C for 1 h. Their optical, structural, and morphological properties were studied using ultraviolet-visible (UV-Vis) spectrophotometry, x-ray diffraction (XRD) analysis, and scanning electron microscopy (SEM). XRD diffraction revealed that the crystalline nature of the thin films increased with increasing annealing temperature. The c-axis orientation improved, and the grain size increased, as indicated by increased intensity of the (002) plane peak at 2θ = 34.42° corresponding to hexagonal ZnO crystal. The average crystallite size of the thin films ranged from 13 nm to 23 nm. Increasing the annealing temperature resulted in larger crystallite size and higher crystallinity with increased surface roughness. The grain size according to SEM analysis was in good agreement with the x-ray diffraction data. The optical bandgap of the thin films narrowed with increasing annealing temperature, lying in the range of 3.14 eV to 3.02 eV. The transmission of the thin films was as high as 94% within the visible region. The thickness of the thin films was 400 nm, as measured by ellipsometry, after annealing at the different temperatures of 300°C, 400°C, and 500°C.

Influence of Mg and Ni substitution on structural, microstructural and magnetic properties of Sr2Co2-xMgx/2Nix/2Fe12O22 (Co2Y) hexaferrite

NASA Astrophysics Data System (ADS)

Alizad Farzin, Y.; Mirzaee, O.; Ghasemi, A.

2014-12-01

In this study, Mg and Ni substituted Y-type hexaferrite particles with narrow size distribution have been prepared by using a sol-gel auto combustion method. The effects on structural, microstructure and magnetic properties have been investigated by substituting Mg2+ and Ni2+ at Co2+ sites. XRD patterns showed that Y-type hexaferrite phase formation has not been affected by substituting magnesium and nickel with cobalt in the range of 0.0≤x≤0.75. Various parameters such as lattice constants, cell volume and crystallite size have been calculated based on XRD data. The morphology and size distribution of the particles have been studied using high resolution field emission scanning electron microscopy (FESEM). It was also understood that the average crystallite size of particles increased from 45 to 63 nm with an increase of x content at Co2Y compound. Magnetic properties were determined using a vibrating sample magnetometer (VSM). The magnetic results revealed that by increasing the Mg and Ni in octahedral and tetrahedral sites, the coercivity was also increased from 949 to 1066 Oe, whereas saturation magnetization and Remnant magnetization were decreased from 47.98 to 40.78 emu/g and 23.05 to 20.99 emu/g, respectively.

50 CFR 648.103 - Minimum fish sizes.

Code of Federal Regulations, 2010 CFR

2010-10-01

... 50 Wildlife and Fisheries 8 2010-10-01 2010-10-01 false Minimum fish sizes. 648.103 Section 648... Summer Flounder Fisheries § 648.103 Minimum fish sizes. (a) The minimum size for summer flounder is 14... carrying more than five crew members. (c) The minimum sizes in this section apply to whole fish or to any...

Preparation of ultrafine grained copper nanoparticles via immersion deposit method

NASA Astrophysics Data System (ADS)

Abbasi-Kesbi, Fatemeh; Rashidi, Ali Mohammad; Astinchap, Bandar

2018-03-01

Today, the exploration about synthesis of nanoparticles is much of interest to materials scientists. In this work, copper nanoparticles have been successfully synthesized by immersion deposit method in the absence of any stabilizing and reducing agents. Copper (II) sulfate pentahydrate as precursor salt and distilled water and Ethylene glycol as solvents were used. The copper nanoparticles were deposited on plates of low carbon steel. The effects of copper sulfate concentrations and solvent type were investigated. X-ray diffraction, scanning electron microscopy and UV-Visible spectroscopy were taken to investigate the crystallite size, crystal structure, and morphology and size distribution and the growth process of the nanoparticles of obtained Cu particles. The results indicated that the immersion deposit method is a particularly suitable method for synthesis of semispherical copper nanoparticles with the crystallites size in the range of 22 to 37 nm. By increasing the molar concentration of copper sulfate in distilled water solvent from 0.04 to 0.2 M, the average particles size is increased from 57 to 81 nm. The better size distribution of Cu nanoparticles was achieved using a lower concentration of copper sulfate. By increasing the molar concentration of copper sulfate in water solvent from 0.04 to 0.2, the location of the SPR peak has shifted from 600 to 630 nm. The finer Cu nanoparticles were formed using ethylene glycol instead water as a solvent. Also, the agglomeration and overlapping of nanoparticles in ethylene glycol were less than that of water solvent.

An Improved X-ray Diffraction Method For Cellulose Crystallinity Measurement

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

Ju, Xiaohui; Bowden, Mark E.; Brown, Elvie E.

2015-06-01

We show in this work a modified X-ray diffraction method to determine cellulose crystallinity index (CrI). Nanocrystalline cellulose (NCC) dervided from bleached wood pulp was used as a model substrate. Rietveld refinement was applied with consideration of March-Dollase preferred orientation at the (001) plane. In contrast to most previous methods, three distinct amorphous peaks identified from new model samples which are used to calculate CrI. A 2 theta range from 10° to 75° was found to be more suitable to determine CrI and crystallite structural parameters such as d-spacing and crystallite size. This method enables a more reliable measurement ofmore » CrI of cellulose and may be applicable to other types of cellulose polymorphs.« less

Nano crystalline Bi2(VO5) phases in lithium bismuth borate glasses containing mixed vanadium-nickel oxides

NASA Astrophysics Data System (ADS)

Yadav, Arti; Khasa, S.; Dahiya, M. S.; Agarwal, A.

2016-05-01

Glass composition 7V2O5.23Li2O.20Bi2O3.50B2O3 and x(2NiO.V2O5).(30-x)Li2O.20Bi2O3.50B2O3, x=0, 2, 5, 7 and 10, were produced by conventional melt quenching technique. The quenched amorphous glass samples were annealed at temperatures 400°C and 500°C for 6 hours. The Bi2(VO5) crystallite were grown in all prepared glass matrix. Tn vanadium lithium bismuth borate glass (annealed), the some phrase of V2O5-crystal were observed along with the nano crystalline Bi2(VO5) phase. The sharp peaks in FTTR spectra of all annealed compositions were also compatible with the XRD diffraction peaks of the system under investigation. Average crystalline size (D) of the Bi2(VO5) nano-crystallite was ~30nm for samples annealed at 400°C and ~42nm for samples annealed at 500°C. Lattice parameter and the lattice strain for all the samples was also calculated corresponding to the (113) plane of Bi2(VO5) crystallite.

Low field magnetocaloric effect in bulk and ribbon alloy La(Fe0.88Si0.12)13

NASA Astrophysics Data System (ADS)

Vuong, Van-Hiep; Do-Thi, Kim-Anh; Nguyen, Duy-Thien; Nguyen, Quang-Hoa; Hoang, Nam-Nhat

2018-03-01

Low-field magnetocaloric effect occurred in itinerant metamagnetic materials is at core for magnetic cooling application. This works reports the magnetocaloric responses obtained at 1.35 T for the silicon-doped iron-based binary alloy La(Fe0.88Si0.12)13 in the bulk and ribbon form. Both samples possess a same symmetry but with different crystallite sizes and lattice parameters. The ribbon sample shows a larger maximum entropy change (nearly 8.5 times larger) and a higher Curie temperature (5 K higher) in comparison with that of the bulk sample. The obtained relative cooling power for the ribbon is also larger and very promising for application (RCP = 153 J/kg versus 25.2 J/kg for the bulk). The origin of the effect observed is assigned to the occurrence of negative magnetovolume effect in the ribbon structure with limit crystallization, caused by rapid cooling process at the preparation, which induced smaller crystallite size and large lattice constant at the overall weaker local crystal field.

Effect of Heat and Laser Treatment on Cu2S Thin Film Sprayed on Polyimide Substrate

NASA Astrophysics Data System (ADS)

Magdy, Wafaa; Mahmoud, Fawzy A.; Nassar, Amira H.

2018-02-01

Three samples of copper sulfide Cu2S thin film were deposited on polyimide substrate by spray pyrolysis using deposition temperature of 400°C and deposition time of about 45 min. One of the samples was left as deposited, another was heat treated, while the third was laser treated. The structural, surface morphological, optical, mechanical, and electrical properties of the films were investigated. X-ray diffraction (XRD) analysis showed that the copper sulfide films were close to copper-rich phase (Cu2S). Increased crystallite size after heat and laser treatment was confirmed by XRD analysis and scanning electron microscopy. Vickers hardness measurements showed that the samples' hardness values were enhanced with increasing crystallite size, representing an inverse Hall-Petch (H-P) effect. The calculated optical bandgap of the treated films was lower than that of the deposited film. Finally, it was found that both heat and laser treatment enhanced the physical properties of the sprayed Cu2S films on polyimide substrate for use in solar energy applications.

Structural and optical properties of ZnO thin films prepared by RF sputtering at different thicknesses

NASA Astrophysics Data System (ADS)

Hammad, Ahmed H.; Abdel-wahab, M. Sh.; Vattamkandathil, Sajith; Ansari, Akhalakur Rahman

2018-07-01

Hexagonal nanocrystallites of ZnO in the form of thin films were prepared by radio frequency sputtering technique. X-ray diffraction analysis reveals two prominent diffraction planes (002) and (103) at diffraction angles around 34.3 and 62.8°, respectively. The crystallite size increases through (103) plane from 56.1 to 64.8 Å as film thickness changed from 31 nm up to 280 nm while crystallites growth through (002) increased from 124 to 136 Å as film thickness varies from 31 to 107 nm and dropped to 115.8 Å at thickness 280 nm. The particle shape changes from spherical to longitudinal form. The particle size is 25 nm for films of thickness below 107 nm and increases at higher thicknesses (134 and 280 nm) from 30 to 40 nm, respectively. Optical band gap is deduced to be direct with values varied from 3.22 to 3.28 eV and the refractive index are evaluated based on the optical band values according to Moss, Ravindra-Srivastava, and Dimitrov-Sakka models. All refractive index models gave values around 2.3.

Gamma-radiolytic preparation of multi-component oxides

NASA Astrophysics Data System (ADS)

Procházková, Lenka; Bárta, Jan; Čuba, Václav; Ekberg, Christian; Tietze, Sabrina; Jakubec, Ivo

2016-07-01

The preparation of solid precursors to Zn1-xCdxO and (Lu,Y)3Al5O12:Ce induced by 60Co gamma-ray irradiation of aqueous solutions containing soluble metal salts and ammonium formate is presented. Due to the irradiation, crystalline zinc carbonate hydroxide Zn4(CO3)(OH)6·H2O or amorphous carbonates of Lu, Y and Al were formed in the solutions. After calcination at 500 °C, the agglomerated phase-pure Zn1-xCdxO with crystallite size about 50 nm was obtained if the Cd concentration in solutions remained below 16 M% (with respect to Zn) with x being up to 0.035. The solid precursors to garnets contained the intended concentration of all elements, according to X-ray fluorescence analysis. After calcination at 1200 °C in mild vacuum, the respective phase-pure garnets with crystallite size 100 nm or their solid solution were produced when the Ce dopation was kept below 2 M% (with respect to rare-earth metals). The Ce solubility in the garnet lattice was estimated as 1-2 M% at the calcination conditions used.

Synthesis of nano-forsterite powder by making use of natural silica sand

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

Nurbaiti, Upik, E-mail: upik-nurbaiti@mail.unnes.ac.id; Department of Physics, Faculty of Mathematics and Natural Sciences Semarang State University Jl. Raya Sekaran GunungPati, Semarang 50221; Suud, Fikriyatul Azizah

2016-02-08

Nano-forsterite powder with natural silica sand and magnesium powder as the raw materials have been succesfully synthesized. The silica sand was purified followed by a coprecipitation process to obtain colloidal silica. The magnesium powder was dissolved in a chloric acid solution to obtain MgCl{sub 2} solution. The nanoforsterite powder was synthesised using a sol-gel method which included the mixing the colloidal silica and the MgCl{sub 2} solution with various aging and filtering processes. The samples were dried at 100 °C using a hot plate and then the dried powders were calcinated at 900 °C for 2 hours. The samples weremore » characetised for their elements and phase compositions using X-ray Flourescence (XRF) and X-ray Diffraction (XRD) methods, respectively. The diffraction data were qualitatively analyzed using Match!2 software and quantitatively using Rietica software. The crystallite size was verified using Transmission Electron Microscopy (TEM). Results of XRD data analysis showed that the forsterite content reached up to 90.5% wt. The TEM average crystallite size was approximately 53(6) nm.« less

Crystal Analysis of Multi Phase Calcium Phosphate Nanoparticles Containing Different amount of Magnesium

NASA Astrophysics Data System (ADS)

Gozalian, Afsaneh; Behnamghader, Ali Asghar; Moshkforoush, Arash

In this study, Mg doped hydroxyapatite [(Ca, Mg)10(PO4)6(OH)2] and β-tricalcium phosphate nanoparticles were synthesized via sol gel method. Triethyl phosphite, calcium nitrate tetrahydrate and magnesium nitrate hexahydrate were used as P, Ca and Mg precursors. The ratio of (Ca+Mg)/P and the amount of magnesium (x) were kept constant at 1.67 and ranging x = 0 up to 3 in molecular formula of Ca10-xMgx (PO4)6(OH)2, respectively. Phase composition and chemical structure were performed using X-ray Diffraction (XRD) and Fourier Transform Infrared Spectroscopy (FT-IR). Phase percentages, crystallite size, degree of crystallinity and lattice parameters were investigated. The presence of magnesium led to form the Mg doped tricalcium phosphate (β-TCMP) and Mg doped hydroxyapatite (Mg-HA). Based on the results of this study, lattice parameters, degree of crystallinity and crystallite size decreased with magnesium content. In addition, with increasing magnesium content, the amount of CaO phase decreased whereas the amount of MgO phase increased significantly. Obtained results can be used for new biomaterials design.

Superparamagnetic behavior of heat treated Mg{sub 0.5}Zn{sub 0.5}Fe{sub 2}O{sub 4} ferrite nanoparticles studied by Mössbauer spectroscopy

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

Srinivas, Ch., E-mail: srinivas.chintoju75@gmail.com; Prasad, S. A. V.; Singh, S. B.

2016-05-23

Nanoparticles of Mg{sub 0.5}Zn{sub 0.5}Fe{sub 2}O{sub 4} ferrite have been synthesized by co-precipitation method. XRD and Mössbauer spectroscopic results of Mg{sub 0.5}Zn{sub 0.5}Fe{sub 2}O{sub 4} annealed at 200 °C, 500 °C and 800 °C are reported. It was observed that the crystallite size increases and the lattice parameter decreases with increase in annealing temperature. The observed decrease in lattice strain supports the increase in crystallite size. The Mössbauer spectra of the samples annealed at 200 °C and 500 °C exhibits superparamagnetic doublets whereas the Mössbauer spectrum of the sample annealed at 800 °C exhibits paramagnetic doublet along with weak sextetmore » of hyperfine interaction. The values of isomer shift resemble the presence of high spin iron ions. The studied ferrite nanoparticles are suitable for biomedical applications. The results are incorporated employing core-shell model and cation redistribution.« less

Effects of optical band gap energy, band tail energy and particle shape on photocatalytic activities of different ZnO nanostructures prepared by a hydrothermal method

NASA Astrophysics Data System (ADS)

Klubnuan, Sarunya; Suwanboon, Sumetha; Amornpitoksuk, Pongsaton

2016-03-01

The dependence of the crystallite size and the band tail energy on the optical properties, particle shape and oxygen vacancy of different ZnO nanostructures to catalyse photocatalytic degradation was investigated. The ZnO nanoplatelets and mesh-like ZnO lamellae were synthesized from the PEO19-b-PPO3 modified zinc acetate dihydrate using aqueous KOH and CO(NH2)2 solutions, respectively via a hydrothermal method. The band tail energy of the ZnO nanostructures had more influence on the band gap energy than the crystallite size. The photocatalytic degradation of methylene blue increased as a function of the irradiation time, the amount of oxygen vacancy and the intensity of the (0 0 0 2) plane. The ZnO nanoplatelets exhibited a better photocatalytic degradation of methylene blue than the mesh-like ZnO lamellae due to the migration of the photoelectrons and holes to the (0 0 0 1) and (0 0 0 -1) planes, respectively under the internal electric field, that resulted in the enhancement of the photocatalytic activities.

Simple synthesis of graphene nanocomposites MgO-rGO and Fe2O3-rGO for multifunctional applications

NASA Astrophysics Data System (ADS)

Abdel-Aal, Seham K.; Ionov, Andrey; Mozhchil, R. N.; Naqvi, Alim H.

2018-05-01

Hummer's method was used to prepare graphene oxide (GO) by chemical exfoliation of graphite. Simple precipitation method was used for the preparation of hybrid nanocomposites MgO-rGO and Fe2O3-rGO. A 0.3 Molar of corresponding metal nitrate solution and GO solution are used for the preparation process. XRD, FT-IR, and XPS were used to characterize the prepared nanocomposites. The reduction of GO into reduced rGO in the formed nanocomposites was confirmed. Morphological characterization showed the formation of needle-shaped nanocrystals of MgO successfully grown on graphene nanosheet with average crystallite size 8.4 nm. Hematite nanocomposite Fe2O3-rGO forms rod-shaped crystals with average crystallite size 27.5 nm. The saturation magnetization observed for Fe2O3-rGO is less than reported value for the pure Fe2O3 nanoparticles. Thermal properties of as-prepared hybrid nanocomposites MgO-rGO and Fe2O3-rGO showed thermal stability of the prepared nanocomposite over long range of temperature.

50 CFR 648.124 - Minimum fish sizes.

Code of Federal Regulations, 2010 CFR

2010-10-01

... 50 Wildlife and Fisheries 8 2010-10-01 2010-10-01 false Minimum fish sizes. 648.124 Section 648... Scup Fishery § 648.124 Minimum fish sizes. (a) The minimum size for scup is 9 inches (22.9 cm) TL for... charter boat, or more than five crew members if a party boat. (c) The minimum size applies to whole fish...

A comparative study of TiN and TiC: Oxidation resistance and retention of xenon at high temperature and under degraded vacuum

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

Gavarini, S.; Bes, R.; Millard-Pinard, N.

2011-01-01

Dense TiN and TiC samples were prepared by hot pressing using micrometric powders. Xenon species (simulating rare gas fission products) were then implanted into the ceramics. The samples were annealed for 1 h at 1500 deg. C under several degraded vacuums with P{sub O{sub 2}} varying from 10{sup -6} to 2x10{sup -4} mbars. The oxidation resistance of the samples and their retention properties with respect to preimplanted xenon species were analyzed using scanning electron microscopy, grazing incidence x-ray diffraction, Rutherford backscattering spectrometry, and nuclear backscattering spectrometry. Results indicate that TiC is resistant to oxidation and does not release xenon formore » P{sub O{sub 2{<=}}}6x10{sup -6} mbars. When P{sub O{sub 2}} increases, geometric oxide crystallites appear at the surface depending on the orientation and size of TiC grains. These oxide phases are Ti{sub 2}O{sub 3}, Ti{sub 3}O{sub 5}, and TiO{sub 2}. Apparition of oxide crystallites is associated with the beginning of xenon release. TiC surface is completely covered by the oxide phases at P{sub O{sub 2}}=2x10{sup -4} mbars up to a depth of 3 {mu}m and the xenon is then completely released. For TiN samples, the results show a progressive apparition of oxide crystallites (Ti{sub 3}O{sub 5} mainly) at the surface when P{sub O{sub 2}} increases. The presence of the oxide crystallites is also directly correlated with xenon release, the more oxide crystallites are growing the more xenon is released. TiN surface is completely covered by an oxide layer at P{sub O{sub 2}}=2x10{sup -4} mbars up to 1 {mu}m. A correlation between the initial fine microstructure of TiN and the properties of the growing layer is suggested.« less

Moessbauer Characterization of Magnetite/Polyaniline Magnetic Nanocomposite

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

Rodriguez, Anselmo F. R.; Faria, Fernando S. E. D. V.; Lopez, Jorge L.

2010-12-02

Aniline surface coated Fe{sub 3}O{sub 4} nanoparticles have been successfully synthesized by UV irradiation varying the time and the acid media (HCl, HNO{sub 3}, or H{sub 2}SO{sub 4}). The synthesized material represents a promising platform for application in nerve regeneration. XRD patterns are consistent with the crystalline structure of magnetite. Nevertheless, for UV irradiation times longer than 2 h, extra XRD lines reveal the presence of goethite. The mean crystallite size of uncoated particles is estimated to be 25.4 nm, meanwhile that size is reduced to 19.9 nm for the UV irradiated sample in HCl medium for 4 h. Moessbauermore » spectra of uncoated nanoparticles reveal the occurrence of thermal relaxation at room temperature, while the 77 K-Moessbauer spectrum suggests the occurrence of electron localization effects similar to that expected in bulk magnetite. The Mossbauer spectra of UV irradiated sample in HCl medium during 4 h, confirms the presence of the goethite phase. For this sample, the thermal relaxation is more evident, since the room temperature spectrum shows larger spectral area for the nonmagnetic component due to the smaller crystallite size. Meanwhile, the 77 K-Moessbauer spectrum suggests the absence of the electron localization effect above 77 K.« less

Williamson-Hall analysis and optical properties of small sized ZnO nanocrystals

NASA Astrophysics Data System (ADS)

Kalita, Amarjyoti; Kalita, Manos P. C.

2017-08-01

We apply Williamson-Hall (WH) method of X-ray diffraction (XRD) line profile analysis for lattice strain estimation of small sized ZnO nanocrystals (crystallite size≈4 nm). The ZnO nanocrystals are synthesized by room temperature chemical co-precipitation followed by heating at 40 °C. Zinc acetate, sodium hydroxide and 2-mercaptoethanol (ME) are used for the synthesis of the nanocrystals. {100}, {002}, {101} and {200}, {112}, {201} line profiles in the XRD pattern are significantly merged, therefore determination of the full width at half maximum values and peak positions of the line profiles required for WH analysis has been carried out by executing Rietveld refinement of the XRD pattern. Lattice strain of the 4 nm sized ZnO nanocrystals is found to be 5.8×10-3 which is significantly higher as compared to the literature reported values for larger ones (crystallite size≈17-47 nm). Role of ME as capping agent is confirmed by Fourier transform infrared spectroscopy. The band gap of the nanocrystals is determined from the UV-Visible absorption spectrum and is found to be 3.68 eV. The photoluminescence spectrum exhibits emissions in the visible (408 nm-violet, 467 nm-blue and 538 nm-green) regions showing presence of zinc interstitial and oxygen vacancy in the ZnO nanocrystals.

Synthesis of fluorapatite–hydroxyapatite nanoparticles and toxicity investigations

PubMed Central

Montazeri, N; Jahandideh, R; Biazar, Esmaeil

2011-01-01

In this study, calcium phosphate nanoparticles with two phases, fluorapatite (FA; Ca10(PO4)6F2) and hydroxyapatite (HA; Ca10(PO4)6(OH)2), were prepared using the solgel method. Ethyl phosphate, hydrated calcium nitrate, and ammonium fluoride were used, respectively, as P, Ca, and F precursors with a Ca:P ratio of 1:72. Powders obtained from the sol-gel process were studied after they were dried at 80°C and heat treated at 550°C. The degree of crystallinity, particle and crystallite size, powder morphology, chemical structure, and phase analysis were investigated by scanning electron microscopy (SEM), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), and Zetasizer experiments. The results of XRD analysis and FTIR showed the presence of hydroxyapatite and fluorapatite phases. The sizes of the crystallites estimated from XRD patterns using the Scherrer equation and the crystallinity of the hydroxyapatite phase were about 20 nm and 70%, respectively. Transmission electron microscope and SEM images and Zetasizer experiments showed an average size of 100 nm. The in vitro behavior of powder was investigated with mouse fibroblast cells. The results of these experiments indicated that the powders were biocompatibile and would not cause toxic reactions. These compounds could be applied for hard-tissue engineering. PMID:21499417

Calcium-deficient apatite synthesized by ammonia hydrolysis of dicalcium phosphate dihydrate: influence of temperature, time, and pressure.

PubMed

Obadia, Laetitia; Rouillon, Thierry; Bujoli, Bruno; Daculsi, Guy; Bouler, Jean Michel

2007-01-01

In this work, calcium-deficient apatites (CDA) were synthesized by ammonia hydrolysis reaction of dicalcium phosphate dihydrate (DCPD; CaHPO4 x 2 H2O) to obtain biphasic calcium phosphates (BCP) without any extraionic substitution. The influence of three parameters was studied: temperature of the reaction (70 and 100 degrees C), time of the reaction (4 and 18 h), and the pressure (open and closed system). Experiments were made according to a factorial design method (FDM) allowing optimization of the number of samples as well as statistical analysis of results. Moreover, the influence of temperature (until 200 degrees C) was investigated. The crystal size of CDA was determined according to the Scherrer's formula and from Rietveld refinements taking the CDA anisotropy into account. The last method seems to be a reliable method to determine crystallite sizes of CDA, since crystallite sizes of CDA along <00l> and directions were accessible. The results describe the hydroxyapatite % (HA%) in BCP by a first-order polynomial equation in the experimental area studied and the HA content was found to increase by raising time and temperature of the reaction. Moreover, the type of reaction system (open/closed vessel) appeared to have little influence on HA%. 2006 Wiley Periodicals, Inc.

Preparation and characterization of nanocrystalline CuO powders with the different surfactants and complexing agent mediated precipitation method

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

Rajendran, V.; Gajendiran, J., E-mail: gaja.nanotech@gmail.com

2014-08-15

Highlights: • CuO nanostructures by surfactants mediated method. • Structural and optical properties of CuO nanostructures changes under the effect of surface modifier. • Citric acid assisted is the best, in terms of size, morphology and optical properties than that of CTAB, SDS and PEG-400. - Abstract: Nanostructures of copper oxide (CuO) was synthesized into crystallite sized ranging from 20 to 50 nm in the presence of different surfactants, and complex agent such as cityl tri methyl ammonium bromide (CTAB), sodium do decyl sulfate (SDS), poly ethylene glycol (PEG-400) and citric acid via a precipitation route. Variations in several parametersmore » and their effects on the structural and optical properties of CuO nanostructures (crystallite size, morphology and band gap) were investigated by XRD, FTIR, SEM and UV analysis. The UV–visible absorption spectra of the different surfactants and complexing agent assisted CuO nanostructures indicates that the estimated optical band gap energy value (1.94–1.98 eV) is higher than that of the bulk CuO value (1.4 eV), which is attributed to the quantum confinement effect. The formation mechanism of different surfactants and complexing agent assisted CuO nanostructures is also proposed.« less

Influence of Zn doping on structural, optical and dielectric properties of LaFeO3

NASA Astrophysics Data System (ADS)

Manzoor, Samiya; Husain, Shahid

2018-05-01

The effect of Zn doping on structural, optical and dielectric properties of nano-crystalline LaFe1‑xZnxO3 (0.0 ≤ x ≤ 0.3) samples have been investigated. These samples are synthesized using conventional solid state reaction route. X-ray diffraction patterns with Rietveld analysis confirm the single phase nature of samples. Further, the sample formation has been confirmed by FTIR spectroscopy. All the samples are formed in orthorhombic crystal symmetry with Pbnm space group. The average crystallite sizes, calculated from the Scherer’s formula, lie in the range below 50 nm. Rietveld refinement technique is used to determine lattice parameters, bond lengths and unit cell volume. Williamson-Hall analysis has been performed to calculate the crystallite size and lattice strain. Crystallite sizes are found to be of nanometer range while the strain is of the order of 10‑3. Zn doping leads to the expansion of volume due to the tensile strain. Optical bandgap has been determined from Kubelka-Munk function using Tauc’s relation. Zinc doping in LaFeO3 leads to decrease in optical bandgap. Dielectric constant as a function of frequency is measured in the frequency range of 75 kHz–5 MHz. The dielectric behavior has been investigated by analyzing ‘universal dielectric response’ (UDR) model. The dielectric constant (ε‧) shows colossal value with Zn doping in the whole frequency range. However, the imaginary part (ε″) shows relaxational behavior which may be attributed to the strong correlation that exists between conduction mechanism and dielectric behavior in ferrites. Cole-Cole analysis has been done that confirms the dielectric material does not follow the ideal Debye theory but shows distribution of relaxation times. The a.c conductivity increases with frequency and with Zn doping due to the increased polaron hopping.

Influence of Fe doping on the structural, optical and acetone sensing properties of sprayed ZnO thin films

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

Prajapati, C.S.; Kushwaha, Ajay; Sahay, P.P., E-mail: dr_ppsahay@rediffmail.com

2013-07-15

Graphical abstract: All the films are found to be polycrystalline ZnO possessing hexagonal wurtzite structure. The intensities of all the peaks are diminished strongly in the Fe-doped films, indicating their lower crystallinity as compared to the undoped ZnO film. The average crystallite size decreases from 35.21 nm (undoped sample) to 15.43 nm (1 at% Fe-doped sample). - Highlights: • Fe-doped ZnO films show smaller crystallinity with crystallite size: 15–26 nm. • Optical band gap in ZnO films decreases on Fe doping. • Fe-doped films exhibit the normal dispersion for the wavelength range 450–600 nm. • PL spectra of the Fe-dopedmore » films show quenching of the broad green-orange emission. • Acetone response of the Fe-doped films increases considerably at 300 °C. - Abstract: The ZnO thin films (undoped and Fe-doped) deposited by chemical spray pyrolysis technique have been analyzed by X-ray powder diffraction (XRD), atomic force microscopy (AFM) and scanning electron microscopy (SEM). Results show that all the films possess hexagonal wurtzite structure of zinc oxide having crystallite sizes in the range 15–36 nm. On 1 at% Fe doping, the surface roughness of the film increases which favors the adsorption of atmospheric oxygen on the film surface and thereby increase in the gas response. Optical studies reveal that the band gap decreases due to creation of some defect energy states below the conduction band edge, arising out of the lattice disorder in the doped films. The refractive index of the films decreases on Fe doping and follows the Cauchy relation of normal dispersion. Among all the films examined, the 1 at% Fe-doped film exhibits the maximum response (∼72%) at 300 °C for 100 ppm concentration of acetone in air.« less

Phase composition and morphological characterization of human kidney stones using IR spectroscopy, scanning electron microscopy and X-ray Rietveld analysis.

PubMed

Chatterjee, Paramita; Chakraborty, Arup; Mukherjee, Alok K

2018-07-05

Pathological calcification in human urinary tract (kidney stones) is a common problem affecting an increasing number of people around the world. Analysis of such minerals or compounds is of fundamental importance for understanding their etiology and for the development of prophylactic measures. In the present study, structural characterization, phase quantification and morphological behaviour of thirty three (33) human kidney stones from eastern India have been carried out using IR spectroscopy (FT-IR), powder X-ray diffraction (PXRD) and scanning electron microscopy (SEM). Quantitative phase composition of kidney stones has been analyzed following the Rietveld method. Based on the quantitative estimates of constituent phases, the calculi samples have been classified into oxalate (OX), uric acid (UA), phosphate (PH) and mixed (MX) groups. Rietveld analysis of PXRD patterns showed that twelve (36%) of the renal calculi were composed exclusively of whewellite (calcium oxalate monohydrate, COM). The remaining twenty one (64%) stones were mixture of phases with oxalate as the major constituent in fourteen (67%) of these stones. The average crystallite size of whewellite in oxalate stones, as determined from the PXRD analysis, varies between 93 (1) nm and 202 (3) nm, whereas the corresponding sizes for the uric acid and struvite crystallites in UA and PH stones are 79 (1)-155 (4) nm and 69 (1)-123(1) nm, respectively. The size of hydroxyapatite crystallites, 10 (1)-21 (1) nm, is smaller by about one order of magnitude compared to other minerals in the kidney stones. A statistical analysis using fifty (50) kidney stones (33 calculi from the present study and 17 calculi reported earlier from our laboratory) revealed that the oxalate group (whewellite, weddellite or mixture of whewellite and weddellite as the major constituent) is the most prevalent (82%) kidney stone type in eastern India. Copyright © 2018 Elsevier B.V. All rights reserved.

Irradiation of zinc single crystal with 500 keV singly-charged carbon ions: surface morphology, structure, hardness, and chemical modifications

NASA Astrophysics Data System (ADS)

Waqas Khaliq, M.; Butt, M. Z.; Saleem, Murtaza

2017-07-01

Cylindrical specimens of (1 0 4) oriented zinc single crystal (diameter  =  6 mm and length  =  5 mm) were irradiated with 500 keV C+1 ions with the help of a Pelletron accelerator. Six specimens were irradiated in an ultra-high vacuum (~10‒8 Torr) with different ion doses, namely 3.94  ×  1014, 3.24  ×  1015, 5.33  ×  1015, 7.52  ×  1015, 1.06  ×  1016, and 1.30  ×  1016 ions cm-2. A field emission scanning electron microscope (FESEM) was utilized for the morphological study of the irradiated specimens. Formation of nano- and sub-micron size rods, clusters, flower- and fork-like structures, etc, was observed. Surface roughness of the irradiated specimens showed an increasing trend with the ions dose. Energy dispersive x-ray spectroscopy (EDX) helped to determine chemical modifications in the specimens. It was found that carbon content varied in the range 22.86-31.20 wt.% and that oxygen content was almost constant, with an average value of 10.16 wt.%. The balance content was zinc. Structural parameters, i.e. crystallite size and lattice strain, were determined by Williamson-Hall analysis using x-ray diffraction (XRD) patterns of the irradiated specimens. Both crystallite size and lattice strain showed a decreasing trend with the increasing ions dose. A good linear relationship between crystallite size and lattice strain was observed. Surface hardness depicted a decreasing trend with the ions dose and followed an inverse Hall-Petch relation. FTIR spectra of the specimens revealed that absorption bands gradually diminish as the dose of singly-charged carbon ions is increased from 3.94  ×  1014 ions cm-1 to 1.30  ×  1016 ions cm-1. This indicates progressive deterioration of chemical bonds with the increase in ion dose.

50 CFR 648.93 - Monkfish minimum fish sizes.

Code of Federal Regulations, 2012 CFR

2012-10-01

... 50 Wildlife and Fisheries 12 2012-10-01 2012-10-01 false Monkfish minimum fish sizes. 648.93... Measures for the NE Multispecies and Monkfish Fisheries § 648.93 Monkfish minimum fish sizes. (a) General... fish size requirements established in this section. Minimum Fish Sizes (Total Length/Tail Length) Total...

50 CFR 648.93 - Monkfish minimum fish sizes.

Code of Federal Regulations, 2013 CFR

2013-10-01

... 50 Wildlife and Fisheries 12 2013-10-01 2013-10-01 false Monkfish minimum fish sizes. 648.93... Measures for the NE Multispecies and Monkfish Fisheries § 648.93 Monkfish minimum fish sizes. (a) General... fish size requirements established in this section. Minimum Fish Sizes (Total Length/Tail Length) Total...

50 CFR 648.93 - Monkfish minimum fish sizes.

Code of Federal Regulations, 2011 CFR

2011-10-01

... 50 Wildlife and Fisheries 10 2011-10-01 2011-10-01 false Monkfish minimum fish sizes. 648.93... Measures for the NE Multispecies and Monkfish Fisheries § 648.93 Monkfish minimum fish sizes. (a) General... fish size requirements established in this section. Minimum Fish Sizes (Total Length/Tail Length) Total...

50 CFR 648.93 - Monkfish minimum fish sizes.

Code of Federal Regulations, 2010 CFR

2010-10-01

... 50 Wildlife and Fisheries 8 2010-10-01 2010-10-01 false Monkfish minimum fish sizes. 648.93... Measures for the NE Multispecies and Monkfish Fisheries § 648.93 Monkfish minimum fish sizes. (a) General... fish size requirements established in this section. Minimum Fish Sizes (Total Length/Tail Length) Total...

Electrical and magnetic properties of nano-sized magnesium ferrite

NASA Astrophysics Data System (ADS)

T, Smitha; X, Sheena; J, Binu P.; Mohammed, E. M.

2015-02-01

Nano-sized magnesium ferrite was synthesized using sol-gel techniques. Structural characterization was done using X-ray diffractometer and Fourier Transform Infrared Spectrometer. Vibration Sample Magnetometer was used to record the magnetic measurements. XRD analysis reveals the prepared sample is single phasic without any impurity. Particle size calculation shows the average crystallite size of the sample is 19nm. FTIR analysis confirmed spinel structure of the prepared samples. Magnetic measurement study shows that the sample is ferromagnetic with high degree of isotropy. Hysterisis loop was traced at temperatures 100K and 300K. DC electrical resistivity measurements show semiconducting nature of the sample.

Self-organization of the magnetization in ferromagnetic nanowires

NASA Astrophysics Data System (ADS)

Ivanov, A. A.; Orlov, V. A.

2017-10-01

In this work we demonstrate the occurrence of the characteristic spatial scale in the distribution of magnetization unrelated to the domain wall or crystallite size with using computer simulation of magnetization in a polycrystalline ferromagnetic nanowire. This is the stochastic domain size. We show that this length is included in the spectral density of the pinning force of domain wall on inhomogeneities of the crystallographic anisotropy. The constant and distribution of easy axes directions of the effective anisotropy of stochastic domain, are analytically calculated.

Size Determination of Y2O3 Crystallites in MgO Composite Using Mie Scattering

DTIC Science & Technology

2017-11-07

particle size, and the path length through the material to generate an expected light transmission spectrum. These calculated curves were compared to...materials. In the current work, light transmission data are compared to the theoretical curves generated by the Mie scattering model in an attempt to...Since the authors wanted to compare the model’s predictions to the experimental %T values, it seemed logical to start with Beer’s Law: )exp()1( 2

Size dependence of magnetorheological properties of cobalt ferrite ferrofluid

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

Radhika, B.; Sahoo, Rasmita; Srinath, S., E-mail: srinath@uohyd.ac.in

2015-06-24

Cobalt Ferrite nanoparticles were synthesized using co-precipitation method at reaction temperatures of 40°C and 80°C. X-Ray diffraction studies confirm cubic phase formation. The average crystallite sizes were found to be ∼30nm and ∼48nm for 40°C sample and 80°C sample respectively. Magnetic properties measured using vibrating sample magnetometer show higher coercivety and magnetization for sample prepared at 80°C. Magnetorheological properties of CoFe2O4 ferrofluids were measured and studied.

Restricting the high-temperature growth of nanocrystalline tin oxide

NASA Astrophysics Data System (ADS)

Savin, S.; Chadwick, A. V.

2003-01-01

The sensitivity of tin oxide is dependent on various factors, one of which is the grain size. Three methods have been investigated with the aim of stabilising the grain size in the nanometer range, namely; (i) encapsulation within a silica matrix, (ii) coating the crystallites with hexamethyldisilazane and (iii) pinning the grain boundaries with a second metal oxide nanocrystal. The resulting materials have been characterised by X-ray powder diffraction (XRPD), Extended X-ray absorption fine structure (EXAFS) and conductivity measurements.

Study on antibacterial alginate-stabilized copper nanoparticles by FT-IR and 2D-IR correlation spectroscopy

PubMed Central

Díaz-Visurraga, Judith; Daza, Carla; Pozo, Claudio; Becerra, Abraham; von Plessing, Carlos; García, Apolinaria

2012-01-01

Background The objective of this study was to clarify the intermolecular interaction between antibacterial copper nanoparticles (Cu NPs) and sodium alginate (NaAlg) by Fourier transform infrared spectroscopy (FT-IR) and to process the spectra applying two-dimensional infrared (2D-IR) correlation analysis. To our knowledge, the addition of NaAlg as a stabilizer of copper nanoparticles has not been previously reported. It is expected that the obtained results will provide valuable additional information on: (1) the influence of reducing agent ratio on the formation of copper nanoparticles in order to design functional nanomaterials with increased antibacterial activity, and (2) structural changes related to the incorporation of Cu NPs into the polymer matrix. Methods Cu NPs were prepared by microwave heating using ascorbic acid as reducing agent and NaAlg as stabilizing agent. The characterization of synthesized Cu NPs by ultraviolet visible spectroscopy, transmission electron microscopy (TEM), electron diffraction analysis, X-ray diffraction (XRD), and semiquantitative analysis of the weight percentage composition indicated that the average particle sizes of Cu NPs are about 3–10 nm, they are spherical in shape, and consist of zerovalent Cu and Cu2O. Also, crystallite size and relative particle size of stabilized Cu NPs were calculated by XRD using Scherrer’s formula and FT from the X-ray diffraction data. Thermogravimetric analysis, differential thermal analysis, differential scanning calorimetry (DSC), FT-IR, second-derivative spectra, and 2D-IR correlation analysis were applied to studying the stabilization mechanism of Cu NPs by NaAlg molecules. The minimum inhibitory concentration (MIC) and minimum bactericidal concentration (MBC) of stabilized Cu NPs against five bacterial strains (Staphylococccus aureus ATCC 6538P, Escherichia coli ATCC 25922 and O157: H7, and Salmonella enterica serovar Typhimurium ATCC 13311 and 14028) were evaluated with macrodilution, agar dilution plate count, and well-diffusion methods. Results On the basis of the semiquantitative analysis, there was a direct correlation between the reducing agent ratio and the percentage of zerovalent Cu. This was confirmed with the statistical analysis of population of Cu NPs from TEM micrographs. At lower reducing agent ratios, two phases coexist (Cu2O and zerovalent Cu) due to incomplete reduction of copper ions by the reducing agent; however, at higher reducing agent ratios, the Cu NPs consist mainly of zerovalent Cu. Crystallite size and relative particle size of stabilized Cu NPs showed considerable differences in results and tendencies in respect to TEM analysis. However, the relative particle size values obtained from FT of XRD data agreed well with the histograms from the TEM observations. From FT results, the relative particle size and reducing agent ratio of stabilized Cu NPs showed an inverse correlation. The incomplete reduction of copper ions at lower reducing agent ratios was also confirmed by DSC studies. FT-IR and 2D-IR correlation spectra analysis suggested the first event involved in the stabilization of Cu NPs is their electrostatic interaction with –C=O of carboxylate groups of NaAlg, followed by the interaction with the available O–C–O−, and finally with the –OH groups. Bacterial susceptibility to stabilized nanoparticles was found to vary depending on the bacterial strains. The lowest MIC and MBC of stabilized Cu NPs ranged between 2 mg/L and 8 mg/L for all studied strains. Disk-diffusion studies with both E. coli strains revealed greater effectiveness of the stabilized Cu NPs compared to the positive controls (cloxacillin, amoxicillin, and nitrofurantoin). S. aureus showed the highest sensitivity to stabilized Cu NPs compared to the other studied strains. Conclusion Cu NPs were successfully synthesized via chemical reduction assisted with microwave heating. Average particle size, polydispersity, and phase composition of Cu NPs depended mainly on the reducing agent ratio. Likewise, thermal stability and antibacterial activity of stabilized Cu NPs were affected by their phase composition. Because of the carboxylate groups in polymer chains, the structural changes of stabilized Cu NPs are different from those of NaAlg. NaAlg acted as a size controller and stabilizing agent of Cu NPs, due to their ability to bind strongly to the metal surface. Our study on the stabilizing agent–dependent structural changes of stabilized NPs is helpful for wide application of NaAlg as an important biopolymer. PMID:22848180

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

Shetty, G. Rajesha; Kumar, R. Madhu; Rao, B. Lakshmeesha

In this work, the structural and mechanical stability of silk fibroin/Hydroxypropylmethyl cellulose (SF-HPMC) blend films were characterized by X-ray diffraction (XRD) and Universal Testing Machine (UTM). The results indicate that with the introduction of HPMC, the interactions between SF and HPMC results in improved crystallite size and increase in mechanical properties. The blend film obtained is more flexible compared to pure SF film.

TEM characterization of nanodiamond thin films.

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

Qin, L.-C.; Zhou, D.; Krauss, A. R.

The microstructure of thin films grown by microwave plasma-enhanced chemical vapor deposition (MPCVD) from fullerene C{sub 60} precursors has been characterized by scanning electron microscopy (SEM), selected-area electron diffraction (SAED), bright-field electron microscopy, high-resolution electron microscopy (HREM), and parallel electron energy loss spectroscopy (PEELS). The films are composed of nanosize crystallites of diamond, and no graphitic or amorphous phases were observed. The diamond crystallite size measured from lattice images shows that most grains range between 3-5 nm, reflecting a gamma distribution. SAED gave no evidence of either sp2-bonded glassy carbon or sp3-bonded diamondlike amorphous carbon. The sp2-bonded configuration found inmore » PEELS was attributed to grain boundary carbon atoms, which constitute 5-10% of the total. Occasionally observed larger diamond grains tend to be highly faulted.« less

Structural Evolution during Milling, Annealing, and Rapid Consolidation of Nanocrystalline Fe–10Cr–3Al Powder

PubMed Central

Kumar, Rajiv; Bakshi, S. R.; Joardar, Joydip; Parida, S.; Raja, V. S.; Singh Raman, R. K.

2017-01-01

Structural changes during the deformation-induced synthesis of nanocrystalline Fe–10Cr–3Al alloy powder via high-energy ball milling followed by annealing and rapid consolidation by spark plasma sintering were investigated. Reduction in crystallite size was observed during the synthesis, which was associated with the lattice expansion and rise in dislocation density, reflecting the generation of the excess grain boundary interfacial energy and the excess free volume. Subsequent annealing led to the exponential growth of the crystallites with a concomitant drop in the dislocation density. The rapid consolidation of the as-synthesized nanocrystalline alloy powder by the spark plasma sintering, on the other hand, showed only a limited grain growth due to the reduction of processing time for the consolidation by about 95% when compared to annealing at the same temperature. PMID:28772633

Structural, magnetic, dielectric, and electrical properties of NiFe2O4 spinel ferrite nanoparticles prepared by honey-mediated sol-gel combustion

NASA Astrophysics Data System (ADS)

Yadav, Raghvendra Singh; Kuřitka, Ivo; Vilcakova, Jarmila; Havlica, Jaromir; Masilko, Jiri; Kalina, Lukas; Tkacz, Jakub; Enev, Vojtěch; Hajdúchová, Miroslava

2017-08-01

In this study, NiFe2O4 nanoparticles were synthesized using a honey-mediated sol-gel combustion method. The synthesized nanoparticles and samples annealed at 800 °C and 1100 °C were characterized by X-ray diffraction (XRD), field emission-scanning electron microscopy (FE-SEM), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), and vibrating sample magnetometry (VSM). XRD and Raman spectroscopy confirmed the formation of a cubic spinel ferrite structure. FE-SEM demonstrated the octahedral morphology of the NiFe2O4 spinel ferrite nanoparticles with sizes ranging from 10 to 70 nm. Quantitative analysis based on XPS suggested a mixed spinel structure comprising NiFe2O4 nanoparticles. XPS analysis determined occupation formulae of (Ni0.212+ Fe0.443+)[Ni0.792+ Fe1.563+]O4 and (Ni0.232+ Fe0.503+)[Ni0.772+ Fe1.503+]O4, for the as-prepared NiFe2O4 nanoparticles and those annealed at 1100 °C, respectively. Magnetic measurements showed that the saturation magnetization increased with the crystallite size from 32.3 emu/g (20 nm) to 49.9 emu/g (163 nm), whereas the coercivity decreased with the crystallite size from 162 Oe (20 nm) to 47 Oe (163 nm). Furthermore, the dielectric constant, dielectric loss tangent, and AC conductivity of the NiFe2O4 nanoparticles were dependent on the frequency (1-107 Hz) and grain size. The influence of the grain size was also observed by modulus spectroscopy based on the Cole-Cole plot.

50 CFR 648.165 - Bluefish minimum fish sizes.

Code of Federal Regulations, 2014 CFR

2014-10-01

... 50 Wildlife and Fisheries 12 2014-10-01 2014-10-01 false Bluefish minimum fish sizes. 648.165... Measures for the Atlantic Bluefish Fishery § 648.165 Bluefish minimum fish sizes. If the MAFMC determines through its annual review or framework adjustment process that minimum fish sizes are necessary to ensure...

50 CFR 648.165 - Bluefish minimum fish sizes.

Code of Federal Regulations, 2013 CFR

2013-10-01

... 50 Wildlife and Fisheries 12 2013-10-01 2013-10-01 false Bluefish minimum fish sizes. 648.165... Measures for the Atlantic Bluefish Fishery § 648.165 Bluefish minimum fish sizes. If the MAFMC determines through its annual review or framework adjustment process that minimum fish sizes are necessary to ensure...

50 CFR 648.165 - Bluefish minimum fish sizes.

Code of Federal Regulations, 2012 CFR

2012-10-01

... 50 Wildlife and Fisheries 12 2012-10-01 2012-10-01 false Bluefish minimum fish sizes. 648.165... Measures for the Atlantic Bluefish Fishery § 648.165 Bluefish minimum fish sizes. If the MAFMC determines through its annual review or framework adjustment process that minimum fish sizes are necessary to ensure...

50 CFR 648.162 - Minimum fish sizes.

Code of Federal Regulations, 2010 CFR

2010-10-01

... 50 Wildlife and Fisheries 8 2010-10-01 2010-10-01 false Minimum fish sizes. 648.162 Section 648... Atlantic Bluefish Fishery § 648.162 Minimum fish sizes. If the Council determines through its annual review or framework adjustment process that minimum fish sizes are necessary to assure that the fishing...

Physics of Hard Spheres Experiment: Significant and Quantitative Findings Made

NASA Technical Reports Server (NTRS)

Doherty, Michael P.

2000-01-01

Direct examination of atomic interactions is difficult. One powerful approach to visualizing atomic interactions is to study near-index-matched colloidal dispersions of microscopic plastic spheres, which can be probed by visible light. Such spheres interact through hydrodynamic and Brownian forces, but they feel no direct force before an infinite repulsion at contact. Through the microgravity flight of the Physics of Hard Spheres Experiment (PHaSE), researchers have sought a more complete understanding of the entropically driven disorder-order transition in hard-sphere colloidal dispersions. The experiment was conceived by Professors Paul M. Chaikin and William B. Russel of Princeton University. Microgravity was required because, on Earth, index-matched colloidal dispersions often cannot be density matched, resulting in significant settling over the crystallization period. This settling makes them a poor model of the equilibrium atomic system, where the effect of gravity is truly negligible. For this purpose, a customized light-scattering instrument was designed, built, and flown by the NASA Glenn Research Center at Lewis Field on the space shuttle (shuttle missions STS 83 and STS 94). This instrument performed both static and dynamic light scattering, with sample oscillation for determining rheological properties. Scattered light from a 532- nm laser was recorded either by a 10-bit charge-coupled discharge (CCD) camera from a concentric screen covering angles of 0 to 60 or by sensitive avalanche photodiode detectors, which convert the photons into binary data from which two correlators compute autocorrelation functions. The sample cell was driven by a direct-current servomotor to allow sinusoidal oscillation for the measurement of rheological properties. Significant microgravity research findings include the observation of beautiful dendritic crystals, the crystallization of a "glassy phase" sample in microgravity that did not crystallize for over 1 year in 1g (Earth's gravity), and the emergence of face-centered-cubic (FCC) crystals late in the coarsening process (as small crystallites lost particles to the slow ripening of large crystallites). Significant quantitative findings from the microgravity experiments have been developed describing complex interactions among crystallites during the growth process, as concentration fields overlap in the surrounding disordered phase. Time-resolved Bragg scattering under microgravity captures one effect of these interactions quite conclusively for the sample at a volume fraction of 0.528. From the earliest time until the sample is almost fully crystalline, the size and overall crystallinity grow monotonically, but the number of crystallites per unit volume (number density) falls. Apparently nucleation is slower than the loss of crystallites because of the transfer of particles from small to large crystals. Thus, coarsening occurs simultaneously with growth, rather than following the completion of nucleation and growth as is generally assumed. In the same sample, an interesting signature appears in the apparent number density of crystallites and the volume fraction within the crystallites shortly before full crystallinity is reached. A brief upturn in both indicates the creation of more domains of the size of the average crystallite simultaneous with the compression of the crystallites. Only the emergence of dendritic arms offers a reasonable explanation. The arms would be "seen" by the light scattering as separate domains whose smaller radii of curvature would compress the interior phase. In fiscal year 1999, numerous papers, a doctoral dissertation, and the PHaSE final report were produced. Although this flight project has been completed, plans are in place for a follow-on colloid experiment by Chaikin and Russel that employs a light microscope within Glenn's Fluids and Combustion Facility on the International Space Station. PHaSE is providing us with a deeper understanding of the nure of phase transitions. The knowledge derived has added to the understanding of condensed matter. In addition, the burgeoning study of the dynamics of colloidal self-assembly may lead to the development of a range of photonic materials that control the desirable properties of light. Thus, applications of ordered colloidal structures include not only ultrastructure ceramics, but also photonic crystals and photothermal nanosecond light-switching devices. Industries dealing with semiconductors, electro-optics, ceramics, and composites stand to benefit from such advancements.

Reasons for the lack of chemical stability of treated water rich in magnesium.

PubMed

Swietlik, Joanna; Raczyk-Stanisławiak, Urszula; Piszora, Paweł; Nawrocki, Jacek

2011-12-01

Chemical stability of water should be high enough to ensure that the water reaching the consumers would have the same composition as at the treatment plant. The drinking water supplied by one of the water treatment plants for the city of Poznań was observed to produce periodically white non-sedimenting precipitate on boiling, deteriorating its organoleptic properties. The phenomenon was found to be related to a high content of magnesium in the water taken for treatment and low content of other ions besides bicarbonates. XRD and SEM analyses have shown that a low ratio of calcium ions to magnesium ions leads to formation of calcite crystals on water boiling in which a fraction of cationic crystallographic sites are substituted with Mg(2+) ions giving (Ca(1-x)Mg(x))CO(3) crystallites. Such crystallites have smaller size than those of calcite formed on boiling water coming from other Poznań suppliers. The smaller size of the crystallites is responsible for their slower sedimentation and hence the observed increase in the water turbidity on its boiling. It has been proved that the appearance of precipitates in drinking water at the consumers can be achieved by reduction of the Mg/(Mg + Ca) ratio to below 3, which would inhibit peptisation of the precipitate and prevent water opacity and/or adjustment of pH of the raw water and removal of the carbon dioxide released to convert some carbonate hardness into non-carbonate one. These measures will limit the amount of the precipitate forming upon water boiling and change its microcrystalline type into an easier sedimenting one. Copyright © 2011 Elsevier Ltd. All rights reserved.

Tailoring the synthesis of supported Pd catalysts towards desired structure and size of metal particles.

PubMed

Suresh, Gatla; Radnik, Jörg; Kalevaru, Venkata Narayana; Pohl, Marga-Martina; Schneider, Matthias; Lücke, Bernhard; Martin, Andreas; Madaan, Neetika; Brückner, Angelika

2010-05-14

In a systematic study, the influence of different preparation parameters on phase composition and size of metal crystallites and particles in Pd-Cu/TiO(2) and Pd-Sb/TiO(2) catalyst materials has been explored. Temperature and atmosphere of thermal pretreatment (pure He or 10% H(2)/He), nature of metal precursors (chlorides, nitrates or acetates) as well as of ammonium additives (ammonium sulfate, nitrate, carbonate) and urea were varied with the aim of tailoring the synthesis procedure for the preferential formation of metal particles with similar size and structure as observed recently in active catalysts after long-term equilibration under catalytic reaction conditions in acetoxylation of toluene to benzylacetate. Among the metal precursors and additives, the chloride metal precursors and (NH(4))(2)SO(4) were most suitable. Upon thermal pretreatment of Pd-Sb or Pd-Cu precursors, chloroamine complexes of Pd and Cu are formed, which decompose above 220 degrees C to metallic phases independent of the atmosphere. In He, metallic Pd particles were formed with both the co-components. In H(2)/He flow, Pd-Cu precursors were converted to core-shell particles with a Cu shell and a Pd core, while Sb(1)Pd(1) and Sb(7)Pd(20) alloy phases were formed in the presence of Sb. Metal crystallites of about 40 nm agglomerate to particles of up to 150 nm in He and to even larger size in H(2)/He.

The Effect of Contact Non-equilibrium Plasma on Structural and Magnetic Properties of Mn Х Fe3 - X О4 Spinels.

PubMed

Frolova, L A; Derhachov, M P

2017-08-23

Nano-sized manganese ferrites Mn х Fe 3 - х О 4 (х = 0-1.3) were prepared using contact non-equilibrium plasma (CNP) in two different pH (11.5 and 12.5). The influence of synthesis conditions (e.g., cation ratio and initial pH) on phase composition, crystallite size, and magnetic properties were investigated employing X-ray diffraction (XRD), differential thermal analysis (DTA), Fourier transform infrared (FTIR), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and magnetic measurement techniques. The formation of monodispersed faceted ferrite particles at х = 0-0.8 was shown. The FTIR spectra revealed reflection in region 1200-1700 cm -1 caused by the presence of water adsorbed on the surface of Fe 3 - x Mn x O 4 micro-granules or embedded into their crystal lattice. The most sensitivity of reflection spectra to the composition changes takes place within a 400-1200 cm -1 range, typical to the stretching vibrations of Fe(Mn)-O (up to 700 cm -1 ), Fe(Mn)-OH, and Fe(Mn)-OH 2 bonds (over 700 cm -1 ). The XRD results showed that the nanocrystalline Mn х Fe 3 - х О 4 (0 < x < 1.0) had cubic spinel crystal structure with average crystallite size 48-49 A. The decrease of crystalline size with the x increase was also observed.

Characterization of Zeolite in Zeolite-Geopolymer Hybrid Bulk Materials Derived from Kaolinitic Clays

PubMed Central

Takeda, Hayami; Hashimoto, Shinobu; Yokoyama, Hiroaki; Honda, Sawao; Iwamoto, Yuji

2013-01-01

Zeolite-geopolymer hybrid materials have been formed when kaolin was used as a starting material. Their characteristics are of interest because they can have a wide pore size distribution with micro- and meso-pores due to the zeolite and geopolymer, respectively. In this study, Zeolite-geopolymer hybrid bulk materials were fabricated using four kinds of kaolinitic clays (a halloysite and three kinds of kaolinite). The kaolinitic clays were first calcined at 700 °C for 3 h to transform into the amorphous aluminosilicate phases. Alkali-activation treatment of the metakaolin yielded bulk materials with different amounts and types of zeolite and different compressive strength. This study investigated the effects of the initial kaolinitic clays on the amount and types of zeolite in the resultant geopolymers as well as the strength of the bulk materials. The kaolinitic clays and their metakaolin were characterized by XRD analysis, chemical composition, crystallite size, 29Si and 27Al MAS NMR analysis, and specific surface area measurements. The correlation between the amount of zeolite formed and the compressive strength of the resultant hybrid bulk materials, previously reported by other researchers was not positively observed. In the studied systems, the effects of Si/Al and crystalline size were observed. When the atomic ratio of Si/Al in the starting kaolinitic clays increased, the compressive strength of the hybrid bulk materials increased. The crystallite size of the zeolite in the hybrid bulk materials increased with decreasing compressive strength of the hybrid bulk materials. PMID:28809241

Synthesis and characterization of arsenic-doped cysteine-capped thoria-based nanoparticles

NASA Astrophysics Data System (ADS)

Pereira, F. J.; Díez, M. T.; Aller, A. J.

2013-09-01

Thoria materials have been largely used in the nuclear industry. Nonetheless, fluorescent thoria-based nanoparticles provide additional properties to be applied in other fields. Thoria-based nanoparticles, with and without arsenic and cysteine, were prepared in 1,2-ethanediol aqueous solutions by a simple precipitation procedure. The synthesized thoria-based nanoparticles were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), energy dispersive X-ray spectrometry (ED-XRS), Raman spectroscopy, Fourier transform infrared (FT-IR) spectroscopy and fluorescence microscopy. The presence of arsenic and cysteine, as well as the use of a thermal treatment facilitated fluorescence emission of the thoria-based nanoparticles. Arsenic-doped and cysteine-capped thoria-based nanoparticles prepared in 2.5 M 1,2-ethanediol solutions and treated at 348 K showed small crystallite sizes and strong fluorescence. However, thoria nanoparticles subjected to a thermal treatment at 873 K also produced strong fluorescence with a very narrow size distribution and much smaller crystallite sizes, 5 nm being the average size as shown by XRD and TEM. The XRD data indicated that, even after doping of arsenic in the crystal lattice of ThO2, the samples treated at 873 K were phase pure with the fluorite cubic structure. The Raman and FT-IR spectra shown the most characteristics vibrational peaks of cysteine together with other peaks related to the bonds of this molecule to thoria and arsenic when present.

Characterization of the enhancement effect of Na2CO3 on the sulfur capture capacity of limestones.

PubMed

Laursen, Karin; Kern, Arnt A; Grace, John R; Lim, C Jim

2003-08-15

It has been known for a long time that certain additives (e.g., NaCl, CaCl2, Na2CO3, Fe2O3) can increase the sulfur dioxide capture-capacity of limestones. In a recent study we demonstrated that very small amounts of Na2CO3 can be very beneficial for producing sorbents of very high sorption capacities. This paper explores what contributes to these significant increases. Mercury porosimetry measurements of calcined limestone samples reveal a change in the pore-size from 0.04-0.2 microm in untreated samples to 2-10 microm in samples treated with Na2CO3--a pore-size more favorable for penetration of sulfur into the particles. The change in pore-size facilitates reaction with lime grains throughout the whole particle without rapid plugging of pores, avoiding premature change from a fast chemical reaction to a slow solid-state diffusion controlled process, as seen for untreated samples. Calcination in a thermogravimetric reactor showed that Na2CO3 increased the rate of calcination of CaCO3 to CaO, an effect which was slightly larger at 825 degrees C than at 900 degrees C. Peak broadening analysis of powder X-ray diffraction data of the raw, calcined, and sulfated samples revealed an unaffected calcite size (approximately 125-170 nm) but a significant increase in the crystallite size for lime (approximately 60-90 nm to approximately 250-300 nm) and less for anhydrite (approximately 125-150 nm to approximately 225-250 nm). The increase in the crystallite and pore-size of the treated limestones is attributed to an increase in ionic mobility in the crystal lattice due to formation of vacancies in the crystals when Ca is partly replaced by Na.

50 CFR 648.126 - Scup minimum fish sizes.

Code of Federal Regulations, 2014 CFR

2014-10-01

... 50 Wildlife and Fisheries 12 2014-10-01 2014-10-01 false Scup minimum fish sizes. 648.126 Section... Scup Fishery § 648.126 Scup minimum fish sizes. (a) Moratorium (commercially) permitted vessels. The... whole fish or any part of a fish found in possession, e.g., fillets. These minimum sizes may be adjusted...

50 CFR 648.126 - Scup minimum fish sizes.

Code of Federal Regulations, 2012 CFR

2012-10-01

... 50 Wildlife and Fisheries 12 2012-10-01 2012-10-01 false Scup minimum fish sizes. 648.126 Section... Scup Fishery § 648.126 Scup minimum fish sizes. (a) Moratorium (commercially) permitted vessels. The... whole fish or any part of a fish found in possession, e.g., fillets. These minimum sizes may be adjusted...

50 CFR 648.126 - Scup minimum fish sizes.

Code of Federal Regulations, 2013 CFR

2013-10-01

... 50 Wildlife and Fisheries 12 2013-10-01 2013-10-01 false Scup minimum fish sizes. 648.126 Section... Scup Fishery § 648.126 Scup minimum fish sizes. (a) Moratorium (commercially) permitted vessels. The... whole fish or any part of a fish found in possession, e.g., fillets. These minimum sizes may be adjusted...

Real-space microscopic electrical imaging of n+-p junction beneath front-side Ag contact of multicrystalline Si solar cells

NASA Astrophysics Data System (ADS)

Jiang, C.-S.; Li, Z. G.; Moutinho, H. R.; Liang, L.; Ionkin, A.; Al-Jassim, M. M.

2012-04-01

We investigated the quality of the n+-p diffused junction beneath the front-side Ag contact of multicrystalline Si solar cells by characterizing the uniformities of electrostatic potential and doping concentration across the junction using the atomic force microscopy-based electrical imaging techniques of scanning Kelvin probe force microscopy and scanning capacitance microscopy. We found that Ag screen-printing metallization fired at the over-fire temperature significantly degrades the junction uniformity beneath the Ag contact grid, whereas metallization at the optimal- and under-fire temperatures does not cause degradation. Ag crystallites with widely distributed sizes were found at the Ag-grid/emitter-Si interface of the over-fired cell, which is associated with the junction damage beneath the Ag grid. Large crystallites protrude into Si deeper than the junction depth. However, the junction was not broken down; instead, it was reformed on the entire front of the crystallite/Si interface. We propose a mechanism of junction-quality degradation, based on emitter Si melting at the temperature around the Ag-Si eutectic point during firing, and subsequent re-crystallization with incorporation of Ag and other impurities and with formation of crystallographic defects during quenching. The effect of this junction damage on solar cell performance is discussed.

Real-Space Microscopic Electrical Imaging of n+-p Junction Beneath Front-Side Ag Contact of Multicrystalline Si Solar Cells

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

Jiang, C. S.; Li, Z. G.; Moutinho, H. R.

2012-04-15

We investigated the quality of the n+-p diffused junction beneath the front-side Ag contact of multicrystalline Si solar cells by characterizing the uniformities of electrostatic potential and doping concentration across the junction using the atomic force microscopy-based electrical imaging techniques of scanning Kelvin probe force microscopy and scanning capacitance microscopy. We found that Ag screen-printing metallization fired at the over-fire temperature significantly degrades the junction uniformity beneath the Ag contact grid, whereas metallization at the optimal- and under-fire temperatures does not cause degradation. Ag crystallites with widely distributed sizes were found at the Ag-grid/emitter-Si interface of the over-fired cell, whichmore » is associated with the junction damage beneath the Ag grid. Large crystallites protrude into Si deeper than the junction depth. However, the junction was not broken down; instead, it was reformed on the entire front of the crystallite/Si interface. We propose a mechanism of junction-quality degradation, based on emitter Si melting at the temperature around the Ag-Si eutectic point during firing, and subsequent re-crystallization with incorporation of Ag and other impurities and with formation of crystallographic defects during quenching. The effect of this junction damage on solar cell performance is discussed.« less

Preparation, structure, and digestibility of crystalline A- and B-type aggregates from debranched waxy starches.

PubMed

Cai, Liming; Shi, Yong-Cheng

2014-05-25

Highly crystalline A- and B-type aggregates were prepared from short linear α-1,4 glucans generated from completely debranched waxy maize and waxy potato starches by manipulating the chain length and crystallization conditions including starch solids concentration and crystallization temperature. The A-type crystalline products were more resistant to enzyme digestion than the B-type crystalline products, and the digestibility of the A- and B-type allomorphs was not correlated with the size of the aggregates formed. Annealing increased the peak melting temperature of the B-type crystallites, making it similar to that of the A-type crystallites, but did not improve the enzyme resistance of the B-type crystalline products. The possible reason for these results was due to the compact morphology as well as the denser packing pattern of double helices in A-type crystallites. Our observations counter the fact that most B-type native starches are more enzyme-resistant than A-type native starches. Crystalline type per se does not seem to be the key factor that controls the digestibility of native starch granules; the resistance of native starches with a B-type X-ray diffraction pattern is probably attributed to the other structural features in starch granules. Copyright © 2014 Elsevier Ltd. All rights reserved.

Changes Found on Run-In and Scuffed Surfaces of Steel Chrome Plate, and Cast Iron

NASA Technical Reports Server (NTRS)

Good, J. N.; Godfrey, Douglas

1947-01-01

A study was made of run-in and scuffed steel, chrome-plate, and cast-iron surfaces. X-ray and electron diffraction techniques, micro-hardness determinations, and microscopy were used. Surface changes varied and were found to include three classes: chemical reaction, hardening, and crystallite-size alteration. The principal chemical reactions were oxidation and carburization.

High capacity Li-ion battery anodes: Impact of crystallite size, surface chemistry and PEG-coating

DOE PAGES

Minnici, Krysten; Kwon, Yo Han; Huie, Matthew M.; ...

2017-12-06

Battery electrodes are complex mesoscale systems comprised of an active material, conductive agent, current collector, and polymeric binder. Previous work showed that introduction of poly [3-(potassium-4-butanoate) thiophene] (PPBT) as a binder component coupled with a polyethylene glycol (PEG) surface coating on magnetite (Fe 3O 4) nanoparticles enhanced electron and ion transport in the high capacity anode system. Here, the impact of Fe 3O 4 crystallite size (10 nm vs. 20 nm) and surface chemistry were explored to evaluate their effects on interfacial interactions within the composite PEG/PPBT based electrodes and resultant battery performance. The Fe 3O 4 synthesis methods inevitablymore » lead to differences in surface chemistry. For instance, the Fe 3O 4 particles synthesized using ammonium hydroxide appeared more dispersed, and afforded improved rate capability performance. Notably, chemical interactions between the active nanoparticles and PPBT binder were only seen with particles synthesized using triethylamine. Capacity retention and cycling performance were unaffected. Thus, this study provides fundamental insights into the significant impact of active material synthesis on the design and fabrication of composite battery electrodes.« less

Temperature dependent surface and spectral modifications of nano V2O5 films

NASA Astrophysics Data System (ADS)

Manthrammel, M. Aslam; Fatehmulla, A.; Al-Dhafiri, A. M.; Alshammari, A. S.; Khan, Aslam

2017-03-01

Nanocrystalline V2O5 films have been deposited on glass substrates at 300°C substrate temperature using thermal evaporation technique and were subjected to thermal annealing at different temperatures 350, 400, and 550°C. X-ray diffraction (XRD) spectra exhibit sharper and broader characteristic peaks respectively indicating the rearrangement of nanocrystallite phases with annealing temperatures. Other phases of vanadium oxides started emerging with the rise in annealing temperature and the sample converted completely to VO2 (B) phase at 550°C annealing. FESEM images showed an increase in crystallite size with 350 and 400°C annealing temperatures followed by a decrease in crystallite size for the sample annealed at 550°C. Transmission spectra showed an initial redshift of the fundamental band edge with 350 and 400°C while a blue shift for the sample annealed at 550°C, which was in agreement with XRD and SEM results. The films exhibited smart window properties as well as nanorod growth at specific annealing temperatures. Apart from showing the PL and defect related peaks, PL studies also supported the observations made in the transmission spectra.

Multifunctional Eu3+- and Er3+/Yb3+-doped GdVO4 nanoparticles synthesized by reverse micelle method

PubMed Central

Gavrilović, Tamara V.; Jovanović, Dragana J.; Lojpur, Vesna; Dramićanin, Miroslav D.

2014-01-01

Synthesis of Eu3+- and Er3+/Yb3+-doped GdVO4 nanoparticles in reverse micelles and their multifunctional luminescence properties are presented. Using cyclohexane, Triton X-100, and n-pentanol as the oil, surfactant, and co-surfactant, respectively, crystalline nanoparticles with ~4 nm diameter are prepared at low temperatures. The particle size assessed using transmission electron microscopy is similar to the crystallite size obtained from X-ray diffraction measurements, suggesting that each particle comprises a single crystallite. Eu3+-doped GdVO4 nanoparticles emit red light through downconversion upon UV excitation. Er3+/Yb3+-doped GdVO4 nanoparticles exhibit several functions; apart from the downconversion of UV radiation into visible green light, they act as upconvertors, transforming near-infrared excitation (980 nm) into visible green light. The ratio of green emissions from 2H11/2 → 2I15/2 and 4S3/2 → 4I15/2 transitions is temperature dependent and can be used for nanoscale temperature sensing with near-infrared excitation. The relative sensor sensitivity is 1.11%K−1, which is among the highest sensitivities recorded for upconversion-luminescence-based thermometers. PMID:24572638

Multifunctional Eu3+- and Er3+/Yb3+-doped GdVO4 nanoparticles synthesized by reverse micelle method

NASA Astrophysics Data System (ADS)

Gavrilović, Tamara V.; Jovanović, Dragana J.; Lojpur, Vesna; Dramićanin, Miroslav D.

2014-02-01

Synthesis of Eu3+- and Er3+/Yb3+-doped GdVO4 nanoparticles in reverse micelles and their multifunctional luminescence properties are presented. Using cyclohexane, Triton X-100, and n-pentanol as the oil, surfactant, and co-surfactant, respectively, crystalline nanoparticles with ~4 nm diameter are prepared at low temperatures. The particle size assessed using transmission electron microscopy is similar to the crystallite size obtained from X-ray diffraction measurements, suggesting that each particle comprises a single crystallite. Eu3+-doped GdVO4 nanoparticles emit red light through downconversion upon UV excitation. Er3+/Yb3+-doped GdVO4 nanoparticles exhibit several functions; apart from the downconversion of UV radiation into visible green light, they act as upconvertors, transforming near-infrared excitation (980 nm) into visible green light. The ratio of green emissions from 2H11/2 --> 2I15/2 and 4S3/2 --> 4I15/2 transitions is temperature dependent and can be used for nanoscale temperature sensing with near-infrared excitation. The relative sensor sensitivity is 1.11%K-1, which is among the highest sensitivities recorded for upconversion-luminescence-based thermometers.

Fe K-Edge X-ray absorption near-edge spectroscopy (XANES) and X-ray diffraction (XRD) analyses of LiFePO4 and its base materials

NASA Astrophysics Data System (ADS)

Latif, C.; Negara, V. S. I.; Wongtepa, W.; Thamatkeng, P.; Zainuri, M.; Pratapa, S.

2018-03-01

XANES analysis has been performed with the aim of knowing the Fe oxidation state in a synthesized LiFePO4 and its base materials. XANES measurements were performed at SLRI on energy around Fe K-edge. An XRD analysis has also been performed with the aim of knowing the phase composition, lattice parameters and crystallite size of the LiFePO4 as well as the base materials. From the XRD analysis, it was found that the dominating phase in the iron sand sample was Fe3O4 and the only phase found after calcination was LiFePO4. The latter phase exhibited crystallite size of 100 nm and lattice parameters a = 10.169916 Å, b = 5.919674 Å, c = 4.627893 Å. Qualitative analysis of XANES data revealed that the oxidation number of Fe in the sample before calcination was greater than that after calcination and Fe in the natural iron sand, indicated by the E0 values of 7129.2 eV, 7120.6 eV and 7124.4 eV respectively.

Stability of Catalyzed Magnesium Hydride Nanocrystalline During Hydrogen Cycling. Part II: Microstructure Evolution

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

Zhou, Chengshang; Fang, Zhigang Zak; Bowman, Robert C.

2015-10-01

In Part I, the cyclic stabilities of the kinetics of catalyzed MgH2 systems including MgH2–TiH2, MgH2–TiMn2, and MgH2–VTiCr were investigated, showing stable kinetics at 300 °C but deteriorations of the hydrogenation kinetics at temperatures below 150 °C. The present Part II describes the characterization of uncycled and cycled catalyzed MgH2 by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and X-ray photoelectron spectroscopy (XPS) analysis. XRD analysis shows the crystallite sizes of the Mg and MgH2 significantly increased after the cycling. The mean crystallite sizes of the catalysts (TiH2 and VTiCr) increased moderately after the cycling. SEMmore » and TEM imaging were used to compare the microstructures of uncycled (as-milled) and cycled materials, revealing a drastic change of the microstructure after 100 cycles. In particular, results from energy-dispersive spectroscopy (EDS) mapping show that a change of distribution of the catalyst particles in the Mg and MgH2 phase occurred during the cycling.« less

High capacity Li-ion battery anodes: Impact of crystallite size, surface chemistry and PEG-coating

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

Minnici, Krysten; Kwon, Yo Han; Huie, Matthew M.

Battery electrodes are complex mesoscale systems comprised of an active material, conductive agent, current collector, and polymeric binder. Previous work showed that introduction of poly [3-(potassium-4-butanoate) thiophene] (PPBT) as a binder component coupled with a polyethylene glycol (PEG) surface coating on magnetite (Fe 3O 4) nanoparticles enhanced electron and ion transport in the high capacity anode system. Here, the impact of Fe 3O 4 crystallite size (10 nm vs. 20 nm) and surface chemistry were explored to evaluate their effects on interfacial interactions within the composite PEG/PPBT based electrodes and resultant battery performance. The Fe 3O 4 synthesis methods inevitablymore » lead to differences in surface chemistry. For instance, the Fe 3O 4 particles synthesized using ammonium hydroxide appeared more dispersed, and afforded improved rate capability performance. Notably, chemical interactions between the active nanoparticles and PPBT binder were only seen with particles synthesized using triethylamine. Capacity retention and cycling performance were unaffected. Thus, this study provides fundamental insights into the significant impact of active material synthesis on the design and fabrication of composite battery electrodes.« less

Multifunctional Eu3+- and Er3+/Yb3+-doped GdVO4 nanoparticles synthesized by reverse micelle method.

PubMed

Gavrilović, Tamara V; Jovanović, Dragana J; Lojpur, Vesna; Dramićanin, Miroslav D

2014-02-27

Synthesis of Eu(3+)- and Er(3+)/Yb(3+)-doped GdVO4 nanoparticles in reverse micelles and their multifunctional luminescence properties are presented. Using cyclohexane, Triton X-100, and n-pentanol as the oil, surfactant, and co-surfactant, respectively, crystalline nanoparticles with ~4 nm diameter are prepared at low temperatures. The particle size assessed using transmission electron microscopy is similar to the crystallite size obtained from X-ray diffraction measurements, suggesting that each particle comprises a single crystallite. Eu(3+)-doped GdVO4 nanoparticles emit red light through downconversion upon UV excitation. Er(3+)/Yb(3+)-doped GdVO4 nanoparticles exhibit several functions; apart from the downconversion of UV radiation into visible green light, they act as upconvertors, transforming near-infrared excitation (980 nm) into visible green light. The ratio of green emissions from (2)H11/2 → (2)I15/2 and (4)S3/2 → (4)I15/2 transitions is temperature dependent and can be used for nanoscale temperature sensing with near-infrared excitation. The relative sensor sensitivity is 1.11%K(-1), which is among the highest sensitivities recorded for upconversion-luminescence-based thermometers.

Investigation on the structural, magnetic and magnetocaloric properties of nanocrystalline Pr-deficient Pr1-xSrxMnO3-δ manganites

NASA Astrophysics Data System (ADS)

Arun, B.; Athira, M.; Akshay, V. R.; Sudakshina, B.; Mutta, Geeta R.; Vasundhara, M.

2018-02-01

We have investigated the structural, magnetic and magnetocaloric properties of nanocrystalline Pr-deficient Pr1-xSrxMnO3-δ Perovskite manganites. Rietveld refinement of the X-ray powder diffraction patterns confirms that all the studied compounds have crystallized into an orthorhombic structure with Pbnm space group. Transmission electron microscopy analysis reveals nanocrystalline compounds with crystallite size less than 50 nm. The selected area electron diffraction patterns reveal the highly crystalline nature of the compounds and energy dispersive X-ray spectroscopic analysis shows that the obtained compositions are nearly identical with the nominal one. The oxygen stoichiometry is estimated by iodometric titration method and stoichiometric compositions are confirmed by X-ray Fluorescence Spectrometry analysis. A large bifurcation is observed in the ZFC/FC curves and Arrott plots not show a linear relation but have a convex curvature nature. The temperature dependence of inverse magnetic susceptibility at higher temperature confirms the existence of ferromagnetic clusters. The experimental results reveal that the reduction of crystallite size to nano metric scale in Pr-deficient manganites adversely influences structural, magnetic and magnetocaloric properties as compared to its bulk counterparts reported earlier.

Thermal stability and chemical resistance of (Ti,Al)N-Cu and (Ti,Al)N-Ni metal-ceramic nanostructured coatings

NASA Astrophysics Data System (ADS)

Belov, D. S.; Blinkov, I. V.; Volkhonskii, A. O.; Kuznetsov, D. V.; Kiryukhantsev-Korneev, F. V.; Pustov, Yu. A.; Sergevnin, V. S.

2016-12-01

This work represents the results of research on thermal stability, oxidation resistance at temperatures of up to 800 °C and electrochemical behaviour of (Ti,Al)N-(∼3 at.%)Cu and (Ti,Al)N-(∼8 at.%)Ni nanocrystalline coatings in acidic and alkaline media. The coatings were deposited by the arc-PVD method with a thickness of approximately 4 μm and crystallite size of less than 20 nm. It has been demonstrated that the composition and properties of the coating structures do not change when the coatings are heated in 10-4 Pa vacuum at temperatures of 600, 700 °C for 1.5 h. Heating up to 800 °C caused an increase of crystallite size and reduction microstrain in the crystal lattice of the ceramic phase. The process is accompanied by deterioration of the coating hardness from 48 to 52 to 33-36 GPa. The (Ti,Al)N-Cu and (Ti,Al)N-Ni metal-ceramic nanostructured coatings are characterized by heat resistance up to the temperatures of 700 and 800 °C respectively. The coatings under study have tendency for self-passivation and resistance to pitting corrosion.

Liquefied petroleum gas sensor based on manganese (III) oxide and zinc manganese (III) oxide nanoparticles

NASA Astrophysics Data System (ADS)

Sharma, Shiva; Chauhan, Pratima; Husain, Shahid

2018-01-01

In this paper, {{{Mn}}}2{{{O}}}3 and {{{ZnMn}}}2{{{O}}}4 nanoparticles (NPs) are successfully synthesized using chemical co-precipitation method at room temperature and further annealed at 450 °C. The structure, crystallite size, morphology, specific surface area (SSA) and band gap energy have been determined by x-ray diffraction, transmission electron microscopy, Brunauer-Emmett-Teller surface area analysis, scanning electron microscopy (SEM-EDS) and UV-visible spectrophotometer. The sensor films of the {{{Mn}}}2{{{O}}}3 NPs and {{{ZnMn}}}2{{{O}}}4 NPs have been fabricated onto glass substrate using spin coater system separately. These sensor films are investigated for different concentrations (200-1200 ppm) of liquefied petroleum gas (LPG) at different operating temperatures ranging from 100 °C to 400 °C. A comparative study of gas sensing properties shows that spinel {{{ZnMn}}}2{{{O}}}4 sensor film exhibit excellent response (≈ 80 % ) towards 1000 ppm LPG at 300 °C in comparison to {{{Mn}}}2{{{O}}}3 sensor films. The enhancement in the gas sensing characteristics of {{{ZnMn}}}2{{{O}}}4 sensor film is attributed to the reduced crystallite size, greater SSA, and modification in structure as well as morphology.

Modified Ni-Cu catalysts for ethanol steam reforming

NASA Astrophysics Data System (ADS)

Dan, M.; Mihet, M.; Almasan, V.; Borodi, G.; Katona, G.; Muresan, L.; Lazar, M. D.

2013-11-01

Three Ni-Cu catalysts, having different Cu content, supported on γ-alumina were synthesized by wet co-impregnation method, characterized and tested in the ethanol steam reforming (ESR) reaction. The catalysts were characterized for determination of: total surface area and porosity (N2 adsorption - desorption using BET and Dollimer Heal methods), Ni surface area (hydrogen chemisorption), crystallinity and Ni crystallites size (X-Ray Diffraction), type of catalytic active centers (Hydrogen Temperature Programmed Reduction). Total surface area and Ni crystallites size are not significantly influenced by the addition of Cu, while Ni surface area is drastically diminished by increasing of Cu concentration. Steam reforming experiments were performed at atmospheric pressure, temperature range 150-350°C, and ethanol - water molar ration of 1 at 30, using Ar as carrier gas. Ethanol conversion and hydrogen production increase by the addition of Cu. At 350°C there is a direct connection between hydrogen production and Cu concentration. Catalysts deactivation in 24h time on stream was studied by Transmission Electron Microscopy (TEM) and temperature-programmed reduction (TPR) on used catalysts. Coke deposition was observed at all studied temperatures; at 150°C amorphous carbon was evidenced, while at 350°C crystalline, filamentous carbon is formed.

50 CFR 648.147 - Black sea bass minimum fish sizes.

Code of Federal Regulations, 2014 CFR

2014-10-01

... 50 Wildlife and Fisheries 12 2014-10-01 2014-10-01 false Black sea bass minimum fish sizes. 648... Measures for the Black Sea Bass Fishery § 648.147 Black sea bass minimum fish sizes. (a) Moratorium (commercially) permitted vessels. The minimum size for black sea bass is 11 inches (27.94 cm) total length for...

50 CFR 648.147 - Black sea bass minimum fish sizes.

Code of Federal Regulations, 2012 CFR

2012-10-01

... 50 Wildlife and Fisheries 12 2012-10-01 2012-10-01 false Black sea bass minimum fish sizes. 648... Measures for the Black Sea Bass Fishery § 648.147 Black sea bass minimum fish sizes. (a) Moratorium (commercially) permitted vessels. The minimum size for black sea bass is 11 inches (27.94 cm) total length for...

50 CFR 648.147 - Black sea bass minimum fish sizes.

Code of Federal Regulations, 2013 CFR

2013-10-01

... 50 Wildlife and Fisheries 12 2013-10-01 2013-10-01 false Black sea bass minimum fish sizes. 648... Measures for the Black Sea Bass Fishery § 648.147 Black sea bass minimum fish sizes. (a) Moratorium (commercially) permitted vessels. The minimum size for black sea bass is 11 inches (27.94 cm) total length for...

50 CFR 648.124 - Minimum fish sizes.

Code of Federal Regulations, 2011 CFR

2011-10-01

... 50 Wildlife and Fisheries 10 2011-10-01 2011-10-01 false Minimum fish sizes. 648.124 Section 648... Scup Fishery § 648.124 Minimum fish sizes. Link to an amendment published at 76 FR 60633, Sept. 29... if a party boat. (c) The minimum size applies to whole fish or any part of a fish found in possession...

"PowerUp"!: A Tool for Calculating Minimum Detectable Effect Sizes and Minimum Required Sample Sizes for Experimental and Quasi-Experimental Design Studies

ERIC Educational Resources Information Center

Dong, Nianbo; Maynard, Rebecca

2013-01-01

This paper and the accompanying tool are intended to complement existing supports for conducting power analysis tools by offering a tool based on the framework of Minimum Detectable Effect Sizes (MDES) formulae that can be used in determining sample size requirements and in estimating minimum detectable effect sizes for a range of individual- and…

Surface morphology of vacuum-evaporated pentacene film on Si substrate studied by in situ grazing-incidence small-angle X-ray scattering: I. The initial stage of formation of pentacene film

NASA Astrophysics Data System (ADS)

Hirosawa, Ichiro; Watanabe, Takeshi; Koganezawa, Tomoyuki; Kikuchi, Mamoru; Yoshimoto, Noriyuki

2018-03-01

The progress of the surface morphology of a growing sub-monolayered pentacene film on a Si substrate was studied by in situ grazing-incidence small angle X-ray scattering (GISAXS). The observed GISAXS profiles did not show sizes of pentacene islands but mainly protuberances on the boundaries around pentacene film. Scattering of X-ray by residual pits in the pentacene film was also detected in the GISAXS profiles of an almost fully covered film. The average radius of pentacene protuberances increased from 13 to 24 nm as the coverage increased to 0.83 monolayer, and the most frequent radius was almost constant at approximately 9 nm. This result suggests that the population of larger protuberances increase with increasing lengths of boundaries of the pentacene film. It can also be considered that the detected protuberances were crystallites of pentacene, since the average size of protuberances was nearly equal to crystallite sizes of pentacene films. The almost constant characteristic distance of 610 nm and amplitudes of pair correlation functions at low coverages suggest that the growth of pentacene films obeyed the diffusion-limited aggregation (DLA) model, as previously reported. It is also considered that the sites of islands show a triangular distribution for small variations of estimated correlation distances.

The gas-sensing potential of nanocrystalline SnO2 produced by a mechanochemical milling via centrifugal action

NASA Astrophysics Data System (ADS)

Kersen, Ü.

In this work, the synthesis of undoped nanocrystalline tin dioxide powders and the subsequent preparation of SnO2 thick-films were studied. An initial mixture of SnCl2 and Ca(OH)2 was sealed in a vial for milling in an air atmosphere. Heat treatment of the milled powder resulted in the formation of tetragonal and orthorhombic SnO2 phases, which was confirmed by X-ray diffraction (XRD) analysis. It was found that crystallite size could be controlled by varying the milling time, the rotation speed and the temperature used for the heat treatment. Crystallite sizes in the range 20 to 30 nm (determined by XRD measurements) were obtained. The total pore volume was 0.22 ml/g for a measured particle size of 37 m2/g. No contamination of the powder during milling was found. The response of the prepared thick-films to H2S gas in the concentration range 0.5 to 10 ppm in air was investigated as a function of the preparation conditions. The advantage of mechanochemical synthesis of powder is its relative simplicity, low cost and possibility of obtaining isolated, unagglomerated nanosized grains. It is shown that chemical reactions, which usually occur in the vibratory mill to produce the SnO phase, can also be initiated during a short processing time in the centrifugal mill.

Ice Recrystallization in a Solution of a Cryoprotector and Its Inhibition by a Protein: Synchrotron X-Ray Diffraction Study.

PubMed

Zakharov, Boris; Fisyuk, Alexander; Fitch, Andy; Watier, Yves; Kostyuchenko, Anastasia; Varshney, Dushyant; Sztucki, Michael; Boldyreva, Elena; Shalaev, Evgenyi

2016-07-01

Ice formation and recrystallization is a key phenomenon in freezing and freeze-drying of pharmaceuticals and biopharmaceuticals. In this investigation, high-resolution synchrotron X-ray diffraction is used to quantify the extent of disorder of ice crystals in binary aqueous solutions of a cryoprotectant (sorbitol) and a protein, bovine serum albumin. Ice crystals in more dilute (10 wt%) solutions have lower level of microstrain and larger crystal domain size than these in more concentrated (40 wt%) solutions. Warming the sorbitol-water mixtures from 100 to 228 K resulted in partial ice melting, with simultaneous reduction in the microstrain and increase in crystallite size, that is, recrystallization. In contrast to sorbitol solutions, ice crystals in the BSA solutions preserved both the microstrain and smaller crystallite size on partial melting, demonstrating that BSA inhibits ice recrystallization. The results are consistent with BSA partitioning into quasi-liquid layer on ice crystals but not with a direct protein-ice interaction and protein sorption on ice surface. The study shows for the first time that a common (i.e., not-antifreeze) protein can have a major impact on ice recrystallization and also presents synchrotron X-ray diffraction as a unique tool for quantification of crystallinity and disorder in frozen aqueous systems. Copyright © 2016 American Pharmacists Association®. Published by Elsevier Inc. All rights reserved.

50 CFR 648.72 - Minimum surf clam size.

Code of Federal Regulations, 2010 CFR

2010-10-01

... Atlantic Surf Clam and Ocean Quahog Fisheries § 648.72 Minimum surf clam size. (a) Minimum length. The minimum length for surf clams is 4.75 inches (12.065 cm). (b) Determination of compliance. No more than 50... 50 Wildlife and Fisheries 8 2010-10-01 2010-10-01 false Minimum surf clam size. 648.72 Section 648...

Procedures for analysis of debris relative to Space Shuttle systems

NASA Technical Reports Server (NTRS)

Kim, Hae Soo; Cummings, Virginia J.

1993-01-01

Debris samples collected from various Space Shuttle systems have been submitted to the Microchemical Analysis Branch. This investigation was initiated to develop optimal techniques for the analysis of debris. Optical microscopy provides information about the morphology and size of crystallites, particle sizes, amorphous phases, glass phases, and poorly crystallized materials. Scanning electron microscopy with energy dispersive spectrometry is utilized for information on surface morphology and qualitative elemental content of debris. Analytical electron microscopy with wavelength dispersive spectrometry provides information on the quantitative elemental content of debris.

Structure of Cu/Ni Nanowires Obtained by Matrix Synthesis

NASA Astrophysics Data System (ADS)

Zhigalina, O. M.; Doludenko, I. M.; Khmelenin, D. N.; Zagorskiy, D. L.; Bedin, S. A.; Ivanov, I. M.

2018-05-01

The structure of layered Cu/Ni nanowires obtained by template synthesis in 100-nm channels of track membranes has been investigated by transmission and scanning electron microscopy. The phase composition and main structural features of individual nanowires are determined. It is shown that nanowires consist of alternating Ni ( Fm3m) and Cu ( Fm3m) layers with grains up to 100 nm in size. It is found that nanowires contain also copper oxide crystallites up to 20 nm in size. The elemental composition of individual layers and their mutual arrangement are determined.

Deposition rate and substrate temperature effects on the structure and properties of bulk-sputtered OFHC Cu and Cu-0.15Zr. [Oxygen-Free High-Conductivity

NASA Technical Reports Server (NTRS)

Hecht, R. J.; Mullaly, J. R.

1975-01-01

Bulk-sputtered OFHC Cu and Cu-0.15 Zr used as inner walls of advanced regeneratively cooled thrust chambers are evaluated as to microstructure, surface topography, and fractography. It is found that under conditions of low substrate temperature, crystallite size and openness of the structure increase with increasing deposition rate for both materials. At elevated temperatures, an equiaxed ductile structure of OFHC Cu is produced only at low deposition rates; at higher deposition rate, open structures are observed with recrystallized equiaxed grains within large poorly bonded crystallites. The Cu-0.15 Zr alloy sputtered from the hollow cathode using a diode discharge shows open-type structures for all conditions evaluated. The use of a triode discharge in generating a dense non-voided structure of Cu-0.15 Zr is discussed.

Nanoscale phase transition behavior of shape memory alloys — closed form solution of 1D effective modelling

NASA Astrophysics Data System (ADS)

Li, M. P.; Sun, Q. P.

2018-01-01

We investigate the roles of grain size (lg) and grain boundary thickness (lb) on the stress-induced phase transition (PT) behaviors of nanocrystalline shape memory alloys (SMAs) by using a Core-shell type "crystallite-amorphous composite" model. A non-dimensionalized length scale lbarg(=lg /lb) is identified as the governing parameter which is indicative of the energy competition between the crystallite and the grain boundary. Closed form analytical solutions of a reduced effective 1D model with embedded microstructure length scales of lg and lb are presented in this paper. It is shown that, with lbarg reduction, the energy of the elastic non-transformable grain boundary will gradually become dominant in the phase transition process, and eventually bring fundamental changes of the deformation behaviors: breakdown of two-phase coexistence and vanishing of superelastic hysteresis. The predictions are supported by experimental data of nanocrystalline NiTi SMAs.

The influence of oxidation time on the properties of oxidized zinc films

NASA Astrophysics Data System (ADS)

Rambu, A. P.

2012-09-01

The effect of oxidation time on the structural characteristics and electronic transport mechanism of zinc oxide thin films prepared by thermal oxidation, have been investigated. Zinc metallic films were deposited by thermal evaporation under vacuum, the subsequent oxidation of Zn films being carried out in open atmosphere. XRD and AFM analysis indicate that obtained films posses a polycrystalline structure, the crystallites having a preferential orientation. Structural analysis reveals that microstructure of the films (crystallite size, surface roughness, internal stress) is depending on the oxidation time of metallic films. The electrical behavior of ZnO films was investigated, during a heat treatment (two heating/cooling cycles). It was observed that after the first heating, the temperature dependences of electrical conductivity become reversible. Mott variable range hopping model was proposed to analyze the temperature dependence of the electrical conductivity, in low temperature ranges. Values of some characteristic parameters were calculated.

Annealing induced reorientation of crystallites in Sn doped ZnO films

NASA Astrophysics Data System (ADS)

Ravichandran, K.; Vasanthi, M.; Thirumurugan, K.; Sakthivel, B.; Karthika, K.

2014-11-01

Tin doped ZnO thin films were prepared by employing a simplified spray pyrolysis technique using a perfume atomizer and subsequently annealed under different temperatures from 350 °C to 500 °C in steps of 50 °C. The structural, optical, electrical, photoluminescence and surface morphological properties of the as-deposited films were studied and compared with that of the annealed films. The X-ray diffraction studies showed that as-deposited film exhibits preferential orientation along the (0 0 2) plane and it changes in favour of (1 0 0) plane after annealing. The increase in crystallite size due to annealing is explained on the basis of Ostwald ripening effect. It is found that the optical transmittance and band gap increases with increase in annealing temperature. A slight decrease in resistivity caused by annealing is discussed in correlation with annealing induced defect modifications and surface morphology.

48 CFR 52.247-61 - F.o.b. Origin-Minimum Size of Shipments.

Code of Federal Regulations, 2010 CFR

2010-10-01

... 48 Federal Acquisition Regulations System 2 2010-10-01 2010-10-01 false F.o.b. Origin-Minimum Size... Clauses 52.247-61 F.o.b. Origin—Minimum Size of Shipments. As prescribed in 47.305-16(c), insert the following clause in solicitations and contracts when volume rates may apply: F.o.b. Origin—Minimum Size of...

Fabrication of Nd3+ and Mn2+ ions Co-doped Spinal Strontium Nanoferrites for High Frequency Device Applications

NASA Astrophysics Data System (ADS)

Ahmad, Iqbal; Shah, Syed Mujtaba; Ashiq, Muhammad Naeem; Nawaz, Faisal; Shah, Afzal; Siddiq, Muhammad; Fahim, Iqra; Khan, Samiullah

2016-10-01

Microemulsion method has been used for the synthesis of high resistive spinal nanoferrites with nominal composition Sr1- x Nd x Fe2- y Mn y O4 (0.0 ≤ x ≤ 0.1, 0.0 ≤ y ≤ 1.0) for high frequency device applications. It has been confirmed by x-ray diffraction (XRD) results that these ferrites have a cubic spinal structure with a mean crystallite size ranging from 34 mm to 47 nm. The co-substitution of Nd3+ and Mn2+ ions was performed, and its effect on electrical, dielectric and impedance properties was analyzed employing direct current (DC) resistivity measurements, dielectric measurements and electrochemical impedance spectroscopy (EIS). The DC resistivity ( ρ) value was the highest for the composition Sr0.90Nd0.1FeMnO4, but for the same composition, dielectric parameters and alternating current (AC) conductivity showed their minimum values. In the lower frequency range, the magnitudes of dielectric parameters decrease with increasing frequency and show an almost independent frequency response at higher frequencies. Dielectric polarization has been employed to explain these results. It was inferred from the results of EIS that the conduction process in the studied ferrite materials is predominantly governed by grain boundary volume.

Synthesis, photoelectrochemical properties and solar light-induced photocatalytic activity of bismuth ferrite nanoparticles

NASA Astrophysics Data System (ADS)

Pattnaik, Sambhu Prasad; Behera, Arjun; Martha, Satyabadi; Acharya, Rashmi; Parida, Kulamani

2018-01-01

Bismuth ferrite (BFO) nanoparticles prepared by solid state reaction route were characterized by various characterization techniques such as XRD, FESEM, HRTEM, UV-Vis DRS, PL etc., and their photocatalytic activities were evaluated by decolorization of aqueous solution of Congo red (CR) under solar light. The photocatalytic activity of BFO was increased by increasing the preparation temperature from 350 to 500 °C and then decreased with rise in temperature. The results of electrochemical measurements such as linear sweep voltammetry (LSV), electrochemical impedence (EIS), and Mott-Schottky analysis of BFO nanoparticles corroborated the findings of their photocatalytic activity. The enhanced photocatalytic response of the sample prepared at 500 °C is attributed to its smallest band gap, minimum crystallite size (30 nm), efficient separation, and lowest possible recombination of photo-generated charge carriers. The effects of amount of nano-BFO, irradiation time, initial CR concentration, and BFO calcination temperature on the decolorization of CR were examined. It was observed that 1 g/L nano-BFO calcined at 500 °C can decolorize up to 77% a 10-ppm CR dye solution under solar irradiation for 60 min. The studies included scavenger tests for identification of reactive species and a possible mechanism of dye decolorization.

Ultrasonically-induced electrical potentials in demineralized bovine cortical bone

NASA Astrophysics Data System (ADS)

Mori, Shunki; Makino, Taiki; Koyama, Daisuke; Takayanagi, Shinji; Yanagitani, Takahiko; Matsukawa, Mami

2018-04-01

While the low-intensity pulsed ultrasound technique has proved useful for healing of bone fractures, the ultrasound healing mechanism is not yet understood. To understand the initial physical effects of the ultrasound irradiation process on bone, we have studied the anisotropic piezoelectric properties of bone in the MHz range. Bone is known to be composed of collagen and hydroxyapatite (HAp) and shows strong elastic anisotropy. In this study, the effects of HAp on the piezoelectricity were investigated experimentally. To remove the HAp crystallites from the bovine cortical bone, demineralization was performed using ethylene diamine tetra-acetic acid (EDTA) solutions. To investigate the piezoelectricity, we have fabricated ultrasound transducers using the cortical bone or demineralized cortical bone. The induced electrical potentials due to the piezoelectricity were observed as the output of these transducers under pulsed ultrasound irradiation in the MHz range. The cortical bone transducer (before mineralization) showed anisotropic piezoelectric behavior. When the ultrasound irradiation was applied normal to the transducer surface, the observed induced electrical potentials had minimum values. The potential increased under off-axis ultrasound irradiation with changes in polarization. In the demineralized bone transducer case, however, the anisotropic behavior was not observed in the induced electrical potentials. These results therefore indicate that the HAp crystallites affect the piezoelectric characteristics of bone.

Microstructural evolution of diamond growth during HFCVD

NASA Technical Reports Server (NTRS)

Singh, J.

1994-01-01

High resolution transmission electron microscopy (HRTEM) was used to study the nucleation and growth mechanism of diamond by hot filament chemical vapor deposition (HFCVD) process. A novel technique has shown a direct evidence for the formation of the diamond-like carbon layer 8-14 nm thick in which small diamond micro-crystallites were embedded. These diamond micro-crystallites were formed as a result of transformation of diamond-like carbon into diamond. The diamond micro-crystallites present in the amorphous diamond-like carbon layer provided nucleation sites for diamond growth. Large diamond crystallites were observed to grow from these micro-crystallites. The mechanism of diamond growth will be presented based on experimental findings.

The effects of the conditions of char formation on the physical properties of charred phenolic-nylon

NASA Technical Reports Server (NTRS)

Smyly, E. D.; Pears, C. D.

1972-01-01

A study was made of the effects of the conditions of char formation on the physical properties of charred phenolic nylon of 0.577 gm/cu cm density. It was found that the thermal conductivity and several of the monitors correlate well with degradation conditions. The monitors included electrical resistivity, sonic velocity, porosity, lattice spacing and crystallite size.

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

Structural, magnetic, and dielectric properties of multiferroic Co1-xMgxCr2O4 nanoparticles

NASA Astrophysics Data System (ADS)

Kamran, M.; Ullah, A.; Rahman, S.; Tahir, A.; Nadeem, K.; Anis ur Rehman, M.; Hussain, S.

2017-07-01

We examined the structural, magnetic, and dielectric properties of Co1-xMgxCr2O4 nanoparticles with composition x = 0, 0.2, 0.4, 0.5, 0.6, 0.8 and 1 in detail. X-ray diffraction (XRD) revealed normal spinel structure for all the samples. Rietveld refinement fitting results of the XRD showed no impurity phases which signifies the formation of single phase Co1-xMgxCr2O4 nanoparticles. The average crystallite size showed a peak behaviour with maxima at x = 0.6. Raman and Fourier transform infrared (FTIR) spectroscopy also confirmed the formation of single phase normal spinel for all the samples and exhibited dominant vibrational changes for x ≥ 0.6. For x = 0 (CoCr2O4), zero field cooled/field cooled (ZFC/FC) magnetization curves showed paramagnetic (PM) to ferrimagnetic (FiM) transition at Tc = 97 K and a conical spiral magnetic order at Ts = 30 K. The end members CoCr2O4 (x = 0) and MgCr2O4 (x = 1) are FiM and antiferromagnetic (AFM), respectively. Tc and Ts showed decreasing trend with increasing x, followed by an additional AFM transition at TN = 15 K for x = 0.6. The system finally stabilized and changed to highly frustrated AFM structure at x = 1 due to formation of pure MgCr2O4. High field FC curves (5T) depicted nearly no effect on spiral magnetic state, which is attributed to strong exchange B-B magnetic interactions at low temperatures. Dielectric parameters showed a non-monotonous behaviour with Mg concentration and were explained with the help of Maxwell-Wagner model and Koop's theory. Dielectric properties were improved for nanoparticles with x = 0.6 and is attributed to their larger average crystallite size. In summary, Mg doping has significantly affects the structural, magnetic, and dielectric properties of CoCr2O4 nanoparticles, which can be attributed to variations in local magnetic exchange interactions and variation in average crystallite size of these chromite nanoparticles.

50 CFR 648.93 - Monkfish minimum fish sizes.

Code of Federal Regulations, 2014 CFR

2014-10-01

... 50 Wildlife and Fisheries 12 2014-10-01 2014-10-01 false Monkfish minimum fish sizes. 648.93... Measures for the NE Multispecies and Monkfish Fisheries § 648.93 Monkfish minimum fish sizes. (a) General provisions. All monkfish caught by vessels issued a valid Federal monkfish permit must meet the minimum fish...

50 CFR 622.492 - Minimum size limit.

Code of Federal Regulations, 2013 CFR

2013-10-01

... ADMINISTRATION, DEPARTMENT OF COMMERCE FISHERIES OF THE CARIBBEAN, GULF OF MEXICO, AND SOUTH ATLANTIC Queen Conch Resources of Puerto Rico and the U.S. Virgin Islands § 622.492 Minimum size limit. (a) The minimum size...

50 CFR 622.492 - Minimum size limit.

Code of Federal Regulations, 2014 CFR

2014-10-01

... ADMINISTRATION, DEPARTMENT OF COMMERCE FISHERIES OF THE CARIBBEAN, GULF OF MEXICO, AND SOUTH ATLANTIC Queen Conch Resources of Puerto Rico and the U.S. Virgin Islands § 622.492 Minimum size limit. (a) The minimum size...

Characterizations of Ca- and Mg-incorporating micro/nano-structured surfaces on titanium fabricated by microarc oxidation and hydrothermal treatments

NASA Astrophysics Data System (ADS)

Ko, Sang-Hoon; Hwang, Moon-Jin; Moon, Won-Jin; Park, Yeong-Joon; Song, Ho-Jun

2015-12-01

The micro/nano-surface characteristics of magnesium- and calcium-incorporating titanium oxide layers fabricated on titanium metal using microarc oxidation (MAO) and hydrothermal (HT) treatments were investigated. Calcium acetate monohydrate (CA), magnesium acetate monohydrate (MA), and β-glycerophosphoric acid disodium salt pentahydrate were used as electrolytes for MAO treatment of titanium disks. CA/MA electrolyte concentrations (all in M) were 0.2/0.0 (CA20-MAO), 0.15/0.05 (CA15MA5-MAO), 0.1/0.1 (CA10MA10-MAO), 0.05/0.15 (CA5MA15-MAO), and 0.0/0.2 (MA20-MAO). MAO-HT groups were prepared by hydrothermal treatment of MAO groups. The porous surface morphology was consistent even after HT treatment. The incorporation of Mg ions in the oxide layer during MAO treatment was more favorable than incorporation of Ca ions. However, Mg ions were released more rapidly than Ca ions after HT treatment. The anatase TiO2 structure was dominant for all the groups and an increase in the rutile TiO2 structure was observed with an increase in MA concentration. Nano-sized crystallites were observed on the porous surface for all MAO-HT groups. Nano-needle-like crystallites were observed on the surface of CA20-MAO-HT. The crystallites exhibited shorter and thicker characteristics with an increase in Mg concentration.

Changes in the mechanism of heat transfer in passing from microparticles to nanoparticles

NASA Astrophysics Data System (ADS)

Shakhov, F. M.; Meilakhs, A. P.; Eidelman, E. D.

2016-03-01

On the basis of experimental data on thermal conduction and sound velocity in composites obtained by sintering detonation nanodiamonds with the crystallite size of 4-5 nm and diamond micropowders with a grain size of about 10 μm at a high pressure (5-7 GPa) and high temperature (1200-1800°C), mechanisms of heat transfer in such structures are suggested. These mechanisms are shown to be different in composites of micro- and nanoparticles. In composites of micrometer particles, the conventional macroscopic mechanism of phonon propagation is active. In composites with a grain size of a few nanometers, the main contribution comes from thermal resistance on grain boundaries.

Direct measurement of free-energy barrier to nucleation of crystallites in amorphous silicon thin films

NASA Technical Reports Server (NTRS)

Shi, Frank G.

1994-01-01

A method is introduced to measure the free-energy barrier W(sup *), the activation energy, and activation entropy to nucleation of crystallites in amorphous solids, independent of the energy barrier to growth. The method allows one to determine the temperature dependence of W(sup *), and the effect of the preparation conditions of the initial amorphous phase, the dopants, and the crystallization methds on W(sup *). The method is applied to determine the free-energy barrier to nucleation of crystallites in amorphous silicon (a-Si) thin films. For thermally induced nucleation in a-Si thin films with annealing temperatures in the range of from 824 to 983 K, the free-energy barrier W(sup *) to nucleation of silicon crystals is about 2.0 - 2.1 eV regardless of the preparation conditions of the films. The observation supports the idea that a-Si transforms into an intermediate amorphous state through the structural relaxation prior to the onset of nucleation of crystallites in a-Si. The observation also indicates that the activation entropy may be an insignificant part of the free-energy barrier for the nucleation of crystallites in a-Si. Compared with the free-energy barrier to nucleation of crystallites in undoped a-Si films, a significant reduction is observed in the free-energy barrier to nucleation in Cu-doped a-Si films. For a-Si under irradiation of Xe(2+) at 10(exp 5) eV, the free-energy barrier to ion-induced nucleation of crystallites is shown to be about half of the value associated with thermal-induced nucleation of crystallites in a-Si under the otherwise same conditions, which is much more significant than previously expected. The present method has a general kinetic basis; it thus should be equally applicable to nucleation of crystallites in any amorphous elemental semiconductors and semiconductor alloys, metallic and polymeric glasses, and to nucleation of crystallites in melts and solutions.

50 CFR 648.83 - Multispecies minimum fish sizes.

Code of Federal Regulations, 2012 CFR

2012-10-01

... vessels are subject to the following minimum fish sizes, determined by total length (TL): Minimum Fish Sizes (TL) for Commercial Vessels Species Size(inches) Cod 22 (55.9 cm) Haddock 18 (45.7 cm) Pollock 19 (48.3 cm) Witch flounder (gray sole) 14 (35.6 cm) Yellowtail flounder 13 (33.0 cm) American plaice...

50 CFR 648.83 - Multispecies minimum fish sizes.

Code of Federal Regulations, 2013 CFR

2013-10-01

... vessels are subject to the following minimum fish sizes, determined by total length (TL): Minimum Fish Sizes (TL) for Commercial Vessels Species Size(inches) Cod 19 (48.3 cm) Haddock 16 (40.6 cm) Pollock 19 (48.3 cm) Witch flounder (gray sole) 13 (33 cm) Yellowtail flounder 12 (30.5 cm) American plaice (dab...

50 CFR 648.83 - Multispecies minimum fish sizes.

Code of Federal Regulations, 2014 CFR

2014-10-01

... vessels are subject to the following minimum fish sizes, determined by total length (TL): Minimum Fish Sizes (TL) for Commercial Vessels Species Size(inches) Cod 19 (48.3 cm) Haddock 16 (40.6 cm) Pollock 19 (48.3 cm) Witch flounder (gray sole) 13 (33 cm) Yellowtail flounder 12 (30.5 cm) American plaice (dab...

50 CFR 648.83 - Multispecies minimum fish sizes.

Code of Federal Regulations, 2011 CFR

2011-10-01

... vessels are subject to the following minimum fish sizes, determined by total length (TL): Minimum Fish Sizes (TL) for Commercial Vessels Species Size(inches) Cod 22 (55.9 cm) Haddock 18 (45.7 cm) Pollock 19 (48.3 cm) Witch flounder (gray sole) 14 (35.6 cm) Yellowtail flounder 13 (33.0 cm) American plaice...

Investigation of photoluminescence and dielectric properties of pure and Fe doped nickel oxide nanoparticles

NASA Astrophysics Data System (ADS)

Gupta, Jhalak; Ahmad, Arham S.

2018-05-01

The nanocrystallites of pure and Fe doped Nickel Oxide (NiO) were synthesized by the cost effective co-precipitation method using nickel nitrate as the initial precursor. The synthesized nickel oxide nanoparticles were characterized by X-Ray Diffraction (XRD), Photoluminiscence Spectroscopy (PL), LCR meter. The crystallite size of synthesized pure Nickel Oxide nanoparticles obtained by XRD using Debye Scherer's formula was found to be 21.8nm and the size decreases on increasing the dopant concentration. The optical properties were analyzed by PL and dielectric ones by using LCR meter.

Use of scanning near-field optical microscope with an aperture probe for detection of luminescent nanodiamonds

NASA Astrophysics Data System (ADS)

Shershulin, V. A.; Samoylenko, S. R.; Shenderova, O. A.; Konov, V. I.; Vlasov, I. I.

2017-02-01

The suitability of scanning near-field optical microscopy (SNOM) to image photoluminescent diamond nanoparticles with nanoscale resolution is demonstrated. Isolated diamond nanocrystals with an average size of 100 nm, containing negatively charged nitrogen-vacancy (NV-) centers, were chosen as tested material. The NV- luminescence was stimulated by continuous 532 nm laser light. Sizes of analyzed crystallites were monitored by an atomic force microscope. The lateral resolution of the order of 100 nm was reached in SNOM imaging of diamond nanoparticles using 150 nm square aperture of the probe.

Freeze drying vs microwave drying-methods for synthesis of sinteractive thoria powders

NASA Astrophysics Data System (ADS)

Annie, D.; Chandramouli, V.; Anthonysamy, S.; Ghosh, Chanchal; Divakar, R.

2017-02-01

Thoria powders were synthesized by oxalate precipitation from an aqueous solution of the nitrate. The filtered precipitates were freeze dried or microwave dried before being calcined at 1073 K. The thoria powders obtained were characterized for crystallite size, specific surface area, bulk density, particle size distribution and residual carbon. Microstructure of the product was studied using scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Sinterability of the synthesized powders was studied by measuring the density of the sintered compacts. Powders that can be consolidated and sintered to densities ∼96% theoretical density (TD) at 1773 K were obtained.

Correlating sampling and intensity statistics in nanoparticle diffraction experiments

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

Öztürk, Hande; Yan, Hanfei; Hill, John P.

2015-07-28

It is shown in a previous article [Öztürk, Yan, Hill & Noyan (2014).J. Appl. Cryst.47, 1016–1025] that the sampling statistics of diffracting particle populations within a polycrystalline ensemble depended on the size of the constituent crystallites: broad X-ray peak breadths enabled some nano-sized particles to contribute more than one diffraction spot to Debye–Scherrer rings. Here it is shown that the equations proposed by Alexander, Klug & Kummer [J. Appl. Phys.(1948),19, 742–753] (AKK) to link diffracting particle and diffracted intensity statistics are not applicable if the constituent crystallites of the powder are below 10 nm. In this size range, (i) themore » one-to-one correspondence between diffracting particles and Laue spots assumed in the AKK analysis is not satisfied, and (ii) the crystallographic correlation between Laue spots originating from the same grain invalidates the assumption that all diffracting plane normals are randomly oriented and uncorrelated. Such correlation produces unexpected results in the selection of diffracting grains. For example, three or more Laue spots from a given grain for a particular reflection can only be observed at certain wavelengths. In addition, correcting the diffracted intensity values by the traditional Lorentz term, 1/cos θ, to compensate for the variation of particles sampled within a reflection band does not maintain fidelity to the number of poles contributing to the diffracted signal. A new term, cos θ B/cos θ, corrects this problem.« less

Characterization of N-doped polycrystalline diamond films deposited on microgrinding tools

NASA Astrophysics Data System (ADS)

Jackson, M. J.; Ahmed, W.

2005-10-01

Chemical vapor deposited diamond films have many industrial applications but are assuming increasing importance in the area of microengineering, most notably in the development of diamond coated microgrinding tools. For these applications the control of structure and morphology is of critical importance. The crystallite size, orientation, surface roughness, and the degree of sp 3 character have a profound effect on the tribological properties of the films deposited. In this article, we present experimental results on the effects of nitrogen doping on the surface morphology, crystallite size, and wear of microgrinding tools. The sp 3 character optimizes at 200 ppm nitrogen, and above this value the surface becomes much smoother and crystal sizes decrease considerably. Fracture-induced wear of the diamond grain is the most important mechanism of material removal from a microgrinding tool during the grinding process. Fracture occurs as a consequence of tensile stresses induced into diamond grains by grinding forces to which they are subjected. The relationship between the wear of diamond coated grinding tools, component grinding forces, and induced stresses in the model diamond grains is described in detail. A significant correlation was found between the maximum value of tensile stress induced in the diamond grain and the appropriate wheel-wear parameter (grinding ratio). It was concluded that the magnitude of tensile stresses induced in the diamond grain by grinding forces at the rake face is the best indicator of tool wear during the grinding process.

Preparation and Scintillating Properties of Sol-Gel Eu3+, Tb3+ Co-Doped Lu2O3 Nanopowders

PubMed Central

de Jesús Morales Ramírez, Ángel; Murillo, Antonieta García; de Jesús Carrillo Romo, Felipe; Hernández, Margarita García; Palmerin, Joel Moreno; Guerrero, Rosario Ruiz

2011-01-01

Nanocrystalline Eu3+, Tb3+ co-doped Lu2O3 powders with a maximum size of 25.5 nm were prepared by the sol-gel process, using lutetium, europium and terbium nitrates as precursors, and ethanol as a solvent. Differential thermal analysis (DTA) and infrared spectroscopy (IR) were used to study the chemical changes during the xerogel annealing. After the sol evaporation at 100 °C, the formed gel was annealed from 300 to 900 °C for 30 min under a rich O2 atmosphere, and the yielded product was analyzed by X-ray diffraction (XRD) to characterize the microstructural behavior and confirm the crystalline structure. The results showed that Lu2O3 nanopowders start to crystallize at 400 °C and that the crystallite size increases along with the annealing temperature. A transmission electron microscopy (TEM) study of samples annealed at 700 and 900 °C was carried out in order to analyze the microstructure, as well as the size, of crystallites. Finally, in regard to scintillating properties, Eu3+ dopant (5 mol%), Tb3+ codoped Lu2O3 exhibited a typical red emission at 611 nm (D°→7F2), furthermore, the effect of Tb3+ molar content (0.01, 0.015 and 0.02% mol) on the Eu3+ radioluminiscence was analyzed and it was found that the higher emission intensity corresponds to the lower Tb3+ content. PMID:22016655

Finely Tuned SnO2 Nanoparticles for Efficient Detection of Reducing and Oxidizing Gases: The Influence of Alkali Metal Cation on Gas-Sensing Properties.

PubMed

Lee, Szu-Hsuan; Galstyan, Vardan; Ponzoni, Andrea; Gonzalo-Juan, Isabel; Riedel, Ralf; Dourges, Marie-Anne; Nicolas, Yohann; Toupance, Thierry

2018-03-28

Tin dioxide (SnO 2 ) nanoparticles were straightforwardly synthesized using an easily scaled-up liquid route that involves the hydrothermal treatment, either under acidic or basic conditions, of a commercial tin dioxide particle suspension including potassium counterions. After further thermal post-treatment, the nanomaterials have been thoroughly characterized by Fourier transform infrared and Raman spectroscopy, powder X-ray diffraction, transmission electron microscopy, X-ray photoelectron spectroscopy, and nitrogen sorption porosimetry. Varying pH conditions and temperature of the thermal treatment provided cassiterite SnO 2 nanoparticles with crystallite sizes ranging from 7.3 to 9.7 nm and Brunauer-Emmett-Teller surface areas ranging from 61 to 106 m 2 ·g -1 , acidic conditions favoring potassium cation removal. Upon exposure to a reducing gas (H 2 , CO, and volatile organic compounds such as ethanol and acetone) or oxidizing gas (NO 2 ), layers of these SnO 2 nanoparticles led to highly sensitive, reversible, and reproducible responses. The sensing results were discussed in regard to the crystallite size, specific area, valence band energy, Debye length, and chemical composition. Results highlight the impact of the counterion residuals, which affect the gas-sensing performance to an extent much higher than that of size and surface area effects. Tin dioxide nanoparticles prepared under acidic conditions and calcined in air showed the best sensing performances because of lower amount of potassium cations and higher crystallinity, despite the lower surface area.

Optical, electrical and magnetic properties of nanostructured Mn3O4 synthesized through a facile chemical route

NASA Astrophysics Data System (ADS)

Bose, Vipin C.; Biju, V.

2015-02-01

Nanostructured Mn3O4 sample with an average crystallite size of ˜15 nm is synthesized via the reduction of potassium permanganate using hydrazine. The average particle size obtained from the Transmission Electron Microscopy analysis is in good agreement with the average crystallite size estimated from X-ray diffraction analysis. The presence of Mn4+ ions at the octahedral sites is inferred from the results of Raman, UV-visible absorption and X-ray photoelectron spectroscopy analyzes. DC electrical conductivity of the sample in the temperature range 313-423 K, is about five orders of magnitude larger than that reported for single crystalline Mn3O4 sample. The dominant conduction mechanism is identified to be of the polaronic hopping of holes between cations in the octahedral sites. The zero field cooled and field cooled magnetization of the sample is studied in the range 20-300 K. The Curie temperature for the sample is about 45 K, below which the sample is ferrimagnetic. A blocking temperature of 35 K is observed in the field cooled curve. It is observed that the sample shows hysteresis at temperatures below the Curie temperature with no saturation, even at an applied field (20 kOe). The presence of an ordered core and disordered surface of spin arrangements is observed from the magnetization studies. Above the Curie temperature, the sample shows linear dependence of magnetization on applied field with no hysteresis characteristic of paramagnetic phase.

Effect of milling atmosphere on structural and magnetic properties of Ni-Zn ferrite nanocrystalline

NASA Astrophysics Data System (ADS)

Hajalilou, Abdollah; Hashim, Mansor; Ebrahimi-Kahrizsangi, Reza; Masoudi Mohamad, Taghi

2015-04-01

Powder mixtures of Zn, NiO, and Fe2O3 are mechanically alloyed by high energy ball milling to produce Ni-Zn ferrite with a nominal composition of Ni0.36Zn0.64Fe2O4. The effects of milling atmospheres (argon, air, and oxygen), milling time (from 0 to 30 h) and heat treatment are studied. The products are characterized using x-ray diffractometry, field emission scanning electron microscopy equipped with energy-dispersive x-ray spectroscopy, and transmitted electron microscopy. The results indicate that the desired ferrite is not produced during the milling in the samples milled under either air or oxygen atmospheres. In those samples milled under argon, however, Zn/NiO/Fe2O3 reacts with a solid-state diffusion mode to produce Ni-Zn ferrite nanocrystalline in a size of 8 nm after 30-h-milling. The average crystallite sizes decrease to 9 nm and 10 nm in 30-h-milling samples under air and oxygen atmospheres, respectively. Annealing the 30-h-milling samples at 600 °C for 2 h leads to the formation of a single phase of Ni-Zn ferrite, an increase of crystallite size, and a reduction of internal lattice strain. Finally, the effects of the milling atmosphere and heating temperature on the magnetic properties of the 30-h-milling samples are investigated. Project supported by the University Putra Malaysia Graduate Research Fellowship Section.

Effect of titanium on the structural and optical property of NiO nano powders

NASA Astrophysics Data System (ADS)

Amin, Ruhul; Mishra, Prashant; Khatun, Nasima; Ayaz, Saniya; Srivastava, Tulika; Sen, Somaditya

2018-05-01

Nickel Oxide (NiO) and Ti doped NiO nanoparticles were prepared by sol-gel auto combustion method. Powder x-ray diffraction (PXRD) structural studies revealed face centered cubic (FCC) structure of the NiO nanopowders. The crystallite size decreased with Ti incorporation. UV-Vis spectroscopy carried out in diffused reflectance mode revealed decrease in band gap with increment in Urbach energy with doping.

Oligonucleotide flexibility dictates crystal quality in DNA-programmable nanoparticle superlattices.

PubMed

Senesi, Andrew J; Eichelsdoerfer, Daniel J; Brown, Keith A; Lee, Byeongdu; Auyeung, Evelyn; Choi, Chung Hang J; Macfarlane, Robert J; Young, Kaylie L; Mirkin, Chad A

2014-11-12

The evolution of crystallite size and microstrain in DNA-mediated nanoparticle superlattices is dictated by annealing temperature and the flexibility of the interparticle bonds. This work addresses a major challenge in synthesizing optical metamaterials based upon noble metal nanoparticles by enabling the crystallization of large nanoparticles (100 nm diameter) at high volume fractions (34% metal). © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Effects of Eu3+ concentration on structural, optical and vibrational properties of multifunctional Ce(1-x)Eu(x)O2-delta) nanoparticles synthesized by thermolysis of 2,4-pentanedione complexes.

PubMed

Kremenovic, A; Bozanic, D K; Welsch, A M; Jancar, B; Nikolic, A S; Boskovic, M; Colomban, Ph; Fabian, Martin; Antic, B

2012-12-01

The 5-10 nm Ce(1-x)Eu(x)O(2-delta) (0 < or = x < or = 0.30) nanoparticles with fluorite structure were synthesized by thermal decomposition of Eu- and Ce-2,4-pentanedione complexes mixtures. X-ray line broadening analysis of mixed samples Ce(1-x)Eu(x)O(2-delta) (0.05 < or = x < or = 0.30) showed that the crystallite size was lower and root mean square strain higher than in pure ceria. However, within mixed samples Ce(1-x)Eu(x)O(2-delta) (0.05 < or = x < or = 0.30) crystallite size and root mean square strain were independent of Eu3+ concentration. Raman spectroscopy results indicated that europium ions yield disorder by breaking the phonon propagation and therefore making the non-centre Brillouin zone modes Raman active. The absorption bands in the spectra of mixed oxides were blue-shifted in comparison to pure CeO(2-delta) nanopowder. The samples show red emission typical for Eu ions. The biggest photoluminescent intensity was observed for the highest Eu3+ concentration (x = 0.30) and further enhanced with the increase in crystallinity.

Spin reorientation transition and hard magnetic properties of MnBi intermetallic compound

NASA Astrophysics Data System (ADS)

Suzuki, K.; Wu, X.; Ly, V.; Shoji, T.; Kato, A.; Manabe, A.

2012-04-01

The effects of mechanical grinding (MG) on the crystallite size, the spin reorientation transition temperature (TSR) and the hard magnetic properties in melt-spun low temperature phase (LTP) MnBi have been investigated in order to understand the origin of magnetic hardening induced by MG. The room-temperature coercive field (μ0Hcj) is enhanced dramatically from 0.08 T before MG to 1.5 T after MG for 43.2 ks while TSR is concurrently suppressed from 110 to 38 K. The coercive force exhibits positive temperature dependence approximately 50-60 K above TSR and the lowered TSR after MG could result in magnetic hardening at room temperature. The room-temperature coercive force of LTP-MnBi is highly dependent on the crystallite size (D) and is found to be described phenomenologically by the following relationship: μ0Hcj = μ0Ha(δ/D)n, where μ0Ha is ˜ 4 T, the Bloch wall width δ is 7 nm, and the exponent n is approximately 0.7. Our results suggest that the grain refinement is the primary origin of the hardening effect induced by MG with a possible minor hardening effect due to the suppression of the spin reorientation transition temperature.

Low-Cost and Facile Synthesis of the Vanadium Oxides V2O3, VO2, and V2O5 and Their Magnetic, Thermochromic and Electrochromic Properties.

PubMed

Mjejri, Issam; Rougier, Aline; Gaudon, Manuel

2017-02-06

In this study, vanadium sesquioxide (V 2 O 3 ), dioxide (VO 2 ), and pentoxide (V 2 O 5 ) were all synthesized from a single polyol route through the precipitation of an intermediate precursor: vanadium ethylene glycolate (VEG). Various annealing treatments of the VEG precursor, under controlled atmosphere and temperature, led to the successful synthesis of the three pure oxides, with sub-micrometer crystallite size. To the best of our knowledge, the synthesis of the three oxides V 2 O 5 , VO 2 , and V 2 O 3 from a single polyol batch has never been reported in the literature. In a second part of the study, the potentialities brought about by the successful preparation of sub-micrometer V 2 O 5 , VO 2 , and V 2 O 3 are illustrated by the characterization of the electrochromic properties of V 2 O 5 films, a discussion about the metal to insulator transition of VO 2 on the basis of in situ measurements versus temperature of its electrical and optical properties, and the characterization of the magnetic transition of V 2 O 3 powder from SQUID measurements. For the latter compound, the influence of the crystallite size on the magnetic properties is discussed.

X-ray diffraction and SEM study of kidney stones in Israel: quantitative analysis, crystallite size determination, and statistical characterization.

PubMed

Uvarov, Vladimir; Popov, Inna; Shapur, Nandakishore; Abdin, Tamer; Gofrit, Ofer N; Pode, Dov; Duvdevani, Mordechai

2011-12-01

Urinary calculi have been recognized as one of the most painful medical disorders. Tenable knowledge of the phase composition of the stones is very important to elucidate an underlying etiology of the stone disease. We report here the results of quantitative X-ray diffraction phase analysis performed on 278 kidney stones from the 275 patients treated at the Department of Urology of Hadassah Hebrew University Hospital (Jerusalem, Israel). Quantification of biominerals in multicomponent samples was performed using the normalized reference intensity ratio method. According to the observed phase compositions, all the tested stones were classified into five chemical groups: oxalates (43.2%), phosphates (7.7%), urates (10.3%), cystines (2.9%), and stones composed of a mixture of different minerals (35.9%). A detailed analysis of each allocated chemical group is presented along with the crystallite size calculations for all the observed crystalline phases. The obtained results have been compared with the published data originated from different geographical regions. Morphology and spatial distribution of the phases identified in the kidney stones were studied with scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDS). This type of detailed study of phase composition and structural characteristics of the kidney stones was performed in Israel for the first time.

Highly active lanthanum doped ZnO nanorods for photodegradation of metasystox.

PubMed

Korake, P V; Dhabbe, R S; Kadam, A N; Gaikwad, Y B; Garadkar, K M

2014-01-05

La-doped ZnO nanorods with different La contents were synthesized by microwave assisted method and characterized by various sophisticated techniques such as XRD, UV-Vis., EDS, XPS, SEM and TEM. The XRD patterns of the La-doped ZnO indicate hexagonal crystal structure with an average crystallite size of 30nm. It was found that the crystallite size of La-doped ZnO is much smaller as compared to pure ZnO and decreases with increasing La content. The photocatalytic activity of 0.5mol% La-doped ZnO in the degradation of metasystox was studied. It was observed that degradation efficiency of metasystox over La-doped ZnO increases up to 0.5mol% doping then decreases for higher doping levels. Among the catalyst studied, the 0.5mol% La-doped ZnO was the most active, showing high photocatalytic activity for the degradation of metasystox. The maximum reduction of concentration of metasystox was observed under static condition at pH 8. Reduction in the Chemical Oxygen Demand (COD) of metasystox was observed after 150min. The cytotoxicological studies of meristematic root tip cells of Allium cepa were studied. The results obtained indicate that photocatalytically degraded products of metasystox were less toxic as compared to metasystox. Copyright © 2013 Elsevier B.V. All rights reserved.

Solid State Reduction of MoO3 with Carbon via Mechanical Alloying to Synthesize Nano-Crystaline MoO2

NASA Astrophysics Data System (ADS)

Saghafi, M.; Ataie, A.; Heshmati-Manesh, S.

In this research, effect of milling time on solid state reduction of MoO3 with carbon has been investigated. It was found that mechanical activation of a mixture of MoO3 and carbon at ambient temperature by high energy ball milling was not able to reduce MoO3 to metallic molybdenum. MoO3 was converted to MoO2 at the first stage of reduction and peaks of the latter phase in X-ray diffraction patterns were detected when the milling time exceeded from 50 hours. The main effect of increased milling time at this stage was decreasing of MoO3 peak intensities and significant peak broadening due to decrease in size of crystallites. After prolonged milling, MoO3 was fully reduced to nano-crystalline MoO2 and its mean crystallite size was calculated using Williamson-Hall technique and found to be 17.5 nm. Thermodynamic investigations also confirm the possibility of reduction of MoO3 to MoO2 during the milling operation at room temperature. But, further reduction to metallic molybdenum requires thermal activation at higher temperature near 1100 K. XRD and SEM techniques were employed to evaluate the powder particles characteristics.

One-step rapid synthesis of ultrafine γ-Ga2O3 nanocrystals by microwave hydrothermal method in ammonium hydroxide medium

NASA Astrophysics Data System (ADS)

Cui, Lu; Wang, Hong; Xin, Baifu; Mao, Guijie

2017-10-01

Ultrafine nanocrystals of γ-gallium oxide (γ-Ga2O3) were rapidly synthesized via microwave hydrothermal method at 140 °C, in which Ga(NO3)3 was used as the gallium source and urea was the precipitant. The samples were characterized by X-ray diffraction (XRD), ultraviolet-visible absorption spectroscopy (UV-Vis), transmission electron microscopy (TEM), nitrogen physisorption and photoluminescence spectroscopy (PL). The crystallite size of ultrafine spinel γ-Ga2O3 was in the range from 4 to 5 nm and the optical bandgap was 4.61 eV. To improve the crystallinity, the ultrafine γ-Ga2O3 nanocrystals were calcined at 300-700 °C further. The ultrafine γ-Ga2O3 calcined at 500 °C (calcined-γ-Ga2O3) still remained the metastable γ-phase with relatively high crystallinity and the crystallite size around 5-7 nm. Photocatalytic performances of the synthesized samples were also evaluated by the degradation of rhodamine B (RhB). Results revealed that the ultrafine γ-Ga2O3 and the calcined-γ-Ga2O3 samples exhibited high photocatalytic efficiencies of 68.2 and 90.7%, respectively.

Biosynthesis of extracellular and intracellular gold nanoparticles by Aspergillus fumigatus and A. flavus.

PubMed

Gupta, Saurabh; Bector, Shruti

2013-05-01

Green chemistry is a boon for the development of safe, stable and ecofriendly nanostructures using biological tools. The present study was carried out to explore the potential of selected fungal strains for biosynthesis of intra- and extracellular gold nanostructures. Out of the seven cultures, two fungal strains (SBS-3 and SBS-7) were selected on the basis of development of dark pink colour in cell free supernatant and fungal beads, respectively indicative of extra- and intracellular gold nanoparticles production. Both biomass associated and cell free gold nanoparticles were characterized using X-ray diffractogram (XRD) analysis and transmission electron microscopy (TEM). XRD analysis confirmed crystalline, face-centered cubic lattice of metallic gold nanoparticles along with average crystallite size. A marginal difference in average crystallite size of extracellular (17.76 nm) and intracellular (26 and 22 nm) Au-nanostructures was observed using Scherrer equation. In TEM, a variety of shapes (triangles, spherical, hexagonal) were observed in both extra- and intracellular nanoparticles. 18S rRNA gene sequence analysis by multiple sequence alignment (BLAST) indicated 99 % homology of SBS-3 to Aspergillus fumigatus with 99 % alignment coverage and 98 % homology of SBS-7 to Aspergillus flavus with 98 % alignment coverage respectively. Native-PAGE and activity staining further confirmed enzyme linked synthesis of gold nanoparticles.

Effect of reaction atmosphere on structural and optical properties of hexagonal molybdenum oxide (h-MoO{sub 3})

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

Doss, V. Arumai; Chithambararaj, A.; Bose, A. Chandra, E-mail: acbose@nitt.edu

2016-05-23

The present work aims to synthesize single phase h-MoO{sub 3} nanocrytals by chemical precipitation method exposed under different reaction atmospheres. The reaction atmosphere have been successfully tuned as air, nitrogen and argon and studied its effects on structural, functional, morphology and optical properties by using X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transform infrared (FT-IR) spectroscopy and diffuse reflectance spectroscopy (DRS) measurements. The XRD result indicates that the sample exhibits characteristic hexagonal phase of MoO{sub 3}. The crystallite size is estimated by well known Scherrer’s method. The crystallite size is relative small in the case of sample prepared atmore » argon atmosphere. The functional groups such as Mo-O, N-H and O-H are identified from FT-IR spectroscopy. The particle exhibits rod like morphology with perfect hexagonal cross-section. The optical absorption observed at 420-450 nm corresponds to fundamental optical absorption by h-MoO{sub 3}. The band gap values are estimated using Kublka-Munk (K-M) function and found to be 2. 87 eV, 2.93 eV and 2.97 eV for samples synthesized under air, nitrogen and argon, respectively.« less

Structure investigations of ferromagnetic Co-Ni-Al alloys obtained by powder metallurgy.

PubMed

Maziarz, W; Dutkiewicz, J; Lityńska-Dobrzyńska, L; Santamarta, R; Cesari, E

2010-03-01

Elemental powders of Co, Ni and Al in the proper amounts to obtain Co(35)Ni(40)Al(25) and Co(40)Ni(35)Al(25) nominal compositions were ball milled in a high-energy mill for 80 h. After 40 h of milling, the formation of a Co (Ni, Al) solid solution with f.c.c. structure was verified by a change of the original lattice parameter and crystallite size. Analytical transmission electron microscopy observations and X-ray diffraction measurements of the final Co (Ni, Al) solid solution showed that the crystallite size scattered from 4 to 8 nm and lattice parameter a = 0.36086 nm. The chemical EDS point analysis of the milled powder particles allowed the calculation of the e/a ratio and revealed a high degree of chemical homogeneity of the powders. Hot pressing in vacuum of the milled powders resulted in obtaining compacts with a density of about 70% of the theoretical one. An additional heat treatment increased the density and induced the martensitic transformation in a parent phase. Selected area diffraction patterns and dark field images obtained from the heat-treated sample revealed small grains around 300 nm in diameter consisting mainly of the ordered gamma phase (gamma'), often appearing as twins, and a small amount of the L1(0) ordered martensite.

Report on the Synchrotron Characterization of U-Mo and U-Zr Alloys and the Modeling Results

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

Okuniewski, Maria A.; Ganapathy, Varsha; Hamilton, Brenden

2016-09-01

ABSTRACT Uranium-molybdenum (U-Mo) and uranium-zirconium (U-Zr) are two promising fuel candidates for nuclear transmutation reactors which burn long-lived minor actinides and fission products within fast spectrum reactors. The objectives of this research are centered on understanding the early stages of fuel performance through the examination of the irradiation induced microstructural changes in U-Zr and U-Mo alloys subjected to low neutron fluences. Specimens that were analyzed include those that were previously irradiated in the Advanced Test Reactor at INL. This most recent work has focused on a sub-set of the irradiated specimens, specifically U-Zr and U-Mo alloys that were irradiated tomore » 0.01 dpa at temperatures ranging from (150-800oC). These specimens were analyzed with two types of synchrotron techniques, including X-ray absorption fine structure and X-ray diffraction. These techniques provide non-destructive microstructural analysis, including phase identification and quantitation, lattice parameters, crystallite sizes, as well as bonding, structure, and chemistry. Preliminary research has shown changes in the phase fractions, crystallite sizes, and lattice parameters as a function of irradiation and temperature. Future data analyses will continue to explore these microstructural changes.« less

Determining size and dispersion of minimum viable populations for land management planning and species conservation

NASA Astrophysics Data System (ADS)

Lehmkuhl, John F.

1984-03-01

The concept of minimum populations of wildlife and plants has only recently been discussed in the literature. Population genetics has emerged as a basic underlying criterion for determining minimum population size. This paper presents a genetic framework and procedure for determining minimum viable population size and dispersion strategies in the context of multiple-use land management planning. A procedure is presented for determining minimum population size based on maintenance of genetic heterozygosity and reduction of inbreeding. A minimum effective population size ( N e ) of 50 breeding animals is taken from the literature as the minimum shortterm size to keep inbreeding below 1% per generation. Steps in the procedure adjust N e to account for variance in progeny number, unequal sex ratios, overlapping generations, population fluctuations, and period of habitat/population constraint. The result is an approximate census number that falls within a range of effective population size of 50 500 individuals. This population range defines the time range of short- to long-term population fitness and evolutionary potential. The length of the term is a relative function of the species generation time. Two population dispersion strategies are proposed: core population and dispersed population.

50 CFR 648.233 - Minimum Fish Sizes. [Reserved

Code of Federal Regulations, 2010 CFR

2010-10-01

... 50 Wildlife and Fisheries 8 2010-10-01 2010-10-01 false Minimum Fish Sizes. [Reserved] 648.233 Section 648.233 Wildlife and Fisheries FISHERY CONSERVATION AND MANAGEMENT, NATIONAL OCEANIC AND... Measures for the Spiny Dogfish Fishery § 648.233 Minimum Fish Sizes. [Reserved] ...

Phosphate-enhanced cytotoxicity of zinc oxide nanoparticles and agglomerates.

PubMed

Everett, W Neil; Chern, Christina; Sun, Dazhi; McMahon, Rebecca E; Zhang, Xi; Chen, Wei-Jung A; Hahn, Mariah S; Sue, H-J

2014-02-10

Zinc oxide (ZnO) nanoparticles (NPs) have been found to readily react with phosphate ions to form zinc phosphate (Zn3(PO4)2) crystallites. Because phosphates are ubiquitous in physiological fluids as well as waste water streams, it is important to examine the potential effects that the formation of Zn3(PO4)2 crystallites may have on cell viability. Thus, the cytotoxic response of NIH/3T3 fibroblast cells was assessed following 24h of exposure to ZnO NPs suspended in media with and without the standard phosphate salt supplement. Both particle dosage and size have been shown to impact the cytotoxic effects of ZnO NPs, so doses ranging from 5 to 50 μg/mL were examined and agglomerate size effects were investigated by using the bioinert amphiphilic polymer polyvinylpyrrolidone (PVP) to generate water-soluble ZnO ranging from individually dispersed 4 nm NPs up to micron-sized agglomerates. Cell metabolic activity measures indicated that the presence of phosphate in the suspension media can led to significantly reduced cell viability at all agglomerate sizes and at lower ZnO dosages. In addition, a reduction in cell viability was observed when agglomerate size was decreased, but only in the phosphate-containing media. These metabolic activity results were reflected in separate measures of cell death via the lactate dehydrogenase assay. Our results suggest that, while higher doses of water-soluble ZnO NPs are cytotoxic, the presence of phosphates in the surrounding fluid can lead to significantly elevated levels of cell death at lower ZnO NP doses. Moreover, the extent of this death can potentially be modulated or offset by tuning the agglomerate size. These findings underscore the importance of understanding how nanoscale materials can interact with the components of surrounding fluids so that potential adverse effects of such interactions can be controlled. Copyright © 2013 Elsevier Ireland Ltd. All rights reserved.

Thermoelectric properties of nano-meso-micro β-MnO₂ powders as a function of electrical resistance

DOE PAGES

Hedden, Morgan; Francis, Nick; Haraldsen, Jason T.; ...

2015-07-15

Particle sizes of manganese oxide (β-MnO₂) powders were modified by using a mortar and pestle ground method for period of times that varied between 15–60 min. Particle size versus ground time clearly shows the existence of a size-induced regime transition (i.e., regime I and II). Thermoelectric properties of β-MnO₂ powders as a function of electrical resistance in the range of R P = 10 - 80Ω were measured. Based on the data presented, we propose a model for the β-MnO₂ system in which nanometer-scale MnO₂ crystallites bond together through weak van der Waals forces to form larger conglomerates that spanmore » in size from nanometer to micrometer scale.« less

Optical absorption and photoluminescence studies of gold nanoparticles deposited on porous silicon

PubMed Central

2013-01-01

We present an investigation on a coupled system consists of gold nanoparticles and silicon nanocrystals. Gold nanoparticles (AuNPs) embedded into porous silicon (PSi) were prepared using the electrochemical deposition method. Scanning electron microscope images and energy-dispersive X-ray results indicated that the growth of AuNPs on PSi varies with current density. X-ray diffraction analysis showed the presence of cubic gold phases with crystallite sizes around 40 to 58 nm. Size dependence on the plasmon absorption was studied from nanoparticles with various sizes. Comparison with the reference sample, PSi without AuNP deposition, showed a significant blueshift with decreasing AuNP size which was explained in terms of optical coupling between PSi and AuNPs within the pores featuring localized plasmon resonances. PMID:23331761

Synthesis and Characterization Hierarchical Three-Dimensional TiO2 Structure via Hydrothermal Method

NASA Astrophysics Data System (ADS)

Syuhada, N.; Yuliarto, B.; Nugraha

2018-05-01

TiO2 is one of the most potential candidates due to its fascinating properties for multi-discipline fields. One dimensional nanostructure TiO2 such as nanotube and nanorods has been widely used for many devices technology. Compare with one-dimensional nanostructure TiO2; the hierarchical TiO2 has not been widely applied. Three dimensional TiO2 play a promising role for application in many different fields such as photovoltaics, photocatalytic and a gas sensor. Herein, we report that the hierarchically structures TiO2 have been successfully obtained by the one-pot Hydrothermal process. The growth mechanism of Titania was controlled by Titanium (IV) isopropoxide (TTIP). Ethylene glycol (EG). Hydrochloric acid (HCl). Hexadecyltrimethylammonium bromide (CTAB) molar ratio. TTIP was used as titanium source and CTAB as a soft template. The molar ratio of TTIP. EG. HCl. CTAB was 0.1:0.2:0.4:0.001. Those samples were synthesized using the hydrothermal method at 180 °C for 20 h. The purpose of this work was focused on investigating morphology, crystallite size, crystalline phase, and particle size. The properties of these materials were characterized by XRay Diffraction, Energy Dispersive Spectroscopy and Scanning Electron Microscope. It was found all particles exhibited unique spherical morphology which arranged by nanorods and good distribution nanoparticle. The Average size of the sphere has range 1 µm to 3 µm with diameter nanorods 60 nm to 100 nm. The TiO2 spheres were constructed of interconnected nanorods and formed a three dimensional (3D) porous framework. XRD analysis confirmed that sample consisted of pure rutile crystal structure with crystallite size was 50 nm, and EDS revealed an elemental content of Ti 61.03 % and O 38.97 %.

Fabrication of TiN nanorods by electrospinning and their electrochemical properties

NASA Astrophysics Data System (ADS)

Sun, Dongfei; Lang, Junwei; Yan, Xingbin; Hu, Litian; Xue, Qunji

2011-05-01

TiN nanorods were synthesized using electrospinning technique followed by thermolysis in different atmospheres. A dimethyl formamide-ethanol solution of poly-(vinyl pyrrolidone) and Ti (IV)-isopropoxide was used as the electrospinning precursor solution and as-spun nanofibers were calcined at 500 °C in air to generate TiO 2 nanofibers. Subsequently, a conversion from TiO 2 nanofibers to TiN nanorods was employed by the nitridation treatment at 600˜1400 °C in ammonia atmosphere. A typical characteristic of the final products was that the pristine nanofibers were cut into nanorods. The conversion from TiO 2 to TiN was realized when the nitridation temperature was above 800 °C. As-prepared nanorods were composed of TiN nano-crystallites and the average crystallite size gradually increased with the increase of the nitridation temperature. Electrochemical properties of TiN nanorods showed strong dependence on the nitridation temperature. The maximum value of the specific capacitance was obtained from the TiN nanorods prepared at 800 °C.

Reduced Iron Sulfide Systems for Removal of Heavy Metal Ions from Groundwater

DTIC Science & Technology

2009-07-01

be gleaned from higher magnification of these samples. Each set of lattice fringes represents a single crystal of mackinawite (Ohfuji and Ricard...diffractograms, the diffraction peaks are broad and weak, indicating a poor degree of crystallization or a small crystallite size. For the non-magnetic...the lattice spacings of synthetic mackinawite in this study are shorter. The 3-day aging in this study resulted in a higher degree of crystallization

50 CFR 622.208 - Minimum mesh size applicable to rock shrimp off Georgia and Florida.

Code of Federal Regulations, 2013 CFR

2013-10-01

... 50 Wildlife and Fisheries 12 2013-10-01 2013-10-01 false Minimum mesh size applicable to rock... mesh size applicable to rock shrimp off Georgia and Florida. (a) The minimum mesh size for the cod end of a rock shrimp trawl net in the South Atlantic EEZ off Georgia and Florida is 17/8 inches (4.8 cm...

50 CFR 622.208 - Minimum mesh size applicable to rock shrimp off Georgia and Florida.

Code of Federal Regulations, 2014 CFR

2014-10-01

... 50 Wildlife and Fisheries 12 2014-10-01 2014-10-01 false Minimum mesh size applicable to rock... mesh size applicable to rock shrimp off Georgia and Florida. (a) The minimum mesh size for the cod end of a rock shrimp trawl net in the South Atlantic EEZ off Georgia and Florida is 17/8 inches (4.8 cm...

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

Li Chengfeng

Calcium phosphate powders with nano-sized crystallinity were synthesized by neutralization using calcium hydroxide and orthophosphoric acid with the assistance of citric acid. The influence of processing parameters, such as free or additive citric acid, synthetic temperature and ripening time, on the crystallinity of hydroxyapatite were investigated. The results of X-ray diffraction and microstructure observations showed that the crystallinity and morphology of nano-sized hydroxyapatite particles were influenced by the presence or absence of citric acid. It was found that the crystallinities and crystallite sizes of hydroxyapatite powders prepared with the additive citric acid increased with increasing synthetic temperature and ripening time.more » Especially, the crystallinities of (h k 0) planes were raised and more homogeneously grown particles were obtained with increasing synthetic temperature.« less

Nanostructured Metal Oxides for Stoichiometric Degradation of Chemical Warfare Agents.

PubMed

Štengl, Václav; Henych, Jiří; Janoš, Pavel; Skoumal, Miroslav

2016-01-01

Metal oxides have very important applications in many areas of chemistry, physics and materials science; their properties are dependent on the method of preparation, the morphology and texture. Nanostructured metal oxides can exhibit unique characteristics unlike those of the bulk form depending on their morphology, with a high density of edges, corners and defect surfaces. In recent years, methods have been developed for the preparation of metal oxide powders with tunable control of the primary particle size as well as of a secondary particle size: the size of agglomerates of crystallites. One of the many ways to take advantage of unique properties of nanostructured oxide materials is stoichiometric degradation of chemical warfare agents (CWAs) and volatile organic compounds (VOC) pollutants on their surfaces.

Effect of Front-Side Silver Metallization on Underlying n+-p Junction in Multicrystalline Silicon Solar Cells: Preprint

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

Jiang, C. S.; Li, Z. G.; Moutinho, H. R.

2012-06-01

We report on the effect of front-side Ag metallization on the underlying n+-p junction of multicrystalline Si solar cells. The junction quality beneath the contacts was investigated by characterizing the uniformities of the electrostatic potential and doping concentration across the junction, using scanning Kelvin probe force microscopy and scanning capacitance microscopy. We investigated cells with a commercial Ag paste (DuPont PV159) and fired at furnace setting temperatures of 800 degrees, 840 degrees, and 930 degrees C, which results in actual cell temperatures ~100 degrees C lower than the setting temperature and the three cells being under-, optimal-, and over-fired. Wemore » found that the uniformity of the junction beneath the Ag contact was significantly degraded by the over-firing, whereas the junction retained good uniformity with the optimal- and under-fire temperatures. Further, Ag crystallites with widely distributed sizes from <100 nm to several μm were found at the Ag/Si interface of the over-fired cell. Large crystallites were imaged as protrusions into Si deeper than the junction depth. However, the junction was not broken down; instead, it was reformed on the entire front of the crystallite/Si interface. We propose a mechanism of the junction-quality degradation, based on emitter Si melting at the temperature around the Ag-Si eutectic point during firing, and subsequent recrystallization with incorporation of impurities in the Ag paste and with formation of crystallographic defects during quenching.« less

Damage creation in porous silicon irradiated by swift heavy ions

NASA Astrophysics Data System (ADS)

Canut, B.; Massoud, M.; Newby, P.; Lysenko, V.; Frechette, L.; Bluet, J. M.; Monnet, I.

2014-05-01

Mesoporous silicon (PS) samples were processed by anodising p+ Si wafers in (1:1) HF-ethanol solution. Different current densities were used to obtain three different porosities (41%, 56% and 75%). In all cases the morphology of the PS layer is columnar with a mean crystallite size between 12 nm (75% porosity) and 19 nm (41% porosity). These targets were irradiated at the GANIL accelerator, using different projectiles (130Xe ions of 91 MeV and 29 MeV, 238U ions of 110 MeV and 850 MeV) in order to vary the incident electronic stopping power Se. The fluences ranged between 1011 and 7 × 1013 cm-2. Raman spectroscopy and cross sectional SEM observations evidenced damage creation in the irradiated nanocrystallites, without any degradation of the PS layer morphology at fluences below 3 × 1012 cm-2. For higher doses, the columnar morphology transforms into a spongy-like structure. The damage cross sections, extracted from Raman results, increase with the electronic stopping power and with the sample porosity. At the highest Se (>10 keV nm-1) and the highest porosity (75%), the track diameter coincides with the crystallite diameter, indicating that a single projectile impact induces the crystallite amorphization along the major part of the ion path. These results were interpreted in the framework of the thermal spike model, taking into account the low thermal conductivity of the PS samples in comparison with that of bulk silicon.

Nano crystalline Bi{sub 2}(VO{sub 5}) phases in lithium bismuth borate glasses containing mixed vanadium-nickel oxides

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

Yadav, Arti, E-mail: artidabhur@gmail.com; Khasa, S.; Dahiya, M. S.

2016-05-23

Glass composition 7V{sub 2}O{sub 5}·23Li{sub 2}O·20Bi{sub 2}O{sub 3}·50B{sub 2}O{sub 3} and x(2NiO·V{sub 2}O{sub 5})·(30-x)Li{sub 2}O·20Bi{sub 2}O{sub 3}·50B{sub 2}O{sub 3}, x=0, 2, 5, 7 and 10, were produced by conventional melt quenching technique. The quenched amorphous glass samples were annealed at temperatures 400°C and 500°C for 6 hours. The Bi{sub 2}(VO{sub 5}) crystallite were grown in all prepared glass matrix. Tn vanadium lithium bismuth borate glass (annealed), the some phrase of V{sub 2}O{sub 5}-crystal were observed along with the nano crystalline Bi{sub 2}(VO{sub 5}) phase. The sharp peaks in FTTR spectra of all annealed compositions were also compatible with the XRDmore » diffraction peaks of the system under investigation. Average crystalline size (D) of the Bi{sub 2}(VO{sub 5}) nano-crystallite was ~30 nm for samples annealed at 400°C and ~42 nm for samples annealed at 500°C. Lattice parameter and the lattice strain for all the samples was also calculated corresponding to the (113) plane of Bi{sub 2}(VO{sub 5}) crystallite.« less

Comparative study on the physical properties of transition metal-doped (Co, Ni, Fe, and Mn) ZnO nanoparticles

NASA Astrophysics Data System (ADS)

Azab, A. A.; Ateia, Ebtesam E.; Esmail, S. A.

2018-07-01

Nano-crystalline of TM-doped ZnO with general formula Zn0.97TM0.03O (TM: Mn, Fe, Co, and Ni) was prepared using sol-gel method. The dependence of crystal structure, morphology, and optical and magnetic properties on the type of transition metals was investigated. The XRD investigation of pure and TM-doped ZnO nanoparticles samples confirms the formation of single-phase hexagonal wurtzite structure. The estimated crystallite sizes are found in the range of 17 and 38 nm for the doped and pure samples, respectively. The obtained data suggest that the dopant type plays a vital role in the physical properties of the investigated samples. The optical band-gap energy Eg has been calculated from near infrared (NIR) and visible (VIS) reflectance spectra using the Kubelka-Munk function. Minimum value of 2.398 eV and maximum one of 3.29 eV were obtained for Manganese-doped ZnO and pure ZnO, respectively. The analysis of XRD and VSM of the samples confirms that the observed room-temperature (RT) ferromagnetism can be attributed to an intrinsic property of doped material sample and not due to formation of any secondary phase. The magnetic results show that Mn is the most effective dopant for producing ferromagnetism in nanoparticles of ZnO.

Fabrication and Characterization of novel W80Ni10Nb10 alloy produced by mechanical alloying

NASA Astrophysics Data System (ADS)

Saxena, R.; Patra, A.; Karak, S. K.; Pattanaik, A.; Mishra, S. C.

2016-02-01

Nanostructured tungsten (W) based alloy with nominal composition of W80Ni10Nb10 (in wt. %) was synthesized by mechanical alloying of elemental powders of tungsten (W), nickel (Ni), niobium (Nb) in a high energy planetary ball-mill for 20 h using chrome steel as grinding media and toluene as process control agent followed by compaction at 500 MPa pressure for 5 mins and sintering at 1500°C for 2 h in Ar atmosphere. The phase evolution and the microstructure of the milled powder and consolidated product were investigated by X-ray diffraction (XRD), Scanning electron microscopy (SEM) and Transmission electron microscopy (TEM). The crystallite size of W in W80Ni10Nb10 powder was reduced from 100 μm at 0 h to 45.6 nm at 10 h and 34.1 nm at 20 h of milling whereas lattice strain increases to 35% at 20 h of milling. The dislocation density shows sharp increase up to 5 h of milling and the rate of increase drops beyond 5 to 20 h of milling. The lattice parameter of tungsten in W80Ni10Nb10 expanded upto 0.04% at 10 h of milling and contracted upto 0.02% at 20 h of milling. The SEM micrograph revealed the presence of spherical and elongated particles in W80Ni10Nb10 powders at 20 h of milling. The particle size decreases from 100 μm to 2 μm with an increase in the milling time from 0 to 20 hours. The crystallite size of W in milled W80Ni10Nb10 alloy as evident from bright field TEM image was in well agreement with the measured crystallite size from XRD. Structure of W in 20 h milled W80Ni10Nb10 alloy was identified by indexing of selected area diffraction (SAD) pattern. Formation of NbNi intermetallic was evident from XRD pattern and SEM micrograph of sintered alloy. Maximum sinterability of 90.8% was achieved in 20 h milled sintered alloy. Hardness and wear study was also conducted to investigate the mechanical behaviour of the sintered product. Hardness of W80Ni10Nb10 alloy reduces with increasing load whereas wear rate increases with increasing load. The evaluated hardness value in the present study for all loads is lower than the literature reported hardness of nanostructured W.

STEM-HAADF electron microscopy analysis of the central dark line defect of human tooth enamel crystallites.

PubMed

Gasga, Jose Reyes; Carbajal-de-la-Torre, Georgina; Bres, Etienne; Gil-Chavarria, Ivet M; Rodríguez-Hernández, Ana G; Garcia-Garcia, Ramiro

2008-02-01

When human tooth enamel is observed with the Transmission Electron Microscope (TEM), a structural defect is registered in the central region of their nanometric grains or crystallites. This defect has been named as Central Dark Line (CDL) and its structure and function in the enamel structure have been unknown yet. In this work we present the TEM analysis to these crystallites using the High Angle Annular Dark Field (HAADF) technique. Our results suggest that the CDL region is the calcium richest part of the human tooth enamel crystallites.

Computational studies of photoluminescence from disordered nanocrystalline systems

NASA Astrophysics Data System (ADS)

John, George

2000-03-01

The size (d) dependence of emission energies from semiconductor nanocrystallites have been shown to follow an effective exponent ( d^-β) determined by the disorder in the system(V.Ranjan, V.A.Singh and G.C.John, Phys. Rev B 58), 1158 (1998). Our earlier calculation was based on a simple quantum confinement model assuming a normal distribution of crystallites. This model is now extended to study the effects of realistic systems with a lognormal distribution in particle size, accounting for carrier hopping and nonradiative transitions. Computer simulations of this model performed using the Microcal Origin software can explain several conflicting experimental results reported in literature.

Solvent free tin oxide nanoparticle for gas sensing application

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

Ranjan, Pranay, E-mail: pranjan@iitp.ac.in; Thakur, Ajay D.; Centre for Energy and Environment, Indian Institute of Technology Patna, Patliputra, Patna 800013 India

2016-05-06

A new modified technique of synthesizing tin oxide nanoparticles with crystallite size of 2 nm to 6 nm has been developed. Surface area of the nanoparticle has been increased as we approached towards the Debye length. Such a techniques for approaching the Debye length is expected to bring remarkable changes in the properties of resistive based gas sensors. The technique used here is less toxic, economical and has high yield. Phase purity, size, shape and composition has been investigated using x-ray diffraction, micro Raman, scanning electron microscopy and energy dispersive x ray spectroscopy. While surface area has been calculated through Brunaur-Emmett-Teller (BET).

Extreme sensitivity of magnetic properties on the synthesis routes in La{sub 0.7}Sr{sub 0.3}MnO{sub 3}

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

Kumar, Ashutosh, E-mail: ashutosh.pph13@iitp.ac.in; Sharma, Himanshu; Tomy, C. V.

2016-05-06

La{sub 0.7}Sr{sub 0.3}MnO{sub 3} polycrystalline samples have been prepared using different synthesis routes. X-ray Diffraction (XRD) confirms that the samples are of single phase with R-3c space group. The surface morphology and particle size has been observed using Field Emission Scanning Electron Microscopy (FESEM). Magnetic measurement shows that the magnetization in the materials are affected by low crystallite size which destroys the spin ordering due to strain at grain boundaries and this also leads to reduction in magnetization as well as high coercivity in the material.

Thermal-induced SPR tuning of Ag-ZnO nanocomposite thin film for plasmonic applications

NASA Astrophysics Data System (ADS)

Singh, S. K.; Singhal, R.

2018-05-01

The formation of silver (Ag) nanoparticles in a ZnO matrix were successfully synthesized by RF-magnetron sputtering at room temperature. As prepared Ag-ZnO nanocomposite (NCs) thin films were annealed in vacuum at three different temperatures of 300 °C, 400 °C and 500 °C, respectively. The structural modifications for as-deposited and annealed films were estimated by X-ray diffraction and TEM techniques. The crystalline behavior preferably along the c-axis of the hexagonal wurtzite structure was observed in as-deposited Ag-ZnO film and improved significantly with increasing the annealing temperature. The crystallite size of as-deposited film was measured to be 13.6 nm, and increases up to 28.5 nm at higher temperatures. The chemical composition and surface structure of the as-deposited films were estimated by X-ray photoelectron spectroscopy. The presence of Ag nanoparticles with average size of 8.2 ± 0.2 nm, was confirmed by transmission electron microscopy. The strong surface plasmon resonance (SPR) band was observed at the wavelength of ∼565 nm for as-deposited film and a remarkable red shift of ∼22 nm was recorded after the annealing treatment as confirmed by UV-visible spectroscopy. Atomic force microscopy confirmed the grain growth from 60.38 nm to 79.42 nm for as-deposited and higher temperature annealed film respectively, with no significant change in the surface roughness. Thermal induced modifications such as disordering and lattice defects in Ag-ZnO NCs thin films were carried out by Raman spectroscopy. High quality Ag-ZnO NCs thin films with minimum strain and tunable optical properties could be useful in various plasmonic applications.

Effect of non-magnetic ions substitution on the structure and magnetic properties of Y3-xSrxFe5-xZrxO12 nanoparticles

NASA Astrophysics Data System (ADS)

Mahmoudi, Soulmaz; Gholizadeh, Ahmad

2018-06-01

In this work, Y3-xSrxZrxFe5O12 (0.0 ≤ x ≤ 0.7) were synthesized by citrate precursor method at 1050 °C. The structural and magnetic properties of Y3-xSrxFe5-xZrxO12 were studied by using the X-ray diffraction technique, scanning electron microscopy, transmission electron microscopy, the Fourier transform infrared spectroscopy and vibrating sample magnetometer. XRD analysis using X'Pert package show a pure garnet phase with cubic structure (space group Ia-3d) and the impurity phase SrZrO3 is observed when the range of x value is exceeded from 0.6. Rietveld refinement using Fullprof program shows the lattice volume expansion with increasing the degree of Sr/Zr substitution. The crystallite sizes remain constant in the range of x = 0.0 - 0.5 and then increase. The different morphology observed in SEM micrographs of the samples can be related to different values of the microstrain in the samples. The hysteresis loops of the samples reveal a superparamagnetic behaviour. Also, the drop in coercivity with increasing of the substitution is mainly originated from a reduction in the magneto-elastic anisotropy energy. The values of the saturation magnetization (MS) indicate a non-monotonically variant with increasing the Sr/Zr substitution and reach a maximum 26.14 emu/g for the sample x = 0.1 and a minimum 17.64 emu/g for x = 0.0 and x = 0.2. The variation of MS, in these samples results from a superposition of three factors; reduction of Fe3+ in a-site, change in angle FeT-O-FeO, and magnetic core size.

Pre-ordering of interfacial water in the pathway of heterogeneous ice nucleation does not lead to a two-step crystallization mechanism.

PubMed

Lupi, Laura; Peters, Baron; Molinero, Valeria

2016-12-07

According to Classical Nucleation Theory (CNT), the transition from liquid to crystal occurs in a single activated step with a transition state controlled by the size of the crystal embryo. This picture has been challenged in the last two decades by several reports of two-step crystallization processes in which the liquid first produces pre-ordered or dense domains, within which the crystal nucleates in a second step. Pre-ordering preceding crystal nucleation has been recently reported in simulations of ice crystallization, raising the question of whether the mechanism of ice nucleation involves two steps. In this paper, we investigate the heterogeneous nucleation of ice on carbon surfaces. We use molecular simulations with efficient coarse-grained models combined with rare event sampling methods and free energy calculations to elucidate the role of pre-ordering of liquid water at the carbon surface in the reaction coordinate for heterogeneous nucleation. We find that ice nucleation proceeds through a classical mechanism, with a single barrier between liquid and crystal. The reaction coordinate that determines the crossing of the nucleation barrier is the size of the crystal nucleus, as predicted by CNT. Wetting of the critical ice nuclei within pre-ordered domains decreases the nucleation barrier, increasing the nucleation rates. The preferential pathway for crystallization involves the early creation of pre-ordered domains that are the birthplace of the ice crystallites but do not represent a minimum in the free energy pathway from liquid to ice. We conclude that a preferential pathway through an intermediate-order precursor does not necessarily result in a two-step mechanism.

50 CFR 622.454 - Minimum size limit.

Code of Federal Regulations, 2013 CFR

2013-10-01

... ADMINISTRATION, DEPARTMENT OF COMMERCE FISHERIES OF THE CARIBBEAN, GULF OF MEXICO, AND SOUTH ATLANTIC Spiny Lobster Fishery of Puerto Rico and the U.S. Virgin Islands § 622.454 Minimum size limit. (a) The minimum...

50 CFR 622.454 - Minimum size limit.

Code of Federal Regulations, 2014 CFR

2014-10-01

... ADMINISTRATION, DEPARTMENT OF COMMERCE FISHERIES OF THE CARIBBEAN, GULF OF MEXICO, AND SOUTH ATLANTIC Spiny Lobster Fishery of Puerto Rico and the U.S. Virgin Islands § 622.454 Minimum size limit. (a) The minimum...

Micro Structural, Optical and Magnetic Properties of Co-SiO2 Nanocomposite Synthesized by Sol-Gel Technique

NASA Astrophysics Data System (ADS)

Saha, Mrinal; Mukherjee, Soumya; Gayen, Arup; Mukherjee, Siddhartha

2017-04-01

Co-SiO2 nano composite has been synthesized via sol-gel technique using dextrose [C6H12O6] as a reducer and tetraethyl orthosilicate [Si(OCH2CH3)4] as oxide forming agent, respectively. The dried gel has been subsequently calcined at different temperature (850 and 900 °C) for 30 min in an inert atmosphere by N2 purging. The synthesized materials have been characterized by X-ray diffraction, high resolution transmission microscope, Fourier transform infrared spectroscopy, UV-Vis spectroscopy, scanning electron microscope, field emission microscope, atomic force microscope and physical property measurement system. The crystallite sizes of the face centered cubic cobalt nano composite materials have been found to be in the range of 14-28 nm. The crystallite size of the material found to be increased at higher calcination temperature due to the grain growth. The surface morphology of the obtained material has been found to be agglomerated but spherical in nature. This agglomeration tendency could be attributed to magnetic interaction between particles, large surface area as well as high surface energy. The band gap value of the obtained material has been determined to be 1.92 eV. The saturation magnetization (Ms) and the coercivity (Hc) of the composite material were found to be 29.45 emu g-1and 23.2 Oe, respectively. This technique has thus been found to be a convenient and effective method to prepare pure metallic cobalt nanoparticles with uniform size and homogeneous distribution throughout the matrix.

Structural elucidation and magnetic behavior evaluation of Cu-Cr doped BaCo-X hexagonal ferrites

NASA Astrophysics Data System (ADS)

Azhar Khan, Muhammad; Hussain, Farhat; Rashid, Muhammad; Mahmood, Asif; Ramay, Shahid M.; Majeed, Abdul

2018-04-01

Ba2-xCuxCo2CryFe28-yO46 (x = 0.0, 0.1, 0.2, 0.3, 0.4, y = 0.0, 0.2, 0.4, 0.6, 0.8) X-type hexagonal ferrites were synthesized via micro-emulsion route. The techniques which were applied to characterize the prepared samples are as follows: X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), Dielectric measurements and vibrating sample magnetometer (VSM). The structural parameters i.e. lattice constant (a, c), cell volume (V), X-ray density, bulk density and crystallite size of all the prepared samples were obtained using XRD analysis. The lattice parameters 'a' and 'c' increase from 5.875 Å to 5.934 Å and 83.367 Å to 83.990 Å respectively. The crystallite size of investigated samples lies in the range of 28-32 nm. The magnetic properties of all samples have been calculated by vibrating sample magnetometer (VSM) analysis. The increase in coercivity (Hc) was observed with the increase of doping contents. It was observed that the coercivity (Hc) of all prepared samples is inversely related to the crystalline size which reflects that all materials are super-paramagnetic. The dielectric parameters i.e. dielectric constant, dielectric loss, tangent loss etc were obtained in the frequency range of 1 MHz-3 GHz and followed the Maxwell-Wagner's model. The significant variation the dielectric parameters are observed with increasing frequency. The maximum Q value is obtained at ∼2 GHz due to which these materials are used for high frequency multilayer chip inductors.

Phase identification and morphology study of hematite (Fe2O3) with sintering time varitions

NASA Astrophysics Data System (ADS)

Yazirin, Cepi; Puspitasari, Poppy; Sasongko, Muhammad Ilman Nur; Tsamroh, Dewi Izzatus; Risdanareni, Puput

2017-09-01

Iron oxide has been the interest of many studies due to its applications in various scientific and industrial fields including in environment, corrosion, soil science, and exhaust emissions. Iron oxide (Fe2O3) has potential applications in catalytic reactions in electronic devices such as semiconductors, paint formulations, and lithium rechargeable batteries. Fe2O3 can be synthesized through the process of stirring, decomposition of organic iron, sol-gel, combustion, and evaporating solvents. Most of the methods used involve several steps and take a long time. The aim of this research was to investigate the phase and morphology characterization of iron oxide (Fe2O3) powder with solvent ethylene glycol after being sintered for 1 hour, 2 hours and 3 hours. The characterization tools utilized were XRD, SEM-EDX, and FTIR. The results of XRD analysis showed that the Fe2O3 sintered for 1 hour had the smallest crystallite size with a diameter of 21.05 nm. In the XRD test, the beam of X-ray was shot directly at the grain being tested. The results of SEM analysis showed thatthe Fe2O3 sintered for 1 hour produced the best result due to its crystallite size of 12.36 nm and hada shape of homogeneous nanosphere; the duration of sintering indeed had a great influence on the grain size of iron oxide (Fe2O3). In addition, the results of the elemental composition analysis indicate that the longer the sintering process, the higher the concentration of O but the lower the Fe.

Thermal-induced structural and optical investigations of Agsbnd ZnO nanocomposite thin films

NASA Astrophysics Data System (ADS)

Singh, S. K.; Singhal, R.

2018-07-01

In the present paper, we have successfully synthesized Agsbnd ZnO nanocomposite thin films by RF-magnetron sputtering technique at room temperature. Systematic investigations of thermal-induced structural and optical modifications in Agsbnd ZnO thin films have been observed and described. The Agsbnd ZnO thin films were annealed at three different temperatures of 300 °C, 400 °C and 500 °C in vacuum to prevent the oxidation of Ag. The presence and formation of Ag nanoparticles were estimated by transmission electron microscopy. X-ray diffraction analysis revealed the structural information about the crystalline quality of ZnO. The crystallinity as well as the crystallite size of the films have been found to be improved with annealing temperatures. The estimated crystallite size was ∼15.8 nm for as-deposited film and 19.0 nm for the film at a higher temperature. The chemical composition and structural analysis of as-deposited film were carried out by X-ray photoelectron spectroscopy. A very sharp absorption band appeared at ∼540 nm for Ag NPs that is associated with the surface plasmon resonance band of Ag. A noticeable red shift of about ∼12 nm has been recorded for films annealed at 500 °C. Atomic force microscopy has been utilized to examine the surface morphology of the as-deposited and annealed films. The grain size was found to be increase with increasing annealing temperature, while no significant changes were observed in the roughness of Agsbnd ZnO thin films. Raman spectroscopy revealed lattice defects and disordering in the films after the thermal annealing.

46 CFR 111.60-4 - Minimum cable conductor size.

Code of Federal Regulations, 2010 CFR

2010-10-01

... 46 Shipping 4 2010-10-01 2010-10-01 false Minimum cable conductor size. 111.60-4 Section 111.60-4...-GENERAL REQUIREMENTS Wiring Materials and Methods § 111.60-4 Minimum cable conductor size. Each cable conductor must be #18 AWG (0.82 mm2) or larger except— (a) Each power and lighting cable conductor must be...

46 CFR 111.60-4 - Minimum cable conductor size.

Code of Federal Regulations, 2011 CFR

2011-10-01

... 46 Shipping 4 2011-10-01 2011-10-01 false Minimum cable conductor size. 111.60-4 Section 111.60-4...-GENERAL REQUIREMENTS Wiring Materials and Methods § 111.60-4 Minimum cable conductor size. Each cable conductor must be #18 AWG (0.82 mm2) or larger except— (a) Each power and lighting cable conductor must be...

50 CFR 648.75 - Shucking at sea and minimum surfclam size.

Code of Federal Regulations, 2012 CFR

2012-10-01

... 50 Wildlife and Fisheries 12 2012-10-01 2012-10-01 false Shucking at sea and minimum surfclam size... Measures for the Atlantic Surf Clam and Ocean Quahog Fisheries § 648.75 Shucking at sea and minimum surfclam size. (a) Shucking at sea—(1) Observers. (i) The Regional Administrator may allow the shucking of...

50 CFR 648.75 - Shucking at sea and minimum surfclam size.

Code of Federal Regulations, 2014 CFR

2014-10-01

... 50 Wildlife and Fisheries 12 2014-10-01 2014-10-01 false Shucking at sea and minimum surfclam size... Measures for the Atlantic Surf Clam and Ocean Quahog Fisheries § 648.75 Shucking at sea and minimum surfclam size. (a) Shucking at sea—(1) Observers. (i) The Regional Administrator may allow the shucking of...

50 CFR 648.75 - Shucking at sea and minimum surfclam size.

Code of Federal Regulations, 2013 CFR

2013-10-01

... 50 Wildlife and Fisheries 12 2013-10-01 2013-10-01 false Shucking at sea and minimum surfclam size... Measures for the Atlantic Surf Clam and Ocean Quahog Fisheries § 648.75 Shucking at sea and minimum surfclam size. (a) Shucking at sea—(1) Observers. (i) The Regional Administrator may allow the shucking of...

40 CFR 1042.310 - Engine selection for Category 1 and Category 2 engines.

Code of Federal Regulations, 2010 CFR

2010-07-01

... Category 2 engines. (a) Determine minimum sample sizes as follows: (1) For Category 1 engines, the minimum sample size is one engine or one percent of the projected U.S.-directed production volume for all your Category 1 engine families, whichever is greater. (2) For Category 2 engines, the minimum sample size is...

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

Moussa, Sana Ben; Bachouâ, Hassen; Gruselle, Michel, E-mail: michel.gruselle@upmc.fr

The present article details the formation of calcium hydroxyapatite synthesized by the hydrothermal way, in presence of glycine or sarcosine. The presence of these amino-acids during the synthetic processes reduces the crystalline growthing through the formation of hybrid organic-inorganic species The crystallite sizes are decreasing and the morphology is modified with the increase of the amino-acid concentration. - Graphical abstract: Formation of Ca carboxylate salt leading to the grafting of glycine and sarcosine on the Ca=Hap surface (R= H, CH3).

Features of structural response of mechanically loaded crystallites to irradiation

NASA Astrophysics Data System (ADS)

Korchuganov, Aleksandr V.

2015-10-01

A molecular dynamics method is employed to investigate the origin and evolution of plastic deformation in elastically deformed iron and vanadium crystallites due to atomic displacement cascades. Elastic stress states of crystallites result from different degrees of specimen deformation. Crystallites are deformed under constant-volume conditions. Atomic displacement cascades with the primary knock-on atom energy up to 50 keV are generated in loaded specimens. It is shown that irradiation may cause not only the Frenkel pair formation but also large-scale structural rearrangements outside the irradiated area, which prove to be similar to rearrangements proceeding by the twinning mechanism in mechanically loaded specimens.

The importance of size-exclusion characteristics of type I collagen in bonding to dentin matrices

PubMed Central

M, Takahashi; M, Nakajima; J, Tagami; DLS, Scheffel; RM, Carvalho; A, Mazzoni; M, Carrilho; A, Tezvergil-Mutluay; L, Breschi; L, Tjäderhane; SS, Jang; FR, Tay; KA, Agee; DH, Pashley

2013-01-01

The mineral phase of dentin is located primarily within collagen fibrils. During development, bone or dentin collagen fibrils are formed first and then water within the fibril is replaced with apatite crystallites. Mineralized collagen contains very little water. During dentin bonding, acid-etching of mineralized dentin solubilizes the mineral crystallites and replaces them with water. During the infiltration phase of dentin bonding, adhesive comonomers are supposed to replace all of the collagen water with adhesive monomers that are then polymerized into copolymers. The authors of a recently published review suggested that dental monomers were too large to enter and displace water from collagen fibrils. If that were true, the endogenous proteases bound to dentin collagen could be responsible for unimpeded collagen degradation that is responsible for the poor durability of resin-dentin bonds. The current work studied the size-exclusion characteristics of dentin collagen, using a gel-filtration-like column chromatography technique, using dentin powder instead of Sephadex. The elution volumes of test molecules, including adhesive monomers, revealed that adhesive monomers smaller than about 1000 Da can freely diffuse into collagen water, while molecules of 10,000 Da begin to be excluded, and bovine serum albumin (66,000 Da) was fully excluded. These results validate the concept that dental monomers can permeate between collagen molecules during infiltration by etch-and-rinse adhesives. PMID:23928333

Thin-walled nanoscrolls by multi-step intercalation from tubular halloysite-10 Å and its rearrangement upon peroxide treatment

NASA Astrophysics Data System (ADS)

Zsirka, Balázs; Horváth, Erzsébet; Szabó, Péter; Juzsakova, Tatjána; Szilágyi, Róbert K.; Fertig, Dávid; Makó, Éva; Varga, Tamás; Kónya, Zoltán; Kukovecz, Ákos; Kristóf, János

2017-03-01

Surface modification of the halloysite-10 Å mineral with tubular morphology can be achieved by slightly modified procedures developed for the delamination of kaolinite minerals. The resulting delaminated halloysite nanoparticles have unexpected surface/morphological properties that display, new potentials in catalyst development. In this work, a four-step intercalation/delamination procedure is described for the preparation of thin-walled nanoscrolls from the multi-layered hydrated halloysite mineral that consists of (1) intercalation of halloysite with potassium acetate, (2) replacement intercalation with ethylene glycol, (3) replacement intercalation with hexylamine, and (4) delamination with toluene. The intercalation steps were followed by X-ray diffraction, transmission electron microscopy, N2 adsorption-desorption, thermogravimetry, and infrared spectroscopy. Delamination eliminated the crystalline order and the crystallite size along the 'c'-axis, increased the specific surface area, greatly decreased the thickness of the mineral tubes to a monolayer, and shifted the pore diameter toward the micropore region. Unexpectedly, the removal of residual organics from intercalation steps adsorbed at the nanoscroll surface with a peroxide treatment resulted in partial recovery of crystallinity and increase of crystallite size along the 'c'-crystal direction. The d(001) value showed a diffuse pattern at 7.4-7.7 Å due to the rearrangement of the thin-walled nanoscrolls toward the initial tubular morphology of the dehydrated halloysite-7 Å mineral.

Structural investigation of Mimosa pudica Linn fibre

NASA Astrophysics Data System (ADS)

Patra, S. R.; Pattojoshi, P.; Tiwari, T. N.; Mallick, B.

2017-04-01

Sensitive plant ( Mimosa pudica Linn.) fibre is a natural fibre with electrically conductive property. Because of its electro-active sensing nature, it has been found very interesting among physicists, chemists, biologists, material scientists and technologists. So far as our knowledge is concerned; there is no report on the X-ray structure of M. pudica fibre using diffraction technique. In the present report, the M. pudica fibre has been extracted from the stem of the herb by sinking the stem in 10% NaOH solution for one week. The diffraction pattern of the fibre is found out to be cellulose-I. The effect of the fibre structure and its orientation due to different mounting have been investigated using X-ray diffraction technique. The I max of cellulose-I has been observed along (002) and (10\\overline{1)} for the perpendicular and parallel mounting of the native-fibre, respectively. Full width at half maxima of the diffraction profile turns out to be decreased with fibre orientation. Dimension of crystallite size D hkl estimated in the perpendicular mounting D_{hkl}^{ \\bot } is more as compared to that of the parallel mounting D_{hkl}^{{^{allel } }}. The smallest crystallite sizes observed in both parallel and perpendicular mounting are 18.78 and 30.78 Å respectively. It is expected that the present study may help to analyse the X-ray diffraction of fibre materials in general and natural fibres in particular.

Mimosa pudica (L.) assisted green synthesis and photoluminescence studies of Y2O3:Mg2+ nanophosphor for display applications

NASA Astrophysics Data System (ADS)

Venkatachalaiah, KN; Venkataravanappa, M.; Nagabhushana, H.; Basavaraj, R. B.

2016-09-01

For the first time green route method was used to synthesize pure and Mg2+(1-11 mol %) doped Y2O3 nanophosphors by using Mimosa pudica leaves extract as a fuel. The final product was well characterized by powder x-ray diffraction (PXRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), diffuse reflectance spectroscopy (DRS) and photoluminescence (PL).The PXRD result shows the formation of single phase, cubic structure of Y2O3 with crystallite sizes ∼25 nm. The SEM results showed porous and agglomerated structures, TEM images showed the crystallite size of the material and was found to be around ∼ 25 nm. PL emission spectra show the blue light emission under the excitation wavelength of 315 nm. The emission peaks of Mg2+were observed at 428 nm, 515 nm and 600 nm corresponding to the transitions of 4F9/2 → 6Hi7/2 (violet), 4F9/2 → 6Hi5/2 (blue), 4F9/2 → 6HJ3/2 (yellow) respectively. The estimated CIE chromaticity co-ordinate was very close to the national television standard committee value of blue emission. CCT was found to be ∼ 6891 K as a result the present phosphor was potential to be used for warm white light emitting display applications.

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

Laser surface treatment for porous and textured Ca-P bio-ceramic coating on Ti-6Al-4V.

PubMed

Paital, Sameer R; Dahotre, Narendra B

2007-12-01

In the present paper the feasibility of depositing a porous calcium phosphate (CaP) bio-ceramic coating using a continuous wave Nd:YAG laser on a Ti-6Al-4V substrate has been demonstrated. The advantages offered by such porous bio-ceramic coating are its inertness combined with the mechanical stability of the highly convoluted interface that develops when bone grows into the pores of ceramic. The formation of different phases with varying laser fluences is studied using x-ray diffraction (XRD). A quantitative estimation of the crystallite size and relative amounts of Ti and other predominant phases such as TiO(2) and alpha-tricalcium phosphate (alpha-TCP) were obtained. An increase in the crystallite size with increasing laser fluence is observed for all the above three phases. It is observed that TiO(2) is the predominant phase for all laser fluences and there is an increase in the alpha-TCP phase with increasing laser fluence. Surface porosity measurements indicated a decreasing trend with increasing laser fluence. Microhardness measurements in the cross section of samples showed a maximum hardness within the coating. The bioactivity of the coatings was further demonstrated by the formation of an apatite-like layer on the surface of the sample after being immersed in a simulated biofluid.

Tunable Crystallization and Nucleation of Planar CH3NH3PbI3 through Solvent-Modified Interdiffusion.

PubMed

Yao, Zhibo; Jones, Timothy W; Grigore, Mihaela; Duffy, Noel W; Anderson, Kenrick F; Dunbar, Ricky B; Feron, Krishna; Hao, Feng; Lin, Hong; Wilson, Gregory J

2018-05-02

A smooth and compact light absorption perovskite layer is a highly desirable prerequisite for efficient planar perovskite solar cells. However, the rapid reaction between CH 3 NH 3 I methylammonium iodide (MAI) and PbI 2 often leads to an inconsistent CH 3 NH 3 PbI 3 crystal nucleation and growth rate along the film depth during the two-step sequential deposition process. Herein, a facile solvent additive strategy is reported to retard the crystallization kinetics of perovskite formation and accelerate the MAI diffusion across the PbI 2 layer. It was found that the ultrasmooth perovskite thin film with narrow crystallite size variation can be achieved by introducing favorable solvent additives into the MAI solution. The effects of dimethylformamide, dimethyl sulfoxide, γ-butyrolactone, chlorobenzene, and diethyl ether additives on the morphological properties and cross-sectional crystallite size distribution were investigated using atomic force microscopy, X-ray diffraction, and scanning electron microscopy. Furthermore, the light absorption and band structure of the as-prepared CH 3 NH 3 PbI 3 films were investigated and correlated with the photovoltaic performance of the equivalent solar cell devices. Details of perovskite nucleation and crystal growth processes are presented, which opens new avenues for the fabrication of more efficient planar solar cell devices with these ultrasmooth perovskite layers.

Structural and electromagnetic characterization of Co-Mn doped Ni-Sn ferrites fabricated via micro-emulsion route

NASA Astrophysics Data System (ADS)

Ali, Rajjab; Azhar Khan, Muhammad; Manzoor, Alina; Shahid, Muhammad; Farooq Warsi, Muhammad

2017-11-01

Ni0.5Sn0.5CoxMnxFe2-2xO4 ferrites with x = 0.0-0.8 have been prepared by the micro-emulsion method, using CTAB as a surfactant material. X-ray diffraction (XRD), Fourier transformed infrared spectroscopy (FTIR) and vibrational sample magnetometer (VSM) were used to investigate the effects of Co and Mn substitutions on cationic distribution, crystallite size, lattice constant, spectral, magnetic and dielectric properties. Lattice constant and crystallite size were found to increase from 7.4 to 9.25 Å and from 11.8 to 19.7 nm respectively with increasing substitution of Co and Mn ions. Saturation magnetization (MS) gradually increased from 20.5 to 47.6 emu/g with increase in the value of x. However, Coercivity increased from 152.7 to 462.4 Oe up to x = 0.4 and then it decreased thereafter. The dielectric constant, complex dielectric constant and tan loss (tanδ) were observed to decrease with increase in frequency, depicting the semiconductor behavior of the ferrites. Dc resistivity was observed to decrease considerably upon addition of Co and Mn content. The outcome for the tunable magnetic properties and achieved modification of the synthesized nanocrystallites may be chosen for tremendous applications; such as miniaturized memory devices that are based on the energy storage principles and capacitive components.

Kinetic and catalytic analysis of mesoporous Co3O4 on the oxidation of morin

NASA Astrophysics Data System (ADS)

Xaba, Morena. S.; Meijboom, Reinout

2017-11-01

Herein we report on the synthesis, characterization and catalytic evaluation of mesoporous cobalt oxides on the oxidation of morin. These mesoporous cobalt oxides were synthesized using an inverse surfactant micelle method, they are connected, well-defined with intra-particle voids. These materials were calcined to different final heating temperatures of 150, 250, 350, 450 and 550 °C, and each mesoporous cobalt oxide catalyst showed unique physical properties and catalytic behavior. Morin oxidation was used as a model reaction in the presence of hydrogen peroxide to evaluate the kinetic and catalytic activity of calcined mesoporous cobalt oxides. The adsorption-desorption equilibrium rate constants of morin and hydrogen peroxide were found to be inversely proportional to the crystallite size of the mesoporous cobalt oxide, and the characteristic path length in which the mass transfer takes place was found to be directly proportional to the crystallite size. The materials were characterized using powder X-Ray Diffraction (p-XRD), N2-sorption isotherms (BET), hydrogen temperature programmed reduction (H2-TPR) and High Resolution-Transmission Electron Microscopy (HR-TEM). UV-vis spectrophotometry was used to monitor the time-resolved absorbance of morin at λmax = 410 nm. The surface reaction in this system is described in terms of the well-established Langmuir-Hinshelwood model. The thermodynamic parameters, EA, ΔH#, ΔS# and ΔG# were calculated and catalyst recycling and reusability is demonstrated.

High hardness BaCb-(BxOy/BN) composites with 3D mesh-like fine grain-boundary structure by reactive spark plasma sintering.

PubMed

Vasylkiv, Oleg; Borodianska, Hanna; Badica, Petre; Grasso, Salvatore; Sakka, Yoshio; Tok, Alfred; Su, Liap Tat; Bosman, Michael; Ma, Jan

2012-02-01

Boron carbide B4C powders were subject to reactive spark plasma sintering (also known as field assisted sintering, pulsed current sintering or plasma assisted sintering) under nitrogen atmosphere. For an optimum hexagonal BN (h-BN) content estimated from X-ray diffraction measurements at approximately 0.4 wt%, the as-prepared BaCb-(BxOy/BN) ceramic shows values of Berkovich and Vickers hardness of 56.7 +/- 3.1 GPa and 39.3 +/- 7.6 GPa, respectively. These values are higher than for the vacuum SPS processed B4C pristine sample and the h-BN -mechanically-added samples. XRD and electronic microscopy data suggest that in the samples produced by reactive SPS in N2 atmosphere, and containing an estimated amount of 0.3-1.5% h-BN, the crystallite size of the boron carbide grains is decreasing with the increasing amount of N2, while for the newly formed lamellar h-BN the crystallite size is almost constant (approximately 30-50 nm). BN is located at the grain boundaries between the boron carbide grains and it is wrapped and intercalated by a thin layer of boron oxide. BxOy/BN forms a fine and continuous 3D mesh-like structure that is a possible reason for good mechanical properties.

Structural and optoelectronic studies on Ag-CdS quantum dots

NASA Astrophysics Data System (ADS)

Ibrahim Mohammed S., M.; Gubari, Ghamdan M. M.; Huse, Nanasaheb P.; Dive, Avinash S.; Sharma, Ramphal

2018-05-01

In the present study, we have successfully deposited CdS quantum dot thin films and Ag doped CdS on a glass slide by simple and economical chemical bath deposition at room temperature. The X-ray diffraction method analysis reveals that CdS thin films exhibit hexagonal structure when compared with standard JCPDS data. The estimated average crystallite size of the quantum dots and resulted in the least crystallite size of ˜9 nm. a comparison between the optical and electrical properties of the films before and after doping Ag was made through measuring and analyzing the curves for UV and I-V. From UV absorption spectra we observed that the samples exhibited a band edge near ˜400 nm with a slight deviation with the presence of excitonic peak for both CdS and Ag doped CdS. The presence of excitonic peak may be referred to the formation of quantum dots. The calculated band gap energy of thin films was found to be 3.45 eV and 3.15 eV for both CdS and Ag doped CdS thin films respectively, where the optical absorption spectra of Ag doped CdS nanoparticles also exhibit shift with respect to that of CdS quantum dots thin films. The photosensitive of CdS thin films show an increase in photocurrent when Ag doped CdS.

Evolution of the atomic order and valence state of rare-earth atoms and uranium in a new carbon-metal composite—diphthalocyanine pyrolysate C64H32N16 Me ( Me = Y, La, Ce, Eu, and U)

NASA Astrophysics Data System (ADS)

Sovestnov, A. E.; Kapustin, V. K.; Tikhonov, V. I.; Fomin, E. V.; Chernenkov, Yu. P.

2014-08-01

The structure of a metal-carbon composite formed by the pyrolysis of diphthalocyanine of some rare-earth elements (Y, La, Ce, Eu) and uranium in the temperature range T ann = 800-1700°C has been investigated for the first time by the methods of X-ray diffraction analysis and X-ray line shift. It has been shown that, in the general case, the studied pyrolysates consist of three phases. One phase corresponds to the structure of graphite. The second phase corresponds to nitrides, carbides, and oxides of basic metal elements with a crystallite size ranging from 5 to 100 nm. The third phase is amorphous or consisting of crystallites with a size of ˜1 nm. It has been found that all the basic elements (Y, La, Ce, Eu, U) and incorporated iodine atoms in the third phase are in a chemically bound state. The previously unobserved electronic configurations have been revealed for europium. The possibility of including not only atoms of elements forming diphthalocyanine but also other elements (for example, iodine) in the composite structure is of interest, in particular, for the creation of a thermally, chemically, and radiation resistant metal-carbon matrix for the radioactive waste storage.

Reproducible Crystallite Size of Mono-Dispersed and Scalable Biologically Produced Metal-Substituted Nanometer-Sized Magnetites

NASA Astrophysics Data System (ADS)

Moon, J.; Rawn, C.; Rondinone, A.; Love, L.; Roh, Y.; Lauf, R.; Phelps, T.

2008-12-01

Our previous research demonstrated that biosynthesized magnetite (biomagnetite) exhibited similar properties as chemically synthesized magnetite. To complement uses of the traditional chemically synthesized magnetite (chem-magnetite) biomagnetite must be exhibit highly reproducible sizes and be available in scalable qualities. Here we emphasize potentially advantageous properties of biomagnetite regarding size, reproducibility and scaling availability. Average crystallite size (ACS) of biomagnetites ranging from 10-100 nm was determined after varied 1) incubation times, 2) substitution of metal and lanthanide species, 3) degrees of congruent incorporation or retardation of substitution elements, 4) bacterial species with their varied ability to substitute elemental species, and 6) incubation temperature that can influence coalescence. The microbial production of biomagnetite has demonstrated capacity to make highly crystalline nanoscale particles of metal-substituted ferrites including compounds of Co, Ni, Cr, Mn, Zn and the rare earths in large quantity. Selected Zn-substituted magnetite (nominal composition of Zn0.6Fe2.4O4) has been recovered at over 1 kg (wet weight) in batches from 30 L fermentations. The massively produced extracellular magnetites were confirmed to exhibit good mono- dispersity via transmission electron microscopy (TEM). TEM also validated highly reproducible ACS of 13.1±0.8 nm size as determined through X-ray diffraction (N=7) at a 99 % confidence level. Based on the scale-up experiments performed using the 35 L reactor, the reduction in ACS variability and shorted incubation times of several days may be attributed to increases of electron donor input, and availability of divalent ions of the substitution metal with less ferrous ions in the case of doped magnetite, or a combination of the above. While costs of commercial nanometer sized magnetite (25-50 nm) may vary from 500/kg to > 1,000/kg, microbial mass production is likely capable of producing 13-90 nm magnetite or doped magnetites at a fraction of the cost of traditional chemical synthesis. While there are numerous approaches for the synthesis of nanoparticles, bacterial fermentation of magnetite or metal-substituted magnetite may represent a disruptive manufacturing technology with respect to yield, reproducibility and scalability.

7 CFR 51.2952 - Size specifications.

Code of Federal Regulations, 2011 CFR

2011-01-01

... specifications. Size shall be specified in accordance with the facts in terms of one of the following classifications: (a) Mammoth size. Mammoth size means walnuts of which not over 12 percent, by count, pass through... foregoing classifications, size of walnuts may be specified in terms of minimum diameter, or minimum and...

7 CFR 51.2952 - Size specifications.

Code of Federal Regulations, 2010 CFR

2010-01-01

... specifications. Size shall be specified in accordance with the facts in terms of one of the following classifications: (a) Mammoth size. Mammoth size means walnuts of which not over 12 percent, by count, pass through... foregoing classifications, size of walnuts may be specified in terms of minimum diameter, or minimum and...

7 CFR 51.1216 - Size requirements.

Code of Federal Regulations, 2013 CFR

2013-01-01

...) The numerical count or a count-size based on equivalent tray pack size designations or the minimum... numerical count is not shown the minimum diameter shall be plainly stamped, stenciled, or otherwise marked...

7 CFR 51.1216 - Size requirements.

Code of Federal Regulations, 2014 CFR

2014-01-01

...) The numerical count or a count-size based on equivalent tray pack size designations or the minimum... numerical count is not shown the minimum diameter shall be plainly stamped, stenciled, or otherwise marked...

Practical implementation of channelized hotelling observers: effect of ROI size

NASA Astrophysics Data System (ADS)

Ferrero, Andrea; Favazza, Christopher P.; Yu, Lifeng; Leng, Shuai; McCollough, Cynthia H.

2017-03-01

Fundamental to the development and application of channelized Hotelling observer (CHO) models is the selection of the region of interest (ROI) to evaluate. For assessment of medical imaging systems, reducing the ROI size can be advantageous. Smaller ROIs enable a greater concentration of interrogable objects in a single phantom image, thereby providing more information from a set of images and reducing the overall image acquisition burden. Additionally, smaller ROIs may promote better assessment of clinical patient images as different patient anatomies present different ROI constraints. To this end, we investigated the minimum ROI size that does not compromise the performance of the CHO model. In this study, we evaluated both simulated images and phantom CT images to identify the minimum ROI size that resulted in an accurate figure of merit (FOM) of the CHO's performance. More specifically, the minimum ROI size was evaluated as a function of the following: number of channels, spatial frequency and number of rotations of the Gabor filters, size and contrast of the object, and magnitude of the image noise. Results demonstrate that a minimum ROI size exists below which the CHO's performance is grossly inaccurate. The minimum ROI size is shown to increase with number of channels and be dictated by truncation of lower frequency filters. We developed a model to estimate the minimum ROI size as a parameterized function of the number of orientations and spatial frequencies of the Gabor filters, providing a guide for investigators to appropriately select parameters for model observer studies.

Practical implementation of Channelized Hotelling Observers: Effect of ROI size.

PubMed

Ferrero, Andrea; Favazza, Christopher P; Yu, Lifeng; Leng, Shuai; McCollough, Cynthia H

2017-03-01

Fundamental to the development and application of channelized Hotelling observer (CHO) models is the selection of the region of interest (ROI) to evaluate. For assessment of medical imaging systems, reducing the ROI size can be advantageous. Smaller ROIs enable a greater concentration of interrogable objects in a single phantom image, thereby providing more information from a set of images and reducing the overall image acquisition burden. Additionally, smaller ROIs may promote better assessment of clinical patient images as different patient anatomies present different ROI constraints. To this end, we investigated the minimum ROI size that does not compromise the performance of the CHO model. In this study, we evaluated both simulated images and phantom CT images to identify the minimum ROI size that resulted in an accurate figure of merit (FOM) of the CHO's performance. More specifically, the minimum ROI size was evaluated as a function of the following: number of channels, spatial frequency and number of rotations of the Gabor filters, size and contrast of the object, and magnitude of the image noise. Results demonstrate that a minimum ROI size exists below which the CHO's performance is grossly inaccurate. The minimum ROI size is shown to increase with number of channels and be dictated by truncation of lower frequency filters. We developed a model to estimate the minimum ROI size as a parameterized function of the number of orientations and spatial frequencies of the Gabor filters, providing a guide for investigators to appropriately select parameters for model observer studies.

Highly thermally conductive and mechanically strong graphene fibers.

PubMed

Xin, Guoqing; Yao, Tiankai; Sun, Hongtao; Scott, Spencer Michael; Shao, Dali; Wang, Gongkai; Lian, Jie

2015-09-04

Graphene, a single layer of carbon atoms bonded in a hexagonal lattice, is the thinnest, strongest, and stiffest known material and an excellent conductor of heat and electricity. However, these superior properties have yet to be realized for graphene-derived macroscopic structures such as graphene fibers. We report the fabrication of graphene fibers with high thermal and electrical conductivity and enhanced mechanical strength. The inner fiber structure consists of large-sized graphene sheets forming a highly ordered arrangement intercalated with small-sized graphene sheets filling the space and microvoids. The graphene fibers exhibit a submicrometer crystallite domain size through high-temperature treatment, achieving an enhanced thermal conductivity up to 1290 watts per meter per kelvin. The tensile strength of the graphene fiber reaches 1080 megapascals. Copyright © 2015, American Association for the Advancement of Science.

Apparently enhanced magnetization of Cu(I)-modified γ-Fe2O3 based nanoparticles

NASA Astrophysics Data System (ADS)

Qiu, Xiaoyan; He, Zhenghong; Mao, Hong; Zhang, Ting; Lin, Yueqiang; Liu, Xiaodong; Li, Decai; Meng, Xiangshen; Li, Jian

2017-11-01

Using a chemically induced transition method in FeCl2 solution, γ-Fe2O3 based magnetic nanoparticles, in which γ-Fe2O3 crystallites were coated with FeCl3ṡ6H2O, were prepared. During the synthesis of the γ-Fe2O3 nanoparticles Cu(I) modification of the particles was attempted. According to the results from both magnetization measurements and structural characterization, it was judged that a magnetic silent "dead layer", which can be attributed to spin disorder in the surface of the γ-Fe2O3 crystallites due to breaking of the crystal symmetry, existed in the unmodified particles. For the Cu(I)-modified sample, the CuCl thin layer on the γ-Fe2O3 crystallites incurred the crystal symmetry to reduce the spin disorder, which "awakened" the "dead layer" on the surface of the γ-Fe2O3 crystallites, enhancing the apparent magnetization of the Cu(I)-modified nanoparticles. It was determined that the surface spin disorder of the magnetic crystallite could be related to the coating layer on the crystallite, and can be modified by altering the coating layer to enhance the effective magnetization of the magnetic nanoparticles.

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

Biasotto, G.; Simoes, A.Z., E-mail: alezipo@yahoo.com; Foschini, C.R.

Highlights: Black-Right-Pointing-Pointer BiFeO{sub 3} (BFO) nanoparticles were grown by hydrothermal microwave method (HTMW). Black-Right-Pointing-Pointer The soaking time is effective in improving phase formation. Black-Right-Pointing-Pointer Rietveld refinement reveals an orthorhombic structure. Black-Right-Pointing-Pointer The observed magnetism of the BFO crystallites is a consequence of particle size. Black-Right-Pointing-Pointer The HTMW is a genuine technique for low temperatures and short times of synthesis. -- Abstract: Hydrothermal microwave method (HTMW) was used to synthesize crystalline bismuth ferrite (BiFeO{sub 3}) nanoparticles (BFO) in the temperature of 180 Degree-Sign C with times ranging from 5 min to 1 h. BFO nanoparticles were characterized by means of X-raymore » analyses, FT-IR, Raman spectroscopy, TG-DTA and FE-SEM. X-ray diffraction results indicated that longer soaking time was benefit to refraining the formation of any impurity phases and growing BFO crystallites into almost single-phase perovskites. Typical FT-IR spectra for BFO nanoparticles presented well defined bands, indicating a substantial short-range order in the system. TG-DTA analyses confirmed the presence of lattice OH{sup -} groups, commonly found in materials obtained by HTMW process. Compared with the conventional solid-state reaction process, submicron BFO crystallites with better homogeneity could be produced at the temperature as low as 180 Degree-Sign C. These results show that the HTMW synthesis route is rapid, cost effective, and could be used as an alternative to obtain BFO nanoparticles in the temperature of 180 Degree-Sign C for 1 h.« less

White random lasing in mixture of ZnSe, CdS and CdSSe micropowders

NASA Astrophysics Data System (ADS)

Alyamani, A. Y.; Leanenia, M. S.; Alanazi, L. M.; Aljohani, M. M.; Aljariwi, A. A.; Rzheutski, M. V.; Lutsenko, E. V.; Yablonskii, G. P.

2016-03-01

Room temperature random lasing with white light emission in a mixture of AIIBVI semiconductor powders was achieved for the first time. The scattering gain media was formed by the mixture of closely packed active micron sized crystallites of ZnSe, CdS, CdSSe semiconductors. The micropowders were produced by grinding bulk crystals of each compound. Optical excitation was performed by 10-nanosecond pulses of tuned Ti:Al2O3-laser at 390 nm. The lasing in the mixture of semiconductor powders was achieved simultaneously at four wavelengths in blue, green, yellow and red spectral regions after exceeding the threshold excitation power density. A drastic integral intensity increase, spectrum narrowing and appearance of mode structure accompanied the laser action. ZnSe crystallites produce the laser light at about 460 nm while CdS particles - at about 520 nm. Two types of CdSSe semiconductor micropowders with different sulfur content lase at 580 nm and 660 nm. The threshold excitation power densities for all laser lines in the emission spectrum are approximately the same of about 0.9 MW/cm2. The sum of the emission spectrum of the mixture of the micropowders forms white light with high brightness. Lasing is due to an appearance of random feedback for amplified radiation in the active medium of closely packed light scattering crystallites. The presented results may find their applications for visualization systems, lighting technology, data transmission, medicine as biosensors and in identification systems. The key feature of random lasers is low cost of its production and possibility to be deposited on any type of surface.

High T(sub c) superconductors fabricated by plasma aerosol mist deposition technique

NASA Technical Reports Server (NTRS)

Wang, X. W.; Vuong, K. D.; Leone, A.; Shen, C. Q.; Williams, J.; Coy, M.

1995-01-01

We report new results on high T(sub c) superconductors fabricated by a plasma aerosol mist deposition technique, in atmospheric environment. Materials fabricated are YBaCuO, BiPbSrCaCuO, BaCaCuO precursor films for TlBaCaCuO, and other buffers such as YSZ. Depending on processing conditions, sizes of crystallites and/or particles are between dozens of nano-meters and several micrometers. Superconductive properties and other material characteristics can also be tailored.

Nanomorphology Characteristics of Thermally Annealed Pre Encapsulated P3HT:PCBM Thin Films Using Atomic Force Microscopy

DTIC Science & Technology

2014-10-30

fib- rils aggregate in bundles with the fullerene as the anneal- ing temperature increases. This bundle formation or grain features could indicate a...the diffusion lengths of charge carriers (∼10 nm). Past work on these fullerene networks have shown that trap distribution in devices is broader for...aver- age distance between polymer and fullerene molecules. The size of crystallites perhaps reach an upper limit in the range of 150 "C; beyond this

Quantification of Changes in Mulberry Silk Fabrics due to Different Laundering: Using WAXS Technique

NASA Astrophysics Data System (ADS)

Parameswara, P.; Nivedita, S.; Somashekar, R.

2011-07-01

Loom finished mulberry silk fabrics (Taffeta) were machine laundered and hand laundered several times. X-ray diffractograms of pure and laundered fabrics were used to calculate microstructural parameters like average crystallite size (D) and lattice strain (Vegr) employing Williamson-Hall plot. Microstructural parameters were compared with measured mechanical properties like breaking load, tenacity, and elongation of warp yarns unraveled from fabrics. Surface morphology and texture of silk fabrics changed upon washing is evident from SEM images.

Rietveld analysis of the cubic crystal structure of Na-stabilized zirconia

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

Fagherazzi, G.; Canton, P.; Benedetti, A.

Using x-ray Rietveld analysis the fcc (fluorite-type) structure of a Na-containing nanocrystalline zirconia powder (9.5 nm estimated of crystallite size) obtained by precipitation and subsequent calcination has been confirmed. The result shows that using conventional x-ray diffraction techniques the cubic crystallographic form of ZrO{sub 2} from the tetragonal one in nanosized powders. These conclusions are supported by the findings of independent Raman scattering experiments. {copyright} {ital 1997 Materials Research Society.}

Structural and spectroscopic study of mechanically synthesized SnO2 nanostructures

NASA Astrophysics Data System (ADS)

Vij, Ankush; Kumar, Ravi

2016-05-01

We report the single step synthesis of SnO2 nanostructures using high energy mechanical attrition method. X-ray diffraction (XRD) pattern reveals the single phase rutile structure with appreciable broadening of diffraction peaks, which is a signature of nanostructure formation. The average crystallite size of SnO2 nanostructures has been calculated to be ~15 nm. The micro-Raman study reveals the shifting of A1g Raman mode towards lower wave number, which is correlated with the nanostructure formation.

Thermophysical and structural studies on some glass-ceramics and role of nano size crystallites

NASA Astrophysics Data System (ADS)

Kothiyal, G. P.; Arvind, A.; Kumar, Rakesh; Dixit, Anupam; Sharma, Kuldeep; Goswami, Madhumita

2009-07-01

In this paper, we present some studies on structure and thermophysical properties of glass and glass-ceramics with possible bio-medical and sealing applications. The glass-ceramics prepared for bio-medical applications include phosphate as well as silico-phosphate compositions. In vitro bio-compatibility/activity of these materials is discussed. The glass-ceramics used for the sealing application are lithium aluminium silicate (LAS) and lithium zinc silicate (LZS). The phase formation and some aspects of thermophysical properties and sealing are discussed.

Effect of annealing on particle size, microstructure and gas sensing properties of Mn substituted CoFe2O4 nanoparticles

NASA Astrophysics Data System (ADS)

Kumar, E. Ranjith; Kamzin, A. S.; Janani, K.

2016-11-01

Microstructure, morphological and gas sensor studies of Mn substituted cobalt ferrite nanoparticles synthesized by a simple evaporation method and auto- combustion method. The influence of heat treatment on phase and particle size of spinel ferrite nanoparticles were determined by X-ray diffraction and Mossbauer spectroscopy. The XRD study reveals that the lattice constant and crystallite size of the samples increases with the increase of annealing temperature. Last one was confirmed by Mossbauer data. The lowest size of particles of MnCoFe2O4 (~3 nm) is obtained by auto combustion method. The spherical shaped nanoparticles are recorded by TEM. Furthermore, conductance response of Mn-Co ferrite nanomaterial was measured by exposing the material to reducing gas like liquefied petroleum gas (LPG) which showed a sensor response of ~0.19 at an optimum operating temperature of 250 °C.

Optimization of the behavior of CTAB coated cobalt ferrite nanoparticles

NASA Astrophysics Data System (ADS)

Kumari, Mukesh; Bhatnagar, Mukesh Chander

2018-05-01

In this work, we have synthesized cetyltrimethyl ammonium bromide (CTAB) mixed cobalt ferrite (CoFe2O4) nanoparticles (NPs) using sol-gel auto-combustion method taking a different weight percent ratio of CTAB i.e., 0%, 1%, 2%, 3% and 4% with respect to metal nitrates. The morphological, structural and magnetic properties of these NPs are characterized by high resolution transmitted electron microscopy (HRTEM), X-ray diffraction (XRD), Raman spectrometer and physical property measurement system (PPMS). It has been found that saturation magnetization of cobalt ferrite increases with increase in crystalline size of the NPs. Saturation magnetization and crystallite size both were found to be lowest in the case of sample containing 2% CTAB.

Morphological characteristics of mechanochemically synthesized Fe/Ti composites

NASA Astrophysics Data System (ADS)

Grigor'eva, T. F.; Kovaleva, S. A.; Kiseleva, T. Yu.; Vosmerikov, S. V.; Devyatkina, E. T.; Pastukhov, E. A.; Lyakhov, N. Z.

2016-08-01

The joint mechanical activation of chemically interacting iron and titanium has been studied by X-ray diffraction and atomic force microscopy. It is shown that chemically interacting metals Fe and Ti do not form any intermetallic compounds or solid solutions upon intense mechanical activation in a high-energy planetary mill. The products of mechanical activation are Fe/Ti mechanocomposites, in which titanium is distributed over the iron grain surface. An increase in the mechanical activation time leads to the agglomeration of powders and the formation of particles with a wide size range (5-25 μm). The iron crystallite sizes and the level of microstresses are reduced, indicating a decrease in the particle strength.

Environment friendly route of iron oxide nanoparticles from Zingiber officinale (ginger) root extract

NASA Astrophysics Data System (ADS)

Xin Hui, Yau; Yi Peng, Teoh; Wei Wen, Liu; Zhong Xian, Ooi; Peck Loo, Kiew

2016-11-01

Iron oxide nanoparticles were prepared from the reaction between the Zingiber officinale (ginger) root extracts and ferric chloride solution at 50°C for 2 h in mild stirring condition. The synthesized powder forms of nanoparticles were further characterized by using UV-Vis spectroscopy and X-ray Diffraction spectrometry. UV-Vis analysis shows the absorption peak of iron oxide nanoparticles is appeared at 370 nm. The calculation of crystallite size from the XRD showed that the average particle size of iron oxide nanoparticles was 68.43 nm. Therefore, this eco-friendly technique is low cost and large scale nanoparticles synthesis to fulfill the demand of various applications.

Conductivity dependence of lithium diffusivity and electrochemical performance for electrospun TiO2 fibers

NASA Astrophysics Data System (ADS)

Qing, Rui; Liu, Li; Bohling, Christian; Sigmund, Wolfgang

2015-01-01

TiO2 is one of the most exciting anode candidates for safe application in lithium ion batteries. However, its low intrinsic electronic conductivity limits application. In this paper, a simple sol-gel based route is presented to produce nanosize TiO2 fibers with 119 ± 27 nm diameters via electrospinning. Subsequent calcination in various atmospheres was applied to achieve anatase and anatase-rutile mixed phase crystallites with and without carbon coating. The crystallite size was 5 nm for argon calcined fibers and 13-20 nm for air calcined fibers. Argon calcined TiO2 nanofibers exhibited electronic conductivity orders of magnitude higher than those of air-calcined samples. Lithium diffusivity was increased by one time and specific capacity by 26.9% due to the enhanced conductivity. It also had a different intercalation mechanism of lithium. Hydrogen post heat-treatment was found to benefit electronic conductivity (by 3-4.5 times), lithium diffusivity (1.5-2 times) and consequently the high rate performance of the TiO2 nanofibers (over 80%). The inner mechanism and structure-property relations among these parameters were also discussed.

Optical and Morphological Properties of P3HT and P3HT: PCBM Thin Films Used in Photovoltaic Applications

NASA Astrophysics Data System (ADS)

Hrostea, L.; Girtan, M.; Mallet, R.; Leontie, L.

2018-06-01

This work is focused on the study of some physical properties of poly(3-hexylthiophene-2,5-diyl) (P3HT) and poly(e-hexylthiophene-2,5-diyl): Methanolfullerene Phenyl-C61-Butyric-Accid-Methyl-Ester (PCBM) blend thin films. Knowing the polymer advantages, such as ease of processing, high thermal stability, strong interaction with light, its properties have captured the attention regarding the changes that can occur in a polymer:fullerene blend in term of them. Polymer and polymer:fullerene blend (1:0.1, 1:0.2, 1:0.4 and 1:0.8 ratios) were deposited by spin coating on glass and SnO2:F (FTO) coated glass. The optical properties were emphasized using spectrophotometry (300 – 2200 nm wavelength range) and spectroscopic ellipsometry models, to obtain the refractive index, extinction coefficient and the transmission (found higher than 80%). According to X-ray diffraction analysis, as-obtained films are amorphous. Investigation of the surface morphology of thin-film samples using Atomic Force Microscopy revealed a crystallite-like surface morphology with crystallite size in the nanometer range.

Features of structural changes in the near-surface aluminum layer under various schemes of ion implantation

NASA Astrophysics Data System (ADS)

Kryzhevich, Dmitrij S.; Zolnikov, Konstantin P.; Korchuganov, Aleksandr V.

2017-10-01

The molecular dynamics simulation of structural rearrangements in the surface layer of aluminum samples under ion implantation of various intensities was carried out. The features of the internal structure and the crystallographic orientation of the irradiated crystallite were taken into account. To describe the interatomic interaction many-body potentials obtained in the framework of the embedded atom method were used. Irradiation of the {100} surface results in much less number of formed defects than irradiation of the {110} and {111} ones. When irradiating surfaces with beams of relatively low energy grains remain unchanged in the surface region and the formation of stacking faults was not observed. At a high intensity of irradiation, the near-surface layer of the crystallite melts. In the absence of heat removal, the centers of crystallization become grains lying on the boundary of the solid and liquid phases. Those grains increase due to the adjustment of the atoms of the liquid phase to their lattice. As a result, the grain size in the near-surface region increases.

One-step synthesis and characterizations of cerium oxide nanoparticles in an ambient temperature via Co-precipitation method

NASA Astrophysics Data System (ADS)

Pujar, Malatesh S.; Hunagund, Shirajahammad M.; Desai, Vani R.; Patil, Shivaprasadgouda; Sidarai, Ashok H.

2018-04-01

We report the simple Co-precipitation method for the synthesis of Cerium oxide (CeO2) nanoparticles (NPs) in an ambient temperature. We have taken the Cerium (III) nitrate hexahydrate (Ce(NO3)3.6H2O) and Sodium hydroxide (NaOH) as the precursors. The obtained NPs were analyzed using the UV-Vis spectrophotometer, Fourier transform infrared spectroscopy (FT-IR) and X-ray diffraction (XRD). The obtained results signify that UV-Vis spectrum exhibited a well-defined absorption peak at 274 nm and the estimated energy gap (Eg) is 4.05 eV. The FT-IR analysis provides the supporting evidence for the presence of bonding of O-H, nitrates, alcohols and O-Ce-O vibrations. The XRD result reveals that the synthesized CeO2 NPs was crystallite with cubic phase structure and the estimated average crystallite size of CeO2 NPs using Scherer's and W-H method was significantly different due to their assumptions. Further, it is purposed to study their photocatalytic biological activities.

Structural and magnetic properties of Ni1-xZnxFe2O4 synthesized through the sol-gel method

NASA Astrophysics Data System (ADS)

Guan, Beh Hoe; Zahari, Muhammad Hanif; Chuan, Lee Kean

2016-11-01

Modification of crystal structure by means of substitution would result in the modification of the overall physical properties of crystallite materials especially in ferrites. This study aims to investigate the effect of non-magnetic Zn substitution in spinel NiFe2O4 and its direct effect towards its microstructural and magnetic properties. Magnetic nanoparticles of Nickel-Zinc ferrite with the chemical formula, Ni1-xZnxFe2O4 (x=0.00, 0.25, 0.50, 0.75) were synthesized through the sol-gel route. Phase formation and structural properties of the synthesized ferrite were identified through X-ray diffraction (XRD) analysis and transmission electron microscopy (TEM). Magnetic properties such as the magnetic saturation, coercivity and remanence were measured by a vibrating sample magnetometer (VSM). XRD measurements reveals successful synthesis of single-phased Nickel ferrite and Nickel—Zinc ferrite. Both crystallite and grain size shows fluctuation with increasing Zn content. The ferrites were found to be ferrimagnetic in nature and show differing values with different x values.

Molecular weight dependent structure and charge transport in MAPLE-deposited poly(3-hexylthiophene) thin films

DOE PAGES

Dong, Ban Xuan; Smith, Mitchell; Strzalka, Joseph; ...

2018-02-06

In this work, poly(3-hexylthiophene) (P3HT) films prepared using the matrix-assisted pulsed laser evaporation (MAPLE) technique are shown to possess morphological structures that are dependent on molecular weight (MW). Specifically, the structures of low MW samples of MAPLE-deposited film are composed of crystallites/aggregates embedded within highly disordered environments, whereas those of high MW samples are composed of aggregated domains connected by long polymer chains. Additionally, the crystallite size along the side-chain (100) direction decreases, whereas the conjugation length increases with increasing molecular weight. This is qualitatively similar to the structure of spin-cast films, though the MAPLE-deposited films are more disordered. In-planemore » carrier mobilities in the MAPLE-deposited samples increase with MW, consistent with the notion that longer chains bridge adjacent aggregated domains thereby facilitating more effective charge transport. The carrier mobilities in the MAPLE-deposited simples are consistently lower than those in the solvent-cast samples for all molecular weights, consistent with the shorter conjugation length in samples prepared by this deposition technique.« less

Molecular weight dependent structure and charge transport in MAPLE-deposited poly(3-hexylthiophene) thin films

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

Dong, Ban Xuan; Smith, Mitchell; Strzalka, Joseph

In this work, poly(3-hexylthiophene) (P3HT) films prepared using the matrix-assisted pulsed laser evaporation (MAPLE) technique are shown to possess morphological structures that are dependent on molecular weight (MW). Specifically, the structures of low MW samples of MAPLE-deposited film are composed of crystallites/aggregates embedded within highly disordered environments, whereas those of high MW samples are composed of aggregated domains connected by long polymer chains. Additionally, the crystallite size along the side-chain (100) direction decreases, whereas the conjugation length increases with increasing molecular weight. This is qualitatively similar to the structure of spin-cast films, though the MAPLE-deposited films are more disordered. In-planemore » carrier mobilities in the MAPLE-deposited samples increase with MW, consistent with the notion that longer chains bridge adjacent aggregated domains thereby facilitating more effective charge transport. The carrier mobilities in the MAPLE-deposited simples are consistently lower than those in the solvent-cast samples for all molecular weights, consistent with the shorter conjugation length in samples prepared by this deposition technique.« less

Microstructure evolution of Al-doped zinc oxide films prepared by in-line reactive mid-frequency magnetron sputtering

NASA Astrophysics Data System (ADS)

Hong, R. J.; Jiang, X.

2006-07-01

Aluminium-doped zinc oxide (ZnO:Al or AZO) thin films were deposited on glass substrates by reactive mid-frequency (MF) magnetron sputtering from Zn/Al metallic targets. Strong (002) preferred orientation was detected by X-ray diffraction (XRD). It was observed by plan-view transmission electron microscopy (TEM) that an AZO film deposited at low substrate temperature was composed of irregular large grains; but the film prepared at high temperature was composed of moderate sized grains with a regular shape. A secondary phase of ZnO2 was also observed for the film deposited at low substrate temperature. The cross-sectional TEM study of the AZO film showed that prior to the well-aligned columnar growth an initial interfacial zone with nano crystallites were formed. The nano crystallites formed initially with a large tilt angle normal to the substrate surface and during the growth of the transition zone, the tilt angle decreased until it vanished. The evolution of the film structure is discussed in terms of evolutionary selection model and the dynamic deposition process.

Novel Synthesis and Structural Analysis of Ferrihydrite

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

Smith, Stacey J.; Page, Katharine; Kim, Hyunjeong

2012-07-25

Naturally occurring ferrihydrite is both impure and difficult to isolate, so the numerous applications and interesting properties of ferrihydrite have spurred the development of various synthetic techniques. Nearly all techniques are based on the hydrolysis of an iron salt and require careful control of temperature, pH, and concentration. In this Article, we report a new synthetic method which does not require such control and is perhaps the fastest and simplest route to synthesizing ferrhydrite. XRD, TEM, BET, and chemical purity characterizations show that the chemically pure, 2-line ferrihydrite product consists of crystallites 2-6 nm in diameter which aggregate to formmore » mesoporous, high surface area agglomerates that are attractive candidates for the many adsorption applications of ferrihydrite. X-ray PDF data were also collected for the ferrihydrite product and refined against the hexagonal structural model recently proposed by Michel et al. These analyses suggest that ferrihydrite has a consistent, repeatable structure independent of variation in the synthetic method, water content of the sample, or particle size of the crystallites, and this structure can be adequately described by the proposed hexagonal model.« less

Study of drying process on starch structural properties and their effect on semolina pasta sensory quality.

PubMed

Padalino, Lucia; Caliandro, Rocco; Chita, Giuseppe; Conte, Amalia; Del Nobile, Matteo Alessandro

2016-11-20

The influence of drying temperature on the starch crystallites and its impact on durum wheat pasta sensory properties is addressed in this work. In particular, spaghetti were produced by means of a pilot plant using 5 different drying temperature profiles. The sensory properties, as well as the cooking quality of pasta were assessed. X-ray powder diffraction was used for investigating changes in the crystallinity content of the samples. Starch crystallinity, size and density of the starch crystallites were determined from the analysis of the diffraction profiles. As expected, spaghetti sensory properties improved as the drying temperatures increased. In particular, attributes as resistance to break for uncooked samples and firmness, elasticity, bulkiness and stickiness for cooked samples, all benefit from drying temperature increase. The spaghetti cooking quality was also positively affected by the drying temperature increase. Diffraction analysis suggested that the improvement of sensory properties and cooking quality of pasta were directly related to the increase in density of both physical crosslink of starch granules and chemical crosslink of protein matrix. Copyright © 2016 Elsevier Ltd. All rights reserved.

Novel synthesis and structural analysis of ferrihydrite.

PubMed

Smith, Stacey J; Page, Katharine; Kim, Hyunjeong; Campbell, Branton J; Boerio-Goates, Juliana; Woodfield, Brian F

2012-06-04

Naturally occurring ferrihydrite is both impure and difficult to isolate, so the numerous applications and interesting properties of ferrihydrite have spurred the development of various synthetic techniques. Nearly all techniques are based on the hydrolysis of an iron salt and require careful control of temperature, pH, and concentration. In this Article, we report a new synthetic method which does not require such control and is perhaps the fastest and simplest route to synthesizing ferrhydrite. XRD, TEM, BET, and chemical purity characterizations show that the chemically pure, 2-line ferrihydrite product consists of crystallites 2-6 nm in diameter which aggregate to form mesoporous, high surface area agglomerates that are attractive candidates for the many adsorption applications of ferrihydrite. X-ray PDF data were also collected for the ferrihydrite product and refined against the hexagonal structural model recently proposed by Michel et al. These analyses suggest that ferrihydrite has a consistent, repeatable structure independent of variation in the synthetic method, water content of the sample, or particle size of the crystallites, and this structure can be adequately described by the proposed hexagonal model.

Biomineralization: Some complex crystallite-oriented skeletal structures.

PubMed

Sahni, Ashok

2013-12-01

The present review focuses on some specific aspects of biomineralization with regard to the evolution of the first focused visioning systems in trilobites, the formation of molluscan shell architecture, dental enamel and its biomechanical properties and the structure of the calcified amniote egg, both fossil and recent. As an interdisciplinary field, biomineralization deals with the formation, structure and mechanical strength of mineralized skeletonized tissue secreted by organisms. Mineral matter formed in this way occurs in all three domains of life and consists of several mineral varieties, of which carbonates, phosphates and opaline silica are the most common. Animals and plants need mechanical support to counteract gravitational forces on land and hydrostatic pressure in the deep ocean, which is provided by a skeletonized framework. Skeleton architecture mainly consists of basic elements represented by small usually micrometer- to nanometer-sized crystallites of calcite and aragonite for carbonate systems and apatite crystallites for phosphatic ones, and then these building blocks develop into structured more complex frameworks. As selective pressures work towards optimizing stress and response, the orientation, morphology and structural arrangement of the crystallites indicates the distribution of the stress field of the biomineralized tissue. Large animals such as the dinosaurs have to deal with large gravitational forces, but in much smaller skeletonized organism such as the coccoliths, a few micrometer in diameter made up of even smaller individual crystallites, van der Waals forces play an increasingly important role and are at present poorly understood. Skeleton formation is dependent upon many factors including ambient water chemistry, temperature and environment. Ocean chemistry has played a vital role in the origins of skeletonization, 500 to 600 million years (ma) ago with the dominance of calcium carbonate as the principal skeleton-forming tissue and with phosphates and silica as important but secondary materials. The preservation of calcareous skeletons in deep time has resulted in providing interesting information: for example, the number of days in the Devonian year has been established on the basis of well-preserved lunar (annual) cycles, and isotope chemistry has led to an elaborate protocol for using O18/O16 stable isotopes for palaeotemperature measurements in the geological past. Stable isotopes of dental apatite have helped to establish ecological shifts (terrestrial to wholly marine) during the evolution of the Cetacea. Biomineralization as a field of specialization is still searching for its own independent identity, but gradually, its importance is being realized as a model for engineering applications especially at the nanometer scale.

24 CFR 984.105 - Minimum program size.

Code of Federal Regulations, 2010 CFR

2010-04-01

... DEVELOPMENT SECTION 8 AND PUBLIC HOUSING FAMILY SELF-SUFFICIENCY PROGRAM General § 984.105 Minimum program... 24 Housing and Urban Development 4 2010-04-01 2010-04-01 false Minimum program size. 984.105 Section 984.105 Housing and Urban Development Regulations Relating to Housing and Urban Development...

Practical implementation of Channelized Hotelling Observers: Effect of ROI size

PubMed Central

Yu, Lifeng; Leng, Shuai; McCollough, Cynthia H.

2017-01-01

Fundamental to the development and application of channelized Hotelling observer (CHO) models is the selection of the region of interest (ROI) to evaluate. For assessment of medical imaging systems, reducing the ROI size can be advantageous. Smaller ROIs enable a greater concentration of interrogable objects in a single phantom image, thereby providing more information from a set of images and reducing the overall image acquisition burden. Additionally, smaller ROIs may promote better assessment of clinical patient images as different patient anatomies present different ROI constraints. To this end, we investigated the minimum ROI size that does not compromise the performance of the CHO model. In this study, we evaluated both simulated images and phantom CT images to identify the minimum ROI size that resulted in an accurate figure of merit (FOM) of the CHO’s performance. More specifically, the minimum ROI size was evaluated as a function of the following: number of channels, spatial frequency and number of rotations of the Gabor filters, size and contrast of the object, and magnitude of the image noise. Results demonstrate that a minimum ROI size exists below which the CHO’s performance is grossly inaccurate. The minimum ROI size is shown to increase with number of channels and be dictated by truncation of lower frequency filters. We developed a model to estimate the minimum ROI size as a parameterized function of the number of orientations and spatial frequencies of the Gabor filters, providing a guide for investigators to appropriately select parameters for model observer studies. PMID:28943699

β-Irradiation Effects on the Formation and Stability of CaMoO4 in a Soda Lime Borosilicate Glass Ceramic for Nuclear Waste Storage.

PubMed

Patel, Karishma B; Boizot, Bruno; Facq, Sébastien P; Lampronti, Giulio I; Peuget, Sylvain; Schuller, Sophie; Farnan, Ian

2017-02-06

Molybdenum solubility is a limiting factor to actinide loading in nuclear waste glasses, as it initiates the formation of water-soluble crystalline phases such as alkali molybdates. To increase waste loading efficiency, alternative glass ceramic structures are sought that prove resistant to internal radiation resulting from radioisotope decay. In this study, selective formation of water-durable CaMoO 4 in a soda lime borosilicate is achieved by introducing up to 10 mol % MoO 3 in a 1:1 ratio to CaO using a sintering process. The resulting homogeneously dispersed spherical CaMoO 4 nanocrystallites were analyzed using electron microscopy, X-ray diffraction (XRD), Raman and electron paramagnetic resonance (EPR) spectroscopies prior to and post irradiation, which replicated internal β-irradiation damage on an accelerated scale. Following 0.77 to 1.34 GGy of 2.5 MeV electron radiation CaMoO 4 does not exhibit amorphization or significant transformation. Nor does irradiation induce glass-in-glass phase separation in the surrounding amorphous matrix, or the precipitation of other molybdates, thus proving that excess molybdenum can be successfully incorporated into a structure that it is resistant to β-irradiation proportional to 1000 years of storage without water-soluble byproducts. The CaMoO 4 crystallites do however exhibit a nonlinear Scherrer crystallite size pattern with dose, as determined by a Rietveld refinement of XRD patterns and an alteration in crystal quality as deduced by anisotropic peak changes in both XRD and Raman spectroscopy. Radiation-induced modifications in the CaMoO 4 tetragonal unit cell occurred primarily along the c-axis indicating relaxation of stacked calcium polyhedra. Concurrently, a strong reduction of Mo 6+ to Mo 5+ during irradiation is observed by EPR, which is believed to enhance Ca mobility. These combined results are used to hypothesize a crystallite size alteration model based on a combination of relaxation and diffusion-based processes initiated by added energy from β-impingement and second-order structural modifications induced by defect accumulation.

Basic molten salt process-A new route for synthesis of nanocrystalline Li 4Ti 5O 12-TiO 2 anode material for Li-ion batteries using eutectic mixture of LiNO 3-LiOH-Li 2O 2

NASA Astrophysics Data System (ADS)

Rahman, M. M.; Wang, Jia-Zhao; Hassan, Mohd Faiz; Chou, Shulei; Wexler, David; Liu, Hua-Kun

A nanocrystalline Li 4Ti 5O 12-TiO 2 duplex phase has been synthesized by a simple basic molten salt process (BMSP) using an eutectic mixture of LiNO 3-LiOH-Li 2O 2 at 400-500 °C. The microstructure and morphology of the Li 4Ti 5O 12-TiO 2 product are characterized by means of X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), and transmission electron microscopy (TEM). The sample prepared by heat-treating at 300 °C for 3 h (S-1) reveals dense agglomerates of ultra-fine nanocrystalline Li 4Ti 5O 12; with heat treatment at 400 °C for 3 h (S-2), there is a duplex crystallite size (fine < 10 nm, and coarse > 20 nm) of Li 4Ti 5O 12-TiO 2; at 500 °C for 3 h (S-3), a much coarser and less-dense distribution of lithium titanate (crystallite size ∼15-30 nm) is observed. According to the results of electrochemical testing, the S-2 sample shows initial discharge capacities of 193 mAh g -1 at 0.2 C, 168 mAh g -1 at 0.5 C, 146 mAh g -1 at 1 C, 135 mAh g -1 at 2 C, and 117 mAh g -1 at 5 C. After 100 cycles, the discharge capacity is 138 mAh g -1 at 1 C with a capacity retention of 95%. The S-2 sample yields the best electrochemical performance in terms of charge-discharge capacity and rate capability compared with other samples. Its superior electrochemical performance can be mainly attributed to the duplex crystallite structure, composed of fine (<10 nm) and coarse (>20) nm nanoparticles, where lithium ions can be stored within the grain boundary interfaces between the spinel Li 4Ti 5O 12 and the anatase TiO 2.

Microstructural evolution and thermal stability of Fe-Zr metastable alloys developed by mechanical alloying followed by annealing

NASA Astrophysics Data System (ADS)

Sooraj, S.; Muthaiah, V. M. Suntharavel; Kang, P. C.; Koch, Carl C.; Mula, Suhrit

2016-09-01

The effect of Zr (up to 1 at.%) addition on the formation of Fe-Zr metastable alloys and their thermal stability were investigated for their possible nuclear applications. Fe-xZr (x = 0.25, 0.5, 1%) alloys were synthesised by mechanical alloying under a high-purity argon atmosphere using stainless steel grinding media in a SPEX 8000M high energy mill. The milling was conducted for 20 h with a ball-to-powder weight ratio of 10:1. The formation of metastable solid solutions after milling was confirmed from the change in the Gibbs free energy analysis as per Miedema's model. The microstructural characterisation was carried out by analysis of X-ray diffraction, atomic force microscopy and transmission electron microscopy. The effect of Zr on the thermal stability of Fe-Zr alloys was investigated by extensive annealing experiments followed by microstructural analysis and microhardness measurements. The stabilisation was found to occur at 800 °C and thereafter, no significant change in the crystallite size was observed for the samples annealed between 800 and 1200 °C. The supersaturated solid solution, especially 1% Zr alloy, found to be highly stable up to 800 °C and the microhardness value of the same measured to be as high as 8.8 GPa corresponding to a crystallite size of 57 nm. The stabilisation effect has been discussed in the light of both the thermodynamic and kinetic mechanisms and the grain size stabilisation is attributed to the grain boundary segregation of Zr atoms and/or Zener pinning by nanoscale precipitation of the Fe2Zr phase.

Preparation of highly ordered mesoporous Al2O3/TiO2 and its application in dye-sensitized solar cells.

PubMed

Kim, Jae-Yup; Kang, Soon Hyung; Kim, Hyun Sik; Sung, Yung-Eun

2010-02-16

Highly ordered mesoporous Al(2)O(3)/TiO(2) was prepared by sol-gel reaction and evaporation-induced self-assembly (EISA) for use in dye-sensitized solar cells. The prepared materials had two-dimensional, hexagonal pore structures with anatase crystalline phases. The average pore size of mesoporous Al(2)O(3)/TiO(2) remained uniform and in the range of 6.33-6.58 nm while the Brunauer-Emmett-Teller (BET) surface area varied from 181 to 212 m(2)/g with increasing the content of Al(2)O(3). The incorporation of Al content retarded crystallite growth, thereby decreasing crystallite size while simultaneously improving the uniformity of pore size and volume. The thin Al(2)O(3) layer was located mostly on the mesopore surface, as confirmed by X-ray photoelectron spectroscopy (XPS). The Al(2)O(3) coating on the mesoporous TiO(2) film contributes to the essential energy barrier which blocks the charge recombination process in dye-sensitized solar cells. Mesoporous Al(2)O(3)/TiO(2) (1 mol % Al(2)O(3)) exhibited enhanced power conversion efficiency (V(oc) = 0.74 V, J(sc) = 15.31 mA/cm(2), fill factor = 57%, efficiency = 6.50%) compared to pure mesoporous TiO(2) (V(oc) = 0.72 V, J(sc) = 16.03 mA/cm(2), fill factor = 51%, efficiency = 5.88%). Therefore, the power conversion efficiency was improved by approximately 10.5%. In particular, the increase in V(oc) and fill factor resulted from the inhibition of charge recombination and the improvement of pore structure.

Phase Competition Induced Bio-Electrochemical Resistance and Bio-Compatibility Effect in Nanocrystalline Zr x -Cu100-x Thin Films.

PubMed

Badhirappan, Geetha Priyadarshini; Nallasivam, Vignesh; Varadarajan, Madhuri; Leobeemrao, Vasantha Priya; Bose, Sivakumar; Venugopal, Elakkiya; Rajendran, Selvakumar; Angleo, Peter Chrysologue

2018-07-01

Nano-crystalline Zrx-Cu100-x (x = 20-100 at.%) thin films with thickness ranging from 50 to 185 nm were deposited by magnetron co-sputtering with individual Zr and Cu targets. The as-sputtered thin films were characterized by Field Emission Scanning Electron Microscope (FE-SEM), Atomic Force Microscopy (AFM) and Glancing Incidence X-ray Diffraction (GIXRD) for structural and morphological properties. The crystallite size was found to decrease from 57 nm to 37 nm upon increasing the Zr content from 20 to 30 at.% with slight increase in the lattice strain from 0.17 to 0.33%. Further, increase in Zr content to 40 at.% leads to increase in the crystallite size to 57 nm due to stabilization of C10Zr7 phase along with the presence of nanocrystalline Cu-Zr phase. A bimodal distribution of grain size was observed from FE-SEM micrograph was attributed to the highest surface roughness in Zr30Cu70 thin films comprised of Cu10Zr7, Cu9Zr2, Cu-Zr intermetallic phases. In-vitro electrochemical behaviors of nano-crystalline Zrx-Cu100-x thin films in simulated body fluid (SBF) were investigated using potentiodynamic polarization studies. Electrochemical impedance spectroscopy (EIS) data fitting by equivalent electrical circuit fit model suggests that inner bulk layer contributes to high bio-corrosion resistance in Zrx-Cu100-x thin films with increase in Zr content. The results of cyto-compatibility assay suggested that Zr-Cu thin film did not introduce cytotoxicity to osteoblast cells, indicating its suitability as a bio-coating for minimally invasive medical devices.

Role of Cu in engineering the optical properties of SnO2 nanostructures: Structural, morphological and spectroscopic studies

NASA Astrophysics Data System (ADS)

Kumar, Virender; Singh, Kulwinder; Jain, Megha; Manju; Kumar, Akshay; Sharma, Jeewan; Vij, Ankush; Thakur, Anup

2018-06-01

We have carried out a systematic study to investigate the effect of Cu doping on the optical properties of SnO2 nanostructures synthesized by chemical route. Synthesized nanostructures were characterized using X-ray diffraction (XRD), Field emission scanning electron microscopy (FE-SEM), High resolution transmission electron microscopy (HR-TEM), Energy dispersive X-ray spectroscopy, Raman spectroscopy, Fourier transform infrared (FTIR) spectroscopy, UV-visible and Photoluminescence (PL) spectroscopy. The Rietveld refinement analysis of XRD patterns of Cu-doped SnO2 samples confirmed the formation of single phase tetragonal rutile structure, however some localized distortion was observed for 5 mol% Cu-doped SnO2. Crystallite size was found to decrease with increase in dopant concentration. FE-SEM images indicated change in morphology of samples with doping. HR-TEM images revealed that synthesized nanostructures were nearly spherical and average crystallite size was in the range 12-21 nm. Structural defects, crystallinity and size effects on doping were investigated by Raman spectroscopy and results were complemented by FTIR spectroscopy. Optical band gap of samples was estimated from reflectance spectra. We have shown that band gap of SnO2 can be engineered from 3.62 to 3.82 eV by Cu doping. PL emission intensity increased as the doping concentration increased, which can be attributed to the development of defect states in the forbidden transition region of band gap of SnO2 with doping. We have also proposed a band model owing to defect states in SnO2 to explain the observed PL in Cu doped SnO2 nanostructures.

Polarization Catastrophe Contributing to Rotation and Tornadic Motion in Cumulo-Nimbus Clouds

NASA Astrophysics Data System (ADS)

Handel, P. H.

2007-05-01

When the concentration of sub-micron ice particles in a cloud exceeds 2.5E21 per cubic cm, divided by the squared average number of water molecules per crystallite, the polarization catastrophe occurs. Then all ice crystallites nucleated on aerosol dust particles align their dipole moments in the same direction, and a large polarization vector field is generated in the cloud. Often this vector field has a radial component directed away from the vertical axis of the cloud. It is induced by the pre-existing electric field caused by the charged screening layers at the cloud surface, the screening shell of the cloud. The presence of a vertical component of the magnetic field of the earth creates a density of linear momentum G=DxB in the azimuthal direction, where D=eE+P is the electric displacement vector and e is the vacuum permittivity. This linear momentum density yields an angular momentum density vector directed upward in the nordic hemisphere, if the polarization vector points away from the vertical axis of the cloud. When the cloud becomes colloidally unstable, the crystallites grow beyond the size limit at which they still could carry a large ferroelectric saturation dipole moment, and the polarization vector quickly disappears. Then the cloud begins to rotate with an angular momentum that has the same direction. Due to the large average number of water molecules in a crystallite, the polarization catastrophe (PC) is present in practically all clouds, and is compensated by masking charges. In cumulo-nimbus (thunder-) clouds the collapse of the PC is rapid, and the masking charges lead to lightning, and in the upper atmosphere also to sprites, elves, and blue jets. In stratus clouds, however, the collapse is slow, and only leads to reverse polarity in dissipating clouds (minus on the bottom), as compared with growing clouds (plus on the bottom, because of the excess polarization charge). References: P.H. Handel: "Polarization Catastrophe Theory of Cloud Electricity", J. Geophysical Research 90, 5857-5863 (1985). P.H. Handel and P.B. James: "Polarization Catastrophe Model of Static Electrification and Spokes in the B-Ring of Saturn", Geophys. Res. Lett. 10, 1-4 (1983).

Investigating Electrochemical Processes in Secondary Batteries

NASA Astrophysics Data System (ADS)

Cama, Christina A.

For the past twenty-six years, the lithium-ion battery has been the most popular recharge- able battery for portable devices and electric vehicles. Despite its success, the energy storage capability of lithium-ion batteries (LIBs) is significantly limited by both the electrodes and electrolytes employed. Typical LIBs rely on intercalation-type electrodes, that are not capable of storing more than 1 Li+ per formula unit. The energy storage capability of LIBs can be improved through the application of conversion-type materials and beyond lithium chemistries. This research involves multiple projects which explore the electrochemistry of conversion electrodes, magnesium-ion chemistry, and lithium-sulfur chemistry. Application of conversion-electrodes like copper ferrite, CuFe2O4, and magnetite, Fe3O4, are capable of lithium storage over five times greater than that achieved by electrodes used in commercial LIBs. The drawback to utilizing the conversion mechanism is that significant energy storage capability is lost during charge. In this research, X- ray characterization methods, including X-ray Diffraction (XRD) and X-ray Absorption Spectroscopy (XAS) are used to elucidate the lithiation and delithiation mechanism for CuFe2O4 and to understand the source of the irreversibility. These experiments provide significant insight into the reduction processes and cation migration within the structure. During lithiation, CuFe2O4 undergoes a three-step reduction mechanism involving (1) lithiation of CuFe2O4, (2) extrusion of copper metal nanoparticles and formation of rock- salt LiFeO2, followed by the (3) formation of iron metal nanoparticles. Upon delithiation, XAS spectra clearly demonstrate the feasibility of Fe0 oxidation to a rock-salt iron oxide; however, Cu0 oxidation is not observed. Additional experiments explored the kinetic limitations of lithiating Fe3O4 nanoparticles, with different crystallite sizes. The experiments demonstrate that the kinetics of the lithiation mechanism are influenced by the electroactive material’s agglomerate and crystallite size. The rate of lithiation involving small crystallites is dependent on diffusion within the agglomerates; however, as the crystallite size increases, the lithiation rate is inhibited by diffusion within both the agglomerate and the crystallite. Battery chemistries beyond lithium can also lead to energy storage capabilities an order of magnitude higher than LIBs. Both magnesium-ion and lithium-sulfur battery chemistries are investigated in this dissertation. The properties of ionic liquid electrolytes are explored as safer alternatives to harmful Grignard-reagent electrolytes commonly used for magnesium chemistries. Electrochemical evaluation of the ionic liquid electrolytes found that although better conductivity can be achieved with unsaturated electrolytes like imidizolium based electrolytes, greater oxidative voltages are possible with saturated electrolytes like the piperidinium and pyridinium based electrolytes. The higher oxidative voltage is a promising attribute for high voltage applications. Cathode additives, including FeS2 and microporous carbon, are studied to inhibit polysulfide dissolution within the electrolyte of Li|S batteries. Although FeS2 exhibited promising electrochemistry as its own cathode, it was found to be an ineffective additive within sulfur cathodes. Instead, the properties of microporous carbons are explored to identify an appropriate carbon additive to both increase conductivity and impede polysulfide dissolution. A wood based carbon exhibited high capacity and long cycle life at low rate compared to conventional microporous carbons. As a whole, this research has provided valuable insight into the electrochemical processes taking place within a battery, as well as the factors which affect these processes. Electrochemical, spectroscopic, and various scattering methods are used to probe processes which span from the reactions occurring within the electrode to the redox reactions which define the voltage limitations of the electrolyte. These studies demonstrate the impact of each battery component on the overall electrochemical performance and provide fundamental insight into battery operation.

Modelling and validation of particle size distributions of supported nanoparticles using the pair distribution function technique

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

Gamez-Mendoza, Liliana; Terban, Maxwell W.; Billinge, Simon J. L.

The particle size of supported catalysts is a key characteristic for determining structure–property relationships. It is a challenge to obtain this information accurately andin situusing crystallographic methods owing to the small size of such particles (<5 nm) and the fact that they are supported. In this work, the pair distribution function (PDF) technique was used to obtain the particle size distribution of supported Pt catalysts as they grow under typical synthesis conditions. The PDF of Pt nanoparticles grown on zeolite X was isolated and refined using two models: a monodisperse spherical model (single particle size) and a lognormal size distribution.more » The results were compared and validated using scanning transmission electron microscopy (STEM) results. Both models describe the same trends in average particle size with temperature, but the results of the number-weighted lognormal size distributions can also accurately describe the mean size and the width of the size distributions obtained from STEM. Since the PDF yields crystallite sizes, these results suggest that the grown Pt nanoparticles are monocrystalline. This work shows that refinement of the PDF of small supported monocrystalline nanoparticles can yield accurate mean particle sizes and distributions.« less

In-situ Micro-structural Studies of Gas Hydrate Formation in Sedimentary Matrices

NASA Astrophysics Data System (ADS)

Kuhs, Werner F.; Chaouachi, Marwen; Falenty, Andrzej; Sell, Kathleen; Schwarz, Jens-Oliver; Wolf, Martin; Enzmann, Frieder; Kersten, Michael; Haberthür, David

2015-04-01

The formation process of gas hydrates in sedimentary matrices is of crucial importance for the physical and transport properties of the resulting aggregates. This process has never been observed in-situ with sub-micron resolution. Here, we report on synchrotron-based micro-tomographic studies by which the nucleation and growth processes of gas hydrate were observed in different sedimentary matrices (natural quartz, glass beds with different surface properties, with and without admixtures of kaolinite and montmorillonite) at varying water saturation. The nucleation sites can be easily identified and the growth pattern is clearly established. In under-saturated sediments the nucleation starts at the water-gas interface and proceeds from there to form predominantly isometric single crystals of 10-20μm size. Using a newly developed synchrotron-based method we have determined the crystallite size distributions (CSD) of the gas hydrate in the sedimentary matrix confirming in a quantitative and statistically relevant manner the impressions from the tomographic reconstructions. It is noteworthy that the CSDs from synthetic hydrates are distinctly smaller than those of natural gas hydrates [1], which suggest that coarsening processes take place in the sedimentary matrix after the initial hydrate formation. Understanding the processes of formation and coarsening may eventually permit the determination of the age of gas hydrates in sedimentary matrices [2], which are largely unknown at present. Furthermore, the full micro-structural picture and its evolution will enable quantitative digital rock physics modeling to reveal poroelastic properties and in this way to support the exploration and exploitation of gas hydrate resources in the future. [1] Klapp S.A., Hemes S., Klein H., Bohrmann G., McDonald I., Kuhs W.F. Grain size measurements of natural gas hydrates. Marine Geology 2010; 274(1-4):85-94. [2] Klapp S.A., Klein H, Kuhs W.F. First determination of gas hydrate crystallite size distribution using high-energy synchrotron radiation. Geophys.Res.Letters, 2007 ; 34 : L13608, DOI:10.1029/2006GL029134

On the Importance of Cycle Minimum in Sunspot Cycle Prediction

NASA Technical Reports Server (NTRS)

Wilson, Robert M.; Hathaway, David H.; Reichmann, Edwin J.

1996-01-01

The characteristics of the minima between sunspot cycles are found to provide important information for predicting the amplitude and timing of the following cycle. For example, the time of the occurrence of sunspot minimum sets the length of the previous cycle, which is correlated by the amplitude-period effect to the amplitude of the next cycle, with cycles of shorter (longer) than average length usually being followed by cycles of larger (smaller) than average size (true for 16 of 21 sunspot cycles). Likewise, the size of the minimum at cycle onset is correlated with the size of the cycle's maximum amplitude, with cycles of larger (smaller) than average size minima usually being associated with larger (smaller) than average size maxima (true for 16 of 22 sunspot cycles). Also, it was found that the size of the previous cycle's minimum and maximum relates to the size of the following cycle's minimum and maximum with an even-odd cycle number dependency. The latter effect suggests that cycle 23 will have a minimum and maximum amplitude probably larger than average in size (in particular, minimum smoothed sunspot number Rm = 12.3 +/- 7.5 and maximum smoothed sunspot number RM = 198.8 +/- 36.5, at the 95-percent level of confidence), further suggesting (by the Waldmeier effect) that it will have a faster than average rise to maximum (fast-rising cycles have ascent durations of about 41 +/- 7 months). Thus, if, as expected, onset for cycle 23 will be December 1996 +/- 3 months, based on smoothed sunspot number, then the length of cycle 22 will be about 123 +/- 3 months, inferring that it is a short-period cycle and that cycle 23 maximum amplitude probably will be larger than average in size (from the amplitude-period effect), having an RM of about 133 +/- 39 (based on the usual +/- 30 percent spread that has been seen between observed and predicted values), with maximum amplitude occurrence likely sometime between July 1999 and October 2000.

Influence of Substrate, Additives, and Pulse Parameters on Electrodeposition of Gold Nanoparticles from Potassium Dicyanoaurate

NASA Astrophysics Data System (ADS)

Vahdatkhah, Parisa; Sadrnezhaad, Sayed Khatiboleslam

2015-12-01

Gold nanoparticles (AuNPs) of less than 50 nm diameter were electrodeposited from cyanide solution by pulsating electric current on modified copper and indium tin oxide (ITO) films coated on glass. Morphology, size, and composition of the deposited AuNPs were studied by X-ray photoelectron spectroscopy, atomic force microscopy, and field emission scanning electron microscopy. Effects of peak current density, pulse frequency, potassium iodide and cysteine on grain size, and morphology of the AuNPs were determined. Experiments showed that cathode current efficiency increases with the pulse frequency and the iodide ion. Size of the AuNPs increased with the current density. The number of nucleation sites was larger on ITO than on Cu layer; while the average diameter of the crystallites on ITO was smaller than on Cu layer.

Simple size control of TiO2 nanoparticles and their electrochemical performance: emphasizing the contribution of the surface area to lithium storage at high-rates

NASA Astrophysics Data System (ADS)

Lim, Joohyun; Um, Ji Hyun; Lee, Kyung Jae; Yu, Seung-Ho; Kim, Young-Jae; Sung, Yung-Eun; Lee, Jin-Kyu

2016-03-01

The particle size effects of TiO2 nanoparticles (TNPs), which are composed of small crystallites, on Li ion storage are a very fundamental and important subject. However, size control of TNPs under 200 nm using a sol-gel method has been limited due to the highly reactive precursor, titanium alkoxide. In this study, TNPs with various sizes even under 100 nm are obtained by controlling the reactant concentrations in a mixed solvent of ethanol and acetonitrile. Among them, three different sizes of TNPs are prepared to compare the Li ion storage capacity, and 60 nm TNPs are found to have the best reversible capacity of 182 mA h g-1 after 50 cycles at 1 C and a remarkable rate performance of 120 mA h g-1 at 10 C. Capacity increase upon cycling is observed in the size-controlled TNPs, and the explanation of this phenomenon is proposed to the lattice volume expansion of TiO2 upon intercalation for enabling further penetration of the electrolyte into the particles' interior. Moreover, the capacity at high rates is more closely related to the surface area from Hg porosimetry analysis than from typical N2 adsorption/desorption analysis.The particle size effects of TiO2 nanoparticles (TNPs), which are composed of small crystallites, on Li ion storage are a very fundamental and important subject. However, size control of TNPs under 200 nm using a sol-gel method has been limited due to the highly reactive precursor, titanium alkoxide. In this study, TNPs with various sizes even under 100 nm are obtained by controlling the reactant concentrations in a mixed solvent of ethanol and acetonitrile. Among them, three different sizes of TNPs are prepared to compare the Li ion storage capacity, and 60 nm TNPs are found to have the best reversible capacity of 182 mA h g-1 after 50 cycles at 1 C and a remarkable rate performance of 120 mA h g-1 at 10 C. Capacity increase upon cycling is observed in the size-controlled TNPs, and the explanation of this phenomenon is proposed to the lattice volume expansion of TiO2 upon intercalation for enabling further penetration of the electrolyte into the particles' interior. Moreover, the capacity at high rates is more closely related to the surface area from Hg porosimetry analysis than from typical N2 adsorption/desorption analysis. Electronic supplementary information (ESI) available. See DOI: 10.1039/c6nr00104a

Shape Modification and Size Classification of Microcrystalline Graphite Powder as Anode Material for Lithium-Ion Batteries

NASA Astrophysics Data System (ADS)

Wang, Cong; Gai, Guosheng; Yang, Yufen

2018-03-01

Natural microcrystalline graphite (MCG) composed of many crystallites is a promising new anode material for lithium-ion batteries (LiBs) and has received considerable attention from researchers. MCG with narrow particle size distribution and high sphericity exhibits excellent electrochemical performance. A nonaddition process to prepare natural MCG as a high-performance LiB anode material is described. First, raw MCG was broken into smaller particles using a pulverization system. Then, the particles were modified into near-spherical shape using a particle shape modification system. Finally, the particle size distribution was narrowed using a centrifugal rotor classification system. The products with uniform hemispherical shape and narrow size distribution had mean particle size of approximately 9 μm, 10 μm, 15 μm, and 20 μm. Additionally, the innovative pilot experimental process increased the product yield of the raw material. Finally, the electrochemical performance of the prepared MCG was tested, revealing high reversible capacity and good cyclability.

Correlating Sampling and Intensity Statistics in Nanoparticle Diffraction Experiments

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

Ozturk, Hande; Yan, Hanfei; Hill, John P.

2015-08-01

In this article, [Öztürk, Yan, Hill & Noyan (2014). J. Appl. Cryst. 47, 1016-1025] it was shown that the sampling statistics of diffracting particle populations within a polycrystalline ensemble depended on the size of the constituent crystallites: broad X-ray peak breadths enabled some nano-sized particles to contribute more than one diffraction spot to Debye-Scherrer rings. Here it is shown that the equations proposed by Alexander, Klug & Kummer [J. Appl. Phys. (1948), 19, 742-753] (AKK) to link diffracting particle and diffracted intensity statistics are not applicable if the constituent crystallites of the powder are below 10 nm. In this sizemore » range, (i) the one-to-one correspondence between diffracting particles and Laue spots assumed in the AKK analysis is not satisfied, and (ii) the crystallographic correlation between Laue spots originating from the same grain invalidates the assumption that all diffracting plane normals are randomly oriented and uncorrelated. Such correlation produces unexpected results in the selection of diffracting grains. Three or more Laue spots from a given grain for a particular reflection can only be observed at certain wavelengths. In addition, correcting the diffracted intensity values by the traditional Lorentz term, 1/cos [theta], to compensate for the variation of particles sampled within a reflection band does not maintain fidelity to the number of poles contributing to the diffracted signal. A new term, cos [theta]B/cos [theta], corrects this problem.« less

An In-situ method for the study of strain broadening usingsynchrotronx-ray diffraction

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

Tang, Chiu C.; Lynch, Peter A.; Cheary, Robert W.

2006-12-15

A tensonometer for stretching metal foils has beenconstructed for the study of strain broadening in x-ray diffraction lineprofiles. This device, which is designed for use on the powderdiffractometer in Station 2.3 at Daresbury Laboratory, allows in-situmeasurements to be performed on samples under stress. It can be used fordata collection in either transmission or reflection modes using eithersymmetric or asymmetric diffraction geometries. As a test case,measurements were carried out on a 18mum thick copper foil experiencingstrain levels of up to 5 percent using both symmetric reflection andsymmetric transmission diffraction. All the diffraction profilesdisplayed peak broadening and asymmetry which increased with strain.more » Themeasured profiles were analysed by the fundamental parameters approachusing the TOPAS peak fitting software. All the observed broadenedprofiles were modelled by convoluting a refineable diffraction profile,representing the dislocation and crystallite size broadening, with afixed instrumental profile pre-determined usinghigh quality LaB6reference powder. The de-convolution process yielded "pure" sampleintegral breadths and asymmetry results which displayed a strongdependence on applied strain and increased almost linearly with appliedstrain. Assuming crystallite size broadening in combination withdislocation broadening arising from fcc a/2<110>111 dislocations,we have extracted the variation of mechanic al property with strain. Theobservation of both peak asymmetry and broadening has been interpreted asa manifestation of a cellular structure with cell walls and cellinteriors possessing high and low dislocation densities.« less

Xenon-ion irradiation of Co/Si bilayers: Magnetic and structural properties

NASA Astrophysics Data System (ADS)

Novaković, M.; Popović, M.; Zhang, K.; Čubrović, V.; Bibić, N.; Rakočević, Z.

2018-07-01

Evolution of the structure of cobalt-silicon films during Xe ions irradiation has been studied and the same is correlated with magnetic properties. The polycrystalline cobalt films were deposited by electron beam evaporation method to a thickness of 50 nm on crystalline silicon (c-Si) and silicon with pre-amorphized surface (a-Si). After deposition the layers were irradiated with 400 keV Xe ions to the fluences in the range of 2-30 × 1015 ions/cm2. Structural analysis was done by means of transmission electron microscopy, atomic force microscopy (AFM) and X-ray diffraction (XRD), while the magnetic properties were analyzed by using magneto-optical Kerr effect (MOKE) technique. For the both types of substrate the AFM and XRD results show that after Xe ions irradiation the layers become more rough and the grain size of the crystallites increases; the effects being more evidenced for all fluences for the layers deposited on pre-amorphized Si. The MOKE measurements provided the in-plane azimuthal angular dependence of the hysteresis loops and the change of magnetization with the structural parameters. Although the coercive field is influenced by the surface roughness, in the case of c-Si substrate we found it is much more determined by the size of the crystallites. Additionally, independently on the substrate used the magnetic anisotropy in the Co films disappeared as the Xe ion fluence increased, indicating that the changes of magnetization in both systems occur for similar reasons.

Tribological Behavior and Corrosion Resistance of Electroless Ni-B-W Coatings

NASA Astrophysics Data System (ADS)

Mukhopadhyay, Arkadeb; Barman, Tapan Kumar; Sahoo, Prasanta

The present study considers the tribological behavior and corrosion resistance of electroless Ni-B-W coatings deposited on AISI 1040 steel substrates. Coating is characterized using scanning electron microscopy, energy dispersive X-ray analysis and X-ray diffraction technique. In as-deposited condition, coatings are found to be amorphous. On heat treatment, precipitation of crystalline Ni (1 1 1) and its borides take place. For as-deposited coating, the microhardness is obtained as ˜759HV100 which increases to ˜1181HV100 and ˜1098HV100 when heat treated at 350∘C and 450∘C, respectively. Incorporation of W in Ni-B coating results in an increase of hardness by 89HV100 in as-deposited condition. Heat treatment also results in increase in crystallite size of Ni (1 1 1). Wear rate and coefficient of friction (COF) of the coatings are evaluated on a pin-on-disc setup under both dry and lubricated sliding conditions. Wear resistance is observed to improve on heat treatment with an increase in crystallite size while COF deteriorates. However, in as-deposited condition, wear rate and COF of Ni-B-W coatings improve by ˜5 and ˜3 times, respectively, compared with Ni-B coatings. Wear and friction performance of the coatings are enhanced under lubrication due to the columnar structure of the coatings that retain lubricants. Corrosion resistance of Ni-B-W coating in 3.5% NaCl solution gets improved on heat treatment.

Quaternary M{sub 0.25}Cu{sub 0.25}Mg{sub 0.5}Fe{sub 2}O{sub 4} (M = Ni, Zn, Co, Mn) ferrite oxides: Synthesis, characterization and magnetic properties

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

Ciocarlan, Radu George; Laboratory of Adsorption and Catalysis, Department of Chemistry, University of Antwerpen; Pui, Aurel, E-mail: aurel@uaic.ro

2016-09-15

Highlights: • Superparamagnetic quaternary nanoferrite (M{sub 0.25}Cu{sub 0.25}Mg{sub 0.5}Fe{sub 2}O{sub 4,} where M = Mn, Zn, Co, Ni) were obtained. • C, O, H and metals were observed by XPS analysis. • Phases purity were confirmed by XRD diffraction and crystallite size (3–10 nm) were determind. - Abstract: We report the synthesis of M{sub 0.25}Cu{sub 0.25}Mg{sub 0.5}Fe{sub 2}O{sub 4} (where M = Mn, Zn, Co, Ni) nanoparticles using the coprecipitation method in the presence of carboxymethyl cellulose (CMC) as the in-situ surfactant. The crystalline structure and surface morphology were examined by means of X-ray diffraction (XRD) and scanning electron microscopymore » (SEM) and it was established that the average diameter of the magnetic nanoparticles (MNPs) is in the range of 3–10 nm. X-ray photoelectron spectroscopy (XPS) and Fourier transform infrared spectroscopy (FTIR) show that the MNPs are activated by the hydrophilic groups of the surfactant, which coat them and enhance their stability. The vibrating sample magnetometry measurements show the superparamagnetic behavior of the nanoparticles. Due to their small crystallite size, which implies large surface area, and their functionalization with organic groups, the obtained nanoparticles could have medical and catalytic applications.« less

Homocomposites of Polylactide (PLA) with Induced Interfacial Stereocomplex Crystallites

PubMed Central

2015-01-01

The demand for “green” degradable composite materials increases with growing environmental awareness. The key challenge is achieving the preferred physical properties and maintaining their eco-attributes in terms of the degradability of the matrix and the filler. Herein, we have designed a series of “green” homocomposites materials based purely on polylactide (PLA) polymers with different structures. Film-extruded homocomposites were prepared by melt-blending PLA matrixes (which had different degrees of crystallinity) with PLLA and PLA stereocomplex (SC) particles. The PLLA and SC particles were spherical and with 300–500 nm size. Interfacial crystalline structures in the form of stereocomplexes were obtained for certain particulate-homocomposite formulations. These SC crystallites were found at the particle/matrix interface when adding PLLA particles to a PLA matrix with d-lactide units, as confirmed by XRD and DSC data analyses. For all homocomposites, the PLLA and SC particles acted as nucleating agents and enhanced the crystallization of the PLA matrixes. The SC particles were more rigid and had a higher Young’s modulus compared with the PLLA particles. The mechanical properties of the homocomposites varied with particle size, rigidity, and the interfacial adhesion between the particles and the matrix. An improved tensile strength in the homocomposites was achieved from the interfacial stereocomplex formation. Hereafter, homocomposites with tunable crystalline arrangements and subsequently physical properties, are promising alternatives in strive for eco-composites and by this, creating materials that are completely degradable and sustainable. PMID:26523245

A Conceptual Model for Shear-Induced Phase Behavior in Crystallizing Cocoa Butter

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

Mazzanti,G.; Guthrie, S.; Marangoni, A.

2007-01-01

We propose a conceptual model to explain the quantitative data from synchrotron X-ray diffraction experiments on the shear-induced phase behavior of cocoa butter, the main structural component of chocolate. We captured two-dimensional diffraction patterns from cocoa butter at crystallization temperatures of 17.5, 20.0, and 22.5 {sup o}C under shear rates from 45 to 1440 s{sup -1} and under static conditions. From the simultaneous analysis of the integrated intensity, correlation length, lamellar thickness, and crystalline orientation, we postulate a conceptual model to provide an explanation for the distribution of phases II, IV, V, and X and the kinetics of the process.more » As previously proposed in the literature, we assume that the crystallites grow layer upon layer of slightly different composition. The shear rate and temperature applied define these compositions. Simultaneously, the shear and temperature define the crystalline interface area available for secondary nucleation by promoting segregation and affecting the size distribution of the crystallites. The combination of these factors (composition, area, and size distribution) favors dramatically the early onset of phase V under shear and determines the proportions of phases II, IV, V, and X after the transition. The experimental observations, the methodology used, and the proposed explanation are of fundamental and industrial interest, since the structural properties of crystalline networks are determined by their microstructure and polymorphic crystalline state. Different proportions of the phases will thus result in different characteristics of the final material.« less

Photocatalytic degradation of methylene blue on Sn-doped titania nanoparticles synthesized by solution combustion route

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

Bhange, P.D., E-mail: pallavi.ncl@gmail.com; Awate, S.V.; Gholap, R.S.

2016-04-15

Highlights: • Series of Sn-doped titania nanoparticles were prepared by solution combustion synthesis method. • Sn-doped titania nanoparticles were tested for degradation of MB under UV light irradiation. • The maximum Sn doping in the TiO{sub 2} lattice is found to be less than 10%. • The crystallite size decreases with increase in the Sn content. • The doping of Sn into TiO{sub 2} lattice hinders the recombination of electrons and holes thus enhance the photocatalytic activity. - Abstract: Series of tin-doped titania nanoparticles with varying tin content in the range 0–20 mol% have been prepared by solution combustion synthesismore » route using urea as a fuel. The structure, surface morphology and optical activity of Sn-doped TiO{sub 2} nanoparticles were investigated by various analytical techniques such as powder XRD, SEM, TEM, UV–vis and N{sub 2} adsorption study. The crystalline structures of the various phases were studied by rietveld refinement of the XRD data. The photocatalytic performance of Sn-doped titania nanoparticles were tested for degradation of MB under UV and visible light irradiation. The results reveal that the photocatalytic activity increases with increase in tin content which may be due to decrease in crystallite size with increase in surface area. The doping of Sn into TiO{sub 2} lattice hinders the recombination of electrons and holes thus enhance the quantum efficiency of photocatalytic reaction.« less

Influences of device structures on microstructure-correlated photovoltaic characteristics of organic solar cells

NASA Astrophysics Data System (ADS)

Wu, Fu-Chiao; Yang, Cheng-Chi; Tseng, Po-Tsung; Chou, Wei-Yang; Cheng, Horng-Long

2017-02-01

Photovoltaic characteristics of organic solar cells (OSCs) are correlated with microstructural qualities of active layers (ALs). Numerous efforts focused on improving process conditions of ALs to attain effective microstructures to achieve high-efficiency OSCs. Aside from AL process conditions, layer properties under AL can also influence microstructural qualities of AL. In this study, we adopted poly(3-hexylthiophene) (P3HT):(6,6)-phenyl C61-butyric acid methyl ester (PCBM) mixture as AL, poly(3,4-ethylenedioxythiophene):poly(styrene sulfonate) (PEDOT:PSS) as hole extraction layer, and branched polyethyleneimine (BPEI) as electron extraction layer to prepare OSCs with different device structures, that is, normal type (PEDOT:PSS/P3HT:PCBM/BPEI) and inverted type (BPEI/P3HT:PCBM/PEDOT:PSS) structures. We discovered that although devices have similar layer components, they have different photovoltaic characteristics. Inverted devices demonstrated higher power conversion efficiency than normal devices. Various methods, including absorption spectroscopy and microscopy, were used to study AL microstructures of different devices. We observed that P3HT crystallites grown on BPEI had longer vertical size and shorter horizontal size compared with those grown on PEDOT:PSS; these properties could result from larger interfacial tension of P3HT with BPEI than with PEDOT:PSS. Observed shape of P3HT crystallites in inverted devices facilitated efficient charge transport to electrodes and suppressed current leakage. As a result, inverted devices generated improved photovoltaic performance.

CTAB assisted growth and characterization of nanocrystalline CuO films by ultrasonic spray pyrolysis technique

NASA Astrophysics Data System (ADS)

Singh, Iqbal; Kaur, Gursharan; Bedi, R. K.

2011-09-01

An aqueous solution of cupric nitrate trihydrate (Cu(NO 3) 2·3H 2O) modified with cetyltrimetylammonium bromide (CTAB) is used to deposit CuO films on glass substrate by chemical spray pyrolysis technique. The thermal analysis shows that the dried CTAB doped precursor decomposes by an exothermic reaction and suggests that minimum substrate temperature for film deposition should be greater than 270 °C. X-ray diffraction (XRD) studies indicate the formation of monoclinic CuO with preferential orientation along (0 0 2) plane for all film samples. The CTAB used as cationic surfactant in precursor results in the suppression of grain growth in films along the (1 1 0), (0 2 0) and (2 2 0) crystal planes of CuO. Surfactant modified films showed an increase in crystallite size of 14 nm at substrate temperature of 300 °C. The scanning electron micrographs (FESEM) confirm the uniform distribution of facets like grains on the entire area of substrate. CTAB modified films show a significant reduction in the particle agglomeration. Electrical studies of the CuO films deposited at substrate temperature of 300 °C with and without surfactant reveal that the CTAB doping increase the activation energy of conduction by 0.217 eV and room temperature response to ammonia by 9%. The kinetics of the ammonia gas adsorption on the film surface follows the Elovich and Diffusion models.

Features of bicrystal growth during the directional crystallization of metal melts

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

Gubernatorov, V. V.; Sycheva, T. S., E-mail: sych@imp.uran.ru; Gundyrev, V. M.

2017-03-15

The factors responsible for the formation of different configurations of boundaries between adjacent crystallites during their growth from melt by Bridgman and Czochralski methods have been considered by an of example Fe–20 wt % Ga alloy and Ni bicrystals. It is found that the configuration of intercrystallite boundary is related to the features of crystallite growth, caused by the strained state of intercrystallite and interphase (crystal–melt) boundaries, the difference in the linear thermal expansion coefficients of the crystallite boundaries and bulk, and the shape (geometry) of the bicrystal cross section. It is suggested that the strained state of boundaries andmore » the formation of substructure in crystallites during directional crystallization from metal melt are significantly affected by their deformation under the melt weight.« less

Muskellunge growth potential in northern Wisconsin: implications for trophy management

USGS Publications Warehouse

Faust, Matthew D.; Isermann, Daniel A.; Luehring, Mark A.; Hansen, Michael J.

2015-01-01

The growth potential of Muskellunge Esox masquinongy was evaluated by back-calculating growth histories from cleithra removed from 305 fish collected during 1995–2011 to determine whether it was consistent with trophy management goals in northern Wisconsin. Female Muskellunge had a larger mean asymptotic length (49.8 in) than did males (43.4 in). Minimum ultimate size of female Muskellunge (45.0 in) equaled the 45.0-in minimum length limit, but was less than the 50.0-in minimum length limit used on Wisconsin's trophy waters, while the minimum ultimate size of male Muskellunge (34.0 in) was less than the statewide minimum length limit. Minimum reproductive sizes for both sexes were less than Wisconsin's trophy minimum length limits. Mean growth potential of female Muskellunge in northern Wisconsin appears to be sufficient for meeting trophy management objectives and angler expectations. Muskellunge in northern Wisconsin had similar growth potential to those in Ontario populations, but lower growth potential than Minnesota's populations, perhaps because of genetic and environmental differences.

Magnetic anisotropy and order parameter in nanostructured CoPt particles

NASA Astrophysics Data System (ADS)

Komogortsev, S. V.; Iskhakov, R. S.; Zimin, A. A.; Filatov, E. Yu.; Korenev, S. V.; Shubin, Yu. V.; Chizhik, N. A.; Yurkin, G. Yu.; Eremin, E. V.

2013-10-01

The correlation of magnetic anisotropy energy with order parameter in the crystallites of CoPt nanostructured particles prepared by thermal decomposition and further annealing has been studied by investigation of the approach magnetization to saturation curves and x-ray powder diffraction pattern profiles. It is shown that magnetic anisotropy energy value in partially ordered CoPt crystallite could be described as an intermediate case between two extremes, corresponding to either single or several c-domains of L10 phase in crystallite.

Structural and optical characterizations of Ca2Al2SiO7:Ce3+, Mn2+ nanoparticles produced via a hybrid route

NASA Astrophysics Data System (ADS)

Teixeira, V. C.; Montes, P. J. R.; Valerio, M. E. G.

2014-07-01

Pure, Ce3+ doped and Ce3+ and Mn2+ co-doped Ca2Al2SiO7 ceramic powders were prepared by two different methodologies which are the proteic sol-gel process and a new hybrid route combining the proteic sol-gel with solid state reaction processes. The second one is an eco-friendly method because it uses natural raw materials in replacement of the metal alkoxides used in the traditional sol-gel routes. X-ray diffraction showed that Ca2Al2SiO7 crystalline phase was obtained for both preparations. Differential thermal analysis indicated that the exothermic event around 850 °C, for sample produced by proteic sol-gel method, and around 927 °C, for ceramics prepared by hybrid synthesis, can be associated to crystallization of Ca2Al2SiO7. Transmission electron microscope indicates that regular and spherical nanoparticles were obtained with average sizes of about 12 nm. The Scherrer's method was used to determine the average crystallite sizes and it was shown that nanometric crystallites were obtained of about 74 nm for samples produced via hybrid route. For all the single phase samples, the crystallite sizes are about the same and that agrees with TEM results. Diffuse optical reflectance measurements were used to estimate the Ca2Al2SiO7 optical band gap and the obtained value is about 6 eV, photoluminescence (PL) spectra presented typical emissions of Ce3+ and Mn2+ ions. Upon excitation at 352 nm the emission spectra showed a broad band centered at 415 nm due to the Ce3+ 4f1 → 5d1 typical transition. This emission is resonant with Mn2+ excitation and it transfers energy to Mn ions generating a second broad emission band centered at 620 nm due to the Mn2+. The PL results were used to obtain, as a fist approach, the Ce3+ energy levels diagram and, using the Tanabe-Sugano diagrams, the transitions due to the Mn2+ were calculated. X-ray excited optical luminescence measurements showed the same emission spectra as the PL emission spectra. Luminescence lifetime decay constants were measured for Ce and Mn co-doped and for Ce doped samples and the results indicate Ca2Al2SiO7:Ce3+, Mn2+ showed quite fast responses with main time constants below 30 ns.

Interspecific geographic range size-body size relationship and the diversification dynamics of Neotropical furnariid birds.

PubMed

Inostroza-Michael, Oscar; Hernández, Cristián E; Rodríguez-Serrano, Enrique; Avaria-Llautureo, Jorge; Rivadeneira, Marcelo M

2018-05-01

Among the earliest macroecological patterns documented, is the range and body size relationship, characterized by a minimum geographic range size imposed by the species' body size. This boundary for the geographic range size increases linearly with body size and has been proposed to have implications in lineages evolution and conservation. Nevertheless, the macroevolutionary processes involved in the origin of this boundary and its consequences on lineage diversification have been poorly explored. We evaluate the macroevolutionary consequences of the difference (hereafter the distance) between the observed and the minimum range sizes required by the species' body size, to untangle its role on the diversification of a Neotropical species-rich bird clade using trait-dependent diversification models. We show that speciation rate is a positive hump-shaped function of the distance to the lower boundary. The species with highest and lowest distances to minimum range size had lower speciation rates, while species close to medium distances values had the highest speciation rates. Further, our results suggest that the distance to the minimum range size is a macroevolutionary constraint that affects the diversification process responsible for the origin of this macroecological pattern in a more complex way than previously envisioned. © 2018 The Author(s). Evolution © 2018 The Society for the Study of Evolution.

Synthesis and crystalline properties of CdS incorporated polyvinylidene fluoride (PVDF) composite film

NASA Astrophysics Data System (ADS)

Patel, Arunendra Kumar; Sunder, Aishwarya; Mishra, Shweta; Bajpai, Rakesh

2018-05-01

This paper gives an insight on the synthesis and crystalline properties of Polyvinylidene Fluoride (PVDF) (host matrix) composites impregnated with Cadmium Sulphide (CdS) using Dimethyl formamide (DMF) as the base, prepared by the well known solvent casting technique. The effect of doping concentration of CdS in to the PVDF matrix was studied using X-ray diffraction technique. The structural properties like crystallinity Cr, interplanar distance d, average size of the crystalline region (D), and average inter crystalline separation (R) have been estimated for the developed composite. The crystallinity index, crystallite size and inter crystalline separation is increasing with increase in the concentration of CdS in to the PVDF matrix while the interplanar distance d is decreasing.

Structural and photoluminescence properties of Ni doped CdS nanoparticles synthesis by sol gel method

NASA Astrophysics Data System (ADS)

Mahdi, Hadeel Salih; Parveen, Azra; Azam, Ameer

2018-05-01

Ni doped CdS nanoparticles have been successfully synthesized by sol-gel method. Nickel nitrate, cadmium nitrate, sodium sulfide has been used as precursors for the preparation of these Ni-doped CdS nanoparticles. The structural properties were studied by X-ray diffraction analysis. Surface morphology and the composition of the samples were studied by scanning electron microscope (SEM). The X-ray diffraction results revealed that the Ni-doped CdS nanoparticles were in hexagonal structure. The crystallite size was determined from Debye-Scherer equation and showed that the particle size increases with the doping of Ni. Optical absorption spectra of Ni doped CdS also was studied by Photoluminescence spectroscopy in the range of 200-600 nm.

Bio-active synthesis of tin oxide nanoparticles using eggshell membrane for energy storage application

NASA Astrophysics Data System (ADS)

Celina Selvakumari, J.; Nishanthi, S. T.; Dhanalakshmi, J.; Ahila, M.; Pathinettam Padiyan, D.

2018-05-01

Nano-sized tin oxide (SnO2) particles were synthesized using eggshell membrane (ESM), a natural bio-waste from the chicken eggshell. The crystallization of SnO2 into the tetragonal structure was confirmed from powder X-ray diffraction and the crystallite size ranged from 13 to 40 nm. Various shapes including rod, hexagonal and spherical SnO2 nanoparticles were observed from the morphological studies. The electrochemical impedance study revealed a lower charge transfer resistance (Rct) of 8.565 Ω and the presence of a constant phase element which arised due to surface roughness and porosity. Capacitive behavior seen in the cyclic voltammetry curve of the prepared SnO2 nanoparticles, find future applications in supercapacitors.

USE OF COMBUSTION SYNTHESIS IN PREPARING CERAMIC-MATRIX AND METAL-MATRIX COMPOSITE POWDERS

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

Weil, K. Scott; Hardy, John S.

A standard combustion-based approach typically used to synthesize nanosize oxide powders has been modified to prepare composite oxide-metal powders for subsequent densification via sintering or hot-pressing into ceramic- or metal-matrix composites. Copper and cerium nitrate salts were dissolved in the appropriate ratio in water and combined with glycine, then heated to cause autoignition. The ratio of glycine-to-total nitrate concentration was found to have the largest effect on the composition, agglomerate size, crystallite size, and dispersivity of phases in the powder product. After consolidation and sintering under reducing conditions, the resulting composite compact consists of a well-dispersed mixture of sub-micron sizemore » reinforcement particles in a fine-grained matrix.« less

Crystallization Mechanism and Charge Carrier Transport in MAPLE-Deposited Conjugated Polymer Thin Films

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

Dong, Ban Xuan; Strzalka, Joseph; Jiang, Zhang

Although spin casting and chemical surface reactions are the most common methods used for fabricating functional polymer films onto substrates, they are limited with regard to producing films of certain morphological characteristics on different wetting and nonwetting substrates. The matrix-assisted pulsed laser evaporation (MAPLE) technique offers advantages with regard to producing films of different morphologies on different types of substrates. Here, we provide a quantitative characterization, using X-ray diffraction and optical methods, to elucidate the additive growth mechanism of MAPLE-deposited poly(3-hexylthiophene) (P3HT) films on substrates that have undergone different surface treatments, enabling them to possess different wettabilities. We show thatmore » MAPLE-deposited films are composed of crystalline phases, wherein the overall P3HT aggregate size and crystallite coherence length increase with deposition time. A complete pole figure constructed from X-ray diffraction measurements reveals that in these MAPLE-deposited films, there exist two distinct crystallite populations: (i) highly oriented crystals that grow from the flat dielectric substrate and (ii) misoriented crystals that preferentially grow on top of the existing polymer layers. The growth of the highly oriented crystals is highly sensitive to the chemistry of the substrate, whereas the effect of substrate chemistry on misoriented crystal growth is weaker. The use of a self-assembled monolayer to treat the substrate greatly enhances the population and crystallite coherence length at the buried interfaces, particularly during the early stage of deposition. Furthermore, the evolution of the in-plane carrier mobilities during the course of deposition is consistent with the development of highly oriented crystals at the buried interface, suggesting that this interface plays a key role toward determining carrier transport in organic thin-film transistors.« less

Crystallization Mechanism and Charge Carrier Transport in MAPLE-Deposited Conjugated Polymer Thin Films

DOE PAGES

Dong, Ban Xuan; Strzalka, Joseph; Jiang, Zhang; ...

2017-11-23

Although spin casting and chemical surface reactions are the most common methods used for fabricating functional polymer films onto substrates, they are limited with regard to producing films of certain morphological characteristics on different wetting and nonwetting substrates. The matrix-assisted pulsed laser evaporation (MAPLE) technique offers advantages with regard to producing films of different morphologies on different types of substrates. Here, we provide a quantitative characterization, using X-ray diffraction and optical methods, to elucidate the additive growth mechanism of MAPLE-deposited poly(3-hexylthiophene) (P3HT) films on substrates that have undergone different surface treatments, enabling them to possess different wettabilities. We show thatmore » MAPLE-deposited films are composed of crystalline phases, wherein the overall P3HT aggregate size and crystallite coherence length increase with deposition time. A complete pole figure constructed from X-ray diffraction measurements reveals that in these MAPLE-deposited films, there exist two distinct crystallite populations: (i) highly oriented crystals that grow from the flat dielectric substrate and (ii) misoriented crystals that preferentially grow on top of the existing polymer layers. The growth of the highly oriented crystals is highly sensitive to the chemistry of the substrate, whereas the effect of substrate chemistry on misoriented crystal growth is weaker. The use of a self-assembled monolayer to treat the substrate greatly enhances the population and crystallite coherence length at the buried interfaces, particularly during the early stage of deposition. Furthermore, the evolution of the in-plane carrier mobilities during the course of deposition is consistent with the development of highly oriented crystals at the buried interface, suggesting that this interface plays a key role toward determining carrier transport in organic thin-film transistors.« less

Li-Ion Localization and Energetics as a Function of Anode Structure.

PubMed

McNutt, Nicholas W; McDonnell, Marshall; Rios, Orlando; Keffer, David J

2017-03-01

In this work, we study the effect of carbon composite anode structure on the localization and energetics of Li-ions. A computational molecular dynamics study is combined with experimental results from neutron scattering experiments to understand the effect of composite density, crystallite size, volume fraction of crystalline carbon, and ion loading on the nature of ion storage in novel, lignin-derived composite materials. In a recent work, we demonstrated that these carbon composites display a fundamentally different mechanism for Li-ion storage than traditional graphitic anodes. The edges of the crystalline and amorphous fragments of aromatic carbon that exist in these composites are terminated by hydrogen atoms, which play a crucial role in adsorption. In this work, we demonstrate how differences in composite structure due to changes in the processing conditions alter the type and extent of the interface between the amorphous and crystalline domains, thus impacting the nature of Li-ion storage. The effects of structural properties are evaluated using a suite of pair distribution functions as well as an original technique to extract archetypal structures, in the form of three-dimensional atomic density distributions, from highly disordered systems. The energetics of Li-ion binding are understood by relating changes in the energy and charge distributions to changes in structural properties. The distribution of Li-ion energies reveals that some structures lead to greater chemisorption, while others have greater physisorption. Carbon composites with a high volume fraction of small crystallites demonstrate the highest ion storage capacity because of the high interfacial area between the crystalline and amorphous domains. At these interfaces, stable H atoms, terminating the graphitic crystallites, provide favorable sites for reversible Li adsorption.

Structural characterization of ZnO thin films grown on various substrates by pulsed laser deposition

NASA Astrophysics Data System (ADS)

Novotný, M.; Čížek, J.; Kužel, R.; Bulíř, J.; Lančok, J.; Connolly, J.; McCarthy, E.; Krishnamurthy, S.; Mosnier, J.-P.; Anwand, W.; Brauer, G.

2012-06-01

ZnO thin films were grown by pulsed laser deposition on three different substrates: sapphire (0 0 0 1), MgO (1 0 0) and fused silica (FS). The structure and morphology of the films were characterized by x-ray diffraction and scanning electron microscopy and defect studies were carried out using slow positron implantation spectroscopy (SPIS). Films deposited on all substrates studied in this work exhibit the wurtzite ZnO structure and are characterized by an average crystallite size of 20-100 nm. However, strong differences in the microstructure of films deposited on various substrates were found. The ZnO films deposited on MgO and sapphire single-crystalline substrates exhibit local epitaxy, i.e. a well-defined relation between film crystallites and the substrate. Domains with different orientation relationships with the substrate were found in both films. On the other hand, the film deposited on the FS substrate exhibits fibre texture with random lateral orientation of crystallites. Extremely high compressive in-plane stress of σ ˜ 14 GPa was determined in the film deposited on the MgO substrate, while the film deposited on sapphire is virtually stress-free, and the film deposited on the FS substrate exhibits a tensile in-plane stress of σ ˜ 0.9 GPa. SPIS investigations revealed that the concentration of open-volume defects in the ZnO films is substantially higher than that in a bulk ZnO single crystal. Moreover, the ZnO films deposited on MgO and sapphire single-crystalline substrates exhibit a significantly higher density of defects than the film deposited on the amorphous FS substrate.

Production of Ti-C presolar carbide grain analogies and its infrared spectra

NASA Astrophysics Data System (ADS)

Kimura, Y.; Ikegami, A.; Tanigaki, T.; Ishikawa, M.; Sato, T.; Suzuki, H.; Kido, O.; Kaito, C.

The infrared emission of the circumstellar environment of carbon-rich stars and dense molecular cloud cores is believed to be dominated by the emissivity of carbon dust. The origins of absorption peaks will be identified on the basis of laboratory studies. Important factors in the determination of absorption features are size, shape and structure of the grain (Bohren and Huffman, 1983). Therefore, the production of presolar grain analogy is important for the identification of the observation spectra. Recently, we succeeded in the formation of Si-, Ti- and Zr-C grains of the order of 50 nm by advanced gas evaporation method. We have started to obtain characteristic data of carbide grains in laboratory experiments. The spectra from ultraviolet to infrared of samples embedded in KBr pellets are presented. In the present study, we will elucidate the correlation between the size of TiC grain or thickness of the carbon mantle layer and spectra of TiC core-carbon mantle grains. Because TiC is one of the candidates of 21 micron feature. The absorption peaks of TiC core (50 nm)-carbon mantle (2 nm) grains were found to be at 9.5 and 12.5 microns. When the thickness of the mantle layer increased to 15 nm, the peak at 12.5 microns disappeared and the peak at 9.5 microns was significantly weakened. These results are similar to the calculated result for SiC core-carbon mantle grains, i.e., increased thickness of the mantle layer weakens the spectrum intensity (Kozasa et al., 1996). The 20.1 micron absorption feature never appeared, even if the same size grains seen in meteorites were produced. Moreover, the infrared spectra were observed when the size of TiC grains was smaller than presolar grain. Carbon was deposited on the surface of Ti grains. Then, TiC nanocrystallites with the size of 2-3 nm were produced by the diffusion of Ti and/or carbon. The new absorption feature was appeared at 14 microns. The 12.5 micron absorption was hardly seen. If the samples are heated at 700circC for 1h, crystallites size of TiC was increased to about 5 nm. The absorption feature at 14 microns was weaken. It was concluded that the infrared absorption feature was depend on the crystallites size.

Microstructure, hardness and modulus of carbon-ion-irradiated new SiC fiber (601-4)

NASA Astrophysics Data System (ADS)

Huang, Qing; Lei, Guanhong; Liu, Renduo; Li, Jianjian; Yan, Long; Li, Cheng; Liu, Weihua; Wang, Mouhua

2018-05-01

Two types of SiC fibers, one is low-oxygen and carbon-rich fiber denoted by 601-4 and the other is low-oxygen and near-stoichiometric Tyranno SA, were irradiated with 450 keV C+ ions at room temperature. The Raman spectra indicate that irradiation induced distortion and amorphization of SiC crystallites in fibers. TEM characterization of Tyranno SA suggests that SiC crystallites undergo a continued fragmentation into smaller crystalline islands and a continued increase of surrounding amorphous structure. The SiC nano-crystallites (<15 nm) in 601-4 fiber are more likely to be amorphized than larger crystallites (∼200 nm) in Tyranno SA. The hardness and modulus of 601-4 continuously decreases with increasing fluence, while that of Tyranno SA first increases and then decreases.

Cadmium-sulfide crystallites in Cd-(. gamma. EC) sub n G peptide complexes from tomato. [Lycopersicon esculentum

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

Reese, R.N.; White, C.A.; Winge, D.R.

Hydroponically grown tomato plants (Lycopersicon esculentum P. Mill cv Golden Boy) exposed to 100 micromolar cadmium sulfate produced metal-({gamma}EC){sub n}G peptide complexes containing acid-labile sulfur. The properties of the complexes resemble those of the cadmium-({gamma}EC){sub n}G peptide complexes from Schizo-saccharomyces pombe and Candida glabrata known to contain a cadmium sulfide crystallite core. The crystallite is stabilized by a sheath of peptides of general structure ({gamma}Glu-Cys){sub n}-Gly. The cadmium-peptide complexes of tomato contained predominantly peptides of n{sub 3}, n{sub 4}, and n{sub 5}. Spectroscopic analyses indicated that the tomato cadmium-sulfide-peptide complex contained CdS crystallite core particles smaller than 2.0 nanometers inmore » diameter.« less

Study of energy versus misorientation for grain boundaries in gold by crystallite rotation method. I. (001) twist boundaries

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

Chan, S.W.; Balluffi, R.W.

1984-11-01

Small gold crystallites (approx. 50 to 80 nm dia) were welded to thin film (001) single crystal gold substrates at a series of predetermined (001) twist angles in the range 0 to 45/sup 0/. A pure (001) twist boundary therefore existed in each welded neck region which could be observed directly by transmission electron microscopy at normal incidence. Upon annealing, the crystallites rotated around (001) when the boundary energy varied with theta. The crystallites rotated into three misorientations corresponding to the special ..sigma..1 and ..sigma..5 misorientations and a symmetry related misorientation at theta=45/sup 0/. These results indicate the existence ofmore » grain boundary dislocation (GBD) related cusps on the boundary energy versus theta curve at ..sigma..1 and ..sigma..« less

A comprehensive physicochemical, thermal, and spectroscopic characterization of zinc (II) chloride using X-ray diffraction, particle size distribution, differential scanning calorimetry, thermogravimetric analysis/differential thermogravimetric analysis, ultraviolet-visible, and Fourier transform-infrared spectroscopy

PubMed Central

Trivedi, Mahendra Kumar; Sethi, Kalyan Kumar; Panda, Parthasarathi; Jana, Snehasis

2017-01-01

Objective: Zinc chloride is an important inorganic compound used as a source of zinc and has other numerous industrial applications. Unfortunately, it lacks reliable and accurate physicochemical, thermal, and spectral characterization information altogether. Hence, the authors tried to explore in-depth characterization of zinc chloride using the modern analytical technique. Materials and Methods: The analysis of zinc chloride was performed using powder X-ray diffraction (PXRD), particle size distribution, differential scanning calorimetry (DSC), thermogravimetric analysis/differential thermogravimetric analysis (TGA/DTG), ultraviolet-visible spectroscopy (UV-vis), and Fourier transform-infrared (FT-IR) analytical techniques. Results: The PXRD patterns showed well-defined, narrow, sharp, and the significant peaks. The crystallite size was found in the range of 14.70–55.40 nm and showed average crystallite size of 41.34 nm. The average particle size was found to be of 1.123 (d10), 3.025 (d50), and 6.712 (d90) μm and average surface area of 2.71 m2/g. The span and relative span values were 5.849 μm and 1.93, respectively. The DSC thermogram showed a small endothermic inflation at 308.10°C with the latent heat (ΔH) of fusion 28.52 J/g. An exothermic reaction was observed at 449.32°C with the ΔH of decomposition 66.10 J/g. The TGA revealed two steps of the thermal degradation and lost 8.207 and 89.72% of weight in the first and second step of degradation, respectively. Similarly, the DTG analysis disclosed Tmax at 508.21°C. The UV-vis spectrum showed absorbance maxima at 197.60 nm (λmax), and FT-IR spectrum showed a peak at 511/cm might be due to the Zn–Cl stretching. Conclusions: These in-depth, comprehensive data would be very much useful in all stages of nutraceuticals/pharmaceuticals formulation research and development and other industrial applications. PMID:28405577

Synthesis and Characterization of CuFe 2O 4 Nano/Submicron Wire–Carbon Nanotube Composites as Binder-free Anodes for Li-Ion Batteries

DOE PAGES

Wang, Lei; Bock, David C.; Li, Jing; ...

2018-02-20

Here, a series of one-dimensional CuFe 2O 4 nano/sub-micron wires possessing different diameters, crystal phases, and crystal sizes have been successfully generated using a facile template-assisted co precipitation reaction at room temperature, followed by a short post-annealing process. The diameter and the crystal structure of the resulting CuFe 2O4 (CFO) wires were judiciously tuned by varying the pore size of the template and the post-annealing temperature, respectively. Carbon nanotubes (CNTs) were incorporated to generate CFO-CNT binder-free anodes, and multiple characterization techniques were employed with the goal of delineating the relationships between electrochemical behavior and the properties of both the CFOmore » wires (crystal phase, wire diameter, crystal size) and the electrode architecture (binder-free vs. conventionally prepared approaches). The study reveals several notable findings. First, the crystal phase (cubic or tetragonal) did not influence the electrochemical behavior in this CFO system. Second, regarding crystallite size and wire diameter, CFO wires with larger crystallite sizes exhibit improved cycling stability, while wires possessing smaller diameters exhibiting higher capacities. Finally, the electrochemical behavior is strongly influenced by the electrode architecture, with CFO-CNT binder-free electrodes demonstrating significantly higher capacities and cycling stability compared to conventionally prepared coatings. The mechanism(s) associated with the high capacities under low current density but limited electrochemical reversibility of CFO electrodes under high current density were probed via x-ray absorption spectroscopy (XAS) mapping with sub-micron spatial resolution for the first time. Results suggest that the capacity of the binder-free electrodes under high rate is limited by the irreversible formation of Cu 0, as well as limited reduction of Fe 3+, to Fe 2+ not Fe 0. The results (1) shed fundamental insight into the reversibility of CuFe 2O 4 materials cycled at high current density and (2) demonstrate that a synergistic effort to control both active material morphology and electrode architecture is an effective strategy for optimizing electrochemical behavior.« less

Synthesis and Characterization of CuFe 2O 4 Nano/Submicron Wire–Carbon Nanotube Composites as Binder-free Anodes for Li-Ion Batteries

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

Wang, Lei; Bock, David C.; Li, Jing

Here, a series of one-dimensional CuFe 2O 4 nano/sub-micron wires possessing different diameters, crystal phases, and crystal sizes have been successfully generated using a facile template-assisted co precipitation reaction at room temperature, followed by a short post-annealing process. The diameter and the crystal structure of the resulting CuFe 2O4 (CFO) wires were judiciously tuned by varying the pore size of the template and the post-annealing temperature, respectively. Carbon nanotubes (CNTs) were incorporated to generate CFO-CNT binder-free anodes, and multiple characterization techniques were employed with the goal of delineating the relationships between electrochemical behavior and the properties of both the CFOmore » wires (crystal phase, wire diameter, crystal size) and the electrode architecture (binder-free vs. conventionally prepared approaches). The study reveals several notable findings. First, the crystal phase (cubic or tetragonal) did not influence the electrochemical behavior in this CFO system. Second, regarding crystallite size and wire diameter, CFO wires with larger crystallite sizes exhibit improved cycling stability, while wires possessing smaller diameters exhibiting higher capacities. Finally, the electrochemical behavior is strongly influenced by the electrode architecture, with CFO-CNT binder-free electrodes demonstrating significantly higher capacities and cycling stability compared to conventionally prepared coatings. The mechanism(s) associated with the high capacities under low current density but limited electrochemical reversibility of CFO electrodes under high current density were probed via x-ray absorption spectroscopy (XAS) mapping with sub-micron spatial resolution for the first time. Results suggest that the capacity of the binder-free electrodes under high rate is limited by the irreversible formation of Cu 0, as well as limited reduction of Fe 3+, to Fe 2+ not Fe 0. The results (1) shed fundamental insight into the reversibility of CuFe 2O 4 materials cycled at high current density and (2) demonstrate that a synergistic effort to control both active material morphology and electrode architecture is an effective strategy for optimizing electrochemical behavior.« less

A comprehensive physicochemical, thermal, and spectroscopic characterization of zinc (II) chloride using X-ray diffraction, particle size distribution, differential scanning calorimetry, thermogravimetric analysis/differential thermogravimetric analysis, ultraviolet-visible, and Fourier transform-infrared spectroscopy.

PubMed

Trivedi, Mahendra Kumar; Sethi, Kalyan Kumar; Panda, Parthasarathi; Jana, Snehasis

2017-01-01

Zinc chloride is an important inorganic compound used as a source of zinc and has other numerous industrial applications. Unfortunately, it lacks reliable and accurate physicochemical, thermal, and spectral characterization information altogether. Hence, the authors tried to explore in-depth characterization of zinc chloride using the modern analytical technique. The analysis of zinc chloride was performed using powder X-ray diffraction (PXRD), particle size distribution, differential scanning calorimetry (DSC), thermogravimetric analysis/differential thermogravimetric analysis (TGA/DTG), ultraviolet-visible spectroscopy (UV-vis), and Fourier transform-infrared (FT-IR) analytical techniques. The PXRD patterns showed well-defined, narrow, sharp, and the significant peaks. The crystallite size was found in the range of 14.70-55.40 nm and showed average crystallite size of 41.34 nm. The average particle size was found to be of 1.123 ( d 10 ), 3.025 ( d 50 ), and 6.712 ( d 90 ) μm and average surface area of 2.71 m 2 /g. The span and relative span values were 5.849 μm and 1.93, respectively. The DSC thermogram showed a small endothermic inflation at 308.10°C with the latent heat (ΔH) of fusion 28.52 J/g. An exothermic reaction was observed at 449.32°C with the ΔH of decomposition 66.10 J/g. The TGA revealed two steps of the thermal degradation and lost 8.207 and 89.72% of weight in the first and second step of degradation, respectively. Similarly, the DTG analysis disclosed T max at 508.21°C. The UV-vis spectrum showed absorbance maxima at 197.60 nm (λ max ), and FT-IR spectrum showed a peak at 511/cm might be due to the Zn-Cl stretching. These in-depth, comprehensive data would be very much useful in all stages of nutraceuticals/pharmaceuticals formulation research and development and other industrial applications.