Better powder diffractometers. II—Optimal choice of U, V and W

NASA Astrophysics Data System (ADS)

Cussen, L. D.

2007-12-01

This article presents a technique for optimising constant wavelength (CW) neutron powder diffractometers (NPDs) using conventional nonlinear least squares methods. This is believed to be the first such design optimisation for a neutron spectrometer. The validity of this approach and discussion should extend beyond the Gaussian element approximation used and also to instruments using different radiation, such as X-rays. This approach could later be extended to include vertical and perhaps horizontal focusing monochromators and probably other types of instruments such as three axis spectrometers. It is hoped that this approach will help in comparisons of CW and time-of-flight (TOF) instruments. Recent work showed that many different beam element combinations can give identical resolution on CW NPDs and presented a procedure to find these combinations and also find an "optimum" choice of detector collimation. Those results enable the previous redundancy in the description of instrument performance to be removed and permit a least squares optimisation of design. New inputs are needed and are identified as the sample plane spacing ( dS) of interest in the measurement. The optimisation requires a "quality factor", QPD, chosen here to be minimising the worst Bragg peak separation ability over some measurement range ( dS) while maintaining intensity. Any other QPD desired could be substituted. It is argued that high resolution and high intensity powder diffractometers (HRPDs and HIPDs) should have similar designs adjusted by a single scaling factor. Simulated comparisons are described suggesting significant improvements in performance for CW HIPDs. Optimisation with unchanged wavelength suggests improvements by factors of about 2 for HRPDs and 25 for HIPDs. A recently quantified design trade-off between the maximum line intensity possible and the degree of variation of angular resolution over the scattering angle range leads to efficiency gains at short wavelengths. This in turn leads in practice to another trade-off between this efficiency gain and losses at short wavelength due to technical effects. The exact gains from varying wavelength depend on the details of the short wavelength technical losses. Simulations suggest that the total potential PD performance gains may be very significant-factors of about 3 for HRPDs and more than 90 for HIPDs.

Utilization of the High Flux Isotope Reactor at Oak Ridge National Laboratory

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

Selby, Douglas L; Bilheux, Hassina Z; Meilleur, Flora

2015-01-01

This paper addresses several aspects of the scientific utilization of the Oak Ridge National Laboratory High Flux Isotope Reactor (HFIR). Topics to be covered will include: 1) HFIR neutron scattering instruments and the formal instrument user program; 2) Recent upgrades to the neutron scattering instrument stations at the reactor, and 3) eMod a new tool for addressing instrument modifications and providing configuration control and design process for scientific instruments at HFIR and the Spallation Neutron Source (SNS). There are 15 operating neutron instrument stations at HFIR with 12 of them organized into a formal user program. Since the last presentationmore » on HFIR instruments at IGORR we have installed a Single Crystal Quasi-Laue Diffractometer instrument called IMAGINE; and we have made significant upgrades to HFIR neutron scattering instruments including the Cold Triple Axis Instrument, the Wide Angle Neutron Diffractometer, the Powder Diffractometer, and the Neutron Imaging station. In addition, we have initiated upgrades to the Thermal Triple Axis Instrument and the Bio-SANS cold neutron instrument detector system. All of these upgrades are tied to a continuous effort to maintain a high level neutron scattering user program at the HFIR. For the purpose of tracking modifications such as those mentioned and configuration control we have been developing an electronic system for entering instrument modification requests that follows a modification or instrument project through concept development, design, fabrication, installation, and commissioning. This system, which we call eMod, electronically leads the task leader through a series of questions and checklists that then identifies such things as ES&H and radiological issues and then automatically designates specific individuals for the activity review process. The system has been in use for less than a year and we are still working out some of the inefficiencies, but we believe that this will become a very effective tool for achieving the configuration and process control believed to be necessary for scientific instrument systems.« less

Role of Bi3+ substitution on structural, magnetic and optical properties of cobalt spinel ferrite

NASA Astrophysics Data System (ADS)

Anjum, Safia; Sehar, Fatima; Awan, M. S.; Zia, Rehana

2016-04-01

Bismuth-doped cobalt ferrite CoBi x Fe(2- x)O4 with x = 0, 0.1,0.2, 0.3, 0.4, 0.5 have been prepared using powder metallurgy route. The structural, morphological, elemental, magnetic and optical properties have been investigated using X-ray diffractometer, Fourier transform infrared spectroscopy, scanning electron microscope, energy dispersive X-rays, vibrating sample magnetometer and ultraviolet-visible spectrometer, respectively. X-ray diffractometer analysis confirms the formation of single-phase cubic spinel structure. As the substitution of larger ionic radii Bi3+ ions increases in cobalt ferrite which is responsible to increase the lattice parameters and decrease the crystallite size. SEM micrographs revealed the spherical shape of the particles with the nonuniform grain boundaries. The saturation magnetization decreases and bandgap energy increases as the concentration of non-magnetic Bi3+ ions increases.

The effect of calcination temperature on the formation and magnetic properties of ZnMn2O4 spinel

NASA Astrophysics Data System (ADS)

Hermanto, B.; Ciswandi; Afriani, F.; Aryanto, D.; Sudiro, T.

2018-03-01

The spinel based on transition-metal oxides has a typical composition of AB2O4. In this study, the ZnMn2O4 spinel was synthesized using a powder metallurgy technique. The Zn and Mn metallic powders with an atomic ratio of 1:2 were mechanically alloyed for 3 hours in aqueous solution. The mixed powder was then calcined in a muffle furnace at elevated temperature of 400, 500 and 600 °C. The X-ray Diffractometer (XRD) was used to evaluate the formation of a ZnMn2O4 spinel structure. The magnetic properties of the sample at varying calcination temperatures were characterized by a Vibrating Sample Magnetometer (VSM). The results show that the fraction of ZnMn2O4 spinel formation increases with the increase of calcination temperature. The calcination temperature also affects the magnetic properties of the samples.

Mesoporous Nitrogen Doped Carbon-Glass Ceramic Cathode for High Performance Lithium-Oxygen Battery

DTIC Science & Technology

2012-06-01

dry room with controlled moisture content. Composite 3 films on nickel foam were used as working cathodes along with lithium metal as anode and the...cathode formulation [6,7,8,9,10], efficient oxygen reduction catalysts [11,12], electrolyte compositions [13,14], effect of moisture [15], etc...specimens. Structure and purity of these materials were performed by powder X-ray diffraction (XRD) on a Rigaku D/MAX-2250 diffractometer fitted with CuKα

Edge-Selectively Functionalized Graphene-Like Platelets as a Co-curing Agent and a Nanoscale Additive to Epoxy Resin

DTIC Science & Technology

2012-08-12

21 For mass production , the Report Documentation Page Form ApprovedOMB No. 0704-0188 Public reporting burden for the collection of information is...analyzer. The field emission scanning electron microscope ( FE -SEM) used in this work was a NanoSem 230 (FEI, USA). High-resolution transmission...WAXD) powder patterns were recorded with a Rigaku RU-200 diffractometer using Ni-filtered Cu K radiation (40 kV, 100 mA,  = 0.15418 nm). Dynamic

PEARL: the high pressure neutron powder diffractometer at ISIS

NASA Astrophysics Data System (ADS)

Bull, C. L.; Funnell, N. P.; Tucker, M. G.; Hull, S.; Francis, D. J.; Marshall, W. G.

2016-10-01

The PEARL instrument at ISIS has been designed for, and dedicated to, in situ studies of materials at high pressure, using the Paris-Edinburgh press. In recent years, upgrades to the instrument have led to improvements in data quality and the range of achievable pressures and temperatures; currently 0.5-28 GPa and 80-1400 K. This paper describes the technical characteristics of the instrument, its current capabilities, and gives a brief overview of the science that has been performed, using representative examples.

Portable X-ray powder diffractometer for the analysis of art and archaeological materials

NASA Astrophysics Data System (ADS)

Nakai, Izumi; Abe, Yoshinari

2012-02-01

Phase identification based on nondestructive analytical techniques using portable equipment is ideal for the analysis of art and archaeological objects. Portable(p)-XRF and p-Raman are very widely used for this purpose, yet p-XRD is relatively rare despite its importance for the analysis of crystalline materials. This paper overviews 6 types of p-XRD systems developed for analysis of art and archaeological materials. The characteristics of each system are compared. One of the p-XRD systems developed by the authors was brought to many museums as well as many archeological sites in Egypt and Syria to characterize the cultural heritage artifacts, e.g., amulet made of Egyptian blue, blue painted pottery, and Islamic pottery from Egypt, jade from China, variscite from Syria, a Japanese classic painting drawn by Korin Ogata, and oil paintings drawn by Taro Okamoto. Practical application data are shown to demonstrate the potential ability of the method for analysis of various art and archaeological materials.

Comparison of characteristics of hydroxyapatite powders synthesized from cuttlefish bone via precipitation and ball milling techniques

NASA Astrophysics Data System (ADS)

Faksawat, K.; Kaewwiset, W.; Limsuwan, P.; Naemchanthara, K.

2017-09-01

The aim of this work was to compare characteristics of hydroxyapatite synthesized by precipitation and ball milling techniques. The cuttlefish bone powder was a precursor in calcium source and the di ammonium hydrogen orthophosphate powders was a precursor in phosphate source. The hydroxyapatite was synthesized by the both techniques such as precipitation and ball milling techniques. The phase formation, chemical structure and morphology of the both hydroxyapatite powders have been examined by X-ray diffractometer (XRD), Fourier transform infrared spectroscope (FTIR) and field emission scanning electron microscope (FESEM), respectively. The results show that the hydroxyapatite synthesized by precipitation technique formed hydroxyapatite phase slower than the hydroxyapatite synthesized by ball milling technique. The FTIR results show the chemical structures of sample in both techniques are similar. The morphology of the hydroxyapatite from the both techniques were sphere like shapes and particle size was about in nano scale. The average particle size of the hydroxyapatite by ball milling technique was less than those synthesized by precipitation technique. This experiment indicated that the ball milling technique take time less than the precipitation technique in hydroxyapatite synthesis.

In vitro study of root fracture treated by CO2 laser and DP-bioactive glass paste.

PubMed

Wang, Yin-Lin; Lee, Bor-Shiunn; Tseng, Ching-Li; Lin, Feng-Huei; Lin, Chun-Pin

2008-01-01

An ideal material has yet to be discovered that can successfully treat vertical root fracture. Therefore, the purpose of this study was to use a continuous-wave CO2 laser of medium-energy density to fuse DP-bioactive glass paste (DPGP) to vertical root fracture. The DP-bioglass powder was based on a Na2O-CaO-SiO2-P2O5 system and it was mixed with phosphoric acid (65% concentration) with a powder/liquid ratio of 2 g/4 mL to form DPGP. The interaction of DPGP and dentin was analyzed by means of X-ray diffractometer (XRD) and differential thermal analysis/thermogravimetric analysis (DTA/TGA). Root fracture line was filled with DPGP followed by CO2 laser irradiation and the result was examined by scanning electron microscopy (SEM). The main crystal phase of DPGP was monocalcium phosphate monohydrate (Ca(H2PO4)2.H2O) and the phase transformed to dicalcium phosphate dihydrate (CaHPO4.2H2O) after mixing DPGP with dentin powder (DPG-D). Additionally, gamma-Ca2P2O7 and beta-Ca2P2O7 were identified when DPG-D was lased by CO2 laser. The reaction temperature was between 500 degrees C and 1100 degrees C. SEM results demonstrated that the fracture line was effectively sealed by DPGP. The chemical reaction of DPGP and dentin indicated that DPGP combined with CO2 laser is a potential regimen for the treatment of vertical root fracture.

Tandem transmission/reflection mode XRD instrument including XRF for in situ measurement of Martian rocks and soils

NASA Astrophysics Data System (ADS)

Delhez, Robert; Van der Gaast, S. J.; Wielders, Arno; de Boer, J. L.; Helmholdt, R. B.; van Mechelen, J.; Reiss, C.; Woning, L.; Schenk, H.

2003-02-01

The mineralogy of the surface material of Mars is the key to disclose its present and past life and climates. Clay mineral species, carbonates, and ice (water and CO2) are and/or contain their witnesses. X-ray powder diffraction (XRPD) is the most powerful analytical method to identify and quantitatively characterize minerals in complex mixtures. This paper discusses the development of a working model of an instrument consisting of a reflection mode diffractometer and a transmission mode CCD-XRPD instrument, combined with an XRF module. The CCD-XRD/XRF instrument is analogous to the instrument for Mars missions developed by Sarrazin et al. (1998). This part of the tandem instrument enables "quick and dirty" analysis of powdered (!) matter to monitor semi-quantitatively the presence of clay minerals as a group, carbonates, and ices and yields semi-quantitative chemical information from X-ray fluorescence (XRF). The reflection mode instrument (i) enables in-situ measurements of rocks and soils and quantitative information on the compounds identified, (ii) has a high resolution and reveals large spacings for accurate identification, in particular of clay mineral species, and (iii) the shape of the line profiles observed reveals the kind and approximate amounts of lattice imperfections present. It will be shown that the information obtained with the reflection mode diffractometer is crucial for finding signs of life and changes in the climate on Mars. Obviously this instrument can also be used for other extra-terrestrial research.

Pressure/temperature fluid cell apparatus for the neutron powder diffractometer instrument: probing atomic structure in situ.

PubMed

Wang, Hsiu-Wen; Fanelli, Victor R; Reiche, Helmut M; Larson, Eric; Taylor, Mark A; Xu, Hongwu; Zhu, Jinlong; Siewenie, Joan; Page, Katharine

2014-12-01

This contribution describes a new local structure compatible gas/liquid cell apparatus for probing disordered materials at high pressures and variable temperatures in the Neutron Powder Diffraction instrument at the Lujan Neutron Scattering Center, Los Alamos National Laboratory. The new sample environment offers choices for sample canister thickness and canister material type. Finite element modeling is utilized to establish maximum allowable working pressures of 414 MPa at 15 K and 121 MPa at 600 K. High quality atomic pair distribution function data extraction and modeling have been demonstrated for a calibration standard (Si powder) and for supercritical and subcritical CO2 measurements. The new sample environment was designed to specifically target experimental studies of the local atomic structures involved in geologic CO2 sequestration, but will be equally applicable to a wide variety of energy applications, including sorption of fluids on nano/meso-porous solids, clathrate hydrate formation, catalysis, carbon capture, and H2 and natural gas uptake/storage.

High-resolution inelastic neutron scattering and neutron powder diffraction study of the adsorption of dihydrogen by the Cu(II) metal-organic framework material HKUST-1

NASA Astrophysics Data System (ADS)

Callear, Samantha K.; Ramirez-Cuesta, Anibal J.; David, William I. F.; Millange, Franck; Walton, Richard I.

2013-12-01

We present new high-resolution inelastic neutron scattering (INS) spectra (measured using the TOSCA and MARI instruments at ISIS) and powder neutron diffraction data (measured on the diffractometer WISH at ISIS) from the interaction of the prototypical metal-organic framework HKUST-1 with various dosages of dihydrogen gas. The INS spectra show direct evidence for the sequential occupation of various distinct sites for dihydrogen in the metal-organic framework, whose population is adjusted during increasing loading of the guest. The superior resolution of TOSCA reveals subtle features in the spectra, not previously reported, including evidence for split signals, while complementary spectra recorded on MARI present full information in energy and momentum transfer. The analysis of the powder neutron patterns using the Rietveld method shows a consistent picture, allowing the crystallographic indenisation of binding sites for dihydrogen, thus building a comprehensive picture of the interaction of the guest with the nanoporous host.

A high performance neutron powder diffractometer at 3 MW Triga Mark-II research reactor in Bangladesh

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

Kamal, I., E-mail: imtiaz-kamal26@yahoo.com; Yunus, S. M., E-mail: yunussm11@yahoo.com; Datta, T. K., E-mail: tk-datta4@yahoo.com

2016-07-12

A high performance neutron diffractometer called Savar Neutron Diffractometer (SAND) was built and installed at radial beam port-2 of TRIGA Mark II research reactor at AERE, Savar, Dhaka, Bangladesh. Structural studies of materials are being done by this technique to characterize materials crystallograpohically and magnetically. The micro-structural information obtainable by neutron scattering method is very essential for determining its technological applications. This technique is unique for understanding the magnetic behavior in magnetic materials. Ceramic, steel, electronic and electric industries can be benefited from this facility for improving their products and fabrication process. This instrument consists of a Popovicimonochromator with amore » large linear position sensitive detector array. The monochromator consists of nine blades of perfect single crystal of silicon with 6 mm thickness each. The monochromator design was optimized to provide maximum flux on 3 mm diameter cylindrical sample with a relatively flat angular dependence of resolution. Five different wave lengths can be selected by orienting the crystal at various angles. A sapphire filter was used before the primary collimator to minimize the first neutron. The detector assembly is composed of 15 linear position sensitive proportional counters placed at either 1.1 m or 1.6 m from the sample position and enclosed in a air pad supported high density polythene shield. Position sensing is obtained by charge division using 1-wide NIM position encoding modules (PEM). The PEMs communicate with the host computer via USB. The detector when placed at 1.1 m, subtends 30° (2θ) at each step and covers 120° in 4 steps. When the detector is placed at 1.6 m it subtends 20° at each step and covers 120° in 6 steps. The instrument supports both low and high temperature sample environment. The instrument supports both low and high temperature sample environment. The diffractometer is a state-of-the art technology for diffraction study in our country.« less

A high performance neutron powder diffractometer at 3 MW Triga Mark-II research reactor in Bangladesh

NASA Astrophysics Data System (ADS)

Kamal, I.; Yunus, S. M.; Datta, T. K.; Zakaria, A. K. M.; Das, A. K.; Aktar, S.; Hossain, S.; Berliner, R.; Yelon, W. B.

2016-07-01

A high performance neutron diffractometer called Savar Neutron Diffractometer (SAND) was built and installed at radial beam port-2 of TRIGA Mark II research reactor at AERE, Savar, Dhaka, Bangladesh. Structural studies of materials are being done by this technique to characterize materials crystallograpohically and magnetically. The micro-structural information obtainable by neutron scattering method is very essential for determining its technological applications. This technique is unique for understanding the magnetic behavior in magnetic materials. Ceramic, steel, electronic and electric industries can be benefited from this facility for improving their products and fabrication process. This instrument consists of a Popovicimonochromator with a large linear position sensitive detector array. The monochromator consists of nine blades of perfect single crystal of silicon with 6mm thickness each. The monochromator design was optimized to provide maximum flux on 3mm diameter cylindrical sample with a relatively flat angular dependence of resolution. Five different wave lengths can be selected by orienting the crystal at various angles. A sapphire filter was used before the primary collimator to minimize the first neutron. The detector assembly is composed of 15 linear position sensitive proportional counters placed at either 1.1 m or 1.6 m from the sample position and enclosed in a air pad supported high density polythene shield. Position sensing is obtained by charge division using 1-wide NIM position encoding modules (PEM). The PEMs communicate with the host computer via USB. The detector when placed at 1.1 m, subtends 30˚ (2θ) at each step and covers 120˚ in 4 steps. When the detector is placed at 1.6 m it subtends 20˚ at each step and covers 120˚ in 6 steps. The instrument supports both low and high temperature sample environment. The instrument supports both low and high temperature sample environment. The diffractometer is a state-of-the art technology for diffraction study in our country.

High-resolution neutron powder diffractometer SPODI at research reactor FRM II

NASA Astrophysics Data System (ADS)

Hoelzel, M.; Senyshyn, A.; Juenke, N.; Boysen, H.; Schmahl, W.; Fuess, H.

2012-03-01

SPODI is a high-resolution thermal neutron diffractometer at the research reactor Heinz Maier-Leibnitz (FRM II) especially dedicated to structural studies of complex systems. Unique features like a very large monochromator take-off angle of 155° and a 5 m monochromator-sample distance in its standard configuration achieve both high-resolution and a good profile shape for a broad scattering angle range. Two dimensional data are collected by an array of 80 vertical position sensitive 3He detectors. SPODI is well suited for studies of complex structural and magnetic order and disorder phenomena at non-ambient conditions. In addition to standard sample environment facilities (cryostats, furnaces, magnet) specific devices (rotatable load frame, cell for electric fields, multichannel potentiostat) were developed. Thus the characterisation of functional materials at in-operando conditions can be achieved. In this contribution the details of the design and present performance of the instrument are reported along with its specifications. A new concept for data reduction using a 2 θ dependent variable height for the intensity integration along the Debye-Scherrer lines is introduced.

Neutron diffraction studies for realtime leaching of catalytic Ni

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

Iles, Gail N., E-mail: gail.iles@helmholtz-berlin.de; Reinhart, Guillaume, E-mail: guillaume.reinhart@im2np.fr; Institut Laue-Langevin, 6 rue Jules Horowitz, BP 156, 38042 Grenoble

2014-07-21

The leaching of Al from intermetallic samples of Nickel Aluminium alloys to form Raney-type nickel catalysts is widely used in the hydrogenation industry, however, little is known of the leaching process itself. In this study, the leaching of Al was measured in realtime, in situ, using the high-flux powder neutron diffractometer, D20, at the Institut Laue-Langevin. Despite the liberation of hydrogen and effervescent nature of the reaction the transformation of the dry powder phases into Raney-type Ni was determined. Samples produced by gas-atomisation were found to leach faster than those produced using the cast and crushed technique. Regardless of processingmore » route of the precursor powder, the formation of spongy-Ni occurs almost immediately, while Ni{sub 2}Al{sub 3} and NiAl{sub 3} continue to transform over longer periods of time. Small-angle scattering and broadening of the diffraction peaks is an evidence for the formation of the smaller Ni particles. Understanding the kinetics of the leaching process will allow industry to refine production of catalysts for optimum manufacturing time while knowledge of leaching dynamics of powders produced by different manufacturing techniques will allow further tailoring of catalytic materials.« less

POWTEX Neutron Diffractometer at FRM II - New Perspectives in Rock Deformation and Recrystallisation Analysis

NASA Astrophysics Data System (ADS)

Walter, J. M.; Stipp, M.; Ullemeyer, K.; Klein, H.; Leiss, B.; Hansen, B.; Kuhs, W. F.

2011-12-01

Neutron diffraction has become a routine method in Geoscience for the quantitative analysis of crystallographic preferred orientations (CPOs) and for (experimental) powder diffraction. Quantitative texture analysis is a common tool for the investigation of fabric development in mono- and polyphase rocks, their deformation histories and kinematics. Furthermore the quantitative characterization of anisotropic physical properties by bulk texture measurements can be achieved due to the high penetration capabilities of neutrons. To cope with increasing needs for beam time at neutron diffraction facilities with the corresponding technical characteristics and equipment, POWTEX (POWder and TEXture Diffractometer) is designed as a high-intensity diffractometer at the neutron research reactor FRM II in Garching, Germany by groups from the RWTH Aachen, Forschungszentrum Jülich and the University of Göttingen. Complementary to existing neutron diffractometers (SKAT at Dubna, Russia; GEM at ISIS, UK; HIPPO at Los Alamos, USA; D20 at ILL, France; and the local STRESS-SPEC and SPODI at FRM II) the layout of POWTEX is focused on fast (texture) measurements for either time-resolved experiments or the measurement of larger sample series as necessary for the study of large scale geological structures. By utilizing a range of neutron wavelengths simultaneously (TOF-technique), a high flux (~1 x 107 n/cm2s) and a high detector coverage ( 9.8 sr) effective texture measurements without sample tilting and rotation are possible. Furthermore the instrument and the angular detector resolution is sufficient for strong recrystallisation textures as well as weak textures of polyphase rocks. Thereby large sample environments will be implemented at POWTEX allowing in-situ time-resolved texture measurements during deformation experiments on rocksalt, ice and other materials. Furthermore a furnace for 3D-recrystallisation analysis of single grains will be realized complementary to the furnace that already exists for fine grained materials at the synchrotron beamline BW5 at HASYLAB, Germany (e.g. Klein et al. 2009). The in-situ triaxial deformation apparatus is operated by a uniaxial spindle drive with a maximum axial load of 200 kN, which will be redesigned to minimize shadowing effects on the detector. The HT experiments will be carried out in uniaxial compression or extension and an upgrade to triaxial deformation conditions is envisaged. The load frame can alternatively be used for ice deformation by inserting a cryostat cell for temperatures down to 77 K with a triaxial apparatus allowing also simple shear experiments on ice. Strain rates range between 10-8 and 10-3 s-1 reaching to at least 50 % axial strain. The furnace for the recrystallization analysis will be a mirror furnace with temperatures up to 1500° C, which will be rotatable around a vertical axis to obtain the required stereologic orientation information.

Pressure/temperature fluid cell apparatus for the neutron powder diffractometer instrument: Probing atomic structure in situ

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

Wang, Hsiu-Wen; Fanelli, Victor R.; Reiche, Helmut M.

This contribution describes a new local structure compatible gas/liquid cell apparatus for probing disordered materials at high pressures and variable temperatures in the Neutron Powder Diffraction instrument at the Lujan Neutron Scattering Center, Los Alamos National Laboratory. The new sample environment offers choices for sample canister thickness and canister material type. Finite element modeling is utilized to establish maximum allowable working pressures of 414 MPa at 15 K and 121 MPa at 600 K. High quality atomic pair distribution function data extraction and modeling have been demonstrated for a calibration standard (Si powder) and for supercritical and subcritical CO{sub 2}more » measurements. The new sample environment was designed to specifically target experimental studies of the local atomic structures involved in geologic CO{sub 2} sequestration, but will be equally applicable to a wide variety of energy applications, including sorption of fluids on nano/meso-porous solids, clathrate hydrate formation, catalysis, carbon capture, and H{sub 2} and natural gas uptake/storage.« less

Pressure/temperature fluid cell apparatus for the neutron powder diffractometer instrument: Probing atomic structure in situ

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

Wang, Hsiu -Wen; Fanelli, Victor R.; Reiche, Helmut M.

This contribution describes a new local structure compatible gas/liquid cell apparatus for probing disordered materials at high pressures and variable temperatures in the Neutron Powder Diffraction instrument at the Lujan Neutron Scattering Center, Los Alamos National Laboratory. The new sample environment offers choices for sample canister thickness and canister material type. Finite element modeling is utilized to establish maximum allowable working pressures of 414 MPa at 15 K and 121 MPa at 600 K. High quality atomic pair distribution function data extraction and modeling have been demonstrated for a calibration standard (Si powder) and for supercritical and subcritical CO 2measurements.more » As a result, the new sample environment was designed to specifically target experimental studies of the local atomic structures involved in geologic CO 2 sequestration, but will be equally applicable to a wide variety of energy applications, including sorption of fluids on nano/meso-porous solids, clathrate hydrate formation, catalysis, carbon capture, and H 2 and natural gas uptake/storage.« less

Pressure/temperature fluid cell apparatus for the neutron powder diffractometer instrument: Probing atomic structure in situ

DOE PAGES

Wang, Hsiu -Wen; Fanelli, Victor R.; Reiche, Helmut M.; ...

2014-12-24

This contribution describes a new local structure compatible gas/liquid cell apparatus for probing disordered materials at high pressures and variable temperatures in the Neutron Powder Diffraction instrument at the Lujan Neutron Scattering Center, Los Alamos National Laboratory. The new sample environment offers choices for sample canister thickness and canister material type. Finite element modeling is utilized to establish maximum allowable working pressures of 414 MPa at 15 K and 121 MPa at 600 K. High quality atomic pair distribution function data extraction and modeling have been demonstrated for a calibration standard (Si powder) and for supercritical and subcritical CO 2measurements.more » As a result, the new sample environment was designed to specifically target experimental studies of the local atomic structures involved in geologic CO 2 sequestration, but will be equally applicable to a wide variety of energy applications, including sorption of fluids on nano/meso-porous solids, clathrate hydrate formation, catalysis, carbon capture, and H 2 and natural gas uptake/storage.« less

X-ray investigations related to the shock history of the Shergotty achondrite

NASA Technical Reports Server (NTRS)

Horz, F.; Hanss, R.; Serna, C.

1986-01-01

The shock stress suffered by naturally shocked materials from the Shergotty achondrite was studied using X-ray diffraction techniques and experimentally shocked augite and enstatite as standards. The Shergotty pyroxenes revealed the formation of continuous diffraction rings, line broadening, preferred orientation of small scale diffraction domains, and other evidence of substantial lattice disorders. As disclosed by the application of Debye-Scherrer techniques, they are hybrids between single crystals and fine-grained random powders. The pyroxene lattice is very resistant to shock damage on smaller scales. While measurable lattice disaggregation and progressive fragmentation occur below 25 GPa, little additional damage is suffered from application of pressures between 30 to 60 GPa, making pressure calibration of naturally shocked pyroxenes via X-ray methods difficult. Powder diffractometer scans on pure maskelynite fractions of Shergotty revealed small amounts of still coherently diffracting plagioclase, which may contribute to the high refractive indices of the diaplectic feldspar glasses of Shergotty.

Macromolecular powder diffraction : structure solution via molecular.

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

Doebbler, J.; Von Dreele, R.; X-Ray Science Division

Macromolecular powder diffraction is a burgeoning technique for protein structure solution - ideally suited for cases where no suitable single crystals are available. Over the past seven years, pioneering work by Von Dreele et al. [1,2] and Margiolaki et al. [3,4] has demonstrated the viability of this approach for several protein structures. Among these initial powder studies, molecular replacement solutions of insulin and turkey lysozyme into alternate space groups were accomplished. Pressing the technique further, Margiolaki et al. [5] executed the first molecular replacement of an unknown protein structure: the SH3 domain of ponsin, using data from a multianalyzer diffractometer.more » To demonstrate that cross-species molecular replacement using image plate data is also possible, we present the solution of hen egg white lysozyme using the 60% identical human lysozyme (PDB code: 1LZ1) as the search model. Due to the high incidence of overlaps in powder patterns, especially in more complex structures, we have used extracted intensities from five data sets taken at different salt concentrations in a multi-pattern Pawley refinement. The use of image plates severely increases the overlap problem due to lower detector resolution, but radiation damage effects are minimized with shorter exposure times and the fact that the entire pattern is obtained in a single exposure. This image plate solution establishes the robustness of powder molecular replacement resulting from different data collection techniques.« less

Octahedral deformations and cationic displacements in the ferroelectric PbHf(0.8)Ti(0.2)O(3): a neutron powder diffraction study from 10 to 770 K

PubMed

Muller; Baudour; Bedoya; Bouree; Soubeyroux; Roubin

2000-02-01

Neutron powder diffraction data, collected over the temperature range 10-770 K, have been analysed in order to make a detailed characterization of the sequence of phase transitions occurring in the Hf-rich ferroelectric PbHf(0.8)Ti(0.2)O3, titanium hafnium lead oxide. Over the whole temperature range this compound undergoes two phase transitions, which involve cationic displacements and octahedral deformations (tilt and/or distortion) leading to strongly distorted perovskite-type structures. The first transition appears around 415 K between two ferroelectric rhombohedral phases: a low-temperature nonzero-tilt phase F(RL) (space group R3c) and an intermediate zero-tilt phase FRH (space group R3m). The second one, detected around 520 K, is associated with a ferroelectric to-paraelectric transition between the FRH phase and the Pc cubic phase (space group Pm3m). From high-resolution neutron powder diffraction data (diffractometer 3T2-LLB, Saclay, France, lambda = 1.2251 A), the crystallographic structure of the three successive phases has been accurately determined at the following temperatures: T = 10 K (FRL): space group R3c, Z = 6, a(hex) = 5.7827 (1), c(hex) = 14.2702 (4) A, V(hex) = 413.26 (2) A3; T = 150 K (F(RL)): space group R3c, Z = 6, a(hex) = 5.7871 (1), C(hex) = 14.2735 (4) A, V(hex) = 413.98 (3) A3; T = 290 K (FRL): space group R3c, Z = 6, a(hex) = 5.7943 (1), C(hex) = 14.2742 (5) A, V(hex) = 415.04 (3) A3; T = 440 K (F(RH)): space group R3c, Z = 6, a(hex) = 5.8025 (1), c(hex) = 14.2648 (4) A, V(hex) = 415.94 (3) A3; T = 520 K (Pc): space group Pm3m, Z = 1, a(cub) = 4.1072 (2) A, V(cub) = 69.29 (1) A3. In addition, a neutron powder thermodiffractometry experiment, performed between 290 and 770 K (diffractometer D1B-ILL, Grenoble, France, lambda = 2.533 A), has been used to study in situ the temperature-induced phase transitions. From sequential Rietveld refinements, the temperature dependence of the cation displacements and the rotation and/or distortion of oxygen octahedra was derived.

Early Years of Neutron Scattering and Its Manpower Development in Indonesia

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

Marsongkohadi

In this paper I shall give a short history of the development of neutron scattering at the Research Centre for Nuclear Techniques (PPTN), in Bandung, and the early development of a more advanced facilities at the Neutron Scattering Laboratory (NSL BATAN), Centre of Technology for Nuclear Industrial Materials, in Serpong. The first research reactor in Indonesia was the TRIGA MARK II in Bandung, which became operational in 1965, with a power of 250 KW, upgraded to 1 MW in 1971, and to 2 MW in 2000. The neutron scattering activities was started in 1967, with the design and construction ofmore » the first powder diffractometer, and put in operation in 1970. It was followed by the second instrument, the filter detector spectrometer built in 1975 in collaboration with the Bhabha Atomic Research Centre (BARC), India. A powder diffractometer for magnetic studies was built in 1980, and finally, a modification of the filter detector spectrometer to measure textures was made in 1986. A brief description of the design and construction of the instruments, and a highlight of some research topics will be presented. Early developments of neutron scattering activities at the 30 MW, RSG-GAS reactor in Serpong in choosing suitable research program, which will be mainly centred around materials testing/characterization, and materials/condensed matter researches has been agreed. Instrument planning and layout which were appropriate to carry out the program had been decided. Manpower development for the neutron scattering laboratory is a severe problem. The efforts to overcome this problem has been solved. International Cooperation through workshops and on the job trainings also support the supply of qualified manpower.« less

Effect of rice variety on the physicochemical properties of the modified rice powders and their derived mucoadhesive gels.

PubMed

Okonogi, Siriporn; Kaewpinta, Adchareeya; Khongkhunthian, Sakornrat; Yotsawimonwat, Songwut

2015-06-01

In the present study; the glutinous Niaw Sanpatong (NSP) and Niaw Koko-6 (NKK), and the non-glutinous Jasmine (JM) and Saohai (SH) were chemically modified. The difference of these rice varieties on the physicochemical characteristics of the modified rice powders and the properties of the derived gels were evaluated. X-ray diffractometer was used for crystalline structure investigation of the rice powders and gels. A parallel plate rheometer was used to measure the rheological property of the gels. It was found that the non-glutinous varieties produced gels with higher mucoadhesive properties than the glutinous rice. Rheological behavior of JM and SH gels was pseudoplastic without yield value whereas that of NSP and NKK gels was plastic with the yield values of 1077.4 ± 185.9 and 536.1 ± 45.8 millipascals-second (mPas), respectively. These different properties are considered to be due to the amylose content in different rice variety. The results suggest that the non-glutinous rice varieties with high amylose content are the most suitable for preparing gels as local delivery systems via the mucosal membrane.

Microstructure control of SOFC cathode material: The role of dispersing agent

NASA Astrophysics Data System (ADS)

Ismail, Ismariza; Jani, Abdul Mutalib Md; Osman, Nafisah

2017-09-01

In the present works, La0.6Sr0.4Co0.2Fe0.8O3-δ (LSCF) cathode powders were synthesized by a sol-gel method with the aid of ethylene glycol which served as the dispersing agent. The phase formation and morphology of the powders were examined by X-Ray diffractometer (XRD) and field emission scanning electron microscopy (FESEM), respectively. The electrochemical properties of the synthesized cathode were obtained using an electrochemical impedance spectroscopy (EIS). The characteristic peaks for LSCF phase appears in the X-ray diffractogram after calcined at 500 °C and complete formation of LSCF single phase was attained at 700 °C. FESEM micrographs showed the presence of spherical particles of the powders with approximate particle size between 10 to 60 nm along with agglomerate morphologies. Well dispersed particles and fewer aggregates were observed for samples prepared with addition of ethylene glycol as the synthesizing aid. The surface area obtained for powder sample prepared with the aid of dispersing agent is 12.0 m2g-1. The EIS measurement results depicts a lower area specific resistance (ASR) obtained for sample prepared with addition of the ethylene glycol as compared to the pristine sample. The present results encourage the optimization of the cathode particle design in order to further improve the cathode performance.

Non-platinum metal-organic framework based electro-catalyst for promoting oxygen reduction reaction

NASA Astrophysics Data System (ADS)

Das, Dipanwita; Raut, Vrushali; Kireeti, Kota V. M. K.; Jha, Neetu

2018-04-01

We developed two non-precious Metal Organic Framework (MOF) based electrocatalysts, MOF-5 and MOF-i using solvothermal and refluxing methods. The MOFs prepared has been characterized by powder X-ray diffractometer (XRD), Fourier Transform Infra-Red Spectroscopy (FTIR) and Scanning Electron Microscopy (SEM) for structural and morphological insights. SEM images reveal cubic shape for solvothermally synthesized MOF-5, whereas refluxing method leads to platelet morphology of MOF-i. The synthesized MOFs has been investigated for Oxygen Reduction Reaction (ORR) studies using Cyclic Voltammetry (CV) and Linear Sweep Voltammetry (LSV), with MOF modified Glassy Carbon (GC) as working electrode. The electrochemical data suggests higher activity of MOF-5 towards ORR compared to MOF-i.

High-resolution neutron diffraction study of microstructural changes in nanocrystalline ball-milled niobium carbide NbC{sub 0.93}

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

Balagurov, Anatoly M.; Bobrikov, Ivan A.; Bokuchava, Gizo D.

2015-11-15

High resolution neutron diffraction was applied for elucidating of the microstructural evolution of nanocrystalline niobium carbide NbC{sub 0.93} powders subjected to high-energy ball milling. The diffraction patterns were collected with the high resolution Fourier diffractometer HRFD by using the reverse time-of-flight (RTOF) mode of data acquisition. The traditional single diffraction line analysis, the Rietveld method and more advanced Whole Powder Pattern Modeling technique were applied for the data analysis. The comparison of these techniques was performed. It is established that short-time milling produces a non-uniform powder, in which two distinct fractions with differing microstructure can be identified. Part of themore » material is in fact milled efficiently, with a reduction in grain size, an increase in the quantity of defects, and a corresponding tendency to decarburize reaching a composition NbC{sub 0.80} after 15 h of milling. The rest of the powder is less efficiently processed and preserves its composition and lower defect content. Larger milling times should have homogenized the system by increasing the efficiently milled fraction, but the material is unable to reach a uniform and homogeneous state. It is definitely shown that RTOF neutron diffraction patterns can provide the very accurate data for microstructure analysis of nanocrystalline powders. - Highlights: • The NbC{sub 0.93} powder was processed by high-energy ball milling. • The microstrain and dislocation density increase with milling time increase. • The corresponding decrease in crystallite size with milling time was observed. • The material exhibits the presence of two fractions after ball milling. • The RTOF neutron diffraction data are suitable for accurate microstructure analysis.« less

Synthesis of BaTiO3 and Ba(ZrxTi1-X)O3 by using the soft combustion method

NASA Astrophysics Data System (ADS)

Ahmad, Atiqah; Razak, Khairunisak Abdul

2017-07-01

In this work, barium titanate, BaTiO3 (BT) and Zr doped BT, BaZrxTi1-xO3 (BZT) with powders were successfully produced using the soft combustion method. Barium nitrate and titanium (IV) isopropoxide were used as the starting materials while zirconium (IV) oxynitrate hydrate as the doping precursors, and glycine as the combustion agent. The produced powders were pressed into 12 mm diameter pellets by using 150 MPa cold press. The effect of Zr dopant in BT was studied with molar ratio of x = 0.00, 0.03, 0.05, 0.08 and 0.10. The phase presence was identified using X-ray diffractometer. Morphology of powders and sintered pellets was observed using a scanning electron microscope. Density of the sintered pellets was measured by using Archimedes' principle, while dielectric properties were analysed by using an LCR meter. Pure perovskite BT and BZT structure were obtained after sintering at 1400 °C for 5 h. BZT with x = 0.03 has grain size of 3.9 µm and shows the highest dielectric constant of 525, compared to undoped BT that has the average grain size of 4.2 µm with dielectric constant 223. The results is in agreement with microstructure observation and density of the sample.

Polymorphism of Alprazolam (Xanax): a review of its crystalline phases and identification, crystallographic characterization, and crystal structure of a new polymorph (form III).

PubMed

de Armas, Héctor Novoa; Peeters, Oswald M; Van den Mooter, Guy; Blaton, Norbert

2007-05-01

A new polymorphic form of Alprazolam (Xanax), 8-chloro-1-methyl-6-phenyl-4H-[1,2,4]triazolo-[4,3-alpha][1,4]benzodiazepine, C(17)H(13)ClN(4), has been investigated by means of X-ray powder diffraction (XRPD), single crystal X-ray diffraction, and differential scanning calorimetry (DSC). This polymorphic form (form III) was obtained during DSC experiments after the exothermic recrystallization of the melt of form I. The crystal unit cell dimensions for form III were determined from diffractometer methods. The monoclinic unit cell found for this polymorph using XRPD after indexing the powder diffractogram was confirmed by the cell parameters obtained from single crystal X-ray diffractometry on a crystal isolated from the DSC pans. The single crystal unit cell parameters are: a = 28.929(9), b = 13.844(8), c = 7.361(3) angstroms, beta = 92.82(3) degrees , V = 2944(2) angstroms(3), Z = 8, space group P2(1) (No.4), Dx = 1.393 Mg/m(3). The structure obtained from single crystal X-ray diffraction was used as initial model for Rietveld refinement on the powder diffraction data of form III. The temperature phase transformations of alprazolam were also studied using high temperature XRPD. A review of the different phases available in the Powder Diffraction File (PDF) database for this drug is described bringing some clarification and corrections. (c) 2007 Wiley-Liss, Inc. and the American Pharmacists Association.

Unconventional Synthesis of γ-Fe2O3: Excellent Low-Concentration Ethanol Sensing Performance

NASA Astrophysics Data System (ADS)

Naskar, Atanu; Narjinary, Mousumi; Kundu, Susmita

2017-01-01

This study reports on a simple unconventional procedure for synthesis of γ-Fe2O3 nanopowder and its fabrication as a resistive ethanol sensor. γ-Fe2O3 powder having an average particle size of ˜15 nm was prepared by thermal decomposition of iron(III) acetylacetonate. Platinum incorporation (0.5-1.5 wt.%) was also carried out for enhancing sensing performance. The powders were characterized using an x-ray diffractometer, x-ray photoelectron spectroscopy, Brunauer-Emmett-Teller surface area, field area scanning electron microscopy, transmission electron microscopy along with energy dispersion x-ray analyses. Sensor fabricated from pure γ-Fe2O3 exhibited excellent ethanol sensing performance at concentrations down to 1 ppm, having a great demand in medical diagnosis and food-processing industries. The response observed for pure γ-Fe2O3 (˜75% for 1 ppm ethanol) was enhanced ˜10% after 1 wt.% Pt impregnation. Sensors were quite stable and selective towards ethanol vapour detection. A possible mechanism for high sensing performance has been discussed.

Crystal growth, structural, thermal and mechanical behavior of l-arginine 4-nitrophenolate 4-nitrophenol dihydrate (LAPP) single crystals.

PubMed

Mahadevan, M; Ramachandran, K; Anandan, P; Arivanandhan, M; Bhagavannarayana, G; Hayakawa, Y

2014-12-10

Single crystals of l-arginine 4-nitrophenolate 4-nitrophenol dihydrate (LAPP) have been grown successfully from the solution of l-arginine and 4-nitrophenol. Slow evaporation of solvent technique was adopted to grow the bulk single crystals. Single crystal X-ray diffraction analysis confirms the grown crystal has monoclinic crystal system with space group of P21. Powder X-ray diffraction analysis shows the good crystalline nature. The crystalline perfection of the grown single crystals was analyzed by HRXRD by employing a multicrystal X-ray diffractometer. The functional groups were identified from proton NMR spectroscopic analysis. Linear and nonlinear optical properties were determined by UV-Vis spectrophotometer and Kurtz powder technique respectively. It is found that the grown crystal has no absorption in the green wavelength region and the SHG efficiency was found to be 2.66 times that of the standard KDP. The Thermal stability of the crystal was found by obtaining TG/DTA curve. The mechanical behavior of the grown crystal has been studied by Vicker's microhardness method. Copyright © 2014 Elsevier B.V. All rights reserved.

Morphological and Wear behaviour of new Al-SiCmicro-SiCnano hybrid nanocomposites fabricated through powder metallurgy

NASA Astrophysics Data System (ADS)

Arif, Sajjad; Tanwir Alam, Md; Aziz, Tariq; Ansari, Akhter H.

2018-04-01

In the present work, aluminium matrix composites reinforced with 10 wt% SiC micro particles along with x% SiC nano particles (x = 0, 1, 3, 5 and 7 wt%) were fabricated through powder metallurgy. The fabricated hybrid composites were characterized by x-ray diffractometer (XRD), scanning electron microscope (SEM), energy dispersive spectrum (EDS) and elemental mapping. The relative density, hardness and wear behaviour of all hybrid nanocomposites were studied. The influence of various control factors like SiC reinforcement, sliding distance (300, 600, 900 and 1200 m) and applied load (20, 30 and 40 N) were explored using pin-on-disc wear apparatus. The uniform distribution of micro and nano SiC particles in aluminium matrix is confirmed by elemental maps. The hardness and wear test results showed that properties of the hybrid composite containing 5 wt% nano SiC was better than other hybrid composites. Additionally, the wear loss of all hybrid nanocomposites increases with increasing sliding distance and applied load. The identification of wear phenomenon were studied through the SEM images of worn surface.

Estimation of Crystallinity of Nifedipine-Polyvinylpyrrolidone Solid Dispersion by Usage of Terahertz Time-Domain Spectroscopy and of X-Ray Powder Diffractometer.

PubMed

Takeuchi, Issei; Shimakura, Kemmaro; Kuroda, Hideki; Nakajima, Takehisa; Goto, Satoru; Makino, Kimiko

2015-12-01

Crystalline state of pharmaceutical materials is of great importance in preparation of pharmaceutics, because their physicochemical properties affect bioavailability, quality of products, therapeutic level and manufacturing process. In this study, we have estimated time-dependent changes of nifedipine in nifedipine-polyvinylpyrrolidone (PVP) solid dispersion by measuring terahertz time-domain spectroscopy (THz-TDS) and by X-ray powder diffractometry (XRPD), and compared their correlativity. Crystallinity of nifedipine-PVP solid dispersion was changed by storing the amorphous sample at 25°C-75°C and relative humidity of over 80% for 0.25-24.00 h. To compare the results of two types of measurements, we have used a general method of linear regression analysis. Crystallinities estimated using THz-TDS were plotted on the x-axis and that of XRPD were on the y-axis. From the result of the calculation, the correlativity of them was confirmed. THz-TDS has the capability of becoming the replacement of XRPD. © 2015 Wiley Periodicals, Inc. and the American Pharmacists Association.

Mineral carbonation of gaseous carbon dioxide using a clay-hosted cation exchange reaction.

PubMed

Kang, Il-Mo; Roh, Ki-Min

2013-01-01

The mineral carbonation method is still a challenge in practical application owing to: (1) slow reaction kinetics, (2) high reaction temperature, and (3) continuous mineral consumption. These constraints stem from the mode of supplying alkaline earth metals through mineral acidification and dissolution. Here, we attempt to mineralize gaseous carbon dioxide into calcium carbonate, using a cation exchange reaction of vermiculite (a species of expandable clay minerals). The mineralization is operated by draining NaCI solution through vermiculite powders and continuously dropping into the pool of NaOH solution with CO2 gas injected. The mineralization temperature is regulated here at 293 and 333 K for 15 min. As a result of characterization, using an X-ray powder diffractometer and a scanning electron microscopy, two types of pure CaCO3 polymorphs (vaterite and calcite) are identified as main reaction products. Their abundance and morphology are heavily dependent on the mineralization temperature. Noticeably, spindle-shaped vaterite, which is quite different from a typical vaterite morphology (polycrystalline spherulite), forms predominantly at 333 K (approximately 98 wt%).

Performance of the Taiwan Contract Beamline BL12B2 at SPring-8

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

Tang, M.-T.; Du, C.-H.; Lee, J.-F.

2004-05-12

The recent status of the SPring-8 Taiwan Contract Beamline BL12B2 is reported. The beamline was designed to provide multiple applications for materials and biological researches. It is equipped with four end stations, including an EXAFS station, a Huber 6-circle diffractometer for X-ray scattering, a curved image plate for the studies of powder diffraction, and a station for the protein crystallography. The beamline construction was completed in 2000 and it has been in full speed operation since September 2001. To enhance the focusing capacity, the beamline optics has been modified in 2002 and a gain of factor of 10 in photonmore » flux was consequently obtained at protein crystallography station.« less

Phase Transition and Texture Evolution in the Ni-Mn-Ga Ferromagnetic Shape-Memory Alloys Studied by a Neutron Diffraction Technique

NASA Astrophysics Data System (ADS)

Nie, Z. H.; Wang, Y. D.; Wang, G. Y.; Richardson, J. W.; Wang, G.; Liu, Y. D.; Liaw, P. K.; Zuo, L.

2008-12-01

The phase transition and influence of the applied stress on the texture evolution in the as-cast Ni-Mn-Ga ferromagnetic shape-memory alloys were studied by the time-of-flight (TOF) neutron diffraction technique. The neutron diffraction experiments were performed on the General Purpose Powder Diffractometer (Argonne National Laboratory). Inverse pole figures were determined from the neutron data for characterizing the orientation distributions and variant selections of polycrystalline Ni-Mn-Ga alloys subjected to different uniaxial compression deformations. Texture analyses reveal that the initial texture for the parent phase in the as-cast specimen was composed of {left\\{ {{text{001}}} right\\}}{left< {{text{100}}} rightrangle } , {left\\{ {{text{001}}} right\\}}{left< {{text{110}}} rightrangle } , {left\\{ {{text{011}}} right\\}}{left< {{text{100}}} rightrangle } , and {left\\{ {{text{011}}} right\\}}{left< {{text{110}}} rightrangle } , which was weakened after the compression deformation. Moreover, a strong preferred selection of martensitic-twin variants ( {left\\{ {{text{110}}} right\\}}{left< {{text{001}}} rightrangle } and {left\\{ {{text{100}}} right\\}}{left< {{text{001}}} rightrangle } ) was observed in the transformed martensite after a compression stress applied on the parent phase along the cyclindrical axis of the specimens. The preferred selection of variants can be well explained by considering the grain/variant-orientation-dependent Bain-distortion energy.

Fundamental Parameters Line Profile Fitting in Laboratory Diffractometers

PubMed Central

Cheary, R. W.; Coelho, A. A.; Cline, J. P.

2004-01-01

The fundamental parameters approach to line profile fitting uses physically based models to generate the line profile shapes. Fundamental parameters profile fitting (FPPF) has been used to synthesize and fit data from both parallel beam and divergent beam diffractometers. The refined parameters are determined by the diffractometer configuration. In a divergent beam diffractometer these include the angular aperture of the divergence slit, the width and axial length of the receiving slit, the angular apertures of the axial Soller slits, the length and projected width of the x-ray source, the absorption coefficient and axial length of the sample. In a parallel beam system the principal parameters are the angular aperture of the equatorial analyser/Soller slits and the angular apertures of the axial Soller slits. The presence of a monochromator in the beam path is normally accommodated by modifying the wavelength spectrum and/or by changing one or more of the axial divergence parameters. Flat analyzer crystals have been incorporated into FPPF as a Lorentzian shaped angular acceptance function. One of the intrinsic benefits of the fundamental parameters approach is its adaptability any laboratory diffractometer. Good fits can normally be obtained over the whole 20 range without refinement using the known properties of the diffractometer, such as the slit sizes and diffractometer radius, and emission profile. PMID:27366594

SMARTSware for SMARTS users to facilitate data reduction and data analysis

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

2005-01-01

The software package SMARTSware is made by one of the instrument scientist on the engineering neutron diffractometer SMARTS at the Lujan Center, a national user facility at Los Alamos Neutron Scattering Center (LANSCE). The purpose of the software is to facilitate the data analysis of powder diffraction data recorded at the Lujan Center, and hence the target audience is users performing experiments at the one of the powder diffractometers (SMARTS, HIPPO, HIPD and NPDF) at the Lujan Center. The beam time at the Lujan Center is allocated by peer review of internally and extenally submitted proposals, and therefore many ofmore » the users who are granted beam time are from the international science community. Generally, the users are only at the Lujan Center for a short period of time while they are performing the experiments, and often they leave with several data sets that have not been analyzed. The distribution of the SMARTSware software package will minimize their efforts when analyzing the data once they are back at their institution. Description of software: There are two main parts of the software; a part used to generate instrument parameter files from a set of calibration runs (Smartslparm, SmartsBin, SmartsFitDif and SmartsFitspec); and a part that facilitates the batch refinement of multiple diffraction patterns (SmartsRunRep, SmartsABC, SmartsSPF and SmartsExtract). The former part may only be peripheral to most users, but is a critical part of the instrument scientists' efforts in calibrating their instruments. The latter part is highly applicable to the users as they often need to analyze or re-analyze large sets of data. The programs within the SMARTSware package heavily rely on GSAS for the Rietveld and single peak refinements of diffraction data. GSAS (General Structure Analysis System) is a public available software also originating from LANL. Subroutines and libraries from the NeXus project (a world wide trust to standardize diffraction data formats) and National Center for Supercomputing Applications (NCSA) at the University of Illinois (the Hierarchical Data Format Software Library and Utilities) are used in the programs. All these subroutines and libraries are publicly available through the GNU Public License and/or Freeware. The package also contains sample input and output text files and a manual (LA-UR 04-6581). The executables and sample files will be available for down load at http://public.lanl.gov/clausen/SMARTSware.html and ftp://lansce.lanl.gov/clausen/SMARTSware/SMARTSware.zip, but the source codes will only be made available by written request to clausen@lanl.gov.« less

POWTEX Neutron Diffractometer at FRM II - New Perspectives for In-Situ Rock Deformation Analysis

NASA Astrophysics Data System (ADS)

Walter, J. M.; Stipp, M.; Ullemeyer, K.; Klein, H.; Leiss, B.; Hansen, B. T.; Kuhs, W. F.

2012-04-01

In Geoscience quantitative texture analysis here defined as the quantitative analysis of the crystallographic preferred orientation (CPO), is a common tool for the investigation of fabric development in mono- and polyphase rocks, their deformation histories and kinematics. Bulk texture measurements also allow the quantitative characterisation of the anisotropic physical properties of rock materials. A routine tool to measure bulk sample volumes is neutron texture diffraction, as neutrons have large penetration capabilities of several cm in geological sample materials. The new POWTEX (POWder and TEXture) Diffractometer at the neutron research reactor FRM II in Garching, Germany is designed as a high-intensity diffractometer by groups from the RWTH Aachen, Forschungszentrum Jülich and the University of Göttingen. Complementary to existing neutron diffractometers (SKAT at Dubna, Russia; GEM at ISIS, UK; HIPPO at Los Alamos, USA; D20 at ILL, France; and the local STRESS-SPEC and SPODI at FRM II) the layout of POWTEX is focused on fast time-resolved experiments and the measurement of larger sample series as necessary for the study of large scale geological structures. POWTEX is a dedicated beam line for geoscientific research. Effective texture measurements without sample tilting and rotation are possible firstly by utilizing a range of neutron wavelengths simultaneously (Time-of-Flight technique) and secondly by the high detector coverage (9.8 sr) and a high flux (~1 - 107 n/cm2s) at the sample. Furthermore the instrument and the angular detector resolution is designed also for strong recrystallisation textures as well as for weak textures of polyphase rocks. These instrument characteristics allow in-situ time-resolved texture measurements during deformation experiments on rocksalt, ice and other materials as large sample environments will be implemented at POWTEX. The in-situ deformation apparatus is operated by a uniaxial spindle drive with a maximum axial load of 250 kN, which will be redesigned to minimize shadowing effects inside the cylindrical detector. The HT deformatione experiments will be carried out in uniaxial compression or extension and an upgrade to triaxial deformation conditions is envisaged. The load frame can alternatively be used for ice deformation by inserting a cryostat cell for temperatures down to 77 K with a triaxial apparatus allowing also simple shear experiments on ice. Strain rates range between 10-8 and 10-3 s-1 reaching to at least 50 % axial strain. The deformation apparatus is designed for continuous long-term deformation experiments and can be exchanged between in-situ and ex-situ placements during continuous operation inside and outside the neutron detector.

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

Magnetic and Structural Characterization of Fe-Ga Using Kerr Microscopy and Neutron Scattering

DTIC Science & Technology

2010-01-01

117 4.6 Schematic of triple axes single crystal neutron diffractometer (left). TriCS intrument at Paul Scherrer Institut, Switzerland (right...Therefore, USANS data is one-dimensional. 4.3.3 Single Crystal Neutron Diffraction The single crystal neutron diffractometer, TriCS at Paul Scherrer...crystal neutron diffractometer (left). TriCS intrument at Paul Scherrer Institut, Switzerland (right) [106] 4.4 Unpolarized SANS In this section, SANS

Standard Reference Material (SRM 1990) for Single Crystal Diffractometer Alignment

USGS Publications Warehouse

Wong-Ng, W.; Siegrist, T.; DeTitta, G.T.; Finger, L.W.; Evans, H.T.; Gabe, E.J.; Enright, G.D.; Armstrong, J.T.; Levenson, M.; Cook, L.P.; Hubbard, C.R.

2001-01-01

An international project was successfully completed which involved two major undertakings: (1) a round-robin to demonstrate the viability of the selected standard and (2) the certification of the lattice parameters of the SRM 1990, a Standard Reference Material?? for single crystal diffractometer alignment. This SRM is a set of ???3500 units of Cr-doped Al2O3, or ruby spheres [(0 420.011 mole fraction % Cr (expanded uncertainty)]. The round-robin consisted of determination of lattice parameters of a pair of crystals' the ruby sphere as a standard, and a zeolite reference to serve as an unknown. Fifty pairs of crystals were dispatched from Hauptman-Woodward Medical Research Institute to volunteers in x-ray laboratories world-wide. A total of 45 sets of data was received from 32 laboratories. The mean unit cell parameters of the ruby spheres was found to be a=4.7608 A?? ?? 0.0062 A??, and c=12.9979 A?? ?? 0.020 A?? (95 % intervals of the laboratory means). The source of errors of outlier data was identified. The SRM project involved the certification of lattice parameters using four well-aligned single crystal diffractometers at (Bell Laboratories) Lucent Technologies and at NRC of Canada (39 ruby spheres), the quantification of the Cr content using a combined microprobe and SEM/EDS technique, and the evaluation of the mosaicity of the ruby spheres using a double-crystal spectrometry method. A confirmation of the lattice parameters was also conducted using a Guinier-Ha??gg camera. Systematic corrections of thermal expansion and refraction corrections were applied. These rubies_ are rhombohedral, with space group R3c. The certified mean unit cell parameters are a=4.76080 ?? 0.00029 A??, and c=12 99568 A?? ?? 0.00087 A?? (expanded uncertainty). These certified lattice parameters fall well within the results of those obtained from the international round-robin study. The Guinier-Ha??gg transmission measurements on five samples of powdered rubies (a=4.7610 A?? ?? 0.0013 A??, and c=12.9954 A?? ?? 0.0034 A??) agreed well with the values obtained from the single crystal spheres.

Standard Reference Material (SRM 1990) For Single Crystal Diffractometer Alignment

PubMed Central

Wong-Ng, W.; Siegrist, T.; DeTitta, G. T.; Finger, L. W.; Evans, H. T.; Gabe, E. J.; Enright, G. D.; Armstrong, J. T.; Levenson, M.; Cook, L. P.; Hubbard, C. R.

2001-01-01

An international project was successfully completed which involved two major undertakings: (1) a round-robin to demonstrate the viability of the selected standard and (2) the certification of the lattice parameters of the SRM 1990, a Standard Reference Material® for single crystal diffractometer alignment. This SRM is a set of ≈3500 units of Cr-doped Al2O3, or ruby spheres [(0.420.011 mole fraction % Cr (expanded uncertainty)]. The round-robin consisted of determination of lattice parameters of a pair of crystals: the ruby sphere as a standard, and a zeolite reference to serve as an unknown. Fifty pairs of crystals were dispatched from Hauptman-Woodward Medical Research Institute to volunteers in x-ray laboratories world-wide. A total of 45 sets of data was received from 32 laboratories. The mean unit cell parameters of the ruby spheres was found to be a=4.7608 ű0.0062 Å, and c=12.9979 ű0.020 Å (95 % intervals of the laboratory means). The source of errors of outlier data was identified. The SRM project involved the certification of lattice parameters using four well-aligned single crystal diffractometers at (Bell Laboratories) Lucent Technologies and at NRC of Canada (39 ruby spheres), the quantification of the Cr content using a combined microprobe and SEM/EDS technique, and the evaluation of the mosaicity of the ruby spheres using a double-crystal spectrometry method. A confirmation of the lattice parameters was also conducted using a Guinier-Hägg camera. Systematic corrections of thermal expansion and refraction corrections were applied. These rubies– are rhombohedral, with space group R3¯c. The certified mean unit cell parameters are a=4.76080±0.00029 Å, and c=12.99568 ű0.00087 Å (expanded uncertainty). These certified lattice parameters fall well within the results of those obtained from the international round-robin study. The Guinier-Hägg transmission measurements on five samples of powdered rubies (a=4.7610 ű0.0013 Å, and c = 12.9954 ű0.0034 Å) agreed well with the values obtained from the single crystal spheres. PMID:27500067

Preparation of Er3+:Y3Al5O12/WO3-KNbO3 composite and application in treatment of methamphetamine under ultrasonic irradiation.

PubMed

Zhang, Hongbo; Huang, Yingying; Li, Guanshu; Wang, Guowei; Fang, Dawei; Song, Youtao; Wang, Jun

2017-03-01

Er 3+ :Y 3 Al 5 O 12 /WO 3 -KNbO 3 composite powder as an effective sonocatalyst was prepared via collosol-gelling-hydrothermal and high-temperature calcination methods. The textures of materials were observed by X-ray diffractometer (XRD), scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS). In order to estimate the sonocatalytic activity of Er 3+ :Y 3 Al 5 O 12 /WO 3 -KNbO 3 composite powder, the sonocatalytic degradation of methamphetamine (MAPA) was performed. Furthermore, the influences of mass ratio of WO 3 and KNbO 3 , ultrasonic irradiation time, catalyst addition amount, initial methamphetamine (MAPA) concentration and used times on the sonocatalytic degradation of methamphetamine (MAPA) caused by Er 3+ :Y 3 Al 5 O 12 /WO 3 -KNbO 3 composite powder were investigated by using gas chromatography. Under optimal conditions of 1.00g/L Er 3+ :Y 3 Al 5 O 12 /WO 3 -KNbO 3 addition amount and 10.00mg/L methamphetamine (MAPA) initial concentration, 68% of methamphetamine (MAPA) could be removed after 150min ultrasonic irradiation. The experimental results showed that the Er 3+ :Y 3 Al 5 O 12 /WO 3 -KNbO 3 as sonocatalyst displayed an excellent sonocatalytic activity in degradation of methamphetamine (MAPA) under ultrasonic irradiation. Copyright © 2016 Elsevier B.V. All rights reserved.

The crystal structure of the new ternary antimonide Dy 3Cu 20+xSb 11-x ( x≈2)

NASA Astrophysics Data System (ADS)

Fedyna, L. O.; Bodak, O. I.; Fedorchuk, A. O.; Tokaychuk, Ya. O.

2005-06-01

New ternary antimonide Dy 3Cu 20+xSb 11-x ( x≈2) was synthesized and its crystal structure was determined by direct methods from X-ray powder diffraction data (diffractometer DRON-3M, Cu Kα-radiation, R=6.99%,R=12.27%,R=11.55%). The compound crystallizes with the own cubic structure type: space group F 4¯ 3m, Pearson code cF272, a=16.6150(2) Å,Z=8. The structure of the Dy 3Cu 20Sb 11-x ( x≈2) can be obtained from the structure type BaHg 11 by doubling of the lattice parameter and subtraction of 16 atoms. The studied structure was compared with the structures of known compounds, which crystallize in the same space group with similar cell parameters.

U-PuO2, U-PuC, U-PuN cermet fuel for fast reactor

NASA Astrophysics Data System (ADS)

Mishra, Sudhir; Kaity, Santu; Banerjee, Joydipta; Nandi, Chiranjeet; Dey, G. K.; Khan, K. B.

2018-02-01

Cermet fuel combines beneficial properties of both ceramic and metal and attracts global interest for research as a candidate fuel for nuclear reactors. In the present study, U matrix PuC/PuN/PuO2 cermet for fast reactor have been fabricated on laboratory scale by the powder metallurgy route. Characterization of the fuel has been carried out using Dilatometer, Differential Thermal analysis (DTA), X-ray diffractometer and Optical microscope. X ray diffraction study of the fuel reveals presence of different phases. The PuN dispersed cermet was observed to have high solidus temperature as compared to PuC and PuO2 dispersed cermet. Swelling was observed in U matrix PuO2 cermet which also showed higher thermal expansion. Among the three cermets studied, U matrix PuC cermet showed maximum thermal conductivity.

Microstructural, optical and electrical properties of LaFe0.5Cr0.5O3 perovskite nanostructures

NASA Astrophysics Data System (ADS)

Ali, S. Asad; Naseem, Swaleha; Khan, Wasi; Sharma, A.; Naqvi, A. H.

2016-05-01

Perovskite nanocrystalline powder of LaFe0.5Cr0.5O3 was synthesized by sol-gel combustion route and characterized by x-ray diffractometer (XRD), scanning electron microscopy (SEM) equipped with EDS, UV-visible and LCR meter at room temperature Rietveld refinement of the XRD data confirms that the sample is in single phase-rhombohedral structure with space group R-3C. SEM micrograph shows clear nanostructure of the sample and EDS ensures the presence of all elements in good stoichiometric. The optical absorption indicates the maximum absorption at 315 nm and optical band gap of 2.94 eV was estimated using Tauc's relation. Dielectric constant (ɛ') and loss were found to decrease with increase in frequencies. The dielectric behavior was explained on the basis of Maxwell-Wagner's two layer model.

The Macromolecular Neutron Diffractometer MaNDi at the Spallation Neutron Source

DOE PAGES

Coates, Leighton; Cuneo, Matthew J.; Frost, Matthew J.; ...

2015-07-18

The Macromolecular Neutron Diffractometer (MaNDi) is located on beamline 11B of the Spallation Neutron Source at Oak Ridge National Laboratory. Moreover, the instrument is a neutron time-of-flight wavelength-resolved Laue diffractometer optimized to collect diffraction data from single crystals. Finally, the instrument has been designed to provide flexibility in several instrumental parameters, such as beam divergence and wavelength bandwidth, to allow data collection from a range of macromolecular systems.

The neutron texture diffractometer at the China Advanced Research Reactor

NASA Astrophysics Data System (ADS)

Li, Mei-Juan; Liu, Xiao-Long; Liu, Yun-Tao; Tian, Geng-Fang; Gao, Jian-Bo; Yu, Zhou-Xiang; Li, Yu-Qing; Wu, Li-Qi; Yang, Lin-Feng; Sun, Kai; Wang, Hong-Li; Santisteban, J. r.; Chen, Dong-Feng

2016-03-01

The first neutron texture diffractometer in China has been built at the China Advanced Research Reactor, due to strong demand for texture measurement with neutrons from the domestic user community. This neutron texture diffractometer has high neutron intensity, moderate resolution and is mainly applied to study texture in commonly used industrial materials and engineering components. In this paper, the design and characteristics of this instrument are described. The results for calibration with neutrons and quantitative texture analysis of zirconium alloy plate are presented. The comparison of texture measurements with the results obtained in HIPPO at LANSCE and Kowari at ANSTO illustrates the reliability of the texture diffractometer. Supported by National Nature Science Foundation of China (11105231, 11205248, 51327902) and International Atomic Energy Agency-TC program (CPR0012)

Applications of RIGAKU Dmax Rapid II micro-X-ray diffractometer in the analysis of archaeological metal objects

NASA Astrophysics Data System (ADS)

Mozgai, Viktória; Szabó, Máté; Bajnóczi, Bernadett; Weiszburg, Tamás G.; Fórizs, István; Mráv, Zsolt; Tóth, Mária

2017-04-01

During material analysis of archaeological metal objects, especially their inlays or corrosion products, not only microstructure and chemical composition, but mineralogical composition is necessary to be determined. X-ray powder diffraction (XRD) is a widely-used method to specify the mineralogical composition. However, when sampling is not or limitedly allowed due to e.g. the high value of the object, the conventional XRD analysis can hardly be used. Laboratory micro-XRD instruments provide good alternatives, like the RIGAKU Dmax Rapid II micro-X-ray diffractometer, which is a unique combination of a MicroMax-003 third generation microfocus, sealed tube X-ray generator and a curved 'image plate' detector. With this instrument it is possible to measure as small as 10 µm area in diameter on the object. Here we present case studies for the application of the micro-XRD technique in the study of archaeological metal objects. In the first case niello inlay of a Late Roman silver augur staff was analysed. Due to the high value of the object, since it is the only piece known from the Roman Empire, only non-destructive analyses were allowed. To reconstruct the preparation of the niello, SEM-EDX analysis was performed on the niello inlays to characterise their chemical composition and microstructure. Two types of niello are present: a homogeneous, silver sulphide niello (acanthite) and an inhomogeneous silver-copper sulphide niello (exsolution of acanthite and jalpaite or jalpaite and stromeyerite). The micro-X-ray diffractometer was used to verify the mineralogical composition of the niello, supposed on the base of SEM results. In the second case corrosion products of a Late Roman copper cauldron with uncertain provenance were examined, since they may hold clues about the burial conditions (pH, Eh, etc.) of the object. A layer by layer analysis was performed in cross sections of small metal samples by using electron microprobe and micro-X-ray diffractometer. The results show two corrosion zones: 1) the original (internal) surface zone of the metallic copper object was replaced by copper(I) oxide (cuprite), while 2) basic copper(II) carbonate (malachite) was deposited (externally) on the original surface. In our view these two minerals were formed during long-time burial, and protected the cauldron from further corrosion. Rarely copper(I) chloride (nantokite), basic copper(II) trihydroxychloride (atacamite/paratacamite) and basic copper(II) sulphate (brochantite) were also identified in the two corrosion zones. Their uneven distribution on the cauldron and their known formation conditions indicate, that these latter mineral phases may be the results of active corrosion, started possibly after excavation.

Structural, electrical and mechanical properties of selenium doped thallium based high-temperature superconductors

NASA Astrophysics Data System (ADS)

Cavdar, S.; Kol, N.; Koralay, H.; Ozturk, O.; Asikuzun, E.; Tasci, A. T.

2016-01-01

In this study, highly-refined chemical powders were synthesized by having them ready in appropriate stoichiometric proportions with conventional solid state reaction method so that they would produce the superconductor TlPb0.3Sr2Ca1-xSexCu2Oy (x = 0; 0.4; 0.6; 1.0). This study aims to understand effect of the selenium doping on the superconducting, structural and mechanical properties of the aforementioned superconducting material. The effect of the doping rates on the structural and electrical properties of the sample has been identified. Electrical characteristics of the TlPb0.3Sr2Ca1-xSexCu2Oy material were measured using standard four point probe method. Structural characteristics were examined with the powder X-ray diffractometer (XRD) and scanning electron microscope (SEM). Mechanical properties were analyzed with Vickers microhardness measurements on the sample surface. According to the results, it was observed that the reflection comes from the (00l) and parallel planes increased with Se doping. Particle size increases with increasing doping ratio. According to results of the mechanical measurements, all samples exhibit indentation size effect (ISE) behavior. Comparing the obtained results with theoretical studies, it was understood that Hays Kendall approach is the best method in determination of mechanical properties and analyzing microhardness of the materials.

Growth and characterization of novel organic 3-Hydroxy Benzaldehyde-N-methyl 4 Stilbazolium Tosylate crystals for NLO applications.

PubMed

Jagannathan, K; Umarani, P; Ratchagar, V; Ramesh, V; Kalainathan, S

2016-01-15

The 3-Hydroxy Benzaldehyde-N-methyl 4-Stilbazolium Tosylate (3- HBST) is a new organic NLO crystal and it is a new derivative in stilbazolium tosylate family. In this work we have synthesized 3-HBST and the single crystal was grown by conventional slow cooling method. The structure and lattice parameters of the grown crystal were determined by the single crystal X-ray diffraction (XRD) technique and it is exhibiting good crystalline nature which is observed from the powder XRD. In order to check the crystalline quality the rocking curve was recorded using multi crystal X-ray diffractometer. The functional groups were identified from both FTIR and NMR spectral analyses. The π-π* and n-π* optical transition energy levels were estimated from the absorption peaks. The NLO property was confirmed by measuring relative SHG efficiency by Kurtz powder test; it shows 24 times higher SHG efficiency than that of urea. In order to test the mechanical stability the Vickers and Knoop micro hardness measurement were carried out and found that the micro hardness number decreases with increasing load. The melting point was determined from Differential Scanning Colorimetry (DSC). Copyright © 2015 Elsevier B.V. All rights reserved.

In Situ Powder Diffraction Studies of Electrode Materials in Rechargeable Batteries.

PubMed

Sharma, Neeraj; Pang, Wei Kong; Guo, Zaiping; Peterson, Vanessa K

2015-09-07

The ability to directly track the charge carrier in a battery as it inserts/extracts from an electrode during charge/discharge provides unparalleled insight for researchers into the working mechanism of the device. This crystallographic-electrochemical information can be used to design new materials or modify electrochemical conditions to improve battery performance characteristics, such as lifetime. Critical to collecting operando data used to obtain such information in situ while a battery functions are X-ray and neutron diffractometers with sufficient spatial and temporal resolution to capture complex and subtle structural changes. The number of operando battery experiments has dramatically increased in recent years, particularly those involving neutron powder diffraction. Herein, the importance of structure-property relationships to understanding battery function, why in situ experimentation is critical to this, and the types of experiments and electrochemical cells required to obtain such information are described. For each battery type, selected research that showcases the power of in situ and operando diffraction experiments to understand battery function is highlighted and future opportunities for such experiments are discussed. The intention is to encourage researchers to use in situ and operando techniques and to provide a concise overview of this area of research. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A method for the monitoring of metal recrystallization based on the in-situ measurement of the elastic energy release using neutron diffraction.

PubMed

Christien, F; Telling, M T F; Knight, K S; Le Gall, R

2015-05-01

A method is proposed for the monitoring of metal recrystallization using neutron diffraction that is based on the measurement of stored energy. Experiments were performed using deformed metal specimens heated in-situ while mounted at the sample position of the High Resolution Powder Diffractometer, HRPD (ISIS Facility), UK. Monitoring the breadth of the resulting Bragg lines during heating not only allows the time-dependence (or temperature-dependence) of the stored energy to be determined but also the recrystallized fraction. The analysis method presented here was developed using pure nickel (Ni270) specimens with different deformation levels from 0.29 to 0.94. In situ temperature ramping as well as isothermal annealing was undertaken. The method developed in this work allows accurate and quantitative monitoring of the recrystallization process. The results from neutron diffraction are satisfactorily compared to data obtained from calorimetry and hardness measurements.

A novel X-ray diffractometer for studies of liquid-liquid interfaces.

PubMed

Murphy, Bridget M; Greve, Matthais; Runge, Benjamin; Koops, Christian T; Elsen, Annika; Stettner, Jochim; Seeck, Oliver H; Magnussen, Olaf M

2014-01-01

The study of liquid-liquid interfaces with X-ray scattering methods requires special instrumental considerations. A dedicated liquid surface diffractometer employing a tilting double-crystal monochromator in Bragg geometry has been designed. This diffractometer allows reflectivity and grazing-incidence scattering measurements of an immobile mechanically completely decoupled liquid sample, providing high mechanical stability. The available energy range is from 6.4 to 29.4 keV, covering many important absorption edges. The instrument provides access in momentum space out to 2.54 Å(-1) in the surface normal and out to 14.8 Å(-1) in the in-plane direction at 29.4 keV. Owing to its modular design the diffractometer is also suitable for heavy apparatus such as vacuum chambers. The instrument performance is described and examples of X-ray reflectivity studies performed under in situ electrochemical control and on biochemical model systems are given.

An X-ray diffractometer using mirage diffraction

PubMed Central

Fukamachi, Tomoe; Jongsukswat, Sukswat; Ju, Dongying; Negishi, Riichirou; Hirano, Keiichi; Kawamura, Takaaki

2014-01-01

Some characteristics are reported of a triple-crystal diffractometer with a (+, −, +) setting of Si(220) using mirage diffraction. The first crystal is flat, while the second and third crystals are bent. Basically, the first crystal is used as a collimator, the second as a monochromator and the third as the sample. The third crystal also works as an analyzer. The advantages of this diffractometer are that its setup is easy, its structure is simple, the divergence angle from the second crystal is small and the energy resolution of the third crystal is high, of the order of sub-meV. PMID:25242911

Experimental study on the relationship between the mineral production capability and the physiochemical properties in the coproduction of Q phase-3CaO·3Al2O3·CaSO4 cement clinker.

PubMed

He, Chao; Tian, Chaochao; Li, Gang; Mei, Yahe; Zhang, Quanguo; Jiao, Youzhou

2018-01-01

A coproduction tests of quaternary (Q) phase(6CaO·4Al2O3·MgO·SiO2) -3CaO·3Al2O3·CaSO4 cement clinker and an experimental study on the relationship between the mineral production capability and the physiochemical properties are conducted in a two-stage multiphase reaction test bed with Changguang coal. X-ray diffractometer (XRD) analyses are performed on the coproduction clinker samples. The results demonstrate that, with the reduction in particle sizes of the coal powder and the additives and expanded screening level differences between them, both the proportion of Q phase and the mass of 3CaO·3Al2O3·CaSO4 in the clinker increase accordingly. When mixed coal powder particles are prepared through reducing particle sizes and expanding screening level differences between coal powder and additives, the additives CaO and MgO are more likely to be enclosed by coal powder to form globular polymerized particles. In addition, this preparation aids in polymerization and promotes even distribution of CaO, MgO and coal minerals, thus facilitating clinker mineral formation reactions of inorganic substances in the mixed coal powder. Target minerals, such as 2CaO·SiO2 and Q phase, are found in both industrial high-calcium limestone and low-calcium limestone coproduction clinker samples. A diffraction peak of free CaO is also evident in both samples. Compared with a coproduction clinker sample of high-calcium limestone, that of low-calcium limestone exhibits higher diffraction peaks for 2CaO·SiO2 and Q phase. With the current state of the art, it is not yet the optimum choice to substitute CaCO3 for CaO in Q-phase cement clinker coproduction. Before the technology matures and gains practical application, further study on the form and the mixing process of calcium-based additives for cement clinker coproduction will be required.

Experimental study on the relationship between the mineral production capability and the physiochemical properties in the coproduction of Q phase-3CaO·3Al2O3·CaSO4 cement clinker

PubMed Central

Tian, Chaochao; Li, Gang; Mei, Yahe; Zhang, Quanguo; Jiao, Youzhou

2018-01-01

A coproduction tests of quaternary (Q) phase(6CaO·4Al2O3·MgO·SiO2) -3CaO·3Al2O3·CaSO4 cement clinker and an experimental study on the relationship between the mineral production capability and the physiochemical properties are conducted in a two-stage multiphase reaction test bed with Changguang coal. X-ray diffractometer (XRD) analyses are performed on the coproduction clinker samples. The results demonstrate that, with the reduction in particle sizes of the coal powder and the additives and expanded screening level differences between them, both the proportion of Q phase and the mass of 3CaO·3Al2O3·CaSO4 in the clinker increase accordingly. When mixed coal powder particles are prepared through reducing particle sizes and expanding screening level differences between coal powder and additives, the additives CaO and MgO are more likely to be enclosed by coal powder to form globular polymerized particles. In addition, this preparation aids in polymerization and promotes even distribution of CaO, MgO and coal minerals, thus facilitating clinker mineral formation reactions of inorganic substances in the mixed coal powder. Target minerals, such as 2CaO·SiO2 and Q phase, are found in both industrial high-calcium limestone and low-calcium limestone coproduction clinker samples. A diffraction peak of free CaO is also evident in both samples. Compared with a coproduction clinker sample of high-calcium limestone, that of low-calcium limestone exhibits higher diffraction peaks for 2CaO·SiO2 and Q phase. With the current state of the art, it is not yet the optimum choice to substitute CaCO3 for CaO in Q-phase cement clinker coproduction. Before the technology matures and gains practical application, further study on the form and the mixing process of calcium-based additives for cement clinker coproduction will be required. PMID:29634732

Design and implementation of a multiaxial loading capability during heating on an engineering neutron diffractometer

DOE PAGES

Benafan, O.; Padula, S. A.; Skorpenske, H. D.; ...

2014-10-02

Here we discuss a gripping capability that was designed, implemented, and tested for in situ neutron diffraction measurements during multiaxial loading and heating on the VULCAN engineering materials diffractometer at the spallation neutron source at Oak Ridge National Laboratory.

Earth, soil and environmental science research facility at sector 13 of the Advanced Photon Source. II. Scientific program and experimental instrumentation (abstract)

NASA Astrophysics Data System (ADS)

Sutton, S.; Eng., P. J.; Jaski, Y. R.; Lazaraz, N.; Pluth, J.; Murray, P.; Rarback, H.; Rivers, M.

1996-09-01

The GSECARS (APS sector 13) scientific program will provide fundamental new information on the deep structure and composition of the Earth and other planets, the formation of economic mineral deposits, the cycles and fate of toxic metals in the environment, and the mechanisms of nutrient uptake and disease in plants. In the four experimental stations (2 per beamline), scientists will have access to three main x-ray techniques: diffraction (microcrystal, powder, diamond anvil cell, and large volume press), fluorescence microprobe, and spectroscopy (conventional, microbeam, liquid and solid surfaces). The high pressure facilities will be capable of x-ray crystallography at P≳360 GPa and T˜6000 K with the diamond anvil cell and P˜25 GPa and T˜2500 °C with the large volume press. Diffractometers will allow study of 1 micrometer crystals and micro-powders. The microprobe (1 micrometer focused beam) will be capable of chemical analyses in the sub-ppm range using wavelength and energy dispersive detectors. Spectroscopy instrumentation will be available for XANES and EXAFS with microbeams as well as high sensitivity conventional XAS and studies of liquid and solid interfaces. Visiting scientists will be able to setup, calibrate, and test experiments in off-line laboratories with equipment such as micromanipulators, optical microscopes, clean bench, glove boxes, high powered optical and Raman spectrometers.

Improved camera for better X-ray powder photographs

NASA Technical Reports Server (NTRS)

Parrish, W.; Vajda, I. E.

1969-01-01

Camera obtains powder-type photographs of single crystals or polycrystalline powder specimens. X-ray diffraction photographs of a powder specimen are characterized by improved resolution and greater intensity. A reasonably good powder pattern of small samples can be produced for identification purposes.

Development of a position sensitive X-ray detector for use in a light weight X-ray diffractometer

NASA Technical Reports Server (NTRS)

Semmler, R. A.

1971-01-01

A position sensitive proportional counter for use in an X-ray diffractometer is developed to permit drastic reductions in the power and weight requirements of the X-ray source and the elimination of the power, weight, and complexity of a moving slit. The final detector constructed and tested has a window spanning 138 and a free standing anode curved along an arc of 7.1 cm radius. Demonstration spectra of a quartz sample in a Debye-Sherrer geometry indicate a spatial resolution of 0.4 - 0.5 mm (0.3 - 0.4 theta). The lunar diffractometer consumed 25 watts in the X-ray generator and weighed about 20 pounds.

Optimization of a multi-channel parabolic guide for the material science diffractometer STRESS-SPEC at FRM II

NASA Astrophysics Data System (ADS)

Rebelo Kornmeier, Joana; Ostermann, Andreas; Hofmann, Michael; Gibmeier, Jens

2014-02-01

Neutron strain diffractometers usually use slits to define a gauge volume within engineering samples. In this study a multi-channel parabolic neutron guide was developed to be used instead of the primary slit to minimise the loss of intensity and vertical definition of the gauge volume when using slits placed far away from the measurement position in bulky components. The major advantage of a focusing guide is that the maximum flux is not at the exit of the guide as for a slit system but at the focal point relatively far away from the exit of the guide. Monte Carlo simulations were used to optimise the multi-channel parabolic guide with respect to the instrument characteristics of the diffractometer STRESS-SPEC at the FRM II neutron source. Also the simulations are in excellent agreement with experimental measurements using the optimised multi-channel parabolic guide at the neutron diffractometer. In addition the performance of the guide was compared to the standard slit setup at STRESS-SPEC using a single bead weld sample used in earlier round robin tests for residual strain measurements.

Study on the surface sulfidization behavior of smithsonite at high temperature

NASA Astrophysics Data System (ADS)

Lv, Jin-fang; Tong, Xiong; Zheng, Yong-xing; Xie, Xian; Wang, Cong-bing

2018-04-01

Surface sulfidization behavior of smithsonite at high temperature was investigated by X-ray powder diffractometer (XRD) along with thermodynamic calculation, X-ray photoelectron spectroscopy (XPS) and electron probe microanalysis (EPMA). The XRD and thermodynamic analyses indicated that the smithsonite was decomposed into zincite at high temperatures. After introducing a small amount of pyrite, artificial sulfides were formed at surface of the obtained zincite. The XPS analyses revealed that the sulfide species including zinc sulfide and zinc disulfide were generated at the zincite surface. The EPMA analyses demonstrated that the film of sulfides was unevenly distributed at the zincite surface. The average concentration of elemental sulfur at the sample surface increased with increasing of pyrite dosage. A suitable mole ratio of FeS2 to ZnCO3 for the surface thermal modification was determined to be about 0.3. These findings can provide theoretical support for improving the process during which the zinc recovery from refractory zinc oxide ores is achieved by xanthate flotation.

Crystal growth, structural, optical, dielectric and thermal studies of an amino acid based organic NLO material: L-Phenylalanine L-phenylalaninium malonate

NASA Astrophysics Data System (ADS)

Prakash, M.; Geetha, D.; Lydia Caroline, M.; Ramesh, P. S.

2011-12-01

Good transparent single crystals of L-phenylalanine L-phenylalaninium malonate (LPPMA) have been grown successfully by slow evaporation technique from aqueous solution. Single crystal X-ray diffractometer was utilized to measure unit cell parameter and to confirm the crystal structure. The chemical structure of compound was established by FT-NMR technique. The vibrational modes of the molecules of elucidated from FTIR spectra. Its optical behaviour has been examined by UV-vis spectral analysis, which shows the absence of absorbance in the visible region. Thermal properties of the LPPMA crystal were carried out by thermo gravimetric analysis (TGA) and differential thermal analysis (DTA) techniques, which indicate that the material does not decompose before melting. The melting point of grown crystal was observed as 180 °C by melting point apparatus. The NLO property was confirmed by the powder technique of Kurtz and Perry. The dielectric behaviour of the sample was also studied for the first time.

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

Synthesis of BiOCl nanosheets with oxygen vacancies for the improved photocatalytic properties

NASA Astrophysics Data System (ADS)

Cai, Yujie; Li, Dongya; Sun, Jingyu; Chen, Mengdie; Li, Yirui; Zou, Zhongwei; Zhang, Hua; Xu, Haiming; Xia, Dongsheng

2018-05-01

The square-sharped BiOCl nanosheets with oxygen vacancies were successfully synthesized via a facile hydrothermal route using xylitol as surfactant. The as-prepared BiOCl samples were characterized by Powder X-ray Diffractometer (XRD), scanning electron microscope (SEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), selected area electron diffraction (SAED), UV-Vis diffuse reflectance spectra (DRS), Brunauer-Emmett-Teller (BET), X-ray photoelectron spectroscopy (XPS) and Electron spin resonance (ESR). The as-prepared samples were phase-pure with the width and the thickness were about 50-400 nm and 20-50 nm respectively. Besides, the photodegradation performances showed the BiOCl nanosheets with 0.1 g concentration of xylitol (BOC-1) had the best photocatalytic activity under visible light due to its special polycrystalline structure, grain boundary and an optimum concentration of oxygen vacancies. The h+ and radO2- were the two main active species during the photocatalytic process and the possible photocatalytic mechanism was proposed.

A method for the monitoring of metal recrystallization based on the in-situ measurement of the elastic energy release using neutron diffraction

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

Christien, F., E-mail: frederic.christien@univ-nantes.fr; Le Gall, R.; Telling, M. T. F.

2015-05-15

A method is proposed for the monitoring of metal recrystallization using neutron diffraction that is based on the measurement of stored energy. Experiments were performed using deformed metal specimens heated in-situ while mounted at the sample position of the High Resolution Powder Diffractometer, HRPD (ISIS Facility), UK. Monitoring the breadth of the resulting Bragg lines during heating not only allows the time-dependence (or temperature-dependence) of the stored energy to be determined but also the recrystallized fraction. The analysis method presented here was developed using pure nickel (Ni270) specimens with different deformation levels from 0.29 to 0.94. In situ temperature rampingmore » as well as isothermal annealing was undertaken. The method developed in this work allows accurate and quantitative monitoring of the recrystallization process. The results from neutron diffraction are satisfactorily compared to data obtained from calorimetry and hardness measurements.« less

Neutron diffraction study of aqueous Laponite suspensions at the NIMROD diffractometer.

PubMed

Tudisca, V; Bruni, F; Scoppola, E; Angelini, R; Ruzicka, B; Zulian, L; Soper, A K; Ricci, M A

2014-09-01

The process of dynamical arrest, leading to formation of different arrested states such as glasses and gels, along with the closely related process of aging, is central for both basic research and technology. Here we report on a study of the time-dependent structural evolution of two aqueous Laponite clay suspensions at different weight concentrations. Neutron diffraction experiments have been performed with the near and intermediate range order diffractometer (NIMROD) that allows studies of the structure of liquids and disordered materials over a continuous length scale ranging from 1 to 300 Å, i.e., from the atomistic to the mesoscopic scales. NIMROD is presently a unique diffractometer, bridging the length scales traditionally investigated by small angle neutron scattering or small angle x-ray scattering with that accessible by traditional diffractometers for liquids. Interestingly, we have unveiled a signature of aging of both suspensions in the length scale region of NIMROD. This phenomenon, ascribed to sporadic contacts between Laponite platelets at long times, has been observed with the sample arrested as gel or as repulsive glass. Moreover, water molecules within the layers closest to Laponite platelets surface show orientational and translational order, which maps into the crystalline structure of Laponite.

Diffractometer data collecting method and apparatus

DOEpatents

Steinmeyer, P.A.

1991-04-16

Diffractometer data is collected without the use of a movable receiver. A scanning device, positioned in the diffractometer between a sample and detector, varies the amount of the beam diffracted from the sample that is received by the detector in such a manner that the beam is detected in an integrated form. In one embodiment, a variable diameter beam stop is used which comprises a drop of mercury captured between a pair of spaced sheets and disposed in the path of the diffracted beam. By varying the spacing between the sheets, the diameter of the mercury drop is varied. In another embodiment, an adjustable iris diaphragm is positioned in the path of the diffracted beam and the iris opening is adjusted to control the amount of the beam reaching the detector. 5 figures.

Diffractometer data collecting method and apparatus

DOEpatents

Steinmeyer, Peter A.

1991-04-16

Diffractometer data is collected without the use of a movable receiving s. A scanning device, positioned in the diffractometer between a sample and detector, varies the amount of the beam diffracted from the sample that is received by the detector in such a manner that the beam is detected in an integrated form. In one embodiment, a variable diameter beam stop is used which comprises a drop of mercury captured between a pair of spaced sheets and disposed in the path of the diffracted beam. By varying the spacing between the sheets, the diameter of the mercury drop is varied. In another embodiment, an adjustable iris diaphragm is positioned in the path of the diffracted beam and the iris opening is adjusted to control the amount of the beam reaching the detector.

Calibration of X-Ray diffractometer by the experimental comparison method

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

Dudka, A. P., E-mail: dudka@ns.crys.ras.ru

2015-07-15

A software for calibrating an X-ray diffractometer with area detector has been developed. It is proposed to search for detector and goniometer calibration models whose parameters are reproduced in a series of measurements on a reference crystal. Reference (standard) crystals are prepared during the investigation; they should provide the agreement of structural models in repeated analyses. The technique developed has been used to calibrate Xcalibur Sapphire and Eos, Gemini Ruby (Agilent) and Apex x8 and Apex Duo (Bruker) diffractometers. The main conclusions are as follows: the calibration maps are stable for several years and can be used to improve structuralmore » results, verified CCD detectors exhibit significant inhomogeneity of the efficiency (response) function, and a Bruker goniometer introduces smaller distortions than an Agilent goniometer.« less

Anisotropic crystal deformation measurements determined using powder X-ray diffraction and a new in situ compression stage.

PubMed

Haware, Rahul V; Kim, Paul; Ruffino, Lauren; Nimi, Brian; Fadrowsky, Catherine; Doyle, Michael; Boerrigter, Stephan X M; Cuitino, Alberto; Morris, Ken

2011-10-14

This report addresses the development of experimental and computational estimations of the anisotropic elastic moduli (EM) of single crystals to aid in the a priori (i.e., starting with the crystal structure) prediction of the trend as a function of the direction of applied stress. Experimentally EM values in the normal direction to the X-, Y- and Z-planes of block shaped aspirin and acetaminophen crystals were determined using data generated by the newly designed compression stage housed in our powder X-ray diffractometer. Computational estimations of EM were made using the applicable modules in Material Studio 5.5. The measured EM values normal to the (100), (020) and (002) planes of aspirin, and (20-1), (020) and (001) planes of acetaminophen crystals by both methods succeeded in detected the anisotropic behavior. However, disparity in the relative values between measured EM values by different techniques was observed. This may be attributed to deformation sources other than lattice compression including inelastic processes such as local failure and plasticity as well as deformation at the crystal-probe interfaces due to crystal surface roughness (asperities). The trend of the ratio of the values from the respective methods showed reasonable agreement and promise for the technique. The present approach demonstrated the suitability of the compression stage to determine and predict anisotropic EM of subjected small molecular organic crystals. Copyright © 2011 Elsevier B.V. All rights reserved.

Low-temperature high magnetic field powder x-ray diffraction setup for field-induced structural phase transition studies from 2 to 300 K and at 0 to 8-T field

NASA Astrophysics Data System (ADS)

Shahee, Aga; Sharma, Shivani; Kumar, Dhirendra; Yadav, Poonam; Bhardwaj, Preeti; Ghodke, Nandkishor; Singh, Kiran; Lalla, N. P.; Chaddah, P.

2016-10-01

A low-temperature and high magnetic field powder x-ray diffractometer (XRD) has been developed at UGC-DAE CSR (UGC: University Grant Commission, DAE: Department of Atomic Energy, and CSR: Consortium for scientific research), Indore, India. The setup has been developed around an 18 kW rotating anode x-ray source delivering Cu-Kα x-rays coming from a vertical line source. It works in a symmetric θ-2θ parallel beam geometry. It consists of a liquid helium cryostat with an 8 T split-pair Nb-Ti superconducting magnet comprising two x-ray windows each covering an angular range of 65°. This is mounted on a non-magnetic type heavy duty goniometer equipped with all necessary motions along with data collection accessories. The incident x-ray beam has been made parallel using a parabolic multilayer mirror. The scattered x-ray is detected using a NaI detector through a 0.1° acceptance solar collimator. To control the motions of the goniometer, a computer programme has been developed. The wide-angle scattering data can be collected in a range of 2°-115° of 2θ with a resolution of ˜0.1°. The whole setup is tightly shielded for the scattered x-rays using a lead hutch. The functioning of the goniometer and the artifacts arising possibly due to the effect of stray magnetic field on the goniometer motions, on the x-ray source, and on the detector have been characterized by collecting powder XRD data of a National Institute of Standards and Technology certified standard reference material LaB6 (SRM-660b) and Si powder in zero-field and in-field conditions. Occurrence of field induced structural-phase transitions has been demonstrated on various samples like Pr0.5Sr0.5MnO3, Nd0.49Sr0.51MnO3-δ and La0.175Pr0.45Ca0.375MnO3 by collecting data in zero field cool and field cool conditions.

Microgravity

NASA Image and Video Library

1998-06-16

Eddie Snell, Post-Doctoral Fellow the National Research Council (NRC) uses a reciprocal space mapping diffractometer for macromolecular crystal quality studies. The diffractometer is used in mapping the structure of macromolecules such as proteins to determine their structure and thus understand how they function with other proteins in the body. This is one of several analytical tools used on proteins crystallized on Earth and in space experiments. Photo credit: NASA/Marshall Space Flight Center (MSFC)

Protein Crystal Quality Studies

NASA Technical Reports Server (NTRS)

1998-01-01

Eddie Snell, Post-Doctoral Fellow the National Research Council (NRC) uses a reciprocal space mapping diffractometer for macromolecular crystal quality studies. The diffractometer is used in mapping the structure of macromolecules such as proteins to determine their structure and thus understand how they function with other proteins in the body. This is one of several analytical tools used on proteins crystallized on Earth and in space experiments. Photo credit: NASA/Marshall Space Flight Center (MSFC)

New Insights on the Recrystallization and New Growth of Extensively Radiation-damaged Zircon

NASA Astrophysics Data System (ADS)

Hanchar, J. M.; Schmitz, M. D.; Wirth, R.

2012-12-01

Approximately 10 grams of cm-sized nearly metamict zircon crystals from the Saranac Prospect in the Bancroft District of Ontario were combined by breaking into small pieces and then ground under ethanol to a fine powder with an agate mortar and pestle in order to make enough homogeneously mixed material for multiple powder X-Ray and diffraction scans, high-resolution transmission electron microscopy (HR-TEM) measurements, and chemical abrasion isotope dilution thermal ionization mass spectrometry (CA-TIMS). While these large zircon crystals ground to a powder have a larger surface area and not in the same physical state (i.e., brown and metamict) as what is typically analyzed in single zircon CA-ID-TIMS U-Pb analysis (clear euhedral grains), the physical and chemical changes that occur during the heat treatment used in CA-TIMS are thought to be similar processes. Aliquots of the ground zircon powder were annealed in situ using a Pt furnace in a powder diffractometer during which time simultaneous powder diffraction patterns were acquired starting at 25°C, at elevated temperature (from 500°C to 1400°C) at selected time intervals, and then again at 25°C. The powder X-ray diffraction results indicate that below ~900°C the recrystallization of the zircon powder commences but is incomplete, even after 36 hours, with diffuse low intensity diffraction peaks. At 1150°C the zircon powder shows significant recrystallization. At 1150°C, the recrystallization is essentially complete in less than one hour. Before heating the zircon powder samples consisted of clear, transparent to brown, translucent, complexly zoned fragments. After heating at 900°C the zircon powder retained a smaller percentage of clear or brown complexly zoned fragments, while the majority of material had transformed to oscillatory or irregularly zoned, dominantly white opaque microcrystalline fragments. The clear fragments were hypothesized to be preexisting original crystalline zircon, the brown complexly zoned fragments preexisting metamict zircon, and the white opaque fragment new recrystallized zircon and other oxides. At 1150°C all that remained after heating were dominantly white opaque fragments and extremely rare clear fragments. A variety of fragment types from unannealed, 900°C and 1150°C anneals were chemically abraded in concentrated hydrofluoric acid at 190°C for 12 hours. Upon treatment with chemical abrasion, all unannealed material, nearly all material from the 900°C anneal, and all white opaque microcrystalline material from the 1150°C anneal dissolved; only the rare residual clear, transparent fragments from the 1150°C anneal were robust to chemical abrasion at these conditions. Residual clear fragments yielded concordant U-Pb ID-TIMS dates of 1064 Ma (considering updated U decay constant ratio), confirming the hypothesis that low-U closed system domains are preserved through annealing up to 1150°C and can be extracted via chemical abrasion from even dominantly metamict zircon crystals. By contrast, newly formed crystallites resulting from metamict zircon breakdown during annealing appear to be quite soluble during chemical abrasion. Further experiments are underway to refine minimum threshold chemical abrasion conditions necessary to eliminate open-system domains in the Saranac zircon.

A temperature-controlled cell for X-ray study of liquid systems using a commercial DRON-UM1 diffractometer

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

Petrun`kin, S.P.; Garavina, E.V.; Trostin, V.N.

1995-02-01

A container (cell) and a temperature-control system have been designed enabling one to carry out x-ray diffraction study of liquid samples both at a fixed temperature and within a certain temperature range using a commercial DRON-UMl x-ray diffractometer. Special features of the cell and the materials used for it allow one to study both chemically inert and corrosive liquids.

Sample holder for X-ray diffractometry

DOEpatents

Hesch, Victor L.

1992-01-01

A sample holder for use with X-ray diffractometers with the capability to rotate the sample, as well as to adjust the position of the sample in the x, y, and z directions. Adjustment in the x direction is accomplished through loosening set screws, moving a platform, and retightening the set screws. Motion translators are used for adjustment in the y and z directions. An electric motor rotates the sample, and receives power from the diffractometer.

In-situ data collection at the photon factory macromolecular crystallography beamlines

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

Yamada, Yusuke, E-mail: yusuke.yamada@kek.jp; Matsugaki, Naohiro; Kato, Ryuichi

Crystallization trial is one of the most important but time-consuming steps in macromolecular crystallography, and in-situ diffraction experiment has a capability to make researchers to proceed this step more efficiently. At the Photon Factory, a new tabletop diffractometer for in-situ diffraction experiments has been developed. It consists of XYZ translation stages with a plate handler, an on-axis viewing system and a plate rack with a capacity for ten crystallization plates. These components sit on a common plate and are able to be placed on the existing diffractometer table. The CCD detector with a large active area and a pixel arraymore » detector with a small active area are used for acquiring diffraction images from crystals. Dedicated control software and a user interface have also been developed. The new diffractometer has been operational for users and used for evaluation of crystallization screening since 2014.« less

High Pressure X-Ray Diffraction Studies of Nanocrystalline Materials

NASA Technical Reports Server (NTRS)

Palosz, B.; Stel'makh, S.; Grzanka, E.; Gierlotka, S.; Palosz, W.

2004-01-01

Experimental evidence obtained for a variety of nanocrystalline materials suggest that the crystallographic structure of a very small size particle deviates from that in the bulk crystals. In this paper we show the effect of the surface of nanocrystals on their structure by the analysis of generation and distribution of macro- and micro-strains at high pressures and their dependence on the grain size in nanocrystalline powders of Sic. We studied the structure of Sic nanocrystals by in-situ high-pressure powder diffraction technique using synchrotron and neutron sources and hydrostatic or isostatic pressure conditions. The diffraction measurements were done in HASYLAB at DESY using a Diamond Anvil Cell (DAC) in the energy dispersive geometry in the diffraction vector range up to 3.5 - 4/A and under pressures up to 50 GPa at room temperature. In-situ high pressure neutron diffraction measurements were done at LANSCE in Los Alamos National Laboratory using the HIPD and HIPPO diffractometers with the Paris-Edinburgh and TAP-98 cells, respectively, in the diffraction vector range up to 26 Examination of the response of the material to external stresses requires nonstandard methodology of the materials characterization and description. Although every diffraction pattern contains a complete information on macro- and micro-strains, a high pressure experiment can reveal only those factors which contribute to the characteristic diffraction patterns of the crystalline phases present in the sample. The elastic properties of powders with the grain size from several nm to micrometers were examined using three methodologies: (l), the analysis of positions and widths of individual Bragg reflections (used for calculating macro- and micro-strains generated during densification) [I], (2). the analysis of the dependence of the experimental apparent lattice parameter, alp, on the diffraction vector Q [2], and (3), the atomic Pair Distribution Function (PDF) technique [3]. The results of our studies show, that Sic nanocrystals have the features of two phases, each with its distinct elastic properties. and under pressures up to 8 GPa.

Effect of hydrothermal condition on the formation of multi-component oxides of Ni-based metallic glass under high temperature water near the critical point

DOE PAGES

Kim, J. S.; Kim, S. Y.; Kim, D. H.; ...

2015-07-01

The specific feature of multi-component oxides synthesized by hydrothermal process under high temperature (633 K) and highly pressurized water (18.9 MPa) near critical point. Effects of hydrothermal processing duration times 24 hours and 72 hours, respectively, on the oxide formation of the Ni 59Zr 20Ti 16Si 2Sn 3 metallic glass synthesized by powder metallurgy process were characterized by X-ray diffractometer, differential scanning calorimeter along with the particle size, morphology and crystalline phase of the oxides. The crystallization of the needle-shape NiTiO 3, ZrTiO 4 and ZrSnO 4 ternary oxide phases observed on the surface of metallic glass at below glassmore » transition temperature and the morphology of oxide phases changed to plate-shape around 2 μm in diameter by the increase processing time. This hydrothermal processing in subcritical water provides accelerated dense metal oxide crystals due to the reaction medium being at higher pressure than conventional oxidation processing.« less

Crystal growth, perfection, linear and nonlinear optical, photoconductivity, dielectric, thermal and laser damage threshold properties of 4-methylimidazolium picrate: an interesting organic crystal for photonic and optoelectronic devices

NASA Astrophysics Data System (ADS)

Rajesh, K.; Arun, A.; Mani, A.; Praveen Kumar, P.

2016-10-01

The 4-methylimidazolium picrate has been synthesized and characterized successfully. Single and powder x-ray diffraction studies were conducted which confirmed the crystal structure, and the value of the strain was calculated. The crystal perfection was determined by a HRXR diffractometer. The transmission spectrum exhibited a better transmittance of the crystal in the entire visible region with a lower cut-off wavelength of 209 nm. The linear absorption value was calculated by the optical limiting method. A birefringence study was also carried out. Second and third order nonlinear optical properties of the crystal were found by second harmonic generation and the z-scan technique. The crystals were also characterized by dielectric measurement and a photoconductivity analyzer to determine the dielectric property and the optical conductivity of the crystal. The laser damage threshold activity of the grown crystal was studied by a Q-switched Nd:YAG laser beam. Thermal studies established that the compound did not undergo a phase transition and was stable up to 240 °C.

Crystal growth, structural, optical, dielectric and thermal studies of an amino acid based organic NLO material: L-phenylalanine L-phenylalaninium malonate.

PubMed

Prakash, M; Geetha, D; Caroline, M Lydia; Ramesh, P S

2011-12-01

Good transparent single crystals of L-phenylalanine L-phenylalaninium malonate (LPPMA) have been grown successfully by slow evaporation technique from aqueous solution. Single crystal X-ray diffractometer was utilized to measure unit cell parameter and to confirm the crystal structure. The chemical structure of compound was established by FT-NMR technique. The vibrational modes of the molecules of elucidated from FTIR spectra. Its optical behaviour has been examined by UV-vis spectral analysis, which shows the absence of absorbance in the visible region. Thermal properties of the LPPMA crystal were carried out by thermo gravimetric analysis (TGA) and differential thermal analysis (DTA) techniques, which indicate that the material does not decompose before melting. The melting point of grown crystal was observed as 180°C by melting point apparatus. The NLO property was confirmed by the powder technique of Kurtz and Perry. The dielectric behaviour of the sample was also studied for the first time. Copyright © 2011 Elsevier B.V. All rights reserved.

Electrical characteristics of organic perylene single-crystal-based field-effect transistors

NASA Astrophysics Data System (ADS)

Lee, Jin-Woo; Kang, Han-Saem; Kim, Min-Ki; Kim, Kihyun; Cho, Mi-Yeon; Kwon, Young-Wan; Joo, Jinsoo; Kim, Jae-Il; Hong, Chang-Seop

2007-12-01

We report on the fabrication of organic field-effect transistors (OFETs) using perylene single crystal as the active material and their electrical characteristics. Perylene single crystals were directly grown from perylene powder in a furnace using a relatively short growth time of 1-3 h. The crystalline structure of the perylene single crystals was characterized by means of a single-crystal x-ray diffractometer. In order to place the perylene single crystal onto the Au electrodes of the field-effect transistor, a polymethlymethacrylate thin layer was spin-coated on top of the crystal surface. The OFETs fabricated using the perylene single crystal showed a typical p-type operating mode. The field-effect mobility of the perylene crystal based OFETs was measured to be ˜9.62×10-4 cm2/V s at room temperature. The anisotropy of the mobility implying the existence of different mobilities when applying currents in different directions was observed for the OFETs, and the existence of traps in the perylene crystal was found through the measurements of the temperature-dependent mobility at various operating drain voltages.

Synchrotron radiation topography studies of the phase transition in LaGaO 3 crystals

NASA Astrophysics Data System (ADS)

Yao, G.-D.; Dudley, M.; Wang, Y.; Liu, X.; Liebermann, R. C.

1991-05-01

An investigation of the orthorhombic to rhombohedral phase transformation occurring at 145°C in lanthanum gallate has been conducted using white beam synchrotron X-ray topography (WBSXRT). The existence of the first order transition was confirmed by differential thermal analysis and X-ray diffractometer powder analysis. Subsequent to this, synchrotron white beam Laue patterns were recorded in situ as a function of temperature, during the transition. Before the transition point was reached, (112) orth type reflection twinning was found to be dominant although a small amount of (110) orth type twinning was also observed in the same crystal. Beyond the transition point, not only did the structural change become evident but also reflection twinning on the (110) rhom planes was observed. The scale of this twinning became finer as the temperature was increased beyond the transition temperature. The twinning observed in both the low and high temperature phases gives rise to deformation of the (011) rhom surface plane which creates problems for the potential use of this material as a substrate for growing high Tc superconducting epitaxial layers.

TiC Reinforcement Composite Coating Produced Using Graphite of the Cast Iron by Laser Cladding

PubMed Central

Liu, Yanhui; Qu, Weicheng; Su, Yu

2016-01-01

In this study, a TiC-reinforced composite coating was produced to improve the wear resistance of a pearlite matrix grey iron using a pre-placed Ti powder by laser cladding. Results of scanning electron microscopy (SEM), X-ray diffractometer (XRD), and energy dispersive X-ray spectroscopy (EDS) confirmed that the coating was composed of TiC particles and two kinds of α-Fe phase. The fine TiC particles were only a few microns in size and uniformly distributed on the matrix phase in the composite coating. The microstructure characteristic of the composite coating resulted in the microhardness rising to about 1000 HV0.3 (China GB/T 4342-1991) and the wear resistance significantly increased relative to the substrate. In addition, the fine and homogeneous solidification microstructure without graphite phase in the transition zone led to a good metallurgical bonding and transition between the coating and the substrate. It was of great significance for the cast iron to modify the surface and repair surface defects or surface damage. PMID:28773934

TiC Reinforcement Composite Coating Produced Using Graphite of the Cast Iron by Laser Cladding.

PubMed

Liu, Yanhui; Qu, Weicheng; Su, Yu

2016-09-30

In this study, a TiC-reinforced composite coating was produced to improve the wear resistance of a pearlite matrix grey iron using a pre-placed Ti powder by laser cladding. Results of scanning electron microscopy (SEM), X-ray diffractometer (XRD), and energy dispersive X-ray spectroscopy (EDS) confirmed that the coating was composed of TiC particles and two kinds of α -Fe phase. The fine TiC particles were only a few microns in size and uniformly distributed on the matrix phase in the composite coating. The microstructure characteristic of the composite coating resulted in the microhardness rising to about 1000 HV0.3 (China GB/T 4342-1991) and the wear resistance significantly increased relative to the substrate. In addition, the fine and homogeneous solidification microstructure without graphite phase in the transition zone led to a good metallurgical bonding and transition between the coating and the substrate. It was of great significance for the cast iron to modify the surface and repair surface defects or surface damage.

Preparation, characterization, and in vitro release of gentamicin from coralline hydroxyapatite-alginate composite microspheres.

PubMed

Sivakumar, M; Rao, K Panduranga

2003-05-01

In this work, composite microspheres were prepared from bioactive ceramics such as coralline hydroxyapatite [Ca(10)(PO(4))(6)(OH)(2)] granules, a biodegradable polymer, sodium alginate, and an antibiotic, gentamicin. Previously, we have shown a gentamicin release from coralline hydroxyapatite granules-chitosan composite microspheres. In the present investigation, we attempted to prepare composite microspheres containing coralline hydroxyapatite granules and sodium alginate by the dispersion polymerization technique with gentamicin incorporated by absorption method. The crystal structure of the composite microspheres was analyzed using X-ray powder diffractometer. Fourier transform infrared spectra clearly indicated the presence of per-acid of sodium alginate, phosphate, and hydroxyl groups in the composite microspheres. Scanning electron micrographs and optical micrographs showed that the composite microspheres were spherical in shape and porous in nature. The particle size of composite microspheres was analyzed, and the average size was found to be 15 microns. The thermal behavior of composite microspheres was studied using thermogravimetric analysis and differential scanning calorimetric analysis. The cumulative in vitro release profile of gentamicin from composite microspheres showed near zero order patterns. Copyright 2003 Wiley Periodicals, Inc.

Preparation, characterization and in vitro release of gentamicin from coralline hydroxyapatite-gelatin composite microspheres.

PubMed

Sivakumar, M; Panduranga Rao, K

2002-08-01

Composite microspheres have been prepared from bioactive ceramics such as coralline hydroxyapatite [CHA, Ca10(PO4)6(OH)2] granules, a biodegradable polymer, gelatin and an antibiotic, gentamicin. In our earlier work, we have shown a gentamicin release from CHA granules--chitosan composite microspheres. In the present investigation, an attempt was made to prepare the composite microspheres containing coralline hydroxyapatite and gelatin (CHA-G), which were prepared by the dispersion polymerization technique and the gentamicin was incorporated by the absorption method. The crystal structure of the composite microspheres was analyzed using X-ray powder diffractometer. The Fourier transformed infrared spectrum clearly indicated the presence of amide and hydroxyl groups in the composite microspheres. Scanning electron micrographs and optical micrographs show that the composite microspheres are spherical in shape and porous in nature. The particle size of composite microspheres was analyzed and the average size was found to be 16 microm. The thermal behavior of composite microspheres was studied using thermogravimetric analysis and differential scanning calorimetric analysis. The cumulative in vitro release profile of gentamicin from composite microspheres showed near zero order patterns.

Microgravity

NASA Image and Video Library

1998-06-16

Eddie Snell (standing), Post-Doctoral Fellow the National Research Council (NRC),and Marc Pusey of Marshall Space Flight Center (MSFC) use a reciprocal space mapping diffractometer for marcromolecular crystal quality studies. The diffractometer is used in mapping the structure of marcromolecules such as proteins to determine their structure and thus understand how they function with other proteins in the body. This is one of several analytical tools used on proteins crystalized on Earth and in space experiments. Photo credit: NASA/Marshall Space Flight Center (MSFC)

Peak broadening and peak shift pole figures investigations by STRESS-SPEC diffractometer at FRM II

NASA Astrophysics Data System (ADS)

Gan, W. M.; Randau, C.; Hofmann, M.; Brokmeier, H. G.; Mueller, M.; Schreyer, A.

2012-02-01

This paper studied for the first time peak intensity, peak position and FHWM pole figures with one time measurement at the neutron diffractometer STRESS-SPEC via in-situ tensile deformation on austenitic steel. Fibre distribution with its evolution from central tensile direction to normal direction of these three kinds of pole figures was obtained. Variation of peak position and FWHM can be correlated to the reorientation of the texture component.

Protein Crystal Quality Studies

NASA Technical Reports Server (NTRS)

1998-01-01

Eddie Snell (standing), Post-Doctoral Fellow the National Research Council (NRC),and Marc Pusey of Marshall Space Flight Center (MSFC) use a reciprocal space mapping diffractometer for marcromolecular crystal quality studies. The diffractometer is used in mapping the structure of marcromolecules such as proteins to determine their structure and thus understand how they function with other proteins in the body. This is one of several analytical tools used on proteins crystalized on Earth and in space experiments. Photo credit: NASA/Marshall Space Flight Center (MSFC)

Thermal stabilization of neutron Larmor diffractometers

NASA Astrophysics Data System (ADS)

Keller, T.; Tralmer, F.

2017-06-01

We report on the design of a support unit for the radio frequency (RF) coils of a Larmor diffractometer (LD) eliminating fluctuations of the Larmor phase resulting from thermal expansion of the support structures. The key component defining the spacing between the RF coils is a Zerodur bar with a very low thermal expansion coefficient (α = 7 × 10-8 K-1). This support unit will allow for LD measurements on the 10-6 accuracy level even if the ambient temperature is fluctuating.

7 CFR 160.93 - Powdered rosin.

Code of Federal Regulations, 2012 CFR

2012-01-01

... STANDARDS FOR NAVAL STORES Labeling, Advertising and Packing § 160.93 Powdered rosin. The classification and grade of any rosin sold in commerce in a powdered or finely broken condition shall be stated in the... broken. For the purpose of preventing coalescence there may be incorporated in such article a limited and...

7 CFR 160.93 - Powdered rosin.

Code of Federal Regulations, 2011 CFR

2011-01-01

... STANDARDS FOR NAVAL STORES Labeling, Advertising and Packing § 160.93 Powdered rosin. The classification and grade of any rosin sold in commerce in a powdered or finely broken condition shall be stated in the... broken. For the purpose of preventing coalescence there may be incorporated in such article a limited and...

7 CFR 160.93 - Powdered rosin.

Code of Federal Regulations, 2014 CFR

2014-01-01

... STANDARDS FOR NAVAL STORES Labeling, Advertising and Packing § 160.93 Powdered rosin. The classification and grade of any rosin sold in commerce in a powdered or finely broken condition shall be stated in the... broken. For the purpose of preventing coalescence there may be incorporated in such article a limited and...

7 CFR 160.93 - Powdered rosin.

Code of Federal Regulations, 2013 CFR

2013-01-01

... STANDARDS FOR NAVAL STORES Labeling, Advertising and Packing § 160.93 Powdered rosin. The classification and grade of any rosin sold in commerce in a powdered or finely broken condition shall be stated in the... broken. For the purpose of preventing coalescence there may be incorporated in such article a limited and...

Rotatable multifunctional load frames for neutron diffractometers at FRM II—design, specifications and applications

NASA Astrophysics Data System (ADS)

Hoelzel, M.; Gan, W. M.; Hofmann, M.; Randau, C.; Seidl, G.; Jüttner, Ph.; Schmahl, W. W.

2013-05-01

Novel tensile rigs have been designed and manufactured at the research reactor Heinz Maier-Leibnitz (FRM II, Garching near Munich). Besides tensile and compressive stress, also torsion can be applied. The unique Eulerian cradle type design (ω, χ, and φ axis) allows orienting the stress axis with respect to the scattering vector. Applications of these tensile rigs at our neutron diffractometers enable various investigations of structural changes under mechanical load, e.g. crystallographic texture evolution, stress-induced phase transformations or lattice expansion, and the anisotropy of mechanical response.

Electrochemical Deposition of Si-Ca/P on Nanotube Formed Beta Ti Alloy by Cyclic Voltammetry Method.

PubMed

Jeong, Yong-Hoon; Choe, Han-Cheol

2015-08-01

The purpose of this study was to investigate electrochemical deposition of Si-Ca/P on nanotube formed Ti-35Nb-10Zr alloy by cyclic voltammetry method. Electrochemical deposition of Si substituted Ca/P was performed by pulsing the applied potential on nanotube formed surface. The surface characteristics were observed by field-emission scanning electron microscopy, X-ray diffractometer, and potentiodynamic polarization test. The phase structure and surface morphologies of Si-Ca/P deposition were affected by deposition cycles. From the anodic polarization test, nanotube formed surface at 20 V showed the high corrosion resistance with lower value of Icorr, I300, and Ipass.

Rapid synthesis of tin oxide nanostructures by microwave-assisted thermal oxidation for sensor applications

NASA Astrophysics Data System (ADS)

Phadungdhitidhada, S.; Ruankham, P.; Gardchareon, A.; Wongratanaphisan, D.; Choopun, S.

2017-09-01

In the present work nanostructures of tin oxides were synthesized by a microwave-assisted thermal oxidation. Tin precursor powder was loaded into a cylindrical quartz tube and further radiated in a microwave oven. The as-synthesized products were characterized by scanning electron microscope, transmission electron microscope, and x-ray diffractometer. The results showed that two different morphologies of SnO2 microwires (MWs) and nanoparticles (NPs) were obtained in one minute of microwave radiation under atmospheric ambient. A few tens of the SnO2 MWs with the length of 10-50 µm were found. Some parts of the MWs were decorated with the SnO2 NPs. However, most of the products were SnO2 NPs with the diameter ranging from 30-200 nm. Preparation under loosely closed system lead to mixed phase SnO-SnO2 NPs with diameter of 30-200 nm. The single-phase of SnO2 could be obtained by mixing the Sn precursor powders with CuO2. The products were mostly found to be SnO2 nanowires (NWs) and MWs. The diameter of SnO2 NWs was less than 50 nm. The SnO2 NPs, MWs, and NWs were in the cassiterite rutile structure phase. The SnO NPs was in the tetragonal structure phase. The growth direction of the SnO2 NWs was observed in (1 1 0) and (2 2 1) direction. The ethanol sensor performance of these tin oxide nanostructures showed that the SnO-SnO2 NPs exhibited extremely high sensitivity. Invited talk at 5th Thailand International Nanotechnology Conference (Nano Thailand-2016), 27-29 November 2016, Nakhon Ratchasima, Thailand.

Examination of the Atomic Pair Distribution Function (PDF) of SiC Nanocrystals by In-situ High Pressure Diffraction

NASA Technical Reports Server (NTRS)

Grzanka, E.; Stelmakh, S.; Gierlotka, S.; Zhao, Y.; Palosz, B.; Palosz, W.

2003-01-01

Key properties of nanocrystals are determined by their real atomic structure, therefore a reasonable understanding and meaningful interpretation of their properties requires a realistic model of the structure. In this paper we present an evidence of a complex response of the lattice distances to external pressure indicating a presence of a complex structure of Sic nanopowders. The experiments were performed on nanocrystalline Sic subjected to hydrostatic or isostatic pressure using synchrotron and neutron powder diffraction. Elastic properties of the samples were examined based on X-ray diffraction data using a Diamond Anvil Cell (DAC) in HASYLAB at DESY. The dependence'of the lattice parameters and of the Bragg reflections width with pressure exhibits a ha1 nature of the properties (compressibilities) of the powders and indicates a complex structure of the grains. We interpreted tws behaviour as originating from different elastic properties of the grain interior and surface. Analysis of the dependence of individual interatomic distances on pressure was based on in-situ neutron diffraction measurements done with HbD diffractometer at LANSCE in Los Alamos National Laboratory with the Paris-Edinburgh cell under pressures up to 8 GPa (Qmax = 26/A). Interatomic distances were obtained by PDF analysis using the PDFgetN program. We have found that the interatomic distances undergo a complex, non-monotonic changes. Even under substantial pressures a considerable relaxation of the lattice may take place: some interatomic distances increase with an increase in pressure. We relate this phenomenon to: (1), changes of the microstructure of the densified material, in particular breaking of its fractal chain structure and, (2), its complex structure resembling that of a material composed of two phases, each with its distinct elastic properties.

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.

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.

Study on preferred crystal orientations of Mg-Zr-O composite protective layer in AC-PDP

NASA Astrophysics Data System (ADS)

Bingang, G.; Chunliang, L.; Zhongxiao, S.; Liu, L.; Yufeng, F.; Xing, X.; Duowang, F.

2006-11-01

In order to study the preferred crystal orientations of Mg-Zr-O composite protective layers in PDP, Mg-Zr-O composite protective layers were deposited by Electron-beam Evaporator using (MgO+ZrO{2}) powder mixture as evaporation source material. X-ray diffractometer (XRD) was used to determine preferred crystal orientations of Mg-Zr-O composite protective layers, surface morphologies of films were analyzed by FESEM and voltage characteristics were examined in a testing macroscopic discharge cell of AC-PDP. On the basis of experimental analysis, the influence of oxide addition and deposition conditions on preferred orientations of Mg-Zr-O composite protective layers were investigated. The results showed that the preferred orientations of Mg-Zr-O films were determined by lattice distortion of MgO crystal. The deposition conditions have great effects on the preferred orientations of Mg-Zr-O films. The preferred orientations affect voltage characteristics through affecting surface morphology of Mg-Zr-O films. A small amount of Zr solution in MgO can decrease firing voltage compared with using pure MgO film. Firing voltage is closely related with the [ ZrO{2}/(MgO+ZrO{2})] ratio of evaporation source materials.

Ternary germanides RERhGe2 (RE = Y, Gd-Ho) - New representatives of the YIrGe2 type

NASA Astrophysics Data System (ADS)

Voßwinkel, Daniel; Heletta, Lukas; Hoffmann, Rolf-Dieter; Pöttgen, Rainer

2016-11-01

The YIrGe2 type ternary germanides RERhGe2 (RE = Y, Gd-Ho) were synthesized from the elements by arc-melting and characterized by powder X-ray diffraction. The structure of DyRhGe2 was refined from single crystal X-ray diffractometer data: Immm, a = 426.49(9), b = 885.0(2), c = 1577.4(3) pm, wR2 = 0.0533, 637 F2 values, 30 variables (300 K data). The structure contains two crystallographically independent dysprosium atoms in pentagonal prismatic and hexagonal prismatic coordination. The three-dimensional [RhGe2] polyanion is stabilized through covalent Rh-Ge (243-261 pm) and Ge-Ge (245-251 pm) bonding. The close structural relationship with the slightly rhodium-poorer germanides RE5Rh4Ge10 (≡ RERh0.8Ge2) is discussed. Temperature-dependent magnetic susceptibility measurements reveal Pauli paramagnetism for YRhGe2 and Curie-Weiss paramagnetism for RERhGe2 with RE = Gd, Tb, Dy and Ho. These germanides order antiferromagnetically at TN = 7.2(5), 10.6(5), 8.1(5), and 6.4(5) K, respectively.

Synthesis of netlike gold nanoparticles using ampicillin as a stabilizing reagent and its application

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

Song, Y.Z., E-mail: singyuanzhi@sina.com; Zhou, J.F.; Song, Y., E-mail: songyang@mail.buct.edu.cn

Graphical abstract: Electrochemical deposition of netlike gold nanoparticles (GNPs) on the surface of glassy carbon electrode and preparation of netlike GNPs in aqueous solution using ampicillin as a stabilizing reagent were proposed. The catalytic properties of netlike gold nanoparticles on the glassy carbon electrode for dopamine were demonstrated. The results indicate that the netlike gold nanoparticle modified electrode has an excellent repeatability and reproducibility. Display Omitted Highlights: ► Synthesis of netlike gold nanoparticles using ampicillin as a stabilizing reagent. ► Excellent repeatability and reproducibility of netlike gold nanoparticle modified glassy carbon electrode. ► The catalytic properties of netlike gold nanoparticlemore » for dopamine. -- Abstract: Electrochemical deposition of netlike gold nanoparticles on the surface of glassy carbon electrode and preparation of netlike GNPs in aqueous solution using ampicillin as a stabilizing reagent were proposed. The netlike gold nanoparticles were characterized by scanning electron microscope, transmission electron microscope, infrared spectrometer, UV spectrophotometer, powder X-ray diffractometer and electrochemical analyzer. The catalysis of the netlike gold nanoparticles on the glassy carbon electrode for dopamine was demonstrated. The results indicate that the gold nanoparticle modified electrode has an excellent repeatability and reproducibility.« less

Synthesis and dc electrical conductivity of Cr-doped CeO2 nanoparticles by solution combustion method

NASA Astrophysics Data System (ADS)

Harish, B. M.; Avinash, B. S.; Chaturmukha, V. S.; Jayanna, H. S.; Suresh, S.; Naveen, C. S.; Lamani, Ashok R.

2018-04-01

NPs of Ce1-xCrxO2 (x=0, 0.04, 0.08, 0.12) have been synthesized by solution combustion method using glycine as fuel. The effect of chromium on structural and dc electrical conductivity of cerium oxide nanoparticles were investigated. The obtained powder is characterized by UV-visible spectrometer, X-ray diffractometer (XRD), Scanning electron microscope (SEM) and Energy dispersive X-Ray analysis (EDS). X-ray diffraction analysis carried out on calcined samples reveals that successful incorporation of Cr2+ in CeO2 lattice where as SEM studies confirms the porous morphological structure of the prepared sample. The Keithley source meter is used to measure the dc conductivity of samples in the temperature range from 303K to 623K. The conductivity was found to be increases with increase of temperature as well as the Cr concentration due to semiconducting behavior of material and change in the charge carrier concentration. The activation energy decreases with increasing chromium concentration. The present work deals with the effect of chromium additive on structural and the D.C electrical properties Ce1-xCrxO2 NPs.

Data acquisition of neutron crystallography on tetragonal and triclinic forms of hen-egg-white (HEW) lysozyme with an elastically bent Si monochromator

NASA Astrophysics Data System (ADS)

Tanaka, I.; Minezaki, Y.; Harada, K.; Niimura, N.

An elastically bent silicon (EBSi) as a monochromator has been optimized for neutron diffractometers of biocrystallography. It was found that several stacked thin Si plates were easier to be bent much for the near focusing point and they increased neutron reflectivity by aligning the plates. Currently, an EBSi(1 1 1) monochromator system was equipped at a diffractometer (BIX-I). It took 50 days to collect about 12 000 reflections of hen-egg-white lysozyme. The minimum d-spacing was 2.1 Å.

Non-destructive and rapid prediction of moisture content in red pepper (Capsicum annuum L.) powder using near-infrared spectroscopy and a partial least squares regression model

USDA-ARS?s Scientific Manuscript database

Purpose: The aim of this study was to develop a technique for the non-destructive and rapid prediction of the moisture content in red pepper powder using near-infrared (NIR) spectroscopy and a partial least squares regression (PLSR) model. Methods: Three red pepper powder products were separated in...

USING POWDERED ACTIVATED CARBON: A CRITICAL REVIEW

EPA Science Inventory

Because the performance of powdered activated carbon (PAC) for uses other than taste and odor control is poorly documented, the purpose of this article is to critically review uses that have been reported (i.e., pesticides and herbicides, synthetic organic chemicals, and trihalom...

A 16-ch module for thermal neutron detection using ZnS:6LiF scintillator with embedded WLS fibers coupled to SiPMs and its dedicated readout electronics

NASA Astrophysics Data System (ADS)

Mosset, J.-B.; Stoykov, A.; Greuter, U.; Gromov, A.; Hildebrandt, M.; Panzner, T.; Schlumpf, N.

2017-02-01

A scalable 16-ch thermal neutron detection system has been developed in the framework of the upgrade of a neutron diffractometer. The detector is based on a ZnS:6LiF scintillator with embedded WLS fibers which are read out with SiPMs. In this paper, we present the 16-ch module, the dedicated readout electronics, a direct comparison between the performance of the diffractometer obtained with the current 3He detector and with the 16-ch detection module, and the channel-to-channel uniformity.

The new materials science diffractometer STRESS-SPEC at FRM-II

NASA Astrophysics Data System (ADS)

Hofmann, M.; Schneider, R.; Seidl, G. A.; Rebelo-Kornmeier, J.; Wimpory, R. C.; Garbe, U.; Brokmeier, H.-G.

2006-11-01

In response to the development of new materials and the application of materials and components in new technologies the direct measurement, calculation and evaluation of textures and residual stresses has gained worldwide significance in recent years. In order to cater for the development of these analytical techniques the Materials Science Diffractometer STRESS-SPEC at FRM-II is designed to be equally applied to texture or residual stress analysis by virtue of its flexible configuration and the high neutron flux at the sample position. The instrument is now available for routine operation and here we present details of first experiments and instrument performance.

90-kilobar diamond-anvil high-pressure cell for use on an automatic diffractometer.

PubMed

Schiferl, D; Jamieson, J C; Lenko, J E

1978-03-01

A gasketed diamond-anvil high-pressure cell is described which can be used on a four-circle automatic diffractometer to collect x-ray intensity data from single-crystal samples subjected to truly hydrostatic pressures of over 90 kilobars. The force generating system exerts only forces normal to the diamond faces to obtain maximum reliability. A unique design allows exceptionally large open areas for maximum x-ray access and is particularly well suited for highly absorbing materials, as the x rays are not transmitted through the sample. Studies on ruby show that high-pressure crystal structure determinations may be done rapidly, reliably, and routinely with this system.

Texture analysis at neutron diffractometer STRESS-SPEC

NASA Astrophysics Data System (ADS)

Brokmeier, H.-G.; Gan, W. M.; Randau, C.; Völler, M.; Rebelo-Kornmeier, J.; Hofmann, M.

2011-06-01

In response to the development of new materials and the application of materials and components in advanced technologies, non-destructive measurement methods of textures and residual stresses have gained worldwide significance in recent years. The materials science neutron diffractometer STRESS-SPEC at FRM II (Garching, Germany) is designed to be applied equally to texture and residual stress analyses by virtue of its very flexible configuration. Due to the high penetration capabilities of neutrons and the high neutron flux of STRESS-SPEC it allows a combined analysis of global texture, local texture, strain pole figure and FWHM pole figure in a wide variety of materials including metals, alloys, composites, ceramics and geological materials. Especially, the analysis of texture gradients in bulk materials using neutron diffraction has advantages over laboratory X-rays and EBSD for many scientific cases. Moreover, neutron diffraction is favourable for coarse-grained materials, where bulk information averaged over texture inhomogeneities is needed, and also stands out due to easy sample preparation. In future, the newly developed robot system for STRESS-SPEC will allow much more flexibility than an Eulerian cradle as on standard instruments. Five recent measurements are shown to demonstrate the wide range of possible texture applications at STRESS-SPEC diffractometer.

Superconducting YBa2Cu3O7 Powder: Reduction of Carbon, Moisture, and Impurity Phase Concentrations in Commercial Powders and the Reactivity with Moisture and Carbon Dioxide

NASA Technical Reports Server (NTRS)

Stecura, Stephan

1994-01-01

The purpose of this study was to determine the experimental parameters under which commercially pure YBa2Cu3O7 (1237) powders would be converted into a single phase (1237) powder only. Carbon (present as carbonate) and impurity phase concentrations in the (1237) powder are very dependent upon the firing temperatures, heat-treating temperatures and times, and atmosphere, while the moisture concentration is not. YBa2Cu3O7 powder with about 0.03 wt/%, carbon, 0.03 wt% moisture, and low impurity phase concentrations was obtained. Moisture and carbon concentrations in heat-treated powders did not increase significantly after 48 and 72 h of exposure to air, respectively, and after 144 h of exposure they were less than 0.26 and 0.08 wt/%, respectively. The (1237) powder first reacts with moisture and then hydroxide reacts with CO2. Firing the as received powders in air led to the decomposition of the superconducting (1237) phase.

Preliminary Tests of Gloss-Reduction and Coloring Agents for Camouflage of Polyvinyl Acetate Dust-Control Film

DTIC Science & Technology

1976-02-01

extenders Kaolin powder Calcium carbonate dust Paint flatteners Celite h99 Nytal 1+00 Dry pigments Chalk dust (various colors) Liquid...a dispersant or wetting agent for satisfactory mixing. Vor this purpose, one of two agents was used: (a) a commercial 10 per- cent determent...pockets of unmixed powder, and in some cases the powder settled to the bottom of the mold. The dispersants that were tried did not effectively disperse

Vacuum System Upgrade for Extended Q-Range Small-Angle Neutron Scattering Diffractometer (EQ-SANS) at SNS

DOE PAGES

Stone, Christopher M.; Williams, Derrick C.; Price, Jeremy P.

2016-09-23

The Extended Q-Range Small-Angle Neutron Scattering Diffractometer (EQ-SANS) instrument at the Spallation Neutron Source (SNS), Oak Ridge, Tennessee, incorporates a 69m3 detector vessel with a vacuum system which required an upgrade with respect to performance, ease of operation, and maintenance. The upgrade focused on improving pumping performance as well as optimizing system design to minimize opportunity for operational error. This upgrade provided the following practical contributions: Reduced time required to evacuate from atmospheric pressure to 2mTorr from 500-1,000 minutes to 60-70 minutes Provided turn-key automated control with a multi-faceted interlock for personnel and machine safety.

In-line metrology for roll-to-roll UV assisted nanoimprint lithography using diffractometry

NASA Astrophysics Data System (ADS)

Kreuzer, Martin; Whitworth, Guy L.; Francone, Achille; Gomis-Bresco, Jordi; Kehagias, Nikolaos; Sotomayor-Torres, Clivia M.

2018-05-01

We describe and discuss the optical design of a diffractometer to carry out in-line quality control during roll-to-roll nanoimprinting. The tool measures diffractograms in reflection geometry, through an aspheric lens to gain fast, non-invasive information of any changes to the critical dimensions of target grating structures. A stepwise tapered linear grating with constant period was fabricated in order to detect the variation in grating linewidth through diffractometry. The minimum feature change detected was ˜40 nm to a precision of 10 nm. The diffractometer was then integrated with a roll-to-roll UV assisted nanoimprint lithography machine to gain dynamic measurements in situ.

Vacuum System Upgrade for Extended Q-Range Small-Angle Neutron Scattering Diffractometer (EQ-SANS) at SNS

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

Stone, Christopher M.; Williams, Derrick C.; Price, Jeremy P.

The Extended Q-Range Small-Angle Neutron Scattering Diffractometer (EQ-SANS) instrument at the Spallation Neutron Source (SNS), Oak Ridge, Tennessee, incorporates a 69m3 detector vessel with a vacuum system which required an upgrade with respect to performance, ease of operation, and maintenance. The upgrade focused on improving pumping performance as well as optimizing system design to minimize opportunity for operational error. This upgrade provided the following practical contributions: Reduced time required to evacuate from atmospheric pressure to 2mTorr from 500-1,000 minutes to 60-70 minutes Provided turn-key automated control with a multi-faceted interlock for personnel and machine safety.

AND/R: Advanced neutron diffractometer/reflectometer for investigation of thin films and multilayers for the life sciences

PubMed Central

Dura, Joseph A.; Pierce, Donald J.; Majkrzak, Charles F.; Maliszewskyj, Nicholas C.; McGillivray, Duncan J.; Lösche, Mathias; O'Donovan, Kevin V.; Mihailescu, Mihaela; Perez-Salas, Ursula; Worcester, David L.; White, Stephen H.

2011-01-01

An elastic neutron scattering instrument, the advanced neutron diffractometer/reflectometer (AND/R), has recently been commissioned at the National Institute of Standards and Technology Center for Neutron Research. The AND/R is the centerpiece of the Cold Neutrons for Biology and Technology partnership, which is dedicated to the structural characterization of thin films and multilayers of biological interest. The instrument is capable of measuring both specular and nonspecular reflectivity, as well as crystalline or semicrystalline diffraction at wave-vector transfers up to approximately 2.20 Å−1. A detailed description of this flexible instrument and its performance characteristics in various operating modes are given. PMID:21892232

Compositional Tuning, Crystal Growth, and Magnetic Properties of Iron Phosphate Oxide

NASA Astrophysics Data System (ADS)

Tarne, Michael

Iron phosphate oxide, Fe3PO4O 3, is a crystalline solid featuring magnetic Fe3+ ions on a complex lattice composed of closely-spaced triangles. Previous work from our research group on this compound has proposed a helical magnetic structure below T = 163 K attributed to J1 - J2 competing interactions between nearest-neighbor and next-nearest-neighbor iron atoms. This was based on neutron powder diffraction featuring unique broad, flat-topped magnetic reflections due to needle-like magnetic domains. In order to confirm the magnetic structure and origins of frustration, this thesis will expand upon the research focused on this compound. The first chapter focuses on single crystal growth of Fe3PO 4O3. While neutron powder diffraction provides insight to the magnetic structure, powder and domain averaging obfuscate a conclusive structure for Fe3PO4O3 and single crystal neutron scattering is necessary. Due to the incongruency of melting, single crystal growth has proven challenging. A number of techniques including flux growth, slow cooling, and optical floating zone growth were attempted and success has been achieved via heterogenous chemical vapor transport from FePO 4 using ZrCl4 as a transport agent. These crystals are of sufficient size for single crystal measurements on modern neutron diffractometers. Dilution of the magnetic sublattice in frustrated magnets can also provide insight into the nature of competing spin interactions. Dilution of the Fe 3+ lattice in Fe3PO4O3 is accomplished by substituting non-magnetic Ga3+ to form the solid solution series Fe3-xGaxPO4O3 with x = 0, 0.012, 0.06, 0.25, 0.5, 1.0, 1.5. The magnetic susceptibility and neutron powder diffraction data of these compounds are presented. A dramatic decrease of the both the helical pitch length and the domain size is observed with increasing x; for x > 0.5, the compounds lack long range magnetic order. The phases that do exhibit magnetic order show a decrease in helical pitch with increasing x as determined from the magnitude of the magnetic propagation vector. This trend can be qualitatively reproduced by increasing the ratio of J2/ J1 in the Heisenberg model. Intriguingly, the domain size extracted from peak broadening of the magnetic reflections is nearly equal to the pitch length for each value of x, which suggests that the two qualities are linked in this unusual antiferromagnet. The last chapter focuses on the oxyfluoride Fe3PO7-x Fx. Through fluorination using low-temperature chimie douce reactions with polytetrafluoroethylene, the magnetic properties show changes in the magnetic susceptibility, isothermal magnetization, and neutron powder diffraction. The magnetic susceptibility shows a peak near T = 13 K and a zero field cooled/field cooled splitting at T = 78 K. The broad, flat-topped magnetic reflections in the powder neutron diffraction exhibit a decrease in width and increase in intensity. The changes in the neutron powder diffraction suggest an increase in correlation length in the ab plane of the fluorinated compound. Iron phosphate oxide is a unique lattice showing a rich magnetic phase diagram in both the gallium-substituted and fluorinated species. While mean-field interactions are sufficient to describe interactions in the solid solution series Fe3-xGaxPO4O3, the additional magnetic transitions in Fe3PO7-xFx suggest a more complicated set of interactions.

METHOD OF PREPARING SINTERED ZIRCONIUM METAL FROM ITS HYDRIDES

DOEpatents

Angier, R.P.

1958-02-11

The invention relates to the preparation of metal shapes from zirconium hydride by powder metallurgical techniques. The zirconium hydride powder which is to be used for this purpose can be prepared by rendering massive pieces of crystal bar zirconium friable by heat treatment in purified hydrogen. This any then be ground into powder and powder can be handled in the air without danger of it igniting. It may then be compacted in the normal manner by being piaced in a die. The compact is sintered under vacuum conditions preferably at a temperature ranging from 1200 to 1300 deg C and for periods of one to three hours.

Phosphorus Effects of Mesoporous Bioactive Glass on Occlude Exposed Dentin

PubMed Central

Chen, Wen-Cheng; Chen, Cheng-Hwei; Kung, Jung-Chang; Hsiao, Yu-Cheng; Shih, Chi-Jen; Chien, Chi-Sheng

2013-01-01

In recent studies, sealing of exposed dentinal tubules is generally considered as one of the most effective strategies to treat dentin hypersensitivity. Mesoporous bioactive glass (MBG) is a potential material for treating dentin hypersensitivity due to its highly specific areas for dissolution and re-precipitated reaction for reduction in dentin permeability. The groups of commercial products of PerioGlas®, synthetic MBG and MBG without phosphorus (MBGNP) were compared. The MBG and MBGNP powders were prepared by the sol-gel method and mixed with different calculated ratios of phosphoric acid (PA) and then was brushed onto dentin surfaces. We used X-ray diffractometer (XRD), scanning electronic microscope (SEM), and Fourier transform infrared spectroscopy (FTIR) to investigate the physiochemistry and the occlusion ability of dentinal tubules. The results showed that MBG paste mixed with PA solution has a better ability for occluding dentinal tubules than MBGNP; it has a short reaction time and good operability. The major crystallite phase of MBG agents was monocalcium phosphate monohydrate [Ca(H2PO4)2·H2O] in the early stages of the reactions. MBG pastes that were mixed with 30% and 40% PA had the ability to create excellent penetration depth greater than 80 μm. These agents have the potential to treat dentin hypersensitivity. PMID:28788393

A novel sol-gel-derived calcium silicate cement with short setting time for application in endodontic repair of perforations

PubMed Central

Lee, Bor-Shiunn; Lin, Hong-Ping; Chan, Jerry Chun-Chung; Wang, Wei-Chuan; Hung, Ping-Hsuan; Tsai, Yu-Hsin; Lee, Yuan-Ling

2018-01-01

Mineral trioxide aggregate (MTA) is the most frequently used repair material in endodontics, but the long setting time and reduced mechanical strength in acidic environments are major shortcomings. In this study, a novel sol-gel-derived calcium silicate cement (sCSC) was developed using an initial Ca/Si molar ratio of 3, with the most effective mixing orders of reactants and optimal HNO3 catalyst volumes. A Fourier transform infrared spectrometer, scanning electron microscope with energy-dispersive X-ray spectroscopy, and X-ray powder diffractometer were used for material characterization. The setting time, compressive strength, and microhardness of sCSC after hydration in neutral and pH 5 environments were compared with that of MTA. Results showed that sCSC demonstrated porous microstructures with a setting time of ~30 min, and the major components of sCSC were tricalcium silicate, dicalcium silicate, and calcium oxide. The optimal formula of sCSC was sn200, which exhibited significantly higher compressive strength and microhardness than MTA, irrespective of neutral or pH 5 environments. In addition, both sn200 and MTA demonstrated good biocompatibility because cell viability was similar to that of the control. These findings suggest that sn200 merits further clinical study for potential application in endodontic repair of perforations. PMID:29386894

A novel sol-gel-derived calcium silicate cement with short setting time for application in endodontic repair of perforations.

PubMed

Lee, Bor-Shiunn; Lin, Hong-Ping; Chan, Jerry Chun-Chung; Wang, Wei-Chuan; Hung, Ping-Hsuan; Tsai, Yu-Hsin; Lee, Yuan-Ling

2018-01-01

Mineral trioxide aggregate (MTA) is the most frequently used repair material in endodontics, but the long setting time and reduced mechanical strength in acidic environments are major shortcomings. In this study, a novel sol-gel-derived calcium silicate cement (sCSC) was developed using an initial Ca/Si molar ratio of 3, with the most effective mixing orders of reactants and optimal HNO 3 catalyst volumes. A Fourier transform infrared spectrometer, scanning electron microscope with energy-dispersive X-ray spectroscopy, and X-ray powder diffractometer were used for material characterization. The setting time, compressive strength, and microhardness of sCSC after hydration in neutral and pH 5 environments were compared with that of MTA. Results showed that sCSC demonstrated porous microstructures with a setting time of ~30 min, and the major components of sCSC were tricalcium silicate, dicalcium silicate, and calcium oxide. The optimal formula of sCSC was sn200, which exhibited significantly higher compressive strength and microhardness than MTA, irrespective of neutral or pH 5 environments. In addition, both sn200 and MTA demonstrated good biocompatibility because cell viability was similar to that of the control. These findings suggest that sn200 merits further clinical study for potential application in endodontic repair of perforations.

Nonstoichiometric Zn Ferrite and ZnFe2O4/Fe2O3 Composite Spheres: Preparation, Magnetic Properties, and Chromium Removal

NASA Astrophysics Data System (ADS)

Hang, Chun-Liang; Yang, Li-Xia; Sun, Chang-Mei; Liang, Ying

2018-03-01

Monodisperse and porous nonstoichiometric Zn ferrite can be prepared by a solvothermal method. Such non-Zn ferrite was used to be the precursor for synthesis of ZnFe2O4/Fe2O3 composite via calcination at 600°C for 3 h in air. X-ray powder diffractometer (XRD) and Energy Dispersive Spectrometer (EDS) proved the nonstoichiometry of Zn ferrite synthesized by solvothermal method and the formation of ZnFe2O4/Fe2O3 composite via calcination. TEM image showed that non-Zn ferrite spheres with wormlike nanopore structure were made of primary nanocrystals. BET surface area of non-Zn ferrite was much higher than that of ZnFe2O4/Fe2O3 composite. Saturation magnetization of non-Zn ferrites was significantly higher than that of ZnFe2O4/Fe2O3 composites. Calcination of non-Zn ferrite resulted in the formation of large amount of non-magnetic Fe2O3,which caused a low magnetization of composite. Because of higher BET surface area and higher saturation magnetization, non-Zn ferrite presented better Cr6+ adsorption property than ZnFe2O4/Fe2O3 composites.

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

Voßwinkel, Daniel; Heletta, Lukas; Hoffmann, Rolf-Dieter

The YIrGe{sub 2} type ternary germanides RERhGe{sub 2} (RE = Y, Gd-Ho) were synthesized from the elements by arc-melting and characterized by powder X-ray diffraction. The structure of DyRhGe{sub 2} was refined from single crystal X-ray diffractometer data: Immm, a = 426.49(9), b = 885.0(2), c = 1577.4(3) pm, wR2 = 0.0533, 637 F{sup 2} values, 30 variables (300 K data). The structure contains two crystallographically independent dysprosium atoms in pentagonal prismatic and hexagonal prismatic coordination. The three-dimensional [RhGe{sub 2}] polyanion is stabilized through covalent Rh–Ge (243–261 pm) and Ge–Ge (245–251 pm) bonding. The close structural relationship with the slightlymore » rhodium-poorer germanides RE{sub 5}Rh{sub 4}Ge{sub 10} (≡ RERh{sub 0.8}Ge{sub 2}) is discussed. Temperature-dependent magnetic susceptibility measurements reveal Pauli paramagnetism for YRhGe{sub 2} and Curie-Weiss paramagnetism for RERhGe{sub 2} with RE = Gd, Tb, Dy and Ho. These germanides order antiferromagnetically at T{sub N} = 7.2(5), 10.6(5), 8.1(5), and 6.4(5) K, respectively. - Graphical abstract: The germanides RERhGe{sub 2} (RE = Y, Gd-Ho) are new representatives of the YIrGe{sub 2} type.« less

Effect of Sc{sup 3+} on structural and magnetic properties of Mn-Zn nano ferrites

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

Angadi, Jagadeesha V.; Matteppanavar, Shidaling; Srinatha, N.

2016-05-23

In the present investigation, for the first time, we report on the effect of Sc{sup 3+} on the structural and magnetic properties of Mn{sub 0.5}Zn{sub 0.5}Sc{sub y}Fe{sub 2-y}O{sub 4} (y = 0.01, 0.03 and 0.05) nanoferrites synthesized by solution combustion method using the mixture of fuels. As synthesized powders were characterized for the detailed structural analysis by X-ray diffractometer (XRD), Fourier transmission infrared spectroscopy (FTIR) and room temperature magnetic properties by using vibrating sample magnetometer (VSM). The results of XRD and FTIR confirm that the formation of nano crystalline, single-phased Mn-Zn ferrite with cubic spinel structure belongs to Fd-3m spacemore » group. The room temperature magnetic studies shows that, the saturation magnetization (M{sub S}), remanence magnetization (M{sub R}) and magnetic moment (η{sub B}), magnetic particle size (D{sub m}) have found to increase with Sc{sup 3+} ion concentration up to x = 0.3 and then decrease. The values of αY-K and the magnetic particle size (D{sub m}) are found to be in the range of 68-75° and 10-19 nm respectively, with Sc{sup 3+} concentration.« less

Correlating capacity and Li content in layered material for Li-ion battery using XRD and particle size distribution measurements

NASA Astrophysics Data System (ADS)

Al-Tabbakh, A. A. A.; Al-Zubaidi, A. B.; Kamarulzaman, N.

2016-03-01

A lithiated transition-metal oxide material was successfully synthesized by a combustion method for Li-ion battery. The material was characterized using thermogravimetric and particle size analyzers, scanning electron microscope and X-ray diffractometer. The calcined powders of the material exhibited a finite size distribution and a single phase of pure layered structure of space group Roverline{3} m . An innovative method was developed to calculate the material electrochemical capacity based on considerations of the crystal structure and contributions of Li ions from specified unit cells at the surfaces and in the interiors of the material particles. Results suggested that most of the Li ions contributing to the electrochemical current originated from the surface region of the material particles. It was possible to estimate the thickness of the most delithiated region near the particle surfaces at any delithiation depth accurately. Furthermore, results suggested that the core region of the particles remained electrochemically inaccessible in the conventional applied voltages. This result was justified by direct quantitative comparison of specific capacity values calculated from the particle size distribution with those measured experimentally. The present analysis is believed to be of some value for estimation of the failure mechanism in cathode compounds, thus assisting the development of Li-ion batteries.

Berberine and zinc oxide-based nanoparticles for the chemo-photothermal therapy of lung adenocarcinoma.

PubMed

Kim, Sungyun; Lee, Song Yi; Cho, Hyun-Jong

2018-05-16

Organic/inorganic hydrid nanoparticles (NPs) composed of berberine (BER) and zinc oxide (ZnO) were developed for the therapy of lung cancers. Without the use of pharmaceutical excipients, NPs were fabricated with only dual anticancer agents (BER and ZnO) by facile blending method. The mean weight ratio between BER and ZnO in BER-ZnO NPs was 39:61 in this study. BER-ZnO NPs dispersed in water exhibited 200-300 nm hydrodynamic size under 5 mg/mL concentration. The exposure of both BER and ZnO in the outer layers of BER-ZnO NPs was identified by X-ray photoelectron spectroscopy analysis. The amorphization of BER and the maintenance of ZnO structure were observed in the results of X-ray powder diffractometer analysis. Improved antiproliferation efficacy, based on the chemo-photothermal therapeutic efficacy, of BER-ZnO NPs in A549 (human lung adenocarcinoma) cells was presented. According to the blood tests in rats after intravenous administration, BER-ZnO NPs did not induce severe hepatotoxicity, renal toxicity, and hemotoxicity. Developed BER-ZnO NPs can be used efficiently and safely for the chemo-photothermal therapy of lung cancers. Copyright © 2018 Elsevier Inc. All rights reserved.

A Nanoporous Carbon/Exfoliated Graphite Composite For Supercapacitor Electrodes

NASA Astrophysics Data System (ADS)

Rosi, Memoria; Ekaputra, Muhamad P.; Iskandar, Ferry; Abdullah, Mikrajuddin; Khairurrijal

2010-12-01

Nanoporous carbon was prepared from coconut shells using a simple heating method. The nanoporous carbon is subjected to different treatments: without activation, activation with polyethylene glycol (PEG), and activation with sodium hydroxide (NaOH)-PEG. The exfoliated graphite was synthesized from graphite powder oxidized with zinc acetate (ZnAc) and intercalated with polyvinyl alcohol (PVA) and NaOH. A composite was made by mixing the nanoporous carbon with NaOH-PEG activation, the exfoliated graphite and a binder of PVA solution, grinding the mixture, and annealing it using ultrasonic bath for 1 hour. All of as-synthesized materials were characterized by employing a scanning electron microscope (SEM), a MATLAB's image processing toolbox, and an x-ray diffractometer (XRD). It was confirmed that the composite is crystalline with (002) and (004) orientations. In addition, it was also found that the composite has a high surface area, a high distribution of pore sizes less than 40 nm, and a high porosity (67%). Noting that the pore sizes less than 20 nm are significant for ionic species storage and those in the range of 20 to 40 nm are very accessible for ionic clusters mobility across the pores, the composite is a promising material for the application as supercapacitor electrodes.

Magnesium and cadmium containing Heusler phases REPd2Mg, REPd2Cd, REAg2Mg, REAu2Mg and REAu2Cd

NASA Astrophysics Data System (ADS)

Johnscher, Michael; Stein, Sebastian; Niehaus, Oliver; Benndorf, Christopher; Heletta, Lukas; Kersting, Marcel; Höting, Christoph; Eckert, Hellmut; Pöttgen, Rainer

2016-02-01

Twenty-eight new Heusler phases REPd2Mg, REPd2Cd, REAg2Mg, REAu2Mg and REAu2Cd with different rare earth elements were synthesized from the elements in sealed niobium ampoules in a water-cooled sample chamber of an induction furnace. The samples were characterized by powder X-ray diffraction. The cell volumes show the expected lanthanide contraction. The structures of YPd2Cd, GdPd2Cd, GdAu2Cd, Y1.12Ag2Mg0.88 and GdAg2Mg were refined based on single crystal diffractometer data. The magnetic properties were determined for fifteen phase pure samples. LuAu2Mg is a weak Pauli paramagnet with a susceptibility of 1.0(2) × 10-5 emu mol-1 at room temperature. The remaining samples show stable trivalent rare earth ions and most of them order magnetically at low temperatures. The ferromagnet GdAg2Mg shows the highest ordering temperature of TC = 98.3 K. 113Cd and 89Y MAS NMR spectra of YAu2Cd and YPd2Cd confirm the presence of unique crystallographic sites. The resonances are characterized by large Knight shifts, whose magnitude can be correlated with electronegativity trends.

Antioxidant Potential of Fruit Juice with Added Chokeberry Powder (Aronia melanocarpa).

PubMed

Šic Žlabur, Jana; Dobričević, Nadica; Pliestić, Stjepan; Galić, Ante; Bilić, Daniela Patricia; Voća, Sandra

2017-12-05

The purpose of this study was to determine the possibility of using chokeberry powder as a supplement in apple juice to increase the nutritional value of the final product with the aim of developing a new functional food product. Also, to determine the influence of ultrasound assisted extraction on the bioactive compounds content, nutritional composition and antioxidant potential of apple juice with added chokeberry powder. The juice samples with added chokeberry powder had higher antioxidant capacity, irrespective of the extraction technique used. Apple juice samples with added chokeberry powder treated with high intensity ultrasound had significantly higher content of all analyzed bioactive compounds. The application of high intensity ultrasound significantly reduced the extraction time of the plant material. A positive correlation between vitamin C content, total phenols, flavonoids and anthocyanins content and antioxidant capacity was determined in juice samples with added chokeberry powder treated with high intensity ultrasound.

The Powdering Process with a Set of Ceramic Mills for Green Tea Promoted Catechin Extraction and the ROS Inhibition Effect.

PubMed

Fujioka, Kouki; Iwamoto, Takeo; Shima, Hidekazu; Tomaru, Keiko; Saito, Hideki; Ohtsuka, Masaki; Yoshidome, Akihiro; Kawamura, Yuri; Manome, Yoshinobu

2016-04-11

For serving green tea, there are two prominent methods: steeping the leaf or the powdered leaf (matcha style) in hot water. The purpose of the present study was to reveal chemical and functional differences before and after the powdering process of green tea leaf, since powdered green tea may contribute to expanding the functionality because of the different ingesting style. In this study, we revealed that the powdering process with a ceramic mill and stirring in hot water increased the average extracted concentration of epigallocatechin gallate (EGCG) by more than three times compared with that in leaf tea using high-performance liquid chromatography (HPLC) and liquid chromatography-tandem mass Spectrometry (LC-MS/MS) analyses. Moreover, powdered green tea has a higher inhibition effect of reactive oxygen species (ROS) production in vitro compared with the same amount of leaf tea. Our data suggest that powdered green tea might have a different function from leaf tea due to the higher catechin contents and particles.

Enhancement of thermal neutron shielding of cement mortar by using borosilicate glass powder.

PubMed

Jang, Bo-Kil; Lee, Jun-Cheol; Kim, Ji-Hyun; Chung, Chul-Woo

2017-05-01

Concrete has been used as a traditional biological shielding material. High hydrogen content in concrete also effectively attenuates high-energy fast neutrons. However, concrete does not have strong protection against thermal neutrons because of the lack of boron compound. In this research, boron was added in the form of borosilicate glass powder to increase the neutron shielding property of cement mortar. Borosilicate glass powder was chosen in order to have beneficial pozzolanic activity and to avoid deleterious expansion caused by an alkali-silica reaction. According to the experimental results, borosilicate glass powder with an average particle size of 13µm showed pozzolanic activity. The replacement of borosilicate glass powder with cement caused a slight increase in the 28-day compressive strength. However, the incorporation of borosilicate glass powder resulted in higher thermal neutron shielding capability. Thus, borosilicate glass powder can be used as a good mineral additive for various radiation shielding purposes. Copyright © 2017 Elsevier Ltd. All rights reserved.

An X-Ray Diffractometer for Mineralogical Analysis of Exomars Mission

NASA Astrophysics Data System (ADS)

Marinangeli, L.; Baliva, A.; Critani, F.; Stevoli, A.; Scandelli, L.; Holland, A.; Hutchinson, I.; Nelms, N.; Delhez, R.

2006-12-01

The new results of the Mars Exploration Rovers and the Mars Express mission outline the importance of a correct assessment of the variety of geological contexts to understand the evolution of a habitable environment. The need of having complex scientific payload to perform a broad range of in situ measurements is a necessary step for a successful exobiological exploration. Furthermore, the compositional analysis of the surface samples is of fundamental importance to characterize the geological environments where life could have arisen and their evolution through time. In the last years, there has been a strong interest in Europe to develop a x-ray diffractometer (XRD) for mineralogical analyses of planetary surfaces. The identification of minerals using the diffraction technique is based on the x-ray interference with the geometrical parameters of the crystal lattice allowing an unequivocal recognition of different minerals. An US XRD instrument, CHEMIN, will flight for the first time in the NASA Mars Science Laboratory in 2009. An European XRD design has also been selected for the Pasteur Payload of the ESA ExoMars mission, planned for 2011. The proposed instrument is a miniaturised concept (1 kg) configured in a reflection geometry and will allow the identification of a large spectrum of minerals including those related to the presence of water, key element for the development of life. The complete mineralogical analysis will be performed on very small quantities of powder rock samples, thought analysis of pristine (no grinded) sample can also be achieved with the reflection configuration. Information on the elemental composition of the sample can be roughly estimated by the analysis of the x-ray fluorescence spectrum simultaneously acquired by the detection system. In order to demonstrate the instrument technological readiness for the ExoMars mission, the construction of a demonstrative prototype is on going with ESA funding. Preliminary result of the scientific evaluation of the prototype will be shown to assess the capability of the proposed concept in the identification of rock mineralogy. IRSPS and and Laben are respectively the team science coordinator and the engineering responsible for the instrument development. The detector assembly for the prototype has been developed by UK and discussion for the UK involvement on the future instrument development is on going. Delft is providing scientific contribution for the prototype evaluation.

Note: Detector collimators for the nanoscale ordered materials diffractometer instrument at the Spallation Neutron Source

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

Tamalonis, A.; Weber, J. K. R.; Neuefeind, J. C.

2015-09-01

Five neutron collimator designs were constructed and tested at the nanoscale ordered materials diffractometer (NOMAD) instrument. Collimators were made from High Density PolyEthylene (HDPE) or 5% borated HDPE. In all cases, collimators improved the signal to background ratio and reduced detection of secondary scattering. In the Q-range 10-20 (angstrom) -1, signal to background ratio improved by factors of approximately 1.6 and 2.0 for 50 and 100 mm deep collimators, respectively. In the Q-range 40-50 angstrom -1, the improvement factors were 1.8 and 2.7. Secondary scattering as measured at Q similar to 9.5 angstrom -1 was significantly decreased when the collimatorsmore » were installed.« less

Improved sample manipulation at the STRESS-SPEC neutron diffractometer using an industrial 6-axis robot for texture and strain analyses

NASA Astrophysics Data System (ADS)

Randau, C.; Brokmeier, H. G.; Gan, W. M.; Hofmann, M.; Voeller, M.; Tekouo, W.; Al-hamdany, N.; Seidl, G.; Schreyer, A.

2015-09-01

The materials science neutron diffractometer STRESS-SPEC located at FRM II is a dedicated instrument for strain and pole figure measurements. Both methods make complementary demands on sample handling. On one hand pole figure measurements need a high degree of freedom to orient small samples and on the other hand in strain investigations it is often necessary to handle large and heavy components. Therefore a robot based sample positioning system was developed, which has the capability to provide both possibilities. Based on this new robot system further developments like a full automated sample changer system for texture measurements were accomplished. Moreover this system opens the door for combined strain and texture analysis at STRESS-SPEC.

Note: Detector collimators for the nanoscale ordered materials diffractometer instrument at the Spallation Neutron Source

DOE PAGES

Tamalonis, A.; Weber, J. K. R.; Neuefeind, J. C.; ...

2015-09-09

We constructed and tested five neutron collimator designs using the nanoscale ordered materials diffractometer (NOMAD) instrument. Collimators were made from High Density PolyEthylene (HDPE) or 5% borated HDPE. In all cases, collimators improved the signal to background ratio and reduced detection of secondary scattering. Moreover, in the Q-range 10-20 Å -1, signal to background ratio improved by factors of approximately 1.6 and 2.0 for 50 and 100 mm deep collimators, respectively. In the Q-range 40-50 Å -1, the improvement factors were 1.8 and 2.7. Secondary scattering as measured at Q similar to 9.5 Å -1 was significantly decreased when themore » collimators were installed.« less

Synthesis Of Nanosized CGYO Powders Via Glycine Nitrate Methods As Precursors For Dense Ceramic Membranes

NASA Astrophysics Data System (ADS)

Kochhar, Savinder P.; Singh, Anirudh P.

2011-12-01

Glycine nitrate combustion method was used to synthesize Ce0.8Gd0.1Y0.1O1.9 powders. Soluble metal-glycine complexes, detected by infrared spectroscopy, were formed by atomic level mixing of metal cations with glycine. The concentration of glycine has been varied in order to change the fuel to oxidant ratio i.e. of glycine to nitrate (g/n) with the purpose to study the effect of concentration of glycine on the parameters of resulting CGYO powder. The ratio of glycine to nitrate per mole is 0.5, 0.7, 0.8, 0.9, 1.0, 1.2, and 1.4. Increasing the glycine increases the temperatures reached during combustion. Powders prepared from GNP method demonstrated that combustion synthesized powders have large surface area as shown by SEM.

Fabrication of zirconia composite membrane by in-situ hydrothermal technique and its application in separation of methyl orange.

PubMed

Kumar, R Vinoth; Ghoshal, Aloke Kumar; Pugazhenthi, G

2015-11-01

The main objective of the work was preparation of zirconia membrane on a low cost ceramic support through an in-situ hydrothermal crystallization technique for the separation of methyl orange dye. To formulate the zirconia film on the ceramic support, hydrothermal reaction mixture was prepared using zirconium oxychloride as a zirconia source and ammonia as a precursor. The synthesized zirconia powder was characterized by X-ray diffractometer (XRD), N2 adsorption/desorption isotherms, Thermogravimetric analysis (TGA), Fourier transform infrared analysis (FTIR), Energy-dispersive X-ray (EDX) analysis and particle size distribution (PSD) to identify the phases and crystallinity, specific surface area, pore volume and pore size distribution, thermal behavior, chemical composition and size of the particles. The porosity, morphological structure and pure water permeability of the prepared zirconia membrane, as well as ceramic support were investigated using the Archimedes' method, Field emission scanning electron microscopy (FESEM) and permeability. The specific surface area, pore volume, pore size distribution of the zirconia powder was found to be 126.58m(2)/g, 3.54nm and 0.3-10µm, respectively. The porosity, average pore size and pure water permeability of the zirconia membrane was estimated to be 42%, 0.66µm and 1.44×10(-6)m(3)/m(2)skPa, respectively. Lastly, the potential of the membrane was investigated with separation of methyl orange by means of flux and rejection as a function of operating pressure and feed concentration. The rejection was found to decrease with increasing the operating pressure and increases with increasing feed concentrations. Moreover, it showed a high ability to reject methyl orange from aqueous solution with a rejection of 61% and a high permeation flux of 2.28×10(-5)m(3)/m(2)s at operating pressure of 68kPa. Copyright © 2015 Elsevier Inc. All rights reserved.

Application of sintered titanium alloys to metal denture bases: a study of titanium powder sheets for complete denture base.

PubMed

Doi, H; Harrori, M; Hasegawa, K; Yoshinari, M; Kawada, E; Oda, Y

2001-02-01

The purpose of this study was the fabrication of titanium powder sheets to enable the application of sintered titanium alloys as metal denture bases. The effects of titanium particle shape and size, binder content, and plasticizer content on the surface smoothness, tensile strength and elongation of titanium powder sheets was investigated. To select a suitable ratio of powdered metal contents for application as a metal denture base, the effects of aluminum content in Ti sheets and various other powder metal contents in Ti-Al sheets on the density, sintering shrinkage, and bending strength were evaluated. Based on the results of the above experiments, we developed a mixed powder sheet composed of 83Ti-7Al-10Cr with TA45 titanium powder (atomized, -45 microm), and 8 mass% binder content. This titanium alloy sheet had good formability and ductility. Its sintered titanium alloy had a density of 3.2 g/cm3, sintering shrinkage of 3.8%, and bending strength of 403 MPa. The titanium alloy sheet is clinically acceptable for fabricating denture bases.

A Novel X-ray Diffractometer for the Florida Split Coil 25 Tesla Magnet

NASA Astrophysics Data System (ADS)

Wang, Shengyu; Kovalev, Alexey; Suslov, Alexey; Siegrist, Theo

2014-03-01

At National High Magnetic Field Laboratory (NHMFL), we are developing a unique X-ray diffractometer for the 25 Tesla Florida Split Coil Magnet for scattering experiments under extremely high static magnetic fields. The X-ray source is a sealed tube (copper or molybdenum anode), connected to the magnet by an evacuated beam tunnel. The detectors are either an image plate or a silicon drift detector, with the data acquisition system based on LabVIEW. Our preliminary experimental results showed that the performance of the detector electronics and the X-ray generator is reliable in the fringe magnetic fields produced at the highest field of 25 T. Using this diffractometer, we will make measurements on standard samples, such as LaB6, Al2O3 and Si, to calibrate the diffraction system. Magnetic samples, such as single crystal HoMnO3 and stainless steel 301 alloys will be measured subsequently. The addition of X-ray diffraction to the unique split coil magnet will significantly expand the NHMFL experimental capabilities. Therefore, external users will be able to probe spin - lattice interactions at static magnetic fields up to 25T. This project is supported by NSF-DMR Award No.1257649. NHMFL is supported by NSF Cooperative Agreement No. DMR-1157490, the State of Florida, and the U.S. DoE.

Ab initio simulation of diffractometer instrumental function for high-resolution X-ray diffraction1

PubMed Central

Mikhalychev, Alexander; Benediktovitch, Andrei; Ulyanenkova, Tatjana; Ulyanenkov, Alex

2015-01-01

Modeling of the X-ray diffractometer instrumental function for a given optics configuration is important both for planning experiments and for the analysis of measured data. A fast and universal method for instrumental function simulation, suitable for fully automated computer realization and describing both coplanar and noncoplanar measurement geometries for any combination of X-ray optical elements, is proposed. The method can be identified as semi-analytical backward ray tracing and is based on the calculation of a detected signal as an integral of X-ray intensities for all the rays reaching the detector. The high speed of calculation is provided by the expressions for analytical integration over the spatial coordinates that describe the detection point. Consideration of the three-dimensional propagation of rays without restriction to the diffraction plane provides the applicability of the method for noncoplanar geometry and the accuracy for characterization of the signal from a two-dimensional detector. The correctness of the simulation algorithm is checked in the following two ways: by verifying the consistency of the calculated data with the patterns expected for certain simple limiting cases and by comparing measured reciprocal-space maps with the corresponding maps simulated by the proposed method for the same diffractometer configurations. Both kinds of tests demonstrate the agreement of the simulated instrumental function shape with the measured data. PMID:26089760

Impregnation of glass fibres with polymethylmethacrylate using a powder-coating method

NASA Astrophysics Data System (ADS)

Vallittu, Pekka K.

1995-01-01

The aim of this study was to evaluate the usefulness of a powder-coating method to impregnate glass fibres with polymethylmethacrylate (PMMA) for dental purposes. The continuous unidirectional E-glass fibres, the surface of which had been treated with precured silane, were powder-coated with spherical PMMA particles. Before the powder-coated prepregs were used, the incorporated PMMA powder was dissolved with methylmethacrylate monomer. The degree of impregnation of the polymerized composite was determined with a scanning electron microscope. The results revealed that the mean degree of impregnation varied from 0.87 to 0.92, being lower in the heat-cured PMMA group (which simulated fabrication of a new denture), and higher in the autopolymerizing group (which simulated the repair of a fractured denture). The means between the two groups did not, however, differ significantly ( p=0.249). The results suggest that, even though the method has some shortcomings in terms of dental laboratory technology, the powder-coating method can be used to fabricate or repair acrylic resin-based dentures.

Design of a uranium-dioxide powder spheroidization system by plasma processing

NASA Astrophysics Data System (ADS)

Cavender, Daniel

The plasma spheroidization system (PSS) is the first process in the development of a tungsten-uranium dioxide (W-UO2) ceramic-metallic (cermet) fuel for nuclear thermal rocket (NTR) propulsion. For the purposes of fissile fuel retention, UO2 spheroids ranging in size from 50 - 100 micrometers (μm) in diameter will be encapsulated in a tungsten shell. The PSS produces spherical particles by melting angular stock particles in an argon-hydrogen plasma jet where they become spherical due to surface tension. Surrogate CeO 2 powder was used in place of UO2 for system and process parameter development. Stock and spheroidized powders were micrographed using optical and scanning electron microscopy and evaluated by statistical methods to characterize and compare the spherocity of pre and post process powders. Particle spherocity was determined by irregularity parameter. Processed powders showed a statistically significant improvement in spherocity, with greater that 60% of the examined particles having an irregularity parameter of equal to or lower than 1.2, compared to stock powder.

The Effect of Mineral Powders Derived From Industrial Wastes on Selected Mechanical Properties of Concrete

NASA Astrophysics Data System (ADS)

Galińska, Anna; Czarnecki, Sławomir

2017-10-01

In recent years, concrete has been the most popular construction material. The main component of the concrete is cement. However, its production and transport causes significant emissions of CO2. Reports in the literature show that many laboratories are attempting to modify the composition of the concrete using various additives. These attempts are primarily designed to eliminate parts of cement. The greater part of the cement will be replaced with the selected additive, the more significant is the economic and ecological effect. Most attempts are related to the replacement of the selected additive in an amount of from 10 to 30% by weight of cement. Mineral powders, which are waste material producing crushed aggregate, are increasingly used for this purpose. Management of the waste carries significant cost related to their storage and disposal. With this in mind, the aim of this study was to evaluate the effect of mineral powders derived from industrial wastes on selected mechanical properties of concrete. In particular, the aim was to determine the effect of quartz and quartz-feldspar powders. For this purpose, 40, 50, 60% by weight of the cement was replaced by the selected powders. The results obtained were analysed and compared with previous attempts to replace the selected additive in an amount of from 10 to 30% by weight of cement.

To Study Capping or Lamination Tendency of Tablets Through Evaluation of Powder Rheological Properties and Tablet Mechanical Properties of Directly Compressible Blends.

PubMed

Dudhat, Siddhi M; Kettler, Charles N; Dave, Rutesh H

2017-05-01

Air entrapment efficiency of the powders is one of the main factors leading to occurrence of capping or lamination tendency of tablets manufactured from the directly compressible powder blends. The purpose of the current research was to study this underlying cause leading to occurrence of capping or lamination of tablets through evaluation of powder rheological properties. Powder blends were prepared by addition of 0% w/w to 100% w/w of individual active pharmaceutical ingredient (API) [two model API: acetaminophen (APAP) and ibuprofen (IBU)] with microcrystalline cellulose without and with 0.5% w/w Magnesium Stearate as lubricant. Powder rheological properties were analyzed using FT4 Powder Rheometer for dynamic, bulk, and shear properties. Tablet mechanical properties of the respective blends were studied by determining the ability of the material to form tablet of specific strength under applied compaction pressure through tabletability profile. The results showed that powder rheometer distinguished the powder blends based on their ability to relieve entrapped air along with the distinctive flow characteristics. Powder blend prepared with increasing addition of APAP displayed low powder permeability as compared to IBU blends with better powder permeability, compressibility and flow characteristics. Also, lubrication of the APAP blends did not ease their ability to relieve air. Tabletability profiles revealed the potential occurrence of capping or lamination in tablets prepared from the powder blends with high APAP content. This study can help scientist to understand tableting performance at the early-developmental stages and can avoid occurrence capping and lamination of tablets.

A new x-ray interface and surface scattering environmental cell design for in situ studies of radioactive and atmosphere-sensitive samples.

PubMed

Schmidt, M; Eng, P J; Stubbs, J E; Fenter, P; Soderholm, L

2011-07-01

We present a novel design of a purpose-built, portable sample cell for in situ x-ray scattering experiments of radioactive or atmosphere sensitive samples. The cell has a modular design that includes two independent layers of containment that are used simultaneously to isolate the sensitive samples. Both layers of containment can be flushed with an inert gas, thus serving a double purpose as containment of radiological material (either as a solid sample or as a liquid phase) and in separating reactive samples from the ambient atmosphere. A remote controlled solution flow system is integrated into the containment system that allows sorption experiments to be performed on the diffractometer. The cell's design is discussed in detail and we demonstrate the cell's performance by presenting first results of crystal truncation rod measurements. The results were obtained from muscovite mica single crystals reacted with 1 mM solutions of Th(IV) with 0.1 M NaCl background electrolyte. Data were obtained in specular as well as off-specular geometry.

Investigation of the solid state properties of amoxicillin trihydrate and the effect of powder pH.

PubMed

Ghassempour, Alireza; Rafati, Hasan; Adlnasab, Laleh; Bashour, Yosef; Ebrahimzadeh, Homeira; Erfan, Mohammad

2007-11-09

The purpose of this research was to investigate some physicochemical and solid-state properties of amoxicillin trihydrate (AMT) with different powder pH within the pharmacopoeia-specified range. AMT batches prepared using Dane salt method with the pH values from 4.39 to 4.97 were subjected to further characterization studies. Optical and scanning electron microscopy showed that different batches of AMT powders were similar in crystal habit, but the length of the crystals increased as the pH increased. Further solid-state investigations using powder x-ray diffraction (PXRD) demonstrated the same PXRD pattern, but the intensity of the peaks raised by the powder pH, indicated increased crystallinity. Differential scanning calorimetry (DSC) studies further confirmed that as the powder pH increased, the crystallinity and, hence, thermal stability of AMT powders increased. Searching for the possible cause of the variations in the solid state properties, HPLC analysis showed that despite possessing the requirements of the United States Pharmacopoeia (USP) for purity/impurity profile, there was a direct relationship between the increase of the powder pH and the purity of AMT, and also decrease in the impurity I (alpha-Hydroxyphenylglycine) concentration in AMT powder. Recrystallization studies confirmed that the powder pH could be controlled by adjusting the pH of the crystallization.

A possibility of parallel and anti-parallel diffraction measurements on neu- tron diffractometer employing bent perfect crystal monochromator at the monochromatic focusing condition

NASA Astrophysics Data System (ADS)

Choi, Yong Nam; Kim, Shin Ae; Kim, Sung Kyu; Kim, Sung Baek; Lee, Chang-Hee; Mikula, Pavel

2004-07-01

In a conventional diffractometer having single monochromator, only one position, parallel position, is used for the diffraction experiment (i.e. detection) because the resolution property of the other one, anti-parallel position, is very poor. However, a bent perfect crystal (BPC) monochromator at monochromatic focusing condition can provide a quite flat and equal resolution property at both parallel and anti-parallel positions and thus one can have a chance to use both sides for the diffraction experiment. From the data of the FWHM and the Delta d/d measured on three diffraction geometries (symmetric, asymmetric compression and asymmetric expansion), we can conclude that the simultaneous diffraction measurement in both parallel and anti-parallel positions can be achieved.

Effect of ZrO2 Powders on the Pyrolysis of Polycarbosilanes Coating Under Laser Ablation

NASA Astrophysics Data System (ADS)

Cheng, Han; Chen, Zhaofeng; Tao, Jie; Yan, Bo; Li, Cong; Wang, Liangbing; Zhang, Ying; Fang, Dan; Wan, Shuicheng; Wu, Wangping

Aircrafts hold the outstanding mastery of the sky in modern wars, however the laser beam weapons can carry out laser attacking to aircrafts. The purpose of the present paper is to research on a new type laser protective material. Polycarbosilanes (PCS)/divinylbenzene mixtures containing ZrO2 powders were brushed to the surface of the aluminum alloy plates and then cured at 150°C for 6 h. The PCS-coated plates were ablated by laser for 3 s. The phase identification of as-ablated powders was examined by X-ray diffraction. The results indicated that the as-ablated powders of cured PCS were composed of major phase β-SiC and smaller amounts of free carbon. The PCS composite coating played a certain role of laser ablation resistance. The effect of added ZrO2 powders on the pyrolysis of PCS-coating under laser ablation is conspicuous.

Effects of high power ultrasonic vibration on the cold compaction of titanium.

PubMed

Fartashvand, Vahid; Abdullah, Amir; Ali Sadough Vanini, Seyed

2017-05-01

Titanium has widely been used in chemical and aerospace industries. In order to overcome the drawbacks of cold compaction of titanium, the process was assisted by an ultrasonic vibration system. For this purpose, a uniaxial ultrasonic assisted cold powder compaction system was designed and fabricated. The process variables were powder size, compaction pressure and initial powder compact thickness. Density, friction force, ejection force and spring back of the fabricated samples were measured and studied. The density was observed to improve under the action of ultrasonic vibration. Fine size powders showed better results of consolidation while using ultrasonic vibration. Under the ultrasonic action, it is thought that the friction forces between the die walls and the particles and those friction forces among the powder particles are reduced. Spring back and ejection force didn't considerably change when using ultrasonic vibration. Copyright © 2016 Elsevier B.V. All rights reserved.

Motorized Beam Alignment of a Commercial X-ray Diffractometer

NASA Technical Reports Server (NTRS)

Van Zandt, Noah R.; Myers, James F.; Rogers, Richard B

2013-01-01

X-ray diffraction (XRD) is a powerful analysis method that allows researchers to noninvasively probe the crystalline structure of a material. This includes the ability to determine the crystalline phases present, quantify surface residual stresses, and measure the distribution of crystallographic orientations. The Structures and Materials Division at the NASA Glenn Research Center (GRC) heavily uses the on-site XRD lab to characterize advanced metal alloys, ceramics, and polymers. One of the x-ray diffractometers in the XRD lab (Bruker D8 Discover) uses three different x-ray tubes (Cu, Cr, and Mn) for optimal performance over numerous material types and various experimental techniques. This requires that the tubes be switched out and aligned between experiments. This alignment maximizes the x-ray tube s output through an iterative process involving four set screws. However, the output of the x-ray tube cannot be monitored during the adjustment process due to standard radiation safety engineering controls that prevent exposure to the x-ray beam when the diffractometer doors are open. Therefore, the adjustment process is a very tedious series of blind adjustments, each followed by measurement of the output beam using a PIN diode after the enclosure doors are shut. This process can take up to 4 hr to perform. This technical memorandum documents an in-house project to motorize this alignment process. Unlike a human, motors are not harmed by x-ray radiation of the energy range used in this instrument. Therefore, using motors to adjust the set screws will allow the researcher to monitor the x-ray tube s output while making interactive adjustments from outside the diffractometer. The motorized alignment system consists of four motors, a motor controller, and a hand-held user interface module. Our goal was to reduce the alignment time to less than 30 min. The time available was the 10-week span of the Lewis' Educational and Research Collaborative Internship Project (LERCIP) summer internship program and the budget goal was $1200. In this report, we will describe our motorization design and discuss the results of its implementation.

Microstructure and Properties of DCP-Derived W-ZrC Composite Using Nontoxic Sodium Alginate to Fabricate WC Preform

NASA Astrophysics Data System (ADS)

Najafzadeh Khoee, Ali Asghar; Habibolahzadeh, Ali; Qods, Fathallah; Baharvandi, Hamidreza

2015-04-01

In the present work, tungsten carbide (WC) preforms were fabricated by gel-casting process, using different nontoxic Na-alginate to tertiary calcium phosphate ratios and different loadings of WC powder in the initial slurries. The gel-cast green bodies were dried and pre-sintered at 1723 K for 4 h and then reactively infiltrated by molten Zr2Cu at 1623 K for 0.5 h, to produce W-ZrC composite via displacive compensation of porosity process. The phases, microstructures, and mechanical properties of the preforms and the W-ZrC composites were investigated by Fourier transform infrared spectroscope, x-ray diffractometer (XRD), scanning electron microscope (SEM), image analyzer, and universal mechanical testing machine. XRD results, SEM micrographs, and elemental maps indicated uniform distribution of phases (W and ZrC) and elements (W, Zr, and C). Flexural strengths and hardness of the fabricated composites were in the ranges of 429-460 MPa and 7.5-9.5 GPa, respectively. Fractography studies revealed two types of dimple rupture and cleavage fracture modes in different composite samples. The W-ZrC composite was ablated by an oxyacetylene flame for 60 s. The mean value of mass and linear ablation rates of the composite were 2.1 ± 0.1 mg/s and 3.6 ± 0.5 µm/s, respectively.

Structural and magnetic properties of Ga-substituted Co 2 ‑W hexaferrites

NASA Astrophysics Data System (ADS)

Mahmood, Sami H.; Al Sheyab, Qusai; Bsoul, Ibrahim; Mohsen, Osama; Awadallah, Ahmad

2018-05-01

Precursor powders of BaMg2-xCoxFe16O27 with (x = 0.0, 1.0, and 2.0) were prepared using high-energy ball milling, and the effects of chemical composition and sintering temperature on the structural and magnetic properties were investigated using x-ray diffractometer (XRD), scanning electron microscopy (SEM), and vibrating sample magnetometry (VSM). XRD patterns of the prepared samples indicated that crystallization of pure BaW hexaferrite phase was achieved at sintering temperature of 1300{\\deg} C, while BaM and cubic spinel phase intermediate phases were obtained at lower sintering temperatures of 1100{\\deg} C and 1200{\\deg} C. SEM images revealed improvement of the crystallization of the structural phases, and growth of the particle size with increasing the sintering temperature. The magnetic data of the samples sintered at 1300{\\deg} C revealed an increase of the saturation magnetization from 59.44 emu/g to 72.56 emu/g with increasing Co concentration (x) from 0.0 to 2.0. The coercive field Hc decreased from 0.07 kOe at x = 0.0, to 0.03 kOe at x = 1.0, and then increases to 0.09 kOe at x = 2.0. The thermomagnetic curves of the samples sintered at 1300{\\deg} C confirmed the existence of the W-type phase, and revealed spin reorientation transitions above room temperature.

Preparation of Nanocrystalline Powders of ZrO2, Stabilized by Y2O3 Dobs for Ceramics

NASA Astrophysics Data System (ADS)

Petrunin, V. F.; Korovin, S. A.

The purpose of this study was to develop a synthesis conditions and produce samples of nanocrystalline zirconia powder in a high-temperature phase state. To increase the stability of this state at room temperature, Y2O3 was used as a dop in the two-stages chemical method including coprecipitation mixture of the corresponding hydroxides and air drying. To reduce agglomeration of nanoparticles during heat treatment of precursors the microwave oven instead of a muffle was used. Different characterisation methods have been used to determine that the obtained powders are nano-scale corresponds to a high-temperature tetragonal phase of ZrO2. It is shown that such nanocrystalline powders may be used to produce highly-dense nanoceramics.

Physico-Chemical Properties, Aerosolization and Dissolution of Co-Spray Dried Azithromycin Particles with L-Leucine for Inhalation

PubMed Central

Mangal, Sharad; Nie, Haichen; Xu, Rongkun; Guo, Rui; Cavallaro, Alex; Zemlyanov, Dmitry; Zhou, Qi (Tony)

2018-01-01

Purpose Inhalation therapy is popular to treat lower respiratory tract infections. Azithromycin is effective against some bacteria that cause respiratory tract infections; but it has poor water solubility that may limit its efficacy when administrated as inhalation therapy. In this study, dry powder inhaler formulations were developed by co-spray drying azithromycin with L-leucine with a purpose to improve dissolution. Methods The produced powder formulations were characterized regarding particle size, morphology, surface composition and in-vitro aerosolization performance. Effects of L-leucine on the solubility and in-vitro dissolution of azithromycin were also evaluated. Results The spray dried azithromycin alone formulation exhibited a satisfactory aerosol performance with a fine particle fraction (FPF) of 62.5 ± 4.1%. Addition of L-leucine in the formulation resulted in no significant change in particle morphology and FPF, which can be attributed to enrichment of azithromycin on the surfaces of composite particles. Importantly, compared with the spray-dried amorphous azithromycin alone powder, the co-spray dried powder formulations of azithromycin and L-leucine demonstrated a substantially enhanced in-vitro dissolution rate. Such enhanced dissolution of azithromycin could be attributed to the formation of composite system and the acidic microenvironment around azithromycin molecules created by the dissolution of acidic L-leucine in the co-spray dried powder. Fourier transform infrared spectroscopic data showed intermolecular interactions between azithromycin and L-leucine in the co-spray dried formulations. Conclusions We developed the dry powder formulations with satisfactory aerosol performance and enhanced dissolution for a poorly water soluble weak base, azithromycin, by co-spray drying with an amino acid, L-leucine. PMID:29374368

A high-temperature neutron diffraction study of Nb 2AlC and TiNbAlC

DOE PAGES

Bentzel, Grady W.; Lane, Nina J.; Vogel, Sven C.; ...

2014-12-16

In this paper, we report on the crystal structures of Nb 2AlC and TiNbAlC actual composition (Ti 0.45,Nb 0.55) 2AlC compounds determined from Rietveld analysis of neutron diffraction patterns in the 300-1173 K temperature range. The average linear thermal expansion coefficients of a Nb 2AlC sample in the a and c directions are, respectively, 7.9(5)x10 -6 K -1 and 7.7(5)x10 -6 K -1 on one neutron diffractometer and 7.3(3)x10 -6 K -1 and 7.0(2)x10 -6 K -1 on a second diffractometer. The respective values for the (Ti 0.45,Nb 0.55) 2AlC composition - only tested on one diffractometer - are 8.5(3)x10more » -6 K -1 and 7.5(5)x10 -6 K -1. These values are relatively low compared to other MAX phases. Like other MAX phases, however, the atomic displacement parameters show that the Al atoms vibrate with higher amplitudes than the Ti and C atoms, and 1 more along the basal planes than normal to them. In addition, when the predictions of the atomic displacement parameters obtained from density functional theory are compared to the experimental results, good quantitative agreement is found for the Al atoms. In case of the Nb and C atoms, the agreement was more qualitative.« less

New hardware and software platform for experiments on a HUBER-5042 X-ray diffractometer with a DISPLEX DE-202 helium cryostat in the temperature range of 20-300 K

NASA Astrophysics Data System (ADS)

Dudka, A. P.; Antipin, A. M.; Verin, I. A.

2017-09-01

Huber-5042 diffractometer with a closed-cycle Displex DE-202 helium cryostat is a unique scientific instrument for carrying out X-ray diffraction experiments when studying the single crystal structure in the temperature range of 20-300 K. To make the service life longer and develop new experimental techniques, the diffractometer control is transferred to a new hardware and software platform. To this end, a modern computer; a new detector reader unit; and new control interfaces for stepper motors, temperature controller, and cryostat vacuum pumping system are used. The system for cooling the X-ray tube, the high-voltage generator, and the helium compressor and pump for maintaining the desired vacuum in the cryostat are replaced. The system for controlling the primary beam shutter is upgraded. A biological shielding is installed. The new program tools, which use the Linux Ubuntu operating system and SPEC constructor, include a set of drivers for control units through the aforementioned interfaces. A program for searching reflections from a sample using fast continuous scanning and a priori information about crystal is written. Thus, the software package for carrying out the complete cycle of precise diffraction experiment (from determining the crystal unit cell to calculating the integral reflection intensities) is upgraded. High quality of the experimental data obtained on this equipment is confirmed in a number of studies in the temperature range from 20 to 300 K.

Titanium dental copings prepared by a powder metallurgy method: a preliminary report.

PubMed

Eriksson, Mikael; Andersson, Matts; Carlström, Elis

2004-01-01

The purpose of this study was to determine if the Procera pressed-powder method can be used to fabricate titanium copings. Commercially pure titanium powder was used to prepare the copings. The powder was pressed onto an enlarged tooth preparation die of aluminum using cold isostatic pressing. The outer shape of the coping was formed using a Procera milling machine, and the copings were vacuum sintered. Titanium copings could be prepared using this method. The density of the sintered copings reached 97% to 99%+ of theoretic density, and the copings showed ductile behavior after sintering. Enlarging the tooth preparation die to compensate for the sintering shrinkage could optimize the final size of the copings. Ductile and dense titanium dental copings can be produced with powder-metal processing using cold isostatic pressing, followed by milling and sintering to final shape. The forming technique has, if properly optimized, a potential of becoming a more cost-efficient production method than spark erosion.

Chlorhexidine binding to mineralized versus demineralized dentin powder

PubMed Central

Kim, Jongryul; Uchiyama, Toshikazu; Carrilho, Marcela; Agee, Kelli A.; Mazzoni, Annalisa; Breschi, Lorenzo; Carvalho, Ricardo M.; Tjäderhane, Leo; Looney, Stephen; Wimmer, Courtney; Tezvergil-Mutluay, Arzu; Tay, Franklin R.; Pashley, David H.

2010-01-01

Objectives The purposes of this work were to quantitate the affinity and binding capacity of chlorhexidine (CHX) digluconate to mineralized vs. demineralized dentin powder, and to determine how much debinding would result from rinsing with water, ethanol, hydroxyethylmethacrylate (HEMA) or 0.5 M NaCl in water. Methods Dentin powder was made from coronal dentin of extracted human third molars. Standard amounts of dentin powder were tumbled with increasing concentrations of CHX (0–30 mM) for 30 min at 37 C. After centrifuging the tubes, the supernatant was removed and the decrease in CHX concentration quantitated by UV-spectroscopy. CHX-treated dentin powder was resuspended in one of the four debinding solutions for 3 min. The amount of debound CHX in the solvents was also quantitated by UV-spectroscopy. Results As the CHX concentration in the medium increased, the CHX binding to mineralized dentin powder also increased up to 6.8 μmoles/g of dry dentin powder. Demineralized dentin powder took up significantly (p<0.01) more CHX, reaching 30.1 μmoles CHX/g of dry dentin powder. Debinding of CHX was in the order: HEMA < ethanol < 0.05 M NaCl < water. The highest CHX binding to demineralized dentin occurred at 30 mM (1.5 wt%). Significance As CHX is not debound by HEMA, it may remain bound to demineralized dentin during resin-dentin bonding. This may be responsible for the long-term efficacy of CHX as an MMP inhibitor in resin-dentin bonds. PMID:20472280

Design and development of dry powder sulfobutylether-β-cyclodextrin complex for pulmonary delivery of fisetin.

PubMed

Mohtar, Noratiqah; Taylor, Kevin M G; Sheikh, Khalid; Somavarapu, Satyanarayana

2017-04-01

This study has investigated complexation of fisetin, a natural flavonoid, with three types of cyclodextrins to improve its solubility. Sulfobutylether-β-cyclodextrin (SBE-β-CD) showed the highest complexation efficiency while maintaining the in vitro antioxidant activity of fisetin. Addition of 20%v/v ethanol in water improved the amount of solubilized fisetin in the complex 5.9-fold compared to the system containing water alone. Spray drying of fisetin-SBE-β-CD complex solution in the presence of ethanol produced a dry powder with improved aerosolization properties when delivered from a dry powder inhaler, indicated by a 2-fold increase in the fine particle fraction (FPF) compared to the powder produced from the complex solution containing water alone. The pitted morphological surface of these particles suggested a more hollow internal structure, indicating a lighter and less dense powder. Incorporation of 20%w/w leucine improved the particle size distribution of the powder and further increased the FPF by 2.3-fold. This formulation also showed an EC 50 value equivalent to fisetin alone in the A549 cell line. In conclusion, an inhalable dry powder containing fisetin-SBE-β-CD complex was successfully engineered with an improved aqueous solubility of fisetin. The dry powder may be useful to deliver high amounts of fisetin to the deep lung region for therapeutic purposes. Copyright © 2016. Published by Elsevier B.V.

21 CFR 182.1 - Substances that are generally recognized as safe.

Code of Federal Regulations, 2010 CFR

2010-04-01

... Commissioner regards such common food ingredients as salt, pepper, vinegar, baking powder, and monosodium... purposes indicated, in accordance with good manufacturing practice, are regarded by the Commissioner as generaly recognized as safe for such uses. (b) For the purposes of this section, good manufacturing...

21 CFR 182.1 - Substances that are generally recognized as safe.

Code of Federal Regulations, 2011 CFR

2011-04-01

... Commissioner regards such common food ingredients as salt, pepper, vinegar, baking powder, and monosodium... purposes indicated, in accordance with good manufacturing practice, are regarded by the Commissioner as generaly recognized as safe for such uses. (b) For the purposes of this section, good manufacturing...

The effect of native silk fibroin powder on the physical properties and biocompatibility of biomedical polyurethane membrane.

PubMed

Zhuang, Yan; Zhang, Qian; Feng, Jinqi; Wang, Na; Xu, Weilin; Yang, Hongjun

2017-04-01

Naturally derived fibers such as silk fibroin can potentially enhance the biocompatibility of currently used biomaterials. This study investigated the physical properties of native silk fibroin powder and its effect on the biocompatibility of biomedical polyurethane. Native silk fibroin powder with an average diameter of 3 µm was prepared on a purpose-built machine. A simple method of phase inversion was used to produce biomedical polyurethane/native silk fibroin powder hybrid membranes at different blend ratios by immersing a biomedical polyurethane/native silk fibroin powder solution in deionized water at room temperature. The physical properties of the membranes including morphology, hydrophilicity, roughness, porosity, and compressive modulus were characterized, and in vitro biocompatibility was evaluated by seeding the human umbilical vein endothelial cells on the top surface. Native silk fibroin powder had a concentration-dependent effect on the number and morphology of human umbilical vein endothelial cells growing on the membranes; cell number increased as native silk fibroin powder content in the biomedical polyurethane/native silk fibroin powder hybrid membrane was increased from 0% to 50%, and cell morphology changed from spindle-shaped to cobblestone-like as the native silk fibroin powder content was increased from 0% to 70%. The latter change was related to the physical characteristics of the membrane, including hydrophilicity, roughness, and mechanical properties. The in vivo biocompatibility of the native silk fibroin powder-modified biomedical polyurethane membrane was evaluated in a rat model; the histological analysis revealed no systemic toxicity. These results indicate that the biomedical polyurethane/native silk fibroin powder hybrid membrane has superior in vitro and in vivo biocompatibility relative to 100% biomedical polyurethane membranes and thus has potential applications in the fabrication of small-diameter vascular grafts and in tissue engineering.

Asbestos in commercial cosmetic talcum powder as a cause of mesothelioma in women

PubMed Central

Gordon, Ronald E; Fitzgerald, Sean; Millette, James

2014-01-01

Background: Cosmetic talcum powder products have been used for decades. The inhalation of talc may cause lung fibrosis in the form of granulomatose nodules called talcosis. Exposure to talc has also been suggested as a causative factor in the development of ovarian carcinomas, gynecological tumors, and mesothelioma. Purpose: To investigate one historic brand of cosmetic talcum powder associated with mesothelioma in women. Methods: Transmission electron microscope (TEM) formvar-coated grids were prepared with concentrations of one brand of talcum powder directly, on filters, from air collections on filters in glovebox and simulated bathroom exposures and human fiber burden analyses. The grids were analyzed on an analytic TEM using energy-dispersive spectrometer (EDS) and selected-area electron diffraction (SAED) to determine asbestos fiber number and type. Results: This brand of talcum powder contained asbestos and the application of talcum powder released inhalable asbestos fibers. Lung and lymph node tissues removed at autopsy revealed pleural mesothelioma. Digestions of the tissues were found to contain anthophyllite and tremolite asbestos. Discussion: Through many applications of this particular brand of talcum powder, the deceased inhaled asbestos fibers, which then accumulated in her lungs and likely caused or contributed to her mesothelioma as well as other women with the same scenario. PMID:25185462

Formulation of a dry powder influenza vaccine for nasal delivery.

PubMed

Garmise, Robert J; Mar, Kevin; Crowder, Timothy M; Hwang, C Robin; Ferriter, Matthew; Huang, Juan; Mikszta, John A; Sullivan, Vincent J; Hickey, Anthony J

2006-03-10

The purpose of this research was to prepare a dry powder vaccine formulation containing whole inactivated influenza virus (WIIV) and a mucoadhesive compound suitable for nasal delivery. Powders containing WIIV and either lactose or trehalose were produced by lyophilization. A micro-ball mill was used to reduce the lyophilized cake to sizes suitable for nasal delivery. Chitosan flakes were reduced in size using a cryo-milling technique. Milled powders were sieved between 45 and 125 microm aggregate sizes and characterized for particle size and distribution, morphology, and flow properties. Powders were blended in the micro-ball mill without the ball. Lyophilization followed by milling produced irregularly shaped, polydisperse particles with a median primary particle diameter of approximately 21 microm and a yield of approximately 37% of particles in the 45 to 125 microm particle size range. Flow properties of lactose and trehalose powders after lyophilization followed by milling and sieving were similar. Cryo-milling produced a small yield of particles in the desired size range (<10%). Lyophilization followed by milling and sieving produced particles suitable for nasal delivery with different physicochemical properties as a function of processing conditions and components of the formulation. Further optimization of particle size and morphology is required for these powders to be suitable for clinical evaluation.

The role of red dragon fruit peel (Hylocereus polyrhizus) to improvement blood lipid levels of hyperlipidaemia male mice

NASA Astrophysics Data System (ADS)

Hernawati; Setiawan, N. A.; Shintawati, R.; Priyandoko, D.

2018-05-01

The purpose of this research was to know the role of red dragon fruit peel powder to total cholesterol, triglyceride, high-density lipoprotein (HDL), low-density lipoprotein (LDL), and weight in the male hyperlipidaemic Balb-C mice (Mus musculus). This study used a completely randomized design (CRD) and four replicates for each dose treatments. Samples were 24 male mice that divided into six groups i.e. positive and negative controls, doses of 50; 100; 150 and 200 mg/kgBW/days red dragon fruit peel powder. Before being given treatment, mice were given feed containing high fat for 20 days until experiencing conditions hyperlipidaemia. The red dragon fruit peel powder was given at oral with used gavage for 30 days. Blood samples were taken from the tail on vena caudalis. Blood lipid samples were analysed at enzymatic with BIOLABO kits. The results of this study indicate that after administration of red dragon fruit peel powder total cholesterol levels, triglycerides and LDL-c decreased, along with increasing doses of red dragon fruit peel powder for 30 days. Furthermore showed that dragon fruit powder can increase HDL-c levels. The conclusion of this research was The red dragon fruit peel powder can improve blood lipid level of male Balb-c mice hyperlipidaemia.

The influence of material type and composition of TiO2- ZnO on manufacturing of paste for the application of DSSC

NASA Astrophysics Data System (ADS)

Retnaningsih, L.; Muliani, L.; Aggraini, P. N.; Hidayat, J.

2016-11-01

Research, fabrication and material selection for the application of Dye- sensitized solar cell (DSSC) has been performed on glass FTO (Flour Tin Oxide). The material is used in the form of TiO2 paste, TiO2 powder and ZnO powder. Dye-sensitized solar cell (DSSC), is a fotoelektrokimia-based solar cells where the absorption process light done by the dye molecules and the process of separation of inorganic semiconductor materials by charge of Titanium dioxide (TiO2) and Zinc oxide (ZnO). The purpose of this research is to know the exact composition of TiO2 and ZnO materials in order to produce the best efficiency with DSSC. On this research was done making prototype dye-sensitized solar cell using dye Z 907, and semiconductor nanoparticles TiO2 and ZnO powder that is made into a paste by mixing different composition in two variations of samples: A = ZnO (powder) + 40% TiO2 (powder) and B = 60% TiO2 (powder) (40%) + TiO2 (pasta) 60%. The second variation of this high efficiency is value at sample B i.e. TiO2 (powder) + 40% TiO2 (paste) of 60%.

New software to model energy dispersive X-ray diffraction in polycrystalline materials

NASA Astrophysics Data System (ADS)

Ghammraoui, B.; Tabary, J.; Pouget, S.; Paulus, C.; Moulin, V.; Verger, L.; Duvauchelle, Ph.

2012-02-01

Detection of illicit materials, such as explosives or drugs, within mixed samples is a major issue, both for general security and as part of forensic analyses. In this paper, we describe a new code simulating energy dispersive X-ray diffraction patterns in polycrystalline materials. This program, SinFullscat, models diffraction of any object in any diffractometer system taking all physical phenomena, including amorphous background, into account. Many system parameters can be tuned: geometry, collimators (slit and cylindrical), sample properties, X-ray source and detector energy resolution. Good agreement between simulations and experimental data was obtained. Simulations using explosive materials indicated that parameters such as the diffraction angle or the energy resolution of the detector have a significant impact on the diffraction signature of the material inspected. This software will be a convenient tool to test many diffractometer configurations, providing information on the one that best restores the spectral diffraction signature of the materials of interest.

Advanced setup for high-pressure and low-temperature neutron diffraction at hydrostatic conditions

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

Lokshin, Konstantin A.; Zhao Yusheng

2005-06-15

We describe a design of the experimental setup for neutron diffraction studies at low temperatures and hydrostatic pressure. The significant benefit of the setup, compared to the previous methods, is that it makes possible the simultaneous collection of neutrons diffracted at the 30 deg. -150 deg. range with no contamination by the primary scattering from the sample surroundings and without cutting out the incident and diffracted beams. The suggested design is most useful for third-generation time-of-flight diffractometers and constant wavelength instruments. Application of the setup expands the capabilities of high-pressure neutron diffraction, allowing time-resolved kinetics and structural studies, multihistogram Rietveld,more » and pair distribution function and texture analyses. The high efficiency of the setup was proven for the HIPPO diffractometer at Los Alamos Neutron Science Center under pressures up to 10 kbar and temperatures from 4 to 300 K.« less

On high-resolution reciprocal-space mapping with a triple-crystal diffractometer for high-energy X-rays.

PubMed

Liss, K D; Royer, A; Tschentscher, T; Suortti, P; Williams, A P

1998-03-01

High-energy X-rav diffraction by means of triple-crystal techniques is a powerful tool for investigating dislocations and strain in bulk materials. Radiation with an energy typically higher than 80 keV combines the advantage of low attenuation with high resolution at large momentum transfers. The triple-crystal diffractometer at the High Energy Beamline of the European Synchrotron Radiation Facility is described. It is shown how the transverse and longitudinal resolution depend on the choice of the crystal reflection, and how the orientation of a reciprocal-lattice distortion in an investigated sample towards the resolution element of the instrument can play an important role. This effect is demonstrated on a single crystal of silicon where a layer of macro pores reveals satellites around the Bragg reflection. The resulting longitudinal distortion can be investigated using the high transverse resolution of the instrument when choosing an appropriate reflection.

SMA texture and reorientation: simulations and neutron diffraction studies

NASA Astrophysics Data System (ADS)

Gao, Xiujie; Brown, Donald W.; Brinson, L. Catherine

2005-05-01

With increased usage of shape memory alloys (SMA) for applications in various fields, it is important to understand how the material behavior is affected by factors such as texture, stress state and loading history, especially for complex multiaxial loading states. Using the in-situ neutron diffraction loading facility (SMARTS diffractometer) and ex situ inverse pole figure measurement facility (HIPPO diffractometer) at the Los Alamos Neutron Science Center (LANCE), the macroscopic mechanical behavior and texture evolution of Nickel-Titanium (Nitinol) SMAs under sequential compression in alternating directions were studied. The simplified multivariant model developed at Northwestern University was then used to simulate the macroscopic behavior and the microstructural change of Nitinol under this sequential loading. Pole figures were obtained via post-processing of the multivariant results for volume fraction evolution and compared quantitatively well to the experimental results. The experimental results can also be used to test or verify other SMA constitutive models.

Composite germanium monochromators - Results for the TriCS single-crystal diffractometer at SINQ

NASA Astrophysics Data System (ADS)

Schefer, J.; Fischer, S.; Böhm, M.; Keller, L.; Horisberger, M.; Medarde, M.; Fischer, P.

Composite germanium monochromators are foremost in application in neutron diffraction due to their good scattering properties, low absorption values and the diamond structure which avoids second-order contamination when using hhk reflections (all odd). Our slices for the monochromator are built from 24 wafers, each 0.4 mm thick. The alignment of the wafers within the final composite wafer package has been improved by adding tin for the soldering process with a sputtering method instead of foils. Nine slices, each 12.5 mm high, are mounted on separate miniature goniometer heads to the focusing monochromator. The focusing angle is controlled by only one motor/digitizer by using a sophisticated mechanism. Turning the monochromator by 9° around overlineω allow access of the 311 (primary) and 511 (secondary) reflection. We also show the importance of permanent quality control with neutrons. The monochromator will be used on the single-crystal diffractometer TriCS at SINQ.

NIMROD: The Near and InterMediate Range Order Diffractometer of the ISIS second target station.

PubMed

Bowron, D T; Soper, A K; Jones, K; Ansell, S; Birch, S; Norris, J; Perrott, L; Riedel, D; Rhodes, N J; Wakefield, S R; Botti, A; Ricci, M-A; Grazzi, F; Zoppi, M

2010-03-01

NIMROD is the Near and InterMediate Range Order Diffractometer of the ISIS second target station. Its design is optimized for structural studies of disordered materials and liquids on a continuous length scale that extends from the atomic, upward of 30 nm, while maintaining subatomic distance resolution. This capability is achieved by matching a low and wider angle array of high efficiency neutron scintillation detectors to the broad band-pass radiation delivered by a hybrid liquid water and liquid hydrogen neutron moderator assembly. The capabilities of the instrument bridge the gap between conventional small angle neutron scattering and wide angle diffraction through the use of a common calibration procedure for the entire length scale. This allows the instrument to obtain information on nanoscale systems and processes that are quantitatively linked to the local atomic and molecular order of the materials under investigation.

A subchronic oral toxicity study of Salacia reticulata extract powder in rats.

PubMed

Oda, Yuriko; Yuasa, Atsuko; Ueda, Fumitaka; Kakinuma, Chihaya

2015-01-01

The safety of Salacia plant ( Salacia reticulata ) extract powder, which is used in Ayurvedic medical practices, was studied in a dose range-finding subchronic toxicity study in Crl:CD Sprague-Dawley rats. Male and female rats were randomly assigned to 4 treatment groups and were treated by oral gavage with 0, 10, 65, and 400 mg/kg body weight/day of the powder for 91 days. Body weight, food consumption, and clinical signs were assessed during the treatment period. Urinalysis, hematology, blood chemistry, and organ weights were determined one day after the final treatment. The animals were euthanized at the end of the treatment and were examined for necropsy and histopathological purposes. No adverse toxicity was observed in the Salacia powder-treated groups with a No Observed Adverse Effect Level of ≧400 mg/kg body weight/day in both male and female SD rats.

Comparative Effects of Gamma Irradiation and Ozone Treatment on Hygienic Quality of Korean Red Ginseng Powder

NASA Astrophysics Data System (ADS)

Byun, Myung-Woo; Yook, Hong-Sun; Kang, Il-Jun; Chung, Cha-Kwon; Kwon, Joong-Ho; Choi, Kang-Ju

1998-06-01

For the purpose of improving hygienic quality of Korean red ginseng powder, the comparative effects of gamma irradiation and ozone treatment on the microbial and physicochemical properties were investigated. Gamma irradiation at 7.5 kGy resulted in sterilization of total aerobic bacteria, molds and coliforms below detective levels, while ozone treatment for 8 hours up to 18 ppm did not sufficiently eliminate the microorganisms of the red ginseng powder. Physicochemical properties including compositions of the red ginseng saponin (ginsenosides) and fatty acids, pH and hydrogen doanting activity were not significantly changed by gamma irradiation, whereas, ozone treatment caused significant changes in fatty acid compositions, TBA value, pH, acidity and hydrogen donating activity. The results from this study led us to conclude that gamma irradiation was more effective than ozone treatment both for the improvement of hygienic quality and for the maintenance of physicochemical quality of red ginseng powder.

Heat transfer model and finite element formulation for simulation of selective laser melting

NASA Astrophysics Data System (ADS)

Roy, Souvik; Juha, Mario; Shephard, Mark S.; Maniatty, Antoinette M.

2017-10-01

A novel approach and finite element formulation for modeling the melting, consolidation, and re-solidification process that occurs in selective laser melting additive manufacturing is presented. Two state variables are introduced to track the phase (melt/solid) and the degree of consolidation (powder/fully dense). The effect of the consolidation on the absorption of the laser energy into the material as it transforms from a porous powder to a dense melt is considered. A Lagrangian finite element formulation, which solves the governing equations on the unconsolidated reference configuration is derived, which naturally considers the effect of the changing geometry as the powder melts without needing to update the simulation domain. The finite element model is implemented into a general-purpose parallel finite element solver. Results are presented comparing to experimental results in the literature for a single laser track with good agreement. Predictions for a spiral laser pattern are also shown.

Preparation and in vivo absorption evaluation of spray dried powders containing salmon calcitonin loaded chitosan nanoparticles for pulmonary delivery

PubMed Central

Sinsuebpol, Chutima; Chatchawalsaisin, Jittima; Kulvanich, Poj

2013-01-01

Purpose The aim of the present study was to prepare inhalable co-spray dried powders of salmon calcitonin loaded chitosan nanoparticles (sCT-CS-NPs) with mannitol and investigate pulmonary absorption in rats. Methods The sCT-CS-NPs were prepared by the ionic gelation method using sodium tripolyphosphate (TPP) as a cross-linking polyion. Inhalable dry powders were obtained by co-spray drying aqueous dispersion of sCT-CS-NPs and mannitol. sCT-CS-NPs co-spray dried powders were characterized with respect to morphology, particle size, powder density, aerodynamic diameter, protein integrity, in vitro release of sCT, and aerosolization. The plasmatic sCT levels following intratracheal administration of sCT-CS-NPs spray dried powders to the rats was also determined. Results sCT-CS-NPs were able to be incorporated into mannitol forming inhalable microparticles by the spray drying process. The sCT-CS-NPs/mannitol ratios and spray drying process affected the properties of the microparticles obtained. The conformation of the secondary structures of sCTs was affected by both mannitol content and spray dry inlet temperature. The sCT-CS-NPs were recovered after reconstitution of spray dried powders in an aqueous medium. The sCT release profile from spray dried powders was similar to that from sCT-CS-NPs. In vitro inhalation parameters measured by the Andersen cascade impactor indicated sCT-CS-NPs spray dried powders having promising aerodynamic properties for deposition in the deep lung. Determination of the plasmatic sCT levels following intratracheal administration to rats revealed that the inhalable sCT-CS NPs spray dried powders provided higher protein absorption compared to native sCT powders. Conclusion The sCT-CS-NPs with mannitol based spray dried powders were prepared to have appropriate aerodynamic properties for pulmonary delivery. The developed system was able to deliver sCT via a pulmonary route into the systemic circulation. PMID:24039397

Identification of powdered Chinese herbal medicines by fluorescence microscopy, Part 1: Fluorescent characteristics of mechanical tissues, conducting tissues, and ergastic substances.

PubMed

Wang, Ya-Qiong; Liang, Zhi-Tao; Li, Qin; Yang, Hua; Chen, Hu-Biao; Zhao, Zhong-Zhen; Li, Ping

2011-03-01

The light microscope has been successfully used in identification of Chinese herbal medicines (CHMs) for more than a century. However, positive identification is not always possible. Given the popularity of fluorescence microscopy in bioanalysis, researchers dedicated to finding new ways to identify CHMs more effectively are now turning to fluorescence microscopy for authentication purposes. Some studies on distinguishing confused species from the same genus and on exploring distributions of chemicals in tissues of CHMs by fluorescence microscopy have been reported; however, no systematic investigations on fluorescent characteristics of powdered CHMs have been reported. Here, 46 samples of 16 CHMs were investigated. Specifically, the mechanical tissues including stone cells and fibers, the conducting tissues including three types of vessels, and ergastic substances including crystals of calcium oxalate and secretions, in various powdered CHMs were investigated by both light microscope and fluorescence microscope. The results showed many microscopic features emit fluorescence that makes them easily observed, even against complex backgrounds. Under the fluorescence microscope, different microscopic features from the same powdered CHM or some same features from different powdered CHMs emitted the different fluorescence, making this information very helpful for the authentication of CHMs in powder form. Moreover, secretions with unique chemical profiles from different powdered CHMs showed different fluorescent characteristics. Hence, fluorescence microscopy could be a useful additional method for the authentication of powdered CHMs if the fluorescent characteristics of specific CHMs are known. Copyright © 2010 Wiley-Liss, Inc.

Studies on copper-yttria nanocomposites: high-energy ball milling versus chemical reduction method.

PubMed

Joshi, P B; Rehani, Bharati; Naik, Palak; Patel, Swati; Khanna, P K

2012-03-01

Oxide dispersion-strengthened copper-base composites are widely used for applications demanding high tensile strength, high hardness along with good electrical and thermal conductivity. Oxides of metals like aluminium, cerium, yttrium and zirconium are often used for this purpose as fine and uniformly distributed dispersoid particles in soft and ductile copper matrix. Such composites find applications as electrical contacts, resistance-welding tips, lead wires, continuous casting moulds, etc. In this investigation an attempt has been made to produce copper-yttria nanocomposites using two different morphologies of copper powder and two different processing routes namely, high-energy milling and in-situ chemical reduction. The synthesized powders were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM) for their phase identification and morphological study. The nanocomposite powders in each case were subsequently processed to obtain bulk solids by classical powder metallurgy route of press-sinter-repress. The resultant bulk solid compacts were subjected to property evaluation. The study revealed that the properties of Cu-Y2O3 nanocomposites depend on the processing route used and in turn on the resultant powder morphology.

Incorporation of dietary fibre-rich oyster mushroom (Pleurotus sajor-caju) powder improves postprandial glycaemic response by interfering with starch granule structure and starch digestibility of biscuit.

PubMed

Ng, Sze Han; Robert, Sathyasurya Daniel; Wan Ahmad, Wan Amir Nizam; Wan Ishak, Wan Rosli

2017-07-15

The purpose of this study was to determine the effects of Pleurotus sajor-caju (PSC) powder addition at 0, 4, 8 and 12% levels on the nutritional values, pasting properties, thermal characteristics, microstructure, in vitro starch digestibility, in vivo glycaemic index (GI) and sensorial properties of biscuits. Elevated incorporation levels of PSC powder increased the dietary fibre (DF) content and reduced the pasting viscosities and starch gelatinisation enthalpy value of biscuits. The addition of DF-rich PSC powder also interfered with the integrity of the starch granules by reducing the sizes and inducing the uneven spherical shapes of the starch granules, which, in turn, resulted in reduced starch susceptibility to digestive enzymes. The restriction starch hydrolysis rate markedly reduced the GI of biscuits. The incorporation of 8% PSC powder in biscuits (GI=49) could be an effective way of developing a nutritious and low-GI biscuit without jeopardizing its desirable sensorial properties. Copyright © 2017 Elsevier Ltd. All rights reserved.

Optimum carrageenan concentration improved the physical properties of cabinet-dried yoghurt powder

NASA Astrophysics Data System (ADS)

Pratama, Y.; Abduh, S. B. M.; Legowo, A. M.; Pramono, Y. B.; Albaarri, AN

2018-01-01

Carrageenan is a hydrocolloid which able to improve the characteristic of dried powder. The purpose of this study was to produce and evaluate the characteristics of yoghurt powder which incorporated carrageenan as stabilizer and dried in a cabinet dryer. Carrageenan of 1 %, 2 % and 3 % (w/v) concentration were added to yoghurt prior to cabinet drying process. Physical properties of the yoghurt powder and the reconstituted one were evaluated. The best result was shown in carrageenan concentration of 2 % where it showed the highest bulk density (0.62 g/ml), and best particle size distribution (65.49 % in the range of 250-500 μm). Moisture and water activity (aw) were 8.02% and 0.37, respectively. The value is lower than what spoilage microorganisms require to grow (aw > 0.6) thus ensuring its long shelf life when combined with proper packaging. Reconstitution at 50°C showed that 2 % carrageenan resulted in a stable yoghurt product with no visible syneresis even after 3 hours. The proposed method shows promising application in the production of long shelf-life yoghurt powder production.

{sup 45}Sc Solid State NMR studies of the silicides ScTSi (T=Co, Ni, Cu, Ru, Rh, Pd, Ir, Pt)

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

Harmening, Thomas; Eckert, Hellmut, E-mail: eckerth@uni-muenster.de; Fehse, Constanze M.

The silicides ScTSi (T=Fe, Co, Ni, Cu, Ru, Rh, Pd, Ir, Pt) were synthesized by arc-melting and characterized by X-ray powder diffraction. The structures of ScCoSi, ScRuSi, ScPdSi, and ScIrSi were refined from single crystal diffractometer data. These silicides crystallize with the TiNiSi type, space group Pnma. No systematic influences of the {sup 45}Sc isotropic magnetic shift and nuclear electric quadrupolar coupling parameters on various structural distortion parameters calculated from the crystal structure data can be detected. {sup 45}Sc MAS-NMR data suggest systematic trends in the local electronic structure probed by the scandium atoms: both the electric field gradients andmore » the isotropic magnetic shifts relative to a 0.2 M aqueous Sc(NO{sub 3}){sub 3} solution decrease with increasing valence electron concentration and within each T group the isotropic magnetic shift decreases monotonically with increasing atomic number. The {sup 45}Sc nuclear electric quadrupolar coupling constants are generally well reproduced by quantum mechanical electric field gradient calculations using the WIEN2k code. Highlights: Black-Right-Pointing-Pointer Arc-melting synthesis of silicides ScTSi. Black-Right-Pointing-Pointer Single crystal X-ray data of ScCoSi, ScRuSi, ScPdSi, and ScIrSi. Black-Right-Pointing-Pointer {sup 45}Sc solid state NMR of silicides ScTSi.« less

The role of order-disorder transitions in the quest for molecular multiferroics: structural and magnetic neutron studies of a mixed valence iron(II)-iron(III) formate framework.

PubMed

Cañadillas-Delgado, Laura; Fabelo, Oscar; Rodríguez-Velamazán, J Alberto; Lemée-Cailleau, Marie-Hélène; Mason, Sax A; Pardo, Emilio; Lloret, Francesc; Zhao, Jiong-Peng; Bu, Xian-He; Simonet, Virginie; Colin, Claire V; Rodríguez-Carvajal, Juan

2012-12-05

Neutron diffraction studies have been carried out to shed light on the unprecedented order-disorder phase transition (ca. 155 K) observed in the mixed-valence iron(II)-iron(III) formate framework compound [NH(2)(CH(3))(2)](n)[Fe(III)Fe(II)(HCOO)(6)](n). The crystal structure at 220 K was first determined from Laue diffraction data, then a second refinement at 175 K and the crystal structure determination in the low temperature phase at 45 K were done with data from the monochromatic high resolution single crystal diffractometer D19. The 45 K nuclear structure reveals that the phase transition is associated with the order-disorder of the dimethylammonium counterion that is weakly anchored in the cavities of the [Fe(III)Fe(II)(HCOO)(6)](n) framework. In the low-temperature phase, a change in space group from P31c to R3c occurs, involving a tripling of the c-axis due to the ordering of the dimethylammonium counterion. The occurrence of this nuclear phase transition is associated with an electric transition, from paraelectric to antiferroelectric. A combination of powder and single crystal neutron diffraction measurements below the magnetic order transition (ca. 37 K) has been used to determine unequivocally the magnetic structure of this Néel N-Type ferrimagnet, proving that the ferrimagnetic behavior is due to a noncompensation of the different Fe(II) and Fe(III) magnetic moments.

Investigation of Pb doping on electrical, structural and superconducting properties of YBa2-xPbxCu3O7-δ superconductors

NASA Astrophysics Data System (ADS)

Ezzatpour, S.; Sharifzadegan, L.; Sarvari, F.; Sedghi, H.

2018-06-01

In this study the high temperature superconductor YBa2-xPbxCu3O7-δ with doping x = ,0.05,0.1,0.15 were prepared by the standard solid-state reaction method. The effect of Pb substitution on Ba site of YBCO superconducting system, structural, electrical and superconducting properties of Y-based superconductor has been investigated. The measurements of dc resisitivity were performed on all samples with four-probe method using low frequency/lowAC current (4 mA) . The superconducting temperature, Tc, were determined from the resistivity versus temperature (R-T) curves. Results show that Pb doping reduced the cirtical temperature(Tc) and superconductivity properties of our samples. The maximum and the minimum Tc were observed for the samples with x = 0.15 and x = 0.1 respectively. The structure and phase purity of samples were examined by the X-ray powder diffraction technique (XRD) performed by means of D8 Advance Bruker diffractometer with Cu kα radiation. The grain morphology of surface of the samples was analyzed by sacanning electron microscopy (SEM). XRD patterns of polycrystalline materials of composition YBa2-xPbxCu3O7-δ revealed that all prepared samples are orthorhombic. All of the peaks of YBCO and YBa2-xPbxCu3O7-δ have been used for the estimation of volume fractions of the phases and ignored the void peaks.

Development of TiN particulates reinforced SS316 based metal matrix composite by direct metal laser sintering technique and its characterization

NASA Astrophysics Data System (ADS)

Hussain, Manowar; Mandal, Vijay; Kumar, Vikas; Das, A. K.; Ghosh, S. K.

2017-12-01

The present study describes the fabrication of TiN particulates reinforced SS316 based Metal Matrix Composites (MMCs) in nitrogen and argon atmosphere. The influence of sintering process parameters on microstructure, density, porosity, wear rate and microhardness of the fabricated samples has been analyzed. The input variable process parameters, such as, laser power density (range: 4.13-5.57 W/cm2 (× 104)), scanning speed (range: 3500-4500 mm/min) and the constant parameters, such as, laser beam diameter (0.4 mm), hatching distance (0.2 mm) and layer thickness (0.4 mm) have been considered in the process. It has been observed from Field Emission Scanning Electron Microscopy (FESEM) analysis that TiN and SS316 powder mixture can be sintered in which chromium acts as a binder. Fine gaps are not found at the interface between TiN and SS316 when the mixture is sintered in nitrogen atmosphere. With an increase in the percentage of TiN, the density and wear rate decreases. However, when the reinforcement is taken beyond 18% by weight, the wear rate starts increasing. The microhardness also increases with an increase in the percentage of TiN. The microstructure, elemental compositions and phase characterization of the developed sintered MMCs have been examined by FESEM, EDX (Energy-dispersive X-ray spectroscopy) and XRD (X-ray diffractometer) analysis, respectively. The results have demonstrated the suitability of the TiN reinforced SS316 MMCs for industrial applications.

Laser Cladding of Ti-6Al-4V Alloy with Ti-Al2O3 Coating for Biomedical Applications

NASA Astrophysics Data System (ADS)

Mthisi, A.; Popoola, A. P. I.; Adebiyi, D. I.; Popoola, O. M.

2018-05-01

The indispensable properties of Ti-6Al-4V alloy coupled with poor tribological properties and delayed bioactivity make it a subject of interest to explore in biomedical application. A quite number of numerous coatings have been employed on titanium alloys, with aim to overcome the poor properties exhibited by this alloy. In this work, the possibility of laser cladding different ad-mixed powders (Ti - 5 wt.% Al2O3 and Ti - 8wt.% Al2O3) on Ti-6Al-4V at various laser scan speed (0.6 and 0.8 m/min) were investigated. The microstructure, phase constituents and corrosion of the resultant coatings were characterized by scanning electron microscope (SEM), Optical microscope, X-Ray diffractometer (XRD) and potentiostat respectively. The electrochemical behaviour of the produced coatings was studied in a simulated body fluid (Hanks solution). The microstructural results show that a defect free coating is achieved at low scan speed and ad-mixed of Ti-5 wt. % Al2O3. Cladding of Ti - Al2O3 improved the corrosion resistance of Ti-6Al-4V alloy regardless of varying neither scan speed nor ad-mixed percentage. However, Ti-5 wt.% Al2O3 coating produced at low scan speed revealed the highest corrosion resistance among the coatings due to better quality coating layer. Henceforth, this coating may be suitable for biomedical applications.

Neutron Diffraction Studies of Carbonate Apatite

NASA Astrophysics Data System (ADS)

Moghaddam, Hadi Y.; Leventouri, Theodora; Chakoumakos, Bryan C.

1998-11-01

Moghaddam H.Y., Leventouri Th.* (Dept. of Physics & Alloy Research Center, Florida Atlantic Univ.) Chakoumakos B.C. (Solid State Division, Oak Ridge National Lab.**,kou@ornl.gov) We report Rietveld structural refinements of neutron diffraction data of a highly crystalline, single-phase natural carbonate apatite,(francolite of Epirus, Greece), in order to elucidate the details of carbonate substitution in the apatites. The composition is Ca9.56Na0.38Mg0.08(PO4)4.82(CO3)0.946(SO4)0.2F2.34, as determined by electron microprobe analysis. We report refinements of data for the native francolite as a function of temperature between 296K and 10K after the material had been heated at 750 °C to drive off adsorbed water and CO2. The neutron diffractioii@data were collected using a wavelength 1.0912 A on the HB4 high resolution powder diffractometer at the High Flux Isotope Reactor at Oak Ridge National Laboratory. Analysis of the temperature dependence of the anisotropic displacement parameters can reveal the contribution from the temperature independent static positional disorder. Difference displacement parameters evaluated along various bonding directions are being used to describe the mechanics and dynamics of the carbonate for phosphate substitution.*Supported by a SURA-ORNL Summer Cooperative Research Program 1998.**Supported by the Division of Materials Sciences,U.S. D.O.E. (contract DE-AC05-96OR22464 with Lockheed Martin Energy Research Corporation).

Comprehensive analysis of structure and temperature, frequency and concentration-dependent dielectric properties of lithium-substituted cobalt ferrites (Li x Co1- x Fe2O4)

NASA Astrophysics Data System (ADS)

Anjum, Safia; Nisa, Mehru; Sabah, Aneeqa; Rafique, M. S.; Zia, Rehana

2017-08-01

This paper has been dedicated to the synthesis and characterization of a series of lithium-substituted cobalt ferrites Li x Co1- x Fe2O4 ( x = 0, 0.2, 0.4, 0.6, 0.8, 1). These samples have been prepared using simple ball milling machine through powder metallurgy route. The structural analysis is carried out using X-ray diffractometer and their 3D vitalization is simulated using diamond software. The frequency and temperature-dependent dielectric properties of prepared samples have been measured using inductor capacitor resistor (LCR) meter. The structural analysis confirms that all the prepared samples have inverse cubic spinel structure. It is also revealed that the crystallite size and lattice parameter decrease with the increasing concentration of lithium (Li+1) ions, it is due to the smaller ionic radii of lithium ions. The comprehensive analysis of frequency, concentration and temperature-dependent dielectric properties of prepared samples is described in this paper. It is observed that the dielectric constant and tangent loss have decreased and conductivity increased as the frequency increases. It is also revealed that the dielectric constant, tangent loss and AC conductivity increase as the concentration of lithium increases due to its lower electronegativity value. Temperature plays a vital role in enhancing the dielectric constant, tangent loss and AC conductivity because the mobility of ions increases as the temperature increases.

Synthesis of Carbonate-Based Micro/Nanoscale Particles With Controlled Morphology and Mineralogy

DTIC Science & Technology

2013-04-01

patterns were obtained using a Panalytical X’Pert Pro diffractometer using iron-filtered cobalt radiation, and analyzed using Panalytical X’Pert...develop composites by hydrothermal recrystallization of metastable phases. 15. SUBJECT TERMS Aragonite Calcite Calcium carbonate Dopant Mineralogy

Reduction in surgical site infection with suprafascial intrawound application of vancomycin powder in instrumented posterior spinal fusion: a retrospective case-control study.

PubMed

Haimoto, Shoichi; Schär, Ralph T; Nishimura, Yusuke; Hara, Masahito; Wakabayashi, Toshihiko; Ginsberg, Howard J

2018-05-04

OBJECTIVE Recent studies have demonstrated the efficacy of subfascial intrawound application of vancomycin powder in spine surgery in reducing the rate of surgical site infections (SSIs). However, to date no study has evaluated the efficacy and safety of suprafascial application of vancomycin powder in spine surgery. The purpose of this study was to quantify the rate of SSIs after open instrumented posterior spinal fusion with and without application of suprafascial vancomycin powder and to evaluate the rate of vancomycin powder-related local adverse effects. METHODS The authors conducted a single-center retrospective case-control study of adult patients undergoing open instrumented posterior fusion of the cervical, thoracic, or lumbar spine performed by a single surgeon from January 2010 through December 2016. In March 2013, routine application of 1 g of suprafascial vancomycin powder was started for all cases in addition to standard systemic antibiotic prophylaxis. Baseline demographics and operative data as well as the SSI rates were compared between the study groups. The incidence of vancomycin powder-related adverse effects was analyzed. RESULTS A total of 515 patients (268 in the untreated group and 247 in the treated group) were included in the study. The mean age was significantly higher in the treated group than in the untreated group (58.4 vs 54.4 years, p < 0.01). Operative variables were similar between the study groups. Patients receiving vancomycin powder had a significantly lower infection rate (5.6% in the untreated group vs 0% in the treated group, p < 0.001). No vancomycin powder-related adverse effects were identified in the treated group. CONCLUSIONS Routine application of suprafascial intrawound vancomycin powder in addition to systemic antibiotic prophylaxis is an easy-to-use, safe, and effective strategy for preventing SSIs after instrumented posterior spinal fusion. Suprafascial application of vancomycin powder could be a valuable alternative to previously reported subfascial distribution, minimizing the risk of local adverse drug reactions.

Development of a novel dry powder inhalation formulation for the delivery of rivastigmine hydrogen tartrate.

PubMed

Simon, Alice; Amaro, Maria Inês; Cabral, Lucio Mendes; Healy, Anne Marie; de Sousa, Valeria Pereira

2016-03-30

The purpose of this study was to prepare engineered particles of rivastigmine hydrogen tartrate (RHT) and to characterize the physicochemical and aerodynamic properties, in comparison to a lactose carrier formulation (LCF). Microparticles were prepared from ethanol/water solutions containing RHT with and without the incorporation of L-leucine (Leu), using a spray dryer. Dry powder inhaler formulations prepared were characterized by scanning electron microscopy, powder X-ray diffraction, laser diffraction particle sizing, ATR-FTIR, differential scanning calorimetry, bulk and tapped density, dynamic vapour sorption and in vitro aerosol deposition behaviour using a next generation impactor. The smooth-surfaced spherical morphology of the spray dried microparticles was altered by adding Leu, resulting in particles becoming increasingly wrinkled with increasing Leu. Powders presented low densities. The glass transition temperature was sufficiently high (>90 °C) to suggest good stability at room temperature. As Leu content increased, spray dried powders presented lower residual solvent content, lower particle size, higher fine particle fraction (FPF<5 μm), and lower mass median aerodynamic diameter (MMAD). The LCF showed a lower FPF and higher MMAD, relative to the spray dried formulations containing more than 10% Leu. Spray dried RHT powders presented better aerodynamic properties, constituting a potential drug delivery system for oral inhalation. Copyright © 2016. Published by Elsevier B.V.

Hot isostatic pressing (HIP) of powder mixtures and composites: Packing, densification, and microstructural effects

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

Li, E.K.H.; Funkenbusch, P.D.

1993-06-01

Hot isostatic pressing (HIP) of powder mixtures (containing differently sized components) and of composite powders is analyzed. Recent progress, including development of a simple scheme for estimating radial distribution functions, has made modeling of these systems practical. Experimentally, powders containing bimodal or continuous size distributions are observed to hot isostatically press to a higher density tinder identical processing conditions and to show large differences in the densification rate as a function of density when compared with the monosize powders usually assumed for modeling purposes. Modeling correctly predicts these trends and suggests that they can be partially, but not entirely, attributedmore » to initial packing density differences. Modeling also predicts increased deformation in the smaller particles within a mixture. This effect has also been observed experimentally and is associated with microstructural changes, such as preferential recrystallization of small particles. Finally, consolidation of a composite mixture containing hard, but deformable, inclusions has been modeled for comparison with existing experimental data. Modeling results match both the densification and microstructural observations reported experimentally. Densification is retarded due to contacts between the reinforcing particles which support a significant portion of the applied pressure. In addition, partitioning of deformation between soft matrix and hard inclusion powders results in increased deformation of the softer material.« less

Neutron apparatus for measuring strain in composites

DOEpatents

Kupperman, David S.; Majumdar, Saurindranath; Faber, Jr., John F.; Singh, J. P.

1990-01-01

A method and apparatus for orienting a pulsed neutron source and a multi-angle diffractometer toward a sample of a ceramic-matrix or metal-matrix composite so that the measurement of internal strain (from which stress is calculated) is reduced to uncomplicated time-of-flight measurements.

A Neutron Diffractometer for a Long Pulsed Neutron Source

NASA Astrophysics Data System (ADS)

Sokol, Paul; Wang, Cailin

Long pulsed neutron sources are being actively developed as small university based sources and are being considered for the next generation of high powered sources, such as the European Neutron Source (ESS) and the Spallation Neutron Source (SNS) second target station. New instrumentation concepts will be required to effectively utilize the full spectrum of neutrons generated by these sources. Neutron diffractometers, which utilize time-of-flight (TOF) techniques for wavelength resolution, are particularly problematic. We describe an instrument for a long pulsed source that provides resolution comparable to that obtained on short pulsed sources without the need of long incident flight paths. We accomplish this by utilizing high speed choppers to impose a time structure on the spectrum of incident neutrons. By strategically positioning these choppers the response matrix assumes a convenient form that can be deconvoluted from the measured TOF spectrum to produce the diffraction pattern of the sample. We compare the performance of this instrument to other possible diffraction instruments that could be utilized on a long pulsed source.

Modeling of the focusing device and the elliptical neutron guide for the DN-6 diffractometer at IBR-2 reactor

NASA Astrophysics Data System (ADS)

Belushkin, A. V.; Manoshin, S. A.; Kozlenko, D. P.; Kichanov, S. E.

2018-06-01

Possible options for modernization of the neutron beam forming system of the DN-6 diffractometer for the study of crystal and magnetic structures of microsamples at high pressures are being considered. It was demonstrated that for samples with the cross-section not exceeding 5 × 5 mm2 the most efficient option would be the use of an elliptical neutron guide. It allows to deliver neutrons for large distances from the source to samples with minimal losses using, as a rule, just one neutron reflection per dimension i.e. one at a side and one at top or bottom. For the present moment due to technical difficulties of such option realization, the simplified solution was proposed. At the end of the curved neutron guide it is planned to install a vertical plane focusing 7-meter-long parabolic section. Such a modernization will increase the neutron flux at the sample by a factor 1.5-3.5 and reduce respectively the typical measurement times.

Development of a cryogenic load frame for the neutron diffractometer at Takumi in Japan Proton Accelerator Research Complex

NASA Astrophysics Data System (ADS)

Jin, Xinzhe; Nakamoto, Tatsushi; Harjo, Stefanus; Hemmi, Tsutomu; Umeno, Takahiro; Ogitsu, Toru; Yamamoto, Akira; Sugano, Michinaka; Aizawa, Kazuya; Abe, Jun; Gong, Wu; Iwahashi, Takaaki

2013-06-01

To prepare for projects such as the Large Hadron Collider upgrade, International Thermonuclear Experimental Reactor and Demonstration reactor, it is important to form a clear understanding of stress-strain properties of the materials that make up superconducting magnets. Thus, we have been studying the mechanical properties of superconducting wires using neutron diffraction measurements. To simulate operational conditions such as temperature, stress, and strain, we developed a cryogenic load frame for stress-strain measurements of materials using a neutron diffractometer at Japan Proton Accelerator Research Complex (J-PARC) Takumi beam line. The maximum load that can be applied to a sample using an external driving machine is 50 kN. Using a Gifford-MacMahon cryocooler, samples can be measured down to temperatures below 10 K when loaded. In the present paper, we describe the details of the cryogenic load frame with its test results by using type-304 stainless steel wire.

A 4 Tesla Superconducting Magnet Developed for a 6 Circle Huber Diffractometer at the XMaS Beamline

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

Thompson, P. B. J.; Brown, S. D.; Bouchenoire, L.

2007-01-19

We report here on the development and testing of a 4 Tesla cryogen free superconducting magnet designed to fit within the Euler cradle of a 6 circle Huber diffractometer, allowing scattering in both the vertical and horizontal planes. The geometry of this magnet allows the field to be applied in three orientations. The first being along the beam direction, the second with the field transverse to the beam direction a horizontal plane and finally the field can be applied vertically with respect to the beam. The magnet has a warm bore and an open geometry of 180 deg. , allowingmore » large access to reciprocal space. A variable temperature insert has been developed, which is capable of working down to a temperature of 1.7 K and operating over a wide range of angles whilst maintaining a temperature stability of a few mK. Initial ferromagnetic diffraction measurements have been carried out on single crystal Tb and Dy samples.« less

Hippo/crates-in-situ deformation strain and testure studies using neutron time-of-flight diffraction.

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

Vogel, S. C.; Hartig, C.; Brissier, T. D.

2005-01-01

In situ deformation studies by diffraction allow studying of deformation mechanisms and provide valuable data to validate and improve deformation models. In particular, deformation studies using time-of-flight neutrons provide averages over large numbers of grains and allow to probing the response of lattice planes parallel and perpendicular to the applied load simultaneously. In this paper we describe the load-frame CRATES, designed for the HIPPO neutron time-of-flight diffractometer at LANSCE. The HIPPO/CRATES combination allows probing up to 20 diffraction vectors simultaneously and provides rotation of the sample in the beam while under load. With this, deformation texture, i.e. the change ofmore » grain orientation due to plastic deformation, or strain pole figures may be measured. We report initial results of a validation experiment, comparing deformation of a Zircaloy specimen measured using the NPD neutron diffractometer with results obtained for the same material using HIPPO/CRATES.« less

A furnace with rotating load frame for in situ high temperature deformation and creep experiments in a neutron diffraction beam line

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

Reiche, H. M.; New Mexico State University, Las Cruces, New Mexico 88003; Vogel, S. C.

2012-05-15

A resistive furnace combined with a load frame was built that allows for in situ neutron diffraction studies of high temperature deformation, in particular, creep. A maximum force of 2700 N can be applied at temperatures up to 1000 deg. C. A load control mode permits studies of, e.g., creep or phase transformations under applied uni-axial stress. In position control, a range of high temperature deformation experiments can be achieved. The examined specimen can be rotated up to 80 deg. around the vertical compression axis allowing texture measurements in the neutron time-of-flight diffractometer HIPPO (High Pressure - Preferred Orientation). Wemore » present results from the successful commissioning, deforming a Zr-2.5 wt.% Nb cylinder at 975 deg. C. The device is now available for the user program of the HIPPO diffractometer at the LANSCE (Los Alamos Neutron Science Center) user facility.« less

Development of a cryogenic load frame for the neutron diffractometer at Takumi in Japan Proton Accelerator Research Complex

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

Jin, Xinzhe; Nakamoto, Tatsushi; Ogitsu, Toru

2013-06-15

To prepare for projects such as the Large Hadron Collider upgrade, International Thermonuclear Experimental Reactor and Demonstration reactor, it is important to form a clear understanding of stress-strain properties of the materials that make up superconducting magnets. Thus, we have been studying the mechanical properties of superconducting wires using neutron diffraction measurements. To simulate operational conditions such as temperature, stress, and strain, we developed a cryogenic load frame for stress-strain measurements of materials using a neutron diffractometer at Japan Proton Accelerator Research Complex (J-PARC) Takumi beam line. The maximum load that can be applied to a sample using an externalmore » driving machine is 50 kN. Using a Gifford-MacMahon cryocooler, samples can be measured down to temperatures below 10 K when loaded. In the present paper, we describe the details of the cryogenic load frame with its test results by using type-304 stainless steel wire.« less

Development of a cryogenic load frame for the neutron diffractometer at Takumi in Japan Proton Accelerator Research Complex.

PubMed

Jin, Xinzhe; Nakamoto, Tatsushi; Harjo, Stefanus; Hemmi, Tsutomu; Umeno, Takahiro; Ogitsu, Toru; Yamamoto, Akira; Sugano, Michinaka; Aizawa, Kazuya; Abe, Jun; Gong, Wu; Iwahashi, Takaaki

2013-06-01

To prepare for projects such as the Large Hadron Collider upgrade, International Thermonuclear Experimental Reactor and Demonstration reactor, it is important to form a clear understanding of stress-strain properties of the materials that make up superconducting magnets. Thus, we have been studying the mechanical properties of superconducting wires using neutron diffraction measurements. To simulate operational conditions such as temperature, stress, and strain, we developed a cryogenic load frame for stress-strain measurements of materials using a neutron diffractometer at Japan Proton Accelerator Research Complex (J-PARC) Takumi beam line. The maximum load that can be applied to a sample using an external driving machine is 50 kN. Using a Gifford-MacMahon cryocooler, samples can be measured down to temperatures below 10 K when loaded. In the present paper, we describe the details of the cryogenic load frame with its test results by using type-304 stainless steel wire.

Pharmacokinetics and Histopathological Findings of Chemoembolization Using Cisplatin Powder Mixed with Degradable Starch Microspheres in a Rabbit Liver Tumor Model

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

Sato, Takeshi; Tanaka, Toshihiro, E-mail: toshihir@bf6.so-net.ne.jp; Nishiofuku, Hideyuki

PurposeThe purpose of this study is to evaluate the pharmacokinetics and histopathological findings of transarterial chemoembolization (TACE) using cisplatin powder mixed with degradable starch microspheres (DSM) (Cis/DSM-TACE) compared with cisplatin arterial infusion (Cis-AI).Materials and MethodsEighteen rabbits with VX2 liver tumors were divided into two groups: Cis/DSM-TACE (n = 9) and Cis-AI (n = 9) groups. In the Cis/DSM-TACE group, a mixture of cisplatin powder and DSM was injected until stasis of hepatic arterial flow was achieved. In the Cis-AI group, cisplatin solution was infused.ResultsThe platinum concentrations in VX2 tumors in the Cis/DSM-TACE group at 24 and 72 h were significantly elevated compared with those inmore » the Cis-AI group (P = .016 and .019, respectively). There were no significant differences in the platinum concentrations in plasma. Histopathological examination revealed the presence of several microspheres inside the tumors at 1 h, which completely disappeared at 24 h. Tumor cell apoptosis at 1 h in the Cis/DSM-TACE group was more frequently observed compared with that in the Cis-AI group (P = .006).ConclusionsTACE using cisplatin powder mixed with DSM provides a higher drug concentration in tumors, thereby achieving stronger antitumor effects compared with arterial infusion of cisplatin solution.« less

Comparison of soymilk, powdered milk, Hank's balanced salt solution and tap water on periodontal ligament cell survival.

PubMed

Moazami, Fariborz; Mirhadi, Hosein; Geramizadeh, Bita; Sahebi, Safoura

2012-04-01

The purpose of this study was to evaluate the ability of soymilk, powdered milk, and Hank's balanced salt solution (HBSS) to maintain human periodontal ligament (PDL) cell viability in vitro. PDL cells were obtained from extracted healthy third molars and cultured in Dulbecco's modified Eagles medium (DMEM). The cultures were exposed for 1, 2, 4, and 8 h to experimental solutions (tap water served as negative control and DMEM as positive control) at 37°C. The viable cells were then counted using the trypan blue exclusion technique. Data were analyzed by using one-way anova, post hoc Scheffe and two-way anova test. Statistical analysis showed that HBSS, powdered baby formula, and soymilk maintain cell viability equally well in different periods of times. Tap water cannot keep cells viable as well as other solutions. Soymilk and powdered baby formula can be recommended as suitable storage media for avulsed teeth for up to 8 h. © 2011 John Wiley & Sons A/S.

Design, characterization, and aerosol dispersion performance modeling of advanced spray-dried microparticulate/nanoparticulate mannitol powders for targeted pulmonary delivery as dry powder inhalers.

PubMed

Li, Xiaojian; Vogt, Frederick G; Hayes, Don; Mansour, Heidi M

2014-04-01

The purpose was to design and characterize inhalable microparticulate/nanoparticulate dry powders of mannitol with essential particle properties for targeted dry powder delivery for cystic fibrosis mucolytic treatment by dilute organic solution spray drying, and, in addition, to tailor and correlate aerosol dispersion performance delivered as dry powder inhalers based on spray-drying conditions and solid-state physicochemical properties. Organic solution advanced spray drying from dilute solution followed by comprehensive solid-state physicochemical characterization and in vitro dry powder aerosolization were used. The particle size distribution of the spray-dried (SD) powders was narrow, unimodal, and in the range of ∼500 nm to 2.0 μm. The particles possessed spherical particle morphology, relatively smooth surface morphology, low water content and vapor sorption (crystallization occurred at exposure above 65% relative humidity), and retention of crystallinity by polymorphic interconversion. The emitted dose, fine particle fraction (FPF), and respirable fraction (RF) were all relatively high. The mass median aerodynamic diameters were below 4 μm for all SD mannitol aerosols. The in vitro aerosol deposition stage patterns could be tailored based on spray-drying pump rate. Positive linear correlation was observed between both FPF and RF values with spray-drying pump rates. The interplay between various spray-drying conditions, particle physicochemical properties, and aerosol dispersion performance was observed and examined, which enabled tailoring and modeling of high aerosol deposition patterns.

Indium doped ZnO nano-powders prepared by RF thermal plasma treatment of In2O3 and ZnO

NASA Astrophysics Data System (ADS)

Lee, Mi-Yeon; Song, Min-Kyung; Seo, Jun-Ho; Kim, Min-Ho

2015-06-01

Indium doped ZnO nano-powders were synthesized by the RF thermal plasma treatment of In2O3 and ZnO. For this purpose, micron-sized ZnO powder was mixed with In2O3 powder at the In/Zn ratios of 0.0, 1.2, and 2.4 at. % by ball milling for 1 h, after which the mixtures were injected into RF thermal plasma generated at the plate power level of ˜140 kV A. As observed from the field emission scanning electron microscopy (FE-SEM) images of the RF plasma-treated powders, hexagonal prism-shaped nano-crystals were mainly obtained along with multi-pod type nano-particles, where the number of multi-pods decreased with increasing In/Zn ratios. In addition, the X-ray diffraction (XRD) data for the as-treated nano-powders showed the diffraction peaks for the In2O3 present in the precursor mixture to disappear, while the crystalline peaks for the single phase of ZnO structure shifted toward lower Bragg angles. In the UV-vis absorption spectra of the as-treated powders, redshifts were also observed with increases of the In/Zn ratios. Together with the FE-SEM images and the XRD data, the redshifts were indicative of the doping process of ZnO with indium, which took place during the RF thermal plasma treatment of In2O3 and ZnO.

Design, Characterization, and Aerosol Dispersion Performance Modeling of Advanced Spray-Dried Microparticulate/Nanoparticulate Mannitol Powders for Targeted Pulmonary Delivery as Dry Powder Inhalers

PubMed Central

Li, Xiaojian; Vogt, Frederick G.; Hayes, Don

2014-01-01

Abstract Background: The purpose was to design and characterize inhalable microparticulate/nanoparticulate dry powders of mannitol with essential particle properties for targeted dry powder delivery for cystic fibrosis mucolytic treatment by dilute organic solution spray drying, and, in addition, to tailor and correlate aerosol dispersion performance delivered as dry powder inhalers based on spray-drying conditions and solid-state physicochemical properties. Methods: Organic solution advanced spray drying from dilute solution followed by comprehensive solid-state physicochemical characterization and in vitro dry powder aerosolization were used. Results: The particle size distribution of the spray-dried (SD) powders was narrow, unimodal, and in the range of ∼500 nm to 2.0 μm. The particles possessed spherical particle morphology, relatively smooth surface morphology, low water content and vapor sorption (crystallization occurred at exposure above 65% relative humidity), and retention of crystallinity by polymorphic interconversion. The emitted dose, fine particle fraction (FPF), and respirable fraction (RF) were all relatively high. The mass median aerodynamic diameters were below 4 μm for all SD mannitol aerosols. Conclusion: The in vitro aerosol deposition stage patterns could be tailored based on spray-drying pump rate. Positive linear correlation was observed between both FPF and RF values with spray-drying pump rates. The interplay between various spray-drying conditions, particle physicochemical properties, and aerosol dispersion performance was observed and examined, which enabled tailoring and modeling of high aerosol deposition patterns. PMID:24502451

Effect of heat treatment on phase composition and crystal structure of thin WSi2 films on silicon substrates

NASA Astrophysics Data System (ADS)

Biryukov, Y. P.; Dostanko, A. P.; Maltsev, A. A.; Shakhlevich, G. M.

1984-10-01

An experimental study of WSi2 films on silicon substrates with either 111 or 100 orientation was made, for the purpose of determining the effect of annealing by heat treatment on their phase composition and crystal structure. Films of 0.2 micron thickness were deposited at a rate of 0.5 nm/s on a silicon surface which was predecontaminated of SiO2 layers and adsorbate atoms by ion sputtering in one vacuum cycle. Deposition was by condensation, with the substrate held at various temperatures from 390 to 500 C, and then annealed in an argon atmosphere at various temperatures from 700 to 1000 C for 30 min. Subsequent phase analysis at room temperature was performed with a DRON-2 X-ray diffractometer, using a CuK (sub alpha)-radiation source and covering the 20 = 10 to 130 deg range of angles by the Debye-Sherer method, while the surface morphology was examined under an electron microscope.

Multiple diffraction in an icosahedral Al-Cu-Fe quasicrystal

NASA Astrophysics Data System (ADS)

Fan, C. Z.; Weber, Th.; Deloudi, S.; Steurer, W.

2011-07-01

In order to reveal its influence on quasicrystal structure analysis, multiple diffraction (MD) effects in an icosahedral Al-Cu-Fe quasicrystal have been investigated in-house on an Oxford Diffraction four-circle diffractometer equipped with an Onyx™ CCD area detector and MoKα radiation. For that purpose, an automated approach for Renninger scans (ψ-scans) has been developed. Two weak reflections were chosen as the main reflections (called P) in the present measurements. As is well known for periodic crystals, it is also observed for this quasicrystal that the intensity of the main reflection may significantly increase if the simultaneous (H) and the coupling (P-H) reflections are both strong, while there is no obvious MD effect if one of them is weak. The occurrence of MD events during ψ-scans has been studied based on an ideal structure model and the kinematical MD theory. The reliability of the approach is revealed by the good agreement between simulation and experiment. It shows that the multiple diffraction effect is quite significant.

Powder-Collection System for Ultrasonic/Sonic Drill/Corer

NASA Technical Reports Server (NTRS)

Sherrit, Stewart; Bar-Cohen, Yoseph; Bao, Xiaoqi; Chang, Zensheu; Blake, David; Bryson, Charles

2005-01-01

A system for collecting samples of powdered rock has been devised for use in conjunction with an ultrasonic/sonic drill/corer (USDC) -- a lightweight, lowpower apparatus designed to cut into, and acquire samples of, rock or other hard material for scientific analysis. The USDC includes a drill bit, corer, or other tool bit, in which ultrasonic and sonic vibrations are excited by an electronically driven piezoelectric actuator. The USDC advances into the rock or other material of interest by means of a hammering action and a resulting chiseling action at the tip of the tool bit. The hammering and chiseling actions are so effective that unlike in conventional twist drilling, a negligible amount of axial force is needed to make the USDC advance into the material. Also unlike a conventional twist drill, the USDC operates without need for torsional restraint, lubricant, or a sharp bit. The USDC generates powder as a byproduct of the drilling or coring process. The purpose served by the present samplecollection system is to remove the powder from the tool-bit/rock interface and deliver the powder to one or more designated location(s) for analysis or storage

Real-time powder diffraction studies of energy materials under non-equilibrium conditions

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

Peterson, Vanessa K.; Auckett, Josie E.; Pang, Wei-Kong

Energy materials form the central part of energy devices. An essential part of their function is the ability to reversibly host charge or energy carriers, and analysis of their phase composition and structure in real time under non-equilibrium conditions is mandatory for a full understanding of their atomic-scale functional mechanism. Real-time powder diffraction is increasingly being applied for this purpose, forming a critical step in the strategic chemical engineering of materials with improved behaviour. This topical review gives examples of real-time analysis using powder diffraction of rechargeable battery electrodes and porous sorbent materials used for the separation and storage ofmore » energy-relevant gases to demonstrate advances in the insights which can be gained into their atomic-scale function.« less

Real-time powder diffraction studies of energy materials under non-equilibrium conditions

PubMed Central

Peterson, Vanessa K.; Auckett, Josie E.; Pang, Wei-Kong

2017-01-01

Energy materials form the central part of energy devices. An essential part of their function is the ability to reversibly host charge or energy carriers, and analysis of their phase composition and structure in real time under non-equilibrium conditions is mandatory for a full understanding of their atomic-scale functional mechanism. Real-time powder diffraction is increasingly being applied for this purpose, forming a critical step in the strategic chemical engineering of materials with improved behaviour. This topical review gives examples of real-time analysis using powder diffraction of rechargeable battery electrodes and porous sorbent materials used for the separation and storage of energy-relevant gases to demonstrate advances in the insights which can be gained into their atomic-scale function. PMID:28989711

Crystallization behavior of polyamide-6 microcellular nanocomposites

Treesearch

Mingjun Yuan; Lih-Sheng Turng; Shaoqin Gong; Andreas Winardi

2004-09-01

The crystallization behaviors of polyamide-6 (PA-6) and its nanocomposites undergoing the microcellular injection molding process are studied using Transmission Electron Microscopy (TEM), X-ray Diffractometer (XRD), Polarized Optical Microscopy (POM), and Differential Scanning Calorimetry (DSC). The relationships among the morphology, the mechanical property of the...

Misuse of Topical Corticosteroids for Cosmetic Purpose in Antananarivo, Madagascar

PubMed Central

Ranaivo, I. M.; Andrianarison, M.; Razanakoto, N. H.; Ramarozatovo, L. S.

2017-01-01

This cross-sectional study was conducted in Antananarivo, Madagascar, from June to September 2012. We aim to evaluate the misuse of TC on the face for cosmetic purpose and the adverse effects due to its application. A questionnaire-based analysis was done among females who use topical corticosteroids on the face for cosmetic purpose. Of the 770 women questioned, 384 (49,8%) used topical corticosteroids for cosmetic purpose whose mean age was 38 years (range 16–73 years). Two hundred and sixty-one females (68%) used TC combined with handcrafted cosmetics, and 123 (32%) used TC alone. “Pandalao,” which contains salicylic acid, peppermint oil, lanolin, powder of Juanes de Vigo (mercury powder), and Vaseline, is the most handcrafted cosmetic combined with TC in our study (used by 29,4% respondents). Only one (0,26%) had obtained the TC by physician's prescription, 234 (61%) from cosmetic retailers, 92 (23%) directly from local pharmacies, 49 (12%) from beauticians, and 15 (4%) from unspecified sources. Lightening of skin color was the main reason for using TC in 44,8% of respondents in the absence of any primary dermatosis. Pigmentation disorders (63,2%) and cutaneous atrophy (52,1%) were the most adverse effects noted. PMID:28904977

Misuse of Topical Corticosteroids for Cosmetic Purpose in Antananarivo, Madagascar.

PubMed

Sendrasoa, F A; Ranaivo, I M; Andrianarison, M; Raharolahy, O; Razanakoto, N H; Ramarozatovo, L S; Rapelanoro Rabenja, F

2017-01-01

This cross-sectional study was conducted in Antananarivo, Madagascar, from June to September 2012. We aim to evaluate the misuse of TC on the face for cosmetic purpose and the adverse effects due to its application. A questionnaire-based analysis was done among females who use topical corticosteroids on the face for cosmetic purpose. Of the 770 women questioned, 384 (49,8%) used topical corticosteroids for cosmetic purpose whose mean age was 38 years (range 16-73 years). Two hundred and sixty-one females (68%) used TC combined with handcrafted cosmetics, and 123 (32%) used TC alone. "Pandalao," which contains salicylic acid, peppermint oil, lanolin, powder of Juanes de Vigo (mercury powder), and Vaseline, is the most handcrafted cosmetic combined with TC in our study (used by 29,4% respondents). Only one (0,26%) had obtained the TC by physician's prescription, 234 (61%) from cosmetic retailers, 92 (23%) directly from local pharmacies, 49 (12%) from beauticians, and 15 (4%) from unspecified sources. Lightening of skin color was the main reason for using TC in 44,8% of respondents in the absence of any primary dermatosis. Pigmentation disorders (63,2%) and cutaneous atrophy (52,1%) were the most adverse effects noted.

Production of inhalation phage powders using spray freeze drying and spray drying techniques for treatment of respiratory infections

PubMed Central

Leung, Sharon S.Y.; Parumasivam, Thaigarajan; Gao, Fiona G.; Carrigy, Nicholas B.; Vehring, Reinhard; Finlay, Warren H.; Morales, Sandra; Britton, Warwick J; Kutter, Elizabeth; Chan, Hak-Kim

2016-01-01

Purpose The potential of aerosol phage therapy for treating lung infections has been demonstrated in animal models and clinical studies. This work compared the performance of two dry powder formation techniques, spray freeze drying (SFD) and spray drying (SD), in producing inhalable phage powders. Method A Pseudomonas podoviridae phage, PEV2, was incorporated into multi-component formulation systems consisting of trehalose, mannitol and L-leucine (F1 = 60:20:20 and F2 = 40:40:20). The phage titer loss after the SFD and SD processes and in vitro aerosol performance of the produced powders were assessed. Results A significant titer loss (~ 2 log) was noted for droplet generation using an ultrasonic nozzle employed in the SFD method, but the conventional two-fluid nozzle used in the SD method was less destructive for the phage (~0.75 log loss). The phage were more vulnerable during the evaporative drying process (~0.75 log further loss) compared with the freeze drying step, which caused negligible phage loss. In vitro aerosol performance showed that the SFD powders (~80% phage recovery) provided better phage protection than the SD powders (~20% phage recovery) during the aerosolization process. Despite this, higher total lung doses were obtained for the SD formulations (SD-F1 = 13.1 ± 1.7 × 104 pfu and SD-F2 = 11.0 ± 1.4 × 104 pfu) than from their counterpart SFD formulations (SFD-F1 = 8.3 ± 1.8 × 104 pfu and SFD-F2 = 2.1 ± 0.3 × 104 pfu). Conclusion Overall, the SD method caused less phage reduction during the powder formation process and the resulted powders achieved better aerosol performance for PEV2. PMID:26928668

Wound infection prophylaxis in pediatric acute appendicitis: a 26-year prospective study.

PubMed

Ein, Sigmund H; Sandler, Anthony

2006-03-01

The purpose of this study was to determine the best wound infection prophylaxis in pediatric acute appendicitis. From 1969 to 1995 inclusive, 453 consecutive pediatric patients at the same children's hospital had an appendix with acute inflammation (acute appendicitis) removed by the same staff surgeon and his resident. The stump was not inverted, and chromic catgut was used throughout. No intraperitoneal antibiotics, irrigation, or drains were used, and the skin closure was with silk sutures initially and then with staples since 1986. The infants and children were divided into 6 consecutive groups of 52 to 96 patients, with each group lasting 2 to 5 years. The wound treatment groups were as follows: no treatment, drain or pack, drain or pack plus antibiotic powder, antibiotic powder, preoperative intravenous antibiotic plus antibiotic powder, and preoperative intravenous antibiotic. The wound Penrose drain, one half-inch gauze pack, and/or antibiotic powder (ampicillin, 1977-1981; cefoxitin, 1982-1995) were all placed in the subcutaneous space. There were a total of 50 (11%) wound infections (pus) that occurred between 4 and 40 days when no antibiotic powder was used and 2 to 14 days with antibiotic powder. In all 6 groups of patients, no organism was grown in most (80%) infections and Escherichia coli was the second commonest (12%). The serous ooze, which occurred only with the use of antibiotic powder (8%), was seen between 6 and 18 days, and no organism was ever cultured. The patients with preoperative (or intraoperative) intravenous antibiotics (cefoxitin) plus wound antibiotic powder (cefoxitin) had the lowest infection rate (2.5%). When this group was compared with the baseline group 1 (no treatment), it was the only group in which wound treatment made a significant difference (P = .003).

Fabrication of individual alginate-TCP scaffolds for bone tissue engineering by means of powder printing.

PubMed

Castilho, Miguel; Rodrigues, Jorge; Pires, Inês; Gouveia, Barbara; Pereira, Manuel; Moseke, Claus; Groll, Jürgen; Ewald, Andrea; Vorndran, Elke

2015-01-06

The development of polymer-calcium phosphate composite scaffolds with tailored architectures and properties has great potential for bone regeneration. Herein, we aimed to improve the functional performance of brittle ceramic scaffolds by developing a promising biopolymer-ceramic network. For this purpose, two strategies, namely, direct printing of a powder composition consisting of a 60:40 mixture of α/β-tricalcium phosphate (TCP) powder and alginate powder or vacuum infiltration of printed TCP scaffolds with an alginate solution, were tracked. Results of structural characterization revealed that the scaffolds printed with 2.5 wt% alginate-modified TCP powders presented a uniformly distributed and interfusing alginate TCP network. Mechanical results indicated a significant increase in strength, energy to failure and reliability of powder-modified scaffolds with an alginate content in the educts of 2.5 wt% when compared to pure TCP, as well as to TCP scaffolds containing 5 wt% or 7.5 wt% in the educts, in both dry and wet states. Culture of human osteoblast cells on these scaffolds also demonstrated a great improvement of cell proliferation and cell viability. While in the case of powder-mixed alginate TCP scaffolds, isolated alginate gels were formed between the calcium phosphate crystals, the vacuum-infiltration strategy resulted in the covering of the surface and internal pores of the TCP scaffold with a thin alginate film. Furthermore, the prediction of the scaffolds' critical fracture conditions under more complex stress states by the applied Mohr fracture criterion confirmed the potential of the powder-modified scaffolds with 2.5 wt% alginate in the educts as structural biomaterial for bone tissue engineering.

Microwave Diffraction Techniques from Macroscopic Crystal Models

ERIC Educational Resources Information Center

Murray, William Henry

1974-01-01

Discusses the construction of a diffractometer table and four microwave models which are built of styrofoam balls with implanted metallic reflecting spheres and designed to simulate the structures of carbon (graphite structure), sodium chloride, tin oxide, and palladium oxide. Included are samples of Bragg patterns and computer-analysis results.…

GeoSoilEnviroCARS: A National User Facility for Synchrotron Radiation Research

NASA Astrophysics Data System (ADS)

Rivers, M. L.; Sutton, S. R.

2002-12-01

GeoSoilEnviroCARS (GSECARS) is a national user facility for frontier research in the earth sciences using synchrotron radiation at the Advanced Photon Source, Argonne National Laboratory. GSECARS provides earth scientists with access to the high-brilliance hard x-rays from this third-generation synchrotron light source. Both an undulator and a bending magnet beamline are available. All principal synchrotron-based analytical techniques in demand by earth scientists are being brought to bear on earth science problems: (1) high-pressure/high-temperature crystallography and spectroscopy using the diamond anvil cell; (2) high-pressure/high-temperature crystallography using the large-volume press; (3) powder, single crystal and interface diffraction; (4) inelastic x-ray scattering; (5) x-ray absorption fine structure (XAFS) spectroscopy; (6) x-ray fluorescence microprobe analysis; and (7) microtomography. The major instrumentation includes 250 and 1000 MN multianvil presses, a double-sided laser heating system, a large general-purpose 5-circle diffractometer, a focused microprobe, and a Raman laboratory. A proposal-based system for beamtime allocation, open to all earth scientists, has been in place since Fall, 1998. Since then, over 450 beamtime proposals have been received and more than 320 outside users have conducted experiments at GSECARS. The research conducted by these investigators has resulted in more than 170 publications. The unique capabilities of the APS and GSECARS have allowed groundbreaking experiments to be conducted. These include: (1) phase transformations in the Mg-Si-O system at mantle conditions; (2) structure of hydrated a-Al2O3 surfaces; (3) alloying properties of silicon in the Earth's core; (4) dynamics of iron-rich melt segregation from silicates during core formation; (5) electronic spin state of FeO at high pressure and temperature; (6) elastic wave velocities of mantle minerals at lower mantle conditions; (7) copper partitioning and speciation in natural hydrothermal fluids; and (8) mechanisms of arsenic sequestration at a Superfund site. The GSECARS mission is to provide a research environment where users receive expert assistance in planning and conducting experiments, and in analyzing data. The facility operation is funded by the NSF EAR Instrumentation and Facilities program and the DOE Geosciences program. Major instrumentation was also provided by the W.M. Keck Foundation. Information and applications for beam time can be found at http://gsecars.org.

The crystal structure of paramagnetic copper(II) oxalate (CuC₂O₄): formation and thermal decomposition of randomly stacked anisotropic nano-sized crystallites.

PubMed

Christensen, Axel Nørlund; Lebech, Bente; Andersen, Niels Hessel; Grivel, Jean-Claude

2014-11-28

Synthetic copper(II) oxalate, CuC2O4, was obtained in a precipitation reaction between a copper(II) solution and an aqueous solution of oxalic acid. The product was identified from its conventional X-ray powder patterns which match that of the copper mineral Moolooite reported to have the composition CuC2O4·0.44H2O. Time resolved in situ investigations of the thermal decomposition of copper(II) oxalate using synchrotron X-ray powder diffraction showed that in air the compound converts to Cu2O at 215 °C and oxidizes to CuO at 345 °C. Thermo gravimetric analysis performed in an inert Ar-gas reveals that the material contains no crystal water and reduces to pure Cu at 295 °C. Magnetic susceptibility measurements in the temperature range from 2 K to 300 K show intriguing paramagnetic behaviour with no sign of magnetic order down to 2 K. A crystal structure investigation is made based on powder diffraction data using one neutron diffraction pattern obtained at 5 K (λ = 1.5949(1) Å) combined with one conventional and two synchrotron X-ray diffraction patterns obtained at ambient temperature using λ = 1.54056, 1.0981 and λ = 0.50483(1) Å, respectively. Based on the X-ray synchrotron data the resulting crystal structure is described in the monoclinic space group P2₁/c (#14) in the P12₁/n1 setting with unit cell parameters a = 5.9598(1) Å, b = 5.6089(1) Å, c = 5.1138 (1) Å, β = 115.320(1)°. The composition is CuC2O4 with atomic coordinates determined by FullProf refinement of the neutron diffraction data. The crystal structure consists of a random stacking of CuC2O4 micro-crystallites where half the Cu-atoms are placed at (2a) and the other half at (2b) positions with the corresponding oxalate molecules centred around the corresponding (2b) and (2a) site positions, respectively. The diffraction patterns obtained for both kinds of radiation show considerable broadening of several Bragg peaks caused by highly anisotropic microstructural size and strain effects. In contrast to the water reported to be present in Moolooite, neither thermogravimetric nor the in situ thermal decomposition investigations and crystal structure analysis of the neutron diffraction data revealed any trace of water. An appendix contains details about the profile parameters for the diffractometers used at the European Synchrotron Radiation Facility and the Institute Max von Laue-Paul Langevin.

Raman-spectroscopy-based chemical contaminant detection in milk powder

NASA Astrophysics Data System (ADS)

Dhakal, Sagar; Chao, Kuanglin; Qin, Jianwei; Kim, Moon S.

2015-05-01

Addition of edible and inedible chemical contaminants in food powders for purposes of economic benefit has become a recurring trend. In recent years, severe health issues have been reported due to consumption of food powders contaminated with chemical substances. This study examines the effect of spatial resolution used during spectral collection to select the optimal spatial resolution for detecting melamine in milk powder. Sample depth of 2mm, laser intensity of 200mw, and exposure time of 0.1s were previously determined as optimal experimental parameters for Raman imaging. Spatial resolution of 0.25mm was determined as the optimal resolution for acquiring spectral signal of melamine particles from a milk-melamine mixture sample. Using the optimal resolution of 0.25mm, sample depth of 2mm and laser intensity of 200mw obtained from previous study, spectral signal from 5 different concentration of milk-melamine mixture (1%, 0.5%, 0.1%, 0.05%, and 0.025%) were acquired to study the relationship between number of detected melamine pixels and corresponding sample concentration. The result shows that melamine concentration has a linear relation with detected number of melamine pixels with correlation coefficient of 0.99. It can be concluded that the quantitative analysis of powder mixture is dependent on many factors including physical characteristics of mixture, experimental parameters, and sample depth. The results obtained in this study are promising. We plan to apply the result obtained from this study to develop quantitative detection model for rapid screening of melamine in milk powder. This methodology can also be used for detection of other chemical contaminants in milk powders.

Production of salbutamol sulfate for inhalation by high-gravity controlled antisolvent precipitation.

PubMed

Chiou, Herbert; Li, Li; Hu, Tingting; Chan, Hak-Kim; Chen, Jian-Feng; Yun, Jimmy

2007-02-22

The purpose of this study was to produce salbutamol sulfate (SS) as a model anti-asthmatic drug using high-gravity controlled precipitation (HGCP) through antisolvent crystallisation. An aqueous solution of SS was passed through a HGCP reactor with isopropanol as antisolvent to induce precipitation. Spray drying was employed to obtain dry powders. Scanning electron microscopy, X-ray powder diffraction (XRD), density measurement, thermal gravimetric analysis, and dynamic vapour sorption were carried out to characterise the powder physical properties. The aerosol performance of the powders was measured using an Aeroliser connected to a multiple stage liquid impinger operating at 60 L/min. The HGCP SS particles were elongated with 0.1 microm in width but varying length of several mum, which formed spherical agglomerates when spray dried. The particles showed the same XRD pattern and true density (1.3g/cm3) as the raw material, indicating that they belonged to the same crystalline form. However, the spray dried agglomerates had a much lower tapped density (0.1g/cm3) than the raw material (0.6g/cm3). Compared with the powder obtained by spray drying directly from an aqueous solution, the SS powders obtained from HGCP were much less hygroscopic (0.6% versus 10% water uptake at 90% RH). The in vitro aerosol performance showed a fine particle fraction FPFloaded and FPFemitted up to 54.5+/-4.9% and 71.3+/-10.0%, respectively. In conclusion, SS powder with suitable physical and aerosol properties can be obtained through antisolvent HGCP followed by spray drying.

Structural, optical, and magnetic properties of Cu- and Ni-codoped CdO dilute magnetic nanocrystalline semiconductor: effect of hydrogen post-treatment

NASA Astrophysics Data System (ADS)

Dakhel, A. A.; Bououdina, M.

2015-06-01

Cadmium oxide codoped with Cu and Ni ions powders was synthesised by thermal co-decomposition of a mixture of cadmium, copper, and nickel acetylacetonates. The mass ratio of Cu/Cd was fixed, while the Ni/Cd mass ratio was varied systematically. The purpose of the present study is to prepare powders having room-temperature ferromagnetic (RT-FM) properties. X-ray fluorescence (XRF) and X-ray diffraction (XRD) confirm the purity and the formation of single nanocrystalline structure of the as-prepared powders. The energy bandgap of the as-prepared powders was found to vary slightly and then increases by 3.96-38.02 % after post-H2-treatment. Magnetic measurements reveal that all as-prepared doped CdO powders gained partial (RT-FM) properties. Furthermore, the created RT-FM is dependent on the Ni% doping level. After annealing under H2 gas, a strong enhancement of RT-FM was observed, especially for 1.2 % Ni-doping-level powder where the whole powder became ferromagnetic with coercivity, remanence, and saturation magnetisation of 249.2 Oe, 4.52 memu/g, and 14.57 memu/g, respectively, representing an increase by ~241.3, 1062, and 1700 %, respectively, in comparison with the as-prepared sample. Thus, it was proved, for the first time, the possibility of producing of codoped CdO with RT-FM, where the magnetic characteristics can be tailored by doping and post-treatment under H2 atmosphere, thus a new potential candidate for dilute magnetic semiconductor (DMS).

Evaluation of effects of geometrical parameters on density distribution in compaction of PM gears

NASA Astrophysics Data System (ADS)

Khodaee, Alireza; Melander, Arne

2017-10-01

The usage of powder metallurgy (PM) for manufacturing of transmission components in automotive industries has been studied by many researchers. PM components have become of interest in recent years due to advancements in post processing possibilities such as hot isostatic pressing (HIP). Still in many of the forming process routes for making components from PM materials, the compaction of the powder into green component is the first step. Compaction is required to put the powder into the near net shape of the desired component and it causes a density gradient in the body of the green component. Basically the friction between powder particles and between the powder particles and die walls are the well-known roots for such density gradients in the compacted component. Looking at forming of PM gears, the gradient in density is one of the most important roots of problems in the processing of PM gears as well. That is because making a gear with full density and no pores will be very costly if large density gradients exist in the green component. The purpose of this study is to find the possible relations between the gear geometry and the density gradients in the green component after compaction in addition to the friction effects. For this purpose several gears should be tested. To reduce the research costs, the finite element (FE) method is used. First a FE model of the compaction process is developed and verified. To investigate the relations between the density gradients and the gear parameters such as addendum diameter (da) and the face width (b) several gear geometries have been studied. The compaction of selected gears is simulated using the FE model. The simulations results which are the distribution of density in the green component are evaluated and discussed and conclusion are made based on them.

The use of functionalized monoalkyl phosphates and phosphonates in the colloidal processing of oxide ceramic powders

NASA Astrophysics Data System (ADS)

Radsick, Timothy Carl

The purpose of this study was to develop phosphorous-based chemicals that could be used to modify the interparticle pair potential of several oxide ceramic particles, thereby enabling their use in colloidal processing schemes. Several procedures for the synthesis of 11-12 carbon alpha,o-functionalized monoalkyl phosphates and phosphonates were developed. Because of its simplicity and its use of mild reagents, a procedure based on the Michaelis-Arbuzov rearrangement was selected to produce the bulk of the chemicals used in this study. Carboxyl- and hydroxyl-terminated monoalkyl phosphonates were adsorbed onto alumina and zirconia powders using either aqueous-based or solvent-based methods to produce a monolayer of "brushlike" steric molecules. In the aqueous-based methods, powders were processed at pH values below their isoelectric point in order to produce a positive charge on the powder, thereby attracting the negatively charged phosphate or phosphonate group onto the powder surface to form the steric monolayer. In solvent-based methods, powder was suspended in an acetone solution of the phosphonates, heated at reflux, washed, dried and heat treated at 120°C under vacuum. The zeta potential of the coated powders was measured to quantify the degree of steric layer adsorption and the shift in the isoelectric point. Slurries of coated alumina and zirconia were prepared having 20 vol % powder. Rheological behavior was studied by measuring viscosity as a function of shear rate for slurries of various pH values and counterion concentrations. Slurries with powder processed via the solvent method were the least sensitive to changes in slurry pH and were straightforward to prepare. It is thought that the solvent-based coating procedure produced a stronger, multi-dentate powder-phosphonate bond than that of the aqueous-based procedure. Dispersed and coagulated slurries were able to be prepared over a wide pH range, including at the isoelectric point of the uncoated powders where a flocculated slurry would typically occur. Slurries were consolidated using pressure filtration. Compressive stress-strain behavior and packing efficiencies were determined. Through consolidation, powder volume fraction was increased to a maximum of 56%, yet through vibration the slurry could be induced to flow, enabling its use in Colloidal Isopressing.

Size dependent structural and magnetic properties of Al substituted Co–Mg ferrites synthesized by the sol–gel auto-combustion method

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

Ahmad, Imran, E-mail: imraan77@yahoo.com; Abbas, Tahir; Ziya, A.B.

2014-04-01

Highlights: • Well-crystalline Co{sub 0.7}Mg{sub 0.3}AlFeO{sub 4} nanoparticles with small grain size were obtained. • The approach is sol–gel auto-combustion technique for obtained nanoparticles. • The prepared Co{sub 0.7}Mg{sub 0.3}AlFeO{sub 4} ferrites are decent soft materials with low coercivity. • The minor decrease in lattice parameter with increase of temperature was observed. - Abstract: Single phased nanocrystalline Co{sub 0.7}Mg{sub 0.3}FeAlO{sub 4} ferrites having low coercivity were synthesized by the sol–gel auto-combustion route. The subsequent powder materials were sintered in a temperature range of 800–1200 °C for 2 h. The effects of sintering temperatures on the structure, morphology and magnetic propertiesmore » of the prepared soft magnetic material were studied. X-ray diffractometer (XRD), scanning electron microscope (SEM), transmission electron microscope (TEM), and magnetic property measurement system (MPMS) were used to characterize the samples. X-ray diffraction analysis confirmed a single-phase cubic spinel structure and ruled out the presence of impurities like hematite. The higher sintering temperatures have caused in enhanced mark of crystallinity and bigger average grain size of the nanocrystals. A slight decrease in lattice parameters was noticed with a rise of grain size. Magnetic measurements revealed that grain size increase led to a decrease in the coercivity and, in difference, an increase in the saturation magnetization.« less

Electrochemical properties of rapidly solidified Si-Ti-Ni(-Cu) base anode for Li-ion rechargeable batteries

NASA Astrophysics Data System (ADS)

Kwon, Hye Jin; Sohn, Keun Yong; Park, Won-Wook

2013-11-01

In this study, rapidly solidified Si-Ti-Ni-Cu alloys have been investigated as high capacity anodes for Li-ion secondary batteries. To obtain nano-sized Si particles dispersed in the inactive matrix, the alloy ribbons were fabricated using the melt spinning process. The thin ribbons were pulverized using ball-milling to make a fine powder of ˜ 4 µm average size. Coin-cell assembly was carried out under an argon gas in a glove box, in which pure lithium was used as a counter-electrode. The cells were cycled using the galvanostatic method in the potential range of 0.01 V and 1.5 V vs. Li/Li+. The microstructure and morphology were examined using an x-ray diffractometer, Field-Emission Scanning Electron Microscopy and High Resolution Transmission Electron Microscopy. Among the anode alloys, the Si70Ti15Ni15 electrodes had the highest discharge capacity (974.1 mAh/g) after the 50th cycle, and the Si60Ti16Ni16Cu8 electrode showed the best coulombic efficiency of ˜95.9% in cyclic behavior. It was revealed that the Si7Ni4Ti4 crystal phase coexisting with an amorphous phase, could more efficiently act as a buffer layer than the fully crystallized Si7Ni4Ti4 phase. Consequently, the electrochemical properties of the anode materials pronouncedly improved when the nano-sized primary Si particle was dispersed in the inactive Si7Ni4Ti4-based matrix mixed with an amorphous structure.

Operational performance characteristics of the WISH detector array on the ISIS spallation neutron source

NASA Astrophysics Data System (ADS)

Duxbury, D.; Khalyavin, D.; Manuel, P.; Raspino, D.; Rhodes, N.; Schooneveld, E.; Spill, E.

2014-12-01

The performance of the position sensitive neutron detector array of the WISH diffractometer is discussed. WISH (Wide angle In a Single Histogram) is one of the seven instruments currently available for users on the second target station (TS2) of the ISIS spallation neutron source, and is used mainly for magnetic studies of materials. WISH is instrumented with an array of 10 detector panels, covering an angular range of 320o, orientated in two semi-cylindrical annuli around a central sample position at a radius of 2.2m. In total the 10 detector panels are composed of 1520 3He based position sensitive detector tubes. Each tube has an active length of one metre, a diameter of 8mm and is filled with 3He at 15 bar. The specification for the WISH detectors included a neutron detection efficiency of 50% at a neutron wavelength of 1Å with good gamma rejection. A position resolution better than 8 mm FWHM along the length of the tubes was also required which has been met experimentally. Results obtained from the detector arrays showing pulse height and positional information both prior to and post installation are shown. The first 5 of the 10 detector panels have been operational since 2009, and comparable diffraction data from powder and single crystal samples taken from the remaining 5 panels (installation completed in 2013) shows that we have a detector array with a highly stable performance which is easily assembled and maintained. Finally some real user data is shown, highlighting the excellent quality of data attainable with this instrument.

Experiments on planetary ices at UCL

NASA Astrophysics Data System (ADS)

Grindrod, P. M.; Fortes, A. D.; Wood, I. G.; Dobson, D.; Sammonds, P. R.; Stone-Drake, L.; Vocadlo, L.

2007-08-01

Using a suite of techniques and equipment, we conduct several different types of experiments on planetary ices at UCL. Samples are prepared in the Ice Physics Laboratory, which consists of a 5 chamber complex of inter-connected cold rooms, controllable from +30 to -30 deg C. Within this laboratory we have a functioning triaxial deformation cell operating at low temperature (down to -90 deg C) and high pressures (300 MPa), an Automatic Ice Fabric Analyser (AIFA) and a low-temperature microscope with CCD output. Polycrystalline samples, 40mm diameter by 100mm long, are compressed in the triaxial rig with a confining pressure; single crystal specimens are compressed in a separate uniaxial creep rig which operates at zero confining pressure for surface studies. A cold stage is also available for study of ice microstructural studies on our new Jeol JSM-6480LV SEM, which also allows tensile, compression and/or bending tests, with load ranges from less than 2N to 5000N. Finally, we also use a cold stage on a new PANalytical, X'pert PRO MPD, high resolution powder diffractometer to study the structure and phase behaviour of icy materials. Recent highlights of our work include: (1) derivation of a manufacturing process for methane clathrate at low temperatures, analysed in the X-Ray Diffraction Laboratory, for future rheological experiments, (2) analysed the growth behaviour of MS11, (3) refurbished and commenced calibration tests on the triaxial deformation cell using ice Ih, and (4) performed creep tests on gypsum and epsomite using the single crystal deformation cell. Further experiments will build on these preliminary results.

A critical Examination of the Phenomenon of Bonding Area - Bonding Strength Interplay in Powder Tableting.

PubMed

Osei-Yeboah, Frederick; Chang, Shao-Yu; Sun, Changquan Calvin

2016-05-01

Although the bonding area (BA) and bonding strength (BS) interplay is used to explain complex tableting behaviors, it has never been experimentally proven. The purpose of this study is to unambiguously establish the distinct contributions of each by decoupling the contributions from BA and BS. To modulate BA, a Soluplus® powder was compressed into tablets at different temperatures and then broken following equilibration at 25°C. To modulate BS, tablets were equilibrated at different temperatures. To simultaneously modulate BA and BS, both powder compression and tablet breaking test were carried out at different temperatures. Lower tablet tensile strength is observed when the powder is compressed at a lower temperature but broken at 25°C. This is consistent with the increased resistance to polymer deformation at lower temperatures. When equilibrated at different temperatures, the tensile strength of tablets prepared under identical conditions increases with decreasing storage temperature, indicating that BS is higher at a lower temperature. When powder compression and tablet breaking are carried out at the same temperature, the profile with a maximum tensile strength at 4°C is observed due to the BA-BS interplay. By systematically varying temperature during tablet compression and breaking, we have experimentally demonstrated the phenomenon of BA-BS interplay in tableting.

Dust Explosion Characteristics of Aluminum, Titanium, Zinc, and Iron-Based Alloy Powders Used in Cold Spray Processing

NASA Astrophysics Data System (ADS)

Sakata, K.; Tagomori, K.; Sugiyama, N.; Sasaki, S.; Shinya, Y.; Nanbu, T.; Kawashita, Y.; Narita, I.; Kuwatori, K.; Ikeda, T.; Hara, R.; Miyahara, H.

2014-01-01

Compared to conventional thermal spray coating, cold spray processing typically employs finer, smaller-diameter metal powders. Furthermore, cold-sprayed particles exhibit fewer surface oxides than thermally sprayed particles due to the absence of particle melting during spraying. For these reasons, it is important to consider the potential for dust explosions or fires during cold spray processing, for both industrial and R&D applications. This work examined the dust explosion characteristics of metal powders typically used in cold spray coating, for the purpose of preventing dust explosions and fires and thus protecting the health and safety of workers and guarding against property damage. In order to safely make use of the new cold spray technology in industrial settings, it is necessary to manage the risks based on an appropriate assessment of the hazards. However, there have been few research reports focused on such risk management. Therefore, in this study, the dust explosion characteristics of aluminum, titanium, zinc, carbonyl iron, and eutectoid steel containing chromium at 4 wt.% (4 wt.% Cr-eutectoid steel) powders were evaluated according to the standard protocols JIS Z 8818, IEC61241-2-3(1994-09) section 3, and JIS Z 8817. This paper reports our results concerning the dust explosion properties of the above-mentioned metal powders.

A comparison between two powder compaction parameters of plasticity: the effective medium A parameter and the Heckel 1/K parameter.

PubMed

Mahmoodi, Foad; Klevan, Ingvild; Nordström, Josefina; Alderborn, Göran; Frenning, Göran

2013-09-10

The purpose of the research was to introduce a procedure to derive a powder compression parameter (EM A) representing particle yield stress using an effective medium equation and to compare the EM A parameter with the Heckel compression parameter (1/K). 16 pharmaceutical powders, including drugs and excipients, were compressed in a materials testing instrument and powder compression profiles were derived using the EM and Heckel equations. The compression profiles thus obtained could be sub-divided into regions among which one region was approximately linear and from this region, the compression parameters EM A and 1/K were calculated. A linear relationship between the EM A parameter and the 1/K parameter was obtained with a strong correlation. The slope of the plot was close to 1 (0.84) and the intercept of the plot was small in comparison to the range of parameter values obtained. The relationship between the theoretical EM A parameter and the 1/K parameter supports the interpretation of the empirical Heckel parameter as being a measure of yield stress. It is concluded that the combination of Heckel and EM equations represents a suitable procedure to derive a value of particle plasticity from powder compression data. Copyright © 2013 Elsevier B.V. All rights reserved.

Compressibility of binary powder formulations: investigation and evaluation with compaction equations.

PubMed

Gentis, Nicolaos D; Betz, Gabriele

2012-02-01

The purpose of this work was to investigate and evaluate the powder compressibility of binary mixtures containing a well-compressible compound (microcrystalline cellulose) and a brittle active drug (paracetamol and mefenamic acid) and its progression after a drug load increase. Drug concentration range was 0%-100% (m/m) with 10% intervals. The powder formulations were compacted to several relative densities with the Zwick material tester. The compaction force and tensile strength were fitted to several mathematical models that give representative factors for the powder compressibility. The factors k and C (Heckel and modified Heckel equation) showed mostly a nonlinear correlation with increasing drug load. The biggest drop in both factors occurred at far regions and drug load ranges. This outcome is crucial because in binary mixtures the drug load regions with higher changeover of plotted factors could be a hint for an existing percolation threshold. The susceptibility value (Leuenberger equation) showed varying values for each formulation without the expected trend of decrease for higher drug loads. The outcomes of this study showed the main challenges for good formulation design. Thus, we conclude that such mathematical plots are mandatory for a scientific evaluation and prediction of the powder compaction process. Copyright © 2011 Wiley Periodicals, Inc.

Three-Arm Randomized Phase III Trial: Quality Aloe and Placebo Cream Versus Powder as Skin Treatment During Breast Cancer Radiation Therapy.

PubMed

Hoopfer, Donna; Holloway, Caroline; Gabos, Zsolt; Alidrisi, Maha; Chafe, Susan; Krause, Barbara; Lees, Alan; Mehta, Nirmal; Tankel, Keith; Strickland, Faith; Hanson, John; King, Charlotte; Ghosh, Sunita; Severin, Diane

2015-06-01

The efficacy of aloe extract in reducing radiation-induced skin injury is controversial. The purpose of the present 3-arm randomized trial was to test the efficacy of quality-tested aloe extract in reducing the severity of radiation-induced skin injury and, secondarily, to examine the effect of a moist cream versus a dry powder skin care regimen. A total of 248 patients with breast cancer were randomized to powder, aloe cream, or placebo cream. Acute skin toxicity was scored weekly and after treatment at weeks 1, 2, and 4 using a modified 10-point Catterall scale. The patients scored their symptom severity using a 6-point Likert scale and kept an acute phase diary. The aloe formulation did not reduce acute skin toxicity or symptom severity. Patients with a greater body mass index were more likely to develop acute skin toxicity. A similar pattern of increased skin reaction toxicity occurred with both study creams compared with the dry powder regimen. No evidence was found to support prophylactic application of quality aloe extract or cream to improve the symptoms or reduce the skin reaction severity. Our results support a dry skin care regimen of powder during radiation therapy. Copyright © 2015 Elsevier Inc. All rights reserved.

Continuous powder feeding for pharmaceutical solid dosage form manufacture: a short review.

PubMed

Blackshields, Caroline A; Crean, Abina M

2018-07-01

There has been a noticeable shift from pharmaceutical batch processing towards a more continuous mode of manufacture for solid oral dosage forms. Continuous solid oral dose processes would not be possible in the absence of a highly accurate feeding system. The performance of feeders defines the content of formulations and is therefore a critical operation in continuous manufacturing of solid dosage forms. It was the purpose of this review to review the role of the initial powder feeding step in a continuous manufacturing process. Different feeding mechanisms are discussed with a particular emphasis on screw controlled loss in weight (LIW) feeding. The importance of understanding the physical properties of the raw materials and its impact on the feeding process is reviewed. Prior knowledge of materials provides an initial indication of how the powders will behave through processing and facilitates in the selection of the most suitable (i) feeder (capacity), (ii) feeding mechanism, and (iii) in the case of screw feeder - screw type. The studies identified in this review focus on the impact of material on powder feeding performance.

A large dataset of synthetic SEM images of powder materials and their ground truth 3D structures.

PubMed

DeCost, Brian L; Holm, Elizabeth A

2016-12-01

This data article presents a data set comprised of 2048 synthetic scanning electron microscope (SEM) images of powder materials and descriptions of the corresponding 3D structures that they represent. These images were created using open source rendering software, and the generating scripts are included with the data set. Eight particle size distributions are represented with 256 independent images from each. The particle size distributions are relatively similar to each other, so that the dataset offers a useful benchmark to assess the fidelity of image analysis techniques. The characteristics of the PSDs and the resulting images are described and analyzed in more detail in the research article "Characterizing powder materials using keypoint-based computer vision methods" (B.L. DeCost, E.A. Holm, 2016) [1]. These data are freely available in a Mendeley Data archive "A large dataset of synthetic SEM images of powder materials and their ground truth 3D structures" (B.L. DeCost, E.A. Holm, 2016) located at http://dx.doi.org/10.17632/tj4syyj9mr.1[2] for any academic, educational, or research purposes.

Experiment to Determine the Absorption Coefficient of Gamma Rays as a Function of Energy.

ERIC Educational Resources Information Center

Ouseph, P. J.; And Others

1982-01-01

Simpler than x-ray diffractometer experiments, the experiment described illustrates certain concepts regarding the interaction of electromagnetic rays with matter such as the exponential decrease in the intensity with absorber thickness, variation of the coefficient of absorption with energy, and the effect of the K-absorption edge on the…

Numerical Simulation for Heat and Mass Transfer During Selective Laser Melting of Titanium alloys Powder

NASA Astrophysics Data System (ADS)

Li, Cheng-Jui; Tsai, Tsung-Wen; Tseng, Chien-Chou

The purpose of this research is to analyse the complex phase change and the heat transfer behavior of the Ti-6Al-4 V powder particle during the Selective Laser Melting (SLM) process. In this study, the rapid melting and solidification process is presented by Computational Fluid Dynamics (CFD) approach under the framework of the volume-of-fluid (VOF) method. The interaction between the laser velocity and power to the solidification shape and defects of the metal components will be studied numerically as a guideline to improve quality and reduce costs.

In situ surface/interface x-ray diffractometer for oxide molecular beam epitaxy

NASA Astrophysics Data System (ADS)

Lee, J. H.; Tung, I. C.; Chang, S.-H.; Bhattacharya, A.; Fong, D. D.; Freeland, J. W.; Hong, Hawoong

2016-01-01

In situ studies of oxide molecular beam epitaxy by synchrotron x-ray scattering has been made possible by upgrading an existing UHV/molecular beam epitaxy (MBE) six-circle diffractometer system. For oxide MBE growth, pure ozone delivery to the chamber has been made available, and several new deposition sources have been made available on a new 12 in. CF (ConFlat, a registered trademark of Varian, Inc.) flange. X-ray diffraction has been used as a major probe for film growth and structures for the system. In the original design, electron diffraction was intended for the secondary diagnostics available without the necessity of the x-ray and located at separate positions. Deposition of films was made possible at the two diagnostic positions. And, the aiming of the evaporation sources is fixed to the point between two locations. Ozone can be supplied through two separate nozzles for each location. Also two separate thickness monitors are installed. Additional features of the equipment are also presented together with the data taken during typical oxide film growth to illustrate the depth of information available via in situ x-ray techniques.

In situ surface/interface x-ray diffractometer for oxide molecular beam epitaxy.

PubMed

Lee, J H; Tung, I C; Chang, S-H; Bhattacharya, A; Fong, D D; Freeland, J W; Hong, Hawoong

2016-01-01

In situ studies of oxide molecular beam epitaxy by synchrotron x-ray scattering has been made possible by upgrading an existing UHV/molecular beam epitaxy (MBE) six-circle diffractometer system. For oxide MBE growth, pure ozone delivery to the chamber has been made available, and several new deposition sources have been made available on a new 12 in. CF (ConFlat, a registered trademark of Varian, Inc.) flange. X-ray diffraction has been used as a major probe for film growth and structures for the system. In the original design, electron diffraction was intended for the secondary diagnostics available without the necessity of the x-ray and located at separate positions. Deposition of films was made possible at the two diagnostic positions. And, the aiming of the evaporation sources is fixed to the point between two locations. Ozone can be supplied through two separate nozzles for each location. Also two separate thickness monitors are installed. Additional features of the equipment are also presented together with the data taken during typical oxide film growth to illustrate the depth of information available via in situ x-ray techniques.

A preliminary neutron crystallographic study of thaumatin

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

Teixeira, Susana C. M.; Institut Laue Langevin, 6 Rue Jules Horowitz, 38042 Grenoble; EPSAM and ISTM, Keele University, Staffordshire ST5 5BG

2008-05-01

Preliminary neutron crystallographic data from the sweet protein thaumatin have been recorded using the LADI-III diffractometer at the Institut Laue Langevin (ILL). The results illustrate the feasibility of a full neutron structural analysis aimed at further understanding the molecular basis of the perception of sweet taste. Such an analysis will exploit the use of perdeuterated thaumatin. A preliminary neutron crystallographic study of the sweet protein thaumatin is presented. Large hydrogenated crystals were prepared in deuterated crystallization buffer using the gel-acupuncture method. Data were collected to a resolution of 2 Å on the LADI-III diffractometer at the Institut Laue Langevin (ILL).more » The results demonstrate the feasibility of a full neutron crystallographic analysis of this structure aimed at providing relevant information on the location of H atoms, the distribution of charge on the protein surface and localized water in the structure. This information will be of interest for understanding the specificity of thaumatin–receptor interactions and will contribute to further understanding of the molecular mechanisms underlying the perception of taste.« less

Precession technique and electron diffractometry as new tools for crystal structure analysis and chemical bonding determination.

PubMed

Avilov, A; Kuligin, K; Nicolopoulos, S; Nickolskiy, M; Boulahya, K; Portillo, J; Lepeshov, G; Sobolev, B; Collette, J P; Martin, N; Robins, A C; Fischione, P

2007-01-01

We have developed a new fast electron diffractometer working with high dynamic range and linearity for crystal structure determinations. Electron diffraction (ED) patterns can be scanned serially in front of a Faraday cage detector; the total measurement time for several hundred ED reflections can be tens of seconds having high statistical accuracy for all measured intensities (1-2%). This new tool can be installed to any type of TEM without any column modification and is linked to a specially developed electron beam precession "Spinning Star" system. Precession of the electron beam (Vincent-Midgley technique) reduces dynamical effects allowing also use of accurate intensities for crystal structure analysis. We describe the technical characteristics of this new tool together with the first experimental results. Accurate measurement of electron diffraction intensities by electron diffractometer opens new possibilities not only for revealing unknown structures, but also for electrostatic potential determination and chemical bonding investigation. As an example, we present detailed atomic bonding information of CaF(2) as revealed for the first time by precise electron diffractometry.

Towards the optimisation and adaptation of dry powder inhalers.

PubMed

Cui, Y; Schmalfuß, S; Zellnitz, S; Sommerfeld, M; Urbanetz, N

2014-08-15

Pulmonary drug delivery by dry powder inhalers is becoming more and more popular. Such an inhalation device must insure that during the inhalation process the drug powder is detached from the carrier due to fluid flow stresses. The goal of the project is the development of a drug powder detachment model to be used in numerical computations (CFD, computational fluid dynamics) of fluid flow and carrier particle motion through the inhaler and the resulting efficiency of drug delivery. This programme will be the basis for the optimisation of inhaler geometry and dry powder inhaler formulation. For this purpose a multi-scale approach is adopted. First the flow field through the inhaler is numerically calculated with OpenFOAM(®) and the flow stresses experienced by the carrier particles are recorded. This information is used for micro-scale simulations using the Lattice-Boltzmann method where only one carrier particle covered with drug powder is placed in cubic flow domain and exposed to the relevant flow situations, e.g. plug and shear flow with different Reynolds numbers. Therefrom the fluid forces on the drug particles are obtained. In order to allow the determination of the drug particle detachment possibility by lift-off, sliding or rolling, also measurements by AFM (atomic force microscope) were conducted for different carrier particle surface structures. The contact properties, such as van der Waals force, friction coefficient and adhesion surface energy were used to determine, from a force or moment balance (fluid forces versus contact forces), the detachment probability by the three mechanisms as a function of carrier particle Reynolds number. These results will be used for deriving the drug powder detachment model. Copyright © 2014 Elsevier B.V. All rights reserved.

Induced wettability and surface-volume correlation of composition for bovine bone derived hydroxyapatite particles

NASA Astrophysics Data System (ADS)

Maidaniuc, Andreea; Miculescu, Florin; Voicu, Stefan Ioan; Andronescu, Corina; Miculescu, Marian; Matei, Ecaterina; Mocanu, Aura Catalina; Pencea, Ion; Csaki, Ioana; Machedon-Pisu, Teodor; Ciocan, Lucian Toma

2018-04-01

Hydroxyapatite powders characteristics need to be determined both for quality control purposes and for a proper control of microstructural features of bone reconstruction products. This study combines bulk morphological and compositional analysis methods (XRF, SEM-EDS, FT-IR) with surface-related methods (XPS, contact angle measurements) in order to correlate the characteristics of hydroxyapatite powders derived from bovine bone for its use in medical applications. An experimental approach for correlating the surface and volume composition was designed based on the analysis depth of each spectral method involved in the study. Next, the influences of powder particle size and forming method on the contact angle between water drops and ceramic surface were evaluated for identifying suitable strategies of tuning hydroxyapatite's wettability. The results revealed a preferential arrangement of chemical elements at the surface of hydroxyapatite particles which could induce a favourable material behaviour in terms of sinterability and biological performance.

Analysis of Pelletizing of Granulometric Separation Powder from Cork Industries

PubMed Central

Montero, Irene; Miranda, Teresa; Sepúlveda, Francisco José; Arranz, José Ignacio; Nogales, Sergio

2014-01-01

Cork industries generate a considerable amount of solid waste during their processing. Its management implies a problem for companies that should reconsider its reuse for other purposes. In this work, an analysis of pelletizing of granulometric separation powder, which is one of the major wastes in cork industries and which presents suitable properties (as an raw material) for its thermal use, is studied. However, its characteristic heterogeneity, along with its low bulk density (which makes its storage and transportation difficult) are restrictive factors for its energy use. Therefore, its densified form is a real alternative in order to make the product uniform and guarantee its proper use in boiler systems. Thus, the cork pellets (from granulometric separation powder) in the study met, except for ash content specification, the specifications in standard European Norm EN-Plus (B) for its application as fuel for domestic use. PMID:28788207

Analysis of Pelletizing of Granulometric Separation Powder from Cork Industries.

PubMed

Montero, Irene; Miranda, Teresa; Sepúlveda, Francisco José; Arranz, José Ignacio; Nogales, Sergio

2014-09-18

Cork industries generate a considerable amount of solid waste during their processing. Its management implies a problem for companies that should reconsider its reuse for other purposes. In this work, an analysis of pelletizing of granulometric separation powder, which is one of the major wastes in cork industries and which presents suitable properties (as an raw material) for its thermal use, is studied. However, its characteristic heterogeneity, along with its low bulk density (which makes its storage and transportation difficult) are restrictive factors for its energy use. Therefore, its densified form is a real alternative in order to make the product uniform and guarantee its proper use in boiler systems. Thus, the cork pellets (from granulometric separation powder) in the study met, except for ash content specification, the specifications in standard European Norm EN-Plus (B) for its application as fuel for domestic use.

Synthesis of Nano-Crystalline Gamma-TiAl Materials

NASA Technical Reports Server (NTRS)

Hales, Stephen J.; Vasquez, Peter

2003-01-01

One of the principal problems with nano-crystalline materials is producing them in quantities and sizes large enough for valid mechanical property evaluation. The purpose of this study was to explore an innovative method for producing nano-crystalline gamma-TiAl bulk materials using high energy ball milling and brief secondary processes. Nano-crystalline powder feedstock was produced using a Fritsch P4(TM) vario-planetary ball mill recently installed at NASA-LaRC. The high energy ball milling process employed tungsten carbide tooling (vials and balls) and no process control agents to minimize contamination. In a collaborative effort, two approaches were investigated, namely mechanical alloying of elemental powders and attrition milling of pre-alloyed powders. The objective was to subsequently use RF plasma spray deposition and short cycle vacuum hot pressing in order to effect consolidation while retaining nano-crystalline structure in bulk material. Results and discussion of the work performed to date are presented.

Modified Antifreeze Liquids for Use on Surfaces

NASA Technical Reports Server (NTRS)

Lynn, R. O.

1983-01-01

Report presents results of evaluation of two antifreeze liquids, dimethyl sulfoxide and ethylene glycol and five viscosity modifiers: gelatin, gum tragacanth, starch, agarose powder and citrus pectin. Purpose of evaluation to find best way of dealing with frost formation on Space Shuttle.

The CheMin XRD on the Mars Science Laboratory Rover Curiosity: Construction, Operation, and Quantitative Mineralogical Results from the Surface of Mars

NASA Technical Reports Server (NTRS)

Blake, David F.

2015-01-01

The Mars Science Laboratory mission was launched from Cape Canaveral, Florida on Nov. 26, 2011 and landed in Gale crater, Mars on Aug. 6, 2012. MSL's mission is to identify and characterize ancient "habitable" environments on Mars. MSL's precision landing system placed the Curiosity rover within 2 km of the center of its 20 X 6 km landing ellipse, next to Gale's central mound, a 5,000 meter high pile of laminated sediment which may contain 1 billion years of Mars history. Curiosity carries with it a full suite of analytical instruments, including the CheMin X-ray diffractometer, the first XRD flown in space. CheMin is essentially a transmission X-ray pinhole camera. A fine-focus Co source and collimator transmits a 50µm beam through a powdered sample held between X-ray transparent plastic windows. The sample holder is shaken by a piezoelectric actuator such that the powder flows like a liquid, each grain passing in random orientation through the beam over time. Forward-diffracted and fluoresced X-ray photons from the sample are detected by an X-ray sensitive Charge Coupled Device (CCD) operated in single photon counting mode. When operated in this way, both the x,y position and the energy of each photon are detected. The resulting energy-selected Co Kalpha Debye-Scherrer pattern is used to determine the identities and amounts of minerals present via Rietveld refinement, and a histogram of all X-ray events constitutes an X-ray fluorescence analysis of the sample.The key role that definitive mineralogy plays in understanding the Martian surface is a consequence of the fact that minerals are thermodynamic phases, having known and specific ranges of temperature, pressure and composition within which they are stable. More than simple compositional analysis, definitive mineralogical analysis can provide information about pressure/temperature conditions of formation, past climate, water activity and the like. Definitive mineralogical analyses are necessary to establish the origin or provenance of a sample. The search for evidence of extant or extinct life on Mars will initially be a search for evidence of present or past conditions supportive of life (e.g., evidence of water), not for life itself.Results of the first 1,000 sols (Mars days) will be discussed, including the discovery of the first habitable environment on Mars.

Electronic Properties and Device Applications of III-V Compound Semiconductor Native Oxides

DTIC Science & Technology

2006-03-02

MRD X-ray diffractometer with CuKa as the radiation source. The doping level in GaAs was meassured by electrochemical voltage (ECV) using an Accent... hard to prevent the gate metal from overlapping the mesa edge thus creating a parasitic leakage path to the channel42. To reduce the gate leakage

Investigation of thermal spray coatings on austenitic stainless steel substrate to enhance corrosion protection

NASA Astrophysics Data System (ADS)

Rogers, Daniel M.

The research is aimed to evaluate thermal spray coatings to address material issues in supercritical and ultra-supercritical Rankine cycles. The primary purpose of the research is to test, evaluate, and eventually implement a coating to improve corrosion resistance and increase efficiency of coal fired power plants. The research is performed as part of a comprehensive project to evaluate the ability of titanium, titanium carbide, or titanium diboride powders to provide fireside corrosion resistance in supercritical and ultra-supercritical steam boilers, specifically, coal driven boilers in Illinois that must utilize high sulfur and high chlorine content coal. [1] The powder coatings that were tested are nano-sized titanium carbide (TiC) and titanium di-boride (TiB2) powders that were synthesized by a patented process at Southern Illinois University. The powders were then sent to Gas Technology Institute in Chicago to coat steel coupons by HVOF (High Velocity Oxy-Fuel) thermal spray technique. The powders were coated on an austenitic 304H stainless steel substrate which is commonly found in high temperature boilers, pipelines, and heat exchangers. The samples then went through various tests for various lengths of time under subcritical, supercritical, and ultra-supercritical conditions. The samples were examined using a scanning electron microscope and x-ray diffraction techniques to study microstructural changes and then determined which coating performed best.

The use of waste materials in asphalt concrete mixtures.

PubMed

Tuncan, Mustafa; Tuncan, Ahmet; Cetin, Altan

2003-04-01

The purpose of this study was to investigate (a) the effects of rubber and plastic concentrations and rubber particle sizes on properties of asphalt cement, (b) on properties of asphalt concrete specimens and (c) the effects of fly ash, marble powder, rubber powder and petroleum contaminated soil as filler materials instead of stone powder in the asphalt concrete specimens. One type of limestone aggregate and one penetration-graded asphalt cement (75-100) were used. Three concentrations of rubber and plastic (i.e. 5%, 10% and 20% of the total weight of asphalt cement), three rubber particle sizes (i.e. No. 4 [4.75mm] - 20 [0.85 mm], No. 20 [0.85mm] - 200 [0.075mm] and No. 4 [4.75mm] - 200 [0.075mm]) and one plastic particle size (i.e. No. 4 [4.75mm] - 10 [2.00mm]) were also used. It was found that while the addition of plastic significantly increased the strength of specimens, the addition of rubber decreased it. No. 4 [4.75mm] - 200 [0.075mm] rubber particles showed the best results with respect to the indirect tensile test. The Marshall stability and indirect tensile strength properties of plastic modified specimens increased. Marble powder and fly ash could be used as filler materials instead of stone powder in the asphalt concrete pavement specimens.

Effects of Process Parameters on Copper Powder Compaction Process Using Multi-Particle Finite Element Method

NASA Astrophysics Data System (ADS)

Güner, F.; Sofuoğlu, H.

2018-01-01

Powder metallurgy (PM) has been widely used in several industries; especially automotive and aerospace industries and powder metallurgy products grow up every year. The mechanical properties of the final product that is obtained by cold compaction and sintering in powder metallurgy are closely related to the final relative density of the process. The distribution of the relative density in the die is affected by parameters such as compaction velocity, friction coefficient and temperature. Moreover, most of the numerical studies utilizing finite element approaches treat the examined environment as a continuous media with uniformly homogeneous porosity whereas Multi-Particle Finite Element Method (MPFEM) treats every particles as an individual body. In MPFEM, each of the particles can be defined as an elastic- plastic deformable body, so the interactions of the particles with each other and the die wall can be investigated. In this study, each particle was modelled and analyzed as individual deformable body with 3D tetrahedral elements by using MPFEM approach. This study, therefore, was performed to investigate the effects of different temperatures and compaction velocities on stress distribution and deformations of copper powders of 200 µm-diameter in compaction process. Furthermore, 3-D MPFEM model utilized von Mises material model and constant coefficient of friction of μ=0.05. In addition to MPFEM approach, continuum modelling approach was also performed for comparison purposes.

Recent advances in graphite powder-based electrodes.

PubMed

Bellido-Milla, Dolores; Cubillana-Aguilera, Laura Ma; El Kaoutit, Mohammed; Hernández-Artiga, Ma Purificación; Hidalgo-Hidalgo de Cisneros, José Luis; Naranjo-Rodríguez, Ignacio; Palacios-Santander, José Ma

2013-04-01

Graphite powder-based electrodes have the electrochemical performance of quasi-noble metal electrodes with intrinsic advantages related to the possibility of modification to enhance selectivity and their easily renewable surface, with no need for hazardous acids or bases for their cleaning. In contrast with commercial electrodes, for example screen-printed or sputtered-chip electrodes, graphite powder-based electrodes can also be fabricated in any laboratory with the form and characteristics desired. They are also readily modified with advanced materials, with relatively high reproducibility. All these characteristics make them a very interesting option for obtaining a large variety of electrodes to resolve different kinds of analytical problems. This review summarizes the state-of-the-art, advantages, and disadvantages of graphite powder-based electrodes in electrochemical analysis in the 21st century. It includes recent trends in carbon paste electrodes, devoting special attention to the use of emergent materials as new binders and to the development of other composite electrodes. The most recent advances in the use of graphite powder-modified sol-gel electrodes are also described. The development of sonogel-carbon electrodes and their use in electrochemical sensors and biosensors is included. These materials extend the possibilities of applications, especially for industrial technology-transfer purposes, and their development could affect not only electroanalytical green chemistry but other interesting areas also, for example catalysis and energy conversion and storage.

The decontamination of industrial casein and milk powder by irradiation

NASA Astrophysics Data System (ADS)

Żegota, H.; Małolepszy, B.

2008-09-01

The efficacy of gamma radiation decontamination of industrial casein, a milk protein utilized as a component of many food and non-food products has been studied. Low-fat milk powder was also included with a purpose to study the microflora survival in protein-rich materials. Microbial analysis of the samples prior to irradiation showed that the initial total viable count was higher than 6.0 log cfu g -1 in both casein and milk powders. The contamination of casein with moulds and yeasts was found to be equal to 3.56 log cfu g -1. The counts of coliforms have not exceeded the value of 2.48 log cfu g -1. Radiation processing of casein and milk powder has substantially reduced the microbial population of all samples. The dose of 5 kGy was sufficient to reduce the total microflora and coliforms counts to the level permitted for food products. Survivals of microorganisms were analyzed by the generalized exponential equation, SF =exp[ -D/ Do) α]. Values of an exponent, α, standing for the dispersion parameter, were equal to 0.65 and 0.70 for microorganisms contaminating casein and milk powders, respectively. The numerical value of the dispersion parameter α<1 indicates the concave dependence of a logarithm of surviving fraction versus radiation dose. No difference in microflora survival in irradiated samples tested immediately and in samples stored for 1-month after irradiation has been noticed.

Flow Function of Pharmaceutical Powders Is Predominantly Governed by Cohesion, Not by Friction Coefficients.

PubMed

Leung, Lap Yin; Mao, Chen; Srivastava, Ishan; Du, Ping; Yang, Chia-Yi

2017-07-01

The purpose of this study was to demonstrate that the flow function (FFc) of pharmaceutical powders, as measured by rotational shear cell, is predominantly governed by cohesion but not friction coefficients. Driven by an earlier report showing an inverse correlation between FFc and the cohesion divided by the corresponding pre-consolidation stress (Wang et al. 2016. Powder Tech. 294:105-112), we performed analysis on a large data set containing 1130 measurements from a ring shear tester and identified a near-perfect inverse correlation between the FFc and cohesion. Conversely, no correlation was found between FFc and friction angles. We also conducted theoretical analysis and estimated such correlations based on Mohr-Coulomb failure model. We discovered that the correlation between FFc and cohesion can sustain as long as the angle of internal friction at incipient flow is not significantly larger than the angle of internal friction at steady-state flow, a condition covering almost all pharmaceutical powders. The outcome of this study bears significance in pharmaceutical development. Because the cohesion value is strongly influenced by the interparticle cohesive forces, this study effectively shows that it is more efficient to improve the pharmaceutical powder flow by lowering the interparticle cohesive forces than by lowering the interparticle frictions. Copyright © 2017 American Pharmacists Association®. Published by Elsevier Inc. All rights reserved.

The effect of operating and formulation variables on the morphology of spray-dried protein particles.

PubMed

Maa, Y F; Costantino, H R; Nguyen, P A; Hsu, C C

1997-08-01

The purpose of this research was to investigate the shape and morphology of various spray-dried protein powders as a function of spray-drying conditions and protein formulations. A benchtop spray dryer was used to spray dry three model proteins in formulation with a sugar or a surfactant. Physical characterizations of the powder included morphology (scanning electron microscopy), particle size, residual moisture, and X-ray powder diffraction analyses. A significant change in particle shape from irregular (e.g., "donut") to spherical was observed as the outlet temperature of the dryer was decreased. The drying air outlet temperature was shown to depend on various operating parameters and was found to correlate with the drying rate of atomized droplets in the drying chamber. The morphology of spray-dried protein particles was also affected by formulation. In protein:sugar formulations, spray-dried particles exhibited a smooth surface regardless of the protein-to-lactose ratio, whereas roughness was observed when mannitol was present at > 30% of total solids, due to recrystallization. Protein particles containing trehalose at concentrations > 50% were highly agglomerated. The presence of surfactant resulted in noticeably smoother, more spherical particles. The shape and the morphology of spray-dried powders are affected by spray drying conditions and protein formulation. This study provides information useful for development of dry proteins for fine powder (e.g., aerosol) applications.

Effect of Powder Leaf Breadfruit Disposals (Arthocarpus Altilis) in Oil Mandar District and Polman Against Cholesterol and Glucose Mice (Mus Musculus)

NASA Astrophysics Data System (ADS)

Mu'nisa, A.; Asmawati, A.; Farida, A.; FA, Fressy; Erni

2018-01-01

The purpose of this study was to determine the effect of powdered leaves of breadfruit (Arthocarpus altilis) on oil is mandated origin of the Polman glucose and cholesterol levels in mice (Mus musculus). This study comprised 4 treatments and each treatment consisted of 5 replicates, ie groups of mice were fed a standard (negative control); 2 groups: group of mice fed with standard and cholesterol feed (positive control); Group 3 that mice fed with standard and Selayar oil; and group 4: group of mice fed with standard and Mandar oil that has been given powdered leaves of breadfruit. Measurement of glucose and blood cholesterol levels in mice done 3 times ie 2 weeks after the adaptation period (phase 1), 2 weeks after administration of the oil (phase 2) and 2 weeks after feeding cholesterol (stage 3). Based on the analysis of data both cholesterol and glucose levels showed that in a group of 4 decreased glucose and cholesterol levels in stage 2 but at stage 3 an increase in the group of mice given only the oil while in the group of mice given the oil and powdered leaves of breadfruit indicate glucose levels and normal cholesterol. The conclusion of this study show that the addition of powdered leaves of breadfruit into cooking oil Mandar influential in glucose levels and normalize blood cholesterol levels in mice.

Precipitation behavior of σ phase in fusion zone of dissimilar stainless steel welds during multi-pass GTAW process

NASA Astrophysics Data System (ADS)

Hsieh, Chih-Chun; Chang, Tao-Chih; Lin, Dong-Yih; Chen, Ming-Che; Wu, Weite

2007-10-01

The purpose of this study is to investigate the precipitation characteristics of σ phase in the fusion zone of stainless steel welds at various welding passes during a tungsten are welding (GTAW) process. The morphology, quantity, and chemical composition of the δ-ferrite and σ phase were analyzed using optical microscopy (OM), a ferritscope (FS), a X-ray diffractometer (XRD), scanning electron microscopy (SEM), an electron probe micro-analyzer (EPMA), and a wavelength dispersive spectrometer (WDS), respectively. Massive δ-ferrite was observed in the fusion zone of the first pass welds during welding of dissimilar stainless steels. The σ phase precipitated at the inner δ-ferrite particles and decreased δ-ferrite content during the third pass welding. The σ and δ phases can be stabilized by Si element, which promoted the phase transformation of σ→ϱ+λ2 in the fusion zone of the third pass welds. It was found that the σ phase was a Fe-Cr-Si intermetallic compound found in the fusion zone of the third pass welds during multi-pass welding.

A study of 23 unicameral bone cysts of the calcaneus: open chip allogeneic bone graft versus percutaneous injection of bone powder with autogenous bone marrow.

PubMed

Park, Il-Hyung; Micic, Ivan Dragoljub; Jeon, In-Ho

2008-02-01

The treatment of unicameral bone cyst varies from percutaneous needle biopsy, aspiration and local injection of steroid, autologous bone marrow, or demineralized bone matrix to curettage and open bone-grafting. The purpose of this study was to compare the results of open chip allogeneic bone graft versus percutaneous injection of demineralized bone powder with autogenous bone marrow in management of calcaneal cysts. Twenty-three calcaneal unicameral cysts in 20 patients were treated. Lyophilized irradiated chip allogeneic bone (CAB) and autogenous bone marrow were used for treatment of 13 cysts in 11 patients, and 10 cysts in 9 patients were treated with percutaneous injection of irradiated allogeneic demineralized bone powder (DBP) and autogenous bone marrow. There were 11 males and 9 female patients with mean age of 17 years. The patients were followed for an average of 49.4 months. Complete healing was achieved in 9 cysts treated with chip allogeneic bone and in 5 cysts treated with powdered bone. Four cysts treated with CAB and 3 cysts treated with DBP healed with a defect. Two cysts treated with powdered bone and autogenous bone marrow were classified as persistent. No infections or pathological fractures were observed during the followup period. Percutaneous injection of a mixture of allogeneic bone powder with autogenous bone marrow is a minimal invasive method and could be an effective alternative in the treatment of unicameral calcaneal bone cysts. The postoperative morbidity was low, the hospital stay was brief, and patient's comfort for unrestricted activity was enhanced.

Effects of Dentin Debris on the Antimicrobial Properties of Sodium Hypochlorite and Etidronic Acid.

PubMed

Arias-Moliz, Maria Teresa; Morago, Ana; Ordinola-Zapata, Ronald; Ferrer-Luque, Carmen María; Ruiz-Linares, Matilde; Baca, Pilar

2016-05-01

The purpose of this study was to determine the influence of dentin powder on the concentration, pH, and antimicrobial activity of sodium hypochlorite (NaOCl) alone and combined with etidronic acid (HEBP). Biofilms of Enterococcus faecalis were grown on the surface of dentin blocks for 5 days and then exposed to 1% and 2.5% NaOCl alone or combined with 9% HEBP for 3 minutes in the absence and presence of dentin powder. The biovolumes of the biofilm were measured using confocal microscopy and the live/dead technique. The available chlorine and pH of the solutions were also measured. Nonparametric tests were used to determine statistical differences (P < .05). The presence of dentin powder resulted in a reduction of the free available chlorine and pH in all the irrigating solutions; 1% NaOCl lost its antimicrobial activity completely in the presence of dentin powder. The antimicrobial activity was significantly reduced in the 2.5% NaOCl and 1% NaOCl/HEBP groups, and it was not affected in the 2.5% NaOCl/HEBP group. The presence of dentin powder significantly decreased the available chlorine and antimicrobial activity of 1% NaOCl, 2.5% NaOCl, and 1% NaOCl/HEBP irrigating solutions. The antimicrobial activity of 2.5% NaOCl/HEBP was not affected by the dentin powder after a 3-minute contact time against E. faecalis biofilms. Copyright © 2016 American Association of Endodontists. Published by Elsevier Inc. All rights reserved.

[Controlled release of prednisolone from suppository prepared using powder of pulverized tablet].

PubMed

Tatsumi, Akitoshi; Oda, Shoko; Nakamoto, Tomoko; Muraoka, Reiko; Takahashi, Yoshiko; Tanaka, Kuniyoshi; Shikata, Toshiyuki; Tatsumi, Sumiyo; Tagawa, Noriko; Kobayashi, Yoshiharu; Hamaguchi, Tsuneo; Kadobayashi, Muneo

2008-04-01

Prednisolone suppositories have been used successfully for the treatment of ulcerative colitis in hospital settings. However, the raw material of prednisolone suppository, JP prednisolone powder (JP Powder), was recently removed from the market. Therefore we studied the effects of raw material and suppository base on the release of prednisolone suppository for the purpose of designing a new suppository with similar effects to those of suppository prepared using JP powder (old suppository). New suppositories consisting of the powder of pulverized tablet as raw material and Witepsol H-15 and Witepsol E-75 as suppository base were prepared according to the fusion method. Suppository release test was performed by reciprocating dialysis tube method with tapping (RDT method) and dialysis tubing method (DT method). Both RDT method and DT method were performed using a suppository dissolution apparatus (modified JP disintegration apparatus) and a JP15 paddle apparatus, respectively. The test fluid was 50 mM phosphate buffer solution (pH 7.4) maintained at 37+/-0.5 degrees C. The results of release test by RDT method were similar to those of DT method. Release rate of prednisolone from the new suppository was much faster than that of old suppository. The addition of Witepsol E-75 to new suppository base markedly delayed the release of prednisolone from the new suppository. Release rate of prednisolone from the new suppository, consisting of pulverized tablet and Witepsol H-15 and Witepsol E-75 (76:24), corresponded well with that of the old suppository. It was suggested that this suppository could be used as incoming preparation of suppository prepared using JP powder.

Transmission electron microscopy characterization of microstructural features of Al-Li-Cu alloys

NASA Technical Reports Server (NTRS)

Avalos-Borja, M.; Pizzo, P. P.; Larson, L. A.

1983-01-01

A transmission electron microscopy (TEM) examination of aluminum-lithium-copper alloys was conducted. The principal purpose is to characterize the nature, size, and distribution of stringer particles which result from the powder metallurgy (P/M) processing of these alloys. Microstructural features associated with the stringer particles are reported that help explain the stress corrosion susceptibility of the powder metallurgy-processed Al-Li-Cu alloys. In addition, matrix precipitation events are documented for a variety of heat treatments and process variations. Hot rolling is observed to significant alter the nature of matrix precipitation, and the observations are correlated with concomitant mechanical property variations.

Transmission electron microscopy characterization of microstructural features in aluminum-lithium-copper alloys

NASA Technical Reports Server (NTRS)

Avalos-Borja, M.; Larson, L. A.; Pizzo, P. P.

1984-01-01

A transmission electron microscopy (TEM) examination of aluminum-lithium-copper alloys was conducted. The principal purpose is to characterize the nature, size, and distribution of stringer particles which result from the powder metallurgy (P/M) processing of these alloys. Microstructural features associated with the stringer particles are reported that help explain the stress corrosion susceptibility of the powder metallurgy-processed Al-Li-Cu alloys. In addition, matrix precipitaton events are documented for a variety of heat treatments and process variations. Hot rolling is observed to significantly alter the nature of matrix precipitation, and the observations are correlated with concomitant mechanical property variations.

High resolution laser micro sintering / melting using q-switched and high brilliant laser radiation

NASA Astrophysics Data System (ADS)

Exner, H.; Streek, A.

2015-03-01

Since the discovery of selective laser sintering/melting, numerous modifications have been made to upgrade or customize this technology for industrial purposes. Laser micro sintering (LMS) is one of those modifications: Powders with particles in the range of a few micrometers are used to obtain products with highly resolved structures. Pulses of a q-switched laser had been considered necessary in order to generate sinter layers from the micrometer scaled metal powders. LMS has been applied with powders from metals as well as from ceramic and cermet feedstock's to generate micro parts. Recent technological progress and the application of high brilliant continuous laser radiation have now allowed an efficient laser sintering/melting of micrometer scaled metal powders. Thereby it is remarkable that thin sinter layers are generated using high continuous laser power. The principles of the process, the state of the art in LMS concerning its advantages and limitations and furthermore the latest results of the recent development of this technology will be presented. Laser Micro Sintering / Laser Micro Melting (LMM) offer a vision for a new dimension of additive fabrication of miniature and precise parts also with application potential in all engineering fields.

Combination Chemotherapeutic Dry Powder Aerosols via Controlled Nanoparticle Agglomeration

PubMed Central

El-Gendy, Nashwa; Berkland, Cory

2014-01-01

Purpose To develop an aerosol system for efficient local lung delivery of chemotherapeutics where nanotechnology holds tremendous potential for developing more valuable cancer therapies. Concurrently, aerosolized chemotherapy is generating interest as a means to treat certain types of lung cancer more effectively with less systemic exposure to the compound. Methods Nanoparticles of the potent anticancer drug, paclitaxel, were controllably assembled to form low density microparticles directly after preparation of the nanoparticle suspension. The amino acid, L-leucine, was used as a colloid destabilizer to drive the assembly of paclitaxel nanoparticles. A combination chemotherapy aerosol was formed by assembling the paclitaxel nanoparticles in the presence of cisplatin in solution. Results Freeze-dried powders of the combination chemotherapy possessed desirable aerodynamic properties for inhalation. In addition, the dissolution rates of dried nanoparticle agglomerate formulations (~60% to 66% after 8 h) were significantly faster than that of micronized paclitaxel powder as received (~18% after 8 h). Interestingly, the presence of the water soluble cisplatin accelerated the dissolution of paclitaxel. Conclusions Nanoparticle agglomerates of paclitaxel alone or in combination with cisplatin may serve as effective chemotherapeutic dry powder aerosols to enable regional treatment of certain lung cancers. PMID:19415471

The effect of additive geometry on the integration of secondary elements during Friction Stir Processing

NASA Astrophysics Data System (ADS)

Zens, A.; Gnedel, M.; Zaeh, M. F.; Haider, F.

2018-06-01

Friction Stir Processing (FSP) can be used to locally modify properties in materials such as aluminium. This may be used, for example, to produce a fine microstructure or to integrate secondary elements into the base material. The purpose of this work is to examine the effect of the properties of the metal additives on the resulting material distribution in the processed region. For this, commercially pure iron and copper were integrated into an EN AW-1050 aluminium base material using FSP. Iron in the form of powder, wire and foil as well as copper in powder form were assessed. The various additive forms represent materials with differing surface-to-volume ratios as well as varying dispersion characteristics in the processing zone. The processing parameters for each additive form remained constant; however, two- and four-pass FSP processes were conducted. The results of CT analysis proved especially insightful regarding the spatial distribution of the various additive form within the workpiece. As expected, the powder additive was most widely distributed within the welding zone. Micro-hardness mappings showed that the powder additive contributed to the hardness within the weld nugget in comparison to the processed material without secondary elements.

Fluid mediated transformation of aragonitic cuttlebone to calcite

NASA Astrophysics Data System (ADS)

Perdikouri, C.; Kasioptas, A.; Putnis, A.

2009-04-01

The aragonite to calcite transition has been studied extensively over the years because of its wide spectra of applications and of its significant geochemical interest. While studies of kinetics (e.g. Topor et al., 1981), thermodynamics (e.g. Wolf et al., 1996) and behavior of ions such as Sr and Mg (e.g. Yoshioka et al., 1986) have been made there are still unanswered questions regarding this reaction especially in the cases where the effects of fluid composition are considered. It is well known that when heated in air, aragonite transforms by a solid state reaction to calcite. The aragonite cuttlebone of the sepia officinalis that was used for our experiments undergoes a phase transition at ~370-390˚ C, measured by in situ heating experiments in a Philips X'pert X-ray powder diffractometer equipped with a HTK 1200 High temperature oven. Successive X-ray scans were taken at isothermal temperatures at 200C intervals. A similar temperature range was found by Vongsavat et al. 2006, who studied this transition in Acropora corals. It is possible however to promote this transition at considerably lower temperatures by means of a fluid mediated reaction where the replacement takes place by a dissolution-precipitation mechanism (Putnis & Putnis, 2007). We have successfully carried out hydrothermal experiments where cuttlebone has been converted to calcite at 200˚ C. Using the PhreeqC program we calculated the required composition of a solution that would be undersaturated with respect to aragonite and saturated with respect to calcite leading to dissolution of the aragonite and to a consequent precipitation of the new calcite phase, similar to the experiments described in an earlier study (Perdikouri et al, 2008). This reaction is not pseudomorphic and results in the destruction of the morphology, presumably due to the molar volume increase. A total transformation of the cuttlebone produced a fine calcite powder. The cuttlebone exhibits a unique microstructure, made up of interconnected chambers. The aragonite grown during biomineralization of the cuttlebone is interlaced with a β-chitin organic phase that provides the framework for the morphology that is observed. Experiments carried out with the same constant conditions but for different periods of time have revealed the evolution of the transformation to calcite. At shorter reaction times the product was made up of calcite powder and of well preserved aragonite septa, as was confirmed by powder X-ray diffraction. In other words, the vertical pillars appear to react at faster rates than the horizontal septa. It has been reported by Florek et al. 2008 that the septa contain higher quantities of β-chitin. The aim of this study is the investigation of these observations and the determination of the effect of the organic component on the kinetics of the aragonite to calcite transformation. Florek M., Fornal E., Gómez-Romero P., Zieba E., Paszkowicz W., Lekki J.,Nowak J., Kuczumow A. Materials Science and Engineering C, In Press (2008) Perdikouri C., Kasioptas A., Putnis C.V., Putnis A. Mineralogical Magazine 72, 111-114 (2008) Putnis A., Putnis C.V. Solid State Chemistry 180, 1783-1786 (2007) Topor N. D., Tolokonnikova L. I., Kadenatsi B. M. Journal of Thermal Analysis 20, 169-174 (1981) Vongsavat V., Winotai P., Meejoo S. Nuclear Instruments and Methods in Physics Research B 243, 167-173 (2006) Wolf G., Lerchner J., Schmidt H., Gamsjäger H., Königsberger E., Schmidt P. Journal of Thermal Analysis 46, 353-359 (1996) Yoshioka S., Ohde S., Kitano Y., Kanamori N. Marine Chemistry 18, 35-48 (1986)

Crystal and Vibrational Structure of Energetic 3,5-dinitro 1,3,5-oxadiazinane (DOD) by Single Crystal X-ray Diffractometry and Raman Spectroscopy

DTIC Science & Technology

2018-03-19

calculations using a temperature of 298 K. 15. SUBJECT TERMS 3,5-dinitro-1,3,5-oxadiazinane (DOD), X-ray crystallography , Raman, energetic material...X-ray analysis. 2.2 Characterization X-ray Crystallography . DOD crystals were characterized with a SuperNova, Dualflex, EosS2 diffractometer using

In situ surface/interface x-ray diffractometer for oxide molecular beam epitaxy

DOE PAGES

Lee, J. H.; Tung, I. C.; Chang, S. -H.; ...

2016-01-05

In situ studies of oxide molecular beam epitaxy by synchrotron x-ray scattering has been made possible by upgrading an existing UHV/molecular beam epitaxy (MBE) six-circle diffractometer system. For oxide MBE growth, pure ozone delivery to the chamber has been made available, and several new deposition sources have been made available on a new 12 in. CF (ConFlat, a registered trademark of Varian, Inc.) flange. X-ray diffraction has been used as a major probe for film growth and structures for the system. In the original design, electron diffraction was intended for the secondary diagnostics available without the necessity of the x-raymore » and located at separate positions. Deposition of films was made possible at the two diagnostic positions. And, the aiming of the evaporation sources is fixed to the point between two locations. Ozone can be supplied through two separate nozzles for each location. Also two separate thickness monitors are installed. Finally, additional features of the equipment are also presented together with the data taken during typical oxide film growth to illustrate the depth of information available via in situ x-ray techniques.« less

Low dose radiation damage effects in silicon strip detectors

NASA Astrophysics Data System (ADS)

Wiącek, P.; Dąbrowski, W.

2016-11-01

The radiation damage effects in silicon segmented detectors caused by X-rays have become recently an important research topic driven mainly by development of new detectors for applications at the European X-ray Free Electron Laser (E-XFEL). However, radiation damage in silicon strip is observed not only after extreme doses up to 1 GGy expected at E-XFEL, but also at doses in the range of tens of Gy, to which the detectors in laboratory instruments like X-ray diffractometers or X-ray spectrometers can be exposed. In this paper we report on investigation of radiation damage effects in a custom developed silicon strip detector used in laboratory diffractometers equipped with X-ray tubes. Our results show that significant degradation of detector performance occurs at low doses, well below 200 Gy, which can be reached during normal operation of laboratory instruments. Degradation of the detector energy resolution can be explained by increasing leakage current and increasing interstrip capacitance of the sensor. Another observed effect caused by accumulation of charge trapped in the surface oxide layer is change of charge division between adjacent strips. In addition, we have observed unexpected anomalies in the annealing process.

75 FR 44247 - Product Cancellation Order for Certain Pesticide Registrations

Federal Register 2010, 2011, 2012, 2013, 2014

2010-07-28

...-Rest AQ Pyrethrins, Piperonyl butoxide 067517-00045 Hard Hitter Permethrin Aerosol 067517-00049 Dog and... Permethrin 067517-00056 Flea And Insect Pyrethrins, Carpet Dust Piperonyl butoxide 067517-00057 Cat And Dog Pyrethrins, Pyrethrin Powder Piperonyl butoxide 067517-00061 Permethrin 10% Permethrin W.B. Multi- Purpose...

A novel open-framework with non-crossing channels in the uranyl vanadates A(UO 2) 4(VO 4) 3 ( A=Li, Na)

NASA Astrophysics Data System (ADS)

Obbade, S.; Dion, C.; Rivenet, M.; Saadi, M.; Abraham, F.

2004-06-01

A new sodium uranyl vanadate Na(UO 2) 4(VO 4) 3 has been synthesized by solid-state reaction and its structure determined from single-crystal X-ray diffraction data. It crystallizes in the tetragonal symmetry with space group I4 1/ amd and following cell parameters: a=7.2267(4) Å and c=34.079(4) Å, V=1779.8(2) Å 3, Z=4 with ρmes=5.36(3) g/cm 3 and ρcal=5.40(2) g/cm 3. A full-matrix least-squares refinement on the basis of F2 yielded R1=0.028 and w R2=0.056 for 52 parameters with 474 independent reflections with I⩾2 σ( I) collected on a BRUKER AXS diffractometer with Mo Kα radiation and a CCD detector. The crystal structure is characterized by ∞2[(UO 2) 2(VO 4)] sheets parallel to (001) formed by corner-shared UO 6 distorted octahedra and V(2)O 4 tetrahedra, connected by V(1)O 4 tetrahedra to ∞1[UO 5] 4- chains of edge-shared UO 7 pentagonal bipyramids alternately parallel to the a- and b-axis. The resulting three-dimensional framework creates mono-dimensional channels running down the a- and b-axis formed by face-shared oxygen octahedra half occupied by Na. The powder of Li analog compound Li(UO 2) 4(VO 4) 3 has been synthesized by solid-state reaction. The two compounds exhibit high mobility of the alkaline ions within the two-dimensional network of non-intersecting channels.

Effect of sintering atmosphere on properties of porous stainless steel for biomedical applications.

PubMed

Dudek, Agata; Włodarczyk, Renata

2013-01-01

This study discusses manufacturing of metallic biomaterials by means of powder metallurgy with consideration for their unquestionable advantages, i.e. opportunities of obtaining materials with controllable porosity. The paper focuses on properties of 316 L stainless steel obtained using the method of powder metallurgy with respect to compacting pressure and sintering atmosphere. All the specimens were compacted at 700, 400 and 225 MPa, and sintered at 1250 °C. In order to analyze the sintering atmosphere, three different media were used: dissociated ammonia, hydrogen and vacuum. The study covered sintering density, porosity, microstructure analysis and corrosion resistance. The proposed method of powder metallurgy allowed for obtaining materials with predictable size and distribution of pores, depending on the parameters of sinter preparation (compaction force, sinter atmosphere). High corrosion resistance of the materials (sintering in the atmosphere of hydrogen and in vacuum) and high porosity in the sinters studied offer opportunities for using them for medical purposes. Copyright © 2012 Elsevier B.V. All rights reserved.

Experimental investigation of amount of nano-Al2O3 on mechanical properties of Al-based nano-composites fabricated by powder metallurgy (PM)

NASA Astrophysics Data System (ADS)

Razzaqi, A.; Liaghat, Gh.; Razmkhah, O.

2017-10-01

In this paper, mechanical properties of Aluminum (Al) matrix nano-composites, fabricated by Powder Metallurgy (PM) method, has been investigated. Alumina (Al2O3) nano particles were added in amounts of 0, 2.5, 5, 7.5 and 10 weight percentages (wt%). For this purpose, Al powder (particle size: 20 µm) and nano-Al2O3 (particle size: 20 nm) in various weight percentages were mixed and milled in a blade mixer for 15 minutes in 1500 rpm. Then, the obtained mixture, compacted by means of a two piece die and uniaxial cold press of about 600 MPa and cold iso-static press (CIP), required for different tests. After that, the samples sintered in 600°C for 90 minutes. Compression and three-point bending tests performed on samples and the results, led us to obtain the optimized particle size for achieving best mechanical properties.

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.

Na3Si2Y0.16Zr1.84PO12-ionic liquid hybrid electrolytes: An approach for realizing solid-state sodium-ion batteries?

NASA Astrophysics Data System (ADS)

de la Torre-Gamarra, Carmen; Appetecchi, Giovanni Battista; Ulissi, Ulderico; Varzi, Alberto; Varez, Alejandro; Passerini, Stefano

2018-04-01

Ceramic electrolytes are prepared through sintering processes which are carried out at high temperatures and require prolonged operating times, resulting unwelcome in industrial applications. We report a physicochemical characterization on hybrid, sodium conducting, electrolyte systems obtained by coating NASICON ceramic powders with the N-butyl-N-methylpyrrolidinium bis(trifluoromethanesulfonyl)imide ionic liquid. The goal is to realize a ceramic-IL interface with improved sodium mobility, aiming to obtain a solid electrolyte with high ion transport properties but avoiding sintering thermal treatment. The purpose of the present work, however, is showing how simply combining NASICON powder and Py14TFSI does not lead to any synergic effect on the resulting hybrid electrolyte, evidencing that an average functionalization of the ceramic powder surface and/or ionic liquid is needed. Also, the processing conditions for preparing the hybrid samples are found to affect their ion transport properties.

Physico-Chemical Properties, Aerosolization and Dissolution of Co-Spray Dried Azithromycin Particles with L-Leucine for Inhalation.

PubMed

Mangal, Sharad; Nie, Haichen; Xu, Rongkun; Guo, Rui; Cavallaro, Alex; Zemlyanov, Dmitry; Zhou, Qi Tony

2018-01-08

Inhalation therapy is popular to treat lower respiratory tract infections. Azithromycin is effective against some bacteria that cause respiratory tract infections; but it has poor water solubility that may limit its efficacy when administrated as inhalation therapy. In this study, dry powder inhaler formulations were developed by co-spray drying azithromycin with L-leucine with a purpose to improve dissolution. The produced powder formulations were characterized regarding particle size, morphology, surface composition and in-vitro aerosolization performance. Effects of L-leucine on the solubility and in-vitro dissolution of azithromycin were also evaluated. The spray dried azithromycin alone formulation exhibited a satisfactory aerosol performance with a fine particle fraction (FPF) of 62.5 ± 4.1%. Addition of L-leucine in the formulation resulted in no significant change in particle morphology and FPF, which can be attributed to enrichment of azithromycin on the surfaces of composite particles. Importantly, compared with the spray-dried amorphous azithromycin alone powder, the co-spray dried powder formulations of azithromycin and L-leucine demonstrated a substantially enhanced in-vitro dissolution rate. Such enhanced dissolution of azithromycin could be attributed to the formation of composite system and the acidic microenvironment around azithromycin molecules created by the dissolution of acidic L-leucine in the co-spray dried powder. Fourier transform infrared spectroscopic data showed intermolecular interactions between azithromycin and L-leucine in the co-spray dried formulations. We developed the dry powder formulations with satisfactory aerosol performance and enhanced dissolution for a poorly water soluble weak base, azithromycin, by co-spray drying with an amino acid, L-leucine.

Effect of lyophilized powder made from enzymolyzed honeybee larvae on tinnitus-related symptoms, hearing levels, and hypothalamus-pituitary-adrenal axis-related hormones.

PubMed

Aoki, Mitsuhiro; Wakaoka, Yoshinori; Hayashi, Hisamitsu; Kuze, Bunya; Mizuta, Keisuke; Ito, Yatsuji

2012-01-01

Tinnitus interferes with sleep and concentration which is associated with depression; however, no drug has been effective in treating tinnitus. Our purpose is to evaluate our hypothesis that the treatment with lyophilized powder of enzymolyzed honeybee larvae as a complementary medicine may provide a therapeutic effect on tinnitus-related symptoms. Sixty tinnitus sufferers participated in a randomized double-blind placebo-controlled trial using the lyophilized powder of enzymolyzed honeybee larvae or a placebo. The Tinnitus Handicap Inventory, a visual analog scale to rate the severity of tinnitus, hearing levels, and hypothalamus-pituitary-adrenal axis-related hormones drawn early in the morning were measured upon entry into the study and after 12 wk of follow-up. The lyophilized powder of enzymolyzed honeybee larvae was not superior to placebo with regard to the total score on the Tinnitus Handicap Inventory and the visual analog scale. However, subjects in the honeybee larvae group showed significant improvements in some items about depression associated with tinnitus, whereas subjects in the placebo group showed no improvement in any items. The honeybee larvae group showed significant improvements in the hearing levels at 2 and 4 kHz in the audiogram of the better ear. The intervention of the lyophilized powder of enzymolyzed honeybee larvae was associated with lower serum cortisol levels, serum prolactin levels, and cortisol/dehydroepiandrosterone sulfate ratios. The ratios in the placebo group significantly were increased. Our results suggest that the lyophilized powder of enzymolyzed honeybee larvae represents an effective complementary medicine to alleviate depression associated with tinnitus by regulating the activity of the hypothalamus-pituitary-adrenal axis.

Development of Experimental Setup of Metal Rapid Prototyping Machine using Selective Laser Sintering Technique

NASA Astrophysics Data System (ADS)

Patil, S. N.; Mulay, A. V.; Ahuja, B. B.

2018-04-01

Unlike in the traditional manufacturing processes, additive manufacturing as rapid prototyping, allows designers to produce parts that were previously considered too complex to make economically. The shift is taking place from plastic prototype to fully functional metallic parts by direct deposition of metallic powders as produced parts can be directly used for desired purpose. This work is directed towards the development of experimental setup of metal rapid prototyping machine using selective laser sintering and studies the various parameters, which plays important role in the metal rapid prototyping using SLS technique. The machine structure in mainly divided into three main categories namely, (1) Z-movement of bed and table, (2) X-Y movement arrangement for LASER movements and (3) feeder mechanism. Z-movement of bed is controlled by using lead screw, bevel gear pair and stepper motor, which will maintain the accuracy of layer thickness. X-Y movements are controlled using timing belt and stepper motors for precise movements of LASER source. Feeder mechanism is then developed to control uniformity of layer thickness metal powder. Simultaneously, the study is carried out for selection of material. Various types of metal powders can be used for metal RP as Single metal powder, mixture of two metals powder, and combination of metal and polymer powder. Conclusion leads to use of mixture of two metals powder to minimize the problems such as, balling effect and porosity. Developed System can be validated by conducting various experiments on manufactured part to check mechanical and metallurgical properties. After studying the results of these experiments, various process parameters as LASER properties (as power, speed etc.), and material properties (as grain size and structure etc.) will be optimized. This work is mainly focused on the design and development of cost effective experimental setup of metal rapid prototyping using SLS technique which will gives the feel of metal rapid prototyping process and its important parameters.

Microstructure and Mechanical Properties of Long Ti-6Al-4V Rods Additively Manufactured by Selective Electron Beam Melting Out of a Deep Powder Bed and the Effect of Subsequent Hot Isostatic Pressing

NASA Astrophysics Data System (ADS)

Lu, S. L.; Tang, H. P.; Ning, Y. P.; Liu, N.; StJohn, D. H.; Qian, M.

2015-09-01

An array of eight long Ti-6Al-4V rods (diameter: 12 mm; height: 300 mm) have been additively manufactured, vertically and perpendicular to the powder bed, by selective electron beam melting (SEBM). The purpose was to identify and understand the challenges of fabricating Ti-6Al-4V samples or parts from a deep powder bed (more than 200-mm deep) by SEBM and the necessity of applying post heat treatment. The resulting microstructure and mechanical properties of these Ti-6Al-4V rods were characterized along their building ( i.e., axial) direction by dividing each rod into three segments (top, middle, and bottom), both before ( i.e., as-built) and after hot isostatic pressing (HIP). The as-built microstructure of each rod was inhomogeneous; it was coarsest in the top segment, which showed a near equilibrium α- β lamellar structure, and finest in the bottom segment, which featured a non-equilibrium mixed structure. The tensile properties varied along the rod axis, especially the ductility, but all tensile properties met the requirements specified by ASTM F3001-14. HIP increased the relative density from 99.03 pct of the theoretical density (TD) to 99.90 pct TD and homogenized the microstructure thereby leading to highly consistent tensile properties along the rod axis. The temperature of the stainless steel substrate used in the powder bed was monitored. The as-built inhomogeneous microstructure is attributed to the temperature gradient in the deep powder bed. Post heat treatment is thus necessary for Ti-6Al-4V samples or parts manufactured from a deep powder bed by SEBM. This differs from the additive manufacturing of small samples or parts from a shallow powder bed (less than 100-mm deep) by SEBM.

Relative bioavailability of iron and folic acid from a new powdered supplement compared to a traditional tablet in pregnant women

PubMed Central

Hartman-Craven, Brenda; Christofides, Anna; O'Connor, Deborah L; Zlotkin, Stanley

2009-01-01

Background Deficiencies of iron and folic acid during pregnancy can lead to adverse outcomes for the fetus, thus supplements are recommended. Adherence to current tablet-based supplements is documented to be poor. Recently a powdered form of micronutrients has been developed which may decrease side-effects and thus improve adherence. However, before testing the efficacy of the supplement as an alternate choice for supplementation during pregnancy, the bioavailability of the iron needs to be determined. Our objective was to measure the relative bioavailability of iron and folic acid from a powdered supplement that can be sprinkled on semi-solid foods or beverages versus a traditional tablet supplement in pregnant women. Methods Eighteen healthy pregnant women (24 – 32 weeks gestation) were randomized to receive the supplements in a crossover design. Following ingestion of each supplement, the changes (over baseline) in serum iron and folate over 8 hours were determined. The powdered supplement contained 30 mg of iron as micronized dispersible ferric pyrophosphate with an emulsifier coating and 600 μg folic acid; the tablet contained 27 mg iron from ferrous fumarate and 1000 μg folic acid. Results Overall absorption of iron from the powdered supplement was significantly lower than the tablet (p = 0.003). There was no difference in the overall absorption of folic acid between supplements. Based on the differences in the area under the curve and doses, the relative bioavailability of iron from powdered supplement was lower than from the tablet (0.22). Conclusion The unexpected lower bioavailability of iron from the powdered supplement is contrary to previously published reports. However, since pills and capsules are known to be poorly accepted by some women during pregnancy, it is reasonable to continue to explore alternative micronutrient delivery systems and forms of iron for this purpose. Trial Registration ClinicalTrials.gov NCT00789490 PMID:19635145

First study of the evolution of the SeDeM expert system parameters based on percolation theory: Monitoring of their critical behavior.

PubMed

Galdón, Eduardo; Casas, Marta; Gayango, Manuel; Caraballo, Isidoro

2016-12-01

The deep understanding of products and processes has become a requirement for pharmaceutical industries to follow the Quality by Design principles promoted by the regulatory authorities. With this aim, SeDeM expert system was developed as a useful preformulation tool to predict the likelihood to process drugs and excipients through direct compression. SeDeM system is a step forward in the rational development of a formulation, allowing the normalisation of the rheological parameters and the identification of the weaknesses and strengths of a powder or a powder blend. However, this method is based on the assumption of a linear behavior of disordered systems. As percolation theory has demonstrated, powder blends behave as non-linear systems that can suffer abrupt changes in their properties near to geometrical phase transitions of the components. The aim of this paper was to analyze for the first time the evolution of the SeDeM parameters in drug/excipient powder blends from the point of view of the percolation theory and to compare the changes predicted by SeDeM with the predictions of Percolation theory. For this purpose, powder blends of lactose and theophylline with varying concentrations of the model drug have been prepared and the SeDeM analysis has been applied to each blend in order to monitor the evolution of their properties. On the other hand, percolation thresholds have been estimated for these powder blends where critical points have been found for important rheological parameters as the powder flow. Finally, the predictions of percolation theory and SeDeM have been compared concluding that percolation theory can complement the SeDeM method for a more accurate estimation of the Design Space. Copyright © 2016 Elsevier B.V. All rights reserved.

Geospatial data for coal beds in the Powder River Basin, Wyoming and Montana

USGS Publications Warehouse

Kinney, Scott A.; Scott, David C.; Osmonson, Lee M.; Luppens, James A.

2015-01-01

The purpose of this report is to provide geospatial data for various layers and themes in a Geographic Information System (GIS) format for the Powder River Basin, Wyoming and Montana. In 2015, as part of the U.S. Coal Resources and Reserves Assessment Project, the U.S. Geological Survey (USGS) completed an assessment of coal resources and reserves within the Powder River Basin, Wyoming and Montana. This report is supplemental to USGS Professional Paper 1809 and contains GIS data that can be used to view digital layers or themes, including the Tertiary limit of the Powder River Basin boundary, locations of drill holes, clinker, mined coal, land use and technical restrictions, geology, mineral estate ownership, coal thickness, depth to the top of the coal bed (overburden), and coal reliability categories. Larger scale maps may be viewed using the GIS data provided in this report supplemental to the page-size maps provided in USGS Professional Paper 1809. Additionally, these GIS data can be exported to other digital applications as needed by the user. The database used for this report contains a total of 29,928 drill holes, of which 21,393 are in the public domain. The public domain database is linked to the geodatabase in this report so that the user can access the drill-hole data through GIS applications. Results of this report are available at the USGS Energy Resources Program Web site,http://energy.usgs.gov/RegionalStudies/PowderRiverBasin.aspx.

The Assessment of Red Beet as a Natural Colorant, and Evaluation of Quality Properties of Emulsified Pork Sausage Containing Red Beet Powder during Cold Storage

PubMed Central

Jin, Sang-Keun; Choi, Jung-Seok; Moon, Sung-Sil; Jeong, Jin-Yeon

2014-01-01

The purpose of this study was to assess red beet as a natural colorant in emulsified pork sausage and to investigate the effect of red beet on quality characteristics of emulsified pork sausage during 20 d of cold storage. Red beet was prepared as a powder and a substitute with sodium nitrite at 0.5% and 1.0% levels in emulsified pork sausage. Red beet significantly increased the moisture content and pH (p<0.0001) and affected color traits. Lightness of emulsified pork sausage decreased by the addition of red beet powder (p<0.01), whereas lightness with red beet treatments slightly increased during 20 d of cold storage at 4℃ (p<0.05). Redness dramatically increased with red beet powder (p<0.0001). Color by sensory evaluation also showed a significant effect from red beet addition (p<0.05), whereas the other sensory properties such as flavor, tenderness, juiciness, and overall acceptability were not affected by the addition of red beet powder (p>0.05). Texture and 2-thiobabituric acid reactive substance were also not affected by red beet addition (p>0.05). Therefore, red beet could be a good natural colorant in emulsified pork sausage but it needs additional processing, such as betalain concentration and extraction as a juice, to be used as an antioxidant in meat products. PMID:26761285

Synergetic Antimicrobial Effects of Mixtures of Ethiopian Honeys and Ginger Powder Extracts on Standard and Resistant Clinical Bacteria Isolates

PubMed Central

Ewnetu, Yalemwork; Lemma, Wossenseged; Birhane, Nega

2014-01-01

Purpose. To evaluate antimicrobial effects of mixtures of Ethiopian honeys and ginger rhizome powder extracts on Staphylococcus aureus (ATCC 25923), Escherichia coli (ATCC 25922), Staphylococcus aureus (MRSA), Escherichia coli (R), and Klebsiella pneumoniae (R). Methods. Agar diffusion and broth assays were performed to determine susceptibility of these standard and resistant clinical bacteria isolates using honey-ginger powder extract mixtures. Results. Honey-ginger powder extract mixtures produced the highest mean inhibition (25.62 mm ± 2.55) compared to the use of honeys (21.63 mm ± 3.30) or ginger extracts (19.23 mm ± 3.42) individually. The ranges of inhibitions produced by honey-ginger extract mixtures on susceptible test organisms (26–30 mm) and resistant strains (range: 19–27 mm) were higher compared to 7–22 mm and 0–14 mm by standard antibiotic discs. Minimum inhibitory concentrations (MIC) of mixture of honeys-ginger extracts were 6.25% (0.625 v/mL) on the susceptible bacteria compared to 75% for resistant clinical isolates. Minimum bactericidal concentration (MBC) of honey-ginger extracts was 12.5% (0.125 g/mL) for all the test organisms. Conclusion. The result of this study showed that honey-ginger powder extract mixtures have the potential to serve as cheap source of antibacterial agents especially for the drug resistant bacteria strains. PMID:24772182

Burial, thermal, and petroleum generation history of the Upper Cretaceous Steele Member of the Cody Shale (Shannon Sandstone Bed Horizon), Powder River Basin, Wyoming (Chapter A). Bulletin

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

Nuccio, V.F.

The purposes of the study are to (1) present burial histories representative of the northwestern and southwestern parts of the Powder River Basin (south of lat 45 N.), (2) show the maximum level of thermal maturity for the Steele Member and its Shannon Sandstone Bed, and (3) show the source-rock potential and timing of petroleum generation for the Steele. It is hoped that data presented in the study will also lead to a better understanding of the burial and temperature history of the Shannon Sandstone Bed, an understanding crucial for diagenetic studies, fluid-flow modeling, and reservoir-rock characterization.

The Measurement of Protein in Powdered Milk Products and Infant Formulas: A Review and Recent Developments.

PubMed

Elgar, Dave; Evers, Jaap M; Holroyd, Stephen E; Johnson, Richard; Rowan, Angela

2016-01-01

Proteins are a key nutritional component of both powdered milk and infant formula types of product, and reliable methods for their determination are important for manufacturing and international trade. In this review, we distinguish between methods used for determining protein quality for nutrition purposes and those used for determining chemically defined protein. The former methods cover the ability of a dietary protein source to meet human nutritional requirements for the indispensable amino acids. The latter are chemical methods for the determination of total protein and can be divided into three broad types: total nitrogen determination, direct protein determination, and indirect protein determination. Current techniques and recent developments in each are reviewed.

Advances in aluminum powder usage as an energetic material and applications for rocket propellant

NASA Astrophysics Data System (ADS)

Sadeghipour, S.; Ghaderian, J.; Wahid, M. A.

2012-06-01

Energetic materials have been widely used for military purposes. Continuous research programs are performing in the world for the development of the new materials with higher and improved performance comparing with the available ones in order to fulfill the needs of the military in future. Different sizes of aluminum powders are employed to produce composite rocket propellants with the bases of Ammonium Perchlorate (AP) and Hydroxyl-Terminated-Polybutadiene (HTPB) as oxidizer and binder respectively. This paper concentrates on recent advances in using aluminum as an energetic material and the properties and characteristics pertaining to its combustion. Nano-sized aluminum as one of the most attractable particles in propellants is discussed particularly.

Physical stability of micronized powders produced by spray-freezing into liquid (SFL) to enhance the dissolution of an insoluble drug.

PubMed

Rogers, True L; Johnston, Keith P; Williams, Robert O

2003-01-01

The objective of this study was to investigate the physical stability of micronized powders produced by the spray-freezing into liquid (SFL) particle engineeringtechnology. Danazol was formulated with polyvinyl alcohol (MW 22,000), poloxamer 407, and polyvinylpyrrolidone K-15 to form a cosolvent solution that was SFL processed. The dried micronized SFL powders were sealed in glass vials with desiccant and exposed to 25 degrees C/60% RH for 3 and 6 mo, 40 degrees C/75% RH for 1, 2, 3, and 6 mo, and conditions where the temperature was cycled between -5 and +40 degrees C (6 cycles/24 hr) with constant 75% RH for 1, 2, 3 and 4 wk. The samples were characterized by using Karl-Fisher titration, differential scanning calorimetry, x-ray diffraction, specific surface area, scanning electron microscopy, and dissolution testing. Micronized SFL powders consisting of porous aggregates with small-particle domains were characterized as having high surface areas and consisted of amorphous danazol embedded within a hydrophilic excipient matrix. Karl-Fischer titration revealed no moisture absorption over the duration of the stability studies. Differential scanning calorimetry studies demonstrated high degrees of molecular interactions between danazol, PVA, poloxamer, and PVP. Scanning electron microscopy studies confirmed these interactions, especially those between danazol and poloxamer. These interactions facilitated API dissolution in the aqueous media. Powder surface area remained constant during storage at the various stability conditions, and danazol recrystallization did not occur during the entirety of the stability studies. Micronized SFL powders containing danazol dissolved rapidly and completely within 5 min in aqueous media. No differences were observed in the enhanced dissolution profiles of danazol after exposure to the storage conditions investigated. Physically stable micronized powders produced by the SFL particle engineering technology were produced for the purpose of enhancing the dissolution of an insoluble drug. The potential of the SFL particle-engineering technology as a micronization technique for enhancing the dissolution of hydrophobic drugs was demonstrated in this study. The robustness of the micronized SFL powders to withstand stressed storage conditions was shown.

Single-crystal diffraction instrument TriCS at SINQ

NASA Astrophysics Data System (ADS)

Schefer, J.; Könnecke, M.; Murasik, A.; Czopnik, A.; Strässle, Th; Keller, P.; Schlumpf, N.

2000-03-01

The single-crystal diffractometer TriCS at the Swiss Continuous Spallation Source (SINQ) is presently in the commissioning phase. A two-dimensional wire detector produced by EMBL was delivered in March 1999. The instrument is presently tested with a single detector. First measurements on magnetic structures have been performed. The instrument is remotely controlled using JAVA-based software and a UNIX DEC-α host computer.

Catalytic oxidation of toluene: comparative study over powder and monolithic manganese-nickel mixed oxide catalysts.

PubMed

Duplančić, Marina; Tomašić, Vesna; Gomzi, Zoran

2017-07-05

This paper is focused on development of the metal monolithic structure for total oxidation of toluene at low temperature. The well-adhered catalyst, based on the mixed oxides of manganese and nickel, is washcoated on the Al/Al 2 O 3 plates as metallic support. For the comparison purposes, results observed for the manganese-nickel mixed oxide supported on the metallic monolith are compared with those obtained using powder type of the same catalyst. Prepared manganese-nickel mixed oxides in both configurations show remarkable low-temperature activity for the toluene oxidation. The reaction temperature T 50 corresponding to 50% of the toluene conversion is observed at temperatures of ca. 400-430 K for the powder catalyst and at ca. 450-490 K for the monolith configuration. The appropriate mathematical models, such as one-dimensional (1D) pseudo-homogeneous model of the fixed bed reactor and the 1D heterogeneous model of the metal monolith reactor, are applied to describe and compare catalytic performances of both reactors. Validation of the applied models is performed by comparing experimental data with theoretical predictions. The obtained results confirmed that the reaction over the monolithic structure is kinetically controlled, while in the case of the powder catalyst the reaction rate is influenced by the intraphase diffusion.

Establishment of powder dustiness evaluation method by dustmeter with small amount of pharmaceutical ingredients.

PubMed

Ohta, Tomoaki; Maeda, Hiroyuki; Kubota, Ryuji; Koga, Akiko; Terada, Katsuhide

2014-09-10

The ratio of high potent materials in the new chemical entities has recently increased in the pharmaceutical industry. Generally, most of them are highly hazardous, but there is little toxicity information about the active pharmaceutical ingredients in the early development period. Even if their handling amount is quite small, the dustiness of high potent powder generated in the manufacturing process has an important impact on worker health; thus, it is important to understand the powder dustiness. The purpose of this study was to establish a method to evaluate the powder dustiness by the consumption of small amount of samples. The optimized measurement conditions for a commercially available dustmeter were confirmed using lactose monohydrate and naproxen sodium. The optimized test conditions were determined: the dustmeter mode, the flow rate, the drum rotation speed, the total measurement time, and sample loaded weight were type I mode, 4 L/min, 10 rpm, 1 min and 1-10 g , respectively. The setup conditions of the dustmeter are considerably valuable to pharmaceutical industries, especially, at the early development stage and especially for expensive materials, because the amount of air-borne dust can be evaluated with accuracy by the consumption of small amount of samples. Copyright © 2014 Elsevier B.V. All rights reserved.

Atmospheric plasma sprayed (APS) coatings of Al2O3-TiO2 system for photocatalytic application.

PubMed

Stengl, V; Ageorges, H; Ctibor, P; Murafa, N

2009-05-01

The goal of this study is to examine the photocatalytic ability of coatings produced by atmospheric plasma spraying (APS). The plasma gun used is a common gas-stabilized plasma gun (GSP) working with a d.c. current and a mixture of argon and hydrogen as plasma-forming gas. The TiO(2) powders are particles of about 100 nm which were agglomerated to a mean size of about 55 mum, suitable for spraying. Composition of the commercial powder is 13 wt% of TiO(2) in Al(2)O(3), whereas also in-house prepared powder with the same nominal composition but with agglomerated TiO(2) and conventional fused and crushed Al(2)O(3) was sprayed. The feedstock materials used for this purpose are alpha-alumina and anatase titanium dioxide. The coatings are analyzed by scanning electron microscopy (SEM), energy dispersion probe (EDS) and X-ray diffraction. Photocatalytic degradation of acetone is quantified for various coatings. All plasma sprayed coatings show a lamellar structure on cross section, as typical for this process. Anatase titania from feedstock powder is converted into rutile titania and alpha-alumina partly to gamma-alumina. Coatings are proven to catalyse the acetone decomposition when irradiated by UV rays.

Toward intradermal vaccination: preparation of powder formulations by collapse freeze-drying.

PubMed

Etzl, Elsa E; Winter, Gerhard; Engert, Julia

2014-03-01

Intradermal powder immunization is an emerging technique in vaccine delivery. The purpose of this study was to generate powder particles for intradermal injection by freeze-drying and subsequent cryo-milling. Two different freeze-drying protocols were compared, a moderate freeze-drying cycle and an aggressive freeze-drying cycle, which induced a controlled collapse of the sugar matrix. Ovalbumin served as model antigen. The influence of collapse drying and cryo-milling on particle morphology and protein stability was investigated. Cryo-milling generated irregularly shaped particles of size 20-70 µm. The recovery of soluble monomer of ovalbumin was not changed during freeze-drying and after cryo-milling, or after 12 months of storage at 2-8 °C. A slight increase in higher molecular weight aggregates was found in formulations containing the polymer dextran after 12 months of storage at 50 °C. Light obscuration measurements showed an increase in cumulative particle counts after cryo-milling that did not further increase during storage at 2-8 °C for 12 months. The applicability of the cryo-milling process to other therapeutic proteins was shown using recombinant human granulocyte-colony stimulating factor. Collapse freeze-drying and subsequent cryo-milling allows the generation of particles suitable for intradermal powder injection.

Inulin rich carbohydrates extraction from Jerusalem artichoke (Helianthus tuberosus L.) tubers and application of different drying methods.

PubMed

Rubel, Irene A; Iraporda, Carolina; Novosad, Rocio; Cabrera, Fernanda A; Genovese, Diego B; Manrique, Guillermo D

2018-01-01

In this study the operational extraction variables to obtain higher yields of inulin from Jerusalem artichoke tubers (JAT), as well as the optimal conditions to obtain a stable and dispersible powdered product by either spray or freeze drying, were studied. With this purpose, the powder yield, moisture content, water activity and flowability or products obtained by different experimental conditions were analyzed. Inulin rich carbohydrates (IRC) extraction was performed from lyophilized and ground tubers employing distilled hot water as solvent. It was proved that the solid:solvent ratio (S:S) was the critical variable in the extraction process, followed by temperature. Thus, the IRC extraction was optimal without ultrasound assistance, at 76°C, employing a S:S of 1:16, during 90min. In addition, the powder obtained by freeze-drying of the IRC extract showed advantages respect to powders obtained by spray-drying regarding the yield and considering that maltodextrin was not necessary as encapsulation agent. In another hand, spray drying process provided IRC powered materials with appropriate flow properties, and taking into account cost and time of production, this method should be considered as an alternative of freeze-drying. Copyright © 2017 Elsevier Ltd. All rights reserved.

Measurement of the differential cross sections of 6Li(d,d0) for Ion Beam Analysis purposes

NASA Astrophysics Data System (ADS)

Ntemou, E.; Aslanoglou, X.; Axiotis, M.; Foteinou, V.; Kokkoris, M.; Lagoyannis, A.; Misaelides, P.; Patronis, N.; Preketes-Sigalas, K.; Provatas, G.; Vlastou, R.

2017-09-01

In the present work, the 6Li(d,d0)6Li elastic scattering differential cross sections were measured in the energy range Ed,lab = 940-2000 keV for Elastic Backscattering Spectroscopy (EBS) purposes, using thin lithium targets, made by evaporating isotopically enriched 6LiF powder on self-supporting carbon foils, with an ultra-thin Au layer on top for normalization purposes. The experiment was carried out in deuteron beam energy steps of 20 or 30 keV and for the laboratory scattering angles of 125°, 140°, 150°, 160°, and 170°.

Infrared Extinction Coefficients of Aerosolized Conductive Flake Powders and Flake Suspensions having a Zero-Truncated Poisson Size Distribution

DTIC Science & Technology

2012-11-01

report may not be cited for purposes of advertisement . This report has been approved for public release. Acknowledgments The authors would...visible wavelengths, the eye perceives an image as a result of color contrasts that consist of differences in luminance and chromaticity (hue and

75 FR 21164 - Safety Zone; Neuse River, New Bern, NC

Federal Register 2010, 2011, 2012, 2013, 2014

2010-04-23

... other users and vessels of the waterway during a Civil War naval bombardment reenactment. DATES: This... limits of a narrow channel and the firing of black powder cannons during a Civil War naval bombardment reenactment. Basis and Purpose The City of New Bern, North Carolina is sponsoring a Civil War naval...

21 CFR 182.1711 - Silica aerogel.

Code of Federal Regulations, 2014 CFR

2014-04-01

... 21 Food and Drugs 3 2014-04-01 2014-04-01 false Silica aerogel. 182.1711 Section 182.1711 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN SERVICES (CONTINUED) SUBSTANCES GENERALLY RECOGNIZED AS SAFE Multiple Purpose GRAS Food Substances § 182.1711 Silica aerogel. (a) Product. Silica aerogel as a finely powdered...

New approach to the calculation of pistachio powder hysteresis

NASA Astrophysics Data System (ADS)

Tavakolipour, Hamid; Mokhtarian, Mohsen

2016-04-01

Moisture sorption isotherms for pistachio powder were determined by gravimetric method at temperatures of 15, 25, 35 and 40°C. A selected mathematical models were tested to determine the best suitable model to predict isotherm curve. The results show that Caurie model had the most satisfactory goodness of fit. Also, another purpose of this research was to introduce a new methodology to determine the amount of hysteresis at different temperatures by using best predictive model of isotherm curve based on definite integration method. The results demonstrated that maximum hysteresis is related to the multi-layer water (in the range of water activity 0.2-0.6) which corresponds to the capillary condensation region and this phenomenon decreases with increasing temperature.

Growth and properties of benzil doped benzimidazole (BMZ) single crystals

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

Babu, R. Ramesh, E-mail: rampap2k@yahoo.co.in; Crystal Growth and Crystallography Section, National Physical Laboratory, Krishnan Marg, New Delhi 110 012; Sukumar, M.

2010-09-15

In the present work, we have made an attempt to study the effect of benzil doping on the properties of benzimidazole single crystals. For this purpose we have grown pure and benzil doped benzimidazole single crystals by vertical Bridgman technique. The grown crystals were characterized by various characterization techniques. The presence of dopants confirmed by powder X-ray diffraction (XRD). Crystalline perfection of the grown crystals has been analysed by high-resolution X-ray diffraction (HRXRD). The transmittance, electrical property and mechanical strength have been analysed using UV-vis-NIR spectroscopic, dielectric and Vicker's hardness studies. The relative second harmonic generation efficiency of pure andmore » doped benzimidazole crystals measured using Kurtz powder test.« less

Acquisition of an X-Ray Diffractometer with WAXS and SAXS for Materials Research

DTIC Science & Technology

2015-03-31

2. This ligand is known as a sensitizer for applications in dye -sensitized solar cells, and the presence of the amino groups could potentially...achieve different surface properties, thus making them excellent candidates for use as fillers in bio-based biodegradable composite materials...These CNCs are environmentally safe sustainable, biodegradable , carbon neutral, and have low environmental, health and safety risks. Figure 9 below

A User’s Manual for Fiber Diffraction: The Automated Picker and Huber Diffractometers

DTIC Science & Technology

1990-07-01

17 3. Layer line scan of degummed silk ( Bombyx mori ) ................................. 18...index (arbitrary units) Figure 3. Layer line scan of degummed silk ( Bombyx mori ) showing layers 0 through 6. If the fit is rejected, new values for... originally made at intervals larger than 0.010. The smoothing and interpolation is done by a least-squares polynomial fit to segments of the data. The number

Bruker SMART X2S Benchtop System: A Means to Making X-Ray Crystallography More Mainstream in the Undergraduate Laboratory

ERIC Educational Resources Information Center

Guzei, Ilia A.; Hill, Nicholas J.; Zakai, Uzma I.

2010-01-01

Bruker SMART X2S is a portable benchtop diffractometer that requires only a 110 V outlet to operate. The instrument operation is intuitive and facile with an automation layer governing the workflow from behind the scenes. The user participation is minimal. At the end of an experiment, the instrument attempts to solve the structure automatically;…

Design and implementation of a multiaxial loading capability during heating on an engineering neutron diffractometer.

PubMed

Benafan, O; Padula, S A; Skorpenske, H D; An, K; Vaidyanathan, R

2014-10-01

A gripping capability was designed, implemented, and tested for in situ neutron diffraction measurements during multiaxial loading and heating on the VULCAN engineering materials diffractometer at the spallation neutron source at Oak Ridge National Laboratory. The proposed capability allowed for the acquisition of neutron spectra during tension, compression, torsion, and/or complex loading paths at elevated temperatures. The design consisted of age-hardened, Inconel(®) 718 grips with direct attachment to the existing MTS load frame having axial and torsional capacities of 100 kN and 400 N·m, respectively. Internal cooling passages were incorporated into the gripping system for fast cooling rates during high temperature experiments up to ∼1000 K. The specimen mounting couplers combined a threaded and hexed end-connection for ease of sample installation/removal without introducing any unwanted loads. Instrumentation of this capability is documented in this work along with various performance parameters. The gripping system was utilized to investigate deformation in NiTi shape memory alloys under various loading/control modes (e.g., isothermal, isobaric, and cyclic), and preliminary results are presented. The measurements facilitated the quantification of the texture, internal strain, and phase fraction evolution in NiTi shape memory alloys under various loading/control modes.

A new fast detection system at the KWS-2 high-intensity SANS diffractometer of the JCNS at MLZ - prototype test

NASA Astrophysics Data System (ADS)

Radulescu, A.; Arend, N.; Drochner, M.; Ioffe, A.; Kemmerling, G.; Ossovyi, V.; Staringer, S.; Vehres, G.; McKinny, K.; Olechnowicz, B.; Yen, D.

2016-09-01

A new detection system based on an array of 3He tubes and innovative fast detection electronics was designed and produced by GE Reuter Stokes for the high-intensity small-angle neutron scattering diffractometer KWS-2, operated by the Jülich Centre for Neutron Science (JCNS) at the Heinz Meier-Leibnitz Zentrum (MLZ). The new detector consists of a panel array of 144 3He tubes and a new fast read-out electronics. The electronics is mounted in a closed case in the backside of the 3He tubes panel array and will operate at ambient atmosphere under cooling air stream. The new detection system is composed of eighteen 8-pack modules of 3He-tubes that work independently of one another (each unit has its own processor and electronics). Knowing beforehand the performance of one detector unit and of one single tube detector is prerequisite for tuning and maximizing the performance of the complete detection system. In this paper we present the results of the tests of the prototyped 8-pack of 3He-tubes and corresponding electronics, which have been carried out at the JCNS instruments KWS-2 (in high flux conditions) and TREFF.

Design and implementation of a multiaxial loading capability during heating on an engineering neutron diffractometer

NASA Astrophysics Data System (ADS)

Benafan, O.; Padula, S. A.; Skorpenske, H. D.; An, K.; Vaidyanathan, R.

2014-10-01

A gripping capability was designed, implemented, and tested for in situ neutron diffraction measurements during multiaxial loading and heating on the VULCAN engineering materials diffractometer at the spallation neutron source at Oak Ridge National Laboratory. The proposed capability allowed for the acquisition of neutron spectra during tension, compression, torsion, and/or complex loading paths at elevated temperatures. The design consisted of age-hardened, Inconel® 718 grips with direct attachment to the existing MTS load frame having axial and torsional capacities of 100 kN and 400 N.m, respectively. Internal cooling passages were incorporated into the gripping system for fast cooling rates during high temperature experiments up to ˜1000 K. The specimen mounting couplers combined a threaded and hexed end-connection for ease of sample installation/removal without introducing any unwanted loads. Instrumentation of this capability is documented in this work along with various performance parameters. The gripping system was utilized to investigate deformation in NiTi shape memory alloys under various loading/control modes (e.g., isothermal, isobaric, and cyclic), and preliminary results are presented. The measurements facilitated the quantification of the texture, internal strain, and phase fraction evolution in NiTi shape memory alloys under various loading/control modes.

Reciprocal Space Mapping of Macromolecular Crystals in the Laboratory

NASA Technical Reports Server (NTRS)

Snell, Edward H.; Boggon, T. J.; Fewster, P. F.; Siddons, D. P.; Stojanof, V.; Pusey, M. L.

1998-01-01

The technique of reciprocal space mapping applied to the physical measurement of macromolecular crystals will be described. This technique uses a triple axis diffractometer setup whereby the monochromator is the first crystal, the sample is the second and the third crystal (of the same material as the monochromator) analyzes the diffracted beam. The geometry is such that it is possible to separate mosaic volume effects from lattice strain effects. The deconvolution of the instrument parameters will also be addressed. Results from measurements at Brookhaven National Synchrotron Radiation Source carried out on microgravity and ground-grown crystals will be presented. The required beam characteristics for reciprocal space mapping are also ideal for topographic studies and the first topographs ever recorded from microgravity protein crystal samples will be shown. We are now working on a system which will enable reciprocal space mapping, mosaicity and topography studies to be carried out in the home laboratory. This system uses a rotating anode X-ray source to provide an intense beam then a Bartels double crystal, four reflection monochromator to provide the spectral and geometric beam conditioning necessary such that the instrument characteristics do not mask the measurement. This is coupled to a high precision diffractometer and sensitive detector. Commissioning data and first results from the system will be presented.

Experience with exchange and archiving of raw data: comparison of data from two diffractometers and four software packages on a series of lysozyme crystals.

PubMed

Tanley, Simon W M; Schreurs, Antoine M M; Helliwell, John R; Kroon-Batenburg, Loes M J

2013-02-01

The International Union of Crystallography has for many years been advocating archiving of raw data to accompany structural papers. Recently, it initiated the formation of the Diffraction Data Deposition Working Group with the aim of developing standards for the representation of these data. A means of studying this issue is to submit exemplar publications with associated raw data and metadata. A recent study on the effects of dimethyl sulfoxide on the binding of cisplatin and carboplatin to histidine in 11 different lysozyme crystals from two diffractometers led to an investigation of the possible effects of the equipment and X-ray diffraction data processing software on the calculated occupancies and B factors of the bound Pt compounds. 35.3 Gb of data were transferred from Manchester to Utrecht to be processed with EVAL. A systematic comparison shows that the largest differences in the occupancies and B factors of the bound Pt compounds are due to the software, but the equipment also has a noticeable effect. A detailed description of and discussion on the availability of metadata is given. By making these raw diffraction data sets available via a local depository, it is possible for the diffraction community to make their own evaluation as they may wish.

Understanding the effect of lactose particle size on the properties of DPI formulations using experimental design.

PubMed

Guenette, Estelle; Barrett, Andrew; Kraus, Debbie; Brody, Rachel; Harding, Ljiljana; Magee, Gavin

2009-10-01

Medicines for delivering therapeutic agents to the lung as dry powders primarily consist of a carrier and a micronised active pharmaceutical ingredient (API). The performance of an inhaled formulation will depend on a number of factors amongst which the particle size distribution (PSD) plays a key role. It is suggested that increasing the number of fine particles in the carrier can improve the aerosolisation of the API. In addition the effect of PSD upon a bulk powder is also broadly understood in terms of powder flow. Other aspects of functionality that different size fractions of the carrier affect are not clearly understood; for example, it is not yet clearly known how different size fractions contribute to the different functionalities of the carrier. It is the purpose of this investigation to examine the effects of different lactose size fractions on fine particle dose, formulation stability and the ability to process and fill the material in the preferred device. In order to understand the true impact of the size fractions of lactose on the performance of dry powder inhaled (DPI) products, a statistically designed study has been conducted. The study comprised various DPI blend formulations prepared using lactose monohydrate carrier systems consisting of mixtures of four size fractions. Interactive mixtures were prepared containing 1% (w/w) salbutamol sulphate. The experimental design enabled the evaluation of the effect of lactose size fractions on processing and performance attributes of the formulation. Furthermore, the results of the study demonstrate that an experimental design approach can be used successfully to support dry powder formulation development.

A SUITABLE TRITIUM CARRIER FOR GAS DISCHARGE TUBES

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

Reifenschweiler, O.

1959-10-31

The application, especially in manufacturing processes, of radium and similar radioactive materials as priming agents in gas discharge tubes is very undesirable owing to the danger to health which they involve. To avoid this danger or to diminish it as much as possible, various attempts were made to employ tritium as a priming agent. This radioactive gas is especially suitable for this purpose because of its extremely soft beta radiation, the absence of hard gamma radiation, its high specific activity at a relatively low price, and above all its extremely high maximum permissible concentration in comparison with radium. To avoidmore » the handling of gaseous tritium, which is undesirable in manufacturing processes, the tritium is applied in a suspension of a tritiated titunium powder. On account of the small energy of the beta particles the grains of this titunium powder have to be extremely small. A powder prepared by careful milling and elutriation with grains of about 1 mu proved to be much too coarse. Only a few percent of the beta particles of the tritium then leave the titunium grains. However, by evaporation of titanium in an atmosphere of rare gases, a powder with a grain diameter of about 300 A is obtained. After absorption of the tritium by this titanium powder a suspension in an organic fluid is prepared by ultrasonic treatment. The electron-emitter surface is then very conveniently obtained by painting this suspension at the desired bremsstrahlung by means of a Geiger counter. The loss of electrons by absorption in the titanium is then only about 10%. (auth)« less

Fabrication and vibration characterization of curcumin extracted from turmeric (Curcuma longa) rhizomes of the northern Vietnam.

PubMed

Van Nong, Hoang; Hung, Le Xuan; Thang, Pham Nam; Chinh, Vu Duc; Vu, Le Van; Dung, Phan Tien; Van Trung, Tran; Nga, Pham Thu

2016-01-01

In this report, we present the research results on using the conventional method and microwave technology to extract curcuminoid from turmeric roots originated in different regions of Northern Vietnam. This method is simple, yet economical, non-toxic and still able to achieve high extraction performance to get curcuminoid from turmeric roots. The detailed results on the Raman vibration spectra combined with X-ray powder diffraction and high-performance liquid chromatography/mass spectrometry allowed the evaluation of each batch of curcumin crystalline powder sample received, under the conditions of applied fabrication technology. Also, the absorption and fluorescence spectroscopies of the samples are presented in the paper. The information to be presented in this paper: absorption and fluorescence spectroscopies of the samples; new experimental study results on applied technology to mass-produce curcumin from turmeric rhizomes; comparative study results between fabricated samples and marketing curcumin products-to state the complexity of co-existing crystalline phase in curcumin powder samples. We noticed that, it is possible to use the vibration line at ~959 cm(-1)-characteristic of the ν C=O vibration, and the ~1625 cm(-1) line-characteristic of the ν C=O and ν C=C vibration in curcumin molecules, for preliminary quality assessment of naturally originated curcumin crystalline powder samples. Data on these new optical spectra will contribute to the bringing of detailed information on natural curcumin in Vietnam, serving research purposes and applications of natural curcumin powder and nanocurcumin in Vietnam, as well as being initial materials for the pharmaceutical, cosmetics or functional food industries.

Analysis and experimental investigation of ceramic powder coating on aluminium piston

NASA Astrophysics Data System (ADS)

Pal, S.; Deore, A.; Choudhary, A.; Madhwani, V.; Vijapuri, D.

2017-11-01

Energy conservation and efficiency have always been the quest of engineers concerned with internal combustion engines. The diesel engine generally offers better fuel economy than its counterpart petrol engine. Even the diesel engine rejects about two thirds of the heat energy of the fuel, one-third to the coolant, and one third to the exhaust, leaving only about one-third as useful power output. Theoretically if the heat rejected could be reduced, then the thermal efficiency would be improved, at least up to the limit set by the second law of thermodynamics. Low Heat Rejection engines aim to do this by reducing the heat lost to the coolant. Thermal Barrier Coatings (TBCs) in diesel engines lead to advantages including higher power density, fuel efficiency, and multifuel capacity due to higher combustion chamber temperature. Using TBC can increase engine power by 8%, decrease the specific fuel consumption by 15-20% and increase the exhaust gas temperature by 200K. Although several systems have been used as TBC for different purposes, yttria stabilized zirconia with 7-8 wt.% yttria has received the most attention. Several factors playing important role in TBC life include thermal conductivity, thermo chemical stability at the service temperature, high thermo mechanical stability to the maximum service temperature and thermal expansion coefficient (TEC). This work mainly concentrates on the behaviour of three TBC powders under the same diesel engine conditions. This work finds out the best powder among yttria, alumina and zirconia to be used as a piston coating material i.e., the one resulting in lowest heat flux and low side skirt and bottom temperature has been chosen for the coating purpose. This work then analyses the coated sample for its surface properties such as hardness, roughness, corrosion resistance and microstructural study. This work aims at making it easier for the manufacturers choose the coating material for engine coating purposes and surface properties for operating them in their service period.

Exploration of geo-mineral compounds in granite mining soils using XRD pattern data analysis

NASA Astrophysics Data System (ADS)

Koteswara Reddy, G.; Yarakkula, Kiran

2017-11-01

The purpose of the study was to investigate the major minerals present in granite mining waste and agricultural soils near and away from mining areas. The mineral exploration of representative sub-soil samples are identified by X-Ray Diffractometer (XRD) pattern data analysis. The morphological features and quantitative elementary analysis was performed by Scanning Electron Microscopy-Energy Dispersed Spectroscopy (SEM-EDS).The XRD pattern data revealed that the major minerals are identified as Quartz, Albite, Anorthite, K-Feldspars, Muscovite, Annite, Lepidolite, Illite, Enstatite and Ferrosilite in granite waste. However, in case of agricultural farm soils the major minerals are identified as Gypsum, Calcite, Magnetite, Hematite, Muscovite, K-Feldspars and Quartz. Moreover, the agricultural soils neighbouring mining areas, the minerals are found that, the enriched Mica group minerals (Lepidolite and Illite) the enriched Orthopyroxene group minerals (Ferrosilite and Enstatite). It is observed that the Mica and Orthopyroxene group minerals are present in agricultural farm soils neighbouring mining areas and absent in agricultural farm soils away from mining areas. The study demonstrated that the chemical migration takes place at agricultural farm lands in the vicinity of the granite mining areas.

Bobjonesite, V4+ O (SO4) (H2O 3, a new mineral species from Temple Mountain, Emery County, Utah, U.S.A

USGS Publications Warehouse

Schindler, M.; Hawthorne, F.C.; Huminicki, D.M.C.; Haynes, P.; Grice, Joel D.; Evans, H.T.

2003-01-01

Bobjonesite, V4+ O (SO4) (H2O 3, is a new mineral species from Temple Mountain, Emery County, Utah, U.S.A. It occurs as blue-green crusts and efflorescences in fractures in a fossil (Triassic) tree: individual crystals are ??1 mm and are intimately intergrown. Bobjonesite hydrates very easily, and is unstable in all but the driest atmosphere. Its structure was determined on a crystal of bobjonesite: however, the physical properties, optical properties and X-ray powder-diffraction pattern were recorded on the synthetic equivalent, and an electron-microprobe analysis was not possible. Bobjonesite has a pale blue streak, a vitreous luster and no observable fluorescence under ultraviolet light. It has no cleavage or parting. The Mohs hardness is ???1, and the calculated density is 2.28 g/cm3. Bobjonesite is biaxial positive, with ?? 1.555(2 , ?? 1.561(1), ?? 1.574(2), 2V(obs.) = 72(1)??, 2V(calc.) = 69??; it is non-pleochroic, X = b, Y ??? 19?? (in ?? obtuse). Bobjonesite is monoclinic, space group P21/n, cell dimensions from single-crystal data: a 7.3940(5), b 7.4111(3), c 12.0597(9) A??, ?? 106.55(1)??, V 633.5(1) A??3, Z=4. The strongest seven lines in the X-ray powder-diffraction pattern [d in A??(I)(hkl)] are as follows: 5.795(100)(002), 3.498(90)(112), 3.881(48)(1??03), 5.408(37) (101), 4.571(20)(012), 6.962(11 (1??01) and 6.254(11)(011). The chemical formula was derived from crystal-structure analysis; the end-member formula is V O (SO4) (H2O)3. The crystal structure of bobjonesite was refined to an R index of 3.6% for 1105 observed (Fo> 5??F) reflections measured with an automated four-circle X-ray diffractometer using MoK?? X-radiation. There is one V site occupied by V4+ and surrounded by three O atoms and three (H2O) groups in an octahedral arrangement, with one short vanadyl bond (1.577 A??), four similar equatorial bonds (<2.022 A??), and one longer V-O bond (2.278 A??) trans to the vanadyl bond. The structure consists of isolated [V4+2 O2 (H2O)6 (SO4)2] clusters linked by hydrogen bonds.

Time-of-flight neutron powder diffraction study on the third row transition metal hexafluorides WF6, OsF6, and PtF6

NASA Astrophysics Data System (ADS)

Marx, R.; Seppelt, K.; Ibberson, R. M.

1996-05-01

A neutron diffraction study on the third-row transition metal hexafluorides MF6 (M≡W, Os, Pt) has been performed using the high resolution neutron powder diffractometer (HRPD) at the spallation source ISIS, England. The previously unknown structures of the low-temperature phases of OsF6 and PtF6 are reported. WF6, OsF6, and PtF6, which exhibit a (5dt2g)0, (5dt2g)2, and (5dt2g)4 electronic configuration, respectively, are found to be isostructural and crystallize in the UF6 structure, space group Pmnb, (No. 62). The geometry of the MF6 molecules is to good approximation octahedral for each compound, the mean M-F bond length increasing only slightly from 182.5 (W) to 185.0 (Pt). For WF6 deviations from ideal octahedral geometry are only marginally significant [181.8(2) to 183.2(2) pm] and may be interpreted on the basis of packing effects. Deviations for the d2 complex OsF6 are somewhat larger [181.5(2) to 184.4(3) pm] and may be assumed to be caused by packing effects essentially the same as for WF6, in addition to a first-order Jahn-Teller effect arising from the (5dt2g)2 electronic configuration. While eliminating the effects of packing by a comparison of individual M-F bond lengths for WF6 and OsF6, the OsF6 molecule shows to have D4h symmetry with two apical M-F bonds about 1.8 pm longer than the four equatorial bonds as a result of the Jahn-Teller distortion. Only small deviations from ideal octahedral geometry [184.4(3) to 185.8(3) pm] are found for the d4 complex PtF6. Within the series W to Pt a substantial shortening of the F...F van der Waals contact distances is observed. This shortening more than compensates for the increase in the M-F bond lengths and leads to unit cell volumes and cell parameters decreasing continuously from W to Pt. The variation of F...F contact distances and M-F bond lengths may be rationalized in terms of polarization of the F-ligands in the field of the highly charged nuclei of the central atoms which are only incompletely shielded by the 5d electrons.

Phosphide oxides RE2AuP2O (RE = La, Ce, Pr, Nd): synthesis, structure, chemical bonding, magnetism, and 31P and 139La solid state NMR.

PubMed

Bartsch, Timo; Wiegand, Thomas; Ren, Jinjun; Eckert, Hellmut; Johrendt, Dirk; Niehaus, Oliver; Eul, Matthias; Pöttgen, Rainer

2013-02-18

Polycrystalline samples of the phosphide oxides RE(2)AuP(2)O (RE = La, Ce, Pr, Nd) were obtained from mixtures of the rare earth elements, binary rare earth oxides, gold powder, and red phosphorus in sealed silica tubes. Small single crystals were grown in NaCl/KCl fluxes. The samples were studied by powder X-ray diffraction, and the structures were refined from single crystal diffractometer data: La(2)AuP(2)O type, space group C2/m, a = 1515.2(4), b = 424.63(8), c = 999.2(2) pm, β = 130.90(2)°, wR2 = 0.0410, 1050 F(2) values for Ce(2)AuP(2)O, and a = 1503.6(4), b = 422.77(8), c = 993.0(2) pm, β = 130.88(2)°, wR2 = 0.0401, 1037 F(2) values for Pr(2)AuP(2)O, and a = 1501.87(5), b = 420.85(5), c = 990.3(3) pm, β = 131.12(1)°, wR2 = 0.0944, 1143 F(2) values for Nd(2)AuP(2)O with 38 variables per refinement. The structures are composed of [RE(2)O](4+) polycationic chains of cis-edge-sharing ORE(4/2) tetrahedra and polyanionic strands [AuP(2)](4-), which contain gold in almost trigonal-planar phosphorus coordination by P(3-) and P(2)(4-) entities. The isolated phosphorus atoms and the P(2) pairs in La(2)AuP(2)O could clearly be distinguished by (31)P solid state NMR spectroscopy and assigned on the basis of a double quantum NMR technique. Also, the two crystallographically inequivalent La sites could be distinguished by static (139)La NMR in conjunction with theoretical electric field gradient calculations. Temperature-dependent magnetic susceptibility measurements show diamagnetic behavior for La(2)AuP(2)O. Ce(2)AuP(2)O and Pr(2)AuP(2)O are Curie-Weiss paramagnets with experimental magnetic moments of 2.35 and 3.48 μ(B) per rare earth atom, respectively. Their solid state (31)P MAS NMR spectra are strongly influenced by paramagnetic interactions. Ce(2)AuP(2)O orders antiferromagnetically at 13.1(5) K and shows a metamagnetic transition at 11.5 kOe. Pr(2)AuP(2)O orders ferromagnetically at 7.0 K.

Comprehensive Laboratory Evaluation of a Highly Specific Lateral Flow Assay for the Presumptive Identification of Bacillus anthracis Spores in Suspicious White Powders and Environmental Samples

PubMed Central

Ramage, Jason G.; Prentice, Kristin W.; DePalma, Lindsay; Venkateswaran, Kodumudi S.; Chivukula, Sruti; Chapman, Carol; Bell, Melissa; Datta, Shomik; Singh, Ajay; Hoffmaster, Alex; Sarwar, Jawad; Parameswaran, Nishanth; Joshi, Mrinmayi; Thirunavkkarasu, Nagarajan; Krishnan, Viswanathan; Morse, Stephen; Avila, Julie R.; Sharma, Shashi; Estacio, Peter L.; Stanker, Larry; Hodge, David R.

2016-01-01

We conducted a comprehensive, multiphase laboratory evaluation of the Anthrax BioThreat Alert® test strip, a lateral flow immunoassay (LFA) for the rapid detection of Bacillus anthracis spores. The study, conducted at 2 sites, evaluated this assay for the detection of spores from the Ames and Sterne strains of B. anthracis, as well as those from an additional 22 strains. Phylogenetic near neighbors, environmental background organisms, white powders, and environmental samples were also tested. The Anthrax LFA demonstrated a limit of detection of about 106 spores/mL (ca. 1.5 × 105 spores/assay). In this study, overall sensitivity of the LFA was 99.3%, and the specificity was 98.6%. The results indicated that the specificity, sensitivity, limit of detection, dynamic range, and repeatability of the assay support its use in the field for the purpose of qualitatively evaluating suspicious white powders and environmental samples for the presumptive presence of B. anthracis spores. PMID:27661796

Neutron and X-ray powder diffraction study of skutterudite thermoelectrics

DOE PAGES

Wang, H.; Kirkham, M. J.; Watkins, T. R.; ...

2016-02-17

N- and p-type filled-skutterudite materials prepared for thermoelectric power generation modules were analyzed by neutron diffraction at the POWGEN beam line of the Spallation Neutron Source (SNS) and X-ray diffraction (XRD). The skutterudite powders were processed by melt spinning, followed by ball milling and annealing. The n-type material consists of Ba–Yb–Co–Sb and the p-type material consists of Di–Fe–Ni–Sb or Di–Fe–Co–Sb (Di = didymium, an alloy of Pr and Nd). Powders for prototype module fabrication from General Motors and Marlow Industries were analyzed in this study. XRD and neutron diffraction studies confirm that both the n- and p-type materials have cubicmore » symmetry. Structural Rietveld refinements determined the lattice parameters and atomic parameters of the framework and filler atoms. The cage filling fraction was found to depend linearly on the lattice parameter, which in turn depends on the average framework atom size. Ultimately, this knowledge may allow the filling fraction of these skutterudite materials to be purposefully adjusted, thereby tuning the thermoelectric properties.« less

Consolidation of commercial pure aluminum particles by hot ECAP

NASA Astrophysics Data System (ADS)

Gudimetla, Kondaiah; Kumar, S. Ramesh; Ravisankar, B.; Prasad Prathipati, R.; Kumaran, S.

2018-03-01

In the current study undertaken, aluminum particles of commercial purity grade were compacted using hot ECAP. Investigation of the structural evolution and mechanical properties was done. Measurements of the densities of the samples was done for the purpose of evaluation the performance of the consolidation process. A tensile strength (UTS) of 98 MPa (after first pass) was obtained under tensile loads and the percent elongation to fracture was found to be 5.5%, which indicated good tensile strength and ductility as compared to the commercial pure Al powders consolidated by ambient temperature ECAP and other techniques. The relative density and Rockwell hardness (HRB) of compacts (after first pass) was 99% and 42 respectively. This is indisputable proof for establishing the compatibility of ECAP in the matter of producing bulk materials. Characterization of the material microstructure and fracture behavior was done through use of optical and scanning electron microscopy (SEM). The Al powders consolidated at 400°C through ECAP process, exhibited the best combination of yield strength and ductility and hence hot ECAP is suitable method for consolidation of micro powders.

Determination of Protein Content by NIR Spectroscopy in Protein Powder Mix Products.

PubMed

Ingle, Prashant D; Christian, Roney; Purohit, Piyush; Zarraga, Veronica; Handley, Erica; Freel, Keith; Abdo, Saleem

2016-01-01

Protein is a principal component in commonly used dietary supplements and health food products. The analysis of these products, within the consumer package form, is of critical importance for the purpose of ensuring quality and supporting label claims. A rapid test method was developed using near-infrared (NIR) spectroscopy as a compliment to current protein determination by the Dumas combustion method. The NIR method was found to be a rapid, low-cost, and green (no use of chemicals and reagents) complimentary technique. The protein powder samples analyzed in this study were in the range of 22-90% protein. The samples were prepared as mixtures of soy protein, whey protein, and silicon dioxide ingredients, which are common in commercially sold protein powder drink-mix products in the market. A NIR regression model was developed with 17 samples within the constituent range and was validated with 20 independent samples of known protein levels (85-88%). The results show that the NIR method is capable of predicting the protein content with a bias of ±2% and a maximum bias of 3% between NIR and the external Dumas method.

Evaluation of mechanically alloyed Cu-based powders as filler alloy for brazing tungsten to a reduced activation ferritic-martensitic steel

NASA Astrophysics Data System (ADS)

de Prado, J.; Sánchez, M.; Ureña, A.

2017-07-01

80Cu-20Ti powders were evaluated for their use as filler alloy for high temperature brazing of tungsten to a reduced activation ferritic/martensitic steel (Eurofer), and its application for the first wall of the DEMO fusion reactor. The use of alloyed powders has not been widely considered for brazing purposes and could improve the operational brazeability of the studied system due to its narrower melting range, determined by DTA analysis, which enhances the spreading capabilities of the filler. Ti contained in the filler composition acts as an activator element, reacting and forming several interfacial layers at the Eurofer-braze, which enhances the wettability properties and chemical interaction at the brazing interface. Brazing thermal cycle also activated the diffusion phenomena, which mainly affected to the Eurofer alloying elements causing in it a softening band of approximately 400 μm of thickness. However, this softening effect did not degrade the shear strength of the brazed joints (94 ± 23 MPa), because failure during testing was always located at the tungsten-braze interface.

Nanocomposite bulk of mechanically milled Al-Pb samples consolidated pore-free by the high-energy rate forming technique.

PubMed

Csanády, Agnes; Sajó, István; Lábár, János L; Szalay, András; Papp, Katalin; Balaton, Géza; Kálmán, Erika

2005-06-01

It is shown that pore-free bulk samples were produced by the high-energy rate forming axis-symmetrical powder compaction method for different application purposes in case of the very different, immiscible Al and Pb metal pair. The starting Al-Pb nanocomposites were made by mechanical milling of atomized Al and Pb powders either in a SPEX 9000 or a Fritsch Pulverisette 4 mill. Due to the conditions that milling was carried out in air, the PbO layer, originally existing at the surface of the atomized Pb powder, ruptured and was also dispersed in the composite. The presence of the nano PbO particles was proven by XRD and TEM (BF, DF, SAED). When the energy of milling was high, the PbO crystallites became so small that they could hardly be seen by XRD technique. Local distribution of the PbO nanoparticles was still visible in a TEM, using the process diffraction method. Both XRD and SAED proved to be useful for the evaluation of the results of the milling process and compaction.

Synthesis of cerium oxide (CeO 2) by co-precipitation for application as a reference material for X-ray powder diffraction peak widths

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

de Lima Batista, Anderson Márcio; Miranda, Marcus Aurélio Ribeiro; Martins, Fátima Itana Chaves Custódio

Several methods can be used to obtain, from powder diffraction patterns, crystallite size and lattice strain of polycrystalline samples. Some examples are the Scherrer equation, Williamson–Hall plots, Warren/Averbach Fourier decomposition, Whole Powder Pattern Modeling, and Debye function analysis. To apply some of these methods, it is necessary to remove the contribution of the instrument to the widths of the diffraction peaks. Nowadays, one of the main samples used for this purpose is the LaB6 SRM660b commercialized by the National Institute of Standard Technology; the width of the diffraction peak of this sample is caused only by the instrumental apparatus. However,more » this sample can be expensive for researchers in developing countries. In this work, the authors present a simple route to obtain micron-sized polycrystalline CeO 2that have a full width at half maximum comparable with the SRM660b and therefore it can be used to remove instrumental broadening.« less

Effect of dairy powders fortification on yogurt textural and sensorial properties: a review.

PubMed

Karam, Marie Celeste; Gaiani, Claire; Hosri, Chadi; Burgain, Jennifer; Scher, Joël

2013-11-01

Yogurts are important dairy products that have known a rapid market growth over the past few decades. Industrial yogurt manufacture involves different processing steps. Among them, protein fortification of the milk base is elemental. It greatly enhances yogurt nutritional and functional properties and prevents syneresis, an undesirable yogurt textural defect. Protein enrichment can be achieved by either concentration process (evaporation under vacuum and membrane processing: reverse osmosis and/or ultrafiltration) or by addition of dairy ingredients. Traditionally, skim milk powder (SMP) is used to enrich the milk base before fermentation. However, increased quality and availability of other dairy ingredients such as milk protein isolates (MPI), milk protein concentrates (MPC) whey protein isolates (WPI) and concentrates (WPC), micellar casein (MC) and caseinates have promoted their use as alternatives to SMP. Substituting different dry ingredients for skim milk powder in yogurt making affects the yogurt mix protein composition and subsequent textural and sensorial properties. This review focuses on various type of milk protein used for fortification purposes and their influence on these properties.

Enhancement of structural and magnetic properties of M-type hexaferrite permanent magnet based on synthesis temperature

NASA Astrophysics Data System (ADS)

Anjum, Safia; Sehar, Fatima; Mustafa, Zeeshan; Awan, M. S.

2018-01-01

The main purpose of this research work is to develop the single domain magnetic particles of M-type barium hexaferrite (BaFe12O19) using oxide precursors employing conventional powder metallurgy technique. The phase formation and magnetic performance of the powders and magnets will be optimized by adjusting calcination and sintering temperatures. The synthesis of M-type barium hexaferrite was carried out in two sections. A series of four samples have been prepared by initial wet mixed powders calcined at different temperatures, i.e., 750, 850, 950 and 1050 °C. On the basis of structural analysis, the sample calcined at 950 °C has been selected and further divided into four parts to sintered them at 1100, 1150, 1200 and 1250 °C. The structural measurements depict the confirmation of M-type barium hexaferrite structure. SEM micrographs show the hexagonal-shaped grains. The abrupt decrease in coercivity for the sample sintered at 1250 °C has been seen which may be due to high sintering temperature, at which the particles have multi-domain properties.

"Fiberoptic variable message signs" : Ladd Canyon - Drinking Fountain Grade Section , Old Oregon Trail Highway (Interstate 84) : final report.

DOT National Transportation Integrated Search

1995-02-01

The SYLVIA fiberoptic variable message signs (VMS) were installed on the Old Oregon Trail Highway (I-84) at milepost 263.4 near La Grande and at milepost 286.7 near North Powder. The purpose of the signs is to warn motorists of fog, winter blizzard c...

Solventless dry powder coating for sustained drug release using mechanochemical treatment based on the tri-component system of acetaminophen, carnauba wax and glidant.

PubMed

Hoashi, Yohei; Tozuka, Yuichi; Takeuchi, Hirofumi

2013-02-01

Solventless dry powder coating methods have many advantages compared to solvent-based methods: they are more economical, simpler, safer, more environmentally friendly and easier to scale up. The purpose of this study was to investigate a highly effective dry powder coating method using the mechanofusion system, a mechanochemical treatment equipped with high compressive and shearing force. Acetaminophen (AAP) and carnauba wax (CW) were selected as core particles of the model drug and coating material, respectively. Mixtures of AAP and CW with and without talc were processed using the mechanofusion system. Sustained AAP release was observed by selecting appropriate processing conditions for the rotation speed and the slit size. The dissolution rate of AAP processed with CW substantially decreased with an increase in talc content up to 40% of the amount of CW loaded. Increasing the coating amount by two-step addition of CW led to more effective coating and extended drug release. Scanning electron micrographs indicated that CW adhered and showed satisfactory coverage of the surface of AAP particles. Effective CW coating onto the AAP surface was successfully achieved by strictly controlling the processing conditions and the composition of core particles, coating material and glidant. Our mechanochemical dry powder coating method using the mechanofusion system is a simple and promising means of solventless pharmaceutical coating.

Comparative evaluation of bioactivity of crystalline trypsin for drying by Fourier-transformed infrared spectroscopy.

PubMed

Otsuka, Makoto; Fukui, Yuya; Ozaki, Yukihiro

2009-03-01

The purpose of this study was to evaluate the enzymatic stability of colloidal trypsin powder during heating in a solid-state by using Fourier transform infrared (FT-IR) spectra with chemoinformatics and generalized two-dimensional (2D) correlation spectroscopy. Colloidal crystalline trypsin powders were heated using differential scanning calorimetry. The enzymatic activity of trypsin was assayed by the kinetic degradation method. Spectra of 10 calibration sample sets were recorded three times with a FT-IR spectrometer. The maximum intensity at 1634cm(-1) of FT-IR spectra and enzymatic activity of trypsin decreased as the temperature increased. The FT-IR spectra of trypsin samples were analyzed by a principal component regression analysis (PCR). A plot of the calibration data obtained was made between the actual and predicted trypsin activity based on a two-component model with gamma(2)=0.962. On the other hand, a 2D method was applied to FT-IR spectra of heat-treated trypsin. The result was consistent with that of the chemoinformetrical method. The results for deactivation of colloidal trypsin powder by heat-treatment indicated that nano-structure of crystalline trypsin changed by heating reflecting that the beta-sheet was mainly transformed, since the peak at 1634cm(-1) decreased with dehydration. The FT-IR chemoinformetrical method allows for a solid-state quantitative analysis of the bioactivity of the bulk powder of trypsin during drying.

Analytical protocol for the sensitive determination of mannitol, sorbitol and glucose containing powders in pharmaceutical workplaces by ion chromatography using a pulsed amperometric detector.

PubMed

Butler, Owen; Forder, James; Saunders, John

2015-03-15

Workers in the pharmaceutical industry can potentially be exposed to airborne dusts and powders that can contain potent active pharmaceutical ingredients (API). Occupational hygienists and health and safety professionals need to assess and ultimately minimise such inhalation and dermal exposure risks. Containment of dusts at source is the first line of defence but the performance of such technologies needs to be verified, for which purpose the good practice guide: assessing the particulate containment performance of pharmaceutical equipment, produced by the International Society for Pharmaceutical Engineering (ISPE), is a widely used reference document. This guide recommends the use of surrogate powders that can be used to challenge the performance of such containment systems. Materials such as lactose and mannitol are recommended as their physical properties (adhesion, compactability, dustiness, flow characteristics and particle sizes) mimic those of API-containing materials typically handled. Furthermore they are safe materials to use, are available in high purity and can be procured at a reasonable cost. The aim of this work was to develop and validate a sensitive ion-chromatography based analytical procedure for the determination of surrogate powders collected on filter samples so as to meet analytical requirements set out in this ISPE guide. Crown Copyright © 2014. Published by Elsevier B.V. All rights reserved.

Chargeability measurements of selected pharmaceutical dry powders to assess their electrostatic charge control capabilities.

PubMed

Ramirez-Dorronsoro, Juan-Carlos; Jacko, Robert B; Kildsig, Dane O

2006-01-01

The purpose of this study was to develop an instrument (the Purdue instrument) and the corresponding methodologies to measure the electrostatic charge development (chargeability) of dry powders when they are in dynamic contact with stainless steel surfaces. The system used an inductive noncontact sensor located inside an aluminum Faraday cage and was optimized to measure the charging capabilities of a fixed volume of powder (0.5 cc). The chargeability of 5,5-diphenyl-hydantoin, calcium sulfate dihydrate, cimetidine, 3 grades of colloidal silicon dioxide, magnesium stearate, 4 grades of microcrystalline cellulose, salicylic acid, sodium carbonate, sodium salicylate, spray-dried lactose, and sulfinpyrazone were tested at 4 linear velocities, and the particle size distribution effect was assessed for 3 different grades of colloidal silicon dioxide and 4 different grades of microcrystalline cellulose. The chargeability values exhibited a linear relationship for the range of velocities studied, with colloidal silicon dioxide exhibiting the maximum negative chargeability and with spray-dried lactose being the only compound to exhibit positive chargeability. The instrument sensitivity was improved by a factor of 2 over the first generation version, and the electrostatic charge measurements were reproducible with relative standard deviations ranging from nondetectable to 33.7% (minimum of 3 replicates). These results demonstrate the feasibility of using the Purdue instrument to measure the electrostatic charge control capabilities of pharmaceutical dry powders with a reasonable level of precision.

Microstructure Evolution and Rapid Solidification Behavior of Blended Nickel-Based Superalloy Powders Fabricated by Laser Powder Deposition

NASA Astrophysics Data System (ADS)

Tian, Y.; Gauvin, R.; Brochu, M.

2016-07-01

Laser powder deposition was performed on a substrate of Inconel 738 using blended powders of Mar M247 and Amdry DF3 with a ratio of 4:1 for repairing purposes. In the as-deposited condition, continuous secondary phases composed of γ-Ni3B eutectics and discrete (Cr, W)B borides were observed in inter-dendritic regions, and time-dependent nucleation simulation results confirmed that (Cr, W)B was the primary secondary phase formed during rapid solidification. Supersaturated solid solution of B was detected in the γ solid solution dendritic cores. The Kurz-Giovanola-Trivedi model was performed to predict the interfacial morphology and correlate the solidification front velocity (SFV) with dendrite tip radius. It was observed from high-resolution scanning electron microscopy that the dendrite tip radius of the upper region was in the range of 15 to 30 nm, which yielded a SFV of approx 30 cm/s. The continuous growth model for solute trapping behavior developed by Aziz and Kaplan was used to determine that the effective partition coefficient of B was approximately 0.025. Finally, the feasibility of the modeling results were rationalized with the Clyne-Kurz segregation simulation of B, where Clyne-Kurz prediction using a partition coefficient of 0.025 was in good agreement with the electron probe microanalysis results.

Predicting the tensile strength of compacted multi-component mixtures of pharmaceutical powders.

PubMed

Wu, Chuan-Yu; Best, Serena M; Bentham, A Craig; Hancock, Bruno C; Bonfield, William

2006-08-01

Pharmaceutical tablets are generally produced by compacting a mixture of several ingredients, including active drugs and excipients. It is of practical importance if the properties of such tablets can be predicted on the basis of the ones for constituent components. The purpose of this work is to develop a theoretical model which can predict the tensile strength of compacted multi-component pharmaceutical mixtures. The model was derived on the basis of the Ryshkewitch-Duckworth equation that was originally proposed for porous materials. The required input parameters for the model are the relative density or solid fraction (ratio of the volume of solid materials to the total volume of the tablets) of the multi-component tablets and parameters associated with the constituent single-component powders, which are readily accessible. The tensile strength of tablets made of various powder blends at different relative density was also measured using diametrical compression. It has been shown that the tensile strength of the multi-component powder compacts is primarily a function of the solid fraction. Excellent agreement between prediction and experimental data for tablets of binary, ternary and four-component blends of some widely used pharmaceutical excipients was obtained. It has been demonstrated that the proposed model can well predict the tensile strength of multi-component pharmaceutical tablets. Thus, the model will be a useful design tool for formulation engineers in the pharmaceutical industry.

Enhancement of the Oral Bioavailability of Fexofenadine Hydrochloride via Cremophor® El-Based Liquisolid Tablets

PubMed Central

Yehia, Soad Ali; El-Ridi, Mohamed Shafik; Tadros, Mina Ibrahim; El-Sherif, Nolwa Gamal

2015-01-01

Purpose: The current work aimed to develop promising Fexofenadine hydrochloride (FXD) liquisolid tablets able to increase its oral bioavailability and shorten time to reach maximum plasma concentrations (Tmax). Methods: Eighteen liquisolid powders were developed based on 3 variables; (i) vehicle type [Propylene glycol (PG) or Cremophor® EL (CR)], (ii) carrier [Avicel® PH102] to coat [Aerosil® 200] ratio (15, 20, 25) and (iii) FXD concentration in vehicle (30, 35, 40 %, w/w). Pre-compression studies involved identification of physicochemical interactions and FXD crystallinity (FT-IR, DSC, XRD), topographic visualization (SEM) and estimation of flow properties (angle of repose, Carr’s index, Hausner’s ratio). CR-based liquisolid powders were compressed as liquisolid tablets (LST 9 – 18) and evaluated for weight-variation, drug-content, friability-percentage, disintegration-time and drug-release. The pharmacokinetics of LST-18 was evaluated in healthy volunteers relative to Allegra® tablets. Results: Pre-compression studies confirmed FXD dispersion in vehicles, conversion to amorphous form and formation of liquisolid powders. CR-based liquisolid powders showed acceptable-to-good flow properties suitable for compaction. CR-based LSTs had appropriate physicochemical properties and short disintegration times. Release profile of LST-18 showed a complete drug release within 5 min. Conclusion: LST-18 succeeded in increasing oral FXD bioavailability by 62% and reducing Tmax to 2.16 h. PMID:26819931

Pharmaceutical preparation of Saubhagya Shunthi Churna: A herbal remedy for puerperal women

PubMed Central

Shukla, Khushbu; Dwivedi, Manjari; Kumar, Neeraj

2010-01-01

Background: In the last few decades, there has been exponential growth in the field of herbal remedies. Pharmacopoeial preparations like avleha or paka (semi-solid), swarasa (expressed juice), kalka (mass), him (cold infusion) and phanta (hot infusion), kwatha (decoction) and churna (powder) form the backbone of Ayurvedic formulations. Newer guidelines for standardization, manufacture, and quality control, and scientifically rigorous research will be necessary for traditional treatments. This traditional knowledge can serve as powerful search engine that will greatly facilitate drug discovery. Purpose: The aim of the present study is to standardize Saubhagya Shunthi Paka in churna (powder) form. The powder form makes this traditional drug more stable for long-term storage and hence, easier to preserve. Materials and Methods: Saubhagya Shunthi Paka is an ayurvedic formulation containing Shunthi (Zingiber officinalis) as one of its chief ingredients. The basic preparation of this drug is a semisolid. We checked the microbial load and nutrient values (using International Standard IS and Association of Official Analytical chemists AOAC methods) Results: The powdered form of Saubhagya Shunthi Churna yielded a weight loss of approximately 17.64% of the total weight of ingredients. The total energy of Churna (calculated based on nutrient content) was found higher over Paka. Conclusion: Saubhagya Shunthi Churna may be a good therapeutic and dietary medicine for Indian women, which may be easily prepared at home. PMID:20532094

Single Crystal Diffractometry

NASA Astrophysics Data System (ADS)

Arndt, U. W.; Willis, B. T. M.

2009-06-01

Preface; Acknowledgements; Part I. Introduction; Part II. Diffraction Geometry; Part III. The Design of Diffractometers; Part IV. Detectors; Part V. Electronic Circuits; Part VI. The Production of the Primary Beam (X-rays); Part VII. The Production of the Primary Beam (Neutrons); Part VIII. The Background; Part IX. Systematic Errors in Measuring Relative Integrated Intensities; Part X. Procedure for Measuring Integrated Intensities; Part XI. Derivation and Accuracy of Structure Factors; Part XII. Computer Programs and On-line Control; Appendix; References; Index.

Unusual Thermal Stability of High-Entropy Alloy Amorphous Structure

DTIC Science & Technology

2012-06-20

incident angle X - ray diffractometer (GIAXRD, RIGAKU D/MAX2500) with Cu Kα radiation and at the incident angle of 1°. The surface morphology and...microanalyzer (EPMA, JEOL JAX-8800). The crystallographic structures of as-deposited and annealed metallic films were characterized utilizing a glancing ...field image and selected-area- diffraction (SAD) patterns of (a) 800 °C-, (b) 850 °C- and (c) 900 °C-annealed alloy thin films, respectively. Both

Boron Carbide Aluminum Cermets for External Pressure Housing Applications

DTIC Science & Technology

1992-09-01

CHEMISTRY AND MICROSTRUCTURES OF THE B4C/Al SYSTEM ......................................... 4 3.2 MECHANICAL PROPERTIES OF B4C/AI COMPOSITES ....... 10...TABLES 1. Phase chemistry of B4C/A1 composites as a function of baking temperature (by stereology) .................. ...... 10 2. Summary of the...diffractometer using CuKo radiation and a scan rate of 2° per minute. The chemistry of all phases was determined from electron microprobe analysis of

Hydrothermal synthesis and characterization of a novel supramolecular network compound of Co(NIA) 2(H 2O) 4 with molecular ladder hydrogen bond chains (NIA=nicotinate)

NASA Astrophysics Data System (ADS)

Jia, Hong-Bin; Yu, Jie-Hui; Xu, Ji-Qing; Ye, Ling; Ding, Hong; Jing, Wei-Jie; Wang, Tie-Gang; Xu, Jia-Ning; Li, Zeng-Chun

2002-10-01

By hydrothermal method, a novel supramolecular compound, Co(NIA) 2(H 2O) 4 was synthesized and its structure was characterized with elemental analysis, FT-IR spectrum, TGA and X-ray diffractometer, indicating that it is a novel polyporous supramolecule with molecular ladder hydrogen-bonded chains. TGA curve shows its thermal stability up to 520 °C.

Production of al-si alloy feedstocks using the solvent hot mixing method

NASA Astrophysics Data System (ADS)

Ni, J. Q.; Han, K. Q.; Yu, M. H.

2018-05-01

Powder injection molding is a promising low-cost technique for net shape processing of metal and ceramic components. This study aimed to investigate a new method for preparing aluminium (Al) – silicon (Si) alloy feedstock using the solvent hot mixing process. For this purpose, micron-sized Al-Si (20 wt. %) alloy powder was mixed with a binder consisting of 55 wt. % carnauba wax, 45 wt. % high-density polyethylene, and 3 wt. % stearic acid in a hot xylene bath. The scanning electron microscopy technique, thermogravimetric analysis, density measurement and torque measurements were used to verify the homogeneity of the feedstock. Moreover, the feedstock was chosen to perform the molding, debinding cycle and sintering. An Al-Si (20 wt. %) alloy part was successfully produced using this new method.

Wear and corrosion behaviour of Al2O3-TiO2 coatings produced by flame thermal projection

NASA Astrophysics Data System (ADS)

Forero-Duran, M.; Dulce-Moreno, H. J.; Ferrer-Pacheco, M.; Vargas-Galvis, F.

2017-12-01

Evaluated the wear resistance and the coatings corrosion behaviour of Al2O3-TiO2 prepared by thermal spraying by flame on AISI 1020 carbon steel substrates, previously coated with an alloy base Ni. For this purpose, were controlled parameters of thermal spraying and the use of powders of similar but different chemical composition is taken as a variable commercial reference for ceramic coating. SEM images allowed to know the morphology of the powders and coatings. Electrochemical techniques (Tafel) were applied to evaluate the protection against corrosion. Coatings were tested for wear with a tribometer configuration bola-disco. It was determined that the phases present in coatings are directly relate to the behaviour against corrosion and wear them. Keywords: wear, corrosion, thermal imaging.

Usefulness of a rotation-revolution mixer for mixing powder-liquid reline material.

PubMed

Yamaga, Yoshio; Kanatani, Mitsugu; Nomura, Shuichi

2015-01-01

The purpose of this study was to evaluate the distribution of bubbles, degree of mixing, flowability and mechanical strength of powder-liquid reline material by manually and with a rotation-revolution (planetary) mixer, and to determine the usefulness of a rotation-revolution mixer for this application. Powder-liquid reline material (Mild Rebaron, GC, Tokyo, Japan) was mixed with a powder to liquid ratio of 1:0.62 according to the manufacturer's instruction. Two methods were used to mix it: mixed by manually ("manual-mixing") and automatically with a rotation-revolution mixer (Super Rakuneru Fine, GC, Tokyo, Japan; "automatic-mixing"). Disc-shaped specimens, 30 mm in diameter and 1.0mm in thickness, were used to observe the distribution of bubbles in at 10× magnifications. Flowability tests were carried out according to the JIS T6521 for denture base hard reline materials. A three point bending test was carried out by a universal testing machine. Elastic modulus and flexural stress at the proportional limit were calculated. A median of 4 bubbles and inhomogeneous were observed in manual-mixed specimens. However, no bubbles and homogeneous were observed in automatic-mixed specimens. Flowability was within the JIS range in all mixing conditions and did not differ significantly across conditions. The elastic modulus was the same for manual-mixed and automatic-mixed specimens. On the other hand, the flexural stress at the proportional limit differed significantly between manual-mixed and automatic-mixed specimens. The results confirm that rotation-revolution mixer is useful for mixing powder-liquid reline material. Automatic-mixing may be recommended for clinical practice. Copyright © 2014 Japan Prosthodontic Society. Published by Elsevier Ltd. All rights reserved.

Effects of different blasting materials on charge generation and decay on titanium surface after sandblasting.

PubMed

Guo, Cecilia Yan; Hong Tang, Alexander Tin; Hon Tsoi, James Kit; Matinlinna, Jukka Pekka

2014-04-01

It has been reported that sandblasting titanium with alumina (Al2O3) powder could generate a negative electric charge on titanium surface. This has been proven to promote osteoblast activities and possibly osseointegration. The purpose of this pilot study was to investigate the effects of different blasting materials, in terms of the grit sizes and electro-negativity, on the generation of a negative charge on the titanium surface. The aim was also to make use of these results to deduct the underlying mechanism of charge generation by sandblasting. Together 60 c.p. 2 titanium plates were machine-cut and polished for sandblasting, and divided into 6 groups with 10 plates in each. Every plate in the study groups was sandblasted with one of the following 6 powder materials: 110µm Al2O3 grits, 50µm Al2O3 grits, 150-300µm glass beads, 45-75µm glass beads, 250µm Al powder and 44µm Al powder. The static voltage on the surface of every titanium plate was measured immediately after sandblasting. The static voltages of the titanium plates were recorded and processed using statistical analysis. The results suggested that only sandblasting with 45-75µm glass beads generated a positive charge on titanium, while using all other blasting materials lead to a negative charge. Furthermore, blasting grits of the same powder material but of different sizes might lead to different amount and polarity of the charges. This triboelectric effect is likely to be the main mechanism for charge generation through sandblasting. Copyright © 2014 Elsevier Ltd. All rights reserved.

Influence of spray drying and dispersing agent on surface and dissolution properties of griseofulvin micro and nanocrystals.

PubMed

Shah, Dhaval A; Patel, Manan; Murdande, Sharad B; Dave, Rutesh H

2016-11-01

The purpose for the current research is to compare and evaluate physiochemical properties of spray-dried (SD) microcrystals (MCs), nanocrystals (NCs), and nanocrystals with a dispersion agent (NCm) from a poorly soluble compound. The characterization was carried out by performing size and surface analysis, interfacial tension (at particle moisture interface), and in-vitro drug dissolution rate experiments. Nanosuspensions were prepared by media milling and were spray-dried. The SD powders that were obtained were characterized morphologically using scanning electron microscopy (SEM), polarized light microscopy (PLM), and Flowchem. Solid-state characterization was performed using X-ray powder diffraction (XRPD), Fourier transfer infrared spectroscopy (FT-IR), and differential scanning calorimetry (DSC) for the identification of the crystalline nature of all the SD powders. The powders were characterized for their redispersion tendency in the water and in pH 1.2. Significant differences in redispersion were noted for both the NCs in both dissolution media. The interfacial tension for particle moisture interface was determined by applying the BET (Braunauer-Emmett-Teller) equation to the vapor sorption data. No significant reduction in the interfacial tension was observed between MCs and NCs; however, a significant reduction in the interfacial tension was observed for NCm at both 25 °C and 35 °C temperatures. The difference in interfacial tension and redispersion behavior can be attributed to a difference in the wetting tendency for all the SD powders. The dissolution studies were carried out under sink and under non-sink conditions. The non-sink dissolution approach was found suitable for quantification of the dissolution rate enhancement, and also for providing the rank order to the SD formulations.

Direct laser metal deposition of WC/Co/Cr powder by means of the functionally graded materials strategy

NASA Astrophysics Data System (ADS)

Angelastro, A.; Campanelli, S. L.

2017-12-01

One of the many applications of direct laser metal deposition (DLMD) is the realization of multilayer thick coatings having particular mechanical characteristics, such as high hardness. The objective of this work was to obtain a thick, very hard and wear resistant coating, containing a high percentage of tungsten carbide (WC), on an AISI 304 stainless steel substrate. In order to achieve this result, a tungsten carbide-cobalt-chrome (WC/Co/Cr) powder was processed by the DLMD method. WC/Co/Cr is a composite widely used as a wear-resistant material for cutting tools, molds, coatings and other severe applications. Because of its high hardness, poor ductility and low thermal expansion coefficient, depositing this material directly on the stainless steel substrate is very difficult. In order to overcome this problem, the strategy of functionally graded materials (FGM) was used. Colmonoy 227-F nickel alloy was chosen for this purpose in order to generate a mixture with the WC/Co/Cr powder. Four different materials were deposited, layer by layer, by mixing Colmonoy 227-F with an increasing amount of WC/Co/Cr powders, until obtaining a thick surface coating with a maximum amount of WC of 77.4 wt%. For each powder mixture, a mathematical model was applied to calculate optimal values of translation speed and overlap percentages. A metallographic examination was performed in order to detect macro- and micro-structures of the different materials. Finally, Vickers micro-hardness was measured at various locations along the transverse section to appreciate the gradual increase of the FGM hardness, starting from the substrate and culminating at the top surface of the last deposited material.

Tolerability and pharmacokinetic profile of a sunitinib powder formulation in pediatric patients with refractory solid tumors: a Children’s Oncology Group study

PubMed Central

Shusterman, Suzanne; Reid, Joel M.; Ingle, Ashish M.; Ahern, Charlotte H.; Baruchel, Sylvain; Glade-Bender, Julia; Ivy, Percy; Adamson, Peter C.; Blaney, Susan M.

2012-01-01

Purpose Sunitinib is an oral tyrosine kinase inhibitor of VEGF, PDGF, c-KIT, and flt-3 receptors. A pediatric phase I study of sunitinib capsules identified the maximum tolerated dose as 15 mg/m2/day. This study was conducted to evaluate sunitinib given as a powder formulation. Methods Sunitinib 15 mg/m2 was administered orally daily for 4 weeks on/2 weeks off to patients <21 years old with refractory solid tumors. Sunitinib capsules were opened, and the powder sprinkled onto applesauce or yogurt. Plasma levels of sunitinib and an active metabolite, SU12662, were measured, and pharmacokinetic parameters were estimated. Results 12 patients, median age 13 (range 4–21) years, were treated. The most common first-cycle toxicities were leucopenia (n = 6), fatigue (n = 5), neutropenia (n = 4), and hypertension (n = 4). Three patients had dose-limiting toxicities (DLTs) in cycle 1 (dizziness/back pain, hand–foot syndrome, and intratumoral hemorrhage/hypoxia). A median peak plasma sunitinib concentration of 21 (range 6–36) ng/ml was reached at a median of 4 (range 4–8) h after the first dose. The median exposure (AUC0–48) was 585 (range 196–1,059) h ng/l. The median half-life was 23 (range 13–36) h. The median trough concentration measured before day 14 dosing was 32 (range 12–58) ng/ml. Conclusions The pharmacokinetic profile of sunitinib appears similar between a powder formulation and published data using capsules. The powder formulation allows patients unable to swallow capsules to receive sunitinib. PMID:22179104

The content of secondary phenol metabolites in pruned leaves of Aloe arborescens, a comparison between two methods: leaf exudates and leaf water extract.

PubMed

Gutterman, Yitzchak; Chauser-Volfson, Elena

2008-10-01

Aloe arborescens plants, originating from the deserts of South Africa, are grown in the Introduction Garden at Sede Boker in the Negev Desert of Israel. In previous studies, we developed agro-technical methods to raise the content of secondary phenol metabolites (SPhMs) in the Aloe leaves. Plants that are subjected to repeated leaf pruning respond by increasing the content of their SPhMs. The SPhMs found in Aloe arborescens include barbaloin, aloenin and derivatives of aloeresin. Such compounds are used for many purposes, including human skin protection from sun and fire burns and high radiation, as products of the pharmaceutics and cosmetics industries, and as food supplements for treating stomach ulcers and diabetes. In the current study, the SPhMs were separated from pruned leaves of the same A. arborescens plants at the same time by two methods: (1) exudation by squeezing the tissues of the leaves, (2) immersion of the leaves' pruned cut bottom in water and collection of the extract. The exudates and extract were frozen, freeze-dried to a powder and the SPhMs were then separated by chromatography. The yield of powder from water extraction from pruned leaves was much lower than the yield from the exudates. However, higher percentages of the powder from the water extraction contained SPhMs (between 80 and 92.7%). The content of powder in leaf exudates from pruned leaves was much higher because the SPhMs were squeezed out from the cells and tissues. However, the percentages of SPhMs in this powder were much lower (between 39 and 62%).

Dietary strawberry powder reduces blood glucose concentrations in obese and lean C57BL/6 mice and selectively lowers plasma C-reactive protein in lean mice

USDA-ARS?s Scientific Manuscript database

Obesity is a public health problem in the United States and is often accompanied by hyperglycemia, insulin resistance, and low grade systemic inflammation. Strawberries contain polyphenols with anti-inflammatory potential. The purpose of this study was to test the anti-inflammatory and blood gluc...

Characterization and Selection of Polymer Materials for Binary Munitions Storage. Part 3. Branch Content Determination.

DTIC Science & Technology

1987-09-01

accuracy. The data aquisition system combines a position- sensitive X-ray detector with a 65 kilobyte microcomputer capable of operating as a...The rapid X-ray diffraction system measures intensity versus 20 patterns by placing the detector with its sensitivity axis positioned parallel to the...plane of the diffractometer (see Figure 2). As shown in Figure 2, the detector sensitivity axis z is coplanar with both the incident beam and the

A brief History of Neutron Scattering at the Oak Ridge High Flux Isotope Reactor

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

Nagler, Stephen E; Mook Jr, Herbert A

2008-01-01

Neutron scattering at the Oak Ridge National Laboratory dates back to 1945 when Ernest Wollan installed a modified x-ray diffractometer on a beam port of the original graphite reactor. Subsequently, Wollan and Clifford Shull pioneered neutron diffraction and laid the foundation for an active neutron scattering effort that continued through the 1950s, using the Oak Ridge Research reactor after 1958, and, starting in 1966, the High Flux Isotope Reactor, or HFIR.

Novel Epitaxy Between Oxides and Semiconductors - Growth and Interfacial Structures

DTIC Science & Technology

2007-05-16

observed to be impressively good. 15. SUBJECT TERMS Nanotechnology, Gallium Nitride 16. SECURITY CLASSIFICATION OF: 17. LIMITATION OF ABSTRACT Same as...with precursors or gases, a high-purity sapphire was employed in this work. E-beam evaporation was used due to the high melting point of sapphire, and...were carried out on a four-circle triple -axes diffractometer, using a 12 kW rotating anode Cu K-alpha source. A pair of graphite crystals is used to

Structural studies on artificial sweeteners: itN-(4-(1-propyloxy)-phenyl)-urea

NASA Astrophysics Data System (ADS)

Hooft, Rob W. W.; Kanters, Jan A.; Kroon, Jan

1991-12-01

C 10N 2O 2H 14, M r=194.23, triclinic, itP1. At T=298 K: a=7.0292 (12), b=7.0394 (14), c=21.761 (2) Å, α=97.637 (13), β=97.326 (12), γ=96.14 (2)°, V=1050.0 (3) Å 3, Z=4, Dx=1.229 Mg m -3, λ(Cu Kα)=1.54184 Å, μ=6.7 cm -1, F(000)=416 and R=0.037 for 4268 unique observed diffractometer data (itI≥ 2.5σ(itI)). At T=100 K: a=6.8724 (4), b=6.8748 (6), c=21.773 (3) Å, α=96.680 (8), β=97.010 (7), γ=94.558 (6)°, V= 1009.5 (2) Å 3, Z=4, Dx=1.278 Mg m -3, λ(Mo Kα)=0.71073 Å, μ=0.8cm -1, F(000)=416 and R=0.056 for 3765 unique observed diffractometer data (itI≥2.5σ(itI)). At room temperature the methyl group C atoms have a high thermal motion which is possibly librational. The molecules form NH⋯0-type hydrogen-bonded networks, each oxygen accepting three hydrogen bonds. A systematic search for the so-called AH⋯B moieties which are thought to be responsible for the sweet taste revealed a number of possible candidates.

Ca-doped LTO using waste eggshells as Ca source to improve the discharge capacity of anode material for lithium-ion battery

NASA Astrophysics Data System (ADS)

Setiawan, D.; Subhan, A.; Saptari, S. A.

2017-07-01

The necessity of high charge-discharge capacity lithium-ion battery becomes very urgent due to its applications demand. Several researches have been done to meet the demand including Ca doping on Li4Ti5O12 for anode material of lithium-ion batteries. Ca-doped Li4Ti5O12 (LTO) in the form of Li4-xCaxTi5O12 (x = 0, 0.05, 0.075, and 0.1) have been synthesized using simple solid state reaction. The materials preparation involved waste eggshells in the form of CaCO3 as Ca source. The structure and capacity of as-prepared samples were characterized using X-Ray Diffractometer and Cyclic Voltametry. X-Ray Diffractometer characterization revealed that all amount of dopant had entered the lattice structure of LTO successfully. The crystalline sizes were obtained by using Scherrer equation. No significant differences are detected in lattice parameters (˜8.35 Å) and crystalline sizes (˜27 nm) between all samples. Cyclic Voltametry characterization shows that Li4-xCaxTi5O12 (x = 0.05) has highest charge-discharge capacity of 177.14 mAh/g and 181.92 mAh/g, respectively. Redox-potentials of samples show no significant differences with the average of 1.589 V.

The influence of direct compression powder blend transfer method from the container to the tablet press on product critical quality attributes: a case study.

PubMed

Teżyk, Michał; Jakubowska, Emilia; Milczewska, Kasylda; Milanowski, Bartłomiej; Voelkel, Adam; Lulek, Janina

2017-06-01

The aim of this article is to compare the gravitational powder blend loading method to the tablet press and manual loading in terms of their influence on tablets' critical quality attributes (CQA). The results of the study can be of practical relevance to the pharmaceutical industry in the area of direct compression of low-dose formulations, which could be prone to content uniformity (CU) issues. In the preliminary study, particle size distribution (PSD) and surface energy of raw materials were determined using laser diffraction method and inverse gas chromatography, respectively. For trials purpose, a formulation containing two pharmaceutical ingredients (APIs) was used. Tablet samples were collected during the compression progress to analyze their CQAs, namely assay and CU. Results obtained during trials indicate that tested direct compression powder blend is sensitive to applied powder handling method. Mild increase in both APIs content was observed during manual scooping. Gravitational approach (based on discharge into the drum) resulted in a decrease in CU, which is connected to a more pronounced assay increase at the end of tableting than in the case of manual loading. The correct design of blend transfer over single unit processes is an important issue and should be investigated during the development phase since it may influence the final product CQAs. The manual scooping method, although simplistic, can be a temporary solution to improve the results of API's content and uniformity when compared to industrial gravitational transfer.

Experiment to Capture Gaseous Products from Shock-Decomposed Materials

NASA Astrophysics Data System (ADS)

Holt, William; Mock, Willis, Jr.

2001-06-01

Recent gas gun experiments have been performed in which initially porous polytetrafluoroethylene (PTFE) powder specimens were shock compressed inside a closed steel container and soft recovered^1,2. Although a powder decomposition residue was produced in the container and analyzed in situ, no attempt was made to recover any gaseous decomposition products for analysis. The purpose of the present experiment is to extend these earlier studies to include the capture of gaseous products. The specimen container is constructed from two metal flanges and a metal gasket, held together by high-strength bolts. A cavity between the flanges contains a porous powder specimen of material to be shock-decomposed, and is connected to a gas sample cylinder via a metal tube and a valve. The system is evacuated prior to the experiment. A gas-gun-accelerated metal disk impacts the flat surface of one of the flanges. On impact, a stress wave passes through the flange and into the specimen material. If gaseous products are formed, they can be collected in the sample cylinder for subsequent analyses by mass spectrometry. Results will be presented for PTFE powder specimens. Work supported by the NSWCDD Independent Research Office. ^1W. Mock, Jr., W. H. Holt, and G. I. Kerley, in Shock Compression of Condensed Matter - 1997, S. C. Schmidt, D. P. Dandekar, and J. W. Forbes (AIP, New York, 1998), p. 671. ^2W. H. Holt, W. Mock, Jr., and F. Santiago, J. Appl. Phys. 88, 5485 (2000).

Mycelial antineoplastic activity of Agaricus blazei.

PubMed

Bertéli, Míria Benetati Delgado; Umeo, Suzana Harue; Bertéli, André; do Valle, Juliana Silveira; Linde, Giani Andrea; Colauto, Nelson Barros

2014-08-01

Basidiocarp of Agaricus blazei (=Agaricus brasiliensis; =Agaricus subrufescens) is used as teas or capsules due to its antineoplastic effect but there are few reports of using mycelium for this purpose. The objective of this study was to evaluate the antineoplastic activity on sarcoma 180 cells implanted in mice of two forms of preparation of the mycelium from two A. blazei strains grown in culture medium with different concentrations of isolated soy protein. Mycelia were grown in Pontecorvo medium with different concentrations of isolated soybean protein (ISP). Mycelial hot water extract, moistened mycelial powder, hot water extract of green tea, Ifosfamida(®) (ifosfamide drug), and saline solution were administered daily by gavage in mice with sarcoma 180 cells to evaluate antineoplastic activity. It was concluded that antineoplastic activity was the same for both strains, except when used as moistened mycelial powder, which rules out the use of mycelial powder in capsules. Mycelial hot water extract had high antineoplastic activity with lower metabolic demand on the spleen and maintenance of normal blood parameters. Mycelial growth in different ISP concentrations had the same antineoplastic activity. Also the vegetative mycelium was as effective as the basidiocarp for sarcoma 180 tumor inhibition. Green tea was as effective as mycelial hot water extract.

Lead Content of Sindoor, a Hindu Religious Powder and Cosmetic: New Jersey and India, 2014-2015.

PubMed

Shah, Manthan P; Shendell, Derek G; Strickland, Pamela Ohman; Bogden, John D; Kemp, Francis W; Halperin, William

2017-10-01

To assess the extent of lead content of sindoor, a powder used by Hindus for religious and cultural purposes, which has been linked to childhood lead poisoning when inadvertently ingested. We purchased 95 samples of sindoor from 66 South Asian stores in New Jersey and 23 samples from India and analyzed samples with atomic absorption spectrophotometry methods for lead. Analysis determined that 79 (83.2%) sindoor samples purchased in the United States and 18 (78.3%) samples purchased in India contained 1.0 or more micrograms of lead per gram of powder. For US samples, geometric mean concentration was 5.4 micrograms per gram compared with 28.1 micrograms per gram for India samples. The maximum lead content detected in both US and India samples was more than 300 000 micrograms per gram. Of the examined US sindoor samples, 19% contained more than 20 micrograms per gram of lead (US Food and Drug Administration [FDA] limit); 43% of the India samples exceeded this limit. Results suggested continued need for lead monitoring in sindoor in the United States and in sindoor carried into the United States by travelers from India, despite FDA warnings.

Retrofitting of Reinforced Concrete Beams using Reactive Powder Concrete (RPC)

NASA Astrophysics Data System (ADS)

Karthik, S.; Sundaravadivelu, Karthik

2017-07-01

Strengthening of existing damaged structures is one of the leading studies in civil engineering. The purpose of retrofitting is to structurally treat the member with an aim to restore the structure to its original strength. The focus of this project is to study the behaviour of damaged Reinforced Concrete beam retrofitted with Reactive Powder Concrete (RPC) Overlay. Reinforced concrete beams of length 1200 mm, width 100 mm and depth 200 mm were casted with M30 grade of concrete in the laboratory and cured for 28 days. One beam is taken as control and are tested under two point loading to find out ultimate load. Remaining beams are subjected to 90 % ultimate load of control beams. The partially damaged beams are retrofitted with Reactive Powder Concrete Overlay at the full tension face of the beam and side overlay depends upon the respectable retrofitting techniques with 10 mm and 20 mm thick layer to find optimum. Materials like steel fibres are added to enhance the ductility by eliminating coarse particle for homogeneity of the structure. Finally, the modes of failure for retrofitted beams are analysed experimentally under two point loading & compared the results with Control beam.

Determination of metalaxyl and identification of adjuvants in wettable powder pesticide technical formulas.

PubMed

Pose-Juan, Eva; Rial-Otero, Raquel; Martínez-Carballo, Elena; López-Periago, Eugenio; Simal-Gándara, Jesús

2009-07-01

Foliar runoff is one of the most important processes affecting off-target movement of fungicides. In this way, Ridomil Gold Plus and Ridomil Gold MZ are two types of wettable powder technical formulations which contain metalaxyl and they are used for such a purpose. A method for quantitative determination of metalaxyl in pesticide formulas has been developed, validated, and subsequently applied to Ridomil Gold Plus and Ridomil Gold MZ. The method employs liquid-liquid extraction followed by liquid chromatography coupled with UV detection (LC-UV), using gas chromatography coupled with mass spectrometry as confirmation technique and to carry out a screening of organic adjuvants of these two selected pesticide formulas. Metalaxyl of 26.5 and 41 g/kg was detected in Ridomil Gold Plus and Ridomil Gold MZ, close to the manufacture specified level of 25 and 40 g/kg, respectively. Activator and utility adjuvants were detected in these two wettable powder technical formulations. Only methyl-ester-based surfactants were found within the group of nonionic surfactants, but the long-term fates of most adjuvants in soils and elsewhere in the environment are largely unknown, partially because of the lack of long-term monitoring data.

Stability of zinc stearate under alpha irradiation in the manufacturing process of SFR nuclear fuels

NASA Astrophysics Data System (ADS)

Gracia, J.; Vermeulen, J.; Baux, D.; Sauvage, T.; Venault, L.; Audubert, F.; Colin, X.

2018-03-01

The manufacture of new fuels for sodium-cooled fast reactors (SFRs) will involve powders derived from recycling existing fuels in order to keep on producing electricity while saving natural resources and reducing the amount of waste produced by spent MOX fuels. Using recycled plutonium in this way will significantly increase the amount of 238Pu, a high energy alpha emitter, in the powders. The process of shaping powders by pressing requires the use of a solid lubricant, zinc stearate, to produce pellets with no defects compliant with the standards. The purpose of this study is to determine the impact of alpha radiolysis on this additive and its lubrication properties. Experiments were conducted on samples in contact with PuO2, as well as under external helium ion beam irradiation, in order to define the kinetics of radiolytic gas generation. The yield results relating to the formation of these gases (G0) show that the alpha radiation of plutonium can be simulated using external helium ion beam irradiation. The isotopic composition of plutonium has little impact on the yield. However, an increased yield was globally observed with increasing the mean linear energy transfer (LET). A radiolytic degradation process is proposed.

Review of Relationship Between Particle Deformation, Coating Microstructure, and Properties in High-Pressure Cold Spray

NASA Astrophysics Data System (ADS)

Rokni, M. R.; Nutt, S. R.; Widener, C. A.; Champagne, V. K.; Hrabe, R. H.

2017-08-01

In the cold spray (CS) process, deposits are produced by depositing powder particles at high velocity onto a substrate. Powders deposited by CS do not undergo melting before or upon impacting the substrate. This feature makes CS suitable for deposition of a wide variety of materials, most commonly metallic alloys, but also ceramics and composites. During processing, the particles undergo severe plastic deformation and create a more mechanical and less metallurgical bond with the underlying material. The deformation behavior of an individual particle depends on multiple material and process parameters that are classified into three major groups—powder characteristics, geometric parameters, and processing parameters, each with their own subcategories. Changing any of these parameters leads to evolution of a different microstructure and consequently changes the mechanical properties in the deposit. While cold spray technology has matured during the last decade, the process is inherently complex, and thus, the effects of deposition parameters on particle deformation, deposit microstructure, and mechanical properties remain unclear. The purpose of this paper is to review the parameters that have been investigated up to now with an emphasis on the existent relationships between particle deformation behavior, microstructure, and mechanical properties of various cold spray deposits.

Effect of milling on the plastic and the elastic stiffness of lactose particles.

PubMed

Pazesh, Samaneh; Persson, Ann-Sofie; Berggren, Jonas; Alderborn, Göran

2018-03-01

The purpose of this study was to investigate the effect of degree of disorder of a series of α-lactose monohydrate powders, prepared by milling for different time periods, on the plastic and the elastic stiffness of the particles. As references, a series of physical mixtures consisting of original crystalline particles and amorphous particles obtained by spray-drying was used. In addition, the effect of powder pre-storage humidity on the mechanical properties was investigated. For milled particles of a low degree of disorder, a decreased particle size increased the particle plastic stiffness. For milled particles of constant particle size, the plastic stiffness decreased with an increased degree of disorder while the elastic stiffness seemed nearly independent of the degree of disorder. The presence of moisture caused a recrystallisation of milled particles with low degree of disorder which increased their plastic stiffness. For the physical mixtures of crystalline and amorphous particles, similar relationships between plastic stiffness and amorphous content as for the milled powders were obtained. A reasonable explanation is that the nature of the milled particles is represented by a two-state system with crystalline and amorphous domains. Copyright © 2018 The Authors. Published by Elsevier B.V. All rights reserved.

Additive Manufacturing of Advanced High Temperature Masking Fixtures for EBPVD TBC Coating

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

List, III, Frederick Alyious; Feuerstein, Albert; Dehoff, Ryan

2016-03-30

The purpose of this Manufacturing Demonstration Facility (MDF) technical collaboration project between Praxair Surface Technologies, Inc. (PST) and Oak Ridge National Laboratory (ORNL) was to develop an additive manufacturing process to fabricate next generation high temperature masking fixtures for coating of turbine airfoils with ceramic Thermal Barrier Coatings (TBC) by the Electron Beam Physical Vapor Deposition (EBPVD) process. Typical masking fixtures are sophisticated designs and require complex part manipulation in order to achieve the desired coating distribution. Fixtures are typically fabricated from high temperature nickel (Ni) based superalloys. The fixtures are fabricated from conventional processes by welding of thin sheetmore » material into a complex geometry, to decrease the weight load for the manipulator and to reduce the thermal mass of the fixture. Recent attempts have been made in order to fabricate the fixtures through casting, but thin walled sections are difficult to cast and have high scrap rates. This project focused on understanding the potential for fabricating high temperature Ni based superalloy fixtures through additive manufacturing. Two different deposition processes; electron beam melting (EBM) and laser powder bed fusion were evaluated to determine the ideal processing route of these materials. Two different high temperature materials were evaluated. The high temperature materials evaluated were Inconel 718 and another Ni base alloy, designated throughout the remainder of this document as Alloy X, as the alloy composition is sensitive. Inconel 718 is a more widely utilized material for additive manufacturing although it is not currently the material utilized for current fixtures. Alloy X is the alloy currently used for the fixtures, but is not a commercially available alloy for additive manufacturing. Praxair determined it was possible to build the fixture using laser powder bed technology from Inconel 718. ORNL fabricated the fixture geometry using the EBM technology in order to compare deposition features such as surface roughness, geometric accuracy, deposition rate, surface and subsurface porosity, and material quality. It was determined that the laser powder bed technology was ideal for the geometry and requirements of the fixture set by Praxair, and Praxair moved forward with the purchase of a laser powder bed system. The subsequent portion of the project focused on determining the ideal processing parameters for alloy X for the laser powder bed system using ORNL’s Renishaw laser powder bed system. Praxair supplied gas atomized powders of alloy X material with properties specified by ORNL. ORNL printed text cube arrays in order to determine the ideal combination of laser powder and laser travel speed in order to maximize material density, improve surface quality, and maintain geometric accuracy. Additional powder supplied by Praxair was used to fabricate a full-scale fixture component.« less

Multivariate curve resolution applied to kinetic-spectroscopic data matrices: Dye determination in foods by means of enzymatic oxidation.

PubMed

Boeris, Valeria; Arancibia, Juan A; Olivieri, Alejandro C

2017-07-01

In this work, the combination of chemometric techniques with kinetic-spectroscopic data allowed quantifying two dyes (tartrazine and carminic acid) in complex matrices as mustard, ketchup, asparagus soup powder, pumpkin soup powder, plum jam and orange-strawberry juice. Quantitative analysis was performed without the use of tedious sample pretreatment, due to the achievement of the second-order advantage. The results obtained showed an improvement in simplicity, speed and cost with respect to usual separation techniques, allowing to properly quantifying these dyes obtaining limits of detection below 0.6mgL -1 . In addition, to the best of our knowledge, is the first time that kinetic-spectroscopic data are obtained from the action of laccase for analytical purposes. Copyright © 2017 Elsevier B.V. All rights reserved.

FLUORIDE CONTENT OF COMMERCIALLY AVAILABLE SOY MILK PRODUCTS IN THAILAND.

PubMed

Rirattanapong, Opas; Rirattanapong, Praphasri

2016-01-01

Abstract. In Thailand, the consumption of soy milk products is common but there is limited data about their fluoride content. The purpose of this study was to es- timate the fluoride content of soy milk products available in Thailand. Fluoride content was determined for 76 brands of soy milk using a F-ion-specific electrode. The fluoride concentrations ranged from 0.01 to 3.78 μg/ml. The fluoride content was not related to sugar content, soy bean content or the sterilization process. Among 3 brands of soy milk containing tea powder extract, the fluoride content was high (1.25 to 3.78 μg/ml). Most brands of soy milk tested in our study had fluoride content below the optimal daily intake but brands containing tea powder extract if consumed by children may increase their risk for fluorosis.

The Infection Dynamics of a Hypothetical Virus in a High School: Use of an Ultraviolet Detectable Powder

ERIC Educational Resources Information Center

Baltezore, Joan M.; Newbrey, Michael G.

2007-01-01

The purpose of this paper is to provide background information about the spread of viruses in a population, to introduce an adaptable procedure to further the understanding of epidemiology in the high school setting, and to show how hypothesis testing and statistics can be incorporated into a high school lab exercise. It describes a project which…

Destination Innovation: Episode 4 CheMin

NASA Image and Video Library

2012-08-02

Destination Innovation is a new series that explores the research, science and other projects underway at the NASA Ames Research Center. Episode 4 focuses on the CheMin instrument aboard the Mars Science Laboratory, NASA' s latest robotic explorer to visit Mars. CheMin, short for 'Chemistry and Mineralogy,' was developed at NASA Ames Research Center and is one of 10 instruments aboard the rover Curiosity. The instrument is an x-ray diffractometer, which will be able to identify minerals in the Martial rock and soil.

High Rate Deposition of Thick CrN and Cr2N Coatings Using Modulated Pulse Power (MPP) Magnetron Sputtering

DTIC Science & Technology

2010-12-01

in the conventional Bragg-Bentano mode. The residual stress of the coatings was measured by glancing incident angle XRD (GIXRD) in the same X - ray ...micro-analysis (EPMA), x - ray diffraction (XRD), field-emission scanning electron microscopy (FESEM), nanoindentation, scratch test, and ball-on...the coatings was determined by XRD using a SIEMENS X - ray diffractometer (Model KRISTALLOFLEX-810) operated with K-alpha Cu radiation (30 kV and 20 mA

Short review on chemical bath deposition of thin film and characterization

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

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

2016-05-06

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

New test of the dynamic theory of neutron diffraction by a moving grating

NASA Astrophysics Data System (ADS)

Zakharov, Maxim; Frank, Alexander; Kulin, German; Goryunov, Semyon

2018-04-01

Recently, multiwave dynamical theory of neutron diffraction by a moving grating was developed. The theory predicts that at a certain height of the grating profile a significant suppression of the zero-order diffraction may occur. The experiment to confirm predictions of this theory was performed. The resulting diffracted UCNs spectra were measured using time-of-flight Fourier diffractometer. The experimental data were compared with the results of numerical simulation and were found in a good agreement with theoretical predictions.

Biaxially textured articles formed by powder metallurgy

DOEpatents

Goyal, Amit; Williams, Robert K.; Kroeger, Donald M.

2003-08-05

A biaxially textured alloy article having a magnetism less than pure Ni includes a rolled and annealed compacted and sintered powder-metallurgy preform article, the preform article having been formed from a powder mixture selected from the group of ternary mixtures consisting of: Ni powder, Cu powder, and Al powder, Ni powder, Cr powder, and Al powder; Ni powder, W powder and Al powder; Ni powder, V powder, and Al powder; Ni powder, Mo powder, and Al powder; the article having a fine and homogeneous grain structure; and having a dominant cube oriented {100}<100> orientation texture; and further having a Curie temperature less than that of pure Ni.

GEODE : In situ planetary compact geochemistry facility

NASA Astrophysics Data System (ADS)

Angrilli, F.; Guizzo, G. P.; Bibring, J. P.; Fulchignoni, M.; Marinangeli, L.

2001-11-01

The purpose of this compact and miniaturised facility is to analyse the composition and physical properties of soils and rocks of the planetary surfaces. This type of assemblage would be suitable for the Mercury and Mars Scout missions (though under different environmental conditions) which require a very lightweight scientific package. In fact, ought to the very small dimensions of this facility, it can be easily allocated either inside a microrover or on a robotic arm of a lander. The scientific experiments we propose to be onboard the facility are: XMAP (x-ray diffractometer and fluorescence), MPE (magnetic properties experiment), VIRCUI (visible and infrared close-up imager). XMAP will perform mineralogical and chemical analysis directly on the sample surface. It will allow to define the textural and petro-mineralogical characteristics of the rocks and thus information of the past environment conditions. MPE will provide answers on the magnetic phase of particles and minerals which are responsible for the magnetisation of the soil. It can perform repeated measurements in different sites or generate variable field intensity and collect particles with different sizes. VIRCUI is a multifunction microscope that can perform visible and infrared analysis of the soil and at the same time it is a support for the MPE experiment; moreover VIRCUI can also be useful for the navigation of a microrover.

Degradation phenomena of magnetic attachments used clinically in the oral environment

NASA Astrophysics Data System (ADS)

Chung, Chae-Heon; Choe, Han-Cheol; Kwak, Jong-Ha

2006-08-01

The purpose of this study was to investigate the mechanisms involved in the failure of magnetic attachments used to retain dental prostheses. Dyna magnets were retrieved from dentures that had failed after 34 months of clinical use. These magnetic attachments were prepared and sectioned so as to observe the corrosion surface and layer in order to analyze the corrosion behaviors of the attachments. The corroded surface was observed under a field emission scanning electron microscope (FE-SEM) (JSM 840A, JEOL, Japan). An X-ray diffractometer (XRD) was used to analyze the corrosion product formed due to corrosion in the oral environment. Erosion-corrosion started in the uneven portion of the stainless steel cover in the magnetic attachments composed with Nd-Fe-B alloy. Corrosion was initiated on the worn stainless steel surface, followed by spalling of magnetic material due to corrosive solution. The corrosion rate increased drastically after the corrosion product caused spalling in Nd-Fe-B alloy. Corrosion initiated in the uneven stainless steel surface as well as in the welded zone. In conclusion, the failure of magnetic attachments may occur by either welding failure or breakdown of the encapsulating material. Thus, we believe that treating the surface of magnetic attachments would resolve the corrosion problem seen in magnetic attachments to some extent.

Yttria-Stabilized Zirconia Ceramic Deposition on SS430 Ferritic Steel Grown by PLD - Pulsed Laser Deposition Method

NASA Astrophysics Data System (ADS)

Khalid Rivai, Abu; Mardiyanto; Agusutrisno; Suharyadi, Edi

2017-01-01

Development of high temperature materials are one of the key issues for the deployment of advanced nuclear reactors due to higher temperature operation. One of the candidate materials for that purpose is ceramic-coated ferritic steel that one of the functions is to be a thermal barrier coating (TBC). Thin films of YSZ (Ytrria-Stabilized Zirconia) ceramic have been deposited on a SS430 ferritic steel using Pulsed Laser Deposition (PLD) at Center For Science and Technology of Advanced Materials laboratory - National Nuclear Energy Agency of Indonesia (BATAN). The thin film was deposited with the chamber pressure range of 200-225 mTorr, the substrate temperature of 800oC, and the number of laser shots of 3×104, 6×104 and 9×104. Afterward, the samples were analyzed using Scanning Electron Microscope - Energy Dispersive X-ray Spectroscope (SEM-EDS), X-Ray Diffractometer (XRD), Atomic Force Microscope (AFM) and Vickers hardness tester. The results showed that the YSZ could homogeneously and sticky deposited on the surface of the ferritic steel. The surfaces were very smoothly formed with the surface roughness was in the range of 70 nm. Furthermore, thickness, composition of Zr4+ dan Y3+, the crystallinity, and hardness property was increased with the increasing the number of the shots.

Synthesis and luminescence properties of Sm3+ doped CaTiO3 nanophosphor for application in white LED under NUV excitation.

PubMed

Shivaram, M; Nagabhushana, H; Sharma, S C; Prashantha, S C; Daruka Prasad, B; Dhananjaya, N; Hari Krishna, R; Nagabhushana, B M; Shivakumara, C; Chakradhar, R P S

2014-07-15

CaTiO3:Sm(3+) (1-11 mol%) nanophosphors were successfully synthesized by a low temperature solution combustion method [LCS]. The structural and morphological properties of the phosphors were studied by using Powder X-ray diffractometer (PXRD), Fourier transform infrared (FTIR), X-ray photo electron spectroscopy (XPS), scanning electron microscope (SEM) and transmission electron microscopy (TEM). TEM studies indicate that the size of the phosphor is ∼20-35 nm. Photoluminescence (PL) properties of Sm(3+) (1-11 mol%) doped CaTiO3 for NUV excitation (407 nm) was studied in order to investigate the possibility of its use in White light emitting diode (WLED) applications. The emission spectra consists of intra 4f transitions of Sm(3+), such as (4)G5/2→(6)H5/2 (561 nm), (4)G5/2→(6)H7/2 (601-611 nm), (4)G5/2→(6)H9/2 (648 nm) and (4)G5/2→(6)H11/2 (703 nm) respectively. Further, the emission at 601-611 nm show strong orange-red emission and can be applied to the orange-red emission of phosphor for the application for near ultra violet (NUV) excitation. Thermoluminescence (TL) of the samples irradiated with gamma source in the dose range 100-500 Gy was recorded at a heating rate of 5°Cs(-1). Two well resolved glow peaks at 164°C and 214°C along with shouldered peak at 186°C were recorded. TL intensity increases up to 300 Gy and thereafter, it decreases with further increase of dose. The kinetic parameters namely activation energy (E), frequency factor (s) and order of kinetics were estimated and results were discussed in detail. Copyright © 2014 Elsevier B.V. All rights reserved.

Calcio-olivine γ-Ca2SiO4: I. Rietveld refinement of the crystal structure

NASA Astrophysics Data System (ADS)

Gobechiya, E. R.; Yamnova, N. A.; Zadov, A. E.; Gazeev, V. M.

2008-05-01

The structure of the natural mineral calcio-olivine (γ-Ca2SiO4) found in skarn xenoliths in the region of the Lakargi Mountain (North Caucasus, Kabardino-Balkaria, Russia) is refined by the Rietveld method [ a = 5.07389(7) Å, b = 11.21128(14) Å, c = 6.75340(9) Å, V = 384.170(5) Å3, Z = 4, ρcalcd = 2.98 g/cm3, space group Pbnm]. The X-ray diffraction pattern of a powdered sample is recorded on a STOE STADI MP diffractometer [λCu K α1; Ge(111) primary monochromator; 6.00° < 2θ < 100.88°; step width, 2.5° in 2θ; number of reflections, 224]. All calculations are performed with the WYRIET (version 3.3) software package. The structural model is refined in the anisotropic approximation to R p = 6.44, R wp = 8.52, R exp = 5.85, R B = 4.98, R F = 6.90, and s = 1.46. It is shown that the sample under investigation is a mixture of several mineral phases, among which calcio-olivine (the natural analogue of the γ-Ca2SiO4 compound) (83%), hillebrandite (13%), and wadalite (4%) are dominant. Only the scale factors and the unit cell parameters are refined for hillebrandite Ca2SiO3(OH)2 [ a = 3.63472(16) Å, b = 16.4140(10) Å, c = 11.7914(8) Å, space group Cmc21, Z = 6] and wadalite Ca6Al5Si2O16Cl3 ( a = 12.0088 Å, space group, I bar 4 3 d Z = 4). The results of the structure refinement of the main component of the sample confirm that the mineral calcio-olivine is isostructural to the synthetic compound γ-Ca2SiO4. The structure of this compound is formed by the heteropolyhedral framework composed of Ca octahedra joined together into olivine-like ribbons and isolated Si tetrahedra.

Ternary aurides La4In3Au10 and Yb4In3Au10 and platinide U4In3Pt10 with ordered Zr7Ni10 type structure

NASA Astrophysics Data System (ADS)

Muts, Ihor; Kharkhalis, Anton; Hlukhyy, Viktor; Kaczorowski, Dariusz; Rodewald, Ute Ch.; Pöttgen, Rainer; Zaremba, Vasyl` I.

2017-09-01

The ternary aurides La4In3Au10 and Yb4In3Au10 and the platinide U4In3Pt10 with ordered Zr7Ni10 type structure were synthesized from the elements by induction-melting in sealed tantalum tubes or via arc-melting. The polycrystalline samples were characterized by powder X-ray diffraction and the structures were refined from single crystal X-ray diffractometer data: Cmce, a = 1426.7(3), b = 1020.3(2), c = 1025.2(2) pm, wR2 = 0.0441, 1510 F2 values, 46 variables for La4In3Au10, a = 1361.5(3), b = 998.3(2), c = 1007.8(2), wR2 = 0.0804, 1404 F2 values, 46 variables for Yb4In3Au10 and a = 1344.4(3), b = 973.9(2), c = 978.9(2), wR2 = 0.0922, 741 F2 values, 48 variables for U4.15In3.03Pt9.82 (with small degrees of In/U, respectively Pt/In mixing on Wyckoff sites 4a and 8 f). The La4In3Au10, Yb4In3Au10 and U4In3Pt10 structures contain pronounced two-dimensional gold, respectively platinum substructures which are filled and condensed by two crystallographically independent indium and rare earth atoms. The crystal chemical features clearly classify these intermetallics as aurides and platinides. The physical properties of U4In3Pt10 were characterized by means of magnetic and electrical transport measurements. The compound exhibits metallic conductivity and shows no magnetic ordering down to 1.72 K. Its magnetic behavior is governed by hybridization between 5f and ligand electrons that results in significant delocalization of the 5f states.

Transmission X-ray Diffraction (XRD) Patterns Relevant to the MSL Chemin Amorphous Component: Sulfates And Silicates

NASA Technical Reports Server (NTRS)

Morris, R. V.; Rampe, E. B.; Graff, T. G.; Archer, P. D., Jr.; Le, L.; Ming, D. W.; Sutter, B.

2015-01-01

The Mars Science Laboratory (MSL) CheMin instrument on the Curiosity rover is a transmission X-ray diffractometer (Co-Kalpha radiation source and a approx.5deg to approx.52deg 2theta range) where the analyzed powder samples are constrained to have discrete particle diameters <150 microns by a sieve. To date, diffraction patterns have been obtained for one basaltic soil (Rocknest (RN)) and four drill fines of coherent rock (John Klein (JK), Cumberland (CB), Windjana (WJ), and Confidence Hills (CH)). The CheMin instrument has detected and quantified the abundance of both primary igneous (e.g., feldspar, olivine, and pyroxene) and secondary (e.g., Ca-sulfates, hematite, akaganeite, and Fe-saponite) minerals. The diffraction patterns of all CheMin samples are also characterized by a broad diffraction band centered near 30deg 2theta and by increasing diffraction intensity (scattering continuum) from approx.15deg to approx.5deg, the 2theta minimum. Both the broad band and the scattering continuum are attributed to the presence of an XRD amorphous component. Estimates of amorphous component abundance, based on the XRD data itself and on mass-balance calculations using APXS data crystalline component chemistry derived from XRD data, martian meteorites, and/or stoichiometry [e.g., 6-9], range from approx.20 wt.% to approx.50 wt.% of bulk sample. The APXSbased calculations show that the amorphous component is rich in volatile elements (esp. SO3) and is not simply primary basaltic glass, which was used as a surrogate to model the broad band in the RN CheMin pattern. For RN, the entire volatile inventory (except minor anhydrite) is assigned to the amorphous component because no volatile-bearing crystalline phases were reported within detection limits [2]. For JK and CB, Fesaponite, basanite, and akaganeite are volatile-bearing crystalline components. Here we report transmission XRD patterns for sulfate and silicate phases relevant to interpretation of MSL-CheMin XRD amorphous components.

Pre-melting Behaviour in fcc Metals

NASA Astrophysics Data System (ADS)

Pamato, M. G.; Wood, I. G.; Dobson, D. P.; Hunt, S.; Vocadlo, L.

2016-12-01

Although the Earth's core is accepted to be made of an iron-nickel alloy with a few percent of light elements, its exact structure and composition are still unknown. Seismological and mineralogical models in the Earth's inner core do not agree, with mineralogical models derived from ab initiocalculations predicting shear-wave velocities up to 30% greater than seismically observed values. Recent computer simulations revealed that such difference may be explained by a dramatic, non-linear, softening of the elastic constants of Fe prior to melting. Up to date, computer calculations are the only result on pre-melting of direct applicability to the Earth's core and it is essential to systematically investigate such phenomena at inner core pressures and temperatures. Measuring the pressure dependence of pre-melting effects at such conditions and to the required precision is however extremely challenging. Also, pre-melting effects have been observed or suggested to occur in other materials, particularly noble metals, which exhibit large departures from linearity (modulus defects) at elevated temperatures. The aim of this study is to investigate to what extent pre-melting behaviour occurs in the physical properties of other metals at more experimentally tractable conditions. In particular, we report measurements of density and thermal expansion coefficients of both pure and alloyed gold (Au) up to their melting points. Au is an ideal test material since it crystallises in a simple monatomic face-centred structure and has a relatively low melting temperature. Precise measurements of unit cell lattice parameters were performed using a PANalytical X'Pert Pro powder diffractometer, equipped with an incident beam monochromator (giving very high resolution diffraction patterns) and with environmental stages covering the range from 40 K to 1373 K, with a readily achievable temperature resolution of 1K. We will discuss the circumstances under which pre-melting occurs, its mechanism(s), the effect of impurities and defects in the solid, and the consequences of pre-melting in the Earth's core.

[Effect of three kinds of rare earth oxides on chromaticity and mechanical properties of zirconia ceramic].

PubMed

Huang, Hui; Zhang, Fu-qiang; Sun, Jing; Gao, Lian

2006-06-01

To evaluate the colouration of zirconia ceramic by adding three kinds of rare earth oxides. The influence of the pigments concentration on the mechanical properties and the microstructure was also analyzed. Added different concentrations of CeO(2), Er(2)O(3) and Pr(6)O(11) in tetragonal zirconia poly crystals stabilized with 3 mol% yttria (3Y-T2P) powder, compacted at 200 MPa using cold isostatic pressure, and sintered to 1 400 degrees C. The heating rate was 150 degrees C/h and the dwelling time was 2 hours. The chromaticity of sintered bodies was measured with chroma meter. The relative density, hardness, flexure strength and fracture toughness were investigated as well. The phase stability of the colorized and pure zirconia was evaluated by X-ray diffraction (XRD) using an automated diffractometer. The microstructures of the specimens were evaluated by scanning electron microscope (SEM). Several kinds of color achieved by the different pigments praseodym oxide, cerium oxide and erbium oxide were presented in the CIELab system. The a* value increased with the added amount of Er(2)O(3), while b* value rose with the increasing amount of CeO(2) and Pr(6)O(11). However, three pigments failed to decrease L* value and the sintered body appeared too bright. Adding three pigments influenced flexure strength of zirconia ceramic significantly, but had little influence on the hardness and fracture toughness. Microscopy revealed the relationship between the porosity and shapes of grains was correlated to strength of the diphase ceramics. No additional phase could be detected by XRD, except t-ZrO(2) in all colorized samples after sintering at 1 400 degrees C for 120 min. Zirconia ceramic can be colorized by CeO(2), Er(2)O(3), and Pr(6)O(11). Pigments even in a small amount influence the mechanical properties of the colorized zirconia material, which necessitates further investigation.

Sol-Gel Synthesis of Fe-Doped TiO2 Nanocrystals

NASA Astrophysics Data System (ADS)

Marami, Mohammad Bagher; Farahmandjou, Majid; Khoshnevisan, Bahram

2018-03-01

Fe-doped TiO2 powders were synthesized by the sol-gel method using titanium (IV) isopropoxide (TTIP) as the starting material, ethanol as solvent, and ethylene glycol (EG) as stabilizer. These prepared samples were characterized by x-ray diffractometer (XRD), field emission scanning electron microscope (FESEM), Fourier-transform infrared (FTIR) spectroscopy, diffuse reflection spectroscopy (DRS), energy-dispersive x-ray spectroscopy (EDX), and photoluminescence (PL) analyses to study their structure, morphology, and optical properties. The particle size of Fe-doped TiO2 was in the range of 18-39 nm and the minimum crystallite size was achieved for 4 mol.% of Fe. The XRD result of the samples that were doped with Fe showed a tetragonal structure. It also revealed the coexistence of the anatase and rutile phases, and showed that their ratio changed with various molar concentrations of Fe dopant. FTIR spectroscopy showed the presence of the Ti-O vibration band in the samples. PL analysis revealed the PL property in the UV region. Visible irradiation and the intensity of PL spectra were both reduced by doping TiO2 with 3 mol.% of Fe as compared to the pure variety. The spectra from the DRS showed a red shift and a reduction of 2.6 eV in the band gap energy for 4 mol.% Fe-doped TiO2. The optimum level of impurity (4 mol.%) for Fe-doped TiO2 nanoparticles (NPs), which improve the optical and electrical properties by using new precursors and can be used in solar cells and electronic devices, was determined. The novelty of this work consists of: the Fe/TiO2 NPs are synthesized by new precursors from sol-gel synthesis of iron and TTIP using acetic acid-catalyzed solvolysis (original idea) and the optical properties optimized with a mixture of phases (anatase/rutile) of Fe-doped TiO2 by this facile method.

The investigation of MCM-48-type and MCM-41-type mesoporous silica as oral solid dispersion carriers for water insoluble cilostazol.

PubMed

Wang, Yanzhu; Sun, Lizhang; Jiang, Tongying; Zhang, Jinghai; Zhang, Chen; Sun, Changshan; Deng, Yihui; Sun, Jin; Wang, Siling

2014-06-01

To explore the suitable application of MCM-41 (Mobil Composition of Matter number forty-one)-type and MCM-48-type mesoporous silica in the oral water insoluble drug delivery system. Cilostazol (CLT) as a model drug was loaded into synthesized MCM-48 (Mobil Composition of Matter number forty-eight) and commercial MCM-41 by three common methods. The obtained MCM-41, MCM-48 and CLT-loaded samples were characterized by means of nitrogen adsorption, thermogravimetric analysis, ultraviolet-visible spectrophotometry, scanning electron microscopy, transmission electron microscopy, differential scanning calorimetry and powder X-ray diffractometer. It was found that solvent evaporation method was preferred according to the drug loading efficiency and the maximum percent cumulative drug dissolution. MCM-48 with 3D cubic pore structure and MCM-41 with 2D long tubular structure are nearly spherical particles in 300-500 nm. Nevertheless, the silica carriers with similar large specific surface areas and concentrating pore size distributions (978.66 m(2)/g, 3.8 nm for MCM-41 and 1108.04 m(2)/g, 3.6 nm for MCM-48) exhibited different adsorption behaviors for CLT. The maximum percent cumulative drug release of the two CLT/silica solid dispersion (CLT-MCM-48 and CLT-MCM-41) was 63.41% and 85.78% within 60 min, respectively; while in the subsequent 12 h release experiment, almost 100% cumulative drug release were both obtained. In the pharmacokinetics aspect, the maximum plasma concentrations of CLT-MCM-48 reached 3.63 mg/L by 0.92 h. The AUC0-∞ values of the CLT-MCM-41 and CLT-MCM-48 were 1.14-fold and 1.73-fold, respectively, compared with the commercial preparation. Our findings suggest that MCM-41-type and MCM-48-type mesoporous silica have great promise as solid dispersion carriers for sustained and immediate release separately.

Deposition, Alteration, and Resuspension of Colorado River Delta Sediments, Lake Powell, Utah

NASA Astrophysics Data System (ADS)

Kramer, N. M.; Parnell, R.

2002-12-01

Current drought conditions in the southwest United States have resulted in lowering water levels in Lake Powell, Utah. Delta sediments forming at the Colorado River inflow for the past 39 years are becoming exposed and reworked as lake levels continue to fall to over 22 meters below full pool level. Fine sediments act as a sink for pollutants by adsorbing contaminants to their surfaces. Reworking these sediments may pose a risk to water quality in the lake. We examine whether burial and time have sufficiently altered fine sediments in the delta and affected materials adsorbed on their surfaces. Fifteen lake cores and six sediment traps were collected from the sediment delta forming at the Colorado River inflow in Lake Powell. This research characterizes fine sediment mineralogy, the composition of exchangeable materials, and organic matter content within delta sediments to determine the type and amount of alteration of these sediments with cycles of burial and resuspension. We hypothesize that as sediments are reworked, organic carbon is degraded and organic nitrogen is released forming ammonium in these reducing conditions. Sediment trap samples will be used to test this hypothesis. Trap samples will be compared to subsamples from sediment cores to determine the amount of alteration of fine sediments. All samples are analyzed for organic carbon, organic nitrogen, ammonium, cation exchange capacity, exchangeable cation composition, and clay mineralogy. Organic carbon and nitrogen are analyzed using a Leco CN analyzer. Ammonium is analyzed using a Lachet ion chromatograph. Clay mineralogy is characterized using a Siemens D500 powder X-ray diffractometer. Cation exchange capacity and exchangeable cations are measured using standard soil chemical techniques. Clay mineral analyses indicate significant spatial and temporal differences in fine sediment entering the Lake Powell delta which complicates the use of a simple deposition/alteration/resuspension model using a single starting material.

Sol-Gel Synthesis of Fe-Doped TiO2 Nanocrystals

NASA Astrophysics Data System (ADS)

Marami, Mohammad Bagher; Farahmandjou, Majid; Khoshnevisan, Bahram

2018-07-01

Fe-doped TiO2 powders were synthesized by the sol-gel method using titanium (IV) isopropoxide (TTIP) as the starting material, ethanol as solvent, and ethylene glycol (EG) as stabilizer. These prepared samples were characterized by x-ray diffractometer (XRD), field emission scanning electron microscope (FESEM), Fourier-transform infrared (FTIR) spectroscopy, diffuse reflection spectroscopy (DRS), energy-dispersive x-ray spectroscopy (EDX), and photoluminescence (PL) analyses to study their structure, morphology, and optical properties. The particle size of Fe-doped TiO2 was in the range of 18-39 nm and the minimum crystallite size was achieved for 4 mol.% of Fe. The XRD result of the samples that were doped with Fe showed a tetragonal structure. It also revealed the coexistence of the anatase and rutile phases, and showed that their ratio changed with various molar concentrations of Fe dopant. FTIR spectroscopy showed the presence of the Ti-O vibration band in the samples. PL analysis revealed the PL property in the UV region. Visible irradiation and the intensity of PL spectra were both reduced by doping TiO2 with 3 mol.% of Fe as compared to the pure variety. The spectra from the DRS showed a red shift and a reduction of 2.6 eV in the band gap energy for 4 mol.% Fe-doped TiO2. The optimum level of impurity (4 mol.%) for Fe-doped TiO2 nanoparticles (NPs), which improve the optical and electrical properties by using new precursors and can be used in solar cells and electronic devices, was determined. The novelty of this work consists of: the Fe/TiO2 NPs are synthesized by new precursors from sol-gel synthesis of iron and TTIP using acetic acid-catalyzed solvolysis (original idea) and the optical properties optimized with a mixture of phases (anatase /rutile) of Fe-doped TiO2 by this facile method.

[Evaluation of antioxidant properties of enriched bakery products in experiment on laboratory animals].

PubMed

Nilova, L P; Pilipenko, T V

2016-01-01

The purpose was to study the effect of enriched bakery products in the diet of rats on indicators of prooxidant-antioxidant system of blood serum. Experiment was carried out on male Wistar rats with initial weight 140-180 g. After a quarantine during the preparatory period rats for 14 days were accustomed to the partial (50%) replacement of the standard diet by bakery products with standard compound­ing. Then, 7 groups of rats were formed: the 1st group of rats (control group, n=10) continued to receive bakery products of a standard composition; groups with the 2nd on 7th (experimental, n=8 in everyone) received enriched bakery products: the 2nd group - with blueberry powder; the 3rd group - with mountain ash powder; the 4th group - with sea-buckthorn powder; the 5th group - with flour of a pine nut; the 6th group - with rice bran oil; the 7th group - with pumpkin oil. The intensity of free radical oxidation and antioxidant activity (by chemiluminescence method), activity of superoxide dismutase and level of secondary oxidation products reacted with thiobarbituric acid (by spectrophotometry) were monitored in rat blood serum. It has been shown that the use of bakery products with different compounding in the animal diet had different effects on indicators of prooxidant-antioxidant system of blood serum. Bakery products containing sea buckthorn pomace powder, flour of pine nut and rice bran oil reduced intensity of free radical oxidation in rat blood serum by 36.0, 24.6 and 18.8%, respectively. It is suggested that bakery products containing flour of pine nut products brake a free radical oxidation in rat blood serum in case of simultaneous content of natural antioxidants and melanoidins. The anthocyanins of powder from blueberry berries can render antioxidant effect and slow down formation of by-products of oxidation. No statistically significant change on indicators of prooxidant-antioxidant system of blood serum of rats treated with bakery products with rowan powder or pumpkin oil was found, that may be due to animal refusal to eat such products.

Effect of layered manufacturing techniques, alloy powders, and layer thickness on metal-ceramic bond strength.

PubMed

Ekren, Orhun; Ozkomur, Ahmet; Ucar, Yurdanur

2018-03-01

Direct metal laser sintering (DMLS) and direct metal laser melting (DMLM) have become popular for fabricating the metal frameworks of metal-ceramic restorations. How the type of layered manufacturing device, layer thickness, and alloy powder may affect the bond strength of ceramic to metal substructure is unclear. The purpose of this in vitro study was to evaluate the bond strength of dental porcelain to metal frameworks fabricated using different layered manufacturing techniques (DMLS and DMLM), Co-Cr alloy powders, and layer thicknesses and to evaluate whether a correlation exists between the bond strength and the number of ceramic remnants on the metal surface. A total of 75 bar-shaped metal specimens (n=15) were fabricated using either DMLS or DMLM. The powder alloys used were Keramit NP-S and EOS-Cobalt-Chrome SP-2 with layer thicknesses of 20 μm and 30 μm. After ceramic application, the metal-ceramic bond strength was evaluated with a 3-point-bend test. Three-way ANOVA followed by the Tukey honest significance difference test were used for statistical analysis (α=.05). De-bonding surface microstructure was observed with scanning electron microscopy. Energy dispersive spectroscopy analysis was conducted to evaluate the correlation between ceramic remnants on the metal surface and bond strength values. The mean bond strength value of DMLS was significantly higher than that of DMLM. While no statistically significant difference was found between layer thicknesses, alloy powders closely affected bond strength. Statistical comparisons revealed that the highest bond strength could be achieved with DMLS-Cobalt-Chrome SP2-20μm, and the lowest bond strength was observed in DMLS-Keramit NP-S-20μm (P≤.05). No correlation was found between porcelain remnants on the metal surface and bond strength values. The layered manufacturing device and the alloy powders evaluated in the current study closely affected the bond strength of dental porcelain to a metal framework. However, layer thickness did not affect the bond strength. Copyright © 2017 Editorial Council for the Journal of Prosthetic Dentistry. Published by Elsevier Inc. All rights reserved.

Catalyst for cracking kerosene

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

Hsie, C. H.

1985-06-04

A catalyst capable of cracking kerosene under lower pressure and temperature comprising kerosene; metal powder mixture of chromium powder, copper powder, lead powder, zinc powder, nickel powder, manganese powder in an amount of 12 to 13 parts by weight per 100 parts by weight of said kerosene; sulfuric acid in an amount of 15 to 30 parts by weight per 100 parts by weight of said kerosene; inorganic powder mixture of aluminum oxide powder, serpentine powder, alum powder, magnesium oxide powder, limestone powder, slake lime powder, silica powder, and granite powder in an amount of 150 to 170 parts bymore » weight per 100 parts by weight of said kerosene.« less

Biaxially textured articles formed by powder metallurgy

DOEpatents

Goyal, Amit; Williams, Robert K.; Kroeger, Donald M.

2005-01-25

A biaxially textured alloy article having a magnetism less than pure Ni includes a rolled and annealed compacted and sintered powder-metallurgy preform article, the preform article having been formed from a powder mixture selected from the group of mixtures consisting of: at least 60 at % Ni powder and at least one of Cr powder, W powder, V powder, Mo powder, Cu powder, Al powder, Ce powder, YSZ powder, Y powder, Mg powder, and RE powder; the article having a fine and homogeneous grain structure; and having a dominant cube oriented {100}<100> orientation texture; and further having a Curie temperature less than that of pure Ni.

Biaxially textured articles formed by powder metallurgy

DOEpatents

Goyal, Amit; Williams, Robert K.; Kroeger, Donald M.

2005-05-10

A biaxially textured alloy article having a magnetism less than pure Ni includes a rolled and annealed compacted and sintered powder-metallurgy preform article, the preform article having been formed from a powder mixture selected from the group of mixtures consisting of at least 60 at % Ni powder and at least one of Cr powder, W powder, V powder, Mo powder, Cu powder, Al powder, Ce powder, YSZ powder, Y powder, Mg powder, and RE powder; the article having a fine and homogeneous grain structure; and having a dominant cube oriented {100}<100> orientation texture; and further having a Curie temperature less than that of pure Ni.

Biaxially textured articles formed by powder metallurgy

DOEpatents

Goyal, Amit; Williams, Robert K.; Kroeger, Donald M.

2003-08-26

A biaxially textured alloy article having a magnetism less than pure Ni includes a rolled and annealed compacted and sintered powder-metallurgy preform article, the preform article having been formed from a powder mixture selected from the group of mixtures consisting of: at least 60 at % Ni powder and at least one of Cr powder, W powder, V powder, Mo powder, Cu powder, Al powder, Ce powder, YSZ powder, Y powder, Mg powder, and RE powder; the article having a fine and homogeneous grain structure; and having a dominant cube oriented {100}<100> orientation texture; and further having a Curie temperature less than that of pure Ni.

Biaxially textured articles formed by powder metallurgy

DOEpatents

Goyal, Amit; Williams, Robert K.; Kroeger, Donald M.

2003-08-19

A biaxially textured alloy article having a magnetism less than pure Ni includes a rolled and annealed compacted and sintered powder-metallurgy preform article, the preform article having been formed from a powder mixture selected from the group of mixtures consisting of: at least 60 at % Ni powder and at least one of Cr powder, W powder, V powder, Mo powder, Cu powder, Al powder, Ce powder, YSZ powder, Y powder, Mg powder, and RE powder; the article having a fine and homogeneous grain structure; and having a dominant cube oriented {100}<100> orientation texture; and further having a Curie temperature less than that of pure Ni.

Biaxially textured articles formed by powder metallurgy

DOEpatents

Goyal, Amit; Williams, Robert K.; Kroeger, Donald M.

2004-09-28

A biaxially textured alloy article having a magnetism less than pure Ni includes a rolled and annealed compacted and sintered powder-metallurgy preform article, the preform article having been formed from a powder mixture selected from the group of mixtures consisting of: at least 60 at % Ni powder and at least one of Cr powder, W powder, V powder, Mo powder, Cu powder, Al powder, Ce powder, YSZ powder, Y powder, Mg powder, and RE powder; the article having a fine and homogeneous grain structure; and having a dominant cube oriented {100}<100> orientation texture; and further having a Curie temperature less than that of pure Ni.

Biaxially textured articles formed by powder metallurgy

DOEpatents

Goyal, Amit; Williams, Robert K.; Kroeger, Donald M.

2004-09-14

A biaxially textured alloy article having a magnetism less than pure Ni includes a rolled and annealed compacted and sintered powder-metallurgy preform article, the preform article having been formed from a powder mixture selected from the group of mixtures consisting of: at least 60 at % Ni powder and at least one of Cr powder, W powder, V powder, Mo powder, Cu powder, Al powder, Ce powder, YSZ powder, Y powder, Mg powder, and RE powder; the article having a fine and homogeneous grain structure; and having a dominant cube oriented {100}<100> orientation texture; and further having a Curie temperature less than that of pure Ni.

Biaxially textured articles formed by powder metallurgy

DOEpatents

Goyal, Amit; Williams, Robert K.; Kroeger, Donald M.

2003-07-29

A biaxially textured alloy article having a magnetism less than pure Ni includes a rolled and annealed compacted and sintered powder-metallurgy preform article, the preform article having been formed from a powder mixture selected from the group of mixtures consisting of: at least 60 at % Ni powder and at least one of Cr powder, W powder, V powder, Mo powder, Cu powder, Al powder, Ce powder, YSZ powder, Y powder, Mg powder, and RE powder; the article having a fine and homogeneous grain structure; and having a dominant cube oriented {100}<100> orientation texture; and further having a Curie temperature less than that of pure Ni.

Biaxially textured articles formed by powder metallurgy

DOEpatents

Goval, Amit; Williams, Robert K.; Kroeger, Donald M.

2005-06-07

A biaxially textured alloy article having a magnetism less than pure Ni includes a rolled and annealed compacted and sintered powder-metallurgy preform article, the preform article having been formed from a powder mixture selected from the group of mixtures consisting of: at least 60 at % Ni powder and at least one of Cr powder, W powder, V powder, Mo powder, Cu powder, Al powder, Ce powder, YSZ powder, Y powder, Mg powder, and RE powder; the article having a fine and homogeneous grain structure; and having a dominant cube oriented {100}<100> orientation texture; and further having a Curie temperature less than that of pure Ni.

Development of Sampling Methods for Powders and Soil for Detection of Biothreat Agents by Electrochemiluminecence

DTIC Science & Technology

2007-06-01

DEC03; dairy creamer, lot number DPG 13MAY04; and flour , lot number DPGLJ24MAY05. In addition, flour (white, enriched , all purpose, Safeway brand...8 Table 2. M IM assay of dairy creamer, flour , and soil from swabs................................... 10 Table 3. M...IM assays of flour and soil in triplicate.................................................... 10 vi DRDC Suffield TM 2007-172 Acknowledgements The

Fort A.P. Hill Soil Permittivity and Conductivity Measurements for the Wide Area Airborne Minefield Detection Program

DTIC Science & Technology

2003-09-01

4 3. Purpose 4 4. Description of Test Equipment 4 4.1 Damaskos Model 3000T Liquid/Powder Cell Permittivity...Permeability System ..........4 4.2 HP8510 Network Analyzer/ Damaskos System Overview..............................................5 5. Soil Sample Site...Permittivity and conductivity values were measured from 100 to 3000 MHz. The soil samples were packed as tight as possible into the Damaskos

Cermets and method for making same

DOEpatents

Aaron, W. Scott; Kinser, Donald L.; Quinby, Thomas C.

1983-01-01

The present invention is directed to a method for making a wide variety of general-purpose cermets and for radioactive waste disposal from ceramic powders prepared from urea-dispersed solutions containing various metal values. The powders are formed into a compact and subjected to a rapid temperature increase in a reducing atmosphere. During this reduction, one or more of the more readily reducible oxides in the compact is reduced to a selected substoichiometric state at a temperature below the eutectic phase for that particular oxide or oxides and then raised to a temperature greater than the eutectic temperature to provide a liquid phase in the compact prior to the reduction of the liquid phase forming oxide to solid metal. This liquid phase forms at a temperature below the melting temperature of the metal and bonds together the remaining particulates in the cermet to form a solid polycrystalline cermet.

Validation of missed space-group symmetry in X-ray powder diffraction structures with dispersion-corrected density functional theory.

PubMed

Hempler, Daniela; Schmidt, Martin U; van de Streek, Jacco

2017-08-01

More than 600 molecular crystal structures with correct, incorrect and uncertain space-group symmetry were energy-minimized with dispersion-corrected density functional theory (DFT-D, PBE-D3). For the purpose of determining the correct space-group symmetry the required tolerance on the atomic coordinates of all non-H atoms is established to be 0.2 Å. For 98.5% of 200 molecular crystal structures published with missed symmetry, the correct space group is identified; there are no false positives. Very small, very symmetrical molecules can end up in artificially high space groups upon energy minimization, although this is easily detected through visual inspection. If the space group of a crystal structure determined from powder diffraction data is ambiguous, energy minimization with DFT-D provides a fast and reliable method to select the correct space group.

Effect of PMMA polymer on the dynamic viscoelasticity and plasticizer leachability of PEMA-based tissue conditioners.

PubMed

Hong, Guang; Maeda, Takeshi; Li, YingAi; Sadamori, Shinsuke; Hamada, Taizo; Murata, Hiroshi

2010-08-01

The purpose of this study was to determine the effect of PMMA polymer on dynamic viscoelasticity and plasticizer leachability of PEMA-based tissue conditioners. One PEMA polymer and one PMMA polymer were used in powder form with four formulations. The combination of 80 wt% ATBC, 15 wt% BPBG and 5 wt% ethyl alcohol was used as the liquid phase. The dynamic viscoelasticity and plasticizer leaching of each specimen were measured after 0, 1, 3, 7, and 14 days of immersion (37 degrees C distilled water) using DMA and HPLC. A significant difference was found among the materials in the dynamic viscoelasticity and leaching of plasticizer. The materials containing 10 wt% PMMA showed the most stable dynamic viscoelasticity, and showed the lowest leaching of plasticizer. The results suggest that the addition of the PMMA polymer to the powder of a tissue conditioner can improve the durability of the PEMA-based tissue conditioner.

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

Fisher, L.M.

Presently some methods of HTS-conductors processing are under study in the authors laboratory. ``Powder-in-tube`` (PIT), ``Jelly-roll``, electrophorethis are among them. PIT process has developed predominantly both in a view of the achieved J{sub c} values Bi-2223 phase was used as a core material for these tapes. Since the main purpose of the task order was to enhance the development of long length high temperature superconductor tapes, the authors have considered reasonable to lay the perfection idea of the PIT process step by step or tape by tape. To realize it they have assumed, keeping stable the basic scheme of PITmore » process, to vary some technological parameters which are as follows: (1) type of initial powder; (2) sheath material; (3) tape construction (filaments number, cross section e.a.); and (4) processing regimes. This report covers the fabrication process and characteristics of the produced conductors.« less

Structure and characteristics of functional powder composite materials obtained by spark plasma sintering

NASA Astrophysics Data System (ADS)

Oglezneva, S. A.; Kachenyuk, M. N.; Kulmeteva, V. B.; Ogleznev, N. B.

2017-07-01

The article describes the results of spark plasma sintering of ceramic materials based on titanium carbide, titanium carbosilicide, ceramic composite materials based on zirconium oxide, strengthened by carbon nanostructures and composite materials of electrotechnical purpose based on copper with addition of carbon structures and titanium carbosilicide. The research shows that the spark plasma sintering can achieve relative density of the material up to 98%. The effect of sintering temperature on the phase composition, density and porosity of the final product has been studied. It was found that with addition of carbon nanostructures the relative density and hardness decrease, but the fracture strength of ZrO2 increases up to times 2. The relative erosion resistance of the electrodes made of composite copper-based powder materials, obtained by spark plasma sintering during electroerosion treatment of tool steel exceeds that parameter of pure copper up to times 15.

Effect of Stemming to Burden Ratio and Powder Factor on Blast Induced Rock Fragmentation- A Case Study

NASA Astrophysics Data System (ADS)

Prasad, Sandeep; Choudhary, B. S.; Mishra, A. K.

2017-08-01

Rock fragmentation size is very important parameters for economical point of view in any surface mining. Rock fragment size direct effects on the costs of drilling, blasting, loading, secondary blasting and crushing. The main purpose of this study is to investigate effect of blast design parameters such as burden, blast hole length, stemming length, and powder factor on rock fragmentation. The fragment sizes (MFS, K50, m), and maximum fragment size (K95, m) of rock were determined by using the computer software. For every blast, after blasting operation, the images of whole muck pile are captured and there images were used for fragmentation analysis by using the Fragalyst software. It was observed that the optimal fragment size (MFS, K50, m and maximum fragment size, K95, m) of rock depends strongly on the blast design parameters and explosive parameters.

Development of an electrostatic propulsion engine using sub-micron powders as the reaction mass

NASA Technical Reports Server (NTRS)

Herbert, F.; Kendall, K. R.

1991-01-01

Asteroid sample return missions would benefit from development of an improved rocket engine. Chemical rockets achieve their large thrust with high mass consumption rate (dm/dt) but low exhaust velocity; therefore, a large fraction of their total mass is fuel. Present day ion thrusters are characterized by high exhaust velocity, but low dm/dt; thus, they are inherently low thrust devices. However, their high exhausy velocity is poorly matched to typical mission requirements and therefore, wastes energy. A better match would be intermediate between the two forms of propulsion. This could be achieved by electrostatically accelerating solid powder grains, raising the possibility that interplanetary material could be processed to use as reaction mass. An experiment to study the charging properties of sub-micron sized powder grains is described. If a suitable material can be identified, then it could be used as the reaction mass in an electrostatic propulsion engine. The experiment employs a time of flight measurement to determine the exhaust velocity (v) of various negatively charged powder grains that were charged and accelerated in a simple device. The purpose is to determine the charge to mass ratio that can be sustained for various substances. In order to be competitive with present day ion thrusters, a specific impulse (v/g) of 3000 to 5000 seconds is required. Preliminary results are presented. More speculatively, there are some mission profiles that would benefit from collection of reaction mass at the remote asteroid site. Experiments that examine the generation of sub-micron clusters by electrostatic self-disruption of geologically derived material are planned.

Studies on the mechanism of printing film-coated tablets containing titanium dioxide in the film by using UV laser irradiation.

PubMed

Kato, Yoshiteru; Nakashima, Yasuhiko; Shino, Naoki; Sasaki, Koichi; Hosokawa, Akihiro; Ishihara, Hiroshi

2010-04-01

The purpose of this article is to study a detailed mechanism of printing when film-coated tablets were irradiated by UV laser at a wavelength of 355 nm. Hydroxypropylmethylcellulose (HPMC) film containing titanium dioxide (TiO(2)) and the film not containing TiO(2) and TiO(2) powder were lirradiated by the UV laser and estimated by the morphological observation by zoom stereo microscope, thermogravimetric analysis (TGA), total color difference (dE), X-ray powder diffraction (XRD), and dispersive Raman microscopy. In the case of the film containing TiO(2), the film showed a visible change in its color from white to gray by the UV laser irradiation. By zoom stereo microscope, it was found that the entire UV laser-irradiated area was not grayed uniformly, but many black particles, whose diameter was about 2 microm, were observed on the film. When TiO(2) powder was irradiated by the UV laser, a visible change in its color from white to gray was observed similar to the case of the film containing TiO(2). There were many black particles locally in the UV laser-treated TiO(2) powder by the morphological observation, and these black particles, agglomerates of the grayed oxygen-defected TiO(2), were associated with the visible change of the TiO(2). It was found that the film-coated tablets were printed utilizing the formation of the black particles by the agglomeration of the grayed oxygen-defected TiO(2) by the UV laser irradiation.

Plasma sprayed coatings on crankshaft used steels

NASA Astrophysics Data System (ADS)

Mahu, G.; Munteanu, C.; Istrate, B.; Benchea, M.

2017-08-01

Plasma spray coatings may be an alternative to conventional heat treatment of main journals and crankpins of the crankshaft. The applications of plasma coatings are various and present multiple advantages compared to electric arc wire spraying or flame spraying. The study examines the layers sprayed with the following powders: Cr3C2- 25(Ni 20Cr), Al2O3- 13TiO2, Cr2O3-SiO2- TiO2 on the surface of steels used in the construction of a crankshaft (C45). The plasma spray coatings were made with the Spray wizard 9MCE facility at atmospheric pressure. The samples were analyzed in terms of micro and morphological using optical microscopy, scanning electron microscopy and X-ray diffraction. Wear tests on samples that have undergone simulates extreme working conditions of the crankshafts. In order to emphasize adherence to the base material sprayed layer, were carried out tests of microscratches and micro-indentation. Results have showed a relatively compact morphological aspect given by the successive coatings with splat-like specific structures. Following the microscratch analysis it can be concluded that Al2O3-13TiO2 coating has a higher purpose in terms of hardness compared to Cr3C2-(Ni 20Cr) and Cr2O3-SiO2- TiO2 powders. Thermal coatings of the deposited powders have increased the mechanical properties of the material. The results stand to confirm that plasma sprayed Al2O3-13TiO2 powder is in fact a efficient solution for preventing mechanical wear, even with a faulty lubrication system.

Improvement of physicomechanical properties of carbamazepine by recrystallization at different pH values.

PubMed

Javadzadeh, Yousef; Mohammadi, Ameneh; Khoei, Nazaninossadat Seyed; Nokhodchi, Ali

2009-06-01

The morphology of crystals has an appreciable impact role on the physicochemical properties of drugs. Drug properties such as flowability, dissolution, hardness and bioavailability may be affected by crystallinity behaviours of drugs. The objective of this study was to achieve an improved physicomechanical property of carbamazepine powder through recrystallization from aqueous solutions at different pH values. For this purpose, carbamazapine was recrystallized from aqueous solutions at different pH values (1, 7, 11). The morphology of crystals was investigated using scanning electron microscopy; X-ray powder diffraction (XRPD) was used to identify polymorphism; thermodynamic properties were analyzed using differential scanning calorimetery (DSC). Dissolution rate was determined using USP dissolution apparatus. Mechanical behavior of recrystallized carbamazepine powders was investigated by making tablets under different compaction pressure and measuring their hardness. SEM studies showed that the carbamazepine crystallization in different media affected the morphology and size of carbamazepine crystals. The shape of carbamazepine crystals changed from flaky or thin plate-like to needle shape. XRPD and DSC results ruled out any crystallinity changes occurring due to the temperature during recrystallization procedure or pH of crystallization media. The crushing strength of tablets indicated that all of the recrystallized carbamazepine samples had better compactiblity than the original carbamazepine powder. In vitro dissolution studies of carbamazepine samples showed a higher dissolution rate for carbamazepine crystals obtained from media with pH 11 and 1. Carbamazepine particles recrystallized from aqueous solutions of different pH values (all media) appeared to have superior mechanical properties to those of the original carbamazepine sample.

Characterisation of the incident beam and current diffraction capabilities on the VESUVIO spectrometer

NASA Astrophysics Data System (ADS)

Romanelli, G.; Krzystyniak, M.; Senesi, R.; Raspino, D.; Boxall, J.; Pooley, D.; Moorby, S.; Schooneveld, E.; Rhodes, N. J.; Andreani, C.; Fernandez-Alonso, F.

2017-09-01

The VESUVIO spectrometer at the ISIS pulsed neutron and muon source is a unique instrument amongst those available at neutron facilities. This is the only inverted-geometry neutron spectrometer accessing values of energy and wavevector transfer above tens of eV and {\\mathringA}-1 , respectively, and where deep inelastic neutron scattering experiments are routinely performed. As such, the procedure at the base of the technique has been previously described in an article published by this journal (Mayers and Reiter 2012 Meas. Sci. Technol. 23 045902). The instrument has recently witnessed an upsurge of interest due to a new trend to accommodate, within a single experiment, neutron diffraction and transmission measurements in addition to deep inelastic neutron scattering. This work presents a broader description of the instrument following these recent developments. In particular, we assess the absolute intensity and two-dimensional profile of the incident neutron beam and the capabilities of the backscattering diffraction banks. All results are discussed in the light of recent changes to the moderator viewed by the instrument. We find that VESUVIO has to be considered a high-resolution diffractometer as much as other diffractometers at ISIS, with a resolution as high as 2× 10-3 in backscattering. Also, we describe the extension of the wavelength range of the instrument to include lower neutron energies for diffraction measurements, an upgrade that could be readily applied to other neutron instruments as well.

Combining Hard with Soft Materials in Nanoscale Under High-Pressure High-Temperature Conditions

NASA Technical Reports Server (NTRS)

Palosz, B.; Gierlotka, S.; Swiderska-Sroda, A.; Fietkiewicz, K.; Kalisz, G.; Grzanka, E.; Stel'makh, S.; Palosz, W.

2004-01-01

Nano-composites with a primary nanocrystalline ceramic matrix and a secondary nanocrystalline material (metal or semiconductor) were synthesized by infiltration of an appropriate liquid into ceramic compacts under pressures of up to 8 GPa and temperatures of up to 2000 K. The purpose of our work is to obtain nanocomposites which constitute homoger?ous mixtures of two phases, both forming nano- grains of about 10 nm in size. The high pressure is used to bring the porosity of the compacted powders down to the nano-scale and force a given liquid into the nano-sized pores. The advantage of the infiltration technique is that, in a single, continuous process, we start with a nanocrystalline powder, compress it to form the matrix of the composite, and crystallize and/or synthesize a second nanomaterial in the matrix pores. The key limitation of this technology is, that the pores in the matrix need to stay open during the entire process of infiltration. Thus the initial powder should form a rigid skeleton, otherwise the so-called self-stop process can limit cr block a further flow of the liquid phase and hinder the process of the composite formation. Therefore powders of only very hard ceramic materials like diamond, Sic, or Alz03, which can withstand a substantial external load without undesired deformation, can be used as the primary phase. With this technique, using diamond and S i c ceramic powders infiltrated by liquid metals (AI, Zn, Sn, Ag, Au) and semiconductors (Si, Ge, GaAs, CdTe), we obtained nano-composites with the grain size in the range of 10 - 30 nm. Our work addresses the key problem in manufacturing bulk nanocrystalline materials, i.e. preservation of nano-scale during the fabrication process. In this paper we discuss basic technical and methodological problems associated with nano-infiltration based on the results obtained for Zn-Sic composites.

Design of an inhalable dry powder formulation of DOTAP-modified PLGA nanoparticles loaded with siRNA.

PubMed

Jensen, Ditte Krohn; Jensen, Linda Boye; Koocheki, Saeid; Bengtson, Lasse; Cun, Dongmei; Nielsen, Hanne Mørck; Foged, Camilla

2012-01-10

Matrix systems based on biocompatible and biodegradable polymers like the United States Food and Drug Administration (FDA)-approved polymer poly(DL-lactide-co-glycolide acid) (PLGA) are promising for the delivery of small interfering RNA (siRNA) due to favorable safety profiles, sustained release properties and improved colloidal stability, as compared to polyplexes. The purpose of this study was to design a dry powder formulation based on cationic lipid-modified PLGA nanoparticles intended for treatment of severe lung diseases by pulmonary delivery of siRNA. The cationic lipid dioleoyltrimethylammoniumpropane (DOTAP) was incorporated into the PLGA matrix to potentiate the gene silencing efficiency. The gene knock-down level in vitro was positively correlated to the weight ratio of DOTAP in the particles, and 73% silencing was achieved in the presence of 10% (v/v) serum at 25% (w/w) DOTAP. Optimal properties were found for nanoparticles modified with 15% (w/w) DOTAP, which reduced the gene expression with 54%. This formulation was spray-dried with mannitol into nanocomposite microparticles of an aerodynamic size appropriate for lung deposition. The spray-drying process did not affect the physicochemical properties of the readily re-dispersible nanoparticles, and most importantly, the in vitro gene silencing activity was preserved during spray-drying. The siRNA content in the powder was similar to the theoretical loading and the siRNA was intact, suggesting that the siRNA is preserved during the spray-drying process. Finally, X-ray powder diffraction analysis demonstrated that mannitol remained in a crystalline state upon spray-drying with PLGA nanoparticles suggesting that the sugar excipient might exert its stabilizing effect by sterical inhibition of the interactions between adjacent nanoparticles. This study demonstrates that spray-drying is an excellent technique for engineering dry powder formulations of siRNA nanoparticles, which might enable the local delivery of biologically active siRNA directly to the lung tissue. Copyright © 2011 Elsevier B.V. All rights reserved.

Physical evaluation of a needle photostimulable phosphor based CR mammography system

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

Marshall, Nicholas W.; Lemmens, Kim; Bosmans, Hilde

2012-02-15

Purpose: Needle phosphor based computed radiography (CR) systems promise improved image quality compared to powder phosphor based CR units for x-ray screening mammography. This paper compares the imaging performance of needle CR cassettes, powder based CR cassettes and a well established amorphous selenium (a-Se) based flat panel based mammography system, using consistent beam qualities. Methods: Detector performance was assessed using modulation transfer function (MTF), normalized noise power spectrum (NNPS), and detective quantum efficiency (DQE). Mammography system performance was assessed against levels from the European Guidelines, including threshold gold thickness (c-d), relative signal difference to noise (SdNR) and mean glandular dose,more » for automatic exposure control settings suggested by the manufacturers. The needle based Agfa HM5.0 CR detector was compared against the single sided readout Agfa MM3.0R and dual sided readout Fuji Profect CS powder CR plates using a 28 kV Mo/Rh spectrum, while a 28 kV W/Rh spectrum was used to compare the Agfa HM5.0 against the Siemens MAMMOMAT Inspiration a-Se based system. Results: MTF at 5 mm{sup -1} was 0.16 and 0.24 for the needle CR detector in the fast and slow scan directions, respectively, indicating a slight improvement ({approx}20%) over the two powder CR systems but remained 50% lower than the result at 5 mm{sup -1} for the a-Se detector ({approx}0.55). Structured screen noise was lower for the needle phosphor compared to the powder plates. CR system gain, estimated from the measured absorption fraction and NNPS results, was 6.3 for the (single sided) needle phosphor and 5.1 and 7.2 for the single sided and dual sided powder phosphor systems. Peak DQE at {approx}100 {mu}Gy was 0.47 for the needle system compared to peak DQE figures of 0.33 and 0.46 for the single sided readout powder plates and dual sided readout plates. The high frequency DQE (at 5 mm{sup -1}) was 0.19 for the needle CR plates, a factor of approximately 3 greater than for the powder CR plates. At 28 kV W/Rh, 2 mm Al, peak DQE for the needle CR system was 0.45 against a value of 0.50 for the a-Se detector. The needle CR detector reached the Acceptable limit for 0.1 mm details in the European Guidelines at a mean glandular dose (MGD) of approximately 1.31 mGy imaged at 28 kV Mo/Rh, compared to figures of 2.19 and 1.43 mGy for the single sided and dual sided readout powder CR systems. The a-Se detector could reach the limit at 0.65 mGy using a 28 kV W/Rh spectrum, while the needle CR system required 1.09 mGy for the same spectrum. Conclusions: Imaging performance for the needle CR phosphor technology, characterized using MTF and DQE and threshold gold thickness demonstrated a clear improvement compared to both single and dual sided reading powder phosphor based CR systems.« less

Biaxially textured articles formed by power metallurgy

DOEpatents

Goyal, Amit; Williams, Robert K.; Kroeger, Donald M.

2003-08-26

A biaxially textured alloy article having a magnetism less than pure Ni includes a rolled and annealed compacted and sintered powder-metallurgy preform article, the preform article having been formed from a powder mixture selected from the group of mixtures consisting of: at least 60 at % Ni powder and at least one of Cr powder, W powder, V powder, Mo powder, Cu powder, Al powder, Ce powder, YSZ powder, Y powder, Mg powder, and RE powder; the article having a fine and homogeneous grain structure; and having a dominant cube oriented {100}<100> orientation texture; and further having a Curie temperature less than that of pure Ni.

Rheological, physical and sensorial evaluation of cookies supplemented with dairy powders.

PubMed

Sert, Durmuş; Demir, M Kürşat; Ertaş, Nilgün

2016-04-01

The effect of dairy powders (skim milk powder, butter milk powder, sodium caseinate, yoghurt powder, milk powder and colostrum powder) on cookie quality was studied. Cookies were tested for aw, calorimetric energy, diameter, thickness, spread ratio, breaking strength, colour, dough consistency and sensory evaluation. The lowest aw values were obtained for cookies containing colostrum powder; also the highest calorimetric energy values were obtained from the colostrum powder-added cookies. Diameter values of cookies with the addition of skim milk powder, butter milk powder, yoghurt powder and milk powder were higher than that of sodium caseinate and colostrum powder. The lowest spread ratio was measured in the cookie samples with added skim milk powder. The addition of yoghurt powder gave the highest breaking strength of cookies. Cookies with sodium caseinate addition exhibited the highest lightness (L*) values than the other cookies with different dairy powders. Cookies prepared with butter milk powder received the highest scores for colour, appearance, texture, crispness and overall acceptability. © The Author(s) 2015.

How people used ochre at Rose Cottage Cave, South Africa: Sixty thousand years of evidence from the Middle Stone Age

PubMed Central

Wadley, Lyn

2017-01-01

We describe colour, hardness, grain size, geological type and surface modifications of ochre pieces excavated, first by Malan and later by Harper, from the Middle Stone Age (MSA) of Rose Cottage Cave, 96, 000 to 30, 000 years ago. Soft, bright-red shales are abundant, and most ochre has clayey or silty grain sizes. The post-Howiesons Poort layers contain the most ochre pieces, but the Howiesons Poort layers have the highest frequency of ochre per sediment volume. The pre-Howiesons Poort layers have the highest utilization rate. Use-traces include rubbing, grinding, combined grinding and rubbing, and rare instances of scoring. The processing techniques are proxies for ochre use. Rubbing transfers red ochre powder directly onto soft surfaces, such as human skin, or animal hide. This is appropriate when skin colouring and marking or skin protection (for example from sun, insects or bacteria) is the purpose. Grinding produces ochre powder that can be used for a variety of tasks. It can be mixed with water or other products to create paint, cosmetics or adhesives. Multiple uses of ochre powder and ochre pieces are therefore implied at Rose Cottage and changes through time are apparent. PMID:28445491

Mechanism of amorphisation of micro-particles of griseofulvin during powder flow in a mixer.

PubMed

Pazesh, Samaneh; Höckerfelt, Mina Heidarian; Berggren, Jonas; Bramer, Tobias; Alderborn, Göran

2013-11-01

The purpose of the research was to investigate the degree of solid-state amorphisation during powder flow and to propose a mechanism for this transformation. Micro-particles of griseofulvin (about 2 μm in diameter) were mixed in a shear mixer under different conditions to influence the inter-particulate collisions during flow, and the degree of amorphisation was determined by micro-calorimeter. The amorphisation of griseofulvin particles (GPs) during repeated compaction was also determined. The GPs generally became disordered during mixing in a range from about 6% to about 86%. The degree of amorphisation increased with increased mixing time and increased batch size of the mixer, whereas the addition of a lubricant to the blend reduced the degree of amorphisation. Repeated compaction using the press with ejection mode gave limited amorphisation, whereas repeated compaction without an ejection process gave minute amorphisation. It is concluded that during powder flow, the most important inter-particulate contact process that cause the transformation of a crystalline solid into an amorphous state is sliding. On the molecular scale, this amorphisation is proposed to be caused by vitrification, that is the melting of a solid because of the generation of heat during sliding followed by solidification into an amorphous phase. © 2013 Wiley Periodicals, Inc. and the American Pharmacists Association.

Flash (Ultra-Rapid) Spark-Plasma Sintering of Silicon Carbide

PubMed Central

Olevsky, Eugene A.; Rolfing, Stephen M.; Maximenko, Andrey L.

2016-01-01

A new ultra-rapid process of flash spark plasma sintering is developed. The idea of flash spark plasma sintering (or flash hot pressing - FHP) stems from the conducted theoretical analysis of the role of thermal runaway phenomena for material processing by flash sintering. The major purpose of the present study is to theoretically analyze the thermal runaway nature of flash sintering and to experimentally address the challenge of uncontrollable thermal conditions by the stabilization of the flash sintering process through the application of the external pressure. The effectiveness of the developed FHP technique is demonstrated by the few seconds–long consolidation of SiC powder in an industrial spark plasma sintering device. Specially designed sacrificial dies heat the pre-compacted SiC powder specimens to a critical temperature before applying any voltage to the powder volume and allowing the electrode-punches of the SPS device setup to contact the specimens and pass electric current through them under elevated temperatures. The experimental results demonstrate that flash sintering phenomena can be realized using conventional SPS devices. The usage of hybrid heating SPS devices is pointed out as the mainstream direction for the future studies and utilization of the new flash hot pressing (ultra-rapid spark plasma sintering) technique. PMID:27624641

Flash (Ultra-Rapid) Spark-Plasma Sintering of Silicon Carbide

DOE PAGES

Olevsky, Eugene A.; Rolfing, Stephen M.; Maximenko, Andrey L.

2016-09-14

A new ultra-rapid process of flash spark plasma sintering is developed. The idea of flash spark plasma sintering (or flash hot pressing - FHP) stems from the conducted theoretical analysis of the role of thermal runaway phenomena for material processing by flash sintering. The major purpose of the present study is to theoretically analyze the thermal runaway nature of flash sintering and to experimentally address the challenge of uncontrollable thermal conditions by the stabilization of the flash sintering process through the application of the external pressure. The effectiveness of the developed FHP technique is demonstrated by the few seconds–long consolidationmore » of SiC powder in an industrial spark plasma sintering device. Specially designed sacrificial dies heat the pre-compacted SiC powder specimens to a critical temperature before applying any voltage to the powder volume and allowing the electrode-punches of the SPS device setup to contact the specimens and pass electric current through them under elevated temperatures. The experimental results demonstrate that flash sintering phenomena can be realized using conventional SPS devices. The usage of hybrid heating SPS devices is pointed out as the mainstream direction for the future studies and utilization of the new flash hot pressing (ultra-rapid spark plasma sintering) technique.« less

Extraction of titanium from low-iron nitrided Malaysian ilmenite by chlorination

NASA Astrophysics Data System (ADS)

Ibrahim, Najwa; Ahmadi, Eltefat; Rahman, Shaik Abdul; Fauzi, M. N. Ahmad; Rezan, Sheikh Abdul

2017-01-01

In this paper, production of TiCl4 from low-iron nitrided ilmenite samples at relatively low temperature using chlorine gas generated from the reaction between KMnO4 and HCl has been investigated. The effects of chlorination soaking time, potassium permanganate (KMnO4) to hydrochloric acid (HCl) molar ratio and aluminium powder catalyst in chlorine gas generation on titanium extraction from nitrided Malaysian ilmenite were examined. The low-iron nitrided Malaysian ilmenite contained titanium oxycarbonitride (TiOxCyNz) after carbothermal reduction and nitridation with subsequent leaching. Chlorination process was performed at 500°C for 30 - 60 minutes. Statistical analysis of the data was done by Design of Experiment (DOE) to identify the significant variables and their interactions. The results achieved in this study showed that the highest extent of chlorination was about 98.34% at 500°C for 60 minutes. The lowest extent of chlorination was about 68.51% obtained in KMnO4 to HCl molar ratio of 2.0 and 0.35 g of aluminium powder. The chlorinated titanium oxycarbonitride powders and TiCl4 solutions were analyzed by X-ray diffraction (XRD) and inductively coupled plasma-optical emission spectroscopy (ICP-OES), respectively. The purpose of this study was to explore the relationship between the processing parameters on extracting titanium via pyrometallurgical technique.

Raman spectroscopy method for subsurface detection of food powders through plastic layers

NASA Astrophysics Data System (ADS)

Dhakal, Sagar; Chao, Kuanglin; Qin, Jianwei; Schmidt, Walter F.; Kim, Moon S.; Chan, Diane E.; Bae, Abigail

2017-05-01

Proper chemical analyses of materials in sealed containers are important for quality control purpose. Although it is feasible to detect chemicals at top surface layer, it is relatively challenging to detect objects beneath obscuring surface. This study used spatially offset Raman spectroscopy (SORS) method to detect urea, ibuprofen and acetaminophen powders contained within one or more (up to eight) layers of gelatin capsules to demonstrate subsurface chemical detection and identification. A 785 nm point-scan Raman spectroscopy system was used to acquire spatially offset Raman spectra for an offset range of 0 to 10 mm from the surfaces of 24 encapsulated samples, using a step size of 0.1 mm to obtain 101 spectral measurements per sample. With increasing offset distance, the fraction of information from the deeper subsurface material increased compared to that from the top surface material. The series of measurements was analyzed to differentiate and identify the top surface and subsurface materials. Containing mixed contributions from the powder and capsule, the SORS of each sample was decomposed using self modeling mixture analysis (SMA) to obtain pure component spectra of each component and corresponding components were identified using spectral information divergence values. Results show that SORS technique together with SMA method has a potential for non-invasive detection of chemicals at deep subsurface layer.

Powder treatment process

DOEpatents

Weyand, J.D.

1988-02-09

Disclosed are: (1) a process comprising spray drying a powder-containing slurry, the slurry containing a powder constituent susceptible of oxidizing under the temperature conditions of the spray drying, while reducing the tendency for oxidation of the constituent by including as a liquid constituent of the slurry an organic liquid; (2) a process comprising spray drying a powder-containing slurry, the powder having been pretreated to reduce content of a powder constituent susceptible of oxidizing under the temperature conditions of the spray drying, the pretreating comprising heating the powder to react the constituent; and (3) a process comprising reacting ceramic powder, grinding the reacted powder, slurrying the ground powder, spray drying the slurried powder, and blending the dried powder with metal powder. 2 figs.

Powder treatment process

DOEpatents

Weyand, John D.

1988-01-01

(1) A process comprising spray drying a powder-containing slurry, the slurry containing a powder constituent susceptible of oxidizing under the temperature conditions of the spray drying, while reducing the tendency for oxidation of the constituent by including as a liquid constituent of the slurry an organic liquid; (2) a process comprising spray drying a powder-containing slurry, the powder having been pretreated to reduce content of a powder constituent susceptible of oxidizing under the temperature conditions of the spray drying, the pretreating comprising heating the powder to react the constituent; and (3) a process comprising reacting ceramic powder, grinding the reacted powder, slurrying the ground powder, spray drying the slurried powder, and blending the dried powder with metal powder.

Marijuana and chocolate.

PubMed

James, J S

1996-10-18

Three substances in chocolate and cocoa powder may mimic cannabinoid by activating receptors or increasing anandamide levels. Anandamide is a lipid that binds to cannabinoid receptors and mimics the psychoactive effects of the drug. Chocolate is widely believed to enhance the effect of marijuana. A practical implication of this finding is that the amount of marijuana needed for medicinal purposes may be decreased by using it with chocolate, reducing both the risks and cost associated with marijuana.

Sensitivity Testing of RDX/Aluminum Powdered Explosive Mixtures for the Improved Dispersed Explosives (IDX) Project

DTIC Science & Technology

1993-04-01

perpendicular to the pipe axis. During assembly, the threads are lubricated and Teflon tape is used for sealing. Aluminum witness plates (25.4 mm thick...3.3 Electrostatic Discharge ( ESD ) ................................. 7 4. INTERMEDIATE-SCALE SENSITIVITY TESTING ..................... 8 4.1 Card Gap...tests include the DWIT, friction, and electrostatic discharge ( ESD ) tests. The purpose of these tests is to enable the researcher to ensure that the

Sizes of X-ray radiation coherent domains in thin SmS films and their visualization

NASA Astrophysics Data System (ADS)

Sharenkova, N. V.; Kaminskii, V. V.; Petrov, S. N.

2011-09-01

The size of X-ray radiation coherent domains (250 ± 20 Å) is determined in a thin polycrystalline SmS film using X-ray diffraction patterns (θ-2θ scanning, DRON-2 diffractometer, Cu K α radiation) and the Selyakov-Scherrer formula with allowance for the effect of microstrains. An image of this film is taken with a transmission electron microscope, and regions with a characteristic size of 240 Å are clearly visible in it. It is concluded that X-ray radiation coherent domains are visualized.

Acquisition of a High-Resolution High-Intensity X-ray Diffractometer for Research and Education

DTIC Science & Technology

2015-07-20

NAME(S) AND ADDRESS (ES) U.S. Army Research Office P.O. Box 12211 Research Triangle Park, NC 27709-2211 X-ray diffraction; germanium- tin alloys...is in progress for others. Comprehensive data were acquired for pseudomorphic germanium- tin alloys grown on germanium by molecular beam epitaxy...Research  100+  2000  Federal grant  Germanium‐ tin  alloys  Tech transfer  9  180  Startup company  Metallurgy  Research  5  100  Federal grant  SAXS  Total

Dissolution Rates of Allophane, FE-Containing Allophane, and Hisingerite and Implications for Gale Crater, Mars

NASA Technical Reports Server (NTRS)

Ralston, S. J.; Hausrath, E. M.; Tschauner, O.; Rampe, E. B.; Christoffersen, R.

2018-01-01

Investigations with the CheMin Xray Diffractometer (XRD) onboard the Curiosity rover in Gale Crater demonstrate that all rock and soil samples measured to date contain approximately 15-70 weight percentage X-ray amorphous materials. The diffuse scattering hump from the X-ray amorphous materials in CheMin XRD patterns can be fit with a combination of allophane, ferrihydrite, and rhyolitic and basaltic glass. Because of the iron-rich nature of Mars' surface, Fe-rich poorly-crystalline phases, such as hisingerite, may be present in addition to allophane.

Magnetic and structural properties of CoFe 2O 4 thin films synthesized via a sol-gel process

NASA Astrophysics Data System (ADS)

dos S. Duque, J. G.; Macêdo, M. A.; Moreno, N. O.; Lopez, J. L.; Pfanes, H.-D.

2001-05-01

Using a sol-gel process having the coconut water as a precursor of organic chain, we synthesized thin films of cobalt ferrite. The films were characterized by using a SQUID magnetometer, an X-ray diffractometer, an X-ray spectrophotometer, Mössbauer spectroscopy and atomic force microscope. Co ferrite films annealed at 500°C for 2 h show grain sizes between 10 and 20 nm, grown as single-phase spinel structure and exhibit high coercivity and a moderate saturation magnetization (above 30 kOe).

The statistical kinematical theory of X-ray diffraction as applied to reciprocal-space mapping

PubMed

Nesterets; Punegov

2000-11-01

The statistical kinematical X-ray diffraction theory is developed to describe reciprocal-space maps (RSMs) from deformed crystals with defects of the structure. The general solutions for coherent and diffuse components of the scattered intensity in reciprocal space are derived. As an example, the explicit expressions for intensity distributions in the case of spherical defects and of a mosaic crystal were obtained. The theory takes into account the instrumental function of the triple-crystal diffractometer and can therefore be used for experimental data analysis.

Viscosity studies of water based magnetite nanofluids

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

Anu, K.; Hemalatha, J.

2016-05-23

Magnetite nanofluids of various concentrations have been synthesized through co-precipitation method. The structural and topographical studies made with the X-Ray Diffractometer and Atomic Force Microscope are presented in this paper. The density and viscosity studies for the ferrofluids of various concentrations have been made at room temperature. The experimental viscosities are compared with theoretical values obtained from Einstein, Batchelor and Wang models. An attempt to modify the Rosensweig model is made and the modified Rosensweig equation is reported. In addition, new empirical correlation is also proposed for predicting viscosity of ferrofluid at various concentrations.

Method and product for phosphosilicate slurry for use in dentistry and related bone cements

DOEpatents

Wagh, Arun S.; Primus, Carolyn

2006-08-01

The present invention is directed to magnesium phosphate ceramics and their methods of manufacture. The composition of the invention is produced by combining a mixture of a substantially dry powder component with a liquid component. The substantially dry powder component comprises a sparsely soluble oxide powder, an alkali metal phosphate powder, a sparsely soluble silicate powder, with the balance of the substantially dry powder component comprising at least one powder selected from the group consisting of bioactive powders, biocompatible powders, fluorescent powders, fluoride releasing powders, and radiopaque powders. The liquid component comprises a pH modifying agent, a monovalent alkali metal phosphate in aqueous solution, the balance of the liquid component being water. The use of calcined magnesium oxide as the oxide powder and hydroxylapatite as the bioactive powder produces a self-setting ceramic that is particularly suited for use in dental and orthopedic applications.

As(III) oxidation by MnO2 during groundwater treatment.

PubMed

Gude, J C J; Rietveld, L C; van Halem, D

2017-03-15

The top layer of natural rapid sand filtration was found to effectively oxidise arsenite (As(III)) in groundwater treatment. However, the oxidation pathway has not yet been identified. The aim of this study was to investigate whether naturally formed manganese oxide (MnO 2 ), present on filter grains, could abiotically be responsible for As(III) oxidation in the top of a rapid sand filter. For this purpose As(III) oxidation with two MnO 2 containing powders was investigated in aerobic water containing manganese(II) (Mn(II)), iron(II) (Fe(II)) and/or iron(III) (Fe(III)). The first MnO 2 powder was a very pure - commercially available - natural MnO 2 powder. The second originated from a filter sand coating, produced over 22 years in a rapid filter during aeration and filtration. Jar test experiments showed that both powders oxidised As(III). However, when applying the MnO 2 in aerated, raw groundwater, As(III) removal was not enhanced compared to aeration alone. It was found that the presence of Fe(II)) and Mn(II) inhibited As(III) oxidation, as Fe(II) and Mn(II) adsorption and oxidation were preferred over As(III) on the MnO 2 surface (at pH 7). Therefore it is concluded that just because MnO 2 is present in a filter bed, it does not necessarily mean that MnO 2 will be available to oxidise As(III). However, unlike Fe(II), the addition of Fe(III) did not hinder As(III) oxidation on the MnO 2 surface; resulting in subsequent effective As(V) removal by the flocculating hydrous ferric oxides. Copyright © 2016 Elsevier Ltd. All rights reserved.

Retention of Polyphenolic Species in Spray-Dried Blackberry Extract Using Mannitol as a Thermoprotectant

PubMed Central

Eldridge, Joshua A.; Repko, Debra

2014-01-01

Abstract The purpose of these studies was to determine if a Büchi Mini Spray Dryer B-290 (Büchi Corporation, New Castle, DE, USA) could be used to prepare blackberry extract powders containing mannitol as a thermoprotectant without extensively degrading anthocyanins and polyphenols in the resulting powders. Three blackberry puree extract samples were each prepared by sonication of puree in 30/70% ethanol/water containing 0.003% HCl. Blackberry puree extract sample 1 (S1) contained no mannitol, while blackberry puree extract sample 2 (S2) contained 3.0:1 (w/w) mannitol:berry extract, and blackberry puree extract sample 3 (S3) contained 6.3:1 (w/w) mannitol:berry extract. The levels of anthocyanins and polyphenols in reconstituted spray-dried powders produced from S1–S3 were compared to solutions of S1–S3 that were held at 4°C as controls. All extract samples could be spray-dried using the Büchi Mini Spray Dryer B-290. S1, with no mannitol, showed a 30.8% decrease in anthocyanins and a 24.1% decrease in polyphenols following spray-drying. However, S2 had a reduction in anthocyanins of only 13.8%, while polyphenols were reduced by only 6.1%. S3, with a ratio of mannitol to berry extract of 6.3:1, exhibited a 12.5% decrease in anthocyanins while the decrease in polyphenols after spray-drying was not statistically significant (P=.16). Collectively, these data indicate that a Büchi Mini Spray Dryer B-290 is a suitable platform for producing stable berry extract powders, and that mannitol is a suitable thermoprotectant that facilitates retention of thermosensitive polyphenolic species in berry extracts during spray-drying. PMID:24892214

Process Simulation of Cold Pressing and Sintering of Armstrong CP-Ti Powders

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

Gorti, Sarma B; Sabau, Adrian S; Peter, William H

A computational methodology is presented for the process simulation of cold pressing and sintering of Armstrong CP-Ti powders. Since the powder consolidation is governed by specific pressure-dependent constitutive equations, solution algorithms were developed for the ABAQUS user material subroutine, UMAT, for computing the plastic strain increments based on an implicit integration of the nonlinear yield function, flow rule, and hardening equations. Sintering was simulated using a model based on diffusional creep using the user subroutine CREEP. The initial mesh, stress, and density for the simulation of sintering were obtained from the results of the cold pressing simulation, minimizing the errorsmore » from decoupling the cold pressing and sintering simulations. Numerical simulation results are presented for the cold compaction followed by a sintering step of the Ti powders. The numerical simulation results for the relative density were compared to those measured from experiments before and after sintering, showing that the relative density can be accurately predicted. Notice: This manuscript has been authored by UT-Battelle, LLC, under Contract No. DE-AC05-00OR22725 with the U.S. Department of Energy. The United States Government retains and the publisher, by accepting the article for publication, acknowledges that the United States Government retains a non-exclusive, paid-up, irrevocable, world-wide license to publish or reproduce the published form of this manuscript, or allow others to do so, for United States Government purposes. ACKNOWLEDGEMENTS This research was sponsored by the U.S. DOE, and carried out at ORNL, under Contract DE-AC05-00OR22725 with UT-Battelle, LLC. This research was sponsored by the U.S. DOE, EERE Industrial Technology Program Office under CPS Agreement # 17881.« less

Laser-aided Directed Metal Deposition of Ni-based superalloy powder

NASA Astrophysics Data System (ADS)

Caiazzo, Fabrizia

2018-07-01

The subject of repairing Ni-based parts with state-of-the-art technologies is increasingly addressed both for research and industrial purposes, aiming to cost saving mainly in aerospace and automotive. In this frame, laser-aided Directed Metal Deposition (DMD) with injection of powder is investigated in this paper since minimal distortion of the work-piece, reduced heat-affected zones and better surface quality are benefited in comparison with conventional techniques. Actual application to overhaul Ni-based components is aimed, therefore homologous powder is fed by means of a 3-way feeding nozzle over the substrate; a disc laser is used as heat source. The chemical composition of both the substrate and the powder is preliminarily investigated via areal and punctual EDS inspections. A 2-factor, 2-level experimental plan is drawn to discuss the main effects of the processing variables laser power and processing speed. Namely, the resulting trends are given and compared with similar findings in the literature. Interestingly, dilution as a measure of metal affection is found to be lower than 25%, hence the operating window is deemed to be suitable for both repairing and fabrication of parts. Eventually, repairing by means of side overlapping and multi-level deposition traces on artificial square-shaped grooves is performed: indeed, similar slots are made before DMD to preliminarily remove any local imperfection upon improper casting of the part in the actual industrial process. Although a number of micropores are found, the process is deemed to comply with usual referred standards; in particular, a proper processing window has been found to prevent the occurrence of hot cracking which usually affects the compliance to stress.

Microstructure of as-fabricated UMo/Al(Si) plates prepared with ground and atomized powder

NASA Astrophysics Data System (ADS)

Jungwirth, R.; Palancher, H.; Bonnin, A.; Bertrand-Drira, C.; Borca, C.; Honkimäki, V.; Jarousse, C.; Stepnik, B.; Park, S.-H.; Iltis, X.; Schmahl, W. W.; Petry, W.

2013-07-01

UMo-Al based fuel plates prepared with ground U8wt%Mo, ground U8wt%MoX (X = 1 wt%Pt, 1 wt%Ti, 1.5 wt%Nb or 3 wt%Nb) and atomized U7wt%Mo have been examined. The first finding is that that during the fuel plate production the metastable γ-UMo phases partly decomposed into two different γ-UMo phases, U2Mo and α'-U in ground powder or α″-U in atomized powder. Alloying small amounts of a third element to the UMo had no measurable effect on the stability of the γ-UMo phase. Second, the addition of some Si inside the Al matrix and the presence of oxide layers in ground and atomized samples is studied. In the case with at least 2 wt%Si inside the matrix a Silicon rich layer (SiRL) forms at the interface between the UMo and the Al during the fuel plate production. The SiRL forms more easily when an Al-Si alloy matrix - which is characterized by Si precipitates with a diameter ⩽1 μm - is used than when an Al-Si mixed powder matrix - which is characterized by Si particles with some μm diameter - is used. The presence of an oxide layer on the surface of the UMo particles hinders the formation of the SiRL. Addition of some Si into the Al matrix [7-11]. Application of a protective barrier at the UMo/Al interface by oxidizing the UMo powder [7,12]. Increase of the Mo content or use of UMo alloys with ternary element addition X (e.g. X = Nb, Ti, Pt) to stabilize the γ-UMo with respect to α-U or to control the UMo-Al interaction layer kinetics [9,12-24]. Use of ground UMo powder instead of atomized UMo powder [10,25] The points 1-3 are to limit the formation of the undesired UMo/Al layer. Especially the addition of Si into the matrix has been suggested [3,7,8,10,11,26,27]. It has been often mentioned that Silicon is efficient in reducing the Uranium-Aluminum diffusion kinetics since Si shows a higher chemical affinity to U than Al to U. Si suppresses the formation of brittle UAl4 which causes a huge swelling during the irradiation. Furthermore it enhances the formation of more stable UAl3 within the diffusion layer [14]. In addition, Si will not notably influence the reactor neutronics due to its low absorption cross section for thermal neutrons of σabs = 0.24 barn. Aluminum has σabs = 0.23 barn.Williams [28], Bierlein [29], Green [30] and de Luca [31] showed the first time in the 1950s that alloying Aluminum with some Silicon reduces the Uranium-Aluminum diffusion kinetics in can-type fuel elements. However, up to now uncertainties remained about the most promising Si concentration and the involved mechanisms.Ground powder - possibility 4 - introduces a high density of defects like dislocations, oxide layers and impurities into UMo grains. Fuel prepared with this kind of powder exhibits a larger porosity. It may also be combined with an AlSi matrix. As a consequence, the degree of swelling due to high-burn up is reduced compared to fuel with atomized powder [5,6,25].This study focuses on the metallurgical characterization of as-fabricated samples prepared with ground UMo and UMoX (X = Ti, Nb, Pt) powders and atomized UMo powder. The influence of some Si into the Al matrix and the presence of oxide layers on the UMo is discussed. Details of the differences of samples with ground UMo from atomized UMo will be discussed.The examined samples originate from non-irradiated spare fuel plates from the IRIS-TUM irradiation campaign [5,6]. The samples containing ground UMoX powders and atomized UMo powders with Si addition into the matrix have been produced for this study [32]. Powder mixing: The UMo powder is mixed with Al powder. Compact production: UMo-Al powder is poured into a mould and undergoes compaction under large force. Plate-processing: An AlFeNi frame is placed on an AlFeNi plate and the UMo-Al compact is placed into the frame. Afterwards it is covered with a second AlFeNi plate. This assembly is hot-rolled to reduce the total thickness to 1.4 mm. Subsequently, a blister test (1-2 h at 400-450 °C) ensures that the fuelplate is sealed. After this step, the UMo particles are tightly covered with Al as shown in Fig. 1. To access the meat layer, small samples have been cut from the fuel plates. The AlFeNi cladding has been removed using abrasive paper and diamond polishing paste. Cross sections were prepared from each sample and examined using SEM/EDX and XRD. Laboratory scale XRD Laboratory sealed-tube XRD on a STOE-STADIP diffractometer equipped with an incident beam focusing monochromator and used in reflection geometry with respect to the sample. MoK-α radiation has been used. Details on the systems used can be found in [39]. mu;-XRD using micro-focused synchrotron radiation at the Swiss Light Source μ-XAS beamline (PSI, Switzerland). At SLS, the beam size was 3 × 3 μm2, the energy was 19.7 keV. Further details on the experimental procedure can be found in [40]. Only very small sample volumes are probed with this technique, therefore the results may not be representative for the whole miniplate. The standard deviation of the lattice parameters obtained with this method is ±0.01 Å in case not different given. High-energy XRD (HE-XRD) in transmission mode using synchrotron radiation at the "High Energy Diffraction and Scattering Beamline ID15B" of ESRF. An X-ray energy of 87 keV has been used, the beam size was 0.3 × 0.3 mm2. Details on the experimental procedure are presented in [41,42]. It was possible to determine the average mass fractions of the phases present inside the sample using this technique. The standard deviation of the lattice parameters obtained with this method is ±0.001 Å in case not different given. laser granulometry to determine the size distribution of the particles, XRD for phase identification. Granulometry measurements showed that a significant amount of very fine particles of a few μm to 10 μm size are present in the first class of powder.In both cases, laboratory XRD analyses evidenced only two phases: γ-UMo and UO2. In contrast to observations on the final fuel plates, there are no signs of α-U. Comparing XRD data of atomized UMo powder (taken form the IRIS4 experiment) and ground UMo powder with almost the same Mo content, the peaks are broader in XRD patterns of ground UMo and there is a higher background [44]. This points that the lattice structure of the UMo inside the ground powder is strongly disordered during the grinding process.Complementary investigations were performed in these ground UMo powder samples using HE-XRD. The obtained data can therefore directly be compared to those measured on pre-oxidized atomized UMo powders [45] and IRIS-TUM fuel plates [41]. For both powder samples the γ-UMo lattice constant has been estimated to 3.433 ± 0.002 Å which corresponds to about 7.2 wt% for Mo in the alloy according to Dwight's law [46]. The existence of two UMo phases inside these ground particles (as in atomized case) could not be investigated because of the huge peak broadening (presence of micro distortions). Whatever the sample granulometry, the analysis of the HE-XRD data showed a non-negligible nitride contamination in ground powders (see Fig. 2). Two uranium nitride phases are indeed found in these samples: UN and U2N3+x[47]. Note that the presence of UN has also been found in the as-fabricated plates. These results confirm the high reactivity of UMo with both Oxygen and Nitrogen in the grinding conditions. As a comparison for temperatures in the 200-250 °C range, it seems that UNx phases are more difficult to grow: they were not present in outer layers obtained by heat treatment under air on atomized particles [45]. Finally it can be seen in Table 3 that the weight fractions of UO2 and U2N3+x phases are lower in the sample with larger UMo particles. This suggests the existence of an oxide, nitride outer shell around UMo ground particle with thickness that does not strongly evolve with particle size. This constant outer shell thickness has also been found in pre-oxidized atomized powders [45].The UMoX powder used for the samples MAFIA-I-18 - MAFIA-I-21 has not been investigated prior to plate fabrication. However, since the grinding process is essentially the same as for the pure UMo powder, similar characteristics are assumed. Thin oxide layers with a thickness ⩽1 μm on some of the particles that were not intentionally oxidized. Although the UMo powder was stored and handled under an inert atmosphere over the whole production process, some residual oxygen has reacted with the UMo. Already this thin oxide layers exhibits cracks (Fig. 5). Thicker oxide layers with a thickness up to 5 μm on the UMo particles that were oxidized purposely. This kind of oxide layer is very brittle and shows large cracks (Fig. 6). The oxidized UMo particles tend to detach with the matrix as gaps between the UMo particles and the oxide layer could be observed (Fig. 6). This is most obvious at spots where a UMo particle has been pulled out during polishing. A part of the oxide layer remained inside the resulting hole (Fig. 7). Atomized UMo powder 2 wt%Si in Al matrix, alloyed AlSi 2 wt%Si in Al matrix, mixed AlSi 5 wt%Si in Al matrix, mixed AlSi 7 wt%Si in Al matrix, mixed AlSi Ground UMo powder 2 wt%Si in Al matrix, alloyed AlSi The influence of an oxide layer around the UMo particles on the formation of the SiRL during fuel plate production is further discussed. The growth of a Si rich layer surrounding the UMo particles in the 2 wt%Si alloyed powder (oxidized UMo), as well as the 5 wt% and 7 wt%Si mixed powder (non-oxidized UMo) during production of the miniplates. The presence of Si precipitates in the Al-matrix (large precipitates in case of mixture, small si particles in alloy). No oxide layer: If no oxide layer is present around the UMo particles a homogeneous SiRL grows at the interface UMo-Al (Fig. 15a). Brittle oxide layer: An oxide layer is present around the UMo particles, the SiRL grows always between the UMo particle and the oxide layer (Fig. 15b). In this case the the SiRL is thin and not homogeneous. As presumed by Ripert et al. [7] it is essential that the oxide layer reveals cracks perpendicular the UMo particle surface to make path for the Si diffusion. Dense oxide layer: In case of a thin (≈1 μm) but compact oxide layer no SiRL is formed even at high Si concentrations inside the matrix (Fig. 15c). The observed effects are pronounced when the thickness of the oxide layer is increased, as shown in Fig. 16: UMo particles covered with a thicker oxide layer (>1 μm) inside an Aluminum matrix with 5 wt%Si (mixed Al-Si powder). The oxide layer is dense at the left side of the particle, no Si can be found there (Fig. 16a). In contrast, the brittle and cracked oxide layer on the right side made path for a Si diffusion but the SiRL is thinner than in the sites where the UMo particle is not covered with an oxide layer. EDX maps at different positions of the sample showed that in general no SiRL forms around UMo particles covered by oxide layers with a thickness greater than 1 μm (Fig. 16b). This behavior is identical for the samples with 5 wt%Si and 7 wt%Si added to the Aluminum matrix (mixed Al-Si powder). Obviously the presence of a (dense) oxide layer hampers the formation of a SiRL. different UXSiY phases with strongly overlapping peaks can be found in the SiRL, these phases are characterized by small sizes of the crystallites (a few tens of nanometers) and/or cell parameter gradients. Two different crystallographic phases have been usually identified: U(Al,Si)3 displaying a small lattice parameter of a0 = 4.16 Å. This indicates that about 40% of the Al lattice sites are occupied by Si atoms. The second phase is isostructural to U3Si54 with a different lattice parameter [59-61]. Although the U-Si-Al phase diagram contains a variety of phases, none of the phases reported in literature [62] could be used to fully refine the measured diagram. Therefore, three different hypotheses are suggested to explain the occurence of this unknown phase: The observed compound consists of two phases: Conventional U3Si5 and USi2, as has been suggested by the authors before [58]. However, only one literature source (Brown et al.) describing the occurrence of USi2 below 450 °C could be found [63,64]. Furthermore, it has not been possible to reproduce the experiments described by Brown et al. Therefore, this hypothesis remains doubtful [59]. The observed phase may be a new unknown phase. For example, a cubic phase with lattice constant a0 = 3.96 Å can be used to refine the observed peaks. This hypothesis can neither be confirmed nor refused based on the existing data. The observed phase can be a U3Si5 variant containing Mo and/or Al atoms. This hypothesis is supported by the authors. Hence in the following sections this structure will be denoted as U3Si5. No traces of SiRL phases are found inside the sample with 2 wt%Si mixed-powder matrix (MAFIA-I-3), all the Si remained inside the matrix. A SiRL is present inside the samples with 2.1 wt%Si alloyed powder matrix (MAFIA-I-4) and 5 wt%Si (MAFIA-I-5) and 7 wt%Si (MAFIA-I-7) mixed powder matrix. However, between 76% and 96% of the Si remained inside the matrix in form of precipitates or Si particles. The SiRL is formed readily when the Si is present inside the matrix in form of precipitates (i.e. Al-Si alloy matrix, MAFIA-I-4 and IRIS-TUM 8502) compared to particles (i.e. Al-Si mixed powder matrix, MAFIA-I-3, MAFIA-I-5 and MAFIA-I-7). This behavior can best be observed on the sample prepared with ground powder and with 2.1 wt%Si alloyed powder matrix (IRIS-TUM-8502): The matrix contains no Si, only SiRL phases are found. Since the sample with 5 wt%Si mixed powder matrix (MAFIA-I-5) has the lowest SiRL fraction but by far the highest UO2 content, it is concluded that the presence of UO2 around the UMo kernels tends to hamper the formation of a SiRL. UMo/Al samples prepared with ground powder contain irregularly shaped UMo kernels. They are in general oxidized and also contain oxide stringers. These samples have a high porosity content of around 8 vol%. In contrast, UMo/Al samples prepared with atomized powder contain spherical UMo kernels. Only the surface of the UMo kernels is oxidized in some cases. Thick oxide layers must be grown intentionally while thinner layers are the result of oxidation during the whole process. The oxide layer is in general brittle and exhibits cracks. The Uranium-oxide content of all examined samples (atomized and ground) varies between 2 and 13 wt%. gamma;-UMo present in the fresh UMo powder destabilizes to transform to an α-U-like phase, U2Mo, and two γ-UMo phases with different Mo content during the fuel plate production. For ground powder, α-U content varies in 28-38 wt%, for atomized powder in 11-14 wt%. The degree of γ-phase destabilization is therefore higher for ground powder. Ternary addition of Nb, Ti or Pt to the UMo did not impact the extent of decomposition. The γ-phase decomposition in the atomized and ground powder does not follow the expected in the U8wt%Mo TTT diagram between 400 and 450 °C [41]. According to Repas et al. [65], the route is γ-UMoa → γ-UMob + α-U → γ-UMoc+α-U + U2Mo . γ-UMoa,b,c differ in the Mo content where γ-UMoa has the lowest and γ-UMoc has the highest Mo content. We observe a new route of decomposition of ground powder into two different γ-UMo phases. One of them has approximately the original Mo content and the other has a higher Mo content. Further U2Mo and a phase with deformed lattice parameters compared to pure α-U have been observed. The latter is known as α' in literature.For atomized powder, also two different γ-UMo phases and traces of U2Mo have been found. However, a different α-U like phase has been identified: α″ [41,53-55].Repas et al. used as cast samples that have been examined with conventional XRD and different metallographic methods [65]. The difference to our data can be explained by the superior resolution of the here used HE-XRD diffraction. Most probably, conventional lab X-ray sourcces could not resolve fine differences in the lattice parameters of α-U and may not enable to separate two γ-UMo phase. To overcome this uncertainty it is highly desirable to examine the TTT diagram of UMo with high resolution. When Si is added into the matrix - by using alloyed Al-Si powder as a matrix or blending Al and Si powder - in general a SiRL is formed at the interface between the UMo and the Al matrix. An exception can be found in MAFIA-I-3 in which the overall Si content was to low to form a SiRL. The SiRL consists of U(Al,Si)3 and U3Si5. The SiRL forms less readily in case of mixed Al-Si than in case of alloyed Al-Si powder. In the latter case (MAFIA-I-4), a Si depleted zone has been observed around the UMo particles. For ground powder in combination with an Al-Si alloyed matrix, the entire Si from the matrix has reacted with the UMo forming SiRL phases. The presence of a dense oxide layer around the UMo kernels can prevent the formation of a SiRL. However, as soon as the oxide layer is cracked a SiRL forms between the UMo and the oxide layer. A dense oxide layer isolates the UMo from the Si inside the matrix and occurring cracks make path for the diffusion of Si towards the UMo. U3Si 5 is also called USi2-x or USi1.66 in literature.

Effects of air-polishing powders on color stability of composite resins.

PubMed

Güler, Ahmet Umut; Duran, Ibrahim; Yücel, Ali Çağin; Ozkan, Pelin

2011-10-01

The purpose of this study was to investigate the effect of different air-polishing powders on the color stability of different types of composite resin restorative materials. Thirty cylindrical specimens (15×2 mm) were prepared for each of 7 composite resin restorative materials. All specimens were polished with a series of aluminum oxide polishing discs (Sof-Lex). The prepared specimens of each composite resin were randomly divided into 3 groups of 10 specimens each, for control (Group-C) and two air-powder applications (Group-CP: Cavitron Prophy-Jet; Group-PS: Sirona ProSmile prophylaxis powder). A standard air-polishing unit (ProSmile Handly) was used. All specimens were air-powdered for 10 s at 4-bar pressure. The distance of the spray nosel from the specimens was approximately 10 mm and angulation of the nosel was 90°. Specimens were stored in 100 mL of coffee (Nescafe Classic) for 24 h at 37°C. Color measurement of all specimens was recorded before and after exposure to staining agent with a colorimeter (Minolta CR-300). Color differences (∆E*) between the 2 color measurements (baseline and after 24 h storage) were calculated. The data were analyzed with a 2-way ANOVA test, and mean values were compared by the Tukey HSD test (p<0.05). According to the 2-way ANOVA results, composite resin restorative materials, air-polishing powders, and their interaction were statistically significant (p<0.05) For Aelite Aesthetic Enemal, Filtek Z250, Grandio, CeramX Mono, and Quixfil composite resin restorative materials, no significant difference was observed between Group-PS and Group-CP (p>.05) and these groups demonstrated the highest ∆E* values. For Filtek Silorane and IntenS, the highest ∆E* values were observed in Group-PS. The lowest ∆E* values for all composite resin groups were observed in Group-C. When comparing the 7 composite resin restorative materials, Aelite Aesthetic Enemal demonstrated significantly less ∆E* values than the other composite resins tested. The highest ∆E* values were observed in Quixfil. Except for Quixfil, all control groups of composite resins that were polished Sof-Lex exhibited clinically acceptable ∆E values (<3.7). Air-polishing applications increased the color change for all composite resin restorative materials tested. Composite restorations may require re-polishing after air-polishing.

Effects of air-polishing powders on color stability of composite resins

PubMed Central

GÜLER, Ahmet Umut; DURAN, Ibrahim; YÜCEL, Ali Çagin; ÖZKAN, Pelin

2011-01-01

Objectives The purpose of this study was to investigate the effect of different air-polishing powders on the color stability of different types of composite resin restorative materials. Material and methods Thirty cylindrical specimens (15×2 mm) were prepared for each of 7 composite resin restorative materials. All specimens were polished with a series of aluminum oxide polishing discs (Sof-Lex). The prepared specimens of each composite resin were randomly divided into 3 groups of 10 specimens each, for control (Group-C) and two air-powder applications (Group-CP: Cavitron Prophy-Jet; Group-PS: Sirona ProSmile prophylaxis powder). A standard air-polishing unit (ProSmile Handly) was used. All specimens were air-powdered for 10 s at 4-bar pressure. The distance of the spray nosel from the specimens was approximately 10 mm and angulation of the nosel was 90º. Specimens were stored in 100 mL of coffee (Nescafe Classic) for 24 h at 37ºC. Color measurement of all specimens was recorded before and after exposure to staining agent with a colorimeter (Minolta CR-300). Color differences (∆E*) between the 2 color measurements (baseline and after 24 h storage) were calculated. The data were analyzed with a 2-way ANOVA test, and mean values were compared by the Tukey HSD test (p≤0.05). Results According to the 2-way ANOVA results, composite resin restorative materials, air-polishing powders, and their interaction were statistically significant (p<0.05) For Aelite Aesthetic Enemal, Filtek Z250, Grandio, CeramX Mono, and Quixfil composite resin restorative materials, no significant difference was observed between Group-PS and Group-CP (p>.05) and these groups demonstrated the highest ∆E* values. For Filtek Silorane and IntenS, the highest ∆E* values were observed in Group-PS. The lowest ∆E* values for all composite resin groups were observed in Group-C. When comparing the 7 composite resin restorative materials, Aelite Aesthetic Enemal demonstrated significantly less ∆E* values than the other composite resins tested. The highest ∆E* values were observed in Quixfil. Conclusion Except for Quixfil, all control groups of composite resins that were polished Sof-Lex exhibited clinically acceptable ∆E values (<3.7). Air-polishing applications increased the color change for all composite resin restorative materials tested. Composite restorations may require re-polishing after air-polishing. PMID:21922122

Predictive modeling, simulation, and optimization of laser processing techniques: UV nanosecond-pulsed laser micromachining of polymers and selective laser melting of powder metals

NASA Astrophysics Data System (ADS)

Criales Escobar, Luis Ernesto

One of the most frequently evolving areas of research is the utilization of lasers for micro-manufacturing and additive manufacturing purposes. The use of laser beam as a tool for manufacturing arises from the need for flexible and rapid manufacturing at a low-to-mid cost. Laser micro-machining provides an advantage over mechanical micro-machining due to the faster production times of large batch sizes and the high costs associated with specific tools. Laser based additive manufacturing enables processing of powder metals for direct and rapid fabrication of products. Therefore, laser processing can be viewed as a fast, flexible, and cost-effective approach compared to traditional manufacturing processes. Two types of laser processing techniques are studied: laser ablation of polymers for micro-channel fabrication and selective laser melting of metal powders. Initially, a feasibility study for laser-based micro-channel fabrication of poly(dimethylsiloxane) (PDMS) via experimentation is presented. In particular, the effectiveness of utilizing a nanosecond-pulsed laser as the energy source for laser ablation is studied. The results are analyzed statistically and a relationship between process parameters and micro-channel dimensions is established. Additionally, a process model is introduced for predicting channel depth. Model outputs are compared and analyzed to experimental results. The second part of this research focuses on a physics-based FEM approach for predicting the temperature profile and melt pool geometry in selective laser melting (SLM) of metal powders. Temperature profiles are calculated for a moving laser heat source to understand the temperature rise due to heating during SLM. Based on the predicted temperature distributions, melt pool geometry, i.e. the locations at which melting of the powder material occurs, is determined. Simulation results are compared against data obtained from experimental Inconel 625 test coupons fabricated at the National Institute for Standards & Technology via response surface methodology techniques. The main goal of this research is to develop a comprehensive predictive model with which the effect of powder material properties and laser process parameters on the built quality and integrity of SLM-produced parts can be better understood. By optimizing process parameters, SLM as an additive manufacturing technique is not only possible, but also practical and reproducible.

Preparation of tris(8-hydroxyquinolinato)aluminum thin films by sputtering deposition using powder and pressed powder targets

NASA Astrophysics Data System (ADS)

Kawasaki, Hiroharu; Ohshima, Tamiko; Yagyu, Yoshihito; Ihara, Takeshi; Tanaka, Rei; Suda, Yoshiaki

2017-06-01

Tris(8-hydroxyquinolinato)aluminum (Alq3) thin films, for use in organic electroluminescence displays, were prepared by a sputtering deposition method using powder and pressed powder targets. Experimental results suggest that Alq3 thin films can be prepared using powder and pressed powder targets, although the films were amorphous. The surface color of the target after deposition became dark brown, and the Fourier transform infrared spectroscopy spectrum changed when using a pressed powder target. The deposition rate of the film using a powder target was higher than that using a pressed powder target. That may be because the electron and ion densities of the plasma generated using the powder target are higher than those when using pressed powder targets under the same deposition conditions. The properties of a thin film prepared using a powder target were almost the same as those of a film prepared using a pressed powder target.

77 FR 28252 - Oral Dosage Form New Animal Drugs; Change of Sponsor; Griseofulvin Powder; Levamisole...

Federal Register 2010, 2011, 2012, 2013, 2014

2012-05-14

... Hydrochloride Powder; Oxytetracycline Powder AGENCY: Food and Drug Administration, HHS. ACTION: Final rule..., levamisole hydrochloride soluble powder, and oxytetracycline hydrochloride soluble powder from Teva Animal... Griseofulvin Powder, ANADAs 200-146 and 200-247 for Oxytetracycline Hydrochloride Soluble Powder, and ANADAs...

Toward a durable superhydrophobic aluminum surface by etching and ZnO nanoparticle deposition.

PubMed

Rezayi, Toktam; Entezari, Mohammad H

2016-02-01

Fabrication of suitable roughness is a fundamental step for acquiring superhydrophobic surfaces. For this purpose, a deposition of ZnO nanoparticles on Al surface was carried out by simple immersion and ultrasound approaches. Then, surface energy reduction was performed using stearic acid (STA) ethanol solution for both methods. The results demonstrated that ultrasound would lead to more stable superhydrophobic Al surfaces (STA-ZnO-Al-U) in comparison with simple immersion method (STA-ZnO-Al-I). Besides, etching in HCl solution in another sample was carried out before ZnO deposition for acquiring more mechanically stable superhydrophobic surface. The potentiodynamic measurements demonstrate that etching in HCl solution under ultrasound leads to superhydrophobic surface (STA-ZnO-Al(E)-U). This sample shows remarkable decrease in corrosion current density (icorr) and long-term stability improvement versus immersion in NaCl solution (3.5%) in comparison with the sample prepared without etching (STA-ZnO-Al-U). Scanning electron micrograph (SEM) and energy-dispersive X-ray spectroscopy (EDX) confirmed a more condense and further particle deposition on Al substrate when ultrasound was applied in the system. The crystallite evaluation of deposited ZnO nanoparticles was carried out using X-ray diffractometer (XRD). Finally, for STA grafting verification on Al surface, Fourier transform infrared in conjunction with attenuated total reflection (FTIR-ATR) was used as a proper technique. Copyright © 2015 Elsevier Inc. All rights reserved.

Hydroxyapatite electrodeposition on anodized titanium nanotubes for orthopedic applications

NASA Astrophysics Data System (ADS)

Parcharoen, Yardnapar; Kajitvichyanukul, Puangrat; Sirivisoot, Sirinrath; Termsuksawad, Preecha

2014-08-01

Nanotubes modification for orthopedic implants has shown interesting biological performances (such as improving cell adhesion, cell differentiation, and enhancing osseointegration). The purpose of this study is to investigate effect of titanium dioxide (TiO2) nanotube feature on performance of hydroxyapatite-coated titanium (Ti) bone implants. TiO2 nanotubes were prepared by anodization using ammonium fluoride electrolyte (NH4F) with and without modifiers (PEG400 and Glycerol) at various potential forms, and times. After anodization, the nanotubes were subsequently annealed. TiO2 nanotubes were characterized by scanning electron microscope and X-ray diffractometer. The amorphous to anatase transformation due to annealing was observed. Smooth and highly organized TiO2 nanotubes were found when high viscous electrolyte, NH4F in glycerol, was used. Negative voltage (-4 V) during anodization was confirmed to increase nanotube thickness. Length of the TiO2 nanotubes was significantly increased by times. The TiO2 nanotube was electrodeposited with hydroxyapatite (HA) and its adhesion was estimated by adhesive tape test. The result showed that nanotubes with the tube length of 560 nm showed excellent adhesion. The coated HA were tested for biological test by live/dead cell straining. HA coated on TiO2 nanotubes showed higher cells density, higher live cells, and more spreading of MC3T3-E1 cells than that growing on titanium plate surface.

Preparation of titanium diboride powder

DOEpatents

Brynestad, Jorulf; Bamberger, Carlos E.

1985-01-01

Finely-divided titanium diboride or zirconium diboride powders are formed by reacting gaseous boron trichloride with a material selected from the group consisting of titanium powder, zirconium powder, titanium dichloride powder, titanium trichloride powder, and gaseous titanium trichloride.

Aluminum powder metallurgy processing

NASA Astrophysics Data System (ADS)

Flumerfelt, Joel Fredrick

In recent years, the aluminum powder industry has expanded into non-aerospace applications. However, the alumina and aluminum hydroxide in the surface oxide film on aluminum powder require high cost powder processing routes. A driving force for this research is to broaden the knowledge base about aluminum powder metallurgy to provide ideas for fabricating low cost aluminum powder components. The objective of this dissertation is to explore the hypothesis that there is a strong linkage between gas atomization processing conditions, as-atomized aluminum powder characteristics, and the consolidation methodology required to make components from aluminum powder. The hypothesis was tested with pure aluminum powders produced by commercial air atomization commercial inert gas atomization and gas atomization reaction synthesis (GARS). The commercial atomization methods are bench marks of current aluminum powder technology. The GARS process is a laboratory scale inert gas atomization facility. A benefit of using pure aluminum powders is an unambiguous interpretation of the results without considering the effects of alloy elements. A comparison of the GARS aluminum powders with the commercial aluminum powders showed the former to exhibit superior powder characteristics. The powders were compared in terms of size and shape, bulk chemistry, surface oxide chemistry and structure, and oxide film thickness. Minimum explosive concentration measurements assessed the dependence of explosibility hazard on surface area, oxide film thickness, and gas atomization processing conditions. The GARS aluminum powders were exposed to different relative humidity levels, demonstrating the effect of atmospheric conditions on post-atomization oxidation of aluminum powder. An Al-Ti-Y GARS alloy exposed in ambient air at different temperatures revealed the effect of reactive alloy elements on post-atomization powder oxidation. The pure aluminum powders were consolidated by two different routes, a conventional consolidation process for fabricating aerospace components with aluminum powder and a proposed alternative. The consolidation procedures were compared by evaluating the consolidated microstructures and the corresponding mechanical properties. A low temperature solid state sintering experiment demonstrated that tap densified GARS aluminum powders can form sintering necks between contacting powder particles, unlike the total resistance to sintering of commercial air atomization aluminum powder.

Improved Pharmacokinetics of Sumatriptan With Breath Powered™ Nasal Delivery of Sumatriptan Powder

PubMed Central

Obaidi, Mohammad; Offman, Elliot; Messina, John; Carothers, Jennifer; Djupesland, Per G; Mahmoud, Ramy A

2013-01-01

Objectives.— The purpose of this study was to directly compare the pharmacokinetic (PK) profile of 22-mg sumatriptan powder delivered intranasally with a novel Breath Powered™ device (11 mg in each nostril) vs a 20-mg sumatriptan liquid nasal spray, a 100-mg oral tablet, and a 6-mg subcutaneous injection. Background.— A prior PK study found that low doses of sumatriptan powder delivered intranasally with a Breath Powered device were efficiently and rapidly absorbed. An early phase clinical trial with the same device and doses found excellent tolerability with high response rates and rapid onset of pain relief, approaching the benefits of injection despite significantly lower predicted drug levels. Methods.— An open-label, cross-over, comparative bioavailability study was conducted in 20 healthy subjects at a single center in the USA. Following randomization, fasted subjects received a single dose of each of the 4 treatments separated by a 7-day washout. Blood samples were taken pre-dose and serially over 14 hours post-dose for PK analysis. Results.— Quantitative measurement of residuals in used Breath Powered devices demonstrated that the devices delivered 8 ± 0.9 mg (mean ± standard deviation) of sumatriptan powder in each nostril (total dose 16 mg). Although the extent of systemic exposure over 14 hours was similar following Breath Powered delivery of 16-mg sumatriptan powder and 20-mg liquid nasal spray (area under the curve [AUC]0-∞ 64.9 ng*hour/mL vs 61.1 ng*hour/mL), sumatriptan powder, despite a 20% lower dose, produced 27% higher peak exposure (Cmax 20.8 ng/mL vs 16.4 ng/mL) and 61% higher exposure in the first 30 minutes compared with the nasal spray (AUC0-30 minutes 5.8 ng*hour/mL vs 3.6 ng*hour/mL). The magnitude of difference is larger on a per-milligram basis. The absorption profile following standard nasal spray demonstrated bimodal peaks, consistent with lower early followed by higher later absorptions. In contrast, the profile following Breath Powered delivery showed higher early and lower late absorptions. Relative to the 100-mg oral tablet (Cmax 70.2 ng/mL, AUC0-∞, 308.8 ng*hour/mL) and 6-mg injection (Cmax 111.6 ng/mL, AUC0-∞ 128.2 ng*hour/mL), the peak and overall exposure following Breath Powered intranasal delivery of sumatriptan powder was substantially lower. Conclusions.— Breath Powered intranasal delivery of sumatriptan powder is a more efficient form of drug delivery, producing a higher peak and earlier exposure with a lower delivered dose than nasal spray and faster absorption than either nasal spray or oral administration. It also produces a significantly lower peak and total systemic exposure than oral tablet or subcutaneous injection. PMID:23992438

Preparation of metal diboride powders

DOEpatents

Brynestad, J.; Bamberger, C.E.

Finely-divided titanium diboride or zirconium diboride powders are formed by reacting gaseous boron trichloride with a material selected from the group of consisting of titanium powder, zirconium powder, titanium dichloride powder, titanium trichloride powder, and gaseous titanium trichloride.

Antimicrobial eugenol nanoemulsion prepared by gum arabic and lecithin and evaluation of drying technologies.

PubMed

Hu, Qiaobin; Gerhard, Hannah; Upadhyaya, Indu; Venkitanarayanan, Kumar; Luo, Yangchao

2016-06-01

The purpose of present work was to develop eugenol oil nanoemulsions using gum arabic and lecithin as food grade natural emulsifiers, and study their antimicrobial activity. In addition, our study also evaluated different drying techniques (spray drying and freeze drying) on the morphology and redispersibility of nanoemulsion powders. The optimal fabrication method, physicochemical and structural characterization, stability, and antimicrobial activity were investigated. Results showed that nanoemusions with a particle size of 103.6±7.5nm were obtained by mixing aqueous phase (0.5% gum arabic, 0.5% lecithin, w/v) and eugenol oil (1.25%, w/v), which was premixed with ethanol (as a co-surfactant), followed by high speed homogenization process. The molecular interactions among emulsifiers and eugenol were evidenced by Fourier transform infrared spectroscopy. Buchi B-90 Nano Spray Dryer was evaluated as a powerful tool to obtain ultrafine spherical powders with a size of less than 500nm, compared to flake-like aggregation obtained by freeze-drying. The dried powders exhibited excellent re-dispersibility in water and maintained their physicochemical properties after re-hydration. The nanoemulsions did not adversely affect the antimicrobial activity of eugenol against Listeria monocytogenes and Salmonella Enteritidis. Therefore, the nanoemulsions have the potential to be applied in the food industry as a food preservative or sanitizer. Copyright © 2016 Elsevier B.V. All rights reserved.

Comparative measurements of mineral elements in milk powders with laser-induced breakdown spectroscopy and inductively coupled plasma atomic emission spectroscopy.

PubMed

Lei, W Q; El Haddad, J; Motto-Ros, V; Gilon-Delepine, N; Stankova, A; Ma, Q L; Bai, X S; Zheng, L J; Zeng, H P; Yu, J

2011-07-01

Mineral elements contained in commercially available milk powders, including seven infant formulae and one adult milk, were analyzed with inductively coupled plasma atomic emission spectrometry (ICP-AES) and laser-induced breakdown spectroscopy (LIBS). The purpose of this work was, through a direct comparison of the analytical results, to provide an assessment of the performance of LIBS, and especially of the procedure of calibration-free LIBS (CF-LIBS), to deal with organic compounds such as milk powders. In our experiments, the matrix effect was clearly observed affecting the analytical results each time laser ablation was employed for sampling. Such effect was in addition directly observed by determining the physical parameters of the plasmas induced on the different samples. The CF-LIBS procedure was implemented to deduce the concentrations of Mg and K with Ca as the internal reference element. Quantitative analytical results with CF-LIBS were validated with ICP-AES measurements and nominal concentrations specified for commercial milks. The obtained good results with the CF-LIBS procedure demonstrate its capacity to take into account the difference in physical parameters of the plasma in the calculation of the concentrations of mineral elements, which allows a significant reduction of the matrix effect related to laser ablation. We finally discuss the way to optimize the implementation of the CF-LIBS procedure for the analysis of mineral elements in organic materials.

Effects of La2O3 content and particle size on the long-term stability and thermal cycling property of La2O3-dispersed SUS430 alloys for SOFC interconnect materials

NASA Astrophysics Data System (ADS)

Lee, Jung-Won; Mehran, Muhammad Taqi; Song, Rak-Hyun; Lee, Seung-Bok; Lee, Jong-Won; Lim, Tak-Hyoung; Park, Seok-Joo; Hong, Jong-Eun; Shim, Joon-Hyung

2017-11-01

We developed oxide-dispersed alloys as interconnect materials for a solid oxide fuel cell by adding La2O3 to SUS430 ferritic steels. For this purpose, we prepared two types of La2O3 with different particle sizes and added different amounts of La2O3 to SUS430 powder. Then, we mixed the powders using a high energy ball mill, so that nano-sized as well as micro-sized oxide particles were able to mix uniformly with the SUS430 powders. After preparing hexahedral green samples using uni-axial and cold isostatic presses, we were finally able to obtain oxide-dispersed alloys having high relative densities after firing at 1,400 °C under hydrogen atmosphere. The nano-sized La2O3 dispersed alloys showed properties superior to those of micro-sized dispersed alloys in terms of long-term stability and thermal cycling. Moreover, we determined the optimum amounts of added La2O3. Finally we were able to develop a new oxide-dispersed alloy showing excellent properties of low area specific resistance (16.23 mΩ cm2) after 1000 h at 800 °C, and no degradation after 10 iterations of thermal cycling under oxidizing atmosphere.

EFFECT OF ULTRA-HIGH PRESSURE HOMOGENIZATION ON THE INTERACTION BETWEEN BOVINE CASEIN MICELLES AND RITONAVIR

PubMed Central

Corzo-Martínez, M.; Mohan, M.; Dunlap, J.; Harte, F.

2014-01-01

Purpose The aim of this work was to develop a milk-based powder formulation appropriate for pediatric delivery of ritonavir (RIT). Methods Ultra-high pressure homogenization (UHPH) at 0.1, 300 and 500 MPa was used to process a dispersion of pasteurized skim milk (SM) and ritonavir. Loading efficiency was determined by RP-HPLC-UV; characterization of RIT:SM systems was carried out by apparent average hydrodynamic diameter and rheological measurements as well as different analytical techniques including Trp fluorescence, UV spectroscopy, DSC, FTIR and SEM; and delivery capacity of casein micelles was determined by in vitro experiments promoting ritonavir release. Results Ritonavir interacted efficiently with milk proteins, especially, casein micelles, regardless of the processing pressure; however, results suggest that, at 0.1 MPa, ritonavir interacts with caseins at the micellar surface, whilst, at 300 and 500 MPa, ritonavir is integrated to the protein matrix during UHPH treatment. Likewise, in vitro experiments showed that ritonavir release from micellar casein systems is pH dependent; with a high retention of ritonavir during simulated gastric digestion and a rapid delivery under conditions simulating the small intestine environment. Conclusions Skim milk powder, especially, casein micelles are potentially suitable and efficient carrier systems to develop novel milk-based and low-ethanol powder formulations of ritonavir appropriate for pediatric applications. PMID:25270571

Additive Manufacturing of Single-Crystal Superalloy CMSX-4 Through Scanning Laser Epitaxy: Computational Modeling, Experimental Process Development, and Process Parameter Optimization

NASA Astrophysics Data System (ADS)

Basak, Amrita; Acharya, Ranadip; Das, Suman

2016-08-01

This paper focuses on additive manufacturing (AM) of single-crystal (SX) nickel-based superalloy CMSX-4 through scanning laser epitaxy (SLE). SLE, a powder bed fusion-based AM process was explored for the purpose of producing crack-free, dense deposits of CMSX-4 on top of similar chemistry investment-cast substrates. Optical microscopy and scanning electron microscopy (SEM) investigations revealed the presence of dendritic microstructures that consisted of fine γ' precipitates within the γ matrix in the deposit region. Computational fluid dynamics (CFD)-based process modeling, statistical design of experiments (DoE), and microstructural characterization techniques were combined to produce metallurgically bonded single-crystal deposits of more than 500 μm height in a single pass along the entire length of the substrate. A customized quantitative metallography based image analysis technique was employed for automatic extraction of various deposit quality metrics from the digital cross-sectional micrographs. The processing parameters were varied, and optimal processing windows were identified to obtain good quality deposits. The results reported here represent one of the few successes obtained in producing single-crystal epitaxial deposits through a powder bed fusion-based metal AM process and thus demonstrate the potential of SLE to repair and manufacture single-crystal hot section components of gas turbine systems from nickel-based superalloy powders.

Evaluation of the color durability of acrylic resin veneer materials after immersion in common beverages at different time intervals: A spectrophotometric study.

PubMed

Kohli, Shivani; Bhatia, Shekhar

2015-01-01

Proper function, esthetics, and cost are the prime factors to be considered while selecting bridge veneering materials. The purpose of the study is to evaluate color durability of acrylic veneer materials after immersion in common beverages at different time intervals. Spectrophotometer was used for taking color measurements based on the transmission of light through the specimens made of the selected materials which were Tooth moulding powder (DPI) and Acrylux (Ruthinium). Thirty specimens of standardized dimensions were prepared from each material. The specimens were divided into three groups of 10 each. One group of each material was immersed in tea (TajMahal) and another group of each material in cola (Pepsi) as the staining solutions. The remaining group of 10 from each material served as control and was stored in distilled water. Color measurements were obtained pre-immersion, and after 1, 15, and 30 days of immersion. Tooth moulding powder displayed better color durability than Acrylux over the 1 month immersion period in both staining solutions. Tea resulted in more discoloration compared to cola (Pepsi). The difference in the color durability of Acrylux and Tooth moulding powder may be attributed to the differences in the composition of tested resin veneering materials, i.e. their polar properties, which contribute to the absorption of staining solution, and the different brands and the strengths of the solutions.

Effect of amorphous phases during the hydraulic conversion of α-TCP into calcium-deficient hydroxyapatite.

PubMed

Hurle, Katrin; Neubauer, Juergen; Bohner, Marc; Doebelin, Nicola; Goetz-Neunhoeffer, Friedlinde

2014-09-01

Powders of α-tricalcium phosphate (α-TCP), which readily react with water to form calcium-deficient hydroxyapatite (CDHA), are frequently used in bone cements. As, for clinical applications, it is important to adjust the setting reaction of the cements to a reasonable reaction time, exact knowledge of the hydration mechanism is essential. It is known that prolonged milling results in partial amorphization of α-TCP powders and that dissolution of the amorphous phase significantly accelerates the hydration, but it is not clear yet when the amorphous phase reacts in comparison to the crystalline α-TCP. Therefore the aim of this study was to investigate the development of quantitative phase content of α-TCP samples during hydration. For this purpose, three α-TCP powders, containing 0, 16 and 71wt.% of amorphous phase (ATCP), were mixed with either deionized water or a 0.1M Na2HPO4 aqueous solution. The crystalline evolution of the paste was assessed quantitatively during the first 48h of hydration at 23°C by G-factor quantification. The present investigations demonstrate that ATCP reacted earlier than crystalline α-TCP. The results also suggest the formation of an X-ray amorphous phase during the hydraulic conversion formation of α-TCP into CDHA. Copyright © 2014 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Development of a New Technique for the Efficient Delivery of Aerosolized Medications to Infants on Mechanical Ventilation

PubMed Central

Longest, P. Worth; Tian, Geng

2014-01-01

Purpose To evaluate the efficiency of a new technique for delivering aerosols to intubated infants that employs a new Y-connector, access port administration of a dry powder, and excipient enhanced growth (EEG) formulation particles that change size in the airways. Methods A previously developed CFD model combined with algebraic correlations were used to predict delivery system and lung deposition of typical nebulized droplets (MMAD = 4.9 μm) and EEG dry powder aerosols. The delivery system consisted of a Y-connector [commercial (CM); streamlined (SL); or streamlined with access port (SL-port)] attached to a 4-mm diameter endotracheal tube leading to the airways of a 6-month-old infant. Results Compared to the CM device and nebulized aerosol, the EEG approach with an initial 0.9 μm aerosol combined with the SL and SL-port geometries reduced device depositional losses by factors of 3-fold and >10-fold, respectively. With EEG powder aerosols, the SL geometry provided the maximum tracheobronchial deposition fraction (55.7%), whereas the SL-port geometry provided the maximum alveolar (67.6%) and total lung (95.7%) deposition fractions, respectively. Conclusions Provided the aerosol can be administered in the first portion of the inspiration cycle, the proposed new method can significantly improve the deposition of pharmaceutical aerosols in the lungs of intubated infants. PMID:25103332

Optimizing adsorption of blue pigment from wastewater by nano-porous modified Na-bentonite using spectrophotometry based on response surface method

NASA Astrophysics Data System (ADS)

Moradi, Neshat; Salem, Shiva; Salem, Amin

2018-03-01

This work highlighted the effective activation of bentonite paste to produce nano-porous powder for removal of cationic dye from wastewater. The effects of activation parameters such as soda and moisture contents, ageing time and temperature were analyzed using response surface methodology (RSM). The significance of independent variables and their interactions were tested by blending the obtained powders with wastewater and then the adsorption was evaluated, spectrophotometrically. The experiments were carried out by preparation of pastes according to response surface methodology and central composite design, which is the standard method, was used to evaluate the effects and interactions of four factors on the treatment efficiency. RSM was demonstrated as an appropriate approach for optimization of alkali activation. The optimal conditions obtained from the desirable responses were 5.0 wt% soda and 45.0 wt% moisture, respectively in which the powder activation was carried out at 150 °C. In order to well understand the role of nano-structured material on dye removal, the adsorbents were characterized through X-ray diffraction, Fourier transform infrared spectroscopy, scanning electron microscopy and Brunauer-Emmett-Teller surface area measurement. Finally, the analysis clearly demonstrates that the dye removal onto prepared adsorbent is well fitted with Langmuir isotherm compared to the other isotherm models. The low cost of material and facile process support the further development for commercial application purpose.

Effect of particle size on mixing degree in dispensation.

PubMed

Nakamura, Hitoshi; Yanagihara, Yoshitsugu; Sekiguchi, Hiroko; Ohtani, Michiteru; Kariya, Satoru; Uchino, Katsuyoshi; Suzuki, Hiroshi; Iga, Tatsuji

2004-03-01

By using lactose colored with erythrocin, we examined the effect of particle size on mixing degree during the preparation of triturations with a mortar and pestle. We used powders with different distributions of particle sizes, i.e., powder that passed through 32-mesh but was trapped on a 42-mesh sieve (32/42-mesh powder), powder that passed through a 42-mesh sieve but was trapped on a 60-mesh sieve (42/60-mesh powder), powder that passed through a 60-mesh sieve but was trapped on a 100-mesh sieve (60/100-mesh powder), and powder that passes through a 100-mesh sieve (> 100-mesh powder). The mixing degree of colored powder and non-colored powder whose distribution of particle sizes was the same as that of the colored powder was excellent. The coefficient of variation (CV) value of the mixing degree was 6.08% after 40 rotations when colored powder was mixed with non-colored powder that both passed through a 100-mesh sieve. The CV value of the mixing degree was low in the case of mixing of colored and non-colored powders with different particle size distributions. After mixing, about 50% of 42/60-mesh powder had become smaller particles, whereas the distribution of particle sizes was not influenced by the mixing of 60/100-mesh powder. It was suggested that the mixing degree is affected by distribution of particle sizes. It may be important to determine the mixing degrees for drugs with narrow therapeutic ranges.

Illicit drug detection with laser 1: investigation of optimal parameters in stomach tissue

NASA Astrophysics Data System (ADS)

Özer, Ayşen Gürkan; Tabakoğlu, Haşim Özgür; Cengiz, Salih

2014-05-01

The main purpose of this study is to establish radiation-safe scanning of passersby at high security areas, such as airports and customs. The stomach was selected as the organ to be analyzed. In order to determine whether a substance found inside a human body as wrapped in a plastic bag is filled narcotics or not, many substances in white powder form including morphine-HCL were inspected. Inspection was carried out with on-ionizing radiation by irradiating stomach tissue with laser light. Optical transmittance of lamb stomach tissue was analyzed at different wavelengths. We showed that detection by 650-nm diode laser irradiation would be suitable for such a radiation-safe scan. Different materials were also investigated for absorptive properties, and closed system Raman studies were performed. The spectrum of a molecule found inside white powder placed behind the lamb stomach tissue was detected as a fingerprint. This allowed the detection of target substances without any physical contact or damage to the biological tissue.

Characterization of Effect of Support Structures in Laser Additive Manufacturing of Stainless Steel

NASA Astrophysics Data System (ADS)

Järvinen, Jukka-Pekka; Matilainen, Ville; Li, Xiaoyun; Piili, Heidi; Salminen, Antti; Mäkelä, Ismo; Nyrhilä, Olli

Laser additive manufacturing (LAM) of stainless steel is a layer wisetechnology for fabricating 3D parts from metal powder via selectively melting powder with laser beam. Support structures play a significant role in LAM process as they help to remove heat away from the process and on the other hand hold the work piece in its place. A successful design of support structures can help to achievea building process fast and inexpensive with high quality. Aimof this study was to characterize the usability of two types of support structures: web and tube supports. Purpose of this studywas also to analyze how suitable they are in two industrial application cases: case for dental application and case for jewelry application. It was concluded that the removability of web supports was much better than tube supports. It was noticed that support structures are an important part of LAM process and they strongly affect the manufacturability and the end quality of the part.

Development ceramic composites based on Al2O3, SiO2 and IG-017 additive

NASA Astrophysics Data System (ADS)

Kurovics, E.; Shmakova, A.; Kanev, B.; Gömze, L. A.

2017-02-01

Based on high purity alumina and quartz powders and IG-017 bio-original additives the authors have developed new ceramic composite materials for different industrial purposes. The main goal was to fine a material and morphological structures of high performance ceramic composites as frames for development complex materials for extreme consumptions in the future. For this the mixed powders of Al2O3 , SiO2 and IG-017 bio-original additive were uniaxially pressed at different compaction pressures into disc shapes and were sintered in electric kiln under air (1) and nitrogrn (2) atmosphere. The grain size distributions of the raw materials were determined by laser granulometry. There thermo-physical properties were also determined by derivatography. The prepared and sintered specimens were tested on geometrical sizes, microstructure and morphology by scanning electron microscopy, porosity and water absorption. In this work the authors present the results of their research and investigation.

Revised Subsurface Stratigraphic Framework of the Fort Union and Wasatch Formations, Powder River Basin, Wyoming and Montana

USGS Publications Warehouse

Flores, Romeo M.; Spear, Brianne D.; Purchase, Peter A.; Gallagher, Craig M.

2010-01-01

Described in this report is an updated subsurface stratigraphic framework of the Paleocene Fort Union Formation and Eocene Wasatch Formation in the Powder River Basin (PRB) in Wyoming and Montana. This framework is graphically presented in 17 intersecting west-east and north-south cross sections across the basin. Also included are: (1) the dataset and all associated digital files and (2) digital files for all figures and table 1 suitable for large-format printing. The purpose of this U.S. Geological Survey (USGS) Open-File Report is to provide rapid dissemination and accessibility of the stratigraphic cross sections and related digital data to USGS customers, especially the U.S. Bureau of Land Management (BLM), to facilitate their modeling of the hydrostratigraphy of the PRB. This report contains a brief summary of the coal-bed correlations and database, and is part of a larger ongoing study that will be available in the near future.

Ball mill tool for crushing coffee and cocoa beans base on fraction size sieving results

NASA Astrophysics Data System (ADS)

Haryanto, B.; Sirait, M.; Azalea, M.; Alvin; Cahyani, S. E.

2018-02-01

Crushing is one of the operation units that aimed to convert the size of solid material to be smoother particle’s size. The operation unit that can be used in this crushing is ball mill. The purpose of this study is to foresee the effect of raw material mass, grinding time, and the number of balls that are used in the ball mill tool related to the amount of raw material of coffee and cocoa beans. Solid material that has become smooth is then sieved with sieve mesh with size number: 50, 70, 100, and 140. It is in order to obtain the mass fraction that escaped from each sieve mesh. From the experiment, it can be concluded that mass percentage fraction of coffee powder is bigger than cocoa powder that escaped from the mesh. Hardness and humidity of coffee beans and cocoa beans have been the important factors that made coffee beans is easier to be crushed than cocoa beans.

Development of a Rational Design Space for Optimizing Mixing Conditions for Formation of Adhesive Mixtures for Dry-Powder Inhaler Formulations.

PubMed

Sarkar, Saurabh; Minatovicz, Bruna; Thalberg, Kyrre; Chaudhuri, Bodhisattwa

2017-01-01

The purpose of the present study was to develop guidance toward rational choice of blenders and processing conditions to make robust and high performing adhesive mixtures for dry-powder inhalers and to develop quantitative experimental approaches for optimizing the process. Mixing behavior of carrier (LH100) and AstraZeneca fine lactose in high-shear and low-shear double cone blenders was systematically investigated. Process variables impacting the mixing performance were evaluated for both blenders. The performance of the blenders with respect to the mixing time, press-on forces, static charging, and abrasion of carrier fines was monitored, and for some of the parameters, distinct differences could be detected. A comparison table is presented, which can be used as a guidance to enable rational choice of blender and process parameters based on the user requirements. Segregation of adhesive mixtures during hopper discharge was also investigated. Copyright © 2016 American Pharmacists Association®. Published by Elsevier Inc. All rights reserved.

Studies on the treatment of surface water using rajma seeds

NASA Astrophysics Data System (ADS)

Merlin, S. Babitha; Abirami, M.; Kumar, R. Suresh

2018-03-01

Indiscriminate disposal of wastewater with suspended solids have led to higher amount of pollution to the natural water bodies. Turbidity removal becomes an essential part in the water treatment when surface water is used for drinking purpose, this can be achieved by means of coagulation process. Coagulation process is the dosing of a coagulant in water, resulting in the destabilization of negatively charged particles. Commercial coagulants which were widely used can synthesize by-products in turn may pollute the environment and deteriorate the ecosystem at a slow rate. So, now-a-days natural coagulants are used as a potential substitute because it's biodegradable, ecofriendly and non-toxic. In this study, the turbid surface water samples were treated using powdered seeds of Rajma (natural coagulant) followed by variations in dosage, settling time and pH were also studied. From the results obtained, it was found that the Rajma seeds powder achieved 48.80% efficiency for 0.5 g/l of optimum dose at pH 6 for 20 min settling time respectively.

Silicon nitride/silicon carbide composite powders

DOEpatents

Dunmead, Stephen D.; Weimer, Alan W.; Carroll, Daniel F.; Eisman, Glenn A.; Cochran, Gene A.; Susnitzky, David W.; Beaman, Donald R.; Nilsen, Kevin J.

1996-06-11

Prepare silicon nitride-silicon carbide composite powders by carbothermal reduction of crystalline silica powder, carbon powder and, optionally, crystalline silicon nitride powder. The crystalline silicon carbide portion of the composite powders has a mean number diameter less than about 700 nanometers and contains nitrogen. The composite powders may be used to prepare sintered ceramic bodies and self-reinforced silicon nitride ceramic bodies.

Particle Morphology Effects on Flow Characteristics of PS304 Plasma Spray Coating Feedstock Powder Blend

NASA Technical Reports Server (NTRS)

Stanford, Malcolm K.; DellaCorte, Christopher; Eylon, Daniel

2002-01-01

The effects of BaF2-CaF 2 particle morphology on PS304 feedstock powder flow ability have been investigated. BaF2-CaF2 eutectic powders were fabricated by comminution (angular) and by gas atomization (spherical). The fluoride powders were added incrementally to the other powder constituents of the PS304 feedstock: nichrome, chromia, and silver powders. A linear relationship between flow time and concentration of BaF2-CaF2 powder was found. Flow of the powder blend with spherical BaF2-CaF2 was better than the angular BaF2-CaF2. Flow ability of the powder blend with angular fluorides decreased linearly with increasing fluoride concentration. Flow of the powder blend with spherical fluorides was independent of fluoride concentration. Results suggest that for this material blend, particle morphology plays a significant role in powder blend flow behavior, offering potential methods to improve powder flow ability and enhance the commercial potential. These findings may have applicability to other difficult-to-flow powders such as cohesive ceramics.

Review of the Methods for Production of Spherical Ti and Ti Alloy Powder

NASA Astrophysics Data System (ADS)

Sun, Pei; Fang, Zhigang Zak; Zhang, Ying; Xia, Yang

2017-10-01

Spherical titanium alloy powder is an important raw material for near-net-shape fabrication via a powder metallurgy (PM) manufacturing route, as well as feedstock for powder injection molding, and additive manufacturing (AM). Nevertheless, the cost of Ti powder including spherical Ti alloy has been a major hurdle that prevented PM Ti from being adopted for a wide range of applications. Especially with the increasing importance of powder-bed based AM technologies, the demand for spherical Ti powder has brought renewed attention on properties and cost, as well as on powder-producing processes. The performance of Ti components manufactured from powder has a strong dependence on the quality of powder, and it is therefore crucial to understand the properties and production methods of powder. This article aims to provide a cursory review of the basic techniques of commercial and emerging methods for making spherical Ti powder. The advantages as well as limitations of different methods are discussed.

Nanocomposites Derived From a Low-Color Aromatic Polyimide (CP2) and Amine-Functionalized Vapor-Grown Carbon Nanofibers: In Situ Polymerization and Characterization (Preprint)

DTIC Science & Technology

2007-01-01

small metal catalyst (e.g., ferrocene, Fe (CO)5, etc.). They have an outer diameter of 60-200 nm, a hollow core of 30-90 nm, and length on the order...diffractions (WAXS) of compression-molded samples were recorded with a Rigaku RU-200 diffractometer using Ni-filtered Cu KR radiation (40 kV, 100 mA, λ...attributable to the sp3 C-H and sp2 C-H defects as methane is used as the major component in the feedstock for its production . Based on hydrogen

New micro-beam beamline at SPring-8, targeting at protein micro-crystallography

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

Hirata, Kunio; Ueno, Go; Nisawa, Atsushi

2010-06-23

A new protein micro-crystallography beamline BL32XU at SPring-8 is under construction and scheduled to start operation in 2010. The beamline is designed to provide the stabilized and brilliant micro-beam to collect high-quality data from micro-crystals. The beamline consists of a hybrid in-vacuum undulator, a liquid-nitrogen cooled double crystal monochromator, and K-B focusing mirrors with large magnification factor. Development of data acquisition system and end station consists of high-precision diffractometer, high-efficiency area detector, sample auto-changer etc. are also in progress.

Investigation on thermo physical characteristics of ethylene glycol based Al:ZnO nanofluids

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

Kiruba, R., E-mail: krbranjini@gmail.com, E-mail: drkingson@karunya.edu; George, Ritty; Gopalakrishnan, M.

2015-06-24

The present work describes the experimental aspects of viscosity and thermal conductivity characteristics of nanofluids. Aluminium doped zinc oxide nanostructures were synthesized by chemical precipitation method. Ultrasonic technique is used to disperse the nanostructures in ethylene glycol. Structural and morphological properties of Al doped ZnO nanostructures are characterized using X-ray diffractometer and scanning electron microscopic technique. The effect of concentration and temperature on thermo-physical properties of Al/ZnO nanofluids is also investigated. The experimental results showed there is enhancement in thermal conductivity with rise in temperature which can be utilized for coolant application.

Role of Hf4+ Doping on Oxygen Grain Boundary Diffusion in Alumina

DTIC Science & Technology

2014-09-01

Statement of Purpose 56 Chapter 4. Experimental Procedure 57 4.1 Powder Processing 57 4.1.1 Hf02-doped Alumina 59 4.1.2 Other Alumina/Ni Composites 60...combination of five to ten other elements alloyed with nickel to achieve a significant improvement in properties such as creep, oxidation and so on, as...lifetime. Considering the growth of the alumina protective layer is a diffusion controUed- process , understanding the transport mechanisms of Al and O in the

LARC-TPI: A multi-purpose thermoplastic polyimide

NASA Technical Reports Server (NTRS)

St.clair, A. K.; St.clair, T. L.

1982-01-01

A linear thermoplastic polyimide, LARC-TPI, was characterized and developed for a variety of high temperature applications. In its fully imidized form, this material can be used as an adhesive for bonding metals such as titanium, aluminum, copper, brass, and stainless steel. LARC-TPI was evaluated as a thermoplastic for bonding large pieces of polyimide film to produce flexible, 100 void-free laminates for flexible circuit applications. The development of LARC-TPI as a potential molding powder, composite matrix resin, high temperature film and fiber is also discussed.

High gradient magnetic beneficiation of dry pulverized coal via upwardly directed recirculating fluidization

DOEpatents

Eissenberg, David M.; Liu, Yin-An

1980-01-01

This invention relates to an improved device and method for the high gradient magnetic beneficiation of dry pulverized coal, for the purpose of removing sulfur and ash from the coal whereby the product is a dry environmentally acceptable, low-sulfur fuel. The process involves upwardly directed recirculating air fluidization of selectively sized powdered coal in a separator having sections of increasing diameters in the direction of air flow, with magnetic field and flow rates chosen for optimum separations depending upon particulate size.

Electrostatics effects in granular materials

NASA Astrophysics Data System (ADS)

Sarkar, Saurabh; Chaudhuri, Bodhisattwa

2013-06-01

This purpose of this study is to investigate the role of physiochemical properties and operational conditions in determining the electrostatic interactions between two species on a surface under typical industrial conditions. The variables considered for the study were particle type, particle size and shape, loading mass, surface type, angle of inclination of chute, nature and concentration of additive. Triboelectrification of simple and binary mixtures in a simple hopper and chute geometry was observed to be strongly linked to work function and moisture content of the powdered material.