Porous metal hydride composite and preparation and uses thereof

DOEpatents

Steyert, William A.; Olsen, Clayton E.

1982-01-01

A composite formed from large pieces of aggregate formed from (1) metal hydride (or hydride-former) powder and (2) either metal powder or plastic powder or both is prepared. The composite has large macroscopic interconnected pores (much larger than the sizes of the powders which are used) and will have a very fast heat transfer rate and low windage loss. It will be useful, for example, in heat engines, hydrogen storage devices, and refrigerator components which depend for their utility upon both a fast rate of hydriding and dehydriding. Additionally, a method of preparing the composite and a method of increasing the rates of hydriding and dehydriding of metal hydrides are also given.

Effects of Sample Preparation on the Infrared Reflectance Spectra of Powders

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

Brauer, Carolyn S.; Johnson, Timothy J.; Myers, Tanya L.

2015-05-22

While reflectance spectroscopy is a useful tool in identifying molecular compounds, laboratory measurement of solid (particularly powder) samples often is confounded by sample preparation methods. For example, both the packing density and surface roughness can have an effect on the quantitative reflectance spectra of powdered samples. Recent efforts in our group have focused on developing standard methods for measuring reflectance spectra that accounts for sample preparation, as well as other factors such as particle size and provenance. In this work, the effect of preparation method on sample reflectivity was investigated by measuring the directional-hemispherical spectra of samples that were hand-packedmore » as well as pressed into pellets using an integrating sphere attached to a Fourier transform infrared spectrometer. The results show that the methods used to prepare the sample have a substantial effect on the measured reflectance spectra, as do other factors such as particle size.« less

Effects of sample preparation on the infrared reflectance spectra of powders

NASA Astrophysics Data System (ADS)

Brauer, Carolyn S.; Johnson, Timothy J.; Myers, Tanya L.; Su, Yin-Fong; Blake, Thomas A.; Forland, Brenda M.

2015-05-01

While reflectance spectroscopy is a useful tool for identifying molecular compounds, laboratory measurement of solid (particularly powder) samples often is confounded by sample preparation methods. For example, both the packing density and surface roughness can have an effect on the quantitative reflectance spectra of powdered samples. Recent efforts in our group have focused on developing standard methods for measuring reflectance spectra that accounts for sample preparation, as well as other factors such as particle size and provenance. In this work, the effect of preparation method on sample reflectivity was investigated by measuring the directional-hemispherical spectra of samples that were hand-loaded as well as pressed into pellets using an integrating sphere attached to a Fourier transform infrared spectrometer. The results show that the methods used to prepare the sample can have a substantial effect on the measured reflectance spectra, as do other factors such as particle size.

Instruments for preparation of heterogeneous catalysts by an impregnation method

NASA Astrophysics Data System (ADS)

Yamada, Yusuke; Akita, Tomoki; Ueda, Atsushi; Shioyama, Hiroshi; Kobayashi, Tetsuhiko

2005-06-01

Instruments for the preparation of heterogeneous catalysts in powder form have been developed. The instruments consist of powder dispensing robot and an automated liquid handling machine equipped with an ultrasonic and a vortex mixer. The combination of these two instruments achieves the catalyst preparation by incipient wetness and ion exchange methods. The catalyst library prepared with these instruments were tested for dimethyl ether steam reforming and characterized by transmission electron microscopy observations.

Modified Pechini's method to prepare LaAlO3:RE thermoluminescent materials

NASA Astrophysics Data System (ADS)

Rivera-Montalvo, T.; Morales-Hernandez, A.; Barrera-Angeles, A. A.; Alvarez-Romero, R.; Falcony, C.; Zarate-Medina, J.

2017-11-01

This work presents an alternative method to prepare rare-earth doped lanthanum aluminates materials for thermoluminescent (TL) dosimetry applications. Modified Pechini´s method was using to prepare praseodymium doped LaAlO3 powders. LaAlO3:Pr3+ powders were prepared using La(NO3)3·6H2O, Al(NO3)3·6H2O, Pr(NO3)3·6H2O, citric acid, and ethylene glycol. The solution was heated to 80 °C for its polyesterification reaction. The obtained powders were submitted at different thermal treatment from 700 up to 1600 °C. The structural and morphological characterizations were carried out using X-ray diffraction (XRD) and scanning electron microscopy techniques. TL glow curves of the X-ray irradiated samples showed one peak for europium and praseodymium dopants, meanwhile for powders doped with dysprosium ion showed two peaks. The technique is low cost, faster and it produces homogeneous particles can be used as thermoluminescent phosphors.

Method for the preparation of ferrous low carbon porous material

DOEpatents

Miller, Curtis Jack

2014-05-27

A method for preparing a porous metal article using a powder metallurgy forming process is provided which eliminates the conventional steps associated with removing residual carbon. The method uses a feedstock that includes a ferrous metal powder and a polycarbonate binder. The polycarbonate binder can be removed by thermal decomposition after the metal article is formed without leaving a carbon residue.

Preparation of LuAG Powders with Single Phase and Good Dispersion for Transparent Ceramics Using Co-Precipitation Method

PubMed Central

Pan, Liangjie; Jiang, Benxue; Fan, Jintai; Yang, Qiuhong; Zhou, Chunlin; Zhang, Pande; Mao, Xiaojian; Zhang, Long

2015-01-01

The synthesis of pure and well dispersed lutetium aluminum garnet (LuAG) powder is crucial and important for the preparation of LuAG transparent ceramics. In this paper, high purity and well dispersed LuAG powders have been synthesized via co-precipitation method with lutetium nitrate and aluminum nitrate as raw materials. Ammonium hydrogen carbonate (AHC) was used as the precipitant. The influence of aging time, pH value, and dripping speed on the prepared LuAG powders were investigated. It showed that long aging duration (>15 h) with high terminal pH value (>7.80) resulted in segregation of rhombus Lu precipitate and Al precipitate. By decreasing the initial pH value or accelerating the dripping speed, rhombus Lu precipitate was eliminated and pure LuAG nano powders were synthesized. High quality LuAG transparent ceramics with transmission >75% at 1064 nm were fabricated using these well dispersed nano LuAG powders. PMID:28793510

Microstructural changes in NiFe2O4 ceramics prepared with powders derived from different fuels in sol-gel auto-combustion technique

NASA Astrophysics Data System (ADS)

Chauhan, Lalita; Bokolia, Renuka; Sreenivas, K.

2016-05-01

Structural properties of Nickel ferrite (NiFe2O4) ceramics prepared from powders derived from sol gel auto-combustion method using different fuels (citric acid, glycine and Dl-alanine) are compared. Changes in the structural properties at different sintering temperatures are investigated. X-ray diffraction (XRD) confirms the formation of single phase material with cubic structure. Ceramics prepared using the different powders obtained from different fuels show that that there are no significant changes in lattice parameters. However increasing sintering temperatures show significant improvement in density and grain size. The DL-alanine fuel is found to be the most effective fuel for producing NIFe2O4 powders by the sol-gel auto combustion method and yields highly crystalline powders in the as-burnt stage itself at a low temperature (80 °C). Subsequent use of the powders in ceramic manufacturing produces dense NiFe2O4 ceramics with a uniform microstructure and a large grain size.

Preparation of LuAG Powders with Single Phase and Good Dispersion for Transparent Ceramics Using Co-Precipitation Method.

PubMed

Pan, Liangjie; Jiang, Benxue; Fan, Jintai; Yang, Qiuhong; Zhou, Chunlin; Zhang, Pande; Mao, Xiaojian; Zhang, Long

2015-08-19

The synthesis of pure and well dispersed lutetium aluminum garnet (LuAG) powder is crucial and important for the preparation of LuAG transparent ceramics. In this paper, high purity and well dispersed LuAG powders have been synthesized via co-precipitation method with lutetium nitrate and aluminum nitrate as raw materials. Ammonium hydrogen carbonate (AHC) was used as the precipitant. The influence of aging time, pH value, and dripping speed on the prepared LuAG powders were investigated. It showed that long aging duration (>15 h) with high terminal pH value (>7.80) resulted in segregation of rhombus Lu precipitate and Al precipitate. By decreasing the initial pH value or accelerating the dripping speed, rhombus Lu precipitate was eliminated and pure LuAG nano powders were synthesized. High quality LuAG transparent ceramics with transmission >75% at 1064 nm were fabricated using these well dispersed nano LuAG powders.

Properties of zirconia-toughened-alumina prepared via powder processing and colloidal processing routes.

PubMed

Rafferty, A; Alsebaie, A M; Olabi, A G; Prescott, T

2009-01-15

Alumina-zirconia composites were prepared by two routes: powder processing, and colloidal processing. Unstabilised zirconia powder was added to alumina in 5 wt%, 10 wt% and 20 wt% quantities. For the colloidal method, zirconium(IV) propoxide solution was added to alumina powder, also in 5 wt%, 10 wt% and 20 wt% quantities. Additions of glacial acetic acid were needed to form stable suspensions. Suspension stability was verified by pH measurements and sedimentation testing. For the powder processed samples Vickers hardness decreased indefinitely with increasing ZrO(2) additions, but for colloidal samples the hardness at first decreased but then increased again above >10 wt% ZrO(2). Elastic modulus (E) values decreased with ZrO(2) additions. However, samples containing 20 wt% zirconia prepared via a colloidal method exhibited a much higher modulus than the powder processed equivalent. This was due to the homogeneous dispersion of zirconia yielding a sample which was less prone to microcracking.

Functionally gradient material of the system Ni-MgO, Ni-NiO, Ni-Si3N4 or Al-AlN, by pressureless sintering

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

Atarashiya, Koji; Kurokawa, Kazuya; Nagai, Tadao

1992-08-01

Generally speaking, the preparation of FGM-blocks, especially in the metal-nitride systems, by the method of powder metallurgy needs an extremely high temperature and high pressure. But, in this work using a ductile nickel metal powder or an ultrafine particle, the FGM-blocks were easily prepared using a powder metallurgy at a lower temperature. A mixture of a metallic powder and a non-metallic powder whose contents were gradually changed was pressed in a steel die under pressure of 20-32 MPa. These green compacts were heated at 900-1573 K in controlled atmosphere under null pressure. The FGM-blocks prepared by this method were characterizedmore » by their properties and were used in joinings. The joinings of metal/FGM/ceramics, metal/FGM and ceramics/FGM were completely accomplished at 900-1573 K. 6 refs.« less

Spheroidization of molybdenum powder by radio frequency thermal plasma

NASA Astrophysics Data System (ADS)

Liu, Xiao-ping; Wang, Kuai-she; Hu, Ping; Chen, Qiang; Volinsky, Alex A.

2015-11-01

To control the morphology and particle size of dense spherical molybdenum powder prepared by radio frequency (RF) plasma from irregular molybdenum powder as a precursor, plasma process parameters were optimized in this paper. The effects of the carrier gas flow rate and molybdenum powder feeding rate on the shape and size of the final products were studied. The molybdenum powder morphology was examined using high-resolution scanning electron microscopy. The powder phases were analyzed by X-ray diffraction. The tap density and apparent density of the molybdenum powder were investigated using a Hall flow meter and a Scott volumeter. The optimal process parameters for the spherical molybdenum powder preparation are 50 g/min powder feeding rate and 0.6 m3/h carrier gas rate. In addition, pure spherical molybdenum powder can be obtained from irregular powder, and the tap density is enhanced after plasma processing. The average size is reduced from 72 to 62 µm, and the tap density is increased from 2.7 to 6.2 g/cm3. Therefore, RF plasma is a promising method for the preparation of high-density and high-purity spherical powders.

Structural and Spectral Characterization of Co2+- and Ni2+-DOPED CdO Powder Prepared From Solution at Room Temperature

NASA Astrophysics Data System (ADS)

Reddy, C. V.; Rao, L. V. Krishna; Satish, D. V.; Shim, J.; Ravikumar, R. V. S. S. N.

2015-11-01

The mild and simple solution method was used for the synthesis of Co2+- and Ni2+-doped CdO powders at room temperature. The prepared powders were characterized using powder X-ray diffraction, scanning electron microscopy (SEM) with energy dispersive spectroscopy (EDS), optical absorption, and Fourier transform infrared spectroscopy (FTIR). From the powder X-ray diffraction patterns, it has been observed that the prepared Co2+ and Ni2+ ion-doped CdO powders belong to the cubic phase, and the evaluated average crystalline sizes of the powders are 20 and 14 nm, respectively. The SEM images and the EDS spectra show that the prepared powders are distributed over different sizes in the grain boundaries. Optical absorption studies allow determination of site symmetry of the metal ion with its ligands. The crystal field (Dq) and inter-electronic repulsion (B and C) parameters have been evaluated from the optical absorption spectra. The FTIR spectra show the characteristic fundamental vibrations of the metal oxide and CdO.

Study on Raman spectral imaging method for simultaneous estimation of ingredients concentration in food powder

USDA-ARS?s Scientific Manuscript database

This study investigated the potential of point scan Raman spectral imaging method for estimation of different ingredients and chemical contaminant concentration in food powder. Food powder sample was prepared by mixing sugar, vanillin, melamine and non-dairy cream at 5 different concentrations in a ...

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.

PLUTONIUM-HYDROGEN REACTION PRODUCT, METHOD OF PREPARING SAME AND PLUTONIUM POWDER THEREFROM

DOEpatents

Fried, S.; Baumbach, H.L.

1959-12-01

A process is described for forming plutonlum hydride powder by reacting hydrogen with massive plutonium metal at room temperature and the product obtained. The plutonium hydride powder can be converted to plutonium powder by heating to above 200 deg C.

Critical current densities of powder-in-tube MgB2 tapes fabricated with nanometer-size Mg powder

NASA Astrophysics Data System (ADS)

Yamada, H.; Hirakawa, M.; Kumakura, H.; Matsumoto, A.; Kitaguchi, H.

2004-03-01

We fabricated powder-in-tube MgB2/Fe tapes using a powder mixture of nanometer-size Mg and commercial amorphous B and investigated the transport properties. High-purity nanometer-size Mg powder was fabricated by applying the thermal plasma method. 5-10 mol % SiC powder doping was tried to enhance the Jc properties. We found that the use of nanometer-size Mg powder was effective to increase the Jc values. The transport Jc values of the nondoped and 10 mol % SiC-doped tapes prepared with nanometer-size Mg powder reached 90 and 250 A/mm2 at 4.2 K and 10 T, respectively. These values were about five times higher than those of the tapes prepared with commercial Mg powder.

Evaluation of Rock Powdering Methods to Obtain Fine-grained Samples for CHEMIN, a Combined XRD/XRF Instrument

NASA Technical Reports Server (NTRS)

Chipera, S. J.; Vaniman, D. T.; Bish, D. L.; Sarrazin, P.; Feldman, S.; Blake, D. F.; Bearman, G.; Bar-Cohen, Y.

2004-01-01

A miniature XRD/XRF (X-ray diffraction / X-ray fluorescence) instrument, CHEMIN, is currently being developed for definitive mineralogic analysis of soils and rocks on Mars. One of the technical issues that must be addressed to enable remote XRD analysis is how best to obtain a representative sample powder for analysis. For powder XRD analyses, it is beneficial to have a fine-grained sample to reduce preferred orientation effects and to provide a statistically significant number of crystallites to the X-ray beam. Although a two-dimensional detector as used in the CHEMIN instrument will produce good results even with poorly prepared powder, the quality of the data will improve and the time required for data collection will be reduced if the sample is fine-grained and randomly oriented. A variety of methods have been proposed for XRD sample preparation. Chipera et al. presented grain size distributions and XRD results from powders generated with an Ultrasonic/Sonic Driller/Corer (USDC) currently being developed at JPL. The USDC was shown to be an effective instrument for sampling rock to produce powder suitable for XRD. In this paper, we compare powder prepared using the USDC with powder obtained with a miniaturized rock crusher developed at JPL and with powder obtained with a rotary tungsten carbide bit to powders obtained from a laboratory bench-scale Retsch mill (provides benchmark mineralogical data). These comparisons will allow assessment of the suitability of these methods for analysis by an XRD/XRF instrument such as CHEMIN.

Method for forming biaxially textured articles by powder metallurgy

DOEpatents

Goyal, Amit; Williams, Robert K.; Kroeger, Donald M.

2002-01-01

A method of preparing a biaxially textured alloy article comprises the steps of preparing a mixture comprising Ni powder and at least one powder selected from the group consisting of Cr, W, V, Mo, Cu, Al, Ce, YSZ, Y, Rare Earths, (RE), MgO, CeO.sub.2, and Y.sub.2 O.sub.3 ; compacting the mixture, followed by heat treating and rapidly recrystallizing to produce a biaxial texture on the article. In some embodiments the alloy article further comprises electromagnetic or electro-optical devices and possesses superconducting properties.

Microstructural changes in NiFe{sub 2}O{sub 4} ceramics prepared with powders derived from different fuels in sol-gel auto-combustion technique

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

Chauhan, Lalita, E-mail: chauhan.lalita5@gmail.com; Sreenivas, K.; Bokolia, Renuka

2016-05-23

Structural properties of Nickel ferrite (NiFe{sub 2}O{sub 4}) ceramics prepared from powders derived from sol gel auto-combustion method using different fuels (citric acid, glycine and Dl-alanine) are compared. Changes in the structural properties at different sintering temperatures are investigated. X-ray diffraction (XRD) confirms the formation of single phase material with cubic structure. Ceramics prepared using the different powders obtained from different fuels show that that there are no significant changes in lattice parameters. However increasing sintering temperatures show significant improvement in density and grain size. The DL-alanine fuel is found to be the most effective fuel for producing NIFe{sub 2}O{submore » 4} powders by the sol-gel auto combustion method and yields highly crystalline powders in the as-burnt stage itself at a low temperature (80 °C). Subsequent use of the powders in ceramic manufacturing produces dense NiFe{sub 2}O{sub 4} ceramics with a uniform microstructure and a large grain size.« less

Method for low temperature preparation of a noble metal alloy

DOEpatents

Even, Jr., William R.

2002-01-01

A method for producing fine, essentially contamination free, noble metal alloys is disclosed. The alloys comprise particles in a size range of 5 to 500 nm. The method comprises 1. A method for preparing a noble metal alloy at low temperature, the method comprising the steps of forming solution of organometallic compounds by dissolving the compounds into a quantity of a compatible solvent medium capable of solvating the organometallic, mixing a portion of each solution to provide a desired molarity ratio of ions in the mixed solution, adding a support material, rapidly quenching droplets of the mixed solution to initiate a solute-solvent phase separation as the solvent freezes, removing said liquid cryogen, collecting and freezing drying the frozen droplets to produce a dry powder, and finally reducing the powder to a metal by flowing dry hydrogen over the powder while warming the powder to a temperature of about 150.degree. C.

Ceramic oxide powders and the formation thereof

DOEpatents

Katz, Joseph L.; Hung, Cheng-Hung

1993-01-01

Ceramic oxide powders and a method for their preparation. Ceramic oxide powders are obtained using a flame process whereby two or more precursors of ceramic oxides are introduced into a counterflow diffusion flame burner wherein said precursors are converted into ceramic oxide powders. The morphology, particle size, and crystalline form of the ceramic oxide powders are determined by process conditions.

Preparation of ZrO II/nano-TiO II composite powder by sol-gel method

NASA Astrophysics Data System (ADS)

Baharvandi, H. R.; Mohammadi, E.; Abdizadeh, H.; Hadian, A. M.; Ehsani, N.

2007-07-01

The effects of concentration of TTIP, amount of distilled water, and calcination temperature on morphology and particle size distribution of ZrO II/nano-TiO II catalysts were investigated. Mixed ZrO II/nano-TiO II powders were prepared by a modified sol-gel method by varying the mole fraction of TTIP from 0.002 to 0.01, H IIO/TTIP fraction from 2 to 8, and various stirring time (2, 4, and 10 h). The prepared ZrO II/nano-TiO II powders have been characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), and TG/DTA. Each oxide was calcined at the temperature between 110 and 1000°C. The results showed that the calcinations temperature has a pronounced effect on the phase formation and particle size of the calcined zirconium titanate (ZT) powders.

Optical properties of titanium-di-oxide (TiO2) prepared by hydrothermal method

NASA Astrophysics Data System (ADS)

Rahman, Kazi Hasibur; Biswas, Sayari; Kar, Asit Kumar

2018-05-01

Research on titanate and its derived TiO2 nanostructures with large specific surface area have received great attention due to their enhanced efficiency in photocatalysis, DSSC etc. Here, in this communication TiO2 powder has been prepared by hydrothermal method at 180 °C. In this work we have shown the changes in optical properties of the powder with two different sintering temperatures ‒ 500 °C and 800 °C. The as prepared powder was also studied. FESEM images show spherical particles for the as prepared samples which look more like agglomeration after sintering. Band gaps of the prepared samples were calculated from UV-Vis spectroscopy which lies in the range 2.85 eV ‒ 3.13 eV. The photoluminescence (PL) spectra of the prepared samples were recorded at room temperature in the range of 300‒700 nm. It shows two distinct peaks at 412 nm and 425 nm.

Internal zone growth method for producing metal oxide metal eutectic composites

DOEpatents

Clark, Grady W.; Holder, John D.; Pasto, Arvid E.

1980-01-01

An improved method for preparing a cermet comprises preparing a compact having about 85 to 95 percent theoretical density from a mixture of metal and metal oxide powders from a system containing a eutectic composition, and inductively heating the compact in a radiofrequency field to cause the formation of an internal molten zone. The metal oxide particles in the powder mixture are effectively sized relative to the metal particles to permit direct inductive heating of the compact by radiofrequency from room temperature. Surface melting is prevented by external cooling or by effectively sizing the particles in the powder mixture.

Green synthesis of nanocrystalline α-Al2O3 powders by both wet-chemical and mechanochemical methods

NASA Astrophysics Data System (ADS)

Gao, Huiying; Li, Zhiyong; Zhao, Peng

2018-03-01

Nanosized α-Al2O3 powders were prepared with AlCl3ṡ6H2O and NH4HCO3 as raw materials by both wet-chemical and mechanochemical methods, through the synthesis of the ammonium aluminum carbonate hydroxide (AACH) precursor followed by calcination. The environmentally benign starch was used as an effective dispersant during the preparation of nanocrystalline α-Al2O3 powders. X-ray diffraction (XRD), thermogravimetric differential thermal analysis (TG-DTA), transmission electron microscopy (TEM) and scanning electron microscopy (SEM) were employed to characterize the precursor AACH and products. The results show that nanosized spherical α-Al2O3 powders without hard agglomeration and with particle size in the range of 20-40 nm can be obtained by the two methods. Comparing the two “green” processes, the mechanochemical method has better prospects for commercial production.

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

Ceramic oxide powders and the formation thereof

DOEpatents

Katz, J.L.; Chenghung Hung.

1993-12-07

Ceramic oxide powders and a method for their preparation. Ceramic oxide powders are obtained using a flame process whereby two or more precursors of ceramic oxides are introduced into a counterflow diffusion flame burner wherein said precursors are converted into ceramic oxide powders. The morphology, particle size, and crystalline form of the ceramic oxide powders are determined by process conditions. 14 figures.

Preparation of SS316L MIM feedstock with biopolymer as a binder

NASA Astrophysics Data System (ADS)

Abdullah, A. A.; Norita, H.; Azlina, H. N.; Sulong, A. B.; Mas'ood, N. N.

2018-01-01

This paper focus on feedstock preparation for SS316L metal injection molding (MIM) part. The primary step of feedstock preparation, critical powder loading determined by two method; maximum filled volume calculation model and torque analysis. The critical powder loading determined by calculation was 70 vol% to 77 vol% while for experimental approaches shows the value of 75 vol%. The feedstock was prepared by mixing SS316L powder and polymer binder with ratio 70:30 at 175 °C with speed of 50 rpm. The feedstock was analyzed by thermogravimetric analysis (TGA) and Scanning electron microscope (SEM). The composition for the feedstock after preparation step was confirmed by TGA. It was found that the prepared feedstock component was compatible to each other and composition is maintain along the mixing step.

Program for plasma-sprayed self-lubricating coatings

NASA Technical Reports Server (NTRS)

Walther, G. C.

1979-01-01

A method for preparing composite powders of the three coating components was developed and a procedure that can be used in applying uniform coatings of the composite powders was demonstrated. Composite powders were prepared by adjusting particle sizes of the components and employing a small amount of monoaluminum phosphate as an inorganic binder. Quantitative microscopy (image analysis) was found to be a convenient method of characterizing the composition of the multiphase plasma-sprayed coatings. Area percentages and distribution of the components were readily obtained by this method. The adhesive strength of the coating to a nickel-chromium alloy substrate was increased by about 40 percent by a heat treatment of 20 hours at 650 C.

Synthesis mechanism and preparation of LaMgAl11O19 powder for plasma spraying

NASA Astrophysics Data System (ADS)

He, Mingtao; Meng, Huimin; Wang, Yuchao; Ren, Pengwei

2018-06-01

Lanthanide magnesium hexaaluminate (LaMgAl11O19) powders were successfully synthesized by the solid-state reaction method. The objective of this study was to investigate the synthesis mechanism of LaMgAl11O19 and prepare LaMgAl11O19 powders suitable for plasma spraying. The results show that LaAlO3 reacts with MgAl2O4 and Al2O3 to form LaMgAl11O19 at approximately 1300 °C. Single-phase LaMgAl11O19 powders were prepared successfully by solid-state reaction at a synthesis temperature of 1600 °C for 6 h. Unlike the particles in the synthesized powders, those of the centrifugally spray-dried powders have a spherical shape with uniform granularity and good flowability, density, and particle size distribution, making them suitable for plasma spraying. The synthesized powders and centrifugally spray-dried powders remained as a single phase after heat treatment at 1300 °C for 100 h, indicating that LaMgAl11O19 has excellent high-temperature stability.

Nucleation of biomimetic apatite in synthetic body fluids: dense and porous scaffold development.

PubMed

Landi, Elena; Tampieri, Anna; Celotti, Giancarlo; Langenati, Ratih; Sandri, Monica; Sprio, Simone

2005-06-01

The effectiveness of synthetic body fluids (SBF) as biomimetic sources to synthesize carbonated hydroxyapatite (CHA) powder similar to the biological inorganic phase, in terms of composition and microstructure, was investigated. CHA apatite powders were prepared following two widely experimented routes: (1) calcium nitrate tetrahydrate and diammonium hydrogen phosphate and (2) calcium hydroxide and ortophosphoric acid, but using SBF as synthesis medium instead of pure water. The characteristics of the as-prepared powders were compared, also with the features of apatite powders synthesized via pure water-based classical methods. The powder thermal resistance and behaviour during densification were studied together with the mechanical properties of the dense samples. The sponge impregnation process was used to prepare porous samples having morphological and mechanical characteristics suitable for bone substitution. Using this novel synthesis was it possible to prepare nanosized (approximately equal to 20 nm), pure, carbonate apatite powder containing Mg, Na, K ions, with morphological and compositional features mimicking natural apatite and with improved thermal properties. After sintering at 1250 degrees C the carbonate-free apatite porous samples showed a surprising, high compressive strength together with a biomimetic morphology.

Method for producing silicon nitride/silicon carbide composite

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.

1996-07-23

Silicon carbide/silicon nitride composites are prepared by carbothermal reduction of crystalline silica powder, carbon powder and optionally crsytalline silicon nitride powder. The crystalline silicon carbide portion of the composite has a mean number diameter less than about 700 nanometers and contains nitrogen.

Stability of levamisole oral solutions prepared from tablets and powder.

PubMed

Chiadmi, Fouad; Lyer, Abdel; Cisternino, Salvatore; Toledano, Audrey; Schlatter, Joël; Ratiney, Robert; Fontan, Jean-Eudes

2005-08-12

To study the stability of levamisole oral solutions (25 mg/mL) prepared from powder and tablets stored at 4 +/- 3 degrees C and 23 +/- 2 degrees C in amber glass prescription bottles. Levamisole 25 mg/mL solutions were prepared from commercially available 50-mg tablets or from pure powder in sterile water. Levamisole concentrations were determined in duplicate by a stability-indicating HPLC method at 0, 1, 2, 3, 4, 7, 14, 30, 60 and 90 days. The initial and final pHs of solutions were measured. The recovery of levamisole from tablets was 100 +/- 2.1%. No color or odour changes were observed during the study period. The oral solutions prepared from powder were stable at least 90 days stored at 4 and 23 degrees C. The oral solutions prepared from tablets were stable at least 90 days at 4 degrees C and 15 days when stored at 23 degrees C. The initial pH of solutions prepared from powder and tablets were 5.30 and 4.55, respectively. Initial and final pH values were significantly different (p<0.001) for the two solutions. Levamisole 25 mg/mL oral solutions can be prepared from tablets or powder with sterile water for irrigation and stored for 90 days under refrigeration, taking account of the lack of microbiological contamination.

Ferromagnetic nanocomposites

NASA Astrophysics Data System (ADS)

Mazaleyrat, F.; Varga, L. K.

2000-06-01

A survey of magnetic nanocomposites applicable in high-frequency signal and power electronics is given. First, the preparation and properties of ribbon and powder cores from the nanocrystalline "bulk" alloys (Finemet and Nanoperm) is reviewed. A technology is presented to apply continuously a large stress during the annealing and winding of the rapidly quenched ribbons in order to induce uniaxial anisotropy in it. The obtained toroidal cores with flat hysteresis curve are applicable up to 1 MHz with considerable permeability (˜250). The powder cores prepared from ground Finemet with powder size of 30-400 μm are applicable up to 1 MHz and in some cases up to 10 MHz for smaller powder sizes with low permeability (˜10). Finally, the most common methods used for the preparation of metallic nano-particle s are presented. Presently, the compacts prepared from nano-size (40-80 nm) iron powders do not show the expected behavior. It is anticipated that the iron-based ferromagnetic nanocomposites should replace partly the ferrite-type materials in the forthcoming years.

Preparation of (Fe, N)-doped TiO2 powders and their antibacterial activities under visible light irradiation.

PubMed

He, Rong-Liang; Wei, Yi; Cao, Wen-Bin

2009-02-01

Yellowish (Fe, N)-doped nanocrystalline TiO2 powders have been prepared using TiOSO4, CO(NH2)2, Fe(NO3)3.9H2O and CN3H5.HCl as precursors by hydrothermal method. The as-synthesized powders were anatase in phase and the grain size was about 10 nm according to the TEM photos. The ratio of Fe/Ti is 2.2 at% and N/O is 0.8 at% respectively. TiO2 powders were mixed with organic silicon and acrylic syrup to test their antibacterial performance by the colony counting method. The results show that the sterilization ratio of E. coli by the heat-treated (Fe, N)-doped nanocrystalline TiO2 powders is reached up to 94.5% while that of the powders without any heat treatment is 91.1% by 8 hours-400 lux-Visible-light irradiation with humidity of 55% RH.

Preparation and enhanced daylight-induced photocatalytic activity of C,N,S-tridoped titanium dioxide powders.

PubMed

Zhou, Minghua; Yu, Jiaguo

2008-04-15

A simple method for preparing highly daylight-induced photoactive nanocrystalline C,N,S-tridoped TiO2 powders was developed by a solid-phase reaction. The as-prepared TiO2 powders were characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), UV-vis diffuse reflectance spectra, N2 adsorption-desorption measurements and transmission electron microscopy (TEM). The photocatalytic activity was evaluated by the photocatalytic oxidation of formaldehyde under daylight irradiation in air. The results show that daylight-induced photocatalytic activities of the as-prepared TiO2 powders were improved by C,N,S-tridoping. The C,N,S-tridoped TiO2 powders exhibited stronger absorption in the near UV and visible-light region with red shift in the band-gap transition. When the molar ratio of CS(NH2)2 to xerogel TiO2 powders (prepared by hydrolysis of Ti(OC4H9)4 in distilled water) (R) was kept in 3, the daylight-induced photocatalytic activities of the as-prepared C,N,S-tridoped TiO2 powders were about more than six times greater than that of Degussa P25 and un-doped TiO2 powders. The high activities of the C,N,S-tridoped TiO2 can be attributed to the results of the synergetic effects of strong absorption in the near UV and visible-light region, red shift in adsorption edge and two phase structures of un-doped TiO2 and C,N,S-tridoped TiO2.

Process for preparing fine grain titanium carbide powder

DOEpatents

Janney, M.A.

1985-03-12

A method for preparing finely divided titanium carbide powder in which an organotitanate is reacted with a carbon precursor polymer to provide an admixture of the titanium and the polymer at a molecular level due to a crosslinking reaction between the organotitanate and the polymer. The resulting gel is dried, pyrolyzed to drive off volatile components and provide carbon. The resulting solids are then heated at an elevated temperature to convert the titanium and carbon to high-purity titanium carbide powder in a submicron size range.

Process for preparing fine grain titanium carbide powder

DOEpatents

Janey, Mark A.

1986-01-01

A method for preparing finely divided titanium carbide powder in which an organotitanate is reacted with a carbon precursor polymer to provide an admixture of the titanium and the polymer at a molecular-level due to a crosslinking reaction between the organotitanate and the polymer. The resulting gel is dried, pyrolyzed to drive off volatile components and provide carbon. The resulting solids are then heated at an elevated temperature to convert the titanium and carbon to high-purity titanium carbide powder in a submicron size range.

Synthesis of nanocrystalline CeO{sub 2} particles by different emulsion methods

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

Supakanapitak, Sunisa; Boonamnuayvitaya, Virote; Jarudilokkul, Somnuk, E-mail: somnuk.jar@kmutt.ac.th

2012-05-15

Cerium oxide nanoparticles were synthesized using three different methods of emulsion: (1) reversed micelle (RM); (2) emulsion liquid membrane (ELM); and (3) colloidal emulsion aphrons (CEAs). Ammonium cerium nitrate and polyoxyethylene-4-lauryl ether (PE4LE) were used as cerium and surfactant sources in this study. The powder was calcined at 500 Degree-Sign C to obtain CeO{sub 2}. The effect of the preparation procedure on the particle size, surface area, and the morphology of the prepared powders were investigated. The obtained powders are highly crystalline, and nearly spherical in shape. The average particle size and the specific surface area of the powders frommore » the three methods were in the range of 4-10 nm and 5.32-145.73 m{sup 2}/g, respectively. The CeO{sub 2} powders synthesized by the CEAs are the smallest average particle size, and the highest surface area. Finally, the CeO{sub 2} prepared by the CEAs using different cerium sources and surfactant types were studied. It was found that the surface tensions of cerium solution and the type of surfactant affect the particle size of CeO{sub 2}. - Graphical Abstract: The emulsion droplet size distribution and the TEM images of CeO{sub 2} prepared by different methods: reversed micelle (RM), emulsion liquid membrane (ELM) and colloidal emulsion aphrons (CEAs). Highlights: Black-Right-Pointing-Pointer Nano-sized CeO{sub 2} was successfully prepared by three different emulsion methods. Black-Right-Pointing-Pointer The colloidal emulsion aphrons method producing CeO{sub 2} with the highest surface area. Black-Right-Pointing-Pointer The surface tensions of a cerium solution have slightly effect on the particle size. Black-Right-Pointing-Pointer The size control could be interpreted in terms of the adsorption of the surfactant.« less

PREPARATION OF COMPACTS MADE FROM URANIUM AND BERYLLIUM BY SINTERING

DOEpatents

Angier, R.P.

1961-04-11

A powder metallurgical method for making high-density compacts of uranium and beryllium is reported. Powdered UBe/sub 9/ and powdered Be are blended, compacted, and then sintered by rapidly heating to a temperature of approximately 1220 to 1280 deg C in an inert atmosphere.

Polymer Infiltration Studies

NASA Technical Reports Server (NTRS)

Marchello, Joseph M.

1993-01-01

Significant progress has been made on the preparation of carbon fiber composites using advanced polymer resins during the past three months. Current and ongoing research activities reported herein include: (1) Prepregger Hot Sled Operation; (2) Ribbonizing Powder-Impregnated Towpreg; (3) Textile Composites from Powder-Coated Towpreg: Role of Bulk Factor; and (4) Powder Curtain Prepreg Process. During the coming months research will be directed toward further development of the new powder curtain prepregging method and on ways to customize dry powder towpreg for textile and robotic applications in aircraft part fabrication. Studies of multi-tow powder prepregging and ribbon preparation will be conducted in conjunction with continued development of prepegging technology and the various aspects of composite part fabrication using customized towpreg. Also, work will continue on the analysis of the new solution prepegger.

Investigation of the Dependences of the Attenuation Properties of Cryogenic Metal-Powder Filters on the Preparation Method

NASA Astrophysics Data System (ADS)

Lee, Sung Hoon; Lee, Soon-Gul

2018-04-01

We fabricated low-pass metal powder filters for use in low-noise measurements at cryogenic temperatures and investigated their attenuation characteristics for different wire-turn densities, metalpowder shapes, and preparation methods at frequencies up to 20 GHz. We used nominally 30-μmsized stainless-steel 304L powder and mixed it with low-temperature binders. The low-temperature binders used were Stycast 2850FT (Emerson and Cumming) with catalyst 23LV and GE-7031 varnish. A 0.1-mm insulated copper wire was wound on preformed powder-mixture bobbins in the shape of a circular rod and was encapsulated in metal tubes with the powder mixture. All the fabricated powder filters showed a large attenuation at high frequencies with a cut-off frequency near 1 GHz. For filters of the same wire length, a lower wiring density showed a larger attenuation, which implies that the amount of powder in close contact with the wire determines the attenuation. Filters made of a powder/varnish mixture showed significantly larger attenuations than those of a powder/stycast mixture, and the attenuation improved with increasing powder ratio in the mixture. The low-temperature thermal conductivities of a 2 : 1 powder/Stycast mixture and a 5 : 1 powder/varnish mixture showed similar values at temperatures up to 4.2 K.

Vacuum Powder Injector

NASA Technical Reports Server (NTRS)

Working, Dennis C.

1991-01-01

Method developed to provide uniform impregnation of bundles of carbon-fiber tow with low-solubility, high-melt-flow polymer powder materials to produce composite prepregs. Vacuum powder injector expands bundle of fiber tow, applies polymer to it, then compresses bundle to hold powder. System provides for control of amount of polymer on bundle. Crystallinity of polymer maintained by controlled melt on takeup system. All powder entrapped, and most collected for reuse. Process provides inexpensive and efficient method for making composite materials. Allows for coating of any bundle of fine fibers with powders. Shows high potential for making prepregs of improved materials and for preparation of high-temperature, high-modulus, reinforced thermoplastics.

Pulsed laser deposition of functionalized Mg-Al layered double hydroxide thin films

NASA Astrophysics Data System (ADS)

Vlad, A.; Birjega, R.; Tirca, I.; Matei, A.; Mardare, C. C.; Hassel, A. W.; Nedelcea, A.; Dinescu, M.; Zavoianu, R.

2018-02-01

In this paper, magnesium-aluminium layered double hydroxide (LDH) has been functionalized with sodium dodecyl sulfate (DS) and deposited as thin film by pulsed laser deposition (PLD). Mg, Al-LDH powders were prepared by co-precipitation and used as reference material. Intercalation of DS as an anionic surfactant into the LDHs host layers has been prepared in two ways: co-precipitation (P) and reconstruction (R). DS intercalation occurred in LDH powder via both preparation methods. The films deposited via PLD, in particular at 532 and 1064 nm, preserve the organic intercalated layered structure of the targets prepared from these powders. The results reveal the ability of proposed deposition technique to produce functional composite organo-modified LDHs thin films.

Method of making tantalum capacitors

DOEpatents

McMillan, April D.; Clausing, Robert E.; Vierow, William F.

1998-01-01

A method for manufacturing tantalum capacitors includes preparing a tantalum compact by cold pressing tantalum powder, placing the compact, along with loose refractory metal powder, in a microwave-transparent casket to form an assembly, and heating the assembly for a time sufficient to effect at least partial sintering of the compact and the product made by the method.

Method for producing microcomposite powders using a soap solution

DOEpatents

Maginnis, Michael A.; Robinson, David A.

1996-01-01

A method for producing microcomposite powders for use in superconducting and non-superconducting applications. A particular method to produce microcomposite powders for use in superconducting applications includes the steps of: (a) preparing a solution including ammonium soap; (b) dissolving a preselected amount of a soluble metallic such as silver nitrate in the solution including ammonium soap to form a first solution; (c) adding a primary phase material such as a single phase YBC superconducting material in particle form to the first solution; (d) preparing a second solution formed from a mixture of a weak acid and an alkyl-mono-ether; (e) adding the second solution to the first solution to form a resultant mixture; (f) allowing the resultant mixture to set until the resultant mixture begins to cloud and thicken into a gel precipitating around individual particles of the primary phase material; (g) thereafter drying the resultant mixture to form a YBC superconducting material/silver nitrate precursor powder; and (h) calcining the YBC superconducting material/silver nitrate precursor powder to convert the silver nitrate to silver and thereby form a YBC/silver microcomposite powder wherein the silver is substantially uniformly dispersed in the matrix of the YBC material.

Improvement of mechanical and thermal properties of high energy electron beam irradiated HDPE/hydroxyapatite nano-composite

NASA Astrophysics Data System (ADS)

Mohammadi, M.; Ziaie, F.; Majdabadi, A.; Akhavan, A.; Shafaei, M.

2017-01-01

In this research work, the nano-composites of high density polyethylene/hydroxyapatite samples were manufactured via two methods: In the first method, the granules of high density polyethylene and nano-structure hydroxyapatite were processed in an internal mixer to prepare the nano-composite samples with a different weight percentage of the reinforcement phase. As for the second one, high density polyethylene was prepared in nano-powder form in boiling xylene. During this procedure, the hydroxyapatite nano-powder was added with different weight percentages to the solvent to obtain the nano-composite. In both of the procedures, the used hydroxyapatite nano-powder was synthesized via hydrolysis methods. The samples were irradiated under 10 MeV electron beam in 70-200 kGy of doses. Mechanical, thermal and morphological properties of the samples were investigated and compared. The results demonstrate that the nano-composites which we have prepared using nano-polyethylene, show better mechanical and thermal properties than the composites prepared from normal polyethylene granules, due to the better dispersion of nano-particles in the polymer matrix.

Refractance Window™ drying of haskap berry--preliminary results on anthocyanin retention and physicochemical properties.

PubMed

Celli, Giovana Bonat; Khattab, Rabie; Ghanem, Amyl; Brooks, Marianne Su-Ling

2016-03-01

The goal of this work was to determine the anthocyanin retention and physicochemical properties of haskap powder prepared by Refractance Window™ (RW) drying. In general, the RW-dried powder particles had a smooth surface with similar thickness, consistent with the preparation method, and had a solubility of 75.63% in water. The RW-dried powder (consisting of 98% haskap berries) retained approximately 93.8% of anthocyanins from the original frozen fruits, as assessed by the pH-differential method. This result is in good agreement with HPLC analysis that indicated 92.9% retention. Three anthocyanins were identified in frozen berries and RW-dried powder: cyanidin 3-glucoside, cyanidin 3-rutinoside, and peonidin 3-glucoside. Surprisingly, cyanidin 3-rutinoside exhibited the lowest retention. Copyright © 2015 Elsevier Ltd. All rights reserved.

Method for forming energetic nanopowders

DOEpatents

Lee, Kien-Yin; Asay, Blaine W.; Kennedy, James E.

2013-10-15

A method for the preparation of neat energetic powders, having nanometer dimensions, is described herein. For these neat powder, a solution of a chosen energetic material is prepared in an aprotic solvent and later combined with liquid hexane that is miscible with such solvent. The energetic material chosen is less soluble in the liquid hexane than in the aprotic solvent and the liquid hexane is cooled to a temperature that is below that of the solvent solution. In order to form a precipitate of said neat powders, the solvent solution is rapidly combined with the liquid hexane. When the resulting precipitate is collected, it may be dried and filtered to yield an energetic nanopowder material.

Method of high-density foil fabrication

DOEpatents

Blue, Craig A.; Sikka, Vinod K.; Ohriner, Evan K.

2003-12-16

A method for preparing flat foils having a high density includes the steps of mixing a powdered material with a binder to form a green sheet. The green sheet is exposed to a high intensity radiative source adapted to emit radiation of wavelengths corresponding to an absorption spectrum of the powdered material. The surface of the green sheet is heated while a lower sub-surface temperature is maintained. An apparatus for preparing a foil from a green sheet using a radiation source is also disclosed.

The Remote Food Photography Method accurately estimates dry powdered foods—the source of calories for many infants

PubMed Central

Duhé, Abby F.; Gilmore, L. Anne; Burton, Jeffrey H.; Martin, Corby K.; Redman, Leanne M.

2016-01-01

Background Infant formula is a major source of nutrition for infants with over half of all infants in the United States consuming infant formula exclusively or in combination with breast milk. The energy in infant powdered formula is derived from the powder and not the water making it necessary to develop methods that can accurately estimate the amount of powder used prior to reconstitution. Objective To assess the use of the Remote Food Photography Method (RFPM) to accurately estimate the weight of infant powdered formula before reconstitution among the standard serving sizes. Methods For each serving size (1-scoop, 2-scoop, 3-scoop, and 4-scoop), a set of seven test bottles and photographs were prepared including the recommended gram weight of powdered formula of the respective serving size by the manufacturer, three bottles and photographs containing 15%, 10%, and 5% less powdered formula than recommended, and three bottles and photographs containing 5%, 10%, and 15% more powdered formula than recommended (n=28). Ratio estimates of the test photographs as compared to standard photographs were obtained using standard RFPM analysis procedures. The ratio estimates and the United States Department of Agriculture (USDA) data tables were used to generate food and nutrient information to provide the RFPM estimates. Statistical Analyses Performed Equivalence testing using the two one-sided t- test (TOST) approach was used to determine equivalence between the actual gram weights and the RFPM estimated weights for all samples, within each serving size, and within under-prepared and over-prepared bottles. Results For all bottles, the gram weights estimated by the RFPM were within 5% equivalence bounds with a slight under-estimation of 0.05 g (90% CI [−0.49, 0.40]; p<0.001) and mean percent error ranging between 0.32% and 1.58% among the four serving sizes. Conclusion The maximum observed mean error was an overestimation of 1.58% of powdered formula by the RFPM under controlled laboratory conditions indicating that the RFPM accurately estimated infant powdered formula. PMID:26947889

Synthesis of highly phase pure BSCCO superconductors

DOEpatents

Dorris, S.E.; Poeppel, R.B.; Prorok, B.C.; Lanagan, M.T.; Maroni, V.A.

1995-11-21

An article and method of manufacture (Bi, Pb)-Sr-Ca-Cu-O superconductor are disclosed. The superconductor is manufactured by preparing a first powdered mixture of bismuth oxide, lead oxide, strontium carbonate, calcium carbonate and copper oxide. A second powdered mixture is then prepared of strontium carbonate, calcium carbonate and copper oxide. The mixtures are calcined separately with the two mixtures then combined. The resulting combined mixture is then subjected to a powder in tube deformation and thermal processing to produce a substantially phase pure (Bi, Pb)-Sr-Ca-Cu-O superconductor. 5 figs.

Synthesis of highly phase pure BSCCO superconductors

DOEpatents

Dorris, Stephen E.; Poeppel, Roger B.; Prorok, Barton C.; Lanagan, Michael T.; Maroni, Victor A.

1995-01-01

An article and method of manufacture of (Bi, Pb)-Sr-Ca-Cu-O superconductor. The superconductor is manufactured by preparing a first powdered mixture of bismuth oxide, lead oxide, strontium carbonate, calcium carbonate and copper oxide. A second powdered mixture is then prepared of strontium carbonate, calcium carbonate and copper oxide. The mixtures are calcined separately with the two mixtures then combined. The resulting combined mixture is then subjected to a powder in tube deformation and thermal processing to produce a substantially phase pure (Bi, Pb)-Sr-Ca-Cu-O superconductor.

Synthesis of highly phase pure (Bi, Pb)-Sr-Ca-Cu-O superconductor

DOEpatents

Dorris, Stephen E.; Poeppel, Roger B.; Prorok, Barton C.; Lanagan, Michael T.; Maroni, Victor A.

1994-01-01

An article and method of manufacture of (Bi,Pb)-Sr-Ca-Cu-O superconductor. The superconductor is manufactured by preparing a first powdered mixture of bismuth oxide, lead oxide, strontium carbonate, calcium carbonate and copper oxide. A second powdered mixture is then prepared of strontium carbonate, calcium carbonate and copper oxide. The mixtures are calcined separately with the two mixtures then combined. The resulting combined mixture is then subjected to a powder in tube deformation and thermal processing to produce a substantially phase pure (Bi,Pb)-Sr-Ca-Cu-O superconductor.

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.

Corrosion Screening of EV31A Magnesium and Other Magnesium Alloys using Laboratory-Based Accelerated Corrosion and Electro-Chemical Methods

DTIC Science & Technology

2014-07-01

corrosion studies (16). A schematic of the SWAP process and example of the powder produced is included in figure 4. This alloy contains amounts of Al ...advanced powder -based alloy and ZAXE1711 (both from Japan) were produced using a Spinning Water Atomization Process (SWAP) to yield powder particles with...and ZAXE1711 Mg alloy powders and (b) morphology of coarse Mg alloy powder prepared by SWAP

Device for preparing combinatorial libraries in powder metallurgy.

PubMed

Yang, Shoufeng; Evans, Julian R G

2004-01-01

This paper describes a powder-metering, -mixing, and -dispensing mechanism that can be used as a method for producing large numbers of samples for metallurgical evaluation or electrical or mechanical testing from multicomponent metal and cermet powder systems. It is designed to make use of the same commercial powders that are used in powder metallurgy and, therefore, to produce samples that are faithful to the microstructure of finished products. The particle assemblies produced by the device could be consolidated by die pressing, isostatic pressing, laser sintering, or direct melting. The powder metering valve provides both on/off and flow rate control of dry powders in open capillaries using acoustic vibration. The valve is simple and involves no relative movement, avoiding seizure with fine powders. An orchestra of such valves can be arranged on a building platform to prepare multicomponent combinatorial libraries. As with many combinatorial devices, identification and evaluation of sources of mixing error as a function of sample size is mandatory. Such an analysis is presented.

Synthesis of Nanometric-Sized Barium Titanate Powders Using Acetylacetone as the Chelating Agent in a Sol-Precipitation Process

NASA Astrophysics Data System (ADS)

Hung, Kun Ming; Hsieh, Ching Shieh; Yang, Wein Duo; Tsai, Hui Ju

2007-03-01

Nanometric-sized barium titanate powders were prepared by using titanium isopropoxid as the raw material and acetylacetone as a chelating agent, in a strong alkaline solution (pH > 13) through the sol-precipitation method. The preparatory variables affect the extent of cross-linking in the structure, change the mode of condensation of the gels, and even control the particle size of the powder. The reaction rate of forming powder, at a higher temperature such as 100°C and more water content (the molar ratio of water to titanium isopropoxide is 25) or fewer acetylacetone (the molar ratio of acetylacetone to titanium isopropoxide is 1), is rapid and the particle size formed is finer at 60 80 nm. On the contrary, that of forming powder, at lower temperature (40°C) and less water content (molar ratio of water/titanium isopropoxide = 5) or higher acetylacetone (acetylacetone/titanium isopropoxide = 7), is slow and the particle size of the powder is larger. The optimal preparatory conditions were obtained by using the experimental statistical method; as a result, nanometric-sized BaTiO3 powder with an average particle size of about 50 nm was prepared.

Optimization of Premix Powders for Tableting Use.

PubMed

Todo, Hiroaki; Sato, Kazuki; Takayama, Kozo; Sugibayashi, Kenji

2018-05-08

Direct compression is a popular choice as it provides the simplest way to prepare the tablet. It can be easily adopted when the active pharmaceutical ingredient (API) is unstable in water or to thermal drying. An optimal formulation of preliminary mixed powders (premix powders) is beneficial if prepared in advance for tableting use. The aim of this study was to find the optimal formulation of the premix powders composed of lactose (LAC), cornstarch (CS), and microcrystalline cellulose (MCC) by using statistical techniques. Based on the "Quality by Design" concept, a (3,3)-simplex lattice design consisting of three components, LAC, CS, and MCC was employed to prepare the model premix powders. Response surface method incorporating a thin-plate spline interpolation (RSM-S) was applied for estimation of the optimum premix powders for tableting use. The effect of tablet shape identified by the surface curvature on the optimization was investigated. The optimum premix powder was effective when the premix was applied to a small quantity of API, although the function of premix was limited in the case of the formulation of large amount of API. Statistical techniques are valuable to exploit new functions of well-known materials such as LAC, CS, and MCC.

PREPARATION OF METAL POWDER COMPACTS PRIOR TO PRESSING

DOEpatents

Mansfield, H.

1958-08-26

A method of fabricating uranium by a powder metallurgical technique is described. It consists in introducing powdered uranium hydride into a receptacle shaped to coincide with the coatour of the die cavity and heating the hydride so that it decomposes to uranium metal. The metal particles cohere in the shapw of the receptacle and thereafter the prefurmed metal powder is pressed and sintered to obtain a dense compact.

[Exploration of one-step preparation of Ganoderma lucidum multicomponent microemulsion].

PubMed

He, Jun-Jie; Chen, Yan; Du, Meng; Cao, Wei; Yuan, Ling; Zheng, Li-Yan

2013-03-01

To explore one-step method for the preparation of Ganoderma lucidum multicomponent microemulsion, according to the dissolution characteristics of triterpenes and polysaccharides in Ganoderma lucidum, formulation of the microemulsion was optimized. The optimal blank microemulsion was used as a solvent to sonicate the Ganoderma lucidum powder to prepare the multicomponent microemulsion, besides, its physicochemical properties were compared with the microemulsion made by conventional method. The results showed that the multicomponent microemulsion was characterized as (43.32 +/- 6.82) nm in size, 0.173 +/- 0.025 in polydispersity index (PDI) and -(3.98 +/- 0.82) mV in zeta potential. The contents of Ganoderma lucidum triterpenes and polysaccharides were (5.95 +/- 0.32) and (7.58 +/- 0.44) mg x mL(-1), respectively. Sonicating Ganoderma lucidum powder by blank microemulsion could prepare the multicomponent microemulsion. Compared with the conventional method, this method is simple and low cost, which is suitable for industrial production.

Process for preparing fine grain silicon carbide powder

DOEpatents

Wei, G.C.

Method of producing fine-grain silicon carbide powder comprises combining methyltrimethoxysilane with a solution of phenolic resin, acetone and water or sugar and water, gelling the resulting mixture, and then drying and heating the obtained gel.

A synthesis of fluorescent starch based on carbon nanoparticles for fingerprints detection

NASA Astrophysics Data System (ADS)

Li, Hongren; Guo, Xingjia; Liu, Jun; Li, Feng

2016-10-01

A pyrolysis method for synthesizing carbon nanoparticles (CNPs) were developed by using malic acid and ammonium oxalate as raw materials. The incorporation of a minor amount of carbon nanoparticles into starch powder imparts remarkable color-tunability. Based on this phenomenon, an environment friendly fluorescent starch powder for detecting latent fingerprints in non-porous surfaces was prepared. The fingerprints on different non-porous surfaces developed with this powder showed very good fluorescent images under ultraviolet excitation. The method using fluorescent starch powder as fluorescent marks is simple, rapid and green. Experimental results illustrated the effectiveness of proposed methods, enabling its practical applications in forensic sciences.

An improved soft-chemistry approach to the preparation of spinel powders

NASA Astrophysics Data System (ADS)

Cook, Ronald

2007-04-01

Spinel powders for the production of transparent polycrystalline ceramic windows have been produced using a number of traditional ceramic and sol-gel methods. We have demonstrated that magnesium aluminate spinel powders produced from the reaction of organo-magnesium compounds with surface modified boehmite precursors can be used to produce high quality transparent spinel parts. In previous work, the spinel powders were prepared by the reaction of surface-modified boehmite nanoparticles with magnesium acetylacetonate. While the magnesium acetylacetonate can produce small quantities of high quality spinel powders, it use for large scale production of spinel powders is problematic. Through a thermodynamic analysis we have identified a new high-purity, low-cost, low-toxicity organomagnesium compound that reacts the with surface modified boehmite nanoparticles to produce a spinel precursor. The magnesium doped precursor readily transforms into pure phase spinel at temperature between 900°C and 1200°C.

Counterflow diffusion flame synthesis of ceramic oxide powders

DOEpatents

Katz, J.L.; Miquel, P.F.

1997-07-22

Ceramic oxide powders and methods for their preparation are revealed. Ceramic oxide powders are obtained using a flame process whereby one or more precursors of ceramic oxides are introduced into a counterflow diffusion flame burner wherein the precursors are converted into ceramic oxide powders. The nature of the ceramic oxide powder produced is determined by process conditions. The morphology, particle size, and crystalline form of the ceramic oxide powders may be varied by the temperature of the flame, the precursor concentration ratio, the gas stream and the gas velocity. 24 figs.

Counterflow diffusion flame synthesis of ceramic oxide powders

DOEpatents

Katz, Joseph L.; Miquel, Philippe F.

1997-01-01

Ceramic oxide powders and methods for their preparation are revealed. Ceramic oxide powders are obtained using a flame process whereby one or more precursors of ceramic oxides are introduced into a counterflow diffusion flame burner wherein the precursors are converted into ceramic oxide powders. The nature of the ceramic oxide powder produced is determined by process conditions. The morphology, particle size, and crystalline form of the ceramic oxide powders may be varied by the temperature of the flame, the precursor concentration ratio, the gas stream and the gas velocity.

Doped-carbon composites, synthesizing methods and applications of the same

DOEpatents

Viswanathan, Tito

2017-05-09

A method of synthesizing a doped carbon composite includes preparing a solution having a carbon source material and a heteroatom containing additive, evaporating the solution to yield a plurality of powders, and subjecting the plurality of powders to a heat treatment for a duration of time effective to produce the doped carbon composite.

Compact Process for the Preparation of Microfine Spherical High-Niobium-Containing TiAl Alloy Powders

NASA Astrophysics Data System (ADS)

Tong, J. B.; Lu, X.; Liu, C. C.; Wang, L. N.; Qu, X. H.

2015-03-01

High-Nb-containing TiAl alloys are a new generation of materials for high-temperature structural applications because of their superior high-temperature mechanical properties. The alloy powders can be widely used for additive manufacturing, thermal spraying, and powder metallurgy. Because of the difficulty of making microfine spherical alloy powders in quantity by conventional techniques, a compact method was proposed, which consisted of two-step ball milling of elemental powders and subsequent radio frequency (RF) argon plasma spheroidization. In comparison with conventional mechanical alloying techniques, the two-step milling process can be used to prepare alloy powders with uniform scale in a short milling time with no addition of process control agent. This makes the process effective and less contaminating. After RF argon plasma spheroidization, the powders produced exhibit good sphericity, and the number-average diameter is about 8.2 μm with a symmetric unimodal particle size distribution. The powders perform high composition homogeneity and contain predominately supersaturated α 2-Ti3Al phase. The oxygen and carbon contents of the spheroidized powder are 0.47% and 0.050%, respectively.

Sol-gel synthesis and densification of aluminoborosilicate powders. Part 1: Synthesis

NASA Technical Reports Server (NTRS)

Bull, Jeffrey; Selvaduray, Guna; Leiser, Daniel

1992-01-01

Aluminoborosilicate powders high in alumina content were synthesized by the sol-gel process utilizing various methods of preparation. Properties and microstructural effects related to these syntheses were examined. After heating to 600 C for 2 h in flowing air, the powders were amorphous with the metal oxides comprising 87 percent of the weight and uncombusted organics the remainder. DTA of dried powders revealed a T(sub g) at approximately 835 C and an exotherm near 900 C due to crystallization. Powders derived from aluminum secbutoxide consisted of particles with a mean diameter 5 microns less than those from aluminum isopropoxide. Powders synthesized with aluminum isopropoxide produced agglomerates comprised of rod shaped particulates while powders made with the secbutoxide precursor produced irregular glassy shards. Compacts formed from these powders required different loadings for equivalent densities according to the method of synthesis.

Final Report for X-ray Diffraction Sample Preparation Method Development

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

Ely, T. M.; Meznarich, H. K.; Valero, T.

WRPS-1500790, “X-ray Diffraction Saltcake Sample Preparation Method Development Plan/Procedure,” was originally prepared with the intent of improving the specimen preparation methodology used to generate saltcake specimens suitable for XRD-based solid phase characterization. At the time that this test plan document was originally developed, packed powder in cavity supports with collodion binder was the established XRD specimen preparation method. An alternate specimen preparation method less vulnerable, if not completely invulnerable to preferred orientation effects, was desired as a replacement for the method.

Synthesis of highly phase pure (Bi, Pb)-Sr-Ca-Cu-O superconductor

DOEpatents

Dorris, S.E.; Poeppel, R.B.; Prorok, B.C.; Lanagan, M.T.; Maroni, V.A.

1994-10-11

An article and method of manufacture of (Bi,Pb)-Sr-Ca-Cu-O superconductor are disclosed. The superconductor is manufactured by preparing a first powdered mixture of bismuth oxide, lead oxide, strontium carbonate, calcium carbonate and copper oxide. A second powdered mixture is then prepared of strontium carbonate, calcium carbonate and copper oxide. The mixtures are calcined separately with the two mixtures then combined. The resulting combined mixture is then subjected to a powder in tube deformation and thermal processing to produce a substantially phase pure (Bi,Pb)-Sr-Ca-Cu-O superconductor. 5 figs.

Preparation, structure and magnetic properties of synthetic ferrihydrite nanoparticles

NASA Astrophysics Data System (ADS)

Stolyar, S. V.; Yaroslavtsev, R. N.; Bayukov, O. A.; Balaev, D. A.; Krasikov, A. A.; Iskhakov, R. S.; Vorotynov, A. M.; Ladygina, V. P.; Purtov, K. V.; Volochaev, M. N.

2018-03-01

Superparamagnetic ferrihydrite powders with average nanoparticle sizes of 2.5 nm produced by the chemical deposition method. Static and dynamic magnetic properties are measured. As a result of ultrasonic treatment in the cavitation regime of suspensions of ferrihydrite powders in a solution of the albumin protein, the Fe ions are reduced to the metallic state. A sol of ferrihydrite nanoparticles is prepared in an aqueous solution of arabinogalactan polysaccharide.

Polymer infiltration studies

NASA Technical Reports Server (NTRS)

Marchello, Joseph M.

1993-01-01

During the past three months, significant progress has been made on the preparation of carbon fiber composites using advanced polymer resins. The results are set forth in recent reports and publications, and will be presented at forthcoming national and international meetings. Current and ongoing research activities reported herein include: textile composites from powder-coated towpreg; role of surface coating in braiding; prepregger hot sled operation; ribbonizing powder-impregenated towpreg; textile composites from powder-coated towpreg; role of bulk factor powder curtain prepreg process advanced tow placement (ATP) open-section part warpage control. During the coming months research will be directed toward further development of the new powder curtain prepregging method and on ways to customize dry powder towpreg for textile and robotic applications in aircraft part fabrication. Studies of multi-tow powder prepregging and ribbon preparation will be conducted in conjunction with continued development of prepregging technology and the various aspects of composite part fabrication using customized towpreg. Also, during the period ahead work will continue on the analysis of the performance of the new solution prepregger.

Influence of ammonium hydroxide solution on LiMn2O4 nanostructures prepared by modified chemical bath method

NASA Astrophysics Data System (ADS)

Koao, Lehlohonolo F.; Motloung, Setumo V.; Motaung, Tshwafo E.; Kebede, Mesfin A.

2018-04-01

LiMn2O4 (LMO) powders were prepared by modified chemical bath deposition (CBD) method by varying ammonium hydroxide solution (AHS). The volume of the AHS was varied from 5 to 120 mL in order to determine the optimum volume that is needed for preparation of LMO powders. The effect of AHS volume on the structure, morphology, and electrochemical properties of LMO powders was investigated. The X-ray diffraction (XRD) patterns of the LMO powders correspond to the cubic spinel LMO phase. It was found that the XRD peaks increased in intensity with increasing volume of the AHS up to 20 mL. The estimated average grain sizes calculated using the XRD patterns were found to be in the order of 66 ± 1 nm. It was observed that the estimated average grain sizes increased up to 20 mL of AHS. The scanning electron microscopy (SEM) results revealed that the AHS volume does not influence the surface morphology of the prepared nano-powders. Elemental energy dispersive (EDS) analysis mapping conducted on the samples revealed homogeneous distribution of Mn and O for the sample synthesized with 120 mL of AHS. The UV-Vis spectra showed a red shift with an increase in AHS up 20 mL. The cyclic voltammetry and galvanostatic charge/discharge cycle testing confirmed that 20 mL of AHS has superior lithium ion kinetics and electrochemical performance.

Silicon nitride/silicon carbide composite densified materials prepared using composite powders

DOEpatents

Dunmead, S.D.; Weimer, A.W.; Carroll, D.F.; Eisman, G.A.; Cochran, G.A.; Susnitzky, D.W.; Beaman, D.R.; Nilsen, K.J.

1997-07-01

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.

Physical characteristics and aerosolization performance of insulin dry powders for inhalation prepared by a spray drying method.

PubMed

You, Yu; Zhao, Min; Liu, Guangli; Tang, Xing

2007-07-01

The objective of this study was to investigate the influence of formulation excipients on the physical characteristics and aerosolization performance of insulin dry powders for inhalation. Insulin dry powders were prepared by a spray drying technique using excipients such as sugars (trehalose, lactose and dextran), mannitol and amino acids (L-leucine, glycine and threonine). High performance liquid chromatography and the mouse blood glucose method were used for determination of the insulin content. The powder properties were determined and compared by scanning electron microscopy, thermo-gravimetric analysis and size distribution analysis by a time-of-flight technique. The in-vitro aerosolization behaviour of the powders was assessed with an Aerolizer inhaler using a twin-stage impinger. Powder yield and moisture absorption were also determined. Results showed that there was no noticeable change in insulin content in any of the formulations by both assay methods. All powders were highly wrinkled, with median aerodynamic diameters of 2-4 microm, and consequently suitable for pulmonary administration. The tapped density was reduced dramatically when glycine was added. The powders containing mannitol, with or without L-leucine, were less sensitive to moisture. The highest respirable fraction of 67.3 +/- 1.3% was obtained with the formulation containing L-leucine, in contrast to formulations containing glycine and threonine, which had a respirable fraction of 11.2 +/- 3.9% and 23.5 +/- 2.5%, respectively. In addition, powders with good physical properties were achieved by the combination of insulin and trehalose. This study suggests that L-leucine could be used to enhance the aerosolization behaviour of the insulin dry powders for inhalation, and trehalose could potentially be used as an excipient in the formulations.

Arc-melting preparation of single crystal LaB.sub.6 cathodes

DOEpatents

Gibson, Edwin D.; Verhoeven, John D.

1977-06-21

A method for preparing single crystals of lanthanum hexaboride (LaB.sub.6) by arc melting a rod of compacted LaB.sub.6 powder. The method is especially suitable for preparing single crystal LaB.sub.6 cathodes for use in scanning electron microscopes (SEM) and scanning transmission electron microscopes (STEM).

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

PubMed

Sinsuebpol, Chutima; Chatchawalsaisin, Jittima; Kulvanich, Poj

2013-01-01

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. 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. 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. 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.

Preparation of Phosphonic Acid Functionalized Graphene Oxide-modified Aluminum Powder with Enhanced Anticorrosive Properties

NASA Astrophysics Data System (ADS)

He, Lihua; Zhao, Yan; Xing, Liying; Liu, Pinggui; Wang, Zhiyong; Zhang, Youwei; Liu, Xiaofang

2017-07-01

To improve the anticorrosive performance of aluminum powder, a common functional filler in polymer coatings, we report a novel method to prepare graphene oxide modified aluminum powder (GO-Al) using 3-aminoproplyphosphoic acid as "link" agent. The GO nanosheets were firstly functionalized with 3-aminoproplyphosphoic acid (APSA) by the reaction of amine groups of APSA and the epoxy groups of GO. Subsequently, a layer of GO nanosheets uniformly and tightly covered the surface of flaky aluminum particle though the strong linking strength between -PO(OH)2 functional groups of the modified GO and aluminum. The hydrogen evolution experiment suggests that the GO attached on the aluminum powder could effectively improve the anticorrosive performance of the pigments.

[Preparation of panax notoginseng saponins-tanshinone H(A) composite method for pulmonary delivery with spray-drying method and its characterization].

PubMed

Wang, Hua-Mei; Fu, Ting-Ming; Guo, Li-Wei

2013-02-01

To prepare panax notoginseng saponins-tanshinone II(A) composite particles for pulmonary delivery, in order to explore a dry powder particle preparation method ensuring synchronized arrival of multiple components of traditional Chinese medicine compounds at absorption sites. Panax notoginseng saponins-tanshinone II(A) composite particles were prepared with spray-drying method, and characterized by scanning electron microscopy (SEM), confocal laser scanning microscope (CLSM), X-ray diffraction (XRD), infrared analysis (IR), dry laser particle size analysis, high performance liquid chromatography (HPLC) and the aerodynamic behavior was evaluated by a Next Generation Impactor (NGI). The dry powder particles produced had narrow particle size distribution range and good aerodynamic behavior, and could realize synchronized administration of multiple components. The spray-drying method is used to combine traditional Chinese medicine components with different physical and chemical properties in the same particle, and product into traditional Chinese medicine compound particles in line with the requirements for pulmonary delivery.

Sonocatalytic degradation of azo fuchsine in the presence of the Co-doped and Cr-doped mixed crystal TiO2 powders and comparison of their sonocatalytic activities.

PubMed

Wang, Jun; Lv, Yanhui; Zhang, Zhaohong; Deng, Yingqiao; Zhang, Liquan; Liu, Bin; Xu, Rui; Zhang, Xiangdong

2009-10-15

In order to degrade some pollutants effectively under ultrasonic irradiation, the Co-doped and Cr-doped mixed crystal TiO(2) powders, with high sonocatalytic activity, were prepared as sonocatalyst. The Co-doped and Cr-doped mixed crystal TiO(2) powders as sonocatalyst were prepared through sol-gel and heat-treated methods from tetrabutylorthotitanate, and then were characterized by XRD and TG-DTA technologies. In order to compare and evaluate the sonocatalytic activity of the Co-doped and Cr-doped mixed crystal TiO(2) powders, the low power ultrasound was as an irradiation source and the azo fuchsine was chosen as a model compound to be degraded. The degradation process was investigated by UV-vis, TOC, ion chromatogram and HPLC techniques. The results indicated that the sonocatalytic activity of Cr-doped mixed crystal TiO(2) powder was higher than that of Co-doped and undoped mixed crystal TiO(2) powder during the sonocatalytic degradation of the azo fuchsine in aqueous solution. These results may be of great significance for driving sonocatalytic method to treat non- or low-transparent industrial wastewaters.

Preparation and Evaluation of Solid Dispersion Tablets by a Simple and Manufacturable Wet Granulation Method Using Porous Calcium Silicate.

PubMed

Fujimoto, Yumi; Hirai, Nobuaki; Takatani-Nakase, Tomoka; Takahashi, Koichi

2016-01-01

The aim of this study was to prepare and evaluate solid dispersion tablets containing a poorly water-soluble drug using porous calcium silicate (PCS) by a wet granulation method. Nifedipine (NIF) was used as the model poorly water-soluble drug. Solid dispersion tablets were prepared with the wet granulation method using ethanol and water by a high-speed mixer granulator. The binder and disintegrant were selected from 7 and 4 candidates, respectively. The dissolution test was conducted using the JP 16 paddle method. The oral absorption of NIF was studied in fasted rats. Xylitol and crospovidone were selected as the binder and disintegrant, respectively. The dissolution rates of NIF from solid dispersion formulations were markedly enhanced compared with NIF powder and physical mixtures. Powder X-ray diffraction (PXRD) confirmed the reduced crystallinity of NIF in the solid dispersion formulations. Fourier transform infrared (FT-IR) showed the physical interaction between NIF and PCS in the solid dispersion formulations. NIF is present in an amorphous state in granules prepared by the wet granulation method using water. The area under the plasma concentration-time curve (AUC) and peak concentration (C(max)) values of NIF after dosing rats with the solid dispersion granules were significantly greater than those after dosing with NIF powder. The solid dispersion formulations of NIF prepared with PCS using the wet granulation method exhibited accelerated dissolution rates and superior oral bioavailability. This method is very simple, and may be applicable to the development of other poorly water-soluble drugs.

Preparation of magnesium metal matrix composites by powder metallurgy process

NASA Astrophysics Data System (ADS)

Satish, J.; Satish, K. G., Dr.

2018-02-01

Magnesium is the lightest metal used as the source for constructional alloys. Today Magnesium based metal matrix composites are widely used in aerospace, structural, oceanic and automobile applications for its light weight, low density(two thirds that of aluminium), good high temperature mechanical properties and good to excellent corrosion resistance. The reason of designing metal matrix composite is to put in the attractive attributes of metals and ceramics to the base metal. In this study magnesium metal matrix hybrid composite are developed by reinforcing pure magnesium with silicon carbide (SiC) and aluminium oxide by method of powder metallurgy. This method is less expensive and very efficient. The Hardness test was performed on the specimens prepared by powder metallurgy method. The results revealed that the micro hardness of composites was increased with the addition of silicon carbide and alumina particles in magnesium metal matrix composites.

Enhancement of the dissolution rate and bioavailability of fenofibrate by a melt-adsorption method using supercritical carbon dioxide

PubMed Central

Cha, Kwang-Ho; Cho, Kyung-Jin; Kim, Min-Soo; Kim, Jeong-Soo; Park, Hee Jun; Park, Junsung; Cho, Wonkyung; Park, Jeong-Sook; Hwang, Sung-Joo

2012-01-01

Background: The aim of this study was to enhance the bioavailability of fenofibrate, a poorly water-soluble drug, using a melt-adsorption method with supercritical CO2. Methods: Fenofibrate was loaded onto Neusilin® UFL2 at different weight ratios of fenofibrate to Neusilin UFL2 by melt-adsorption using supercritical CO2. For comparison, fenofibrate-loaded Neusilin UFL2 was prepared by solvent evaporation and hot melt-adsorption methods. The fenofibrate formulations prepared were characterized by differential scanning calorimetry, powder x-ray diffractometry, specific surface area, pore size distribution, scanning electron microscopy, and energy-dispersive x-ray spectrometry. In vitro dissolution and in vivo bioavailability were also investigated. Results: Fenofibrate was distributed into the pores of Neusilin UFL2 and showed reduced crystal formation following adsorption. Supercritical CO2 facilitated the introduction of fenofibrate into the pores of Neusilin UFL2. Compared with raw fenofibrate, fenofibrate from the prepared powders showed a significantly increased dissolution rate and better bioavailability. In particular, the area under the drug concentration-time curve and maximal serum concentration of the powders prepared using supercritical CO2 were 4.62-fold and 4.52-fold greater than the corresponding values for raw fenofibrate. Conclusion: The results of this study highlight the usefulness of the melt-adsorption method using supercritical CO2 for improving the bioavailability of fenofibrate. PMID:23118538

Preparation and antibacterial properties of titanium-doped ZnO from different zinc salts

PubMed Central

2014-01-01

To research the relationship of micro-structures and antibacterial properties of the titanium-doped ZnO powders and probe their antibacterial mechanism, titanium-doped ZnO powders with different shapes and sizes were prepared from different zinc salts by alcohothermal method. The ZnO powders were characterized by X-ray powder diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), ultraviolet-visible spectroscopy (UV-vis), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and selected area electron diffraction (SAED), and the antibacterial activities of titanium-doped ZnO powders on Escherichia coli and Staphylococcus aureus were evaluated. Furthermore, the tested strains were characterized by SEM, and the electrical conductance variation trend of the bacterial suspension was characterized. The results indicate that the morphologies of the powders are different due to preparation from different zinc salts. The XRD results manifest that the samples synthesized from zinc acetate, zinc nitrate, and zinc chloride are zincite ZnO, and the sample synthesized from zinc sulfate is the mixture of ZnO, ZnTiO3, and ZnSO4 · 3Zn (OH)2 crystal. UV-vis spectra show that the absorption edges of the titanium-doped ZnO powders are red shifted to more than 400 nm which are prepared from zinc acetate, zinc nitrate, and zinc chloride. The antibacterial activity of titanium-doped ZnO powders synthesized from zinc chloride is optimal, and its minimum inhibitory concentration (MIC) and minimum bactericidal concentration (MBC) are lower than 0.25 g L−1. Likewise, when the bacteria are treated by ZnO powders synthesized from zinc chloride, the bacterial cells are damaged most seriously, and the electrical conductance increment of bacterial suspension is slightly high. It can be inferred that the antibacterial properties of the titanium-doped ZnO powders are relevant to the microstructure, particle size, and the crystal. The powders can damage the cell walls; thus, the electrolyte is leaked from cells. PMID:24572014

A convenient method to prepare emulsified polyacrylate nanoparticles from powders [corrected] for drug delivery applications.

PubMed

Garay-Jimenez, Julio C; Turos, Edward

2011-08-01

We describe a method to obtain purified, polyacrylate nanoparticles in a homogeneous powdered form that can be readily reconstituted in aqueous media for in vivo applications. Polyacrylate-based nanoparticles can be easily prepared by emulsion polymerization using a 7:3 mixture of butyl acrylate and styrene in water containing sodium dodecyl sulfate as a surfactant and potassium persulfate as a water-soluble radical initiator. The resulting emulsions contain nanoparticles measuring 40-50 nm in diameter with uniform morphology, and can be purified by centrifugation and dialysis to remove larger coagulants as well as residual surfactant and monomers associated with toxicity. These purified emulsions can be lyophilized in the presence of maltose (a non-toxic cryoprotectant) to provide a homogeneous dried powder, which can be reconstituted as an emulsion by addition of an aqueous diluent. Dynamic light scattering and microbiological experiments were carried out on the reconstituted nanoparticles. This procedure allows for ready preparation of nanoparticle emulsions for drug delivery applications. Copyright © 2011 Elsevier Ltd. All rights reserved.

Green fabrication of composite cathode with attractive performance for solid oxide fuel cells through facile inkjet printing

NASA Astrophysics Data System (ADS)

Li, Chao; Chen, Huili; Shi, Huangang; Tade, Moses O.; Shao, Zongping

2015-01-01

The inkjet printing technique has numerous advantages and is attractive in solid oxide fuel cell (SOFC) fabrication, especially for the dense thin electrolyte layer because of its ultrafine powder size. In this study, we exploited the technique for the fabrication of a porous SDC/SSC composite cathode layer using environmentally friendly water-based ink. An optimized powder synthesis method was applied to the preparation of the well-dispersed suspension. In view of the easy sintering of the thin film layer prepared by inkjet printing, 10 wt.% pore former was introduced to the ink. The results indicate that the cell with the inkjet printing cathode layer exhibits a fantastic electrochemical performance, with a PPD as high as 940 mW cm-2 at 750 °C, which is comparable to that of a cell prepared using the conventional wet powder spraying method, suggesting a promising application of inkjet printing on electrode layer fabrication.

Improved tretinoin photostability in a topical nanomedicine replacing original liquid suspension with spray-dried powder with no loss of effectiveness.

PubMed

Marchiori, M C L; Rascovetzki, R H; Ourique, A F; Rigo, L A; Silva, C B; Beck, R C R

2013-04-01

The use of spray-dried powders containing tretinoin-loaded nanocapsules instead of the original liquid suspension, aimed at the preparation of dermatological nanomedicines with improved photostability, was investigated. Powders were prepared using lactose as a drying adjuvant. Hydrogels were prepared using two approaches: dispersing Carbopol Ultrez 10 in an aqueous redispersion of the powder or incorporating the powder in previously formed hydrogels. The photodegradation of tretinoin in hydrogels prepared with the powders showed similar half-life times (around 19.5 h) compared to preparations with the original liquid nanocapsules (20.7 ± 1.4 h), regardless of the preparation approach. In addition, the topical nanomedicines prepared with the spray-dried powders presented a significant improvement in tretinoin photostability compared to the formulation containing the non-encapsulated drug. This study verified that the addition of the spray-dried powders containing tretinoin-loaded lipid-core nanocapsules to hydrogels did not influence the photoprotection of the drug compared with the preparation procedure using the original liquid suspension.

Polymer infiltration studies

NASA Technical Reports Server (NTRS)

Marchello, Joseph M.

1992-01-01

Significant progress has been made during the past three months on the preparation of carbon fiber composites using advanced polymer resins. The results are set forth in recent reports and publications, and will be presented at forthcoming national and international meetings. Current and ongoing research activities reported herein include: powdered tow ribbonizing; unitape from powdered tow; customized towpreg for textiles and ATP; and textile composite research. During the period ahead research will be directed toward further development of the new powder curtain prepregging method and on ways to customize dry powder towpreg for textile and robotic applications in aircraft part fabrication. Studies of multi-tow powder prepregging and ribbon preparation will be initiated in conjunction with continued development of prepregging technology and the various aspects of composite part fabrication using customized towpreg. Also, a major effort during the coming months will be participating in the analysis of the performance of the new solution prepregger.

Use of Powder PEG-3350 as a Sole Bowel Preparation

PubMed Central

Arora, Manish

2008-01-01

Objective: To assess the efficacy of low-volume powder polyethylene glycol (PEG)-3350 as a sole bowel preparation for colonoscopy. Methods: This case series examined 245 consecutive patients (a mixture of inpatients and outpatients undergoing screening colonoscopy) at a hospital endoscopy center over a 2-year period. The patients received powder PEG-3350 in the amount of 204 g dissolved in 32 oz of water and taken in 3 divided doses 1 hour apart with 8 oz of water in between each dose. Colon preparation scores (CPS) were used to assess the quality of colon cleansing. The results obtained from the 245 patients were collated and compared to those of patients receiving sodium phosphate, the historical control. Results: The mean CPS was calculated to be 3.43, with a standard deviation of 1.12. Of the 245 patients, 92 were scored with a grade of 4, and 5 patients had incomplete colonoscopies secondary to failure of bowel preparation (CPS=0). Among the remaining patients, 22 and 26 were graded as poor (CPS=1) or fair (CPS=2) bowel preparations, respectively. Conclusion: The low-volume powder PEG-3350 formula used in our case series showed effective colon cleansing and may be considered for use as a sole bowel preparation. PMID:21960925

A critical evaluation and a search for the ideal colonoscopic preparation.

PubMed

Arora, Manish; Senadhi, Viplove; Arora, Deepika; Weinstock, Joyce; Dubin, Ethan; Okolo, Patrick I; Dutta, Sudhir K

2013-04-01

The aim of this study was to evaluate the efficacy of various bowel preparations in accomplishing colonic cleansing for optimal mucosal visualization during colonoscopy. The study included a cohort of 980 patients who underwent colonoscopy at our endoscopy center within the last 3 years. All of the study patients were subdivided into four groups. Each group included 245 patients, all receiving a different type of bowel preparation. The bowel preparations used in this study included: magnesium citrate (Group I), a combination of oral sodium phosphate (fleets) and powder PEG-3350 (Group II), powder polyethylene glycol-3350 (PEG-3350 powder for Group III), and oral sodium phosphate (fleets for Group IV). A Colon Prep Score (CPS) was devised to compare the quality of the different bowel preparations used. The colonoscopy results from all of these patients were tabulated and analyzed statistically and expressed as mean ± 1 standard deviation. Statistical analysis was performed using a one way ANOVA with Holm-Sidak method for intergroup analysis. Group I patients received magnesium citrate and had a mean CPS ± 1 SD of 3.11 ± 0.91. Group II patients (fleets and powder PEG-3350 combination) achieved a CPS of 3.37 ± 1.16. The patients in Group III (powder PEG-3350) actually showed the highest mean CPS of 3.44 ± 1.12. Group IV patients who used oral sodium phosphate alone reached a mean CPS of 3.23 ± 1.01. Group III patients (powder PEG-3350 only) demonstrated a statistically higher CPS (P<0.0006) in colon cleansing as compared to Group I patients (magnesium citrate). Similarly, Group II patients (oral sodium phosphate and powder PEG-3350 combination) also showed improved colon cleansing statistically (P<0.006) as compared to Group I patients (magnesium citrate). Overall, all four colon preparations achieved an average CPS greater than 3.0 indicating clinically adequate colonic cleansing. However, powder PEG-3350 alone and in combination with oral sodium phosphate was observed to be statistically superior to magnesium citrate, when used for colon preparation for colonoscopy. Copyright © 2012 Elsevier Masson SAS. All rights reserved.

METHOD FOR THE PREPARATION OF STABLE ACTINIDE METAL OXIDE-CONTAINING SLURRIES AND OF THE OXIDES THEREFOR

DOEpatents

Hansen, R.S.; Minturn, R.E.

1958-02-25

This patent deals with a method of preparing actinide metal oxides of a very fine particle size and of forming stable suspensions therefrom. The process consists of dissolving the nitrate of the actinide element in a combustible organic solvent, converting the solution obtained into a spray, and igniting the spray whereby an oxide powder is obtained. The oxide powder is then slurried in an aqueous soiution of a substance which is adsorbable by said oxides, dspersed in a colloid mill whereby a suspension is obtained, and electrodialyzed until a low spectiic conductance is reached.

Microstructural and mechanical characteristics of porous iron prepared by powder metallurgy.

PubMed

Capek, Jaroslav; Vojtěch, Dalibor

2014-10-01

The demand for porous biodegradable load-bearing implants has been increasing recently. Based on investigations of biodegradable stents, porous iron may be a suitable material for such applications. In this study, we prepared porous iron samples with porosities of 34-51 vol.% by powder metallurgy using ammonium bicarbonate as a space-holder material. We studied sample microstructure (SEM-EDX and XRD), flexural and compressive behaviors (universal loading machine) and hardness HV5 (hardness tester) of the prepared samples. Sample porosity increased with the amount of spacer in the initial mixtures. Only the pore surfaces had insignificant oxidation and no other contamination was observed. Increasing porosity decreased the mechanical properties of the samples; although, the properties were still comparable with human bone and higher than those of porous non-metallic biomaterials and porous magnesium prepared in a similar way. Based on these results, powder metallurgy appears to be a suitable method for the preparation of porous iron for orthopedic applications. Copyright © 2014 Elsevier B.V. All rights reserved.

Methods for and products of processing nanostructure nitride, carbonitride and oxycarbonitride electrode power materials by utilizing sol gel technology for supercapacitor applications

DOEpatents

Huang, Yuhong; Wei, Oiang; Chu, Chung-tse; Zheng, Haixing

2001-01-01

Metal nitride, carbonitride, and oxycarbonitride powder with high surface area (up to 150 m.sup.2 /g) is prepared by using sol-gel process. The metal organic precursor, alkoxides or amides, is synthesized firstly. The metal organic precursor is modified by using unhydrolyzable organic ligands or templates. A wet gel is formed then by hydrolysis and condensation process. The solvent in the wet gel is then be removed supercritically to form porous amorphous hydroxide. This porous hydroxide materials is sintered to 725.degree. C. under the ammonia flow and porous nitride powder is formed. The other way to obtain high surface area nitride, carbonitride, and oxycarbonitride powder is to pyrolyze polymerized templated metal amides aerogel in an inert atmosphere. The electrochemical capacitors are prepared by using sol-gel prepared nitride, carbonitride, and oxycarbonitride powder. Two methods are used to assemble the capacitors. Electrode is formed either by pressing the mixture of nitride powder and binder to a foil, or by depositing electrode coating onto metal current collector. The binder or coating is converted into a continuous network of electrode material after thermal treatment to provide enhanced energy and power density. Liquid electrolyte is soaked into porous electrode. The electrochemical capacitor assembly further has a porous separator layer between two electrodes/electrolyte and forming a unit cell.

Method of preparing a powdered, electrically insulative separator for use in an electrochemical cell

DOEpatents

Cooper, Tom O.; Miller, William E.

1978-01-01

A secondary electrochemical cell includes electrodes separated by a layer of electrically insulative powder. The powder includes refractory materials selected from the oxides and nitrides of metals and metaloids. The powdered refractory material, blended with electrolyte particles, is compacted as layers onto an electrode to form an integral electrode structure and assembled into the cell. The assembled cell is heated to its operating temperature leaving porous layers of electrically insulative, refractory particles, containing molten electrolyte between the electrodes.

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

Method of preparing porous, rigid ceramic separators for an electrochemical cell

DOEpatents

Bandyopadhyay, Gautam; Dusek, Joseph T.

1981-01-01

Porous, rigid separators for electrochemical cells are prepared by first calcining particles of ceramic material at temperatures above about 1200.degree. C. for a sufficient period of time to reduce the sinterability of the particles. A ceramic powder that has not been calcined is blended with the original powder to control the porosity of the completed separator. The ceramic blend is then pressed into a sheet of the desired shape and sintered at a temperature somewhat lower than the calcination temperature. Separator sheets of about 1 to 2.5 mm thickness and 30 to 70% porosity can be prepared by this technique. Ceramics such as yttria, magnesium oxide and magnesium-aluminum oxide have advantageously been used to form separators by this method.

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.

Method of manufacturing a high temperature superconductor with improved transport properties

DOEpatents

Balachandran, Uthamalingam; Siegel, Richard W.; Askew, Thomas R.

2001-01-01

A method of preparing a high temperature superconductor. A method of preparing a superconductor includes providing a powdered high temperature superconductor and a nanophase paramagnetic material. These components are combined to form a solid compacted mass with the paramagnetic material disposed on the grain boundaries of the polycrystaline high temperature superconductor.

Effect of annealing on the structural and optical properties of TiO2 powder prepared by sol-gel route

NASA Astrophysics Data System (ADS)

Halder, Nilanjan; Misra, Kamakhya Prakash

2016-05-01

Using titanium isopropoxide as the precursor, Titanium dioxide (TiO2) powder was synthesized via sol-gel method, a promising low temperature route for preparing nanosized metal oxide semiconductors with good homogeneity at low cost. The as-prepared nano powder was thermally treated in air at 550, 650, 750, 900 and 1100°C for 1hr after drying at room temperature and used for further characterization. X-ray diffraction measurements showed that the annealing treatment has a strong impact on the crystal phase of TiO2 samples. The crystallite size as calculated from Debye Scherer formula lies in the range 29-69 nm and is found to increase with increase in annealing temperature. Photoluminescence studies exhibit an improvement in the optical efficiency of the samples with post synthesis heat treatment. Annealing at temperature above 900°C results in a degradation of the structural and optical quality of the TiO2 nano powder samples.

Extemporaneous (magistral) preparation of oral medicines for children in European hospitals.

PubMed

Brion, F; Nunn, A J; Rieutord, A

2003-04-01

To evaluate methods of preparation of oral medicines in European children's hospitals when drugs prescribed are unlicensed or off-label, and to determine whether such extemporaneously prepared medicines are available as suitable, authorized products in other countries. A questionnaire was distributed to 41 hospital pharmacists in 18 European countries, requesting information on the most frequent extemporaneously prepared oral liquid, powder and capsule medicines, and on their formulation and stability. Information was gathered on the availability of suitable authorized forms of these medicines in other European countries, the USA and Australia. 21 questionnaires from 16 countries returned showed that the methods of extemporaneous preparation vary in different European countries with, for example, liquid preparations predominating in England and Sweden, capsules in France and Spain, and powders in Finland and Italy. The top 20 preparations are made in many different strengths and formulations. The same drug may be prepared in liquid, capsule or powder form, depending on the country. Many of the extemporaneous preparations were available as suitable authorized paediatric medicines in other countries. The quality of information available on formulation and stability was limited, and there was concern about the availability and quality of chemical ingredients. Preparation of children's oral medicines is subject to much variation in hospitals throughout Europe and there is little harmonization of formulations or information on stability of products. The European Union could be the focus for improving the availability of appropriate authorized medicines for children and ensuring that when extemporaneous preparation is necessary it is of a common high standard.

METHOD OF PREPARING A FUEL ELEMENT FOR A NUCLEAR REACTOR

DOEpatents

Hauth, J.J.; Anicetti, R.J.

1962-12-01

A method is described for preparing a fuel element for a nuclear reactor. According to the patent uranium dioxide is compacted in a metal tabe by directlng intense sound waves at the tabe prior to tamp packing or vibration compaction of the powder. (AEC)

Optical properties of titanium di-oxide thin films prepared by dip coating method

NASA Astrophysics Data System (ADS)

Biswas, Sayari; Rahman, Kazi Hasibur; Kar, Asit Kumar

2018-05-01

Titanium dioxide (TiO2) thin films were prepared by sol-gel dip coating method on ITO coated glass substrate. The sol was synthesized by hydrothermal method at 90°C. The sol was then used to make TiO2 films by dip coating. After dip coating the rest of the sol was dried at 100°C to make TiO2 powder. Thin films were made by varying the number of dipping cycles and were annealed at 500°C. XRD study was carried out for powder samples that confirms the formation of anatase phase. Transmission spectra of thin films show sharp rise in the violet-ultraviolet transition region and a maximum transmittance of ˜60%. Band gap of the prepared films varies from 3.15 eV to 3.22 eV.

Melamine detection in infant formula powder using near- and mid-infrared spectroscopy.

PubMed

Mauer, Lisa J; Chernyshova, Alona A; Hiatt, Ashley; Deering, Amanda; Davis, Reeta

2009-05-27

Near- and mid-infrared spectroscopy methods (NIR, FTIR-ATR, FTIR-DRIFT) were evaluated for the detection and quantification of melamine in infant formula powder. Partial least-squares (PLS) models were established for correlating spectral data to melamine concentration: R(2) > 0.99, RMSECV ≤ 0.9, and RPD ≥ 12. Factorization analysis of spectra was able to differentiate unadulterated infant formula powder from samples containing 1 ppm melamine with no misclassifications, a confidence level of 99.99%, and selectivity > 2. These nondestructive methods require little or no sample preparation. The NIR method has an assay time of 1 min, and a 2 min total time to detection. The FTIR methods require up to 5 min for melamine detection. Therefore, NIR and FTIR methods enable rapid detection of 1 ppm melamine in infant formula powder.

Consumer acceptance and aroma characterization of navy bean (Phaseolus vulgaris) powders prepared by extrusion and conventional processing methods.

PubMed

Szczygiel, Edward J; Harte, Janice B; Strasburg, Gale M; Cho, Sungeun

2017-09-01

Food products produced with bean ingredients are gaining in popularity among consumers due to the reported health benefits. Navy bean (Phaseolus vulgaris) powder produced through extrusion can be considered as a resource-efficient alternative to conventional methods, which often involve high water inputs. Therefore, navy bean powders produced with extrusion and conventional methods were assessed for the impact of processing on consumer liking in end-use products and odor-active compounds. Consumer acceptance results reveal significant differences in flavor, texture and overall acceptance scores of several products produced with navy bean powder. Crackers produced with extruded navy bean powder received higher hedonic flavor ratings than those produced with commercial navy bean powder (P < 0.001). GC-O data showed that the commercial powder produced through conventional processing had much greater contents of several aliphatic aldehydes commonly formed via lipid oxidation, such as hexanal, octanal and nonanal with descriptors of 'grassy', 'nutty', 'fruity', 'dusty', and 'cleaner', compared to the extruded powder. Extrusion processed navy bean powders were preferred over commercial powders for certain navy bean powder applications. This is best explained by substantial differences in aroma profiles of the two powders that may have been caused by lipid oxidation. © 2017 Society of Chemical Industry. © 2017 Society of Chemical Industry.

C18-coated stir bar sorptive extraction combined with high performance liquid chromatography-electrospray tandem mass spectrometry for the analysis of sulfonamides in milk and milk powder.

PubMed

Yu, Chunhe; Hu, Bin

2012-02-15

A simple, rapid, sensitive, inexpensive and less sample consuming method of C(18)-stir bar sorptive extraction (SBSE)-high performance liquid chromatography (HPLC)-tandem mass spectrometry (MS/MS) was proposed for the determination of six sulfonamides in milk and milk powder samples. C(18) silica particles coated stir bar was prepared by adhesion method, and two kinds of adhesive glue, polydimethylsiloxane (PDMS) sol and epoxy glue were tried. It was found that the C(18)-coated stir bar prepared by PDMS sol as adhesive glue is more robust than that prepared by epoxy glue when liquid desorption was employed, in terms of both lifetime and organic solvent tolerance. The preparation of C(18) stir bar was simple with good mechanic strength and the stir bar could be reused for more than 20 times. Granular coating has relatively high specific surface area and is propitious to sorptive extraction based process. Compared to conventional PDMS SBSE coating, C(18) coating shows good affinity to the target polar/weak polar sulfonamides. To achieve optimum SBSE extraction performance, several parameters including extraction and desorption time, ionic strength, sample pH and stirring speed were investigated. The detection limits of the proposed method for six sulfonamides were in the range of 0.9-10.5 μg/L for milk and 2.7-31.5 μg/kg for milk powder. Good linearities were obtained for sulfonamides with the correlation coefficients (R) above 0.9922. Finally, the proposed method was successfully applied to the determination of sulfonamides in milk and milk powder samples and satisfied recoveries of spiked target compounds in real samples were obtained. Copyright © 2012 Elsevier B.V. All rights reserved.

Method of producing Pb-stabilized superconductor precursors and method of producing superconductor articles therefrom

DOEpatents

Kroeger, D.M.; Hsu, H.S.; Brynestad, J.

1995-03-07

Metal oxide superconductor powder precursors are prepared in an aerosol pyrolysis process. A solution of the metal cations is introduced into a furnace at 600--1,000 C for 0.1 to 60 seconds. The process produces micron to submicron size powders without the usual loss of the lead stabilizer. The resulting powders have a narrow particle size distribution, a small grain size, and are readily converted to a superconducting composition upon subsequent heat treatment. The precursors are placed in a metal body deformed to form a wire or tape and heated to form a superconducting article. The fine powders permit a substantial reduction in heat treatment time, thus enabling a continuous processing of the powders into superconducting wire, tape or multifilamentary articles by the powder-in-tube process. 3 figs.

Method of producing Pb-stabilized superconductor precursors and method of producing superconductor articles therefrom

DOEpatents

Kroeger, Donald M.; Hsu, Huey S.; Brynestad, Jorulf

1995-01-01

Metal oxide superconductor powder precursors are prepared in an aerosol pyrolysis process. A solution of the metal cations is introduced into a furnace at 600.degree.-1000.degree. C. for 0.1 to 60 seconds. The process produces micron to submicron size powders without the usual loss of the lead stabilizer. The resulting powders have a narrow particle size distribution, a small grain size, and are readily converted to a superconducting composition upon subsequent heat treatment. The precursors are placed in a metal body deformed to form a wire or tape and heated to form a superconducting article. The fine powders permit a substantial reduction in heat treatment time, thus enabling a continuous processing of the powders into superconducting wire, tape or multifilamentary articles by the powder-in-tube process.

Grinding Si3N4 Powder In Si3N4 Equipment

NASA Technical Reports Server (NTRS)

Herbell, Thomas P.; Freedman, Marc R.; Kiser, James D.

1989-01-01

Three methods of grinding compared. Report based on study of grinding silicon nitride powder in preparation for sintering into solid ceramic material. Attrition, vibratory, and ball mills lined with reaction-bonded silicon nitride tested. Rates of reduction of particle sizes and changes in chemical compositions of powders measured so grinding efficiences and increases in impurity contents from wear of mills and media evaluated for each technique.

Study of AC Magnetic Properties and Core Losses of Fe/Fe3O4-epoxy Resin Soft Magnetic Composite

NASA Astrophysics Data System (ADS)

Laxminarayana, T. A.; Manna, Subhendu Kumar; Fernandes, B. G.; Venkataramani, N.

Soft Magnetic Composites (SMC) were prepared by coating of nanocrystalline Fe3O4 particles, synthesized by co-precipitation method, on atomized iron powder of particle size less than 53 μm in size using epoxy resin as a binder between iron and Fe3O4. Fe3O4 was chosen, for its high electric resistivity and suitable magnetic properties, to keep the coating layer magnetic and seek improvement to the magnetic properties of SMC. SEM images and XRD patterns were recorded in order to investigate the coatings on the surface of iron powder. A toroid was prepared by cold compaction of coated iron powder at 1050 MPa and subsequently cured at 150˚C for 1 hr in argon atmosphere. For comparison of properties, a toroid of uncoated iron powder was also compacted at 1050 MPa and annealed at 600˚C for 2 hr in argon atmosphere. The coated iron powder composite has a resistivity of greater than 200 μΩm, measured by four probe method. A comparison of Magnetic Hysteresis loops and core losses using B-H Loop tracer in the frequency range 0 to 1500 Hz on the coated and uncoated iron powder is reported.

Effect of milling methods on performance of Ni-Y 2O 3-stabilized ZrO 2 anode for solid oxide fuel cell

NASA Astrophysics Data System (ADS)

Cho, Hyoup Je; Choi, Gyeong Man

A Ni-YSZ (Y 2O 3-stabilized ZrO 2) composite is commonly used as a solid oxide fuel cell anode. The composite powders are usually synthesized by mixing NiO and YSZ powders. The particle size and distribution of the two phases generally determine the performance of the anode. Two different milling methods are used to prepare the composite anode powders, namely, high-energy milling and ball-milling that reduce the particle size. The particle size and the Ni distribution of the two composite powders are examined. The effects of milling on the performance are evaluated by using both an electrolyte-supported, symmetric Ni-YSZ/YSZ/Ni-YSZ cell and an anode-supported, asymmetric cell. The performance is examined at 800 °C by impedance analysis and current-voltage measurements. Pellets made by using high-energy milled NiO-YSZ powders have much smaller particle sizes and a more uniform distribution of Ni particles than pellets made from ball-milled powder, and thus the polarization resistance of the electrode is also smaller. The maximum power density of the anode-supported cell prepared by using the high-energy milled powder is ∼850 mW cm -2 at 800 °C compared with ∼500 mW cm -2 for the cell with ball-milled powder. Thus, high-energy milling is found to be more effective in reducing particle size and obtaining a uniform distribution of Ni particles.

Preparation of fine powdered composite for latent heat storage

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

Fořt, Jan, E-mail: jan.fort.1@fsv.cvut.cz; Trník, Anton, E-mail: anton.trnik@fsv.cvut.cz; Pavlíková, Milena, E-mail: milena.pavlikova@fsv.cvut.cz

Application of latent heat storage building envelope systems using phase-change materials represents an attractive method of storing thermal energy and has the advantages of high-energy storage density and the isothermal nature of the storage process. This study deals with a preparation of a new type of powdered phase change composite material for thermal energy storage. The idea of a composite is based upon the impregnation of a natural silicate material by a reasonably priced commercially produced pure phase change material and forming the homogenous composite powdered structure. For the preparation of the composite, vacuum impregnation method is used. The particlemore » size distribution accessed by the laser diffraction apparatus proves that incorporation of the organic phase change material into the structure of inorganic siliceous pozzolana does not lead to the clustering of the particles. The compatibility of the prepared composite is characterized by the Fourier transformation infrared analysis (FTIR). Performed DSC analysis shows potential of the developed composite for thermal energy storage that can be easily incorporated into the cement-based matrix of building materials. Based on the obtained results, application of the developed phase change composite can be considered with a great promise.« less

Straightforward fabrication of black nano silica dusting powder for latent fingerprint imaging

NASA Astrophysics Data System (ADS)

Komalasari, Isna; Krismastuti, Fransiska Sri Herwahyu; Elishian, Christine; Handayani, Eka Mardika; Nugraha, Willy Cahya; Ketrin, Rosi

2017-11-01

Imaging of latent fingerprint pattern (aka fingermark) is one of the most important and accurate detection methods in forensic investigation because of the characteristic of individual fingerprint. This detection technique relies on the mechanical adherence of fingerprint powder to the moisture and oily component of the skin left on the surface. The particle size of fingerprint powder is one of the critical parameter to obtain excellent fingerprint image. This study develops a simple, cheap and straightforward method to fabricate Nano size black dusting fingerprint powder based on Nano silica and applies the powder to visualize latent fingerprint. The nanostructured silica was prepared from tetraethoxysilane (TEOS) and then modified with Nano carbon, methylene blue and sodium acetate to color the powder. Finally, as a proof-of-principle, the ability of this black Nano silica dusting powder to image latent fingerprint is successfully demonstrated and the results show that this fingerprint powder provides clearer fingerprint pattern compared to the commercial one highlighting the potential application of the nanostructured silica in forensic science.

Diamond-Silicon Carbide Composite And Method For Preparation Thereof

DOEpatents

Qian, Jiang; Zhao, Yusheng

2005-09-06

Fully dense, diamond-silicon carbide composites are prepared from ball-milled microcrystalline diamond/amorphous silicon powder mixture. The ball-milled powder is sintered (P=5-8 GPa, T=1400K-2300K) to form composites having high fracture toughness. A composite made at 5 GPa/1673K had a measured fracture toughness of 12 MPa.multidot.m.sup.1/2. By contrast, liquid infiltration of silicon into diamond powder at 5 GPa/1673K produces a composite with higher hardness but lower fracture toughness. X-ray diffraction patterns and Raman spectra indicate that amorphous silicon is partially transformed into nanocrystalline silicon at 5 GPa/873K, and nanocrystalline silicon carbide forms at higher temperatures.

Synthesis and characterization of 2D graphene sheets from graphite powder

NASA Astrophysics Data System (ADS)

Patel, Rakesh V.; Patel, R. H.; Chaki, S. H.

2018-05-01

Graphene is 2D material composed of one atom thick hexagonal layer. This material has attracted great attention among scientific community because of its high surface area, excellent mechanical properties and conductivity due to free electrons in the 2D lattice. There are various approaches to prepare graphene nanosheets such as top-down approach where graphite exfoliation and nanotube unwrapping can be done. The bottom up approach involves deposition of hydrocarbon through CVD, epitaxial method and organo-synthesis etc.. In present studies top down approach method was used to prepare graphene. The graphite powder with around 20 µm to 150µm particle size was subjected to concentrated strong acid in presence of strong oxidizing agent in order to increase the d-spacing between layers which leads to the disruption of crystal lattice as confirmed by XRD (X'pert Philips). FT Raman spectra taken via (Renishaw InVia microscope) of pristine powder and Graphene oxide revealed the increase in D-band and reduction in G-Band. These exfoliated sheets have oxygen rich complexes at the surface of the layers as characterised by FTIR technique. The GO powder was ultrasonicated to prepare the stable suspension of Graphene. The graphene layers were observed under TEM (Philips Tecnai 20) as 2dimensional sheets with around 1µm sizes.

Method of freeform fabrication by selective gelation of powder suspensions

DOEpatents

Baskaran, S.; Graff, G.L.

1997-12-09

The present invention is a novel method for freeform fabrication. Specifically, the method of solid freeform fabrication has the steps of: (a) preparing a slurry by mixing powder particles with a suspension medium and a gelling polysaccharide; (b) making a layer by depositing an amount of said powder slurry in a confined region; (c) hardening a selected portion of the layer by applying a gelling agent to the selected portion; and (d) repeating steps (b) and (c) to make successive layers and forming a layered object. In many applications, it is desirable to remove unhardened material followed by heating to remove gellable polysaccharide then sintering. 2 figs.

Method of freeform fabrication by selective gelation of powder suspensions

DOEpatents

Baskaran, Suresh; Graff, Gordon L.

1997-01-01

The present invention is a novel method for freeform fabrication. Specifically, the method of solid freeform fabrication has the steps of: (a) preparing a slurry by mixing powder particles with a suspension medium and a gelling polysaccharide; (b) making a layer by depositing an amount of said powder slurry in a confined region; (c) hardening a selected portion of the layer by applying a gelling agent to the selected portion; and (d) repeating steps (b) and (c) to make successive layers and forming a layered object. In many applications, it is desirable to remove unhardened material followed by heating to remove gellable polysaccharide then sintering.

Method of preparing porous, rigid ceramic separators for an electrochemical cell. [Patent application

DOEpatents

Bandyopadhyay, G.; Dusek, J.T.

Porous, rigid separators for electrochemical cells are prepared by first calcining particles of ceramic material at temperatures above about 1200/sup 0/C for a sufficient period of time to reduce the sinterability of the particles. A ceramic powder that has not been calcined is blended with the original powder to control the porosity of the completed separator. The ceramic blend is then pressed into a sheet of the desired shape and sintered at a temperature somewhat lower than the calcination temperature. Separator sheets of about 1 to 2.5 mm thickness and 30 to 70% porosity can be prepared by this technique. Ceramics such as yttria, magnesium oxide, and magnesium-aluminium oxide have advantageously been used to form separators by this method.

Process for the synthesis of iron powder

DOEpatents

Not Available

1982-03-06

A process for preparing iron powder suitable for use in preparing the iron-potassium perchlorate heat-powder fuel mixture used in thermal batteries, comprises preparing a homogeneous, dense iron oxide hydroxide precipitate by homogeneous precipitation from an aqueous mixture of a ferric salt, formic or sulfuric acid, ammonium hydroxide and urea as precipitating agent; and then reducing the dense iron oxide hydroxide by treatment with hydrogen to prepare the iron powder.

Process for the synthesis of iron powder

DOEpatents

Welbon, William W.

1983-01-01

A process for preparing iron powder suitable for use in preparing the iron-potassium perchlorate heat-powder fuel mixture used in thermal batteries, comprises preparing a homogeneous, dense iron oxide hydroxide precipitate by homogeneous precipitation from an aqueous mixture of a ferric salt, formic or sulfuric acid, ammonium hydroxide and urea as precipitating agent; and then reducing the dense iron oxide hydroxide by treatment with hydrogen to prepare the iron powder.

Fabrication of metal matrix composites by powder metallurgy: A review

NASA Astrophysics Data System (ADS)

Manohar, Guttikonda; Dey, Abhijit; Pandey, K. M.; Maity, S. R.

2018-04-01

Now a day's metal matrix components are used in may industries and it finds the applications in many fields so, to make it as better performable materials. So, the need to increase the mechanical properties of the composites is there. As seen from previous studies major problem faced by the MMC's are wetting, interface bonding between reinforcement and matrix material while they are prepared by conventional methods like stir casting, squeeze casting and other techniques which uses liquid molten metals. So many researchers adopt PM to eliminate these defects and to increase the mechanical properties of the composites. Powder metallurgy is one of the better ways to prepare composites and Nano composites. And the major problem faced by the conventional methods are uniform distribution of the reinforcement particles in the matrix alloy, many researchers tried to homogeneously dispersion of reinforcements in matrix but they find it difficult through conventional methods, among all they find ultrasonic dispersion is efficient. This review article is mainly concentrated on importance of powder metallurgy in homogeneous distribution of reinforcement in matrix by ball milling or mechanical milling and how powder metallurgy improves the mechanical properties of the composites.

MoS2 thin films prepared by sulfurization

NASA Astrophysics Data System (ADS)

Sojková, M.; Chromik, Å.; Rosová, A.; Dobročka, E.; Hutár, P.; Machajdík, D.; Kobzev, A. P.; Hulman, M.

2017-08-01

Sulfurization of a Mo layer is one of the most used methods for preparation of thin MoS2 films. In the method, a sulfur powder and Mo covered substrate are placed in different positions within a furnace, and heated separately. This requires a furnace having at least two zones. Here, we present a simplified version of the method where a one-zone tube furnace was used. A molybdenum film on a substrate and a sulfur powder were placed in the center of the furnace and heated at temperatures above 800°C. Mo films transform into MoS2 in vapors of sulphur at high temperatures. As-prepared films were characterized by number of techniques including X-ray diffraction (XRD), atomic force microscopy (AFM), transmission electron microscopy (TEM), Raman, Rutherford backscattering (RBS) and X-ray photoelectron spectroscopy (XPS). It appears that one-zone sulfurization, with just one annealing temperature used, is a suitable method for fabrication of MoS2 thin films. This method is fast, cheap and easy to scale up.

Electrochemical properties of Sn-based nanopowders synthesized by a pulsed wire evaporation method and effect of binder coating

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

Ha, Jong-Keun; Song, Ju-Seok; Cho, Gyu-Bong

Highlights: • Sn-based nanoparticles are fabricated by using the pulsed wire evaporation method. • The electrodes are prepared by mixing the graphene and coating the surface. • Coating the surface of electrode is used with brushing of simple and facile method. • The electrochemical measurements are performed with galvanostatic experiments. • The coating electrode maintains capacity nearly of 501 mAh g{sup −1} up to 100 cycles. - Abstract: Sn-based nanoparticles are prepared with the O{sub 2} concentrations in chamber of Ar atmosphere (by v/v) by using the pulsed wire evaporation (PWE) method. The prepared electrodes are only Sn-based powder electrode,more » its binder coating electrode and Sn-based powder/graphene nanocomposite electrode. Morphology and structure of the synthesized powders and electrodes are investigated with a field emission scanning electron microscope (FE-SEM) and an X-ray diffraction (XRD) analysis. The electrochemical measurements were performed with galvanostatic cycling experiments using a coin type cell of CR2032 (Ø20, T3.2 mm). The binder coating electrode is superior to others and maintains delithiation capacity nearly of 501 mAh g{sup −1} as 58.3% of first delithiation capacity at 0.2 C-rate up to 100 cycles.« less

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.

Boron-copper neutron absorbing material and method of preparation

DOEpatents

Wiencek, Thomas C.; Domagala, Robert F.; Thresh, Henry

1991-01-01

A composite, copper clad neutron absorbing material is comprised of copper powder and boron powder enriched with boron 10. The boron 10 content can reach over 30 percent by volume, permitting a very high level of neutron absorption. The copper clad product is also capable of being reduced to a thickness of 0.05 to 0.06 inches and curved to a radius of 2 to 3 inches, and can resist temperatures of 900.degree. C. A method of preparing the material includes the steps of compacting a boron-copper powder mixture and placing it in a copper cladding, restraining the clad assembly in a steel frame while it is hot rolled at 900.degree. C. with cross rolling, and removing the steel frame and further rolling the clad assembly at 650.degree. C. An additional sheet of copper can be soldered onto the clad assembly so that the finished sheet can be cold formed into curved shapes.

Comparative studies of industrial grade carbon black powders

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

Chawla, Komal, E-mail: komalchawla.rs@gmail.com; Chauhan, Alok P. S., E-mail: chauhan.alok@gmail.com, E-mail: alok.chauhan@alumni.stonybrook.edu

Comparative studies of two dissimilar industrial grade Carbon Black (CB) powders (N375 and N405) were conducted. The structure, surface area and particle size are the three important characteristics of CB powder that determine their processability and application as filler in preparing rubber compounds. The powders were characterized for their structure using dibutyl phthalate absorption (DBPA), particle size via laser particle size analyzer and surface area by nitrogen adsorption method. The structural characterization showed that N405 had lower DBPA in comparison to N375, confirming low structure of N405 grade CB powder. It was observed from the particle size analysis that N375more » was coarser than N405 grade CB. The total surface area values were determined by the BET method based on the cross sectional area of the nitrogen molecule. N375, a coarse grade CB powder with high structure, depicted less surface area as compared to N405.« less

Influence of porcelain firing and cementation on the marginal adaptation of metal-ceramic restorations prepared by different methods.

PubMed

Kaleli, Necati; Saraç, Duygu

2017-05-01

Marginal adaptation plays an important role in the survival of metal-ceramic restorations. Porcelain firings and cementation may affect the adaptation of restorations. Moreover, conventional casting procedures and casting imperfections may cause deteriorations in the marginal adaptation of metal-ceramic restorations. The purpose of this in vitro study was to compare the marginal adaptation after fabrication of the framework, porcelain application, and cementation of metal-ceramic restorations prepared by using the conventional lost-wax technique, milling, direct metal laser sintering (DMLS), and LaserCUSING, a direct process powder-bed system. Alterations in the marginal adaptation of the metal frameworks during the fabrication stages and the precision of fabrication methods were evaluated. Forty-eight metal dies simulating prepared premolar and molar abutment teeth were fabricated to investigate marginal adaptation. They were divided into 4 groups (n=12) according to the fabrication method used (group C serving as the control group: lost-wax method; group M: milling method; group LS: DMLS method; group DP: direct process powder-bed method). Sixty marginal discrepancy measurements were recorded separately on each abutment tooth after fabrication of the framework, porcelain application, and cementation by using a stereomicroscope. Thereafter, each group was divided into 3 subgroups according to the measurements recorded in each fabrication stage: subgroup F (framework), subgroup P (porcelain application), and subgroup C (cementation). Data were statistically analyzed with univariate analysis of variance (followed by 1-way ANOVA and Tamhane T2 test (α=.05). The lowest marginal discrepancy values were observed in restorations prepared by using the direct process powder-bed method, and this was significantly different (P<.001) from the other methods. The highest marginal discrepancy values were recorded after the cementation procedure in all groups. The results showed that the direct process powder-bed method is quite successful in terms of marginal adaptation. The marginal discrepancy increased after porcelain application and cementation. Copyright © 2016 Editorial Council for the Journal of Prosthetic Dentistry. Published by Elsevier Inc. All rights reserved.

Assesment of (Mn,Co)33O4 powders for possible coating material for SOFC/SOEC interconnects

NASA Astrophysics Data System (ADS)

Szymczewska, D.; Molin, S.; Venkatachalam, V.; Chen, M.; Jasinski, P.; Hendriksen, P. V.

2016-01-01

In this work (Mn,Co)3O4 spinel powders with different Mn:Co ratio (1:1 and 1:2) and from different commercial suppliers are evaluated for possible powder for production of interconnect coatings. Sinterability of the powders is evaluated on pressed pellets sintered in oxidizing and in reducing/oxidizing atmospheres. For selected powder, coatings are then prepared by the electrophoretic deposition method on Crofer 22 APU stainless steel coupons. Effects of dispersant/iodine content and deposition voltage and times are evaluated. Thickness as a function of deposition parameters is described. Results show that with appropriate powder it is possible to produce adherent protective coating with a well-controlled thickness.

Non-aqueous solution preparation of doped and undoped lixmnyoz

DOEpatents

Boyle, Timothy J.; Voigt, James A.

1997-01-01

A method for generation of phase-pure doped and undoped Li.sub.x Mn.sub.y O.sub.z precursors. The method of this invention uses organic solutions instead of aqueous solutions or nonsolution ball milling of dry powders to produce phase-pure precursors. These precursors can be used as cathodes for lithium-polymer electrolyte batteries. Dopants may be homogeneously incorporated to alter the characteristics of the powder.

Surface segregation of additives on SnO 2 based powders and their relationship with macroscopic properties

NASA Astrophysics Data System (ADS)

Pereira, Gilberto J.; Castro, Ricardo H. R.; Hidalgo, Pilar; Gouvêa, Douglas

2002-07-01

Surface properties of ceramic powders frequently play an important role in producing high-quality, high-performance, and reliable ceramic products. These properties are related to the surface bond types and interactions with the surroundings. Oxide surfaces generally contain adsorbed hydroxyl groups and modifications in the chemical composition of the surface may be studied by infrared spectroscopy. In this work, we prepared SnO 2 containing Fe or Mg ions by organic chemical route derived from Pechini's method. The prepared powders were characterized by infrared spectroscopy (FT-IR), X-ray diffraction (XRD), dynamic electrophoretic mobility and surface area determination. Results demonstrated that the studied additives segregate onto the oxide surface and modify the hydroxyl IR bands of the adsorbed hydroxyl groups. These surface modifications change some macroscopic properties of the powder such as the isoelectric point (IEP) in aqueous suspensions and the final specific surface area. The increase of the surface area with additive concentration is supposedly due to the reduction of surface energy of the powders when additives segregate on the powder surface.

Characterization of Ni ferrites powders prepared by plasma arc discharge process

NASA Astrophysics Data System (ADS)

Safari, A.; Gheisari, Kh.; Farbod, M.

2017-01-01

The aim of this work was to synthesize a single-phase spinel structure from a mixture of zinc, iron and nickel powders by plasma arc discharge method. A mixture of zinc, iron and nickel powders with the appropriate molar ratio was prepared and formed into a cylindrical shape. The synthesis process was performed in air, oxygen and argon atmospheres with the applied arc current of 400 A and pressure of 1 atm. After establishing an arc between the electrodes, the produced powders were collected and their structure and magnetic properties were examined by XRD and VSM, respectively. ZnO as an impurity was appeared in the as-produced powders owing to the high reactivity of zinc atoms, preventing the formation of Ni-Zn ferrite. A pure spinel structure with the highest saturation magnetization (43.8 emu/g) was observed as zinc powders removed completely from the initial mixture. Morphological evaluations using field emission scanning electron microscopy showed that the mean size of fabricated nanoparticles was in the range 100-200 nm and was dependent on the production conditions.

Process for the synthesis of iron powder

DOEpatents

Welbon, W.W.

1983-11-08

A process for preparing iron powder suitable for use in preparing the iron-potassium perchlorate heat-powder fuel mixture used in thermal batteries, comprises preparing a homogeneous, dense iron oxide hydroxide precipitate by homogeneous precipitation from an aqueous mixture of a ferric salt, formic or sulfuric acid, ammonium hydroxide and urea as precipitating agent; and then reducing the dense iron oxide hydroxide by treatment with hydrogen to prepare the iron powder. 2 figs.

Preparation of extrusions of bulk mixed oxide compounds with high macroporosity and mechanical strength

DOEpatents

Flytzani-Stephanopoulos, Maria; Jothimurugesan, Kandaswami

1990-01-01

A simple and effective method for producing bulk single and mixed oxide absorbents and catalysts is disclosed. The method yields bulk single oxide and mixed oxide absorbent and catalyst materials which combine a high macroporosity with relatively high surface area and good mechanical strength. The materials are prepared in a pellet form using as starting compounds, calcined powders of the desired composition and physical properties these powders are crushed to broad particle size distribution, and, optionally may be combined with an inorganic clay binder. The necessary amount of water is added to form a paste which is extruded, dried and heat treated to yield and desired extrudate strength. The physical properties of the extruded materials (density, macroporosity and surface area) are substantially the same as the constituent powder is the temperature of the heat treatment of the extrudates is approximately the same as the calcination temperature of the powder. If the former is substantially higher than the latter, the surface area decreases, but the macroporosity of the extrusions remains essentially constant.

Nano-sized ZnO powders prepared by co-precipitation method with various pH

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

Purwaningsih, S. Y., E-mail: sriyanisaputri@gmail.com; Pratapa, S.; Triwikantoro,

2016-04-19

In this work, nano-sized ZnO powders have been synthesized by the co-precipitation method with Zn(CH3COOH)2.2H2O, HCl, and NH3.H2O as raw materials in various pH ranging from 8 to 10. The purity, microstructure, chemical group analysis, morphology of the prepared ZnO powders were studied by X-ray diffraction (XRD), Fourier transform infrared spectrometer (FTIR), energy dispersive X-ray spectrometry (EDX), and scanning electron microscope (SEM), respectively. Rietveld refinement of XRD data showed that ZnO crystallizes in the wurtzite structure with high purity. The obtained powders were nano-sized particles with the average crystallite size about 17.9 ± 2.1 nm synthesized with pH of 9.5, atmore » 85°C, and stirring time of 6 h. The SEM results have visualied the morphology of ZnO nanoparticles with spherical-like shape. The effect of processing conditions on morphology of ZnO was also discussed.« less

Preparation and optical characteristics of layered perovskite-type lead-bromide-incorporated azobenzene chromophores

NASA Astrophysics Data System (ADS)

Sasai, Ryo; Shinomura, Hisashi

2013-02-01

Lead bromide-based layered perovskite powders with azobenzene derivatives were prepared by a homogeneous precipitation method. From the diffuse reflectance (DR) and photoluminescence (PL) spectra of the hybrid powder materials, the present hybrids exhibited sharp absorption and PL peaks originating from excitons produced in the PbBr42- layer. When the present hybrid powder was irradiated with UV light at 350 nm, the absorption band from the trans-azobenzene chromophore, observed around 350 nm, decreased, while the absorption band from the cis-azobenzene chromophore, observed around 450 nm, increased. These results indicate that azobenzene chromophores in the present hybrid materials exhibit reversible photoisomerization. Moreover, it was found that the PL intensity from the exciton also varied due to photoisomerization of the azobenzene chromophores in the present hybrid. Thus, for the first time we succeeded in preparing the azobenzene derivative lead-bromide-based layered perovskite with photochromism before and after UV light irradiation.

Fuel additives and heat treatment effects on nanocrystalline zinc ferrite phase composition

NASA Astrophysics Data System (ADS)

Hu, Ping; Pan, De-an; Wang, Xin-feng; Tian, Jian-jun; Wang, Jian; Zhang, Shen-gen; Volinsky, Alex A.

2011-03-01

Nanocrystalline ZnFe 2O 4 powder was prepared by the auto-combustion method using citric acid, acetic acid, carbamide and acrylic acid as fuel additives. Pure spinel zinc ferrite with the crystallite size of about 15 nm can be obtained by using acrylic acid as fuel additive. Samples prepared using other fuel additives contain ZnO impurities. In order to eliminate ZnO impurities, the sample prepared with citric acid as fuel additive was annealed at different temperatures up to 1000 °C in air and in argon. Annealed powders have pure ZnFe 2O 4 phase when annealing temperature is higher than 650 °C in air. Sample annealed at 650 °C in air is paramagnetic. However, annealed powders become a mixture of Fe 3O 4 and FeO after annealing at 1000 °C in argon atmosphere due to Zn volatility and the reduction reaction.

Biocompatibility assessment of SiO2-TiO2 composite powder on MG63 osteoblast cell lines for orthopaedic applications.

PubMed

Chellappa, Maniickam; Thejaswini, Bezawada; Vijayalakshmi, Uthirapathy

2017-02-01

The objective of this study is to evaluate the biocompatibility of composite powder consisting of silica and titania (SiO 2 -TiO 2 ) for biomedical applications. The advancement of nanoscience and nanotechnology encourages researchers to actively participate in reinvention of existing materials with improved physical, chemical and biological properties. Hence, a composite/hybrid material has given birth of new materials with intriguing properties. In the present investigation, SiO 2 -TiO 2 composite powder was synthesised by sol-gel method and the prepared nanocomposite was characterised for its phase purity, functional groups, surface topography by powder X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR) and scanning electron microscopy. Furthermore, to understand the adverse effects of composite, biocompatibility test was analysed by cell culture method using MG63 osteoblast cell lines as a basic screening method. From the results, it was observed that typical Si-O-Ti peaks in FT-IR confirms the formation of composite and the crystallinity of the composite powder was analysed by XRD analysis. Further in vitro biocompatibility and acridine orange results have indicated better biocompatibility at different concentrations on osteoblast cell lines. On the basis of these observations, we envision that the prepared silica-titania nanocomposite is an intriguing biomaterial for better biomedical applications.

Comparative physicochemical properties of hydrocortisone-PVP composites prepared using supercritical carbon dioxide by the GAS anti-solvent recrystallization process, by coprecipitation and by spray drying.

PubMed

Corrigan, Owen I; Crean, Abina M

2002-10-01

Hydrocortisone-PVP composites were successfully prepared using the supercritical fluid gas anti-solvent method (GAS). Analysis by differential scanning calorimetry DSC and powder X-ray diffraction (XRD) indicated that these systems were more crystalline than corresponding systems prepared by spray drying. These systems, prepared by the GAS method were more similar in physicochemical properties to coprecipitates prepared by conventional solvent evaporation. Compressed composites of hydrocortisone-PVP systems, prepared by the GAS method, had dissolution rates lower than those of corresponding systems prepared by the other processing methods but equivalent to those of corresponding physical mixtures.

Effect of annealing on the structural and optical properties of TiO{sub 2} powder prepared by sol-gel route

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

Halder, Nilanjan; Misra, Kamakhya Prakash

2016-05-06

Using titanium isopropoxide as the precursor, Titanium dioxide (TiO{sub 2}) powder was synthesized via sol-gel method, a promising low temperature route for preparing nanosized metal oxide semiconductors with good homogeneity at low cost. The as-prepared nano powder was thermally treated in air at 550, 650, 750, 900 and 1100°C for 1hr after drying at room temperature and used for further characterization. X-ray diffraction measurements showed that the annealing treatment has a strong impact on the crystal phase of TiO{sub 2} samples. The crystallite size as calculated from Debye Scherer formula lies in the range 29-69 nm and is found to increasemore » with increase in annealing temperature. Photoluminescence studies exhibit an improvement in the optical efficiency of the samples with post synthesis heat treatment. Annealing at temperature above 900°C results in a degradation of the structural and optical quality of the TiO{sub 2} nano powder samples.« less

Preparation of La 0.75Sr 0.25Cr 0.5Mn 0.5O 3- δ fine powders by carbonate coprecipitation for solid oxide fuel cells

NASA Astrophysics Data System (ADS)

Ha, Sang Bu; Cho, Pyeong-Seok; Cho, Yoon Ho; Lee, Dokyol; Lee, Jong-Heun

A range of La 0.75Sr 0.25Cr 0.5Mn 0.5O 3- δ (LSCM) powders is prepared by the carbonate coprecipitation method for use as anodes in solid oxide fuel cells. The supersaturation ratio (R = [(NH 4) 2CO 3]/([La 3+] + [Sr 2+] + [Cr 3+] + [Mn 2+])) during the coprecipitation determines the relative compositions of La, Sr, Cr, and Mn. The composition of the precursor approaches the stoichiometric one at the supersaturation range of 4 ≤ R ≤ 12.5, whereas Sr and Mn components are deficient at R < 4 and excessive at R = 25. The fine and phase-pure LSCM powders are prepared by heat treatment at very low temperature (1000 °C) at R = 7.5 and 12.5. By contrast, the solid-state reaction requires a higher heat-treatment temperature (1400 °C). The catalytic activity of the LSCM electrodes is enhanced by using carbonate-derived powders to manipulate the electrode microstructures.

Preparation and optical properties of iron-modified titanium dioxide obtained by sol-gel method

NASA Astrophysics Data System (ADS)

Hreniak, Agnieszka; Gryzło, Katarzyna; Boharewicz, Bartosz; Sikora, Andrzej; Chmielowiec, Jacek; Iwan, Agnieszka

2015-08-01

In this paper twelve TiO2:Fe powders prepared by sol-gel method were analyzed being into consideration the kind of iron compound applied. As a precursor titanium (IV) isopropoxide (TIPO) was used, while as source of iron Fe(NO3)3 or FeCl3 were tested. Fe doped TiO2 was obtained using two methods of synthesis, where different amount of iron was added (1, 5 or 10% w/w). The size of obtained TiO2:Fe particles depends on the iron compound applied and was found in the range 80-300 nm as it was confirmed by SEM technique. TiO2:Fe particles were additionally investigated by dynamic light scattering (DLS) method. Additionally, for the TiO2:Fe particles UV-vis absorption and the zeta potential were analyzed. Selected powders were additionally investigated by magnetic force microscopy (MFM) and X-ray diffraction techniques. Photocatalytic ability of Fe doped TiO2 powders was evaluated by means of cholesteryl hemisuccinate (CHOL) degradation experiment conducted under the 30 min irradiation of simulated solar light.

Nanograin Ceramic Optical Composite Window

DTIC Science & Technology

2005-07-15

parts are sintered in air at 1100 C̊. Table 1: Carbon content of the calcined Alumina- Zirconia powders analyzed by LECO Calcination Temperature Carbon...estimated particle size of the Alumina and Zirconia powders Material name Surface area (m2/g) Estimated particle size (nm) Alumina 315.7 4.7 Zirconia...200 300 400 500 600 700 800 900 1000 2-Theta - Scale 20 30 40 50 60 70 80 Figure 3: XRD patterns of zirconia powder prepared by sonochemical method

Methods for preparation of three-dimensional bodies

DOEpatents

Mulligan, Anthony C.; Rigali, Mark J.; Sutaria, Manish P.; Artz, Gregory J.; Gafner, Felix H.; Vaidyanathan, K. Ranji

2004-09-28

Processes for mechanically fabricating two and three-dimensional fibrous monolith composites include preparing a fibrous monolith filament from a core composition of a first powder material and a boundary material of a second powder material. The filament includes a first portion of the core composition surrounded by a second portion of the boundary composition. One or more filaments are extruded through a mechanically-controlled deposition nozzle onto a working surface to create a fibrous monolith composite object. The objects may be formed directly from computer models and have complex geometries.

Methods for preparation of three-dimensional bodies

DOEpatents

Mulligan, Anthony C [Tucson, AZ; Rigali, Mark J [Carlsbad, NM; Sutaria, Manish P [Malden, MA; Artz, Gregory J [Tucson, AZ; Gafner, Felix H [Tucson, AZ; Vaidyanathan, K Ranji [Tucson, AZ

2008-06-17

Processes for mechanically fabricating two and three-dimensional fibrous monolith composites include preparing a fibrous monolith filament from a core composition of a first powder material and a boundary material of a second powder material. The filament includes a first portion of the core composition surrounded by a second portion of the boundary composition. One or more filaments are extruded through a mechanically-controlled deposition nozzle onto a working surface to create a fibrous monolith composite object. The objects may be formed directly from computer models and have complex geometries.

Effect of preparation conditions on the nanostructure of hydroxyapatite and brushite phases

NASA Astrophysics Data System (ADS)

Mansour, S. F.; El-dek, S. I.; Ahmed, M. A.; Abd-Elwahab, S. M.; Ahmed, M. K.

2016-10-01

Hydroxyapatite (HAP) and dicalcium phosphate dihydrate (brushite) nanoparticles were prepared by co-precipitation method. The obtained products were characterized by X-ray powder diffraction (XRD), Fourier transformation infra-red spectroscopy (FTIR) and thermo-gravimetric analysis (TGA). Scanning electron microscopy (SEM) and transmission electron microscope (TEM) were used to investigate the morphology of the powdered samples as well as their microstructure, respectively. Brushite samples were obtained in a spherical shape, while hydroxyapatite was formed in a needle and rice shape depending on the pH value.

Chemical plating method of preparing radiation source material

DOEpatents

Smith, P.K.; Huntoon, R.T.; Mosley, W.C. Jr.

1973-12-11

A uniform dispersion of a radioisotope within a noble metal matrix is provided by chemically plating a noble metal coating onto particles including a dissociable compound of the mdioisotope. A suspension of the dissociable compound in a chemically reductive solution is prepared and noble metal cations added to produce the noble metal coatings. The coated particles are filtered, dried and heated to calcine the dissociable compound to a refractory powder. The powder can be encapsulated in measured portions or consolidated and shaped into an elongated form for easy apportionnnent as radiation source material. (Official Gazette)

Preparation of redispersible liposomal dry powder using an ultrasonic spray freeze-drying technique for transdermal delivery of human epithelial growth factor

PubMed Central

Yin, Fei; Guo, Shiyan; Gan, Yong; Zhang, Xinxin

2014-01-01

In this work, an ultrasonic spray freeze-drying (USFD) technique was used to prepare a stable liposomal dry powder for transdermal delivery of recombinant human epithelial growth factor (rhEGF). Morphology, particle size, entrapment efficiency, in vitro release, and skin permeability were systematically compared between rhEGF liposomal dry powder prepared using USFD and that prepared using a conventional lyophilization process. Porous and spherical particles with high specific area were produced under USFD conditions. USFD effectively avoided formation of ice crystals, disruption of the bilayer structure, and drug leakage during the liposome drying process, and maintained the stability of the rhEGF liposomal formulation during storage. The reconstituted rhEGF liposomes prepared from USFD powder did not show significant changes in morphology, particle size, entrapment efficiency, or in vitro release characteristics compared with those of rhEGF liposomes before drying. Moreover, the rhEGF liposomal powder prepared with USFD exhibited excellent enhanced penetration in ex vivo mouse skin compared with that for powder prepared via conventional lyophilization. The results suggest that ultrasonic USFD is a promising technique for the production of stable protein-loaded liposomal dry powder for application to the skin. PMID:24729702

Preparation of redispersible liposomal dry powder using an ultrasonic spray freeze-drying technique for transdermal delivery of human epithelial growth factor.

PubMed

Yin, Fei; Guo, Shiyan; Gan, Yong; Zhang, Xinxin

2014-01-01

In this work, an ultrasonic spray freeze-drying (USFD) technique was used to prepare a stable liposomal dry powder for transdermal delivery of recombinant human epithelial growth factor (rhEGF). Morphology, particle size, entrapment efficiency, in vitro release, and skin permeability were systematically compared between rhEGF liposomal dry powder prepared using USFD and that prepared using a conventional lyophilization process. Porous and spherical particles with high specific area were produced under USFD conditions. USFD effectively avoided formation of ice crystals, disruption of the bilayer structure, and drug leakage during the liposome drying process, and maintained the stability of the rhEGF liposomal formulation during storage. The reconstituted rhEGF liposomes prepared from USFD powder did not show significant changes in morphology, particle size, entrapment efficiency, or in vitro release characteristics compared with those of rhEGF liposomes before drying. Moreover, the rhEGF liposomal powder prepared with USFD exhibited excellent enhanced penetration in ex vivo mouse skin compared with that for powder prepared via conventional lyophilization. The results suggest that ultrasonic USFD is a promising technique for the production of stable protein-loaded liposomal dry powder for application to the skin.

Nifedipine capsules may provide a viable alternative to oral powders for paediatric patients.

PubMed

Helin-Tanninen, M; Naaranlahti, T; Kontra, K; Savolainen, K

2007-02-01

To compare content uniformities between different sizes of extemporaneously compounded nifedipine oral powders and capsules, in order to find out if capsules could be used instead of oral powders as paediatric medications. Actual content and content uniformity of extemporaneously compounded 1-mg nifedipine oral powders and capsules were evaluated by a high performance liquid chromatographic assay. Capsules and powders were prepared by triturating 10-mg nifedipine tablets with different amounts of lactose or microcrystalline cellulose with a mortar and pestle using a standard geometric dilution technique. Oral powders were weighed individually and capsules were filled by a hand-operated capsule-filling machine. Four different sizes of powders (500, 300, 100 and 50 mg) and three different sizes of capsules (numbers 1, 3 and 4) were prepared. Ten oral powders and 10 capsules from each batch were randomly selected and individually assayed for nifedipine amount. The extemporaneously prepared nifedipine oral powders and capsules were within acceptable limits for content uniformity, as defined by the European Pharmacopoeia, but the results indicate that the loss of nifedipine during the preparation process may be considerable for both preparations. The concentration on nifedipine decreased while the total mass of the oral powder decreased. These results demonstrate that nifedipine oral powders can be replaced by capsules, whose contents are emptied for use, in paediatric medications. Compounding small capsules, such as size number 3 or 4, is acceptable when considering the average drug content. The total weight of the oral powder should be at least 300 mg. The preparation of nifedipine in all studied capsule sizes was safe with either lactose monohydrate or microcrystalline cellulose as excipients. Thus, emptied capsules seem to be a good choice for delivering a paediatric medication. The loss of nifedipine was considerable in oral powders with low total weight.

Color-tunable up-conversion emission in Y2O3:Yb3+, Er3+ nanoparticles prepared by polymer complex solution method

PubMed Central

2013-01-01

Abstract Powders of Y2O3 co-doped with Yb3+ and Er3+ composed of well-crystallized nanoparticles (30 to 50 nm in diameter) with no adsorbed ligand species on their surface are prepared by polymer complex solution method. These powders exhibit up-conversion emission upon 978-nm excitation with a color that can be tuned from green to red by changing the Yb3+/Er3+ concentration ratio. The mechanism underlying up-conversion color changes is presented along with material structural and optical properties. PACS 42.70.-a, 78.55.Hx, 78.60.-b PMID:23522083

Sol-gel preparation of lead magnesium niobate (PMN) powders and thin films

DOEpatents

Boyle, T.J.

1999-01-12

A method of preparing a lead magnesium niobium oxide (PMN), Pb(Mg{sub 1/3}Nb{sub 2/3})O{sub 3}, precursor solution by a solvent method wherein a liquid solution of a lead-complex PMN precursor is combined with a liquid solution of a niobium-complex PMN precursor, the combined lead- and niobium-complex liquid solutions are reacted with a magnesium-alkyl solution, forming a PMN precursor solution and a lead-based precipitate, and the precipitate is separated from the reacted liquid PMN precursor solution to form a precipitate-free PMN precursor solution. This precursor solution can be processed to form both ferroelectric powders and thin films. 3 figs.

Method development and validation for measuring the particle size distribution of pentaerythritol tetranitrate (PETN) powders.

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

Young, Sharissa Gay

2005-09-01

Currently, the critical particle properties of pentaerythritol tetranitrate (PETN) that influence deflagration-to-detonation time in exploding bridge wire detonators (EBW) are not known in sufficient detail to allow development of a predictive failure model. The specific surface area (SSA) of many PETN powders has been measured using both permeametry and gas absorption methods and has been found to have a critical effect on EBW detonator performance. The permeametry measure of SSA is a function of particle shape, packed bed pore geometry, and particle size distribution (PSD). Yet there is a general lack of agreement in PSD measurements between laboratories, raising concernsmore » regarding collaboration and complicating efforts to understand changes in EBW performance related to powder properties. Benchmarking of data between laboratories that routinely perform detailed PSD characterization of powder samples and the determination of the most appropriate method to measure each PETN powder are necessary to discern correlations between performance and powder properties and to collaborate with partnering laboratories. To this end, a comparison was made of the PSD measured by three laboratories using their own standard procedures for light scattering instruments. Three PETN powder samples with different surface areas and particle morphologies were characterized. Differences in bulk PSD data generated by each laboratory were found to result from variations in sonication of the samples during preparation. The effect of this sonication was found to depend on particle morphology of the PETN samples, being deleterious to some PETN samples and advantageous for others in moderation. Discrepancies in the submicron-sized particle characterization data were related to an instrument-specific artifact particular to one laboratory. The type of carrier fluid used by each laboratory to suspend the PETN particles for the light scattering measurement had no consistent effect on the resulting PSD data. Finally, the SSA of the three powders was measured using both permeametry and gas absorption methods, enabling the PSD to be linked to the SSA for these PETN powders. Consistent characterization of other PETN powders can be performed using the appropriate sample-specific preparation method, so that future studies can accurately identify the effect of changes in the PSD on the SSA and ultimately model EBW performance.« less

Superconductor precursor mixtures made by precipitation method

DOEpatents

Bunker, Bruce C.; Lamppa, Diana L.; Voigt, James A.

1989-01-01

Method and apparatus for preparing highly pure homogeneous precursor powder mixtures for metal oxide superconductive ceramics. The mixes are prepared by instantaneous precipitation from stoichiometric solutions of metal salts such as nitrates at controlled pH's within the 9 to 12 range, by addition of solutions of non-complexing pyrolyzable cations, such as alkyammonium and carbonate ions.

One-Step Hydrothermal-Electrochemical Route to Carbon-Stabilized Anatase Powders

NASA Astrophysics Data System (ADS)

Tao, Ying; Yi, Danqing; Zhu, Baojun

2013-04-01

Black carbon-stabilized anatase particles were prepared by a simple one-step hydrothermal-electrochemical method using glucose and titanium citrate as the carbon and titanium source, respectively. Morphological, chemical, structural, and electrochemical characterizations of these powders were carried out by Raman spectroscopy, Fourier-transform infrared spectroscopy, x-ray diffraction, scanning electron microscopy, and cyclic voltammetry. It was revealed that 200-nm carbon/anatase TiO2 was homogeneously dispersed, and the powders exhibited excellent cyclic performance at high current rates of 0.05 V/s. The powders are interesting potential materials that could be used as anodes for lithium-ion batteries.

Pastes: what do they contain? How do they work?

PubMed

Juch, R D; Rufli, T; Surber, C

1994-01-01

Pastes are semisolid stiff preparations containing a high proportion of finely powdered material. Powders such as zinc oxide, titanium dioxide, starch, kaolin or talc are incorporated in high concentrations into a preferably lipophilic, greasy vehicle. A clinically distinctive feature which is generally attributed to pastes is the quality to absorb exudates by nature of the powder or other absorptive components. Reviewing the various pharmacopoeias serious doubts arise from the various formulas of pastes and their absorptive features. The zinc oxide pastes of the USP XXII, the DAB 10 and BP 88 (US, German and British pharmacopoeias). are composed of petrolatum, zinc oxide and starch. Petrolatum, a highly lipophilic, water-immiscible vehicle surrounds the powder particles preventing any absorption of water or exudates. The goal of our investigation was to test a simple experimental setting to characterize the clinically important absorptive feature of powders and pastes. The absorptive features of the powders were determined by the method of Enslin. The absorptive features of the paste preparations were calculated from the weight difference between the paste preparation before and after incubation with water using a simple standardized procedure. The absorptive features of titanium dioxide, zinc oxide, kaolin, corn starch and methylcellulose powder in pharmacopoeia quality were determined. Zinc oxide and kaolin powder showed the highest absorption of 1,000 mg water/g powder (100%). The water absorption of corn starch and titanium dioxide was 700 and 450 mg/g powder, respectively. The absorptive features of a series of paste preparations were studied in a simple experimental setting. The data show that two-phase pastes consisting of two immiscible components, one (the dispersed or inner phase; powder) being suspended in the other (the continuous or outer phase; lipophilic vehicle), have no absorptive features. In contrast, three-phase pastes consisting of a hydrophilic two-phase emulsion with high concentrations of incorporated powder (cream pastes) show considerable water uptake. We conclude that the classical two-phase pastes such as the zinc oxide pastes have no absorptive features. On the contrary, these formulations are highly occlusive. Therefore lipophilic pastes are only indicated when protection of intact skin against aggressive body exudates and humidity is required. The hydrophilic three-phase pastes or cream pastes show considerable water uptake and fulfil common expectations of pastes to dry the skin.

Development of Ceramic Systems for High temperature Coatings

NASA Technical Reports Server (NTRS)

Eslamloo-Grami, Maryame

2003-01-01

Professor Eslamloo-Grami will synthesize ceramic powders of various compositions based on pyrochlore, perovskite, and magnetoplumbite structures by doping with various oxides. Sol-gel and combustion synthesis routes will be used for powder syntheses. The powders will be characterized for particle size, surface area, microstructure, sintering etc. Thermal conductivity of the hot pressed specimens will also be measured at various temperatures. At the end, a project report will be prepared describing in details the experimental methods, results, discussion, and future research.

Preparation of titanium phosphates with additives in hydrothermal process and their powder properties for cosmetics.

PubMed

Onoda, Hiroaki; Yamaguchi, Taisuke

2013-04-01

In this study, titanium phosphates were prepared from titanium chloride and phosphoric acid, sodium pyrophosphate and sodium triphosphate solutions with water retention compounds in hydrothermal process as a novel white pigment for cosmetics. Their chemical composition, powder properties, photo catalytic activity, water retention and smoothness were studied. The addition of glycerin in the preparation from sodium pyrophosphate has the useful method to obtain homogenized spherical particles of titanium phosphate pigments for the cosmetics. These titanium phosphates had less photo catalytic activity to protect the sebum on the skin. © 2012 Society of Cosmetic Scientists and the Société Française de Cosmétologie.

Magnetic properties of co-precipitated hexaferrite powders with Sm-Co substitutions optimized with the molten flux method

NASA Astrophysics Data System (ADS)

Serletis, C.; Litsardakis, G.; Pavlidou, E.; Efthimiadis, K. G.

2017-11-01

In this work, using the chemical coprecipitation method, Sr1-xSmxFe12-xCoxO19 (x = 0, 0.1, 0.2) hexaferrite powders were prepared. Major magnetization loops were recorded at room temperature in order to determine the correct calcination temperature for optimum hard magnetic properties. It is found that a small degree of substitution increases substantially the coercive field. Also, the use of the molten flux calcination method increases the remanent magnetization. SEM/EDXS and XRD measurements were performed at the calcined powders: the results show that a single hexaferrite phase is formed and that the substituted powders consist of an assembly of grains with a mean diameter of 40 nm. Measurements of minor magnetization loops and of the temperature and time dependence of the magnetization confirm that the powders consist of a non-oriented single domain magnetic particles assembly. The results indicate that Sm could be a viable replacement for La in the manufacturing of hexaferrites with a high-energy product.

[Preparation of coated tablets of glycyrrhetic acid-HP-beta-cyclodextrin tablets for colon-specific release].

PubMed

Cui, Qi-Hua; Cui, Jing-Hao; Zhang, Jin-Jin

2008-10-01

To prepare coated tablets of glycyrrhetinic acid and hydroxypropyl-beta-cyclodextrin (GTA-HP-beta-CYD) inclusion complex tablets for colon-specific release. In order to improve the solubility of GTA, the GTA-HP-beta-CYD inclusion complex was prepared by ultrasonic-lyophilization technique and its formation were characterized by X-ray powder diffraction profiles and infrared spectrometry. The effects of inclusion condition on the inclusion efficiency and stability coefficient of inclusion complex were investigated, respectively. After prepared GTA-HP-beta-CYD tablets by powder direct compression, the pH dependant polymer Eudragit III and/or mixed with Eudragit II were used for further coating materials in fluid-bed coater. The influences of coating weight on the GTA release in different pH conditions were evaluated to establish the method for prepering colon specific delivery tablets with pulsed release properties. The formation of inclusion complexes were proved by X-ray powder diffraction profile and phase solubility curve. The effect of pH value of solvent was played critical role on the preparation of GTA- HP-beta-CYD inclusion complex. And the inclusion efficiency of GTA was 9. 3% and the solubility was increased to 54. 6 times at optimized method. The Eudragit III coated GTA- HP-beta-CYD tablets with coating weight 10% and 16% were showed pH dependant colon specific release profiles with slow release rate. The release profile of tablets coated with the mixture of Eudragit II and Eudragit III (1:2) were indicated typical pH dependant colon specific and pulsed release properties while the coating weight was 17%. The preliminary method for preparation of colon specific release tablets containing glycyrrhetinic acid with improved solubility was established for further in vivo therapeutic experiment.

Preparation and characterisation of hydrocortisone particles using a supercritical fluids extraction process.

PubMed

Velaga, Sitaram P; Ghaderi, Raouf; Carlfors, Johan

2002-01-14

Crystallisation and subsequent milling of pharmaceutical powders by traditional methods often cause variations in physicochemical properties thereby influencing bioavailability of the formulation. Crystallisation of drug substances using supercritical fluids (SFs) offers some advantages over existing traditional methods in controlling particle characteristics. The novel particle formation method, solution enhanced dispersion by supercritical (SEDS) fluids was used for the preparation of hydrocortisone (HC) particles. The influence of processing conditions on the solid-state properties of the particles was studied. HC, an anti-inflammatory corticosteroid, particles were prepared from acetone and methanol solutions using the SEDS process. The solutions were dispersed with supercritical CO(2), acting as an anti-solvent, through a specially designed co-axial nozzle into a pressured vessel maintained at a specific constant temperature and pressure. The temperatures and pressures studied were 40-90 degrees C and 90-180 bar, respectively. The relative flow rates of drug solution to CO(2) were varied between 0.002 and 0.03. Solid-state characterisation of particles included differential scanning calorimetry (DSC), X-ray powder diffraction (XRPD), solubility studies and scanning electron microscopy (SEM) examination. The aerodynamic properties of SEDS prepared particles were determined by a multistage liquid impinger (MLI). Particles produced from acetone solutions were crystalline needles, melting at 221+/-2 degrees C. Their morphology was independent of processing conditions. With methanol solutions, particles were flakes or needles depending on the processing temperature and pressure. This material melted at 216+/-1 degrees C, indicating a different crystal structure from the original material, in agreement with observed differences in the position and intensity of the XRPD peaks. The simulated lung deposition, using the MLI, for HC powder was improved after SEDS processing. It was possible to produce and control the crystallinity, morphology, and aerodynamic properties of HC particles with the SEDS technique. This method may be useful for the processing of inhalation powders.

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

Taketomo, C.K.; Chu, S.A.; Cheng, M.H.

The stability of captopril in powder papers under three different storage conditions was determined. Captopril 12.5-mg tablets were triturated with lactose to a final concentration of 2 mg of captopril in 100 mg of powder. A total of 240 powder papers were prepared and stored in class A prescription vials (80 papers), 002G plastic zip-lock bags (80 papers), and Moisture Proof Barrier Bags (80 papers). Immediately after preparation and at 1, 2, 3, 4, 8, 12, and 24 weeks of storage at room temperature, powder papers under each storage condition were reweighed and the contents were assayed for captopril concentrationmore » by a stability-indicating high-performance liquid chromatographic method. More than 90% of the initial captopril concentration was retained under all storage conditions during the first 12 weeks of the study. Captopril disulfide, a degradation product, was detected in one sample stored in a plastic zip-lock bag at 24 weeks. Captopril was stable for the entire 24-week period in powder papers stored in either the class A prescription vial or the Moisture Proof Barrier Bag. Captopril in powder papers is stable for at least 12 weeks when stored at room temperature under all three storage conditions.« less

Influence of thermal treatment on the formation of zirconia nanostructured powder by thermal decomposition of different precursors

NASA Astrophysics Data System (ADS)

Stoia, Marcela; Barvinschi, Paul; Barbu-Tudoran, Lucian; Negrea, Adina; Barvinschi, Floricica

2013-10-01

The paper presents some results concerning the preparation of zirconia powders starting from ZrOCl2·8H2O by using two synthesis methods: (a) precipitation with NH3, at 90 °C, and (b) thermal decomposition of carboxylate precursors, obtained in the reaction of zirconium nitrate and two different alcohols, 1,3-propanediol (PD) and poly(vinyl alcohol) (PVA), at 150 °C. The precursors obtained at different temperatures have been characterized by thermal analysis (TG, DTA) and FT-IR spectroscopy. DTA analysis evidenced very clearly the transition temperatures between zirconia crystalline phases. The precursors have been annealed at different temperatures in order to obtain zirconia powders and the as obtained powders have been characterized by means of X-Ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR), and Scanning Electron Microscopy (SEM). In case of precipitation method the presence of the tetragonal phase was observed at 400 °C, while the monoclinic phase appears at temperatures higher than 400 °C, becoming major crystalline phase starting with 700 °C. In case of the powders prepared by thermal decomposition of carboxylate precursors, the tetragonal phase was formed at temperatures below 700 °C, when the monoclinic phase begin to crystallize as secondary phase, in a higher proportion for the samples synthesized with 1,3-propanediol. All powders annealed at 1200 °C are pure monoclinic zirconia. SEM images have evidenced for the zirconia powders annealed at 1000 °C particles with diameters up to 150 nm, agglomerated in micrometer-sized aggregates, more individualized and homogenous than that obtained in the case of zirconia powder synthesized with poly(vinyl alcohol).

Research on microstructure properties of the TiC/Ni-Fe-Al coating prepared by laser cladding technology

NASA Astrophysics Data System (ADS)

Jiao, Junke; Xu, Zifa; Zan, Shaoping; Zhang, Wenwu; Sheng, Liyuan

2017-10-01

In this paper, the laser cladding method was used to preparation the TiC reinforced Ni-Fe-Al coating on the Ni base superalloy. The Ti/Ni-Fe-Al powder was preset on the Ni base superalloy and the powder layer thickness is 0.5mm. A fiber laser was used the melting Ti/Ni-Fe-Al powder in an inert gas environment. The shape of the cladding layer was tested using laser scanning confocal microscope (LSCM) under different cladding parameters such as the laser power, the melting velocity and the defocused amount. The microstructure, the micro-hardness was tested by LSCM, SEM, Vickers hardness tester. The test result showed that the TiC particles was distributed uniformly in the cladding layer and hardness of the cladding layer was improved from 180HV to 320HV compared with the Ni-Fe-Al cladding layer without TiC powder reinforced, and a metallurgical bonding was produced between the cladding layer and the base metal. The TiC powder could make the Ni-Fe-Al cladding layer grain refining, and the more TiC powder added in the Ni-Fe-Al powder, the smaller grain size was in the cladding layer.

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.

Preparation and characterization of nanosilica from oil shale ash.

PubMed

Li, Jinhong; Qian, Tingting; Tong, Lingxin; Shen, Jie

2014-05-01

Nano-sized silica powders was prepared using oil shale ash (OSA) as starting materials. A combined process was proposed for the utilization of OSA in the production of the nanosilica, including three stages: calcination, alkaline leaching and carbon dioxide separation. Effects of the calcining temperature, sodium hydroxide concentration and holding time on the desilication ratio were investigated. The microstructure and morphologies of the nano-sized silica were characterized by X-ray diffraction, transmission electron microscopy, and Brunauer-Emmett-Teller nitrogen-gas adsorption method. The results indicated that the obtained powders with particle size of about 40 nm are homegeneously dispersed and its specific surface area is 387 m2/g. The properties of the nano-sized silica powder meet the requirements of the Chinese Chemical Industry Standard HG/T 3061-1999.

Piroxicam cocrystals with phenolic coformers: preparation, characterization, and dissolution properties.

PubMed

Emami, Shahram; Adibkia, Khosro; Barzegar-Jalali, Mohammad; Siahi-Shadbad, Mohammadreza

2018-04-04

This study explores the preparation and investigation of dissolution properties of piroxicam cocrystals. Differential scanning calorimetry (DSC) was used to determine the capability of resorcinol (RES), methylparaben (MPB), and vanillin (VAN) to form cocrystals with piroxicam (PRX). Generation of cocrystals was attempted by liquid assisted grinding and slurry methods. Cocrystals were characterized by thermal methods, powder X-ray diffraction, and Fourier-transform infrared spectroscopy. Apparent solubility, intrinsic dissolution rate (IDR), and powder dissolution profile of cocrystals were compared with anhydrous piroxicam, piroxicam monohydrate (PRXMH), and previously reported piroxicam-succinic acid cocrystal. Contact angles and particle sizes of the studied solids were also measured. Based on the DSC screening results, we prepared and characterized PRX-RES and PRX-MPB cocrystals. Interestingly, the cocrystals not only failed to improve apparent solubility and IDR of PRX but also showed lower values than PRX that were attributed to induction of phase transformation of PRX to PRXMH. In contrary, cocrystals performed better than PRX in powder dissolution studies. The higher dissolution rates of cocrystals were explained by improved wettability and reduced sizes. This study has highlighted the complexity of solid state properties of cocrystals and has provided new evidence for the in-solution stability issues of cocrystals.

Molten salt synthesis of nanocrystalline phase of high dielectric constant material CaCu3Ti4O12.

PubMed

Prakash, B Shri; Varma, K B R

2008-11-01

Nanocrystalline powders of giant dielectric constant material, CaCu3Ti4O12 (CCTO), have been prepared successfully by the molten salt synthesis (MSS) using KCl at 750 degrees C/10 h, which is significantly lower than the calcination temperature (approximately 1000 degrees C) that is employed to obtain phase pure CCTO in the conventional solid-state reaction route. The water washed molten salt synthesized powder, characterized by X-ray powder diffraction (XRD), Scanning electron microscopy (SEM), and Transmission electron microscopy (TEM) confirmed to be a phase pure CCTO associated with approximately 150 nm sized crystallites of nearly spherical shape. The decrease in the formation temperature/duration of CCTO in MSS method was attributed to an increase in the diffusion rate or a decrease in the diffusion length of reacting ions in the molten salt medium. As a consequence of liquid phase sintering, pellets of as-synthesized KCl containing CCTO powder exhibited higher sinterability and grain size than that of KCl free CCTO samples prepared by both MSS method and conventional solid-state reaction route. The grain size and the dielectric constant of KCl containing CCTO ceramics increased with increasing sintering temperature (900 degrees C-1050 degrees C). Indeed the dielectric constants of these ceramics were higher than that of KCl free CCTO samples prepared by both MSS method and those obtained via the solid-state reaction route and sintered at the same temperature. Internal barrier layer capacitance (IBLC) model was invoked to correlate the observed dielectric constant with the grain size in these samples.

Method for preparing thin-walled ceramic articles of configuration

DOEpatents

Holcombe, C.E.; Powell, G.L.

1975-11-01

A method for preparing a hollow thin-walled ceramic product is described. Ceramic powder is plasma-sprayed onto a concave surface of a substrate having a coefficient of thermal expansion less than that of the ceramic. The coated substrate is heated to sinter the ceramic and then cooled to effect a separation of the ceramic product from the substrate. (auth)

A primary study into graphene/polyether ether ketone (PEEK) nanocomposite for laser sintering

NASA Astrophysics Data System (ADS)

Chen, Binling; Berretta, Silvia; Evans, Ken; Smith, Kaylie; Ghita, Oana

2018-01-01

This paper proposes two methods of preparation of graphene/PEEK powders for Laser Sintering (LS) and investigates their behaviour in relation to their microstructure and their properties. Thin composite films were fabricated in an attempt to replicate the thin layer formation of the powder bed process. Both methods of composite powder preparation (wet and dry) led to enhanced mechanical performance of the composite films at 0.1 and 0.5 wt% graphene nano-platelets (GNP) concentrations. The TEM images show that the GNP act as a nucleation point in crystallisation of PEEK, being at the centre of the spherulites. The hot stage microscopy reveals a 20 s delay in the onset of GNP/PEEK nanocomposite coalescence in comparison with plain PEEK. This is a very important observation for laser sintering, as it will influence the build strategy and specific parameters (e.g. time between layers deposition, multiple exposures). The excellent electrical conductivity properties of graphene were noticeable in the nanocomposite films at concentrations above 1 wt% GNP.

Preparation and characterization of natural bentonite in to nanoparticles by co-precipitation method

NASA Astrophysics Data System (ADS)

Sirait, Makmur; Bukit, Nurdin; Siregar, Nurdin

2017-01-01

The nanoparticle based on natural bentonite from Pahae village had been prepared using co-precipitation method. Bentonite was dried in the oven at 100°C during a week. Bentonite is crushed using a mortal and milled by planetary ball mill to obtain the powder form. Further, the bentonite powder is activated with chemical reaction by dissolves the 50 g bentonite to 100 ml of HCl at 10 M. The magnetic stirrer was employed to mix the solution at 300 rpm and temperature 70°C. After that, the bentonite solution is washed using distilled water until the pH is neutral. The bentonite powder is calcined at temperature of 600°C for 1 hour with fix increment 150°C. Finally, the powder is given High Energy Milling (HEM) treatment for 30 minutes to obtain the particle size. The X-ray Difractometer (XRD) and Scanning Electron Microscope (SEM) were used to characterize. From the characterization results it is reported that the average of bentonite nanoparticle size is 35.26 nm and the chemical constituents of natural bentonite Pahae are Al, Si, Ca, Fe and Ti.

Electrode structures and surfaces for Li batteries

DOEpatents

Thackeray, Michael M.; Kang, Sun-Ho; Balasubramanian, Mahalingam; Croy, Jason

2017-03-14

This invention relates to methods of preparing positive electrode materials for electrochemical cells and batteries. It relates, in particular, to a method for fabricating lithium-metal-oxide electrode materials for lithium cells and batteries. The method comprises contacting a hydrogen-lithium-manganese-oxide material with one or more metal ions, preferably in an acidic solution, to insert the one or more metal ions into the hydrogen-lithium-manganese-oxide material; heat-treating the resulting product to form a powdered metal oxide composition; and forming an electrode from the powdered metal oxide composition.

FABRICATION OF NEUTRON SOURCES

DOEpatents

Birden, J.H.

1959-04-21

A method is presented for preparing a neutron source from polonium-210 and substances, such as beryllium and boron, characterized by emission of neutrons upon exposure to alpha particles from the polonium. According to the invention, a source is prepared by placing powdered beryllium and a platinum foil electroplated with polonium-2;.0 in a beryllium container. The container is sealed and then heated by induction to a temperature of 450 to 1100 deg C to volatilize the polonium off the foil into the powder. The heating step is terminated upon detection of a maximum in the neutron flux level.

METHOD OF PREPARING POLONIUM-BORON SOURCES

DOEpatents

Birden, J.H.

1959-08-01

An improved technique is described for preparation of a polonium-boron neutron source. A selected amount of Po-210 is vaporized into a thin walled nickel container, then the desired amcunt of boron powder is added. After sealing the container, it is heated quickly by induction heating to vaporize the Po-210 and deposit it in the still cool boron powder. The unit is then quickly cooled to prevent revaporization of the Po-210 from the boron. The build-up of neutron emission may be followed by means of a neutron counter in order to terminate the heating at the optimum level of neutron yield.

Preparation and characterization of calcium phosphate ceramics and composites as bone substitutes

NASA Astrophysics Data System (ADS)

Zhang, Xing

Marine CaCO3 skeletons have tailored architectures created by nature, which give them structural support and other functions. For example, seashells have dense lamellar structures, while coral, cuttlebone and sea urchin spines have interconnected porous structures. In our experiments, seashells, coral and cuttlebone were hydrothermally converted to hydroxyapatite (HAP), and sea urchin spines were converted to Mg-substituted tricalcium phosphate (beta-TCMP), while maintaining their original structures. Partially converted shell samples have mechanical strength, which is close to that of compact human bone. After implantation of converted shell and spine samples in rat femoral defects for 6 weeks, there was newly formed bone growth up to and around the implants. Some new bone was found to migrate through the pores of converted spine samples and grow inward. These results show good bioactivity and osteoconductivity of the implants, indicating the converted shell and spine samples can be used as bone defect fillers. Calcium phosphate powders were prepared through different synthesis methods. Micro-size HAP rods were synthesized by hydrothermal method through a nucleation-growth mechanism. On the other hand, HAP particles, which have good crystallinity, were prepared by wet precipitation with further hydrothermal treatment. beta-TCP or beta-TCMP powders were prepared by a two-step process: wet precipitation of apatitic tricalcium phosphate ('precursor') and calcination of the precursor at 800°C for 3 hours. beta-TCMP or beta-TCP powders were also prepared by solid-state reactions from CaHPO4 and CaCO 3 with/without MgO. Biphasic calcium phosphate, which is mixture of HAP and beta-TCP, can be prepared though mechanical mixing of HAP and beta-TCP powders synthesized as above. Dense beta-TCP and beta-TCMP ceramics can be produced by pressing green bodies at 100MPa and further sintering above 1100°C for 2 hours. beta-TCMP ceramics ˜99.4% relative dense were prepared by this method. Dense beta-TCP ceramics have average strength up to 540MPa. Macroporous beta-TCMP ceramics were produced with sucrose as the porogen following a two-step pressing method. Porous beta-TCMP ceramics were also prepared by replication of polyurethane sponge. beta-TCMP ceramics with porous structures in the center surrounded by dense structures were created. The outside dense structures give the scaffold mechanical strength, while the central porous structures enable cells migration and vascular infiltration, and finally in-growth of new bone into the scaffold.

The analysis of carbohydrates in milk powder by a new "heart-cutting" two-dimensional liquid chromatography method.

PubMed

Ma, Jing; Hou, Xiaofang; Zhang, Bing; Wang, Yunan; He, Langchong

2014-03-01

In this study, a new"heart-cutting" two-dimensional liquid chromatography method for the simultaneous determination of carbohydrate contents in milk powder was presented. In this two dimensional liquid chromatography system, a Venusil XBP-C4 analysis column was used in the first dimension ((1)D) as a pre-separation column, a ZORBAX carbohydrates analysis column was used in the second dimension ((2)D) as a final-analysis column. The whole process was completed in less than 35min without a particular sample preparation procedure. The capability of the new two dimensional HPLC method was demonstrated in the determination of carbohydrates in various brands of milk powder samples. A conventional one dimensional chromatography method was also proposed. The two proposed methods were both validated in terms of linearity, limits of detection, accuracy and precision. The comparison between the results obtained with the two methods showed that the new and completely automated two dimensional liquid chromatography method is more suitable for milk powder sample because of its online cleanup effect involved. Crown Copyright © 2013. Published by Elsevier B.V. All rights reserved.

Effect of the powder characteristics of Sisub3Nsub4 on the microstructure of sintered bodies

NASA Technical Reports Server (NTRS)

Woetting, G.; Hausner, H.

1981-01-01

Silicon nitride powders sintered with the addition of 2 wt% Mg0 to 95% theoretical density after attrition milling and subsequent purification were evaluated. Preparation of the powders is described. The powder characteristics (specific surfaces, iron concentration, and oxygen content), and density, weight loss, and phase state of the sinter bodies as a function of powder preparation are presented.

Effect of ball milling and heat treatment process on MnBi powders magnetic properties

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

Xie, Wei; Polikarpov, Evgueni; Choi, Jung-Pyung

The metallic compound MnBi has high intrinsic coercivity with large positive temperature coefficient. The coercivity of MnBi exceeds 12 kOe and 26 kOe at 300 K and 523 K, respectively. Hence MnBi is a good candidate for the hard phase in exchange coupled nanocomposite magnets. In order to maximize the loading of the soft phase, the size of the MnBi particle has to be close to 500 nm, the size of single magnetic domain. Low energy milling is the common method to reduce MnBi particle size. However, only 3-7 mu m size particle can be achieved without significant decomposition. Here,more » we report our effort on preparing submicron MnBi powders using traditional powder metallurgy methods. Mn55Bi45 magnetic powders were prepared using arc melting method, followed by a series of thermal-mechanical treatment to improve purity, and finished with low energy ball milling at cryogenic temperature to achieve submicron particle size. The Mn55Bi45 powders were decomposed during ball milling process and recovered during 24 h 290 degrees C annealing process. With increasing ball-milling time, the saturation magnetization of MnBi decreases, while the coercivity increases. Annealing after ball milling recovers some of the magnetization, indicating the decomposition occurred during the ball-milling process can be reversed. The coercivity of Mn55Bi45 powders are also improved as a result of the heat treatment at 290 degrees C for 24 h. The world record magnetization 71.2 emu/g measured applying a field of 23 kOe has been achieved via low energy ball mill at room temperature« less

Structural, electrical and dielectric properties of spinel nickel ferrite prepared by soft mechanochemical synthesis

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

Lazarević, Zorica Ž., E-mail: lzorica@yahoo.com; Jovalekić, Čedomir; Sekulić, Dalibor L.

2013-10-15

Graphical abstract: - Highlights: • Sintered NiFe{sub 2}O{sub 4} was prepared by a soft mechanochemical route from mixture powders. • XRD and Raman measurements indicate that the prepared samples have spinel structure. • The activation energy ΔE are 0.653 and 0.452 eV for NiFe{sub 2}O{sub 4} samples. • Ferrite from Ni(OH){sub 2}/Fe{sub 2}O{sub 3} has lower DC conductivity than from Ni(OH){sub 2}/Fe(OH){sub 3} powders. • The values of dielectric constant of samples NiFe{sub 2}O{sub 4} are 70 and 200, respectively. - Abstract: Nickel ferrite, NiFe{sub 2}O{sub 4} was prepared by a soft mechanochemical route from a mixture of (1) Ni(OH){submore » 2} and α-Fe{sub 2}O{sub 3} and (2) Ni(OH){sub 2} and Fe(OH){sub 3} powders in a planetary ball mill for 25 h. The powder samples were sintered at 1100 °C for 2 h and were characterized by X-ray diffraction (XRD), Raman spectroscopy and scanning electron microscopy (SEM). Impedance spectroscopy techniques were used to study the effect of grain and grain boundary on the electrical properties of the prepared samples. A difference in dielectric constant (ε) and dielectric loss tangent (tan δ) of NiFe{sub 2}O{sub 4} samples obtained by the same methods but starting from different initial components was observed.« less

Sealed glass coating of high temperature ceramic superconductors

DOEpatents

Wu, W.; Chu, C.Y.; Goretta, K.C.; Routbort, J.L.

1995-05-02

A method and article of manufacture of a lead oxide based glass coating on a high temperature superconductor is disclosed. The method includes preparing a dispersion of glass powders in a solution, applying the dispersion to the superconductor, drying the dispersion before applying another coating and heating the glass powder dispersion at temperatures below oxygen diffusion onset and above the glass melting point to form a continuous glass coating on the superconductor to establish compressive stresses which enhance the fracture strength of the superconductor. 8 figs.

Sealed glass coating of high temperature ceramic superconductors

DOEpatents

Wu, Weite; Chu, Cha Y.; Goretta, Kenneth C.; Routbort, Jules L.

1995-01-01

A method and article of manufacture of a lead oxide based glass coating on a high temperature superconductor. The method includes preparing a dispersion of glass powders in a solution, applying the dispersion to the superconductor, drying the dispersion before applying another coating and heating the glass powder dispersion at temperatures below oxygen diffusion onset and above the glass melting point to form a continuous glass coating on the superconductor to establish compressive stresses which enhance the fracture strength of the superconductor.

Non-aqueous solution preparation of doped and undoped Li{sub x}Mn{sub y}O{sub z}

DOEpatents

Boyle, T.J.; Voigt, J.A.

1997-05-20

A method is described for generation of phase-pure doped and undoped Li{sub x}Mn{sub y}O{sub z} precursors. The method of this invention uses organic solutions instead of aqueous solutions or nonsolution ball milling of dry powders to produce phase-pure precursors. These precursors can be used as cathodes for lithium-polymer electrolyte batteries. Dopants may be homogeneously incorporated to alter the characteristics of the powder. 1 fig.

Development of Biodegradable Polycation-Based Inhalable Dry Gene Powders by Spray Freeze Drying

PubMed Central

Okuda, Tomoyuki; Suzuki, Yumiko; Kobayashi, Yuko; Ishii, Takehiko; Uchida, Satoshi; Itaka, Keiji; Kataoka, Kazunori; Okamoto, Hirokazu

2015-01-01

In this study, two types of biodegradable polycation (PAsp(DET) homopolymer and PEG-PAsp(DET) copolymer) were applied as vectors for inhalable dry gene powders prepared by spray freeze drying (SFD). The prepared dry gene powders had spherical and porous structures with a 5~10-μm diameter, and the integrity of plasmid DNA could be maintained during powder production. Furthermore, it was clarified that PEG-PAsp(DET)-based dry gene powder could more sufficiently maintain both the physicochemical properties and in vitro gene transfection efficiencies of polyplexes reconstituted after powder production than PAsp(DET)-based dry gene powder. From an in vitro inhalation study using an Andersen cascade impactor, it was demonstrated that the addition of l-leucine could markedly improve the inhalation performance of dry powders prepared by SFD. Following pulmonary delivery to mice, both PAsp(DET)- and PEG-PAsp(DET)-based dry gene powders could achieve higher gene transfection efficiencies in the lungs compared with a chitosan-based dry gene powder previously reported by us. PMID:26343708

Effect of processing route for preparation of mullite from kaolinite and alumina

NASA Astrophysics Data System (ADS)

Behera, Pallavi Suhasinee; Bhattacharyya, Sunipa

2018-05-01

In current work, two different types of mullite ceramic powder were prepared using kaolinite and alumina by solid state and chemical precipitation route. The phases, bond types and microstructural evolution of the mullite powders were investigated by X-ray diffraction, infrared analysis, and field emission scanning electron microscopy to study the mullitisation behavior. The solid state method evident a pure mullite phase formation at 1550 °C. In case of chemical precipitation route small amount of alumina peak was noticed along with major phase of mullite which was also clearly apprehended from FESEM micrographs and IR spectra. Densification was more for the samples prepared by solid state process which may be correlated to the delayed mullitization process in chemical precipitation route.

A cost-effective process to prepare VO{sub 2} (M) powder and films with superior thermochromic properties

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

Xiao, Xiudi; Zhang, Hua; Chai, Guanqi

2014-03-01

Graphical abstract: Combining codeposition and short time post annealing, VO{sub 2} (M) with high quality and excellent phase transition performance is obtained. After mixing the VO{sub 2} powder with acrylic resin, the composite films deposited on glass show superior visible transmission and solar modulation, which can be used as an excellent candidate of low cost smart window in energy saving field. - Highlights: • The VO{sub 2} powder obtained by short time thermolysis method is high purity and crystallinity with superior phase transition performance. • The maximum decreasing efficiency of phase transition temperature is about −30 K/at% with w =more » 0.4 at%. • After mixing VO{sub 2} powder with acrylic resin, the maximal visible transmission of the composite films is 48% and the transmission modulation at 2000 nm is 37.3% with phase transition temperature of 66.2 °C. • Though the phase transition performance is weakened by tungsten doping, the film prepared by 1.3 at% tungsten doped VO{sub 2} still show superior transmission modulation about 26.4%, which means that it is a potential candidate as smart windows. - Abstract: VO{sub 2} powder with superior phase transition performance was prepared by convenient thermolysis method. The results illustrated that VO{sub 2} powder show high purity and crystallinity. VO{sub 2} particles are transformed from cluster to quasi-sphere with the increase of annealing temperature. The DSC analysis proves that VO{sub 2} show superior phase transition performance around 68 °C. The phase transition temperature can be reduced to 33.5 °C by 1.8 at% tungsten doping. The maximum decreasing efficiency of phase transition temperature is about −30 K/at% with w = 0.4 at%. After mixing VO{sub 2} powder with acrylic resin, the maximal visible transmission of the composite thin films on glass is 48% and the transmission modulation at 2000 nm is 37.3% with phase transition temperature of 66.2 °C. Though the phase transition performance is weakened by tungsten doping, the film prepared by 1.3 at% tungsten doped VO{sub 2} still show superior transmission modulation about 26.4% at 2000 nm, which means that it is a potential candidate as smart windows.« less

A validated spectrofluorimetric method for the determination of citalopram in bulk and pharmaceutical preparations based on the measurement of the silver nanoparticles-enhanced fluorescence of citalopram/terbium complexes.

PubMed

Khan, Muhammad Naeem; Shah, Jasmin; Jan, Muhammad Rasul; Lee, Sang Hak

2013-01-01

A simple, sensitive, and accurate spectrofluorimetric method was developed for the determination of citalopram in bulk and pharmaceutical preparations. The method is based on the enhancement of the weak fluorescence signal (FL) of the Tb (III)-citalopram system in the presence of silver nanoparticles. Fluorescence intensities were measured at 555 nm after excitation at 281 nm. Prepared silver nanoparticles (AgNPs) were characterized by UV-Visible spectra and transmission electron microscopy (TEM). Various factors affecting the formation of citalopram-Tb (III)-AgNPs complexes were studied and optimized. The fluorescence intensity versus concentration plot was linear over the range 0.02-14 μg mL(-1), with an excellent correlation coefficient of 0.9978. The limit of detection (LOD) and limit of quantification (LOQ) were found to be 7.15 × 10(-6) μg mL(-1) and 2.38 × 10(-5) μg mL(-1) respectively. The proposed method was found to have good reproducibility with a relative standard deviation of 3.66% (n = 6). The interference effects of common excipients found in pharmaceutical preparations were studied. The developed method was validated statistically by performing recoveries studies and successfully applied for the assay of citalopram in bulk powder and pharmaceutical preparations. Percent recoveries were found to range from 98.98% to 100.97% for bulk powder and from 96.57% to 101.77% for pharmaceutical preparations.

Photon up-conversion production in Tb{sup 3+}–Yb{sup 3+} co-doped CaF{sub 2} phosphors prepared by combustion synthesis

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

Rakov, Nikifor, E-mail: nikifor.gomez@univasf.edu.br; Guimarães, Renato B.; Maciel, Glauco S., E-mail: glauco@if.uff.br

2016-02-15

Graphical abstract: Up-conversion luminescence from Tb{sup 3+} obtained by energy transfer from Yb{sup 3+} pairs in CaF{sub 2} powder prepared by combustion synthesis. - Highlights: • Calcium fluoride (CaF{sub 2}) powders were prepared by combustion synthesis. • Rare-earth ions doped in this material were found in interstitial sites. • Cooperative up-conversion was observed in Tb{sup 3+}:Yb{sup 3+}:CaF{sub 2} powder. • Energy transfer between Tb{sup 3+} and pairs of Yb{sup 3+} was analyzed using rate equations. - Abstract: Calcium fluoride (CaF{sub 2}) crystalline powders were successfully prepared by the combustion synthesis method. The powder material containing luminescent rare-earth ions, more specificallymore » terbium (Tb{sup 3+}) and ytterbium (Yb{sup 3+}), was studied by X-ray diffraction, scanning electronic microscopy and optical spectroscopy. These ions are allocated in charge compensated interstitial positions of tetragonal (C{sub 4v}) and trigonal (C{sub 3v}) symmetry sites of the cubic (O{sub h}) CaF{sub 2} lattice. Up-conversion (UC) luminescence in Tb{sup 3+} was achieved using a low power diode laser operating at 975 nm. Tb{sup 3+} is insensitive to near-infrared radiation but UC can be achieved via energy transfer from pairs of Yb{sup 3+} ions to Tb{sup 3+} ions. The UC luminescence dynamics of Tb{sup 3+} was used to study the energy transfer mechanism.« less

Combined Effect of Kimchi Powder and Onion Peel Extract on Quality Characteristics of Emulsion Sausages Prepared with Irradiated Pork.

PubMed

Lee, Soo-Yoen; Kim, Hyun-Wook; Hwang, Ko-Eun; Song, Dong-Heon; Choi, Min-Sung; Ham, Youn-Kyung; Choi, Yun-Sang; Lee, Ju-Woon; Lee, Si-Kyung; Kim, Cheon-Jei

2015-01-01

This study was conducted to investigate the effects of kimchi powder and onion peel extract on the quality characteristics of emulsion sausage manufactured with irradiated pork. The emulsion sausages were formulated with 2% kimchi powder and/or 0.05% onion peel extract. The changes in pH value of all treatments were similar, depending on storage periods. The addition of kimchi powder increased the redness and yellowness of the emulsion sausage. The addition of onion peel extract decreased the thiobarbituric acid reactive substances value of the emulsion sausages prepared with irradiated pork. The volatile basic nitrogen value of the emulsion sausage prepared with kimchi powder was the highest, whereas that of the emulsion sausage prepared with onion peel extract was the lowest. The treatment without kimchi powder or onion peel extract and the treatments prepared with onion peel extract showed lower microbial populations than the other treatment. Sensory evaluations indicated that a higher acceptability was attained when kimchi powder was added to the emulsion sausages manufactured with irradiated pork. In conclusion, our results suggest that combined use of kimchi powder and onion peel extract could improve quality characteristics and shelf stability of the emulsion sausage formulated with irradiated pork during chilled storage.

Combined Effect of Kimchi Powder and Onion Peel Extract on Quality Characteristics of Emulsion Sausages Prepared with Irradiated Pork

PubMed Central

Choi, Yun-Sang; Lee, Ju-Woon; Lee, Si-Kyung

2015-01-01

This study was conducted to investigate the effects of kimchi powder and onion peel extract on the quality characteristics of emulsion sausage manufactured with irradiated pork. The emulsion sausages were formulated with 2% kimchi powder and/or 0.05% onion peel extract. The changes in pH value of all treatments were similar, depending on storage periods. The addition of kimchi powder increased the redness and yellowness of the emulsion sausage. The addition of onion peel extract decreased the thiobarbituric acid reactive substances value of the emulsion sausages prepared with irradiated pork. The volatile basic nitrogen value of the emulsion sausage prepared with kimchi powder was the highest, whereas that of the emulsion sausage prepared with onion peel extract was the lowest. The treatment without kimchi powder or onion peel extract and the treatments prepared with onion peel extract showed lower microbial populations than the other treatment. Sensory evaluations indicated that a higher acceptability was attained when kimchi powder was added to the emulsion sausages manufactured with irradiated pork. In conclusion, our results suggest that combined use of kimchi powder and onion peel extract could improve quality characteristics and shelf stability of the emulsion sausage formulated with irradiated pork during chilled storage. PMID:26761840

Characteristics of Fe powders prepared by spray pyrolysis from a spray solution with ethylene glycol as the source material of heat pellet

NASA Astrophysics Data System (ADS)

Koo, H. Y.; Kim, J. H.; Hong, S. K.; Ko, Y. N.; Jang, H. C.; Jung, D. S.; Han, J. M.; Hong, Y. J.; Kang, Y. C.; Kang, S. H.; Cho, S. B.

2012-06-01

Fe powders as the heat pellet material for thermal batteries are prepared from iron oxide powders obtained by spray pyrolysis from a spray solution of iron nitrate with ethylene glycol. The iron oxide powders with hollow and thin wall structure produce Fe powders with elongated structure and fine primary particle size at a low reducing temperature of 615 °C. The mean size of the primary Fe powders with elongated structure decreases with increasing concentration of ethylene glycol dissolved into the spray solution. The heat pellets prepared from the fine-size Fe powders with elongated structure have good ignition sensitivities below 1 watt. The heat pellets formed from the Fe powders obtained from the spray solution with 0.5 M EG have an extremely high burn rate of 26 cms-1.

Bimodal metal micro-nanopowders for powder injection molding

NASA Astrophysics Data System (ADS)

Pervikov, Aleksandr; Rodkevich, Nikolay; Glazkova, Elena; Lerner, Marat

2017-12-01

The paper studies a bimodal metal powder composition designed to prepare feedstock for powder injection molding, as well as microstructure and porosity of sintered pats. Two kinds of metal powder compositions are used, in particular, a mixture of micro- and nanopowders and a bimodal powder prepared with dispersion of steel wire. The feedstock is prepared by mixing a bimodal metal powder composition with acetylacetone and paraffin wax. The microstructure of the debound parts is observed by scanning electron microscopy. The sintered parts are characterized by density measurements and metallographic analysis. The technique of the metal powder composition proves to affect the characteristics of sintered parts. Nanoparticles are shown in the interstitial spaces among the microparticles upon mixing micro- and nanopowders, but the regular distribution of nanoparticles on the surface of microparticles is observed in the bimodal powder providing the reduction of the porosity of sintered parts and increasing the density to the proper density of steel.

Preparation of superconductor precursor powders

DOEpatents

Bhattacharya, R.

1998-08-04

A process for the preparation of a precursor metallic powder composition for use in the subsequent formation of a superconductor. The process comprises the steps of providing an electrodeposition bath comprising an electrolyte medium and a cathode substrate electrode, and providing to the bath one or more soluble salts of one or more respective metals which are capable of exhibiting superconductor properties upon subsequent appropriate treatment. The bath is continually energized to cause the metallic and/or reduced particles formed at the electrode to drop as a powder from the electrode into the bath, and this powder, which is a precursor powder for superconductor production, is recovered from the bath for subsequent treatment. The process permits direct inclusion of all metals in the preparation of the precursor powder, and yields an amorphous product mixed on an atomic scale to thereby impart inherent high reactivity. Superconductors which can be formed from the precursor powder include pellet and powder-in-tube products. 7 figs.

Preparation of superconductor precursor powders

DOEpatents

Bhattacharya, Raghunath

1998-01-01

A process for the preparation of a precursor metallic powder composition for use in the subsequent formation of a superconductor. The process comprises the steps of providing an electrodeposition bath comprising an electrolyte medium and a cathode substrate electrode, and providing to the bath one or more soluble salts of one or more respective metals which are capable of exhibiting superconductor properties upon subsequent appropriate treatment. The bath is continually energized to cause the metallic and/or reduced particles formed at the electrode to drop as a powder from the electrode into the bath, and this powder, which is a precursor powder for superconductor production, is recovered from the bath for subsequent treatment. The process permits direct inclusion of all metals in the preparation of the precursor powder, and yields an amorphous product mixed on an atomic scale to thereby impart inherent high reactivity. Superconductors which can be formed from the precursor powder include pellet and powder-in-tube products.

Synthesis of boron nitride powders

NASA Astrophysics Data System (ADS)

Dreissig, Dirk Horst

2002-09-01

In the materials science community there is much interest in the development of new, efficient approaches for preparing ceramic powders having properties or performance characteristics not found with powders produced by traditional metallurgical synthesis methods. In this regard, aerosol-based syntheses are finding general acceptance for the preparation of non-metal and metal oxide powders. In contrast, much less effort has been given to aerosol-type syntheses for non-oxide powders despite potentially useful benefits. This dissertation describes the application of two chemical systems in aerosol assisted vapor phase synthesis (AAVS) for the preparation of spherical morphology boron oxynitride, BNxOy, powders that are subsequently converted to spherical morphology boron nitride in a second nitridation step. Chapter 1 describes the AAVS synthesis of BNxOy powders using a reaction of an aqueous boric acid containing aerosol with ammonia at 1000°C. The effect of reactor tube material, total gas flow rate, ammonia concentration, boric acid concentration, and urea addition to the boric acid aerosol on the percent oxygen composition is described. The resulting BNxOy powders contain significant amounts of oxygen that require replacement in a second stage nitridation reaction at elevated temperature under ammonia. The influences of the reaction temperature profile, crucible geometry and transformation additive on final oxygen composition and powder crystallinity are described. Chapter 2 outlines the formation of BNxOy powders from an AAVS reaction between the boron precursor (MeO)3B and ammonia. The formation of the powders is studied as a function of total gas flow rate and ammonia concentration. In all cases the resulting powders contain lower levels of oxygen compared to powders produced from aqueous boric acid aerosols. The conversion of the BNxOy powders in the second stage nitridation reaction with ammonia is examined as a function of crucible geometry, temperature profile and ammonia flow rate. In support of this process, the molecular reaction between (MeO)3B and NH3 was reexamined. The adduct, (MeO)3B·NH3, was isolated and its molecular structure determined by single crystal X-ray diffraction techniques. The results of these studies provide guidance for more detailed studies that should result in industrial scale synthesis of spherical morphology BN which currently is not formed by standard metallurgical syntheses. This new material has potential applications in several areas including the formation of BN loaded organic polymer composites.

Synthesis and mechanical/magnetic properties of nano-grained iron-oxides prepared with an inert gas condensation and pulse electric current sintering process

NASA Astrophysics Data System (ADS)

Choa, Yong-Ho; Nakayama, Tatachika; Sekino, Tohru; Niihara, Koichi

1999-04-01

Nanocrystalline iron-oxide powder was fabricated with an inert gas condensation (IGC) method combined with evaporation, and in-situ oxidation techniques. The particle size of iron-oxide powder was controlled by varying the helium gas pressure between 0.1 and 10 Torr, with the smallest one =10 nm at 0.1 Torr. The nanostructure was characterized by TEM. Nanocrystalline iron-oxide powder was sintered with the pulse electric current sintering (PECS) method to obtain densified γ-Fe2O3 materials, and suitably densified nano-grained γ-Fe2O3 materials (≈ 40 nm) of great hardness were obtained. The correlation between the nanostructure and magnetic properties of nanocrystalline powder and densified γ-Fe2O3 materials was also investigated.

Preparation and biological efficacy of haddock bone calcium tablets

NASA Astrophysics Data System (ADS)

Huo, Jiancong; Deng, Shanggui; Xie, Chao; Tong, Guozhong

2010-03-01

To investigate the possible use of waste products obtained after processing haddock, the present study prepared haddock bone calcium powder by NaOH and ethanol soaking (alkalinealcohol method) and prepared haddock bone calcium tablets using the powder in combination with appropriate excipients. The biological efficacy of the haddock bone calcium tablets was investigated using Wistar rats as an experiment model. Results show that the optimal parameters for the alkalinealcohol method are: NaOH concentration 1 mol/L, immersion time 30 h; ethanol concentration 60%, immersion time 15 h. A mixture of 2% polyvinylpyrrolidone in ethanol was used as an excipient at a ratio of 1:2 to full-cream milk powder, without the use of a disintegrating agent. This process provided satisfactory tablets in terms of rigidity and taste. Animal studies showed that the haddock bone calcium tablets at a dose of 2 g·kg-1·d-1 or 5g·kg-1·d-1 significantly increased blood calcium and phosphorus levels and bone calcium content in rats. Therefore, these tablets could be used for calcium supplementation and prevent osteoporosis. Although the reasons of high absorption in the rats fed with haddock bone calcium tablets are unclear, it is suggested that there are some factors, such as treatment with method of alkaline-alcohol or the added milk, may play positive roles in increasing absorption ratio.

Evaluation of Turmeric Powder Adulterated with Metanil Yellow Using FT-Raman and FT-IR Spectroscopy

PubMed Central

Dhakal, Sagar; Chao, Kuanglin; Schmidt, Walter; Qin, Jianwei; Kim, Moon; Chan, Diane

2016-01-01

Turmeric powder (Curcuma longa L.) is valued both for its medicinal properties and for its popular culinary use, such as being a component in curry powder. Due to its high demand in international trade, turmeric powder has been subject to economically driven, hazardous chemical adulteration. This study utilized Fourier Transform-Raman (FT-Raman) and Fourier Transform-Infra Red (FT-IR) spectroscopy as separate but complementary methods for detecting metanil yellow adulteration of turmeric powder. Sample mixtures of turmeric powder and metanil yellow were prepared at concentrations of 30%, 25%, 20%, 15%, 10%, 5%, 1%, and 0.01% (w/w). FT-Raman and FT-IR spectra were acquired for these mixture samples as well as for pure samples of turmeric powder and metanil yellow. Spectral analysis showed that the FT-IR method in this study could detect the metanil yellow at the 5% concentration, while the FT-Raman method appeared to be more sensitive and could detect the metanil yellow at the 1% concentration. Relationships between metanil yellow spectral peak intensities and metanil yellow concentration were established using representative peaks at FT-Raman 1406 cm−1 and FT-IR 1140 cm−1 with correlation coefficients of 0.93 and 0.95, respectively. PMID:28231130

Fabricating the spherical and flake silver powder used for the optoelectronic devices

NASA Astrophysics Data System (ADS)

Ju, Wei; Ma, Wangjing; Zhang, Fangzhi; Chen, Yixiang; Xie, Jinpeng

2018-01-01

The spherical and flake silver powder with different particle size for the optoelectronic devices was partly prepared by using chemical reduction and ball milling method, and charactered by scanning electron microscope (SEM), X-ray diffraction (XRD), laser particle size analyzer and thermo-gravimetric(TG) analyzer. The particle size of three series of spherical silver powder fabricated by chemical reduction is about 1.5μm, 1μm and 0.6μm, respectively; after being mechanical milling, the particle size of flake silver powder with high flaky rate is about 10μm, 6μm and 2μm respectively. Thermo gravimetric (TG) and XRD analyses showed that the silver powders have high purity and crystalline, and then the laser particle size and SEM analyses showed that the silver powders has good uniformity.

Novel Budesonide Particles for Dry Powder Inhalation Prepared Using a Microfluidic Reactor Coupled With Ultrasonic Spray Freeze Drying.

PubMed

Saboti, Denis; Maver, Uroš; Chan, Hak-Kim; Planinšek, Odon

2017-07-01

Budesonide (BDS) is a potent active pharmaceutical ingredient, often administered using respiratory devices such as metered dose inhalers, nebulizers, and dry powder inhalers. Inhalable drug particles are conventionally produced by crystallization followed by milling. This approach tends to generate partially amorphous materials that require post-processing to improve the formulations' stability. Other methods involve homogenization or precipitation and often require the use of stabilizers, mostly surfactants. The purpose of this study was therefore to develop a novel method for preparation of fine BDS particles using a microfluidic reactor coupled with ultrasonic spray freeze drying, and hence avoiding the need of additional homogenization or stabilizer use. A T-junction microfluidic reactor was employed to produce particle suspension (using an ethanol-water, methanol-water, and an acetone-water system), which was directly fed into an ultrasonic atomization probe, followed by direct feeding to liquid nitrogen. Freeze drying was the final preparation step. The result was fine crystalline BDS powders which, when blended with lactose and dispersed in an Aerolizer at 100 L/min, generated fine particle fraction in the range 47.6% ± 2.8% to 54.9% ± 1.8%, thus exhibiting a good aerosol performance. Subsequent sample analysis confirmed the suitability of the developed method to produce inhalable drug particles without additional homogenization or stabilizers. The developed method provides a viable solution for particle isolation in microfluidics in general. Copyright © 2017 American Pharmacists Association®. All rights reserved.

Preparation and visible-light photocatalytic properties of BiNbO₄ and BiTaO₄ by a citrate method

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

Zhai, Hai-Fa, E-mail: haifazhai@126.com; Li, Ai-Dong, E-mail: adli@nju.edu.cn; Kong, Ji-Zhou

2013-06-01

Visible-light photcatalysts of BiNbO₄ and BiTaO₄ powders have been successfully synthesized by a citrate method. The formation of pure triclinic phase of BiNbO₄ and BiTaO₄ at low temperature of 700 °C can be attributed to the advantage of the citrate method. The photocatalytic activity and possible mechanism were investigated deeply. For BiNbO₄ particles, the mechanism of methyl violet (MV) degradation under visible light irradiation involves photocatalytic and photosensitization pathways and the catalyst specific surface area has dominant influence. While for BiTaO₄ particles, the dominant mechanism arises from photosensitization pathways and a trade off between high specific surface area and goodmore » crystallinity is achieved. BiNbO₄ powder calcined at 700 °C shows the best photocatalytic efficiency among these catalysts, which is ascribed to its large surface area and more positive conduction band level. The optimal catalyst loading, additive H₂O₂ concentration and pH value is around 1 g/L, 2 mmol/L and 8 mmol/L, respectively. - Graphical abstract: Photodegradation performance and adsorption ability of BiNbO₄ and BiTaO₄ powders, respectively. BNO700 with the best photocatalytic efficiency is ascribed to its large surface area and more positive conduction band level. Highlights: • Pure BiNbO₄ and BiTaO₄ powders were prepared by a citrate method. • Excellent performance of visible-light degradation of MV was observed. • Different MV degradation mechanism for BiNbO₄ and BiTaO₄ powders was proposed. • BNO700 has large surface area and more positive conduction band level.« less

Characterization of calcium phosphate powders originating from Phyllacanthus imperialis and Trochidae Infundibulum concavus marine shells.

PubMed

Tămăşan, M; Ozyegin, L S; Oktar, F N; Simon, V

2013-07-01

The study reports the preparation and characterization of powders consisting of the different phases of calcium phosphates that were obtained from the naturally derived raw materials of sea-shell origins reacted with H3PO4. Species of sea origin, such as corals and nacres, attracted a special interest in bone tissue engineering area. Nacre shells are built up of calcium carbonate in aragonite form crystallized in an organic matrix. In this work two natural marine origin materials (shells of echinoderm Sputnik sea urchin - Phyllacanthus imperialis and Trochidae Infundibulum concavus mollusk) were involved in the developing powders of calcium phosphate based biomaterials (as raw materials for bone-scaffolds) by hotplate and ultrasound methods. Thermal analyses of the as-prepared materials were made for an assessment of the thermal behavior and heat treatment temperatures. Samples from both sea shells each of them prepared by the above mentioned methods were subjected to thermal treatments at 450 °C and 850 °C in order to evaluate the crystalline transformations of the calcium phosphate structures in the heating process. By X-ray diffraction analyses various calcium phosphate phases were identified. In Sputnik sea urchins originated samples were found predominantly brushite and calcite as a small secondary phase, while in Trochidae I. concavus samples mainly monetite and HA phases were identified. Thermal treatment at 850 °C resulted flat-plate whitlockite crystals - β-MgTCP [(Ca, Mg)3 (PO4)2] for both samples regardless the preparation method (ultrasound or hotplate) or the targeted Ca/P molar ratio according with XRD patterns. Scanning electron microscopy and Fourier transformed infrared spectroscopy were involved more in the characterization of these materials and the good correlations of the results of these methods were made. Copyright © 2013 Elsevier B.V. All rights reserved.

Citrate gel-combustion synthesis and sintering of nanocrystalline ThO2 powders

NASA Astrophysics Data System (ADS)

Sanjay Kumar, D.; Ananthasivan, K.; Amirthapandian, S.; Dasgupta, Arup; Jogeswara Rao, G.

2017-12-01

A systematic study of the influence of citric acid to nitrate mole (R) ratio (R = 0 to 0.50) on the citrate gel-combustion synthesis of nanocrystalline (nc) ThO2 in bulk quantities (30 g) by using citrate gel-combustion was carried out. The nc-ThO2 powders were characterized for their bulk density, size distribution of particles, specific surface area, carbon residue and X-ray crystallite size. All these powders were compacted at pressures varying from 60 to 353 MPa and sintered by using the "two-step sintering" method. Powders prepared from a mixture with an "R" value of 0.125 compacted at 243 MPa yielded a maximum sintered density of 98.8 ± 0.3% T.D. For nc-ThO2, this is the highest sintered density reported so far. The microstructural investigations on nc-ThO2 powders were carried out by using both scanning electron microscopy (SEM) and transmission electron microscopy (TEM). SEM images of the sintered thoria monoliths revealed faceted grains with well defined grain boundaries. Shrinkage anisotropy factor (α) revealed that the compacts prepared from the powders obtained from starting mixtures with R values of 0.125-0.50 had undergone uniform sintering (near isotropic shrinkage).

Effect of sample preparation method on quantification of polymorphs using PXRD.

PubMed

Alam, Shahnwaz; Patel, Sarsvatkumar; Bansal, Arvind Kumar

2010-01-01

The purpose of this study was to improve the sensitivity and accuracy of quantitative analysis of polymorphic mixtures. Various techniques such as hand grinding and mixing (in mortar and pestle), air jet milling and ball milling for micronization of particle and mixing were used to prepare binary mixtures. Using these techniques, mixtures of form I and form II of clopidogrel bisulphate were prepared in various proportions from 0-5% w/w of form I in form II and subjected to x-ray powder diffraction analysis. In order to obtain good resolution in minimum time, step time and step size were varied to optimize scan rate. Among the six combinations, step size of 0.05 degrees with step time of 5 s demonstrated identification of maximum characteristic peaks of form I in form II. Data obtained from samples prepared using both grinding and mixing in ball mill showed good analytical sensitivity and accuracy compared to other methods. Powder x-ray diffraction method was reproducible, precise with LOD of 0.29% and LOQ of 0.91%. Validation results showed excellent correlation between actual and predicted concentration with R2 > 0.9999.

[Selection of an optimum solvent for administration of oxinorm powder through a tube].

PubMed

Fukawa, Misako; Kokubun, Hideya; Sasaki, Hisako; Matsubara, Hajime; Yago, Kazuo

2008-05-01

Oxinorm powder is a rapid-release preparation of oxycodone hydrochloride for oral administration recently marketed for the first time in Japan. Administration of a powdered drug through a nasal tube is known to involve the risk of tube obstruction by the drug. For narcotic preparations like oxinorm powder, it is desirable from the perspective of drug control, that the drug administered be unlikely to remain in the cup, syringe or catheter used, and that the drug be dispensable in precise amounts. The present study was undertaken to identify problems associated with administration of oxinorm powder through a nasal tube and to determine an appropriate method for its administration. First, the solubility of the powder in various solvents was evaluated macroscopically to select initially appropriate solvents. Then, the drug dissolved in each of these solvents was administered through 3 types of catheters with different raw materials and forms, to simulate drug administration through a nasal tube. Percent residual drug remaining on/within the cup, syringe, and catheter was measured by HPLC, to evaluate the adhesiveness of the drug. When dissolved in distilled water, black vinegar, or milk, the drug was easy to administer through the catheter, with a low percentage of drug remaining on the cup, syringe, and catheter, suggesting that these fluids can be used as solvents for oxinorm powder. Semidigested nutrients such as Ensure.H were found to be unsuitable solvents for oxinorm powder.

Structural, negative thermal expansion and photocatalytic properties of ZrV{sub 2}O{sub 7}: a comparative study between fibers and powders

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

Liu, Qinqin, E-mail: liu_qin_qin@126.com; Yang, Juan; Rong, Xiaoqing

2014-10-15

Novel ZrV{sub 2}O{sub 7} microfibers with diameters about 1–3 μm were synthesized using a sol–gel technique. For comparison, ZrV{sub 2}O{sub 7} powders were prepared by the same method. The resultant structures were studied by X-ray diffraction, field-emission scanning electron microscopy and transmission electron microscopy. The results indicated that both the pure ZrV{sub 2}O{sub 7} microfibers and powders could be synthesized by the sol–gel technique. The thermal expansion property of the as-prepared ZrV{sub 2}O{sub 7} microfibers and powders was characterized by a thermal mechanical analyzer, both the fibers with cylindrical morphology and irregular powders with average size between 100 and 200more » nm showed negative thermal expansion between 150 °C and 600 °C. The photocatalytic activity of the microfibers was compared to that of powders under UV radiations. The band gap of ZrV{sub 2}O{sub 7} microfibers decreased and its absorption edge exhibited red shift. The microfibers also had a higher surface area compared with the powders, resulting in considerably higher photocatalytic characteristics. The large surface area and the enhanced photocatalytic activity of the ZrV{sub 2}O{sub 7} microfibers also offer potential applications in sensors and inorganic ion exchangers. - Graphical abstract: (a and c) SEM photos of ZrV{sub 2}O{sub 7} powders and fibers. (b and d) TEM images of ZrV{sub 2}O{sub 7} powders and fibers. (e) Thermal expansion curves of ZrV{sub 2}O{sub 7} powders and fibers. (f) Degradation curves of ZrV{sub 2}O{sub 7} powders and ZrV{sub 2}O{sub 7} fibers. - Highlights: • Novel ZrV{sub 2}O{sub 7} fibers could be synthesized using sol–gel technique. • ZrV{sub 2}O{sub 7} powders with irregular shape are also prepared for comparison. • Both ZrV{sub 2}O{sub 7} microfibers and powders exhibit negative thermal expansion property. • ZrV{sub 2}O{sub 7} microfibers show outstanding photocatalytic activity under UV irradiation. • This synthesis technique can be easily extended to many other functional fibers.« less

Optimization of formulation and processing of Moringa oleifera and spirulina complex tablets.

PubMed

Zheng, Yi; Zhu, Fan; Lin, Dan; Wu, Jun; Zhou, Yichao; Mark, Bohn

2017-01-01

Objective: To prepare a more comprehensive nutrition, more balanced proportion of natural nutritional supplement tablets with Moringa oleifera leaves and spirulina the two nutrients which have complementary natural food ingredients. Method: On the basis of research M. oleifera leaves with spirulina nutrient composition was determined on M. oleifera leaves and spirulina ratio of raw materials, and the choice of microcrystalline cellulose, sodium salt of caboxy methyl cellulose(CMC),magnesium stearate excipient, through single factor and orthogonal experiment, selecting the best formula tablets prepared by powder direct compression technology, for preparation of M. oleifera and spirulina complex tablets. Results: The best ratio of raw material for the M. oleifera leaves powder: spirulina powder was 7:3, the best raw materials for the tablet formulation was 88.5%, 8.0% microcrystalline cellulose, CMC 2.0%, stearin magnesium 1.5%, the optimum parameters for the raw material crushing 200-300 mesh particle size, moisture content of 7%, tableting pressure 40 kN. Conclusion: Through formulation and process optimization, we can prepare more comprehensive and balanced nutrition M. oleifera and spirulina complex tablets, its sheet-shaped appearance, piece weight variation, hardness, friability, disintegration and other indicators have reached the appropriate quality requirements.

Highly transparent cerium doped gadolinium gallium aluminum garnet ceramic prepared with precursors fabricated by ultrasonic enhanced chemical co-precipitation.

PubMed

Zhang, Ji-Yun; Luo, Zhao-Hua; Jiang, Hao-Chuan; Jiang, Jun; Chen, Chun-Hua; Zhang, Jing-Xian; Gui, Zhen-Zhen; Xiao, Na

2017-11-01

Cerium doped gadolinium gallium aluminum garnet (GGAG:Ce) ceramic precursors have been synthesized with an ultrasonic chemical co-precipitation method (UCC) and for comparison with a traditional chemical co-precipitation method (TCC). The effect of ultra-sonication on the morphology of powders and the transmittance of GGAG:Ce ceramics are studied. The results indicate that the UCC method can effectively improve the homogenization and sinterability of GGAG:Ce powders, which contribute to obtain high transparent GGAG ceramic with the highest transmittance of 81%. Copyright © 2017 Elsevier B.V. All rights reserved.

Arc melting and homogenization of ZrC and ZrC + B alloys

NASA Technical Reports Server (NTRS)

Darolia, R.; Archbold, T. F.

1973-01-01

A description is given of the methods used to arc-melt and to homogenize near-stoichiometric ZrC and ZrC-boron alloys, giving attention to the oxygen contamination problem. The starting material for the carbide preparation was ZrC powder with an average particle size of 4.6 micron. Pellets weighing approximately 3 g each were prepared at room temperature from the powder by the use of an isostatic press operated at 50,000 psi. These pellets were individually melted in an arc furnace containing a static atmosphere of purified argon. A graphite resistance furnace was used for the homogenization process.

High performance p-type thermoelectric materials and methods of preparation

NASA Technical Reports Server (NTRS)

Caillat, Thierry (Inventor); Borshchevsky, Alexander (Inventor); Fleurial, Jean-Pierre (Inventor)

2005-01-01

The present invention is embodied in high performance p-type thermoelectric materials having enhanced thermoelectric properties and the methods of preparing such materials. In one aspect of the invention, p-type semiconductors of formula Zn4-xAxSb3-yBy wherein 0?x?4, A is a transition metal, B is a pnicogen, and 0?y?3 are formed for use in manufacturing thermoelectric devices with substantially enhanced operating characteristics and improved efficiency. Two methods of preparing p-type Zn4Sb3 and related alloys of the present invention include a crystal growth method and a powder metallurgy method.

Synthesis and in vitro bioactivity of bredigite powders.

PubMed

Wu, Chengtie; Chang, Jiang

2007-01-01

Pure bredigite (Ca7MgSi4O16) powders are synthesized by the sol-gel method. The bredigite powders are composed of polycrystalline particles with dimensions of 1-10 micro m. The in vitro bioactivity of the bredigite powders are examined by evaluation of hydroxyapatite (HAp) formation ability in simulated body fluid (SBF) and the effect of ionic products from bredigite dissolution on osteoblast proliferation. The results showed that bredigite induced the formation of nanocrystalline HAp after soaking in SBF for 10 days. The Ca, Si, and Mg ions from bredigite dissolution at a certain concentration range stimulates osteoblast proliferation. Our study indicates that bredigite is bioactive and might be used for preparation of new biomaterials.

Preparation of nano fluids by mechanical method

NASA Astrophysics Data System (ADS)

Boopathy, J.; Pari, R.; Kavitha, M.; Angelo, P. C.

2012-07-01

Nanofluids are conventional heat transfer fluids that contain nano particles of metals, oxides, carbides, nitrides, or nanotubes. Nanofluids exhibit enhanced thermal conductivity and heat transfer coefficients compared to the base fluids. This paper presents the procedure for preparing nanofluids consisting of Copper and Aluminium nano powders in base fluids. Copper and Aluminium nano powders were produced by planetary ball wet milling at 300rpm for 50hrs. Toluene was added to ensure wet milling. These powders were characterized in XRD and SEM for their purity, particle size and shape. The XRD results confirmed the final particle sizes of Copper and Aluminium in the nano range. Then the 0.01 gm of nano metal powders was added in 150 ml of double distilled water and magnetic stirring was done at 1500 rpm for 15 minutes. Sodium lauryl sulphate (0.05%) was added in water as surfactant to ensure the stability of the dispersion. Ultrasonication in the 3000 watts bath was done for 10 minutes to enhance the uniform dispersion of metal powders in water. The pH, dynamic viscosity, ionic conductivity and the stability of the fluids were determined for further usage of synthesized nanofluids as coolant during grinding operation.

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

NASA Astrophysics Data System (ADS)

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

2013-08-01

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

Bend strengths of reaction bonded silicon nitride prepared from dry attrition milled silicon powder

NASA Technical Reports Server (NTRS)

Herbell, T. P.; Glasgow, T. K.

1979-01-01

Dry attrition milled silicon powder was compacted, sintered in helium, and reaction bonded in nitrogen-4 volume percent hydrogen. Bend strengths of bars with as-nitrided surfaces averaged as high as 210 MPa at room temperature and 220 MPa at 1400 C. Bars prepared from the milled powder were stronger than those prepared from as-received powder at both room temperature and at 1400 C. Room temperature strength decreased with increased milling time and 1400 C strength increased with increased milling time.

Effect of starting powder morphology on film texture for bismuth layer-structured ferroelectrics prepared by aerosol deposition method

NASA Astrophysics Data System (ADS)

Suzuki, Muneyasu; Tsuchiya, Tetsuo; Akedo, Jun

2017-06-01

We report grain orientation control for bismuth layer-structured ferroelectrics (BLSFs) films deposited by aerosol deposition (AD) method at room temperature. Bi4Ti3O12 (BiT), SrBi2Ta2O9 (SBTa), and SrBi4Ti4O15 (SBTi) starting powders with particles of various shape (plate-like, spherical, and angular) were prepared by solid-state reaction and fused salt synthesis. Their AD films represented fine microstructures without pores, which agrees well with previous reports. Although the SBTa AD films deposited by using spherical particles exhibited an extremely low Lotgering factor (F), the BiT AD films deposited by using plate-like particles exhibited a marked c-axis orientation. The F of BiT and SBTi AD films decreased with increasing film thickness (t). We consider that the dispersion of agglomerated plate-like particles on the film surface and the densification of the compacted powder layer occurring while under particle impact are important in obtaining the grain-oriented AD films. These results of using the AD method with shape-controlled particles are expected to result in open up an innovative functional coating technique.

Novel Injectable Calcium Phosphate Bone Cement from Wet Chemical Precipitation Method

NASA Astrophysics Data System (ADS)

Hablee, S.; Sopyan, I.; Mel, M.; Salleh, H. M.; Rahman, M. M.; Singh, R.

2017-06-01

Calcium phosphate cement has been prepared via chemical precipitation method for injectable bone filling materials. Calcium hydroxide, Ca(OH)2, and diammonium hydrogen phosphate, (NH4)2HPO4, were used as calcium and phosphorus precursors respectively. The synthesized powder was mixed with water at different powder-to-liquid (P/L) ratios, which was adjusted at 0.8, 0.9, 1.0, 1.1 and 1.2. The influence of P/L ratio on the injectability, setting time and mechanical strength of calcium phosphate cement paste has been evaluated. The synthesized powder appeared as purely hydroxyapatite with nanosized and agglomerated spherical particles. All cement pastes show excellent injectability except for the paste with P/L ratio 1.2. Calcium phosphate cement with P/L ratio 1.1 shows the ideal cement for bone filler application with good injectability, the initial and final setting times of 30 min and 160 min, and the compression strength of 2.47 MPa. The result indicated that the newly developed calcium phosphate cement is physically suitable for bone filler application. This paper presents our investigation on the effect of P/L ratio on the handling and mechanical properties of calcium phosphate cement prepared via wet chemical precipitation method.

Standards for electron probe microanalysis of silicates prepared by convenient method

NASA Technical Reports Server (NTRS)

Walter, L. S.

1966-01-01

Standard compositions suitable for electron probe microanalysis of various silicates are prepared by coprecipitation of specified salts with colloidal silica to form a gel which is decomposed into a powdered oxide mixture and compressed into thin pellets. These pellets of predetermined standard are compared with a silicate sample to determine its composition.

Initial Study on Thin Film Preparation of Carbon Nanodots Composites as Luminescence Material

NASA Astrophysics Data System (ADS)

Iskandar, F.; Aimon, A. H.; Akmaluddin, A. R.; Nuryadin, B. W.; Abdullah, M.

2016-08-01

Nowadays, the developments of phosphors materials require elements without noble metals and simple production process. Carbon nanodots (C-dots) are one of phosphor materials with wide range of emission band, and high biocompatibility. In this research thin film carbon nanodots composite have been prepared by spin coating method. Prior deposition, powder carbon nanodots were synthesized from a mixture of commercial urea as the nitrogen sources and citric acid as a carbon source by using hydrothermal and microwave-assisted heating method. The prepared powder was dispersed in transparent epoxy resin and then coated on glass substrate. The photoluminescence result for sample with 0.035 g citric acid exhibited an intense, single, homogeneous and broad spectrum with yellowish emission upon excitation at 365 nm. The Fourier Transform Infrared Spectroscopy (FTIR) result showed the existences of C=C, C-H, C=O, N-H and O-H functional groups which confirmed the quality of the sample. Further, based on UV-Vis measurement, the prepared thin film was highly transparent (transmittance 90%) with estimated film thickness around 764 nm. This result may open an opportunity for optoelectronic devices.

A validated high performance thin layer chromatography method for determination of yohimbine hydrochloride in pharmaceutical preparations

PubMed Central

Badr, Jihan M.

2013-01-01

Background: Yohimbine is an indole alkaloid used as a promising therapy for erectile dysfunction. A number of methods were reported for the analysis of yohimbine in the bark or in pharmaceutical preparations. Materials and Method: In the present work, a simple and sensitive high performance thin layer chromatographic method is developed for determination of yohimbine (occurring as yohimbine hydrochloride) in pharmaceutical preparations and validated according to International Conference of Harmonization (ICH) guidelines. The method employed thin layer chromatography aluminum sheets precoated with silica gel as the stationary phase and the mobile phase consisted of chloroform:methanol:ammonia (97:3:0.2), which gave compact bands of yohimbine hydrochloride. Results: Linear regression data for the calibration curves of standard yohimbine hydrochloride showed a good linear relationship over a concentration range of 80–1000 ng/spot with respect to the area and correlation coefficient (R2) was 0.9965. The method was evaluated regarding accuracy, precision, selectivity, and robustness. Limits of detection and quantitation were recorded as 5 and 40 ng/spot, respectively. The proposed method efficiently separated yohimbine hydrochloride from other components even in complex mixture containing powdered plants. The amount of yohimbine hydrochloride ranged from 2.3 to 5.2 mg/tablet or capsule in preparations containing the pure alkaloid, while it varied from zero (0) to 1.5–1.8 mg/capsule in dietary supplements containing powdered yohimbe bark. Conclusion: We concluded that this method employing high performance thin layer chromatography (HPTLC) in quantitative determination of yohimbine hydrochloride in pharmaceutical preparations is efficient, simple, accurate, and validated. PMID:23661986

Design, Development and Rationalization of Sarpagandha Ghanvati

PubMed Central

Pundarikakshudu, K.; Bhatt, C. J.

2015-01-01

Sarpagandha ghanvati is a classical Ayurvedic formulation widely prescribed for anxiety and insomnia. It contains Sarpagandha (roots of Rauwolfia serpentina L. (Benth.) Ex Kurz; Family: Apocyanaceae), Khurasani ajowan (Hyocyamus niger L.; Family: Solanaceae) seeds, Jatamansi (Nardostachys jatamansi DC. Family: Valerianaceae) roots and Pipplamul (root of Piper longum L.; Family: Piperaceae). The objective of this study was to make a comparative evaluation of Ghanvatis and tablets of this formulation. Two tablet formulations were prepared; one incorporating only powders of all ingredients; the other with ethanol extracts of the first three ingredients and powder of Piper longum root. Similarly, two types of Sarpagandha ghanvati pills were prepared; one as per Ayurvedic Formulary of India; the other with ethanol extracts of the first three ingredients and powder of Piper longum root. Alcohol extracted 0.22% w/w of total alkaloids as against 0.061% w/w extracted by water. Tablets prepared with powders of all the ingredients had friability more than 3.0% where as those prepared with ethanol extract had very low friability. Ghanvatis, prepared as per the Ayurvedic formulary, did not show reserpine although other alkaloids were present. They showed less content uniformity and lower drug release. Ethanol extracted reserpine along with other alkaloids. Ghanvatis made with the alcoholic extracts exhibited better content uniformity and drug release than the traditional formulation. Tablets prepared with powders or extracts of the ingredients exhibited good content uniformity but the release of alkaloids from the tablets of powders was only 80%. Tablets of the extracts had good content uniformity with 90% release of the total alkaloids. Tablets prepared with alcoholic extracts using 1% polyvinylpyrrolidone as binder and 5% dried starch powder as disintegrating agent confirmed to all the requirements. Thus, the study shows tablets made with the extracts are superior to Ghanvatis and powder tablets. PMID:26798180

Effect of titanium on the structural and optical property of NiO nano powders

NASA Astrophysics Data System (ADS)

Amin, Ruhul; Mishra, Prashant; Khatun, Nasima; Ayaz, Saniya; Srivastava, Tulika; Sen, Somaditya

2018-05-01

Nickel Oxide (NiO) and Ti doped NiO nanoparticles were prepared by sol-gel auto combustion method. Powder x-ray diffraction (PXRD) structural studies revealed face centered cubic (FCC) structure of the NiO nanopowders. The crystallite size decreased with Ti incorporation. UV-Vis spectroscopy carried out in diffused reflectance mode revealed decrease in band gap with increment in Urbach energy with doping.

Diamond-silicon carbide composite and method

DOEpatents

Zhao, Yusheng [Los Alamos, NM

2011-06-14

Uniformly dense, diamond-silicon carbide composites having high hardness, high fracture toughness, and high thermal stability are prepared by consolidating a powder mixture of diamond and amorphous silicon. A composite made at 5 GPa/1673K had a measured fracture toughness of 12 MPam.sup.1/2. By contrast, liquid infiltration of silicon into diamond powder at 5 GPa/1673K produces a composite with higher hardness but lower fracture toughness.

NUCLEAR REACTOR FUEL ELEMENTS AND METHOD OF PREPARATION

DOEpatents

Kingston, W.E.; Kopelman, B.; Hausner, H.H.

1963-07-01

A fuel element consisting of uranium nitride and uranium carbide in the form of discrete particles in a solid coherent matrix of a metal such as steel, beryllium, uranium, or zirconium and clad with a metal such as steel, aluminum, zirconium, or beryllium is described. The element is made by mixing powdered uranium nitride and uranium carbide with powdered matrix metal, then compacting and sintering the mixture. (AEC)

[Effect of non-genetically modified (non-GM) soy varieties on the measured value of GM soy by a quantitative PCR method].

PubMed

Watanabe, Takahiro; Sekino, Ayako; Shiramasa, Yuko; Matsuda, Rieko; Maitani, Tamio

2008-08-01

It is very important to examine the effect of non-genetically modified (non-GM) soy varieties, which constitute the matrix of the testing sample used to quantify GM soy (RRS), on the measured value of RRS by quantitative PCR methods. Therefore, we quantified the amount of RRS in powder-mixed samples containing 1 or 5% RRS prepared by using 10 different varieties of non-GM soy as the matrix. The results revealed that the measured values were not in agreement with the powder-mixing levels and that the extent of the difference depended on the variety of non-GM soy used as the matrix. The yields of DNA extracted differed among the soy varieties. On the other hand, analysis of DNA-mixed samples, that were prepared with the DNAs extracted from RRS and non-GM soy varieties, showed that the measured values of RRS were in agreement with the DNA-mixing levels. These results strongly suggest that the proportions of DNA derived from RRS and non-GM soy were not consistent with the powder-mixing ratio in the case of some non-GM soy varieties used as a matrix, resulting in the discrepancy between the measured values and the powder-mixing levels.

Preparation of High-Quality FeV55N Using Ammonia as a Reductant and Nitrogen Source

NASA Astrophysics Data System (ADS)

Wu, Yue-Dong; Zhang, Guo-Hua; Chou, Kuo-Chih

2018-05-01

High-quality FeV55N has been prepared by using ammonia as a reductant and nitrogen source. The raw materials comprised ammonium vanadate and Fe2O3, which were first reduced and nitrided by ammonia to prepare FeV55N composite powders of VN and Fe2N. Subsequently, the composite powders were sintered at high temperature to obtain a bulk FeV55N alloy. The final products obtained by this method do not contain elemental Al, Si, or C impurities. Furthermore, the residual oxygen content of the final products can be reduced to 0.56 wt.%. After sintering, it is possible to obtain a FeV55N alloy with a density of up to 5.4 g/cm3.

Perylene and Perylene-Derivative Nano-Cocrystals: Preparation and Physicochemical Property

NASA Astrophysics Data System (ADS)

Baba, Koichi; Konta, Sayaka; Oliveira, Daniel; Sugai, Kenji; Onodera, Tsunenobu; Masuhara, Akito; Kasai, Hitoshi; Oikawa, Hidetoshi; Nakanishi, Hachiro

2012-12-01

Organic nano-cocrystals of functional dyes of perylene and a perylene derivative were successfully prepared by the reprecipitation method. The particle sizes, optical properties, and powder X-ray diffraction patterns of nano-cocrystals were evaluated. Typically, the size with size distribution of nano-cocrystals was 55±15 nm when the molar ratio of perylene to the perylene derivative was 50:50. The particular intermolecular electronic interaction between perylene and the perylene derivative in the nano-cocrystal state was observed by absorption and fluorescence spectra measurements. The powder X-ray diffraction pattern analysis confirmed that the structure of nano-cocrystals was different from those prepared from perylene and the perylene derivative. The nano-cocrystal having unique physicochemical properties will be potentially classified as a new type of functional nanomaterial.

Use of B4C powder for preparing in situ Al-Ti-B-C inoculant in Al-Ti melt and its refining effect on A356 alloy

NASA Astrophysics Data System (ADS)

Liu, Shuiqing; Cui, Chunxiang; Wang, Xin; Zhao, Lichen; Sun, Yijiao; Shi, Jiejie; Cui, Sen; Ding, Jinhua

2018-01-01

A novel preparation technology of Al-Ti-B-C inoculant with uniform microstructure is prepared using B4C powder instead of graphite in Al-Ti melt reaction method in this study. It is found that the addition of B4C powder improves the wettability between carbon element and liquid aluminum and reduce the tendency to the gravity segregation simultaneously. The result shows that Al-Ti-B-C inoculant using B4C powder presents excellent grain refinement performance than the conventional approach. After T6 heat treatment, the ultimate tensile strength, the yield strength and elongation of A356 alloy are increased to 292 ± 6 MPa, 238 ± 7 MPa and 8.2% ± 0.5% from 260 ± 7 MPa, 218 ± 5 MPa and 4.9% ± 0.6% by addition of Al-Ti-B-C inoculant with a very small ratio of 0.3% in weight. The increase of strength in Al-Ti-B-C refined alloy is attributed to the grain refinement of primary α-Al, while the increase of ductility results from the submicron particles in Al-Ti-B-C inoculant adsorb impurity atoms as well as decreased grain size.

Pharmaceutical production of tableting granules in an ultra-small-scale high-shear granulator as a pre-formulation study.

PubMed

Ogawa, Tatsuya; Uchino, Tomohiro; Takahashi, Daisuke; Izumi, Tsuyoshi; Otsuka, Makoto

2012-11-01

In some of drug developments, the amount of bulk drug powder to use in early stages is limited and it is not easy to supply a sufficient drug amount for conventional preparation methods. Therefore, an ultra-small-scale high-shear granulator (less than 5 g) (USG) was developed and applied to small-scale granulation as a pre-formulation. The sample powder consisted of 66.5% lactose, 28.5% microcrystalline cellulose and 5.0% hydroxypropylcellulose. The granules were obtained to agitate 5 g of the sample powder with 1.0 mL of water at 300 rpm for 5 min after pre-powder mixing for 3 min by the USG and the manual hand (HM) methods. The granules were evaluated by the 10% and 90% accumulated particle size and the recoveries of the granules and the powder solid. Median particle size for the USG and the HM methods was 159.2 ± 2.3 and 270.9 ± 14.9 µm, respectively. The USG method had a narrower particle size distribution than those by the HM method. The recovery of the granules by USG was significantly larger than that by the HM method. Characteristics of all of the granules indicated that the USG method could produce higher quality granules within a shorter time than the HM methods.

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.

Preparation of superconductor precursor powders

DOEpatents

Bhattacharya, Raghunath; Blaugher, Richard D.

1995-01-01

A process for the preparation of a precursor metallic powder composition for use in the subsequent formation of a superconductor. The process comprises the steps of providing an electrodeposition bath comprising an electrolyte medium and a cathode substrate electrode, and providing to the bath one or more soluble salts of one or more respective metals, such as nitrate salts of thallium, barium, calcium, and copper, which are capable of exhibiting superconductor properties upon subsequent appropriate treatment. The bath is continually energized to cause the metallic particles formed at the electrode to drop as a powder from the electrode into the bath, and this powder, which is a precursor powder for superconductor production, is recovered from the bath for subsequent treatment. The process permits direct inclusion of thallium in the preparation of the precursor powder, and yields an amorphous product mixed on an atomic scale to thereby impart inherent high reactivity. Superconductors which can be formed from the precursor powder include pellet and powder-in-tube products.

Production of zinc oxide nanowires power with precisely defined morphology

NASA Astrophysics Data System (ADS)

Mičová, Júlia; Remeš, Zdeněk; Chan, Yu-Ying

2017-12-01

The interest about zinc oxide is increasing thanks to its unique chemical and physical properties. Our attention has focused on preparation powder of 1D nanostructures of ZnO nanowires with precisely defined morphology include characterization size (length and diameter) and shape controlled in the scanning electron microscopy (SEM). We have compared results of SEM with dynamic light scattering (DLS) technique. We have found out that SEM method gives more accurate results. We have proposed transformation process from ZnO nanowires on substrates to ZnO nanowires powder by ultrasound peeling to colloid followed by lyophilization. This method of the mass production of the ZnO nanowires powder has some advantages: simplicity, cost effective, large-scale and environment friendly.

Variation of the shape and morphological properties of silica and metal oxide powders by electro homogeneous precipitation

DOEpatents

Harris, M.T.; Basaran, O.A.; Sisson, W.G.; Brunson, R.R.

1997-02-18

The present invention provides a method for preparing irreversible linear aggregates (fibrils) of metal oxide powders by utilizing static or pulsed DC electrical fields across a relatively non-conducting liquid solvent in which organometal compounds or silicon alkoxides have been dissolved. The electric field is applied to the relatively non-conducting solution throughout the particle formation and growth process promoting the formation of either linear aggregates (fibrils) or spherical shaped particles as desired. Thus the present invention provides a physical method for altering the size, shape and porosity of precursor hydrous metal oxide or hydrous silicon oxide powders for the development of advanced ceramics with improved strength and insulating capacity. 3 figs.

Phase composition, microstructure, and mechanical properties of porous Ti-Nb-Zr alloys prepared by a two-step foaming powder metallurgy method.

PubMed

Rao, X; Chu, C L; Zheng, Y Y

2014-06-01

Porous Ti-Nb-Zr alloys with different porosities from 6.06 to 62.8% are prepared by a two-step foaming powder metallurgy method using TiH2, Nb, and Zr powders together with 0 to 50wt% of NH4HCO3. The effects of the amounts of Nb and Zr as well as the sintering temperature (1473 to 1673K) on their phase composition, porosity, morphology, and mechanical characteristics are investigated. By controlling the porosity, Nb and Zr concentrations as well as the sintering temperature, porous Ti-Nb-Zr alloys with different mechanical properties can be obtained, for example, the hardness between 290 and 63HV, the compressive strength between 1530.5 and 73.4MPa, and the elastic modulus between 10.8 and 1.2GPa. The mechanical properties of the sintered porous Ti-Nb-Zr alloys can be tailored to match different requirements for the human bones and are thus potentially useful in the hard tissue implants. Copyright © 2014 Elsevier Ltd. All rights reserved.

The Remote Food Photography Method Accurately Estimates Dry Powdered Foods-The Source of Calories for Many Infants.

PubMed

Duhé, Abby F; Gilmore, L Anne; Burton, Jeffrey H; Martin, Corby K; Redman, Leanne M

2016-07-01

Infant formula is a major source of nutrition for infants, with more than half of all infants in the United States consuming infant formula exclusively or in combination with breast milk. The energy in infant powdered formula is derived from the powder and not the water, making it necessary to develop methods that can accurately estimate the amount of powder used before reconstitution. Our aim was to assess the use of the Remote Food Photography Method to accurately estimate the weight of infant powdered formula before reconstitution among the standard serving sizes. For each serving size (1 scoop, 2 scoops, 3 scoops, and 4 scoops), a set of seven test bottles and photographs were prepared as follow: recommended gram weight of powdered formula of the respective serving size by the manufacturer; three bottles and photographs containing 15%, 10%, and 5% less powdered formula than recommended; and three bottles and photographs containing 5%, 10%, and 15% more powdered formula than recommended (n=28). Ratio estimates of the test photographs as compared to standard photographs were obtained using standard Remote Food Photography Method analysis procedures. The ratio estimates and the US Department of Agriculture data tables were used to generate food and nutrient information to provide the Remote Food Photography Method estimates. Equivalence testing using the two one-sided t tests approach was used to determine equivalence between the actual gram weights and the Remote Food Photography Method estimated weights for all samples, within each serving size, and within underprepared and overprepared bottles. For all bottles, the gram weights estimated by the Remote Food Photography Method were within 5% equivalence bounds with a slight underestimation of 0.05 g (90% CI -0.49 to 0.40; P<0.001) and mean percent error ranging between 0.32% and 1.58% among the four serving sizes. The maximum observed mean error was an overestimation of 1.58% of powdered formula by the Remote Food Photography Method under controlled laboratory conditions, indicating that the Remote Food Photography Method accurately estimated infant powdered formula. Copyright © 2016 Academy of Nutrition and Dietetics. Published by Elsevier Inc. All rights reserved.

Characterization of powdered fish heads for bone graft biomaterial applications.

PubMed

Oteyaka, Mustafa Ozgür; Unal, Hasan Hüseyin; Bilici, Namık; Taşçı, Eda

2013-01-01

The aim of this study was to define the chemical composition, morphology and crystallography of powdered fish heads of the species Argyrosomus regius for bone graft biomaterial applications. Two sizes of powder were prepared by different grinding methods; Powder A (coarse, d50=68.5 µm) and Powder B (fine, d50=19.1 µm). Samples were analyzed using X-ray diffraction (XRD), X-ray fluorescence (XRF), scanning electron microscopy (SEM), thermogravimetry (TG), and energy dispersive X-ray spectroscopy (EDS). The powder was mainly composed of aragonite (CaCO3) and calcite (CaCO3). The XRD pattern of Powder A and B matched standard aragonite and calcite patterns. In addition, the calcium oxide (CaO) phase was found after the calcination of Powder A. Thermogravimetry analysis confirmed total mass losses of 43.6% and 47.3% in Powders A and B, respectively. The microstructure of Powder A was mainly composed of different sizes and tubular shape, whereas Powder B showed agglomerated particles. The high quantity of CaO and other oxides resemble the chemical composition of bone. In general, the powder can be considered as bone graft after transformation to hydroxyapatite phase.

Monoclinic β-Li2TiO3 nanocrystalline particles employing novel urea assisted solid state route: Synthesis, characterization and sintering behavior

NASA Astrophysics Data System (ADS)

Tripathi, Biranchi M.; Mohanty, Trupti; Prakash, Deep; Tyagi, A. K.; Sinha, P. K.

2017-07-01

Pure phase monoclinic nano-crystalline Li2TiO3 powder was synthesized by a novel urea assisted solid state synthesis method using readily available and economical precursors. A single phase and well crystalline Li2TiO3 powder has been obtained at slightly lower temperature (600-700 °C) and shorter duration (2 h) as compared to the conventional solid state method. The proposed method has significant advantages in comparison to other viable methods mainly in terms of phase purity, powder properties and sinterability. Analysis of chemical composition using inductively coupled plasma atomic emission spectroscopy (ICP-AES) shows no loss of lithium from Li2TiO3 in the proposed method. The emergence of monoclinic Li2TiO3 phase was confirmed by X-ray diffraction (XRD) pattern of as-synthesized powder. The crystallite size of Li2TiO3 powder was calculated to be in the range of 15-80 nm, which varied as a function of urea composition and temperature. The morphology of as-prepared Li2TiO3 powders was examined by scanning electron microscope (SEM). The effect of urea composition on phase and morphology was investigated so as to delineate the role of urea. Upon sintering at < 1000 °C temperature, the Li2TiO3 powder compact attained about 98% of the theoretical density with fine grained (grain size: 2-3 μm) microstructure. It indicates excellent sinter-ability of Li2TiO3 powder synthesized by the proposed method. The fine grained structure is desirable for better tritium breeding performance of Li2TiO3. Electrochemical impedance spectroscopy at variable temperature showed good electrical properties of Li2TiO3. The proposed method is simple, anticipated to be cost effective and convenient to realise for large scale production of phase pure nanocrystalline and having significantly enhanced sinter-ability Li2TiO3 powder.

Preparation of bone samples in the Gliwice Radiocarbon Laboratory for AMS radiocarbon dating.

PubMed

Piotrowska, N; Goslar, T

2002-12-01

In the Gliwice Radiocarbon Laboratory, a system for preparation of samples for AMS dating has been built. At first it was used to produce graphite targets from plant macrofossils and sediments. In this study we extended its capabilities with the preparation of bones. We dealt with 3 methods; the first was the classical Longin method of collagen extraction, the second one included additional treatment of powdered bone in alkali solution, while in the third one carboxyl carbon was separated from amino acids obtained after hydrolysis of protein. The suitability of the methods was tested on 2 bone samples. Most of our samples gave ages > 40 kyr BP, suggesting good performance of the adapted methods, except for one sample prepared with simple Longin method. For routine preparation of bones we chose the Longin method with additional alkali treatment.

Synthesis and characterization of CoFe2O4/polyaniline nanocomposites for electromagnetic interference applications.

PubMed

Praveena, K; Srinath, S

2014-06-01

The Cobalt ferrite (CoFe2O4) powders were synthesized by Co-precipitation method. The as prepared ferrite powders were incorporated into a polyaniline matrix at various volumetric ratios. The as prepared composites of ferrite and polyaniline powders were characterized using X-ray diffraction (XRD), transmission electron microscope (TEM). The particle size of CoFe2O4 is found to be 20 nm. The saturation magnetization (M(s)) of all the composites was found to be decreasing with decrease of ferrite content, while coercivity (H(c)) remained at the value corresponding to pure cobalt ferrite nanopowders. The complex permittivity (epsilon' and epsilon") and permeability (mu' and mu") of composite samples were measured in the range of 1 MHz to 1.1 GHz. The value of epsilon' and mu' found to be increased with ferrite volume concentration.

Silica powders for powder evacuated thermal insulating panel and method

DOEpatents

Harris, Michael T.; Basaran, Osman A.; Kollie, Thomas G.; Weaver, Fred J.

1996-01-01

A powder evacuated thermal insulating panel using generally spherical and porous silica particles of a median size less than about 100 nanometers in diameter, a pour packing density of about 0.4 to 0.6 g/cm.sup.3 and an external surface area in the range of about 90 to 600 m.sup.2/ g is described. The silica powders are prepared by reacting a tetraakyl silicate with ammonia and water in an alcohol solvent, distilling the solution after the reaction to remove the ammonia and recover the alcohol. The resulting aqueous slurry was dried, ball-milled, and dried again to provide the silica particles with defined internal and external porosity. The nanometer size and the large external surface area of the silica particles along with the internal and external porosity of the silica particles provide powder evacuated thermal insulating panels with significantly higher R-values than obtainable using previously known silica powders.

Silica powders for powder evacuated thermal insulating panel and method

DOEpatents

Harris, Michael T.; Basaran, Osman A.; Kollie, Thomas G.; Weaver, Fred J.

1994-01-01

A powder evacuated thermal insulating panel using generally spherical and porous silica particles of a median size less than about 100 nanometers in diameter, a pour packing density of about 0.4 to 0.6 g/cm.sup.3 and an external surface area in the range of about 90 to 600 m.sup.2 /g is described. The silica powders are prepared by reacting a tetraakyl silicate with ammonia and water in an alcohol solvent, distilling the solution after the reaction to remove the ammonia and recover the alcohol. The resulting aqueous slurry was dried, ball-milled, and dried again to provide the silica particles with defined internal and external porosity. The nanometer size and the large external surface area of the silica particles along with the internal and external porosity of the silica particles provide powder evacuated thermal insulating panels with significantly higher R-values than obtainable using previously known silica powders.

Silica powders for powder evacuated thermal insulating panel and method

DOEpatents

Harris, Michael T.; Basaran, Osman A.; Kollie, Thomas G.; Weaver, Fred J.

1995-01-01

A powder evacuated thermal insulating panel using generally spherical and porous silica particles of a median size less than about 100 nanometers in diameter, a pour packing density of about 0.4 to 0.6 g/cm.sup.3 and an external surface area in the range of about 90 to 600 m.sup.2/ g is described. The silica powders are prepared by reacting a tetraakyl silicate with ammonia and water in an alcohol solvent, distilling the solution after the reaction to remove the ammonia and recover the alcohol. The resulting aqueous slurry was dried, ball-milled, and dried again to provide the silica particles with defined internal and external porosity. The nanometer size and the large external surface area of the silica particles along with the internal and external porosity of the silica particles provide powder evacuated thermal insulating panels with significantly higher R-values than obtainable using previously known silica powders.

Silica powders for powder evacuated thermal insulating panel and method

DOEpatents

Harris, M.T.; Basaran, O.A.; Kollie, T.G.; Weaver, F.J.

1996-01-02

A powder evacuated thermal insulating panel using generally spherical and porous silica particles of a median size less than about 100 nanometers in diameter, a pour packing density of about 0.4 to 0.6 g/cm{sup 3} and an external surface area in the range of about 90 to 600 m{sup 2}/g is described. The silica powders are prepared by reacting a tetraalkyl silicate with ammonia and water in an alcohol solvent, distilling the solution after the reaction to remove the ammonia and recover the alcohol. The resulting aqueous slurry was dried, ball-milled, and dried again to provide the silica particles with defined internal and external porosity. The nanometer size and the large external surface area of the silica particles along with the internal and external porosity of the silica particles provide powder evacuated thermal insulating panels with significantly higher R-values than obtainable using previously known silica powders. 2 figs.

Infrared-optical transmission and reflection measurements on loose powders

NASA Astrophysics Data System (ADS)

Kuhn, J.; Korder, S.; Arduini-Schuster, M. C.; Caps, R.; Fricke, J.

1993-09-01

A method is described to determine quantitatively the infrared-optical properties of loose powder beds via directional-hemispherical transmission and reflection measurements. Instead of the integration of the powders into a potassium bromide (KBr) or a paraffin oil matrix, which would drastically alter the scattering behavior, the powders are placed onto supporting layers of polyethylene (PE) and KBr. A commercial spectrometer is supplemented by an external optics, which enables measurements on horizontally arranged samples. For data evaluation we use a solution of the equation of radiative transfer in the 3-flux approximation under boundary conditions adapted to the PE or KBr/powder system. A comparison with Kubelka-Munk's theory and Schuster's 2-flux approximation is performed, which shows that 3-flux approximation yields results closest to the exact solution. Equations are developed, which correct transmission and reflection of the samples for the influence of the supporting layer and calculate the specific extinction and the albedo of the powder and thus enables us to separate scattering and absorption part of the extinction spectrum. Measurements on TiO2 powder are presented, which show the influence of preparation techniques and data evaluation with different methods to obtain the albedo. The specific extinction of various TiO2 powders is presented.

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.

A validated high performance thin layer chromatography method for determination of yohimbine hydrochloride in pharmaceutical preparations.

PubMed

Badr, Jihan M

2013-01-01

Yohimbine is an indole alkaloid used as a promising therapy for erectile dysfunction. A number of methods were reported for the analysis of yohimbine in the bark or in pharmaceutical preparations. In the present work, a simple and sensitive high performance thin layer chromatographic method is developed for determination of yohimbine (occurring as yohimbine hydrochloride) in pharmaceutical preparations and validated according to International Conference of Harmonization (ICH) guidelines. The method employed thin layer chromatography aluminum sheets precoated with silica gel as the stationary phase and the mobile phase consisted of chloroform:methanol:ammonia (97:3:0.2), which gave compact bands of yohimbine hydrochloride. Linear regression data for the calibration curves of standard yohimbine hydrochloride showed a good linear relationship over a concentration range of 80-1000 ng/spot with respect to the area and correlation coefficient (R(2)) was 0.9965. The method was evaluated regarding accuracy, precision, selectivity, and robustness. Limits of detection and quantitation were recorded as 5 and 40 ng/spot, respectively. The proposed method efficiently separated yohimbine hydrochloride from other components even in complex mixture containing powdered plants. The amount of yohimbine hydrochloride ranged from 2.3 to 5.2 mg/tablet or capsule in preparations containing the pure alkaloid, while it varied from zero (0) to 1.5-1.8 mg/capsule in dietary supplements containing powdered yohimbe bark. We concluded that this method employing high performance thin layer chromatography (HPTLC) in quantitative determination of yohimbine hydrochloride in pharmaceutical preparations is efficient, simple, accurate, and validated.

Preparation, Characterization and Performances of Powdered Polycarboxylate Superplasticizer with Bulk Polymerization.

PubMed

Liu, Xiao; Wang, Ziming; Zheng, Yunsheng; Cui, Suping; Lan, Mingzhang; Li, Huiqun; Zhu, Jie; Liang, Xu

2014-08-29

A polycarboxylate superplasticizer (PCE) was synthesized in a non-solvent system with bulk polymerization and then was pulverized into powdered form to achieve a rapid transportation and convenient preparation. PCE synthesized by using isopentenyl polyethylene glycol (TPEG) or isobutenyl polyethylene glycol (IPEG) as a macromonomer exhibited the best fluidities and retaining properties at 80 °C and 75 °C, respectively. Besides, azobisisobutyronitrile (AIBN) was suitable as an initiator, and the fumaric acid was suitable as the third monomer. The test results of ¹H nuclear magnetic resonance (¹H NMR) confirmed the occurrences of polymerization, and the measurement results of molecular weight and distribution showed that PCE molecular weight characteristics were in accordance with their fluidity properties in cement paste. The application performances in cement showed that PCEs with the best paste fluidity retentions had the longest final setting time and the shortest setting time interval, and the PCEs with good fluidity properties can obviously delay the hydration process and lower the hydration heat. Accordingly, this is a novel, energy-saving and economical method to prepare powdered PCE in the field of concrete admixtures.

Preparation, Characterization and Performances of Powdered Polycarboxylate Superplasticizer with Bulk Polymerization

PubMed Central

Liu, Xiao; Wang, Ziming; Zheng, Yunsheng; Cui, Suping; Lan, Mingzhang; Li, Huiqun; Zhu, Jie; Liang, Xu

2014-01-01

A polycarboxylate superplasticizer (PCE) was synthesized in a non-solvent system with bulk polymerization and then was pulverized into powdered form to achieve a rapid transportation and convenient preparation. PCE synthesized by using isopentenyl polyethylene glycol (TPEG) or isobutenyl polyethylene glycol (IPEG) as a macromonomer exhibited the best fluidities and retaining properties at 80 °C and 75 °C, respectively. Besides, azobisisobutyronitrile (AIBN) was suitable as an initiator, and the fumaric acid was suitable as the third monomer. The test results of 1H nuclear magnetic resonance (1H NMR) confirmed the occurrences of polymerization, and the measurement results of molecular weight and distribution showed that PCE molecular weight characteristics were in accordance with their fluidity properties in cement paste. The application performances in cement showed that PCEs with the best paste fluidity retentions had the longest final setting time and the shortest setting time interval, and the PCEs with good fluidity properties can obviously delay the hydration process and lower the hydration heat. Accordingly, this is a novel, energy-saving and economical method to prepare powdered PCE in the field of concrete admixtures. PMID:28788184

Preparation and optical characteristics of layered perovskite-type lead-bromide-incorporated azobenzene chromophores

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

Sasai, Ryo, E-mail: rsasai@riko.shimane-u.ac.jp; Shinomura, Hisashi

Lead bromide-based layered perovskite powders with azobenzene derivatives were prepared by a homogeneous precipitation method. From the diffuse reflectance (DR) and photoluminescence (PL) spectra of the hybrid powder materials, the present hybrids exhibited sharp absorption and PL peaks originating from excitons produced in the PbBr{sub 4}{sup 2-} layer. When the present hybrid powder was irradiated with UV light at 350 nm, the absorption band from the trans-azobenzene chromophore, observed around 350 nm, decreased, while the absorption band from the cis-azobenzene chromophore, observed around 450 nm, increased. These results indicate that azobenzene chromophores in the present hybrid materials exhibit reversible photoisomerization.more » Moreover, it was found that the PL intensity from the exciton also varied due to photoisomerization of the azobenzene chromophores in the present hybrid. Thus, for the first time we succeeded in preparing the azobenzene derivative lead-bromide-based layered perovskite with photochromism before and after UV light irradiation. - Graphical abstract: For the first time, we succeeded in preparing the azobenzene derivative lead-bromide-based layered perovskite with photochromism before and after UV light irradiation. Highlights: Black-Right-Pointing-Pointer PbBr-based layered perovskite with azobenezene derivatives could be synthesized by a homogeneous precipitation method. Black-Right-Pointing-Pointer Azobenzene derivatives incorporated the present hybrid that exhibited reversible photoisomerization under UV and/or visible light irradiation. Black-Right-Pointing-Pointer PL property of the present hybrid could also be varied by photoisomerization.« less

Influence of scanning system and dentist's level of training in the accuracy of digital impressions

NASA Astrophysics Data System (ADS)

Hategan, Simona; Gabor, Alin; Zaharia, Cristian; Sinescu, Cosmin; Negrutiu, Meda Lavinia; Jivanescu, Anca

2016-03-01

Background: The principal aim of our study was to evaluate digital impressions, taken with spray powder and powderfree scan systems, in order to determine the influence of the dentist's commitment to training as a critical factor regarding quality. Material and method: Two digital intraoral impression systems from the same manufacture (Sirona) : Apollo DI and CEREC Omnicam, were used to scan 16 crown preparations on teeth on a typodont maxillary model. Because an Apollo Di intraoral camera is a powder system, an adhesive was applied before using the powder spray. Three groups were used to scan the crown preparations in order to determine coating thickness homogeneity. One group consisted of senior year dental students, a second consisted of prosthodontics residents, and the third consisted of prosthodontics specialists. The same procedure was applied with a CEREC Omnicam intraoral camera, which is a powder-free system. By using the two systems software parameters we were able to determine the scanning precision. Results: Homogeneity scores for Apollo Di regarding the spray layer was significantly thinner for all dental surfaces in the first group, while the second group had thinner coatings for buccal and distal surfaces. For the third group, the crown preparations were coated more homogeneously than the first two groups. The powder-free system CEREC Omnicam can, to a degree, mask the lack of experience in direct optical impressions by avoiding the poor quality coating, which can lead to defective marginal adaptation of definitive restoration. Conclusions: The dentist's lack of experience can be mitigated, and partially avoided, by using powder-free systems. At the same time, the dentist can give more time towards learning how to integrate computerized fabricated restoration into the practice. The commitment to training is a critical factor in the successful integration of the technology. In addition, scanning marginal preparation details needs time in order to develop technical and manual skills.

[Preparation of freeze-dried powder of recombinate hirudin-2 nanoparticle for nasal delivery and permeability through nasal membrane in vitro].

PubMed

Chen, Ming-Xia; Zhang, Jian-Bao; Yu, Ji-Ping; Ye, Jing; Wei, Bao-Hong; Zhang, Yu-Jie

2013-06-01

To optimize the freeze-dried powder preparation technology of recombinate hirudin-2 (rHV2) nanoparticle which has bio-adhesive characteristic for nasal delivery, also to investigate its stability and permeability through nasal membrane in vitro. Taking the appearance, rediffusion of nanoparticle and rHV2 encapsulation efficiency as the evaluation indexes. Cryoprotector, the preparative technique and the effect of illumination and high temperature factors on its stability for rHV2 freeze-dried powder were investigated. Using Fraze diffusion cell technique, the permeability of rHV2 across rabbit nasal mucous membrane in chitosan solution, chitosan nanoparticle, and nanoparticle frozen-dried powder were compared with that in normal saline solution. The optimized preparation of rHV2 nanoparticle freeze-dried powder was as follows: 5% trehalose and glucose (1:1) was used as cryoprotector, nanoparticle solution was freezed for 24 h in vacuum frozen-dryer after being pre-freezed for 24 h. The content of rHV2 in the freeze-dried powder was 1.1 ug/mg. Illumination had little effect on the appearance, rediffusion and encapsulation efficiency of the rHV2 freeze-dried powder. High temperature could obviously influence the appearance of nanoparticle freeze-dried powder. The permeability coefficient (P) of nanoparticle was 5 times more than that in chictonson solution. It was indicated that chitosan nanoparticle has effect on increasing the permeability of rHV2. The freeze-dried powder of chitosan nanoparticle can be a good nasal preparation of rHV2.

Microencapsulation of Natural Anthocyanin from Purple Rosella Calyces by Freeze Drying

NASA Astrophysics Data System (ADS)

Nafiunisa, A.; Aryanti, N.; Wardhani, D. H.; Kumoro, A. C.

2017-11-01

Anthocyanin extract in powder form will improve its use since the powder is easier to store and more applicable. Microencapsulation method is introduced as an efficient way for protecting pigment such as anthocyanin. This research was aimed to characterise anthocyanin encapsulated products prepared from purple Roselle calyces by freeze drying. The liquid anthocyanin extracts from ultrasound-assisted extraction were freeze-dried with and without the addition of 10% w/w maltodextrins as a carrier and coating agents. The quality attributes of the powders were characterised by their colour intensity, water content, and solubility. Analysis of encapsulated material was performed for the powder added by maltodextrin. The stability of the microencapsulated pigment in solution form was determined for 11 days. Total anthocyanin content was observed through pH differential method. The results of the colour intensity analysis confirm that the product with maltodextrin addition has more intense colour with L* value of 29.69 a* value of 54.29 and b* value of 8.39. The result with the addition of maltodextrin has less moisture content and more soluble in water. It is verified that better results were obtained for powder with maltodextrin addition. Anthocyanin in the powder form with maltodextrin addition exhibits higher stability even after 11 days. In conclusion, the microencapsulation of anthocyanin with maltodextrin as a carrier and coating agent presented a potential method to produce anthocyanin powder from purple Roselle.

Synthesis and characterization of scandia ceria stabilized zirconia powders prepared by polymeric precursor method for integration into anode-supported solid oxide fuel cells

NASA Astrophysics Data System (ADS)

Tu, Hengyong; Liu, Xin; Yu, Qingchun

2011-03-01

Scandia ceria stabilized zirconia (10Sc1CeSZ) powders are synthesized by polymeric precursor method for use as the electrolyte of anode-supported solid oxide fuel cell (SOFC). The synthesized powders are characterized in terms of crystalline structure, particle shape and size distribution by X-ray diffraction (XRD), transmission electron microscopy (TEM) and photon correlation spectroscopy (PCS). 10Sc1CeSZ electrolyte films are deposited on green anode substrate by screen-printing method. Effects of 10Sc1CeSZ powder characteristics on sintered films are investigated regarding the integration process for application as the electrolytes in anode-supported SOFCs. It is found that the 10Sc1CeSZ films made from nano-sized powders with average size of 655 nm are very porous with many open pores. In comparison, the 10Sc1CeSZ films made from micron-sized powders with average size of 2.5 μm, which are obtained by calcination of nano-sized powders at higher temperatures, are much denser with a few closed pinholes. The cell performances are 911 mW cm-2 at the current density of 1.25 A cm-2 and 800 °C by application of Ce0.8Gd0.2O2 (CGO) barrier layer and La0.6Sr0.4CoO3 (LSC) cathode.

Preparation and Evaluation of Herbal Shampoo Powder

PubMed Central

Dubey, Sachin; Nema, Neelesh; Nayak, S.

2004-01-01

Two preparations of herbal shampoo powder were formulated using some common traditional drugs used by folk and traditional people of Bundelkhand region (M.P) India, for hair care. The preparations were formulated using bahera, amla, neem tulsi, shikakai henna & brahmi evaluated for organoleptic, powder charecterestics, foam test and physical evaluation. As the selected drugs being used since long time as single drug or in combination, present investigations will further help to establish a standard formulation and evaluation parameters, which will certainly help in the standardization for quality and purity of such type of herbal powder shampoos. PMID:22557149

Comparison of directly compressed vitamin B12 tablets prepared from micronized rotary-spun microfibers and cast films.

PubMed

Sebe, István; Bodai, Zsolt; Eke, Zsuzsanna; Kállai-Szabó, Barnabás; Szabó, Péter; Zelkó, Romána

2015-01-01

Fiber-based dosage forms are potential alternatives of conventional dosage forms from the point of the improved extent and rate of drug dissolution. Rotary-spun polymer fibers and cast films were prepared and micronized in order to direct compress after homogenization with tabletting excipients. Particle size distribution of powder mixtures of micronized fibers and films homogenized with tabletting excipients were determined by laser scattering particle size distribution analyzer. Powder rheological behavior of the mixtures containing micronized fibers and cast films was also compared. Positron annihilation lifetime spectroscopy was applied for the microstructural characterization of micronized fibers and films. The water-soluble vitamin B12 release from the compressed tablets was determined. It was confirmed that the rotary spinning method resulted in homogeneous supramolecularly ordered powder mixture, which was successfully compressed after homogenization with conventional tabletting excipients. The obtained directly compressed tablets showed uniform drug release of low variations. The results highlight the novel application of micronized rotary-spun fibers as intermediate for further processing reserving the original favorable powder characteristics of fibrous systems.

Method of preparing nuclear wastes for tansportation and interim storage

DOEpatents

Bandyopadhyay, Gautam; Galvin, Thomas M.

1984-01-01

Nuclear waste is formed into a substantially water-insoluble solid for temporary storage and transportation by mixing the calcined waste with at least 10 weight percent powdered anhydrous sodium silicate to form a mixture and subjecting the mixture to a high humidity environment for a period of time sufficient to form cementitious bonds by chemical reaction. The method is suitable for preparing an interim waste form from dried high level radioactive wastes.

Low temperature synthesis & characterization of lead-free BCZT ceramics using molten salt method

NASA Astrophysics Data System (ADS)

Jai Shree, K.; Chandrakala, E.; Das, Dibakar

2018-04-01

Piezoelectric properties are greatly influenced by the synthesis route, microstructure, stoichiometry of the chemical composition, purity of the starting materials. In this study, molten salt method was used to prepare lead-free BCZT ceramics. Molten salt method is one of the simplestmethods to prepare chemically-purified, single phase powders in high yield often at lower temperatures and shorten reaction time. Calcination of the molten salt synthesized powders resulted in asingle-phase perovskite structure at 1000 °C which is ˜ 350 °C less than the conventional solid-sate reaction method. With increasing calcination temperature the average template size was increased (˜ 0.5-2 µm). Formation of well dispersive templates improves the sinterability at lower temperatures. Lead-free BCZT ceramics sintered at 1500 °C for 2 h resulted in homogenous and highly dense microstructure with ˜92% of the theoretical density and a grain size of ˜ 35 µm. This highly dense microstructure could enhance the piezoelectric properties of the system.

Preparation of regenerable granular carbon nanotubes by a simple heating-filtration method for efficient removal of typical pharmaceuticals

NASA Astrophysics Data System (ADS)

Shan, Danna; Deng, Shubo; Zhao, Tianning; Yu, Gang; Winglee, Judith; Wiesner, Mark R.

2017-04-01

A simple and convenient method was used to prepare novel granular carbon nanotubes (CNTs) for enhanced adsorption of pharmaceuticals. By heating CNTs powder at 450 degree centigrade in air, followed by filtration, the obtained granular adsorbent exhibited high surface area and pore volume since the heating process produced some oxygen-containing functional groups on CNT surface, making CNTs more dispersible in the formation of granular cake. The porous granular CNTs not only had more available surfaces for adsorption but also were more easily separated from solution than pristine CNTs (p-CNTs) powder. This adsorbent exhibited relatively fast adsorption for carbamazepine (CBZ), tetracycline (TC) and diclofe- nac sodium (DS), and the maximum adsorption capacity on the granular CNTs was 369.5 μmol/g for CBZ, 284.2 μmol/g for TC and 203.1 μmol/g for DS according to the Langmuir fitting, increasing by 42.4%, 37.8% and 38.0% in comparison with the pristine CNTs powder. Moreover, the spent granular CNTs were successfully regenerated at 400 degree centigrade in air without decreasing the adsorption capacity in five regeneration cycles. The adsorbed CBZ and DS were completely degraded, while the adsorbed TC was partially oxidized and the residual was favorable for the subsequent adsorption. This research develops an easy method to prepare and regenerate granular CNT adsorbent for the enhanced removal of organic pollutants from water or wastewater.

Contamination Effects on Improving the Hydrogenation/Dehydrogenation Kinetics of Binary Magnesium Hydride/Titanium Carbide Systems Prepared by Reactive Ball Milling

PubMed Central

El-Eskandarany, M. Sherif; Shaban, Ehab

2015-01-01

Ultrafine MgH2 nanocrystalline powders were prepared by reactive ball milling of elemental Mg powders after 200 h of high-energy ball milling under a hydrogen gas pressure of 50 bar. The as-prepared metal hydride powders were contaminated with 2.2 wt. % of FeCr-stainless steel that was introduced to the powders upon using stainless steel milling tools made of the same alloy. The as-synthesized MgH2 was doped with previously prepared TiC nanopowders, which were contaminated with 2.4 wt. % FeCr (materials of the milling media), and then ball milled under hydrogen gas atmosphere for 50 h. The results related to the morphological examinations of the fabricated nanocomposite powders beyond the micro-and nano-levels showed excellent distributions of 5.2 wt. % TiC/4.6 wt. % FeCr dispersoids embedded into the fine host matrix of MgH2 powders. The as-fabricated nanocomposite MgH2/5.2 wt. % TiC/4.6 wt. % FeCr powders possessed superior hydrogenation/dehydrogenation characteristics, suggested by the low value of the activation energy (97.74 kJ/mol), and the short time required for achieving a complete absorption (6.6 min) and desorption (8.4 min) of 5.51 wt. % H2 at a moderate temperature of 275 °C under a hydrogen gas pressure ranging from 100 mbar to 8 bar. van’t Hoff approach was used to calculate the enthalpy (∆H) and entropy (∆S) of hydrogenation for MgH2, which was found to be −72.74 kJ/mol and 112.79 J/mol H2/K, respectively. Moreover, van’t Hoff method was employed to calculate the ΔH and ΔS of dehydrogenation, which was found to be 76.76 kJ/mol and 119.15 J/mol H2/K, respectively. This new nanocomposite system possessed excellent absorption/desorption cyclability of 696 complete cycles, achieved in a cyclic-life-time of 682 h. PMID:28793606

Semisolid Microstructural Evolution during Partial Remelting of a Bulk Alloy Prepared by Cold Pressing of the Ti-Al-2024Al Powder Mixture

PubMed Central

Qin, Yahong; Chen, Tijun; Wang, Yingjun; Zhang, Xuezheng; Li, Pubo

2016-01-01

A new method, powder thixoforming, has been proposed to fabricate an in situ Al3Tip/2024Al composite. During partial remelting, the microstructural evolution of the bulk alloy prepared by cold pressing of the Ti, Al, 2024Al powder mixture was investigated, and the formation mechanism of the Al3Ti particles produced by the reaction between the Ti powder and the Al alloy melt is also discussed in detail. The results indicate that the microstructural evolution of the 2024 alloy matrix can be divided into three stages: a rapid coarsening of the powder grains; a formation of primary α-Al particles surrounded with a continuous liquid film; and a slight coarsening of the primary α-Al particles. Simultaneously, a reaction layer of Al3Ti can be formed on the Ti powder surface when the bulk is heated for 10 min at 640 °C The thickness (X) of the reaction layer increases with the time according to the parabolic law of X=−0.43t2+4.21t+0.17. The stress generated in the reaction layer due to the volume dilatation can be calculated by using the equation σAl3Ti=−EAl3Ti6(1−υAl3Ti)t2Al3TitTi(1R−1R0). Comparing the obtained data with the results of the drip experiment, the reaction rate for the Ti powder and Al powder mixture is greater than that for the Ti plate and Al alloy mixture, respectively.

Self-propagating high-temperature synthesis and luminescent properties of ytterbium doped rare earth (Y, Sc, Lu) oxides nanopowders

NASA Astrophysics Data System (ADS)

Permin, D. A.; Novikova, A. V.; Balabanov, S. S.; Gavrishchuk, E. M.; Kurashkin, S. V.; Savikin, A. P.

2018-04-01

This paper describes a comparative study of structural and luminescent properties of 5%Yb-doped yttrium, scandium, and lutetium oxides (Yb:RE2O3) powders and ceramics fabricated by self-propagating high-temperature synthesis. According to X-ray diffractometry and electron microscopy the chosen method ensures preparation of low-agglomerated cubic Ctype crystal structured powders at one step. No crucial differences in luminescence spectra were found the Yb:RE2O3 powders and ceramics. It was shown that the emission lifetimes of the Yb:RE2O3 powders are lowered by crystal structure defects, while its values for ceramics samples are compared to that of monocrystals and more influenced by rare earth impurities.

High performance P-type thermoelectric materials and methods of preparation

NASA Technical Reports Server (NTRS)

Caillat, Thierry (Inventor); Borshchevsky, Alexander (Inventor); Fleurial, Jean-Pierre (Inventor)

2002-01-01

The present invention is embodied in high performance p-type thermoelectric materials having enhanced thermoelectric properties and the methods of preparing such materials. In one aspect of the invention, p-type semiconductors of formula Zn.sub.4-x A.sub.x Sb.sub.3-y B.sub.y wherein 0.ltoreq.x.ltoreq.4, A is a transition metal, B is a pnicogen, and 0.ltoreq.y.ltoreq.3 are formed for use in manufacturing thermoelectric devices with substantially enhanced operating characteristics and improved efficiency. Two methods of preparing p-type Zn.sub.4 Sb.sub.3 and related alloys of the present invention include a crystal growth method and a powder metallurgy method.

METHOD OF PREPARATION OF MATERIAL FOR NEUTRON BOMBARDMENT

DOEpatents

Ura, C.L.; Sisman, O.; Briggs, R.B.

1959-02-01

A method is presented for forming slugs or cartridges of sample material to be proeessed in a neutronic reactor. Aceording to this invention, the sample material is originally in the fcrm of powder. The powder is placed within a tube formed of a metallic foil. The material encased in the foil is then placed in a die and compressed under sufficient pressure to form a rigid cartridge. The cartridge is then sealed in a metallic can. As a result of this process, crumbling of the compact during handling is eliminated and it is not necessary to clean ana relubricate the die after compression of each cartridge. ~ A method is presented for producing small spherical shot-type pellets from ceramic or refractory materials. According to this process the material to be pelletized is first formed into a powder. The powdered material is then suspended in a liquid carrier or vehicle. Small drops of the suspension, produced by a capillary-drop apparatus, are deposited on the surfacc of a liquid repellent powder, which causes the drops to assume a spherical shape. The liquid is then evaporated from the spherical pellets and tbe pellets are collected and fired to produce the finished product.

Methods for producing monodispersed particles of barium titanate

DOEpatents

Hu, Zhong-Cheng

2001-01-01

The present invention is a low-temperature controlled method for producing high-quality, ultrafine monodispersed nanocrystalline microsphere powders of barium titanate and other pure or composite oxide materials having particles ranging from nanosized to micronsized particles. The method of the subject invention comprises a two-stage process. The first stage produces high quality monodispersed hydrous titania microsphere particles prepared by homogeneous precipitation via dielectric tuning in alcohol-water mixed solutions of inorganic salts. Titanium tetrachloride is used as an inorganic salt precursor material. The second stage converts the pure hydrous titania microsphere particles into crystalline barium titanate microsphere powders via low-temperature, hydrothermal reactions.

Effect of boric acid on the properties of Li{sub 2}MnO{sub 3}·LiNi{sub 0.5}Mn{sub 0.5}O{sub 2} composite cathode powders prepared by large-scale spray pyrolysis with droplet classifier

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

Hong, Young Jun; Choi, Seung Ho; Sim, Chul Min

2012-12-15

Graphical abstract: Display Omitted Highlights: ► Spherical shape Li{sub 2}MnO{sub 3}·LiNi{sub 0.5}Mn{sub 0.5}O{sub 2} composite cathode powders are prepared by large-scale spray pyrolysis with droplet classifier. ► Boric acid improves the morphological and electrochemical properties of the composite cathode powders. ► The discharge capacity of the composite cathode powders decreases from 217 to 196 mAh g{sup −1} by the 30th cycle. -- Abstract: Spherically shaped 0.3Li{sub 2}MnO{sub 3}·0.7LiNi{sub 0.5}Mn{sub 0.5}O{sub 2} composite cathode powders with filled morphology and narrow size distribution are prepared by large-scale spray pyrolysis. A droplet classification reduces the standard deviation of the size distribution of themore » composite cathode powders. Addition of boric acid improves the morphological properties of the product powders by forming a lithium borate glass material with low melting temperature. The optimum amount of boric acid dissolved in the spray solution is 0.8 wt% of the composite powders. The powders prepared from the spray solution with 0.8 wt% boric acid have a mixed layered crystal structure comprising Li{sub 2}MnO{sub 3} and LiNi{sub 0.5}Mn{sub 0.5}O{sub 2} phases, thus forming a composite compound. The initial charge and discharge capacities of the composite cathode powders prepared from the 0.8 wt% boric acid spray solution are 297 and 217 mAh g{sup −1}, respectively. The discharge capacity of the powders decreases from 217 to 196 mAh g{sup −1} by the 30th cycle, in which the capacity retention is 90%.« less

Synthesis of polycrystalline CoFe2O4 and NiFe2O4 powders by auto-combustion method using a novel amino-based gel

NASA Astrophysics Data System (ADS)

Jiang, Linwen; Yang, Shanshan; Zheng, Mengyao; Wu, Anhua; Chen, Hongbing

2017-12-01

Polycrystalline CoFe2O4/NiFe2O4 powders were prepared by auto-combustion method using a novel amino-based gel. The thermal evolution of gel precursors, as well as the microstructure, morphology and magnetic properties of as-synthesized powders were studied in detail. Energy dispersive x-ray spectroscopy indicated that the ratios of Ni:Fe was close to the theoretical value (Ni:Fe  =  1:2), suggesting high purity of synthesized NiFe2O4 powders. The saturated magnetization (M s) and residual magnetization (M r) of CoFe2O4 were highly dependent upon the annealed temperatures. The M s increased from 77.5 to 84.7 emu g-1, and M r increased from 37.7 emu g-1 to 42.5 emu g-1 by annealing from room temperature to 600 °C. The M s of NiFe2O4 was 38.7 emu g-1, much lower than that of CoFe2O4. The experimental results indicated that this auto-combustion method using amino-based gel was a suitable method for synthesizing high-quality CoFe2O4/NiFe2O4 powders.

Preparation of UO2, ThO2 and (Th,U)O2 pellets from photochemically-prepared nano-powders

NASA Astrophysics Data System (ADS)

Pavelková, Tereza; Čuba, Václav; de Visser-Týnová, Eva; Ekberg, Christian; Persson, Ingmar

2016-02-01

Photochemically-induced preparation of nano-powders of crystalline uranium and/or thorium oxides and their subsequent pelletizing has been investigated. The preparative method was based on the photochemically induced formation of amorphous solid precursors in aqueous solution containing uranyl and/or thorium nitrate and ammonium formate. The EXAFS analyses of the precursors shown that photon irradiation of thorium containing solutions yields a compound with little long-range order but likely "ThO2 like" and the irradiation of uranium containing solutions yields the mixture of U(IV) and U(VI) compounds. The U-containing precursors were carbon free, thus allowing direct heat treatment in reducing atmosphere without pre-treatment in the air. Subsequent heat treatment of amorphous solid precursors at 300-550 °C yielded nano-crystalline UO2, ThO2 or solid (Th,U)O2 solutions with high purity, well-developed crystals with linear crystallite size <15 nm. The prepared nano-powders of crystalline oxides were pelletized without any binder (pressure 500 MPa), the green pellets were subsequently sintered at 1300 °C under an Ar:H2 (20:1) mixture (UO2 and (Th,U)O2 pellets) or at 1600 °C in ambient air (ThO2 pellets). The theoretical density of the sintered pellets varied from 91 to 97%.

Spheroidization of glass powders for glass ionomer cements.

PubMed

Gu, Y W; Yap, A U J; Cheang, P; Kumar, R

2004-08-01

Commercial angular glass powders were spheroidized using both the flame spraying and inductively coupled radio frequency plasma spraying techniques. Spherical powders with different particle size distributions were obtained after spheroidization. The effects of spherical glass powders on the mechanical properties of glass ionomer cements (GICs) were investigated. Results showed that the particle size distribution of the glass powders had a significant influence on the mechanical properties of GICs. Powders with a bimodal particle size distribution ensured a high packing density of glass ionomer cements, giving relatively high mechanical properties of GICs. GICs prepared by flame-spheroidized powders showed low strength values due to the loss of fine particles during flame spraying, leading to a low packing density and few metal ions reacting with polyacrylic acid to form cross-linking. GICs prepared by the nano-sized powders showed low strength because of the low bulk density of the nano-sized powders and hence low powder/liquid ratio of GICs.

Preparation and handling of powdered infant formula: a commentary by the ESPGHAN Committee on Nutrition.

PubMed

Agostoni, Carlo; Axelsson, Irene; Goulet, Olivier; Koletzko, Berthold; Michaelsen, Kim F; Puntis, John W L; Rigo, Jacques; Shamir, Raanan; Szajewska, Hania; Turck, Dominique; Vandenplas, Yvan; Weaver, Lawrence T

2004-10-01

Powdered infant formulae are not sterile and may contain pathogenic bacteria. In addition, milk products are excellent media for bacterial proliferation. Multiplication of Enterobacter sakazakii in prepared formula feeds can cause devastating sepsis, particularly in the first 2 months of life. In approximately 50 published case reports of severe infection, there are high rates of meningitis, brain abscesses and necrotizing enterocolitis, with an overall mortality from 33% to 80%. Breast feeding provides effective protection against infection, one of the many reasons why it deserves continued promotion and support. To minimize the risk of infection in infants not fully breastfed, recommendations are made for preparation and handling of powdered formulae for children younger than 2 months of age. In the home setting, powdered infant formulae should be freshly prepared for each feed. Any milk remaining should be discarded rather than used in the following feed. Infant feeds should never be kept warm in bottle heaters or thermoses. In hospitals and other institutions written guidelines for preparation and handling of infant formulae should be established and their implementation monitored. If formula needs to be prepared in advance, it should be prepared on a daily basis and kept at 4 degrees C or below. Manufacturers of infant formulae should make every effort to minimize bacterial contamination of powdered products.

Preparation and characterization of Dendrobium officinale powders through superfine grinding.

PubMed

Meng, Qingran; Fan, Haoran; Chen, Feng; Xiao, Tiancun; Zhang, Lianfu

2018-03-01

Dendrobium officinale has been used in China for several thousand years as a health food and has become one of the most expensive tea materials worldwide as a result of extremely scarce resources in the wild and an increasing demand. Hence, it is very important to improve the depth and width of its application. In the present study, the physico-chemical, surface chemistry and thermal properties of micron range particles and coarse particles prepared by superfine grinding and shear pulverization were investigated. As the particle size decreased, the specific surface area of D. officinale powders increased significantly. Microscopy observations confirmed that superfine grinding effectively changed the original structure of D. officinale. The Fourier transform infrared spectroscopy spectra depicted the characteristic bands shifted in terms of absorbance and/or wave number as the powder particle size decreased. The crystallinity and intensity of the crystal peaks of D. officinale powders increased as the particle size decreased. Moisture sorption isotherms suggested that superfine powders were more unstable as a result of the increase in surface area, as well as the exposure of polar groups. The results of the present study suggest that superfine grinding may provide new methods of processing for D. officinale with respect to further enhancement of its application value. © 2017 Society of Chemical Industry. © 2017 Society of Chemical Industry.

Cryomilled and spark plasma sintered titanium: the evolution of microstructure

NASA Astrophysics Data System (ADS)

Kozlík, Jiří; Becker, Hanka; Harcuba, Petr; Stráský, Josef; Janeček, Milos

2017-05-01

Bulk ultra-fine grained (UFG) commercially pure Ti was prepared by cryogenic milling in liquid argon and subsequent spark plasma sintering (SPS). During cryogenic milling, individual powder particles are repetitively severely deformed by attrition forces. Powder particles were not significantly refined, but due to severe repetitive plastic deformation, ultra-fine grained microstructure emerges within each powder particle. Cryogenic milling can be therefore considered as a specific severe plastic deformation (SPD) method. Compactization of cryomilled powder by SPS technique (also referred to as field assisted sintering technique - FAST) requires significantly lower sintering temperatures and shorter sintering times for successful compaction when compared to any other sintering technique. This is crucial for maintaining the UFG microstructure due to its limited thermal stability. Several specimens were prepared by varying processing parameters, in particular the sintering temperature. The microstructure of powders and compacted samples was observed by scanning electron microscopy (SEM). Increased sintering temperature results in recrystallization and grain growth. A trade-off relationship between the density of compacted material and grain size was identified. Microhardness of the material was found to depend on residual porosity rather than grain size. This contribution presents cryogenic milling and spark plasma sintering as a viable alternative for achieving UFG microstructure in commercially pure Ti.

Effect of freeze-drying and self-ignition process on the microstructural and electrochemical properties of Li{sub 4}Ti{sub 5}O{sub 12}

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

Jamin, Claire; Traina, Karl; APTIS, Department of Physics, B5a, University of Liège, Sart-Tilman, 4000 Liège

2013-11-15

Graphical abstract: - Highlights: • Li{sub 4}Ti{sub 5}O{sub 12} is prepared by a method involving self-ignition of a freeze-dried gel. • Addition of NH{sub 4}NO{sub 3} modifies the self-ignition propagation mode. • Well-crystallized Li{sub 4}Ti{sub 5}O{sub 12} phase is obtained after only 2 h at 800 °C. • Li{sub 4}Ti{sub 5}O{sub 12} powder has 161 mAh g{sup −1} capacity and good retention at C/4 rate. - Abstract: Crystalline Li{sub 4}Ti{sub 5}O{sub 12} is synthesized by a method involving the freeze-drying and self-ignition of a gel prepared from titanium isopropoxide, lithium nitrate and hydroxypropylmethylcellulose (HPMC). This synthesis route yields crystalline Li{submore » 4}Ti{sub 5}O{sub 12} particles after calcination at 800 °C for 2 h. In an alternative route, addition of ammonium nitrate shifts the self-ignition mode from wave-like propagation to simultaneous. Powders with different microstructures are thereby obtained. Electrochemical characterization shows that the best results for Li{sup +} intercalation/desintercalation are obtained for the powder prepared without ammonium nitrate addition. These results highlight the necessity for a control of the self-ignition mode to obtain adequate properties.« less

Comparison of Reactive and Non-Reactive Spark Plasma Sintering Routes for the Fabrication of Monolithic and Composite Ultra High Temperature Ceramics (UHTC) Materials

PubMed Central

Orrù, Roberto; Cao, Giacomo

2013-01-01

A wider utilization of ultra high temperature ceramics (UHTC) materials strongly depends on the availability of efficient techniques for their fabrication as dense bodies. Based on recent results reported in the literature, it is possible to state that Spark Plasma Sintering (SPS) technology offers a useful contribution in this direction. Along these lines, the use of two different SPS-based processing routes for the preparation of massive UHTCs is examined in this work. One method, the so-called reactive SPS (R-SPS), consists of the synthesis and densification of the material in a single step. Alternatively, the ceramic powders are first synthesized by Self-propagating High-temperature Synthesis (SHS) and then sintered by SPS. The obtained results evidenced that R-SPS method is preferable for the preparation of dense monolithic products, while the sintering of SHS powders requires relatively milder conditions when considering binary composites. The different kinetic mechanisms involved during R-SPS of the monolithic and composite systems, i.e., combustion-like or gradual solid-diffusion, respectively, provides a possible explanation. An important role is also played by the SHS process, particularly for the preparation of composite powders, since stronger interfaces are established between the ceramic constituents formed in situ, thus favoring diffusion processes during the subsequent SPS step. PMID:28809229

Preparation of transparent conductors ferroelectric memory materials and ferrites

DOEpatents

Bhattacharya, Raghu Nath; Ginley, David S.

1998-01-01

A process for the preparation by electrodeposition of metal oxide film and powder compounds for ferroelectric memory materials and ferrites wherein the metal oxide includes a plurality of metals. The process comprises providing an electrodeposition bath, providing soluble salts of the metals to this bath, electrically energizing the bath to thereby cause formation of a recoverable film of metal on the electrode, recovering the resultant film as a film or a powder, and recovering powder formed on the floor of the bath. The films and powders so produced are subsequently annealed to thereby produce metal oxide for use in electronic applications. The process can be employed to produce metal-doped metal oxide film and powder compounds for transparent conductors. The process for preparation of these metal-doped metal oxides follows that described above.

FT-Raman and chemometric tools for rapid determination of quality parameters in milk powder: Classification of samples for the presence of lactose and fraud detection by addition of maltodextrin.

PubMed

Rodrigues Júnior, Paulo Henrique; de Sá Oliveira, Kamila; de Almeida, Carlos Eduardo Rocha; De Oliveira, Luiz Fernando Cappa; Stephani, Rodrigo; Pinto, Michele da Silva; de Carvalho, Antônio Fernandes; Perrone, Ítalo Tuler

2016-04-01

FT-Raman spectroscopy has been explored as a quick screening method to evaluate the presence of lactose and identify milk powder samples adulterated with maltodextrin (2.5-50% w/w). Raman measurements can easily differentiate samples of milk powder, without the need for sample preparation, while traditional quality control methods, including high performance liquid chromatography, are cumbersome and slow. FT-Raman spectra were obtained from samples of whole lactose and low-lactose milk powder, both without and with addition of maltodextrin. Differences were observed between the spectra involved in identifying samples with low lactose content, as well as adulterated samples. Exploratory data analysis using Raman spectroscopy and multivariate analysis was also developed to classify samples with PCA and PLS-DA. The PLS-DA models obtained allowed to correctly classify all samples. These results demonstrate the utility of FT-Raman spectroscopy in combination with chemometrics to infer about the quality of milk powder. Copyright © 2015 Elsevier Ltd. All rights reserved.

Engineered flux-pinning centers in BSCCO TBCCO and YBCO superconductors

DOEpatents

Goretta, Kenneth C.; Lanagan, Michael T.; Miller, Dean J.; Sengupta, Suvankar; Parker, John C.; Hu, Jieguang; Balachandran, Uthamalingam; Siegel, Richard W.; Shi, Donglu

1999-01-01

A method of preparing a high temperature superconductor. A method of preparing a superconductor includes providing a powdered high temperature superconductor and a nanophase material. These components are combined to form a solid compacted mass with the material disposed in the polycrystalline high temperature superconductor. This combined mixture is rapidly heated, forming a dispersion of nanophase size particles without a eutectic reaction. These nanophase particles can have a flat plate or columnar type morphology.

Abnormal variation of magnetic properties with Ce content in (PrNdCe)2Fe14B sintered magnets prepared by dual alloy method

NASA Astrophysics Data System (ADS)

Xue-Feng, Zhang; Jian-Ting, Lan; Zhu-Bai, Li; Yan-Li, Liu; Le-Le, Zhang; Yong-Feng, Li; Qian, Zhao

2016-05-01

Resource-saving (PrNdCe)2Fe14B sintered magnets with nominal composition (PrNd)15-x Ce x Fe77B8 (x = 0-10) were prepared using a dual alloy method by mixing (PrNd)5Ce10Fe77B8 with (PrNd)15Fe77B8 powders. For Ce atomic percent of 1% and 2%, coercivity decreases dramatically. With further increase of Ce atomic percent, the coercivity increases, peaks at 6.38 kOe in (PrNd)11Ce4Fe77B8, and then declines gradually. The abnormal dependence of coercivity is likely related to the inhomogeneity of rare earth chemical composition in the intergranular phase, where PrNd concentration is strongly dependent on the additive amount of (PrNd)5Ce10Fe77B8 powders. In addition, for Ce atomic percent of 8%, 7%, and 6% the coercivity is higher than that of magnets prepared by the conventional method, which shows the advantage of the dual alloy method in preparing high abundant rare earth magnets. Project supported by the National Natural Science Foundation of China (Grant Nos. 51461033, 51571126, 51541105, and 11547032), the Natural Science Foundation of Inner Mongolia, China (Grant No. 2013MS0110), and the Inner Mongolia University of Science and Technology Innovation Fund, China.

Phase quantification by X-ray photoemission valence band analysis applied to mixed phase TiO2 powders

NASA Astrophysics Data System (ADS)

Breeson, Andrew C.; Sankar, Gopinathan; Goh, Gregory K. L.; Palgrave, Robert G.

2017-11-01

A method of quantitative phase analysis using valence band X-ray photoelectron spectra is presented and applied to the analysis of TiO2 anatase-rutile mixtures. The valence band spectra of pure TiO2 polymorphs were measured, and these spectral shapes used to fit valence band spectra from mixed phase samples. Given the surface sensitive nature of the technique, this yields a surface phase fraction. Mixed phase samples were prepared from high and low surface area anatase and rutile powders. In the samples studied here, the surface phase fraction of anatase was found to be linearly correlated with photocatalytic activity of the mixed phase samples, even for samples with very different anatase and rutile surface areas. We apply this method to determine the surface phase fraction of P25 powder. This method may be applied to other systems where a surface phase fraction is an important characteristic.

FABRICATION OF NEUTRON SOURCES

DOEpatents

Birden, J.H.

1959-01-20

A method is presented for preparing a more efficient neutron source comprising inserting in a container a quantity of Po-210, inserting B powder coated with either Ag, Pt, or Ni. The container is sealed and then slowly heated to about 450 C to volatilize the Po and effect combination of the coated powder with the Po. The neutron flux emitted by the unit is moritored and the heating step is terminated when the flux reaches a maximum or selected level.

IR-doped ruthenium oxide catalyst for oxygen evolution

NASA Technical Reports Server (NTRS)

Valdez, Thomas I. (Inventor); Narayanan, Sekharipuram R. (Inventor)

2012-01-01

A method for preparing a metal-doped ruthenium oxide material by heating a mixture of a doping metal and a source of ruthenium under an inert atmosphere. In some embodiments, the doping metal is in the form of iridium black or lead powder, and the source of ruthenium is a powdered ruthenium oxide. An iridium-doped or lead-doped ruthenium oxide material can perform as an oxygen evolution catalyst and can be fabricated into electrodes for electrolysis cells.

Spectroscopic detection of exogenous materials in latent fingerprints treated with powders and lifted off with adhesive tapes.

PubMed

Banas, A; Banas, K; Breese, M B H; Loke, J; Lim, S K

2014-07-01

Fingerprint evidence offers great value to criminal investigations since it is an internationally recognized and established means of human identification. With recent advances in modern technology, scientists have started analyzing not only the ridge patterns of fingerprints but also substances which can be found within them. The aim of this work was to determine whether Fourier transform infrared (FTIR) spectromicroscopy could be used to detect contamination in a fingerprint which was dusted with powder (a technique already recognized as an effective and reliable method for developing latent fingerprints) and subsequently lifted off with adhesive tape. Explosive materials (pentaerythritol tetranitrate, C-4, TNT) and noncontrolled substances (sugar, aspirin) were used to prepare contaminated fingerprints on various substrates. Freshly deposited fingermarks with powders which were lifted off with adhesive tapes (provided by Singapore Police Force) were analyzed using a Bruker Hyperion 2000 microscope at the ISMI beamline (Singapore Synchrotron Light Source) with an attenuated total reflection objective. FTIR spectroscopy is a nondestructive technique which requires almost no sample preparation. Further, the fingerprint under analysis remains in pristine condition, allowing subsequent analysis if necessary. All analyzed substances were successfully distinguished using their FTIR spectra in powdered and lifted fingerprints. This method has the potential to significantly impact forensic science by greatly enhancing the information that can be obtained from the study of fingerprints.

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.

Processable Aromatic Polyimide Thermoplastic Blends

NASA Technical Reports Server (NTRS)

Baucom, Robert M; Johnston, Norman J.; St. Clair, Terry L.; Nelson, James B.; Gleason, John R.; Proctor, K. Mason

1988-01-01

Method developed for preparing readily-processable thermoplastic polyimides by blending linear, high-molecular-weight, polyimic acid solutions in ether solvents with ultrafine, semicrystalline, thermoplastic polyimide powders. Slurries formed used to make prepregs. Consolidation of prepregs into finsihed composites characterized by excellent melt flow during processing. Applied to film, fiber, fabric, metal, polymer, or composite surfaces. Used to make various stable slurries from which prepregs prepared.

Method of preparing a high solids content, low viscosity ceramic slurry

DOEpatents

Tiegs, Terry N.; Wittmer, Dale E.

1995-01-01

A method for producing a high solids content, low viscosity ceramic slurry composition comprises turbomilling a dispersion of a ceramic powder in a liquid to form a slurry having a viscosity less than 100 centipoise and a solids content equal to or greater than 48 volume percent.

Method of preparing a high solids content, low viscosity ceramic slurry

DOEpatents

Tiegs, T.N.; Wittmer, D.E.

1995-10-10

A method for producing a high solids content, low viscosity ceramic slurry composition comprises turbomilling a dispersion of a ceramic powder in a liquid to form a slurry having a viscosity less than 100 centipoise and a solids content equal to or greater than 48 volume percent.

Agarose encapsulated mesoporous carbonated hydroxyapatite nanocomposites powder for drug delivery.

PubMed

Kolanthai, Elayaraja; Abinaya Sindu, P; Thanigai Arul, K; Sarath Chandra, V; Manikandan, E; Narayana Kalkura, S

2017-01-01

The powder composites are predominantly used for filling of voids in bone and as drug delivery carrier to prevent the infection or inflammatory reaction in the damaged tissues. The objective of this work was to study the synthesis of agarose encapsulation on carbonated hydroxyapatite powder and their biological and drug delivery properties. Mesoporous, nanosized carbonated hydroxyapatite/agarose (CHAp/agarose) powder composites were prepared by solvothermal method and subsequently calcined to study the physico-chemical changes, if it subjected to thermal exposure. The phase of the as-synthesized powder was CHAp/agarose whereas the calcinated samples were non-stoichiometric HAp. The CHAp/agarose nanorods were of length 10-80nm and width 40-190nm for the samples synthesized at temperatures 120°C (ST120) and 150°C (ST150). The calcination process produced spheres (10-50nm) and rods with reduced size (40-120nm length and 20-30nm width). Composites were partially dissolved in SBF solution followed by exhibited better bioactivity than non-stoichiometric HAp confirmed by gravimetric method. Hemo and biocompatibility remained unaffected by presence of agarose or carbonate in the HAp. Specific surface area of the composites was high and exhibited an enhanced amoxicillin and 5-fluorouracil release than the calcined samples. The composites demonstrated a strong antimicrobial activity against E. coli, S. aureus and S. epidermidis. The ST120 showed prolonged drug (AMX and 5-Fcil) release and antimicrobial efficacy than ST150 and calcined samples. This technique would be simple and rapid for composites preparation, to produce high quality crystalline, resorbable, mesoporous and bioactive nanocomposite (CHAp/agarose) powders. This work provides new insight into the role of agarose coated on bioceramics by solvothermal technique and suggests that CHAp/agarose composites powders are promising materials for filling of void in bone and drug delivery applications. Copyright © 2016 Elsevier B.V. All rights reserved.

Photocatalytic activity of SnO{sub 2} nanoparticles in methylene blue degradation

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

Kim, Sung Phil; Choi, Myong Yong, E-mail: mychoi@gnu.ac.kr; Choi, Hyun Chul, E-mail: chc12@chonnam.ac.kr

2016-02-15

Highlights: • Nanosized SnO{sub 2} photocatalysts were prepared with a precipitation method. • SnO{sub 2} nanoparticles displayed high photocatalytic activities for the MB degradation. • OH radicals are the main active species in photocatalysis on the SnO{sub 2} nanoparticles. - Abstract: Nanosized SnO{sub 2} photocatalysts were prepared with a precipitation method and were characterized by performing transmission electron microscopy (TEM), powder X-ray diffraction (XRD), and X-ray absorption spectroscopy (XAS). The powder XRD results revealed that the SnO{sub 2} nanoparticles have a typical tetragonal rutile (cassiterite) structure and the average crystallite size was found to be approximately 4.5 nm by usingmore » the Debye–Scherrer equation. The prepared SnO{sub 2} nanoparticles consist of agglomerated particles with a mean diameter of around 4–5 nm according to the analysis of TEM images. The XAS data confirmed that the prepared samples have cassiterite structures with tin oxidation state of +4. The prepared SnO{sub 2} nanoparticles were found to exhibit approximately 3.8 times higher activity than bulk SnO{sub 2} in the photodegradation of methylene blue. On the basis of a trapping experiment, we developed a possible mechanism for the photodegradation on SnO{sub 2} nanoparticles.« less

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

PubMed

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

2012-06-01

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

Fabrication, characterization and fracture study of a machinable hydroxyapatite ceramic.

PubMed

Shareef, M Y; Messer, P F; van Noort, R

1993-01-01

In this study the preparation of a machinable hydroxyapatite from mixtures of a fine, submicrometer powder and either a coarse powder composed of porous aggregates up to 50 microns or a medium powder composed of dense particles of 3 microns median size is described. These were characterized using X-ray diffraction, transmission and scanning electron microscopy and infra-red spectroscopy. Test-pieces were formed by powder pressing and slip casting mixtures of various combinations of the fine, medium and coarse powders. The fired test-pieces were subjected to measurements of firing shrinkage, porosity, bulk density, tensile strength and fracture toughness. The microstructure and composition were examined using scanning electron microscopy and X-ray diffraction. For both processing methods, a uniform interconnected microporous structure was produced of a high-purity hydroxyapatite. The maximum tensile strength and fracture toughness that could be attained while retaining machinability were 37 MPa and 0.8 MPa m1/2 respectively.

Porous aerosil loading probucol using supercritical carbon dioxide: preparation, in vitro and in vivo characteristics.

PubMed

Chu, Chunxia; Liu, Muhua; Wang, Dongmei; Guan, Jibin; Cai, Cuifang; Sun, Yuanpeng; Zhang, Tianhong

2014-06-01

The aim of this study was to enhance the dissolution rate and oral bioavailability of probucol. Probucol was adsorbed onto aerosils via supercritical carbon dioxide (ScCO2) and the physicochemistry properties of probucol-aerosil powder were evaluated by differential scanning calorimetry, X-ray diffraction, infrared spectroscopy and scanning electron microscopy. Tablets of the probucol-aerosil powder were prepared by direct compression method. In the dissolution test, the probucol-aerosil tablets showed a significant enhanced dissolution rate compared with commercial tablets. Bioavailability study was carried out in beagle dogs. Probucol-aerosil tablets exhibited higher AUC and Cmax than commercial tablets. The improved dissolution and bioavailability of probucol-aerosil tablets were attributed to the amorphous state and good dispersion of probucol. It is a feasible method to enhance the oral bioavailability by adsorbing probucol onto aerosils via ScCO2.

Effect of heat treatment on the optical properties of perovskite BaZr0.5Ce0.3Y0.2O3-δ ceramic prepared by spark plasma sintering

NASA Astrophysics Data System (ADS)

Xing, Bohang; Cheng, Zhi; Wang, Cao; Zhao, Zhe

2017-09-01

The effect of heat treatment on the in-line transmittance of BaZr0.5Ce0.3Y0.2O3-δ (BZCY532) ceramics prepared by spark plasma sintering method was investigated. The loss of Ba in transparent BZCY532 ceramics is the key reason for the loss of transmittance during the annealing process. This problem can be effectively alleviated by using a powder bed of BZCY532. Heat treatment atmospheres, wet air and dry air, were also found to be critical for obtaining high quality transparent ceramics. A highly transparent BZCY532 ceramic with the in-line transmittance (Tin) of 71.4% at 2000 nm can be obtained by using SPS method followed by an annealing in powder bed at 1500 °C in wet air.

The preparation of BP single crystals by high pressure flux method

NASA Technical Reports Server (NTRS)

Kumashiro, Y.; Misawa, S.; Gonda, S.

1984-01-01

Single crystals of BP, a III-V compound semiconductor, were obtained by the high pressure flux method. Cu3P and Ni12P5 powders were used as the flux, and mixed with BP powder. Two kinds of mixtures were prepared: (1) 1.8g (BP) + 35 G (Cu3P) and (2) 1.7 g (BP) + 25 g (Ni12P5). They were compressed into pellets, heated at 1300 C for 24 h in an induction furnace under a pressure of 1 MPa using Ar-P2 gas, and slowly cooled to room temperature. In case (1), BP single crystals grew along the (III) plane, and in case (2) they grew as an aggregate of crystallites. The cathodoluminescence spectra of the synthetic BP crystals showed peaks near 680 nm (1.82 eV) for case (1), and 500 nm (2.47 eV) for case (2). By using the high pressure flux method conventional sized crystals were obtained in a relatively short time.

Structural, morphological and dielectric properties of BiNbO{sub 4} ceramics prepared by the sol-gel method

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

Devesa, S.; Graça, M.P.; Costa, L.C., E-mail: kady@ua.pt

2016-06-15

Highlights: • The thermal treatment at 1200 °C generates a non-stoichiometric secondary phase. • The secondary phase Bi{sub 3.54}Nb{sub 7.09}O{sub 22.7}, is responsible for the highest Q × f and density. • The samples with triclinic BiNbO{sub 4} have the highest ε′. - Abstract: BiNbO{sub 4} ceramic powders were prepared using the sol-gel method. The fine particles were pressed into cylinders and, then, they were treated at temperatures between 500 and 1150 °C. The structure was studied by X-ray diffraction and Raman spectroscopy and the morphology was observed by scanning electron microscopy. The measurements of the complex permittivity were mademore » in a resonant cavity operating at 2.7 GHz, using the small perturbation method. The reversible phase transformation between β-BiNbO{sub 4} and α-BiNbO{sub 4} was observed. The density, dielectric constant (ε') and the dielectric loss (tg δ) of the prepared powders increase with the sintering temperature, and the sample treated at 1150 °C shows the highest ε' and the highest Q × f.« less

Solid state neutron detector and method for use

DOEpatents

Doty, F. Patrick; Zwieback, Ilya; Ruderman, Warren

2002-01-01

Crystals of lithium tetraborate or alpha-barium borate had been found to be neutron detecting materials. The crystals are prepared using known crystal growing techniques, wherein the process does not include the common practice of using a fluxing agent, such as sodium oxide or sodium fluoride, to reduce the melting temperature of the crystalline compound. Crystals prepared by this method can be sliced into thin single or polycrystalline wafers, or ground to a powder and prepared as a sintered compact or a print paste, and then configured with appropriate electronic hardware, in order to function as neutron detectors.

Improved sample preparation to determine acrylamide in difficult matrixes such as chocolate powder, cocoa, and coffee by liquid chromatography tandem mass spectroscopy.

PubMed

Delatour, Thierry; Périsset, Adrienne; Goldmann, Till; Riediker, Sonja; Stadler, Richard H

2004-07-28

An improved sample preparation (extraction and cleanup) is presented that enables the quantification of low levels of acrylamide in difficult matrixes, including soluble chocolate powder, cocoa, coffee, and coffee surrogate. Final analysis is done by isotope-dilution liquid chromatography-electrospray ionization tandem mass spectrometry (LC-MS/MS) using d3-acrylamide as internal standard. Sample pretreatment essentially encompasses (a) protein precipitation with Carrez I and II solutions, (b) extraction of the analyte into ethyl acetate, and (c) solid-phase extraction on a Multimode cartridge. The stability of acrylamide in final extracts and in certain commercial foods and beverages is also reported. This approach provided good performance in terms of linearity, accuracy and precision. Full validation was conducted in soluble chocolate powder, achieving a decision limit (CCalpha) and detection capability (CCbeta) of 9.2 and 12.5 microg/kg, respectively. The method was extended to the analysis of acrylamide in various foodstuffs such as mashed potatoes, crisp bread, and butter biscuit and cookies. Furthermore, the accuracy of the method is demonstrated by the results obtained in three inter-laboratory proficiency tests. Copyright 2004 American Chemical Society

METHOD FOR PREPARING URANIUM MONOCARBIDE-PLUTONIUM MONOCARBIDE SOLID SOLUTION

DOEpatents

Ogard, A.E.; Leary, J.A.; Maraman, W.J.

1963-03-19

A method is given for preparing solid solutions of uranium monocarbide- plutonium monocarbide. In this method, the powder form of uranium dioxide, plutonium dioxide, and graphite are mixed in a ratio determined by the equation: xUO/sub 2/ + yPuO/sub 2/ + (2+z)C yields UxPu/sub y/C/sub z/ +2CO, where x + y equ al 1.0 and z is greater than 0.9 but less than 1.0. The resulting mixture is compacted and heated in a vacuum at a temperature of 1850 deg C. (AEC)

The importance of the solids loading on confirming the dielectric nanosize dependence of BaTiO₃ powders by slurry method.

PubMed

Zhou, Wei; Nie, Yi Mei; Li, Shu Jing; Liang, Hai Yan

2013-01-01

The dielectric nanosize dependence of BaTiO₃ powders was investigated by the slurry method, where two series of BaTiO₃ slurries with 10 vol% and 30 vol% solids loadings were prepared as model samples. Applying the Bruggeman-Hanai equation, the high-frequency limiting permittivity (ε(h)) of the slurries was extracted from the dielectric spectra. The ε(h) of the 10 vol% slurry showed abnormal size independence in the range from 100 nm to 700 nm, and the ε(h) of the 30 vol% slurry exhibited good agreement with the previous prediction. Through analysing quantitatively the response of ε(h) to the changing permittivity of the powders under different solids loading, it was found that the ε h of the slurry with lower solids loading is more inclined to be interfered by the systematic and random errors. Furthermore, a high permittivity value was found in the BaTiO₃ powders with 50 nm particle size.

Preparation of transparent conductors ferroelectric memory materials and ferrites

DOEpatents

Bhattacharya, R.N.; Ginley, D.S.

1998-07-28

A process is described for the preparation by electrodeposition of metal oxide film and powder compounds for ferroelectric memory materials and ferrites wherein the metal oxide includes a plurality of metals. The process comprises providing an electrodeposition bath, providing soluble salts of the metals to this bath, electrically energizing the bath to thereby cause formation of a recoverable film of metal on the electrode, recovering the resultant film as a film or a powder, and recovering powder formed on the floor of the bath. The films and powders so produced are subsequently annealed to thereby produce metal oxide for use in electronic applications. The process can be employed to produce metal-doped metal oxide film and powder compounds for transparent conductors. The process for preparation of these metal-doped metal oxides follows that described above.

Preparation, characterizations and photocatalytic activity of a ZnO/TiO2 nanocomposite

NASA Astrophysics Data System (ADS)

Lachom, Vichuda; Poolcharuansin, Phitsanu; Laokul, Paveena

2017-03-01

Nanoparticles of TiO2, ZnO and nanocomposite ZnO/TiO2 were prepared via a co-precipitation method. The precursor powders were calcined in air at 400 and 500 °C for 2 h. Crystallite sizes of the calcined samples ranged from 11-43 nm. The XRD patterns of ZnO/TiO2 powder showed two phases of anatase and wurtzite, with no ZnTiO3 impurity phase. TEM images showed three types of particles in the ZnO/TiO2 samples: a fine particle type of TiO2 and submicron ellipsoidal and rod-like particles of ZnO. The energy gap (E g) of the calcined powders was evaluated using UV-vis absorption spectra and found to be in the range of 3.15-3.60 eV. Photodegradation efficiencies of the prepared samples in methyl orange aqueous solution were investigated under UVA irradiation. The results showed that nanocomposite ZnO/TiO2 calcined at 400 °C exhibited the highest apparent rate constant (k), and a higher capacity for methyl orange removal than TiO2 and ZnO nanoparticles.

Porous-electrode preparation method

DOEpatents

Arons, R.M.; Dusek, J.T.

1981-09-17

A porous sintered plaque is provided with a bimodal porosity that is especially well suited for use as an electrode within a molten carbonate fuel cell. The coarse porosity is sufficient for admitting gases into contact with the reaction surfaces while the fine porosity is wetted with and retains molten electrolyte on the reaction sites. The electrode structure is prepared by providing a very fine powder such as nickel oxide and blending the powder with a suitable decomposable binder to form a solid mass. The mass is comminuted into agglomerate size particles substantially larger than the fine oxide particles and formed into a cohesive compact for subsequent sintering. Sintering is carried out at sufficient conditions to bind the agglomerates together into a porous structure having both coarse and fine porosity. Where lithiated nickel oxide cathodes are prepared, the sintering conditions can be moderate enough to retain substantial quantities of lithium within the electrode for adequate conductivity.

Porous electrode preparation method

DOEpatents

Arons, Richard M.; Dusek, Joseph T.

1983-01-01

A porous sintered plaque is provided with a bimodal porosity that is especially well suited for use as an electrode within a molten carbonate fuel cell. The coarse porosity is sufficient for admitting gases into contact with the reaction surfaces while the fine porosity is wetted with and retains molten electrolyte on the reaction sites. The electrode structure is prepared by providing a very fine powder of such as nickel oxide and blending the powder with a suitable decomposable binder to form a solid mass. The mass is comminuted into agglomerate size particles substantially larger than the fine oxide particles and formed into a cohesive compact for subsequent sintering. Sintering is carried out at sufficient conditions to bind the agglomerates together into a porous structure having both coarse and fine porosity. Where lithiated nickel oxide cathodes are prepared, the sintering conditions can be moderate enough to retain substantial quantities of lithium within the electrode for adequate conductivity.

Method of preparing thermal insulation for high temperature microwave sintering operations

DOEpatents

Holcombe, Cressie E.; Dykes, Norman L.; Morrow, Marvin S.

1996-01-01

Superior microwave transparent thermal insulations for high temperature microwave sintering operations were prepared. One embodiment of the thermal insulation comprises granules of boron nitride coated with a very thin layer of glassy carbon made by preparing a glassy carbon precursor and blending it with boron nitride powder to form a mixture. The blended mixture is granulated to form a grit which is dried and heated to form the granules of boron nitride coated with a glassy carbon. Alternatively, grains of glassy carbon are coated with boron nitride by blending a mixture of a slurry comprising boron nitride, boric acid binder, and methyl alcohol with glassy carbon grains to form a blended mixture. The blended mixture is dried to form grains of glassy carbon coated with boron nitride. In addition, a physical mixture of boron nitride powder and glassy carbon grains has also been shown to be an excellent thermal insulation material for microwave processing and sintering.

Porous electrode preparation method

DOEpatents

Arons, R.M.; Dusek, J.T.

1983-10-18

A porous sintered plaque is provided with a bimodal porosity that is especially well suited for use as an electrode within a molten carbonate fuel cell. The coarse porosity is sufficient for admitting gases into contact with the reaction surfaces while the fine porosity is wetted with and retains molten electrolyte on the reaction sites. The electrode structure is prepared by providing a very fine powder of such as nickel oxide and blending the powder with a suitable decomposable binder to form a solid mass. The mass is comminuted into agglomerate size particles substantially larger than the fine oxide particles and formed into a cohesive compact for subsequent sintering. Sintering is carried out at sufficient conditions to bind the agglomerates together into a porous structure having both coarse and fine porosity. Where lithiated nickel oxide cathodes are prepared, the sintering conditions can be moderate enough to retain substantial quantities of lithium within the electrode for adequate conductivity. 2 figs.

Synthesis of fine-grained .alpha.-silicon nitride by a combustion process

DOEpatents

Holt, J. Birch; Kingman, Donald D.; Bianchini, Gregory M.

1990-01-01

A combustion synthesis process for the preparation of .alpha.-silicon nitride and composites thereof is disclosed. Preparation of the .alpha.-silicon nitride comprises the steps of dry mixing silicon powder with an alkali metal azide, such as sodium azide, cold-pressing the mixture into any desired shape, or loading the mixture into a fused, quartz crucible, loading the crucible into a combustion chamber, pressurizing the chamber with nitrogen and igniting the mixture using an igniter pellet. The method for the preparation of the composites comprises dry mixing silicon powder (Si) or SiO.sub.2, with a metal or metal oxide, adding a small amount of an alkali metal azide such as sodium azide, introducing the mixture into a suitable combustion chamber, pressurizing the combustion chamber with nitrogen, igniting the mixture within the combustion chamber, and isolating the .alpha.-silicon nitride formed as a reaction product.

Synthesis of structured lipid enriched with omega fatty acids and sn-2 palmitic acid by enzymatic esterification and its incorporation in powdered infant formula.

PubMed

Nagachinta, Supakana; Akoh, Casimir C

2013-05-08

Structured lipid (SL) enriched with arachidonic (ARA) and docosahexaenoic (DHA) acids was produced from tripalmitin using Lipozyme TL IM. The effects of acyl donors, that is, free fatty acids vs fatty acid ethyl esters, on the reactions were compared. The highest total incorporation of ARA and DHA was obtained when the reaction continued for 24 h, at a substrate mole ratio of 9, using free fatty acids as acyl donors (acidolysis). The SL prepared by a large-scale acidolysis reaction contained 17.69 ± 0.09% total ARA, 10.75 ± 0.15% total DHA, and 48.53 ± 1.40% sn-2 palmitic acid. SL thermograms exhibited multiple peaks indicating complexity of the triacylglycerol (TAG) distribution. RP-HPLC analysis of SL revealed nine of 26 TAG molecular species that were similar to those of human milk fat. Powdered infant formulas containing the SL were prepared by wet-mixing/spray-drying and dry-blending methods. Formula prepared with microencapsulated SL and the dry-blending method had better oxidative stability and color quality.

Engineered flux-pinning centers in BSCCO TBCCO and YBCO superconductors

DOEpatents

Goretta, K.C.; Lanagan, M.T.; Miller, D.J.; Sengupta, S.; Parker, J.C.; Hu, J.; Balachandran, U.; Siegel, R.W.; Shi, D.

1999-07-27

A method of preparing a high temperature superconductor is disclosed. A method of preparing a superconductor includes providing a powdered high temperature superconductor and a nanophase material. These components are combined to form a solid compacted mass with the material disposed in the polycrystalline high temperature superconductor. This combined mixture is rapidly heated, forming a dispersion of nanophase size particles without a eutectic reaction. These nanophase particles can have a flat plate or columnar type morphology. 4 figs.

A novel in situ synthesis of SiBCN-Zr composites prepared by a sol-gel process and spark plasma sintering.

PubMed

Miao, Yang; Yang, Zhihua; Liang, Bin; Li, Quan; Chen, Qingqing; Jia, Dechang; Cheng, Yi-Bing; Zhou, Yu

2016-08-09

In the work reported here, SiBCN amorphous powders were first prepared by a mechanical alloying technique, employing cubic silicon, graphite and hexagonal boron nitride powders as raw materials. Zirconia was then introduced via sol-gel methods. The resulting powder composite was then consolidated via SPS sintering. The SPS sintering sample was evaluated using XRD, SEM and TEM. XRD reveals a chemical transformation wherein amorphous BN(C) and ZrO2 form the primary ZrC and ZrB2 phases after SPS processing along with SiC and BN(C). Thereafter ZrC reacts with BN(C) completely to form ZrB2. The reaction starts at the temperature of 1500 °C and is complete at the temperature of 1900 °C. The fracture toughness of the sintered composites reaches 4.9 ± 0.2 MPa m(1/2) due to the presence of the laminated structure of the BN(C) phase.

Investigation of optimal route to fabricate submicron-sized Sm{sub 2}Fe{sub 17} particles with reduction-diffusion method

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

Okada, Shusuke, E-mail: shusuke-okada@aist.go.jp; Takagi, Kenta; Ozaki, Kimihiro

Submicron-sized Sm{sub 2}Fe{sub 17} powder samples were fabricated by a non-pulverizing process through reduction-diffusion of precursors prepared by a wet-chemical technique. Three precursors having different morphologies, which were micron-sized porous Sm-Fe oxide-impregnated iron nitrate, acicular goethite impregnated-samarium nitrate, and a conventional Sm-Fe coprecipitate, were prepared and subjected to hydrogen reduction and reduction-diffusion treatment to clarify whether these precursors could be convert to Sm{sub 2}Fe{sub 17} without impurity phases and which precursor is the most attractive for producing submicron-sized Sm{sub 2}Fe{sub 17} powder. As a result, all three precursors were successfully converted to Sm{sub 2}Fe{sub 17} powders without impurity phases, andmore » the synthesis route using iron-oxide particle-impregnated samarium oxide was revealed to have the greatest potential among the three routes.« less

Influence of the pressure applied to make LATP pellets

NASA Astrophysics Data System (ADS)

Lu, Xiaojuan

2018-02-01

NASICON structured Li1+xAlxTi2-x(PO4)3 (0.1≤x≤0.7) powders were prepared by hydrothermal synthesis method and the pressure applied to press the powders into pellets was investigated in this study. The conductivity was measured by an impedance analyzer and the microstructures were examined by SEM. The variation trend with Al amount was almost identical for LATP pressed at high pressure and low pressure. Both the total conductivities of LATP prepared at high pressures and low pressures peaked at x=0.6. The conductivities of LATP pressed at high pressures were all higher than those at low pressures. The reason was mainly attributed to the denser microstructures achieved at higher pressure.

Method for fabricating beryllium structures

DOEpatents

Hovis, Jr., Victor M.; Northcutt, Jr., Walter G.

1977-01-01

Thin-walled beryllium structures are prepared by plasma spraying a mixture of beryllium powder and about 2500 to 4000 ppm silicon powder onto a suitable substrate, removing the plasma-sprayed body from the substrate and placing it in a sizing die having a coefficient of thermal expansion similar to that of the beryllium, exposing the plasma-sprayed body to a moist atmosphere, outgassing the plasma-sprayed body, and then sintering the plasma-sprayed body in an inert atmosphere to form a dense, low-porosity beryllium structure of the desired thin-wall configuration. The addition of the silicon and the exposure of the plasma-sprayed body to the moist atmosphere greatly facilitate the preparation of the beryllium structure while minimizing the heretofore deleterious problems due to grain growth and grain orientation.

Calcination and solid state reaction of ceramic-forming components to provide single-phase superconducting materials having fine particle size

DOEpatents

Balachandran, Uthamalingam; Poeppel, Roger B.; Emerson, James E.; Johnson, Stanley A.

1992-01-01

An improved method for the preparation of single phase, fine grained ceramic materials from precursor powder mixtures where at least one of the components of the mixture is an alkali earth carbonate. The process consists of heating the precursor powders in a partial vacuum under flowing oxygen and under conditions where the partial pressure of CO.sub.2 evolved during the calcination is kept to a very low level relative to the oxygen. The process has been found particularly suitable for the preparation of high temperature copper oxide superconducting materials such as YBa.sub.2 Cu.sub.3 O.sub.x "123" and YBa.sub.2 Cu.sub.4 O.sub.8 "124".

Bulk synthesis of nanoporous palladium and platinum powders

DOEpatents

Robinson, David B [Fremont, CA; Fares, Stephen J [Pleasanton, CA; Tran, Kim L [Livermore, CA; Langham, Mary E [Pleasanton, CA

2012-04-17

Disclosed is a method for providing nanoporous palladium and platinum powders. These materials were synthesized on milligram to gram scales by chemical reduction of tetrahalo-complexes with ascorbate in a concentrated aqueous surfactant at temperatures between -20.degree. C. and 30.degree. C. The prepared particles have diameters of approximately 50 nm, wherein each particle is perforated by pores having diameters of approximately 3 nm, as determined by electron tomography. These materials are of potential value for hydrogen and electrical charge storage applications.

Bulk synthesis of nanoporous palladium and platinum powders

DOEpatents

Robinson, David B; Fares, Stephen J; Tran, Kim L; Langham, Mary E

2014-04-15

Disclosed is a method for providing nanoporous palladium and platinum powders. These materials were synthesized on milligram to gram scales by chemical reduction of tetrahalo-complexes with ascorbate in a concentrated aqueous surfactant at temperatures between -20.degree. C. and 30.degree. C. The prepared particles have diameters of approximately 50 nm, wherein each particle is perforated by pores having diameters of approximately 3 nm, as determined by electron tomography. These materials are of potential value for hydrogen and electrical charge storage applications.

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.

Preparation of ultra-fine powders from polysaccharide-coated solid lipid nanoparticles and nanostructured lipid carriers by innovative nano spray drying technology.

PubMed

Wang, Taoran; Hu, Qiaobin; Zhou, Mingyong; Xue, Jingyi; Luo, Yangchao

2016-09-10

In this study, five polysaccharides were applied as natural polymeric coating materials to prepare solid lipid nanoparticles (SLN) and nanostructure lipid carriers (NLC), and then the obtained lipid colloidal particles were transformed to solid powders by the innovative nano spray drying technology. The feasibility and suitability of this new technology to generate ultra-fine lipid powder particles were evaluated and the formulation was optimized. The spray dried SLN powder exhibited the aggregated and irregular shape and dimension, but small, uniform, well-separated spherical powder particles of was obtained from NLC. The optimal formulation of NLC was prepared by a 20-30% oleic acid content with carrageenan or pectin as coating material. Therefore, nano spray drying technology has a potential application to produce uniform, spherical, and sub-microscale lipid powder particles when the formulation of lipid delivery system is appropriately designed. Copyright © 2016 Elsevier B.V. All rights reserved.

Preparation of molecularly imprinted polymers for strychnine by precipitation polymerization and multistep swelling and polymerization and their application for the selective extraction of strychnine from nux-vomica extract powder.

PubMed

Nakamura, Yukari; Matsunaga, Hisami; Haginaka, Jun

2016-04-01

Monodisperse molecularly imprinted polymers for strychnine were prepared by precipitation polymerization and multistep swelling and polymerization, respectively. In precipitation polymerization, methacrylic acid and divinylbenzene were used as a functional monomer and crosslinker, respectively, while in multistep swelling and polymerization, methacrylic acid and ethylene glycol dimethacrylate were used as a functional monomer and crosslinker, respectively. The retention and molecular recognition properties of the molecularly imprinted polymers prepared by both methods for strychnine were evaluated using a mixture of sodium phosphate buffer and acetonitrile as a mobile phase by liquid chromatography. In addition to shape recognition, ionic and hydrophobic interactions could affect the retention of strychnine in low acetonitrile content. Furthermore, molecularly imprinted polymers prepared by both methods could selectively recognize strychnine among solutes tested. The retention factors and imprinting factors of strychnine on the molecularly imprinted polymer prepared by precipitation polymerization were 220 and 58, respectively, using 20 mM sodium phosphate buffer (pH 6.0)/acetonitrile (50:50, v/v) as a mobile phase, and those on the molecularly imprinted polymer prepared by multistep swelling and polymerization were 73 and 4.5. These results indicate that precipitation polymerization is suitable for the preparation of a molecularly imprinted polymer for strychnine. Furthermore, the molecularly imprinted polymer could be successfully applied for selective extraction of strychnine in nux-vomica extract powder. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Influence of Ultrafine 2CaO·SiO₂ Powder on Hydration Properties of Reactive Powder Concrete.

PubMed

Sun, Hongfang; Li, Zishanshan; Memon, Shazim Ali; Zhang, Qiwu; Wang, Yaocheng; Liu, Bing; Xu, Weiting; Xing, Feng

2015-09-17

In this research, we assessed the influence of an ultrafine 2CaO·SiO₂ powder on the hydration properties of a reactive powder concrete system. The ultrafine powder was manufactured through chemical combustion method. The morphology of ultrafine powder and the development of hydration products in the cement paste prepared with ultrafine powder were investigated by scanning electron microscopy (SEM), mineralogical composition were determined by X-ray diffraction, while the heat release characteristics up to the age of 3 days were investigated by calorimetry. Moreover, the properties of cementitious system in fresh and hardened state (setting time, drying shrinkage, and compressive strength) with 5% ordinary Portland cement replaced by ultrafine powder were evaluated. From SEM micrographs, the particle size of ultrafine powder was found to be up to several hundred nanometers. The hydration product started formulating at the age of 3 days due to slow reacting nature of belitic 2CaO·SiO₂. The initial and final setting times were prolonged and no significant difference in drying shrinkage was observed when 5% ordinary Portland cement was replaced by ultrafine powder. Moreover, in comparison to control reactive powder concrete, the reactive powder concrete containing ultrafine powder showed improvement in compressive strength at and above 7 days of testing. Based on above, it can be concluded that the manufactured ultrafine 2CaO·SiO₂ powder has the potential to improve the performance of a reactive powder cementitious system.

Influence of Ultrafine 2CaO·SiO2 Powder on Hydration Properties of Reactive Powder Concrete

PubMed Central

Sun, Hongfang; Li, Zishanshan; Memon, Shazim Ali; Zhang, Qiwu; Wang, Yaocheng; Liu, Bing; Xu, Weiting; Xing, Feng

2015-01-01

In this research, we assessed the influence of an ultrafine 2CaO·SiO2 powder on the hydration properties of a reactive powder concrete system. The ultrafine powder was manufactured through chemical combustion method. The morphology of ultrafine powder and the development of hydration products in the cement paste prepared with ultrafine powder were investigated by scanning electron microscopy (SEM), mineralogical composition were determined by X-ray diffraction, while the heat release characteristics up to the age of 3 days were investigated by calorimetry. Moreover, the properties of cementitious system in fresh and hardened state (setting time, drying shrinkage, and compressive strength) with 5% ordinary Portland cement replaced by ultrafine powder were evaluated. From SEM micrographs, the particle size of ultrafine powder was found to be up to several hundred nanometers. The hydration product started formulating at the age of 3 days due to slow reacting nature of belitic 2CaO·SiO2. The initial and final setting times were prolonged and no significant difference in drying shrinkage was observed when 5% ordinary Portland cement was replaced by ultrafine powder. Moreover, in comparison to control reactive powder concrete, the reactive powder concrete containing ultrafine powder showed improvement in compressive strength at and above 7 days of testing. Based on above, it can be concluded that the manufactured ultrafine 2CaO·SiO2 powder has the potential to improve the performance of a reactive powder cementitious system. PMID:28793560

Process for preparing active oxide powders

DOEpatents

Berard, Michael F.; Hunter, Jr., Orville; Shiers, Loren E.; Dole, Stephen L.; Scheidecker, Ralph W.

1979-02-20

An improved process for preparing active oxide powders in which cation hydroxide gels, prepared in the conventional manner are chemically dried by alternately washing the gels with a liquid organic compound having polar characteristics and a liquid organic compound having nonpolar characteristics until the mechanical water is removed from the gel. The water-free cation hydroxide is then contacted with a final liquid organic wash to remove the previous organic wash and speed drying. The dried hydroxide treated in the conventional manner will form a highly sinterable active oxide powder.

The effect of immediate dentin sealing and optical powder removal method on the fracture resistance of CAD/CAM-fabricated endocrowns.

PubMed

El-Damanhoury, Hatem M; Gaintantzopoulou, Marianna

2016-01-01

To evaluate the effect of immediate dentin sealing and optical powder removal method on the fracture resistance of CAD/CAM-fabricated ceramic endocrowns. Seventy-eight extracted premolars were endodontically treated. Standardized endocrown preparations were done in 60 teeth. Teeth were divided equally (n = 10) depending on the treatment of dentin (delayed sealing [DS] or immediate sealing [IS]), and the methods of optical powder removal (air-water spray washing [AW]; microabrasion [MA]; or aqueous suspension of pumice [PB], followed by air-water spray washing). After cementation, specimens were thermocycled (5,000 cycles, 5°C/50°C) and stored in distilled water for 1 week. Specimens were loaded in compression using a universal testing machine until failure. Failure load was recorded, and modes of failure were examined under a stereomicroscope. Micromorphological evaluation of different dentin treatments was done under SEM (n = 3). Results were analyzed using two-way ANOVA and Bonferroni post hoc multiple comparison tests (α = 0.05). Fracture resistance of all IS groups was significantly lower than DS groups, except for AW. There was no statistically significant difference between powder removal methods. Immediate dentin sealing does not improve the fracture resistance of endocrown restorations. Air-water spray washing is adequate to remove the optical powder after optical scanning impression taking.

Different amorphous solid-state forms of roxithromycin: A thermodynamic and morphological study.

PubMed

Milne, Marnus; Liebenberg, Wilna; Aucamp, Marique Elizabeth

2016-02-10

The striking impact that different preparation methods have on the characteristics of amorphous solid-state forms has attracted considerable attention during the last two decades. The pursuit of more extensive knowledge regarding polyamorphism therefore continues. The aim of this study was firstly, to investigate the influence of different preparation techniques to obtain amorphous solid-state forms for the same active pharmaceutical ingredient, namely roxithromycin. The preparation techniques also report on a method utilizing hot air, which although it is based on a melt intermediary step, is considered a novel preparation method. Secondly, to conduct an in-depth investigation into any physico-chemical differences between the resulting amorphous forms and thirdly, to bring our findings into context with that of previous work done, whilst simultaneously discussing a well-defined interpretation for the term polyamorphism and propose a discernment between true polyamorphism and pseudo-polyamorphism/atypical-polyamorphism. The preparation techniques included melt, solution, and a combination of solution-mechanical disruption as intermediary steps. The resulting amorphous forms were investigated using differential scanning calorimetry, X-ray powder diffraction, hot-stage microscopy, scanning electron microscopy, and vapor sorption. Clear and significant thermodynamic differences were determined between the four amorphous forms. It was also deduced from this study that different preparation techniques have a mentionable impact on the morphological properties of the resulting amorphous roxithromycin powders. Thermodynamic properties as well as the physical characteristics of the amorphous forms greatly governed other physico-chemical properties i.e. solubility and dissolution. Copyright © 2015 Elsevier B.V. All rights reserved.

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).

Physical properties evaluation of roselle extract-egg white mixture under various drying temperatures

NASA Astrophysics Data System (ADS)

Triyastuti, M. S.; Kumoro, A. C.; Djaeni, M.

2017-03-01

Roselle contains anthocyanin that is potential for food colorant. Occasionally, roselle extract is provided in dry powder prepared under high temperature. In this case, the anthocyanin color degrades due to the intervention of heat. The foammat drying with egg white is a potential method to speed up the drying process as well as minimize color degradation. This research aims to study the physical properties of roselle extract under foam mat drying. As indicators, the powder size and color intensity were observed. The result showed that at high temperatures, roselle powder under foam mat drying has the fine size with porous structure. However, at the higher the drying temperature the color retention decreased.

Thin, porous metal sheets and methods for making the same

DOEpatents

Liu, Wei; Li, Xiaohong Shari; Canfield, Nathan L.

2015-07-14

Thin, porous metal sheets and methods for forming them are presented to enable a variety of applications and devices. The thin, porous metal sheets are less than or equal to approximately 200 .mu.m thick, have a porosity between 25% and 75% by volume, and have pores with an average diameter less than or equal to approximately 2 .mu.m. The thin, porous metal sheets can be fabricated by preparing a slurry having between 10 and 50 wt % solvent and between 20 and 80 wt % powder of a metal precursor. The average particle size in the metal precursor powder should be between 100 nm and 5 .mu.m.

Preparation of High-Grade Powders from Tomato Paste Using a Vacuum Foam Drying Method.

PubMed

Sramek, Martin; Schweiggert, Ralf Martin; van Kampen, Andreas; Carle, Reinhold; Kohlus, Reinhard

2015-08-01

We present a rapid and gentle drying method for the production of high-grade tomato powders from double concentrated tomato paste, comparing results with powders obtained by foam mat air drying and freeze dried powders. The principle of this method consists of drying tomato paste in foamed state at low temperatures in vacuum. The formulations were dried at temperatures of 50, 60, and 70 °C and vacuum of 200 mbar. Foam stability was affected by low serum viscosity and the presence of solid particles in tomato paste. Consequently, serum viscosity was increased by maltodextrin addition, yielding optimum stability at tomato paste:maltodextrin ratio of 2.4:1 (w/w) in dry matter. Material foamability was improved by addition of 0.5% (w/w, fresh weight) egg white. Because of solid particles in tomato paste, foam air filling had to be limited to critical air volume fraction of Φ = 0.7. The paste was first pre-foamed to Φ = 0.2 and subsequently expanded in vacuo. After drying to a moisture content of 5.6% to 7.5% wet base (w.b.), the materials obtained were in glassy state. Qualities of the resulting powders were compared with those produced by freeze and air drying. Total color changes were the least after vacuum drying, whereas air drying resulted in noticeable color changes. Vacuum foam drying at 50 °C led to insignificant carotenoid losses, being equivalent to the time-consuming freeze drying method. In contrast, air drying caused lycopene and β-carotene losses of 18% to 33% and 14% to 19% respectively. Thus, vacuum foam drying enables production of high-grade tomato powders being qualitatively similar to powders obtained by freeze drying. © 2015 Institute of Food Technologists®

Spectroscopy investigation of nanostructured nickel–zinc ferrite obtained by mechanochemical synthesis

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

Lazarević, Zorica Ž., E-mail: lzorica@yahoo.com; Milutinović, Aleksandra N.; Jovalekić, Čedomir D.

2015-03-15

Highlights: • Nano powder of Ni{sub 0.5}Zn{sub 0.5}Fe{sub 2}O{sub 4} prepared by a soft mechanochemicaly after 10 h milling. • Phase formation controlled by XRD, Raman and IR spectroscopy. • Spectroscopy measurements indicate that the prepared samples have spinel structure. • The average particles size are found to be around 20 nm. • The degree of inversion is δ = 0.36 for NZF obtained from hydroxides for 10 h. - Abstract: Nano crystalline samples of nickel–zinc ferrite, Ni{sub 0.5}Zn{sub 0.5}Fe{sub 2}O{sub 4} were prepared by mechanochemical route in a planetary ball mill starting from two mixtures of the appropriate quantitiesmore » of the powders: case (1) oxide powders: NiO, ZnO and α-Fe{sub 2}O{sub 3} in one case, and in the second case (2) hydroxide powders: Ni(OH){sub 2}, Zn(OH){sub 2} and Fe(OH){sub 3}. In order to monitor the progress of chemical reaction and confirm phase formation, powder samples obtained after 5 h and 10 h of milling were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), Raman, IR and Mössbauer spectroscopy. It is shown that the soft mechanochemical method, i.e. mechanochemical activation of hydroxides, produces high quality single phase Ni{sub 0.5}Zn{sub 0.5}Fe{sub 2}O{sub 4} samples in much more efficient way. From the IR spectroscopy of single phase samples it is obvious that energy of modes depends on the ratio of cations. The deconvolution of Raman spectra allows to separate contributions of different cations to a particular type of vibration and to estimate the degree of inversion.« less

A Dry Powder Process for Preparing Uni-Tape Prepreg from Polymer Powder Coated Filamentary Towpregs

NASA Technical Reports Server (NTRS)

Wilkinson, Steven P. (Inventor); Johnston, Norman J. (Inventor); Marchello, Joseph M. (Inventor)

1995-01-01

A process for preparing uni-tape prepreg from polymer powder coated filamentary towpregs is provided. A plurality of polymer powder coated filamentary towpregs are provided. The towpregs are collimated so that each towpreg is parallel. The sandwich is heated to a temperature wherein the polymer flows and intimately contacts the filaments and pressure is repeatedly applied perpendicularly to the sandwich with a longitudinal oscillating action wherein the filaments move apart and the polymer wets the filaments forming a uni-tape prepreg. The uni-tape prepreg is subsequently cooled.

Development of an analytical method for detecting nitrofurans in bee pollen by liquid chromatography-electrospray ionization tandem mass spectrometry.

PubMed

Park, Mi Sun; Kim, Kyung Tae; Kang, Jong Seong

2017-03-01

Bee pollen collected by honeybees, which is in powdered form, is a good nutritional supplement. Nitrofuran antibiotics are assumed not to be present in bee pollen, which is important as the level of antibiotics in bee pollen is strongly regulated in many countries. A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method to detect nitrofurans in honey has been developed, but this method is not suitable for bee pollen because of it being in powdered form. During preparation of bee pollen samples, the dispersal of powder particles in an aqueous solution often makes them susceptible to forming an emulsion with solvent components such as hexane and ethyl acetate. This may reduce the reproducibility and sensitivity of analyses of nitrofuran levels in bee pollen. Therefore, we attempted to optimize the sample preparation conditions to detect nitrofurans in bee pollen by determining three nitrofuran residues, namely, 3-amino-2-oxazolidinone (AOZ), 3-amino-5-methyl-morpholino-2-oxazolidinone (AMOZ), and 1-aminohydantoin (AHD), using LC-MS/MS. The optimized method prevented the formation of powder-induced emulsion. To verify the reproducibility and sensitivity of this method, it was validated using nitrofuran-free bee pollen spiked with analytes with different side chains at 1.0, 2.0, and 5.0μgkg -1 . The accuracy levels were 94.1%-104.0% and the coefficients of variation were less than 12%. The limits of detection for AOZ, AMOZ, and AHD were 0.18, 0.25, and 0.30μgkg -1 , respectively, while their limits of quantitation were 0.59, 0.83, and 1.00μgkg -1 . The LC-MS/MS method developed to analyze nitrofuran in bee pollen should contribute to the quality control of bee pollen and food safety. Copyright © 2016 Elsevier B.V. All rights reserved.

Morphology and conductivity study of solid electrolyte Li{sub 3}PO{sub 4}

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

Prayogi, Lugas Dwi, E-mail: ldprayodi@gmail.com; Faisal, Muhamad; Kartini, Evvy, E-mail: kartini@batan.go.id

2016-02-08

The comparison between two different methods of synthesize of solid electrolyte Li{sub 3}PO{sub 4} as precursor material for developing lithium ion battery, has been performed. The first method is to synthesize Li{sub 3}PO{sub 4} prepared by wet chemical reaction from LiOH and H{sub 3}PO{sub 4} which provide facile, abundant available resource, low cost, and low toxicity. The second method is solid state reaction prepared by Li{sub 2}CO{sub 3} and NH{sub 4}H{sub 2}PO{sub 4.} In addition, the possible morphology identification of comparison between two different methods will also be discussed. The composition, morphology, and additional identification phase and another compound ofmore » Li{sub 3}PO{sub 4} powder products from two different reaction are characterized by SEM, EDS, and EIS. The Li{sub 3}PO{sub 4} powder produced from wet reaction and solid state reaction have an average diameter of 0.834 – 7.81 µm and 2.15 – 17.3 µm, respectively. The density of Li{sub 3}PO{sub 4} prepared by wet chemical reaction is 2.238 gr/cm{sup 3}, little bit lower than the sample prepared by solid state reaction which density is 2.3560 gr/cm{sup 3}. The EIS measurement result shows that the conductivity of Li{sub 3}PO{sub 4} is 1.7 x 10{sup −9} S.cm{sup −1} for wet chemical reaction and 1.8 x 10{sup −10} S.cm{sup −1} for solid state reaction. The conductivity of Li{sub 3}PO{sub 4} is not quite different between those two samples even though they were prepared by different method of synthesize.« less

Preparation, chemical composition and storage studies of quamachil (Pithecellobium dulce L.) aril powder.

PubMed

Rao, Galla Narsing; Nagender, Allani; Satyanarayana, Akula; Rao, Dubasi Govardhana

2011-02-01

Quamachil aril powder samples were prepared and evaluated for chemical composition and sensory quality by packing in two packaging systems during storage for six months. The protein contents were 12.4 and 15.0% in white and pink aril powders respectively. The titrable acidity of white and pink aril powders were 2.4 and 4.8% respectively. Ca and Fe contents in white aril powder samples were 60 and 12 mg/100 g where as in pink aril powder 62 and 16 mg/100 g, respectively. The anthocyanin content in pink powder decreased from 50.5 to 11.2 and 14.1 mg/100 g in samples packed in polyethylene (PE) and metalised polyester polyethylene laminated pouches respectively. Total polyphenol amount increased in both the powders irrespective of packaging material. Sorption isotherms indicated that both white and pink aril powders were hygroscopic and equilibrated at low relative humidity of 28 and 32%, respectively.

Characterisation of Sol-Gel Synthesis of Phase Pure CaTiO3 Nano Powders after Drying

NASA Astrophysics Data System (ADS)

Mallik, P. K.; Biswal, G.; Patnaik, S. C.; Senapati, S. K.

2015-02-01

According to a few recent studies, calcium titanate (CT) is a material that is similar to hydroxyapatite in biological properties. However, calcium titanate is not currently being used in the biomedical applications as to hydroxyapatite. The objective is to prepare nano calcium titanate powders from the equimolar solution of calcium oxide, ethanol and Titanium (IV) isopropoxide via sol-gel synthesis. The phase analysis and morphology of powder particles were studied by X-ray diffraction (XRD), while the composition and size of powder particles were determined by Transmission electron microscope (TEM) attached with energy dispersive x-ray spectrometer (EDS). As results, XRD confirm the presence of phase pure crystalline CaTiO3 after drying at 100°C for 24 hours, while TEM analysis confirms about 13 nm sizes of CaTiO3 particles and some agglomerated particle of 20-30 nm. Moreover, EDS analysis indicates that the approximately stoichiometric Ca/Ti ratio 1:1 was obtained in the CaTiO3 powders. Finally, it can be concluded that described sol-gel synthesis could be novel method for the production of nano CaTiO3 particles at lower temperature compared to any other methods of production.

Effect of vanadium carbide on dry sliding wear behavior of powder metallurgy AISI M2 high speed steel processed by concentrated solar energy

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

García, C.

Mixtures of AISI M2 high speed steel and vanadium carbide (3, 6 or 10 wt.%) were prepared by powder metallurgy and sintered by concentrated solar energy (CSE). Two different powerful solar furnaces were employed to sinter the parts and the results were compared with those obtained by conventional powder metallurgy using a tubular electric furnace. CSE allowed significant reduction of processing times and high heating rates. The wear resistance of compacts was studied by using rotating pin-on-disk and linearly reciprocating ball-on-flat methods. Wear mechanisms were investigated by means of scanning electron microscopy (SEM) observations and chemical inspections of the microstructuresmore » of the samples. Better wear properties than those obtained by conventional powder metallurgy were achieved. The refinement of the microstructure and the formation of carbonitrides were the reasons for this. - Highlights: •Powder metallurgy of mixtures of M2 high speed steel and VC are studied. •Some sintering is done by concentrated solar energy. •Rotating pin-on-disk and linearly reciprocating ball-on-flat methods are used. •The tribological properties and wear mechanisms, under dry sliding, are studied.« less

Innovative edible packaging from mango kernel starch for the shelf life extension of red chili powder.

PubMed

Nawab, Anjum; Alam, Feroz; Haq, Mohammad Abdul; Haider, Mohammad Samee; Lutfi, Zubala; Kamaluddin, Sheikh; Hasnain, Abid

2018-07-15

In this study mango kernel starch (MKS) based heat sealable pouches were developed for packing of red chili powder. The films were prepared by casting technique using glycerol, sorbitol and 1:1 mixture of glycerol and sorbitol and were sealed. All films showed better heat sealing capacity but glycerol films plasticized exhibited higher seal strength than their counterparts. The red chili powder was packed in the MKS film pouches while commercially available polyethylene (PE) film was used as control. The pungency and color of red chili powder was monitored during six months storage at 40°C. The capsaicinoid content was extracted from the red chili with acetonitrile and evaluated quantitatively using spectrophotometric method. The extractable color was measured by ASTA method using acetone. The results showed significant differences in color and pungency of chili packed in MKS and PE pouches. The highest reduction in capsaicinoid content (pungency) of chili powder was observed in PE pouch (25.9%) while lowest was observed in MKS pouch containing sorbitol (15.7%). Similarly color loss was also highest in chili packed in PE pouch while lowest in MKS-sorbitol pouch. Copyright © 2018 Elsevier B.V. All rights reserved.

Optimized pulmonary gene transfection in mice by spray-freeze dried powder inhalation.

PubMed

Mohri, Kohta; Okuda, Tomoyuki; Mori, Asami; Danjo, Kazumi; Okamoto, Hirokazu

2010-06-01

Spray-freeze drying (SFD) is an attractive technique to prepare highly porous dry powders for inhalation. However, there have been few reports of its application to dry powder inhalers (DPIs). Therefore, in this study, we prepared dry plasmid DNA (pDNA) powders with different molecular ratios of chitosan to pDNA (N/P ratios) by SFD. All the pDNA powders were spherical and highly porous, with particles approximately 20-40microm in geometric diameter. The morphology changed little with the alteration of the N/P ratio. On electrophoresis, a band of linear pDNA was detected in the preparation without chitosan, suggesting the destabilization of pDNA through SFD. However, the addition of chitosan protected pDNA from destabilization. Moreover, the pDNA powders were evaluated for pulmonary gene transfection efficiency using an in vivo dual imaging technique for gene DPIs developed previously. Maximum gene expression was observed at 9-12h following pulmonary administration of the powders into mice. The powder with the N/P ratio of 10 had the highest gene transfection efficiency. A higher affinity of chitosan for pDNA and a smaller (approximately 100nm) pDNA/chitosan complex (N/Pf10) were found at pH 6.5 (in lung) than at pH 7.4 (in physiological conditions), suggesting that the effective compaction of pDNA by chitosan at the N/P ratio of 10 at pH 6.5 contributes to the gene transfection efficiency in the lung. These results suggest inhalable dry pDNA powders with chitosan prepared by SFD to be a suitable formulation for pulmonary gene therapy. Copyright (c) 2010 Elsevier B.V. All rights reserved.

A novel strategy for pharmaceutical cocrystal generation without knowledge of stoichiometric ratio: myricetin cocrystals and a ternary phase diagram.

PubMed

Hong, Chao; Xie, Yan; Yao, Yashu; Li, Guowen; Yuan, Xiurong; Shen, Hongyi

2015-01-01

To develop a streamlined strategy for pharmaceutical cocrystal preparation without knowledge of the stoichiometric ratio by preparing and characterizing the cocrystals of myricetin (MYR) with four cocrystal coformers (CCF). An approach based on the phase solubility diagram (PSD) was used for MYR cocrystals preparation and the solid-state properties were characterized by differential scanning calorimetry (DSC), fourier transform-infrared spectroscopy (FT-IR), powder X-ray diffraction (PXRD), and scanning electron microscopy (SEM). The ternary phase diagram (TPD) was constructed by combining the PSD and nuclear magnetic resonance (NMR) data. After that, the TPD was verified by traditional methods. The dissolution of MYR in the four cocrystals and pure MYR within three different media were also evaluated. A simple research method for MYR cocrystal preparation was obtained as follows: first, the PSD of MYR and CCF was constructed and analyzed; second, by transforming the curve in the PSD to a TPD, a region of pure cocrystals formation was exhibited, and then MYR cocrystals were prepared and identified by DSC, FT-IR, PXRD, and SEM; third, with the composition of the prepared cocrystal from NMR, the TPD of the MYR-CCF-Solvent system was constructed. The powder dissolution data showed that the solubility and dissolution rate of MYR was significantly enhanced by the cocrystals. A novel strategy for pharmaceutical cocrystals preparation without knowledge of the stoichiometric ratio based on the TPD was established and MYR cocrystals were successfully prepared. The present study provides a systematic approach for pharmaceutical cocrystal generation, which benefits the development and application of cocrystal technology in drug delivery.

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.

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

Tian, Liang; Ames Lab. and Iowa State Univ., Ames, IA; Anderson, Iver

Recently, a novel Al/Ca composite was produced by severe plastic deformation of Al powders and Ca granules for possible use as a high-voltage power transmission conductor. Since the strength of such composites is inversely proportional to the Ca filament size, fine Ca powders (less than ~250 μm) are needed to achieve the desired high strength for the powder metallurgy production of an Al-matrix composite reinforced by nano-scale Ca filaments. However, fine Ca powders are not commercially available. Therefore, we have developed a method to produce fine Ca powders via centrifugal atomization to supply Ca powder for prototype development of Al/Camore » composite conductor. A secondary goal of the project was to demonstrate that Ca powder can be safely prepared, stored, and handled and could potentially be scaled for commercial production. Our results showed that centrifugal atomization can yield as much as 83 vol. % Ca powder particles smaller than 250 μm. The mean particle size sometimes matches, sometimes deviates substantially from the predictions of the Champagne & Anger equation likely due to unexpected secondary atomization. The particle size distribution is typical for a ligament-disintegration atomization mode. Scanning electron micrographs showed that the morphology of these Ca powders varied with powder size. Spark testing and auto-ignition tests indicated that the atomized powders were difficult to ignite, providing confidence that this material can be handled safely in air.« less

Sintered rare earth-iron Laves phase magnetostrictive alloy product and preparation thereof

DOEpatents

Malekzadeh, Manoochehr; Pickus, Milton R.

1979-01-01

A sintered rare earth-iron Laves phase magnetostrictive alloy product characterized by a grain oriented morphology. The grain oriented morphology is obtained by magnetically aligning powder particles of the magnetostrictive alloy prior to sintering. Specifically disclosed are grain oriented sintered compacts of Tb.sub.x Dy.sub.1-x Fe.sub.2 and their method of preparation. The present sintered products have enhanced magnetostrictive properties.

Influence of Starting Powders on Hydroxyapatite Coatings Fabricated by Room Temperature Spraying Method.

PubMed

Seo, Dong Seok; Lee, Jong Kook; Hwang, Kyu Hong; Hahn, Byung Dong; Yoon, Seog Young

2015-08-01

Three types of raw materials were used for the fabrication of hydroxyapatite coatings by using the room temperature spraying method and their influence on the microstructure and in vitro characteristics were investigated. Starting hydroxyapatite powders for coatings on titanium substrate were prepared by a heat treatment at 1100 °C for 2 h of bovine bone, bone ash, and commercial hydroxyapatite powders. The phase compositions and Ca/P ratios of the three hydroxyapatite coatings were similar to those of the raw materials without decomposition or formation of a new phase. All hydroxyapatite coatings showed a honeycomb structure, but their surface microstructures revealed different features in regards to surface morphology and roughness, based on the staring materials. All coatings consisted of nano-sized grains and had dense microstructure. Inferred from in vitro experiments in pure water, all coatings have a good dissolution-resistance and biostability in water.

Hydroxyapatite nanocrystals: simple preparation, characterization and formation mechanism.

PubMed

Mohandes, Fatemeh; Salavati-Niasari, Masoud; Fathi, Mohammadhossein; Fereshteh, Zeinab

2014-12-01

Crystalline hydroxyapatite (HAP) nanoparticles and nanorods have been successfully synthesized via a simple precipitation method. To control the shape and particle size of HAP nanocrystals, coordination ligands derived from 2-hydroxy-1-naphthaldehyde were first prepared, characterized by Fourier transform infrared (FT-IR) and proton nuclear magnetic resonance ((1)H-NMR) spectroscopies, and finally applied in the synthesis process of HAP. On the other hand, the HAP nanocrystals were also characterized by several techniques including powder X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM). According to the FE-SEM and TEM micrographs, it was found that the morphology and crystallinity of the HAP powders depended on the coordination mode of the ligands. Copyright © 2014 Elsevier B.V. All rights reserved.

New Tubular Ceramic Membranes from Natural Moroccan Clay for Microfiltration Application

NASA Astrophysics Data System (ADS)

Ait Taleb, A.; El Baraka, N.; Saffaj, N.; Laknifli, A.; Mamouni, R.; Fatni, A.; El Hammadi, A.; El Qacimi, N.

2018-05-01

This paper is devoted the preparation of low cost microfiltration membranes using Moroccan clay powder. The preparation of membrane was composed with two steps: First a macroporous tubular support with a pore diameter 10 μm and porosity 43%. Secondly a microfiltration layer was performed by the slip casting method. A deflocculated slip was obtained by mixing mineral powder of ZrO2, PVA (polyvinyl alcohol) and water, after drying at room temperature for 24 h, the microfiltration layer was heated to 800°C for consolidation. Scanning electron microscopy observation showed homogeneous layers without cracks with an average pore diameter of 0.19 μm for the active layer. Water permeability obtained is about 841 L/h.m2.bar. The membranes have been tested to cleaning of colored wastewater.

Highly surface-roughened quasi-spherical silver powders in back electrode paste for silicon solar cells

NASA Astrophysics Data System (ADS)

Yin, Peng; Liu, Shouchao; Li, Qiuying; Chen, Xiaolei; Guo, Weihong; Wu, Chifei

2017-08-01

In our work, highly surface-roughened quasi-spherical silver powders with controllable size and superior dispersibility, which have narrow size distribution and relatively high tap density, were successfully prepared by reducing silver nitrate with ascorbic acid in aqueous solutions. Gum arabic (AG) was selected as dispersant to prevent the agglomeration of silver particles. Furthermore, the effects of preparation conditions on the characteristics of the powders were systematically investigated. By varying the concentration of the reactants, dosage of dispersant, the feeding modes, synthesis temperature and the pH value of the mixture solution of silver nitrate and AG, the resulted silver particles displayed controllable size, different morphologies and surface roughness. The spherical silver powder with mean particle size of 1.20 µm, tap density of 4.1 g cm-3 and specific area value of 0.46 m2 g-1 was prepared by adjusting preparation conditions. The AG absorbed on the surface preventing the silver particles from diffusion and aggregation was proved by the ultraviolet spectra. Observations of SEM images showed that the as-prepared silver powders were relatively monodisperse silver spheres with highly roughened surface and the particle size was controllable from 1 µm to 5 µm, specific surface area value from approximately 0.2 m2 g-1 to 0.8 m2 g-1. X-ray diffraction (XRD) patterns, energy dispersive spectroscopy (EDS), x-ray photoelectron spectra (XPS) and thermal gravity analysis (TGA) demonstrated high crystallinity and purity of the obtained silver powders.

CH3 NH3 PbI3 and HC(NH2 )2 PbI3 Powders Synthesized from Low-Grade PbI2 : Single Precursor for High-Efficiency Perovskite Solar Cells.

PubMed

Zhang, Yong; Kim, Seul-Gi; Lee, Do-Kyoung; Park, Nam-Gyu

2018-05-09

High-efficiency perovskite solar cells are generally fabricated by using highly pure (>99.99 %) PbI 2 mixed with an organic iodide in polar aprotic solvents. However, the use of such an expensive chemical may impede progress toward large-scale industrial applications. Here, we report on the synthesis of perovskite powders by using inexpensive low-grade (99 %) PbI 2 and on the photovoltaic performance of perovskite solar cells prepared from a powder-based single precursor. Pure APbI 3 [A=methylammonium (MA) or formamidinium (FA)] perovskite powders were synthesized by treating low-grade PbI 2 with MAI or FAI in acetonitrile at ambient temperature. The structural phase purity was confirmed by X-ray diffraction. The solar cell with a MAPbI 3 film prepared from the synthesized perovskite powder demonstrated a power conversion efficiency (PCE) of 17.14 %, which is higher than the PCE of MAPbI 3 films prepared by using both MAI and PbI 2 as precursors (PCE=13.09 % for 99 % pure PbI 2 and PCE=16.39 % for 99.9985 % pure PbI 2 ). The synthesized powder showed better absorption and photoluminescence, which were responsible for the better photovoltaic performance. For the FAPbI 3 powder, a solution with a yellow non-perovskite δ-FAPbI 3 powder synthesized at room temperature was found to lead to a black perovskite film, whereas a solution with the black perovskite α-FAPbI 3 powder synthesized at 150 °C was not transformed into a black perovskite film. The α↔δ transition between the powder and film was assumed to correlate with the difference in the iodoplumbates in the powder-dissolved solution. An average PCE of 17.21 % along with a smaller hysteresis [ΔPCE=PCE reverse -PCE forward )=1.53 %] was demonstrated from the perovskite solar cell prepared by using δ-FAPbI 3 powder; this PCE is higher than the average PCE of 17.05 % with a larger hysteresis (ΔPCE=2.71 %) for a device based on a conventional precursor solution dissolving MAI with high-purity PbI 2 . The smaller hysteresis was indicative of fewer defects in the resulting FAPbI 3 film prepared by using the δ-FAPbI 3 powder. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Direct Compositional Characterization of (U,Th)O2 Powders, Microspheres, and Pellets Using TXRF.

PubMed

Dhara, Sangita; Prabhat, Parimal; Misra, N L

2015-10-20

A total reflection X-ray fluorescence (TXRF) analysis method for direct compositional characterization of sintered and green (U,Th)O2 samples in different forms (e.g., pellets, powders, and microspheres) without sample dissolution has been developed for the first time. The methodology involves transfer of only a few nanograms of the sample on the TXRF sample support by gently rubbing the samples on supports or taking their tiny uniform slurry in collodion on the sample support, drying them to make thin film, and measuring the TXRF spectra of the specimens thus prepared. This approach minimizes the matrix effects. Uranium determinations from the TXRF spectra of such specimens were made with respect to thorium, considering it as an internal standard. Samples having uranium atom percent (at%) from 0 to 100 in (U,Th)O2 were analyzed for uranium in comparison to thorium. The results showed an average precision of 2.6% (RSD, 2σ, n = 8). The TXRF-determined results deviated from expected values within 5%. The TXRF results were compared with those of biamperometry with good agreement. The lattice parameters of the solid solutions were calculated using their XRD patterns. A good correlation between lattice parameters and TXRF-determined U at% and between TXRF-determined U at% and expected U at%, calculated on the basis of preparation of (U,Th)O2 solid solutions, was obtained. The developed method is capable of analyzing (U,Th)O2 samples directly with almost negligible sample preparation and is well suited for radioactive samples. The present study suggests that this method can be extended for the determination of U,Th and Pu in other nuclear fuel materials (e.g., nitrides, carbides, etc.) in the form of pellets, powders, and microspheres after suitable modifications in sample handling procedure.

Abrasion resistant coating and method of making the same

DOEpatents

Sordelet, Daniel J.; Besser, Matthew F.

2001-06-05

An abrasion resistant coating is created by adding a ductile phase to a brittle matrix phase during spray coating where an Al--Cu--Fe quasicrystalline phase (brittle matrix) and an FeAl intermetallic (ductile phase) are combined. This composite coating produces a coating mostly of quasicrystal phase and an inter-splat layer of the FeAl phase to help reduce porosity and cracking within the coating. Coatings are prepared by plasma spraying unblended and blended quasicrystal and intermetallic powders. The blended powders contain 1, 5, 10 and 20 volume percent of the intermetallic powders. The unblended powders are either 100 volume percent quasicrystalline or 100 volume percent intermetallic; these unblended powders were studied for comparison to the others. Sufficient ductile phase should be added to the brittle matrix to transform abrasive wear mode from brittle fracture to plastic deformation, while at the same time the hardness of the composite should not be reduced below that of the original brittle phase material.

Combined control of morphology and polymorph in spray drying of mannitol for dry powder inhalation

NASA Astrophysics Data System (ADS)

Lyu, Feng; Liu, Jing J.; Zhang, Yang; Wang, Xue Z.

2017-06-01

The morphology and polymorphism of mannitol particles were controlled during spray drying with the aim of improving the aerosolization properties of inhalable dry powders. The obtained microparticles were characterized using scanning electron microscopy, infrared spectroscopy, differential scanning calorimetry, powder X-ray diffraction and inhaler testing with a next generation impactor. Mannitol particles of varied α-mannitol content and surface roughness were prepared via spray drying by manipulating the concentration of NH4HCO3 in the feed solution. The bubbles produced by NH4HCO3 led to the formation of spheroid particles with a rough surface. Further, the fine particle fraction was increased by the rough surface of carriers and the high α-mannitol content. Inhalable dry powders with a 29.1 ± 2.4% fine particle fraction were obtained by spray-drying using 5% mannitol (w/v)/2% NH4HCO3 (w/v) as the feed solution, proving that this technique is an effective method to engineer particles for dry powder inhalation.

Electrochemical investigation of powder coatings and their application to magnesium-rich primers for corrosion protection

NASA Astrophysics Data System (ADS)

Orgon, Casey Roy

Corrosion is the decomposition of metal and metal alloys which threatens the integrity of man-made structures. One of the more efficient methods of delaying the corrosion process in metals is by coatings. In this work, the durability of two polyester powder coatings were investigated for corrosion protection of AA-2024-T3. Polyester powder coatings crosslinked by either triglycidyl isocyanurate (TGIC) or beta-hydroxyalkyl amide (HAA) compounds were prepared and investigated for barrier protection of metal substrates by electrochemical impedance spectroscopy (EIS). Polyester-TGIC coatings were found to provide better long-term protection, which can be attributed to the increased mechanical strength and higher concentration of crosslinking in the coating films. Additionally, the polyester powder coatings, along with a fusion bonded epoxy (FBE) were investigated for their compatibility as a topcoat for magnesium-rich primers (MgRP). Under proper application conditions, powder topcoats were successfully applied to cured MgRP while corrosion protection mechanisms of each system were maintained.

Co-Precipitation Synthesis of Gadolinium Aluminum Gallium Oxide (GAGG) via Different Precipitants

NASA Astrophysics Data System (ADS)

Sun, Yan; Yang, Shenghui; Zhang, Ye; Jiang, Jun; Jiang, Haochuan

2014-02-01

In order to obtain a uniform transparent ceramic scintillator, well-dispersed fine starting powders with high-purity, small grain size, spherical morphology and high sinter-ability are necessary. In this study, Ce3+ doped gadolinium aluminum gallium garnet Gd3Al3Ga2O12 (GAGG) powders were synthesized by the co-precipitation method. NH4OH, NH4HCO3 and the mixed solution of NH4OH and NH4HCO3 were used as precipitants, respectively. The precursor composition, phase formation process, microstructure, morphology, particle size distribution and luminescent properties of obtained GAGG powders were measured. The results show that powders prepared using the mixed precipitant exhibit the best microstructural morphology, good sinter-ability and highest luminescent intensity. Pure GAGG polycrystalline powders could be obtained at about 950°C for 1.5 h and the average size of the particles is about 50 nm. The photoluminescence spectrum shows a strong green-yellow emission near 540 nm.

[METHOD OF INCREASING MICROBIOLOGICAL PURITY OF POWDER FROM COCOA-VELLA].

PubMed

Magomedov, G O; Cheremushkina, L V; Plotnikova, I V

2015-01-01

In the article there is described in detail the characteristic of the product of processing cocoa beans--cocoa-vella, there is presented a comparative analysis of the chemical composition, quality indices, the dispersive pattern, microbiological indices of the powder from the cocoa-vella in comparison to cocoa powder, obtained by traditional technology from the core of the cocoa beans. To improve the microbiological purity of the powder from the cocoa-vella there was suggested to be the modern and environmentally safe manner for the preparation of the powder The use of cocoa-vella disinfecting power by means of the electromagnetic field of ultrahigh frequency (RF EMF) was established to allow to obtain a product that meets the requirements of Technical Regulations of the Customs Union (TRCU 021/2011) on Food Safety. This work is of practical interest, since it helps to improve the safety of the powder from the cocoa-vella, and thus the quality of confectionery and food products based on it, which is relevant in terms of the management of a healthy diet.

Photocatalytic Water Splitting for O2 Production under Visible Light Irradiation Using NdVO4-V2O5 Hybrid Powders

PubMed Central

Chiang, Tzu Hsuan; Chen, Tso-Ming

2017-01-01

The study investigated photocatalytic water splitting for O2 production under visible light irradiation using neodymium vanadium oxide (NdVO4) and vanadium oxide (V2O5) hybrid powders. The results in a sacrificial agent of 0.01 M AgNO3 solution were obtained, and the highest photocatalytic O2 evolution was 2.63 μmol/h, when the hybrid powders were prepared by mixing Nd and V at a volume ratio of 1:3 at a calcination temperature of 350 °C for 1 h. The hybrid powders were synthesized by neodymium nitrate and ammonium metavanadate using the glycothermal method in ethylene glycol at 120 °C for 1 h. The hybrid powders consisted of two shapes, NdVO4 nanoparticles and the cylindrical V2O5 particles, and they possessed the ability for photocatalytic oxygen (O2) evolution during irradiation with visible light. The band gaps and structures of the hybrid powders were analyzed using UV-visible spectroscopy and transmission electron microscopy. PMID:28772692

Preparation of porous Si and TiO 2 nanofibres using a sulphur-templating method for lithium storage

DOE PAGES

McCormac, Kathleen; Byrd, Ian; Brannen, Rodney; ...

2015-02-03

We prepared highly porous Si/TiO 2 composite nanofibres using a unique sulphur-templating method combined with electrospinning. The structure, morphology, surface area, phase and composition of these nanofibres were characterized using Raman spectroscopy, scanning electron microscopy, powder X-ray diffraction, surface area analyser and thermogravimetric analyser. The specific surface area of Si/TiO 2 porous NFs is as large as 387m 2g -1, whose silicon capacity can be maintained above 1580mAhg -1 in 180 cycles.

Preparation and Characterization of Mesoporous Zirconia Made by Using a Poly (methyl methacrylate) Template

NASA Astrophysics Data System (ADS)

Duan, Guorong; Zhang, Chunxiang; Li, Aimei; Yang, Xujie; Lu, Lude; Wang, Xin

2008-03-01

Superfine powders of poly (methyl methacrylate) (PMMA) have been prepared by means of an emulsion polymerization method. These have been used as templates in the synthesis of tetragonal phase mesoporous zirconia by the sol gel method, using zirconium oxychloride and oxalic acid as raw materials. The products have been characterized by infrared spectroscopy, X-ray diffraction analysis, transmission electron microscopy, N2 adsorption-desorption isotherms, and pore size distribution. The results indicate that the average pore size was found to be 3.7 nm.

METHOD OF PREPARING A CERAMIC FUEL ELEMENT

DOEpatents

Ross, W.T.; Bloomster, C.H.; Bardsley, R.E.

1963-09-01

A method is described for preparing a fuel element from -325 mesh PuO/ sub 2/ and -20 mesh UO/sub 2/, and the steps of screening --325 mesh UO/sub 2/ from the -20 mesh UO/sub 2/, mixing PuO/sub 2/ with the --325 mesh UO/sub 2/, blending this mixture with sufficient --20 mesh UO/sub 2/ to obtain the desired composition, introducing the blend into a metal tube, repeating the procedure until the tube is full, and vibrating the tube to compact the powder are included. (AEC)

Preparation, certification and interlaboratory analysis of workplace air filters spiked with high-fired beryllium oxide.

PubMed

Oatts, Thomas J; Hicks, Cheryl E; Adams, Amy R; Brisson, Michael J; Youmans-McDonald, Linda D; Hoover, Mark D; Ashley, Kevin

2012-02-01

Occupational sampling and analysis for multiple elements is generally approached using various approved methods from authoritative government sources such as the National Institute for Occupational Safety and Health (NIOSH), the Occupational Safety and Health Administration (OSHA) and the Environmental Protection Agency (EPA), as well as consensus standards bodies such as ASTM International. The constituents of a sample can exist as unidentified compounds requiring sample preparation to be chosen appropriately, as in the case of beryllium in the form of beryllium oxide (BeO). An interlaboratory study was performed to collect analytical data from volunteer laboratories to examine the effectiveness of methods currently in use for preparation and analysis of samples containing calcined BeO powder. NIST SRM(®) 1877 high-fired BeO powder (1100 to 1200 °C calcining temperature; count median primary particle diameter 0.12 μm) was used to spike air filter media as a representative form of beryllium particulate matter present in workplace sampling that is known to be resistant to dissolution. The BeO powder standard reference material was gravimetrically prepared in a suspension and deposited onto 37 mm mixed cellulose ester air filters at five different levels between 0.5 μg and 25 μg of Be (as BeO). Sample sets consisting of five BeO-spiked filters (in duplicate) and two blank filters, for a total of twelve unique air filter samples per set, were submitted as blind samples to each of 27 participating laboratories. Participants were instructed to follow their current process for sample preparation and utilize their normal analytical methods for processing samples containing substances of this nature. Laboratories using more than one sample preparation and analysis method were provided with more than one sample set. Results from 34 data sets ultimately received from the 27 volunteer laboratories were subjected to applicable statistical analyses. The observed performance data show that sample preparations using nitric acid alone, or combinations of nitric and hydrochloric acids, are not effective for complete extraction of Be from the SRM 1877 refractory BeO particulate matter spiked on air filters; but that effective recovery can be achieved by using sample preparation procedures utilizing either sulfuric or hydrofluoric acid, or by using methodologies involving ammonium bifluoride with heating. Laboratories responsible for quantitative determination of Be in workplace samples that may contain high-fired BeO should use quality assurance schemes that include BeO-spiked sampling media, rather than solely media spiked with soluble Be compounds, and should ensure that methods capable of quantitative digestion of Be from the actual material present are used.

Rocket Research at Georgia Tech.

DTIC Science & Technology

1981-11-01

samples were prepared by dry pressing 30% Valley Met H- 30 aluminum, 7% carnauba wax , and 63% 100 P AP. One sample was prepared using as received H-30, a...Al, and Carnauba wax powders. Sandwiches with aluminum in the binder lamina. Both pre-oxidation and pre-stretching treatments of aluminum particles...two different processes. 1. Dry-pressing powder mixtures in which polymeric binder is replaced by carnauba wax powder. 2. Hand mixing small samples of

Iron oxide nanoparticles supported on ultradispersed diamond powders: Effect of the preparation procedure

NASA Astrophysics Data System (ADS)

Dimitrov, Momtchil; Ivanova, Ljubomira; Paneva, Daniela; Tsoncheva, Tanya; Stavrev, Stavry; Mitov, Ivan; Minchev, Christo

2009-01-01

The state of the iron oxide nanoparticles, supported on ultradispersed diamond (UDD) powders is studied by X-ray diffraction, nitrogen physisorption, temperature-programmed reduction, FTIR and Mössbauer spectroscopy. Methanol decomposition to hydrogen and CO is used as a catalytic test. The peculiarities of the iron oxide species strongly depend on the detonation procedure used for the UDD powders preparation as well as on the iron modification procedure.

Quantitative analysis of perfumes in talcum powder by using headspace sorptive extraction.

PubMed

Ng, Khim Hui; Heng, Audrey; Osborne, Murray

2012-03-01

Quantitative analysis of perfume dosage in talcum powder has been a challenge due to interference of the matrix and has so far not been widely reported. In this study, headspace sorptive extraction (HSSE) was validated as a solventless sample preparation method for the extraction and enrichment of perfume raw materials from talcum powder. Sample enrichment is performed on a thick film of poly(dimethylsiloxane) (PDMS) coated onto a magnetic stir bar incorporated in a glass jacket. Sampling is done by placing the PDMS stir bar in the headspace vial by using a holder. The stir bar is then thermally desorbed online with capillary gas chromatography-mass spectrometry. The HSSE method is based on the same principles as headspace solid-phase microextraction (HS-SPME). Nevertheless, a relatively larger amount of extracting phase is coated on the stir bar as compared to SPME. Sample amount and extraction time were optimized in this study. The method has shown good repeatability (with relative standard deviation no higher than 12.5%) and excellent linearity with correlation coefficients above 0.99 for all analytes. The method was also successfully applied in the quantitative analysis of talcum powder spiked with perfume at different dosages. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Eu-doped BaTiO₃powder and film from sol-gel process with polyvinylpyrrolidone additive.

PubMed

García-Hernández, Margarita; García-Murillo, Antonieta; de J Carrillo-Romo, Felipe; Jaramillo-Vigueras, David; Chadeyron, Geneviève; De la Rosa, Elder; Boyer, Damien

2009-09-17

Transparent BaTiO(3):Eu(3+) films were prepared via a sol-gel method and dip-coating technique, using barium acetate, titanium butoxide, and polyvinylpyrrolidone (PVP) as modifier viscosity. BaTiO(3):Eu(3+) films ~500 nm thick, crystallized after thermal treatment at 700 masculineC. The powders revealed spherical and rod shape morphology. The optical quality of films showed a predominant band at 615 nm under 250 nm excitation. A preliminary luminescent test provided the properties of the Eu(3+) doped BaTiO(3).

Sandwich-type electrode

DOEpatents

Lu, Wen-Tong P.; Garcia, Earl R.

1983-01-01

Disclosed is an improvement on a method of making an electrode wherein a suspension in a liquid is prepared of a powdered catalyst containing a noble metal, carbon powder and a binder, and the suspension is poured over a carbon substrate dried, compressed and sintered to form a solid catalyst layer bonded to the carbon substrate. The improvement is placing a carbon paper on the catalyst layer prior to compressing. The improved electrode can be used as either a cathode or an anode in a sulfur dioxide depolarized electrolyzer in a process for producing hydrogen from water.

Silane surface modification effects on the electromagnetic properties of phosphatized iron-based SMCs

NASA Astrophysics Data System (ADS)

Fan, Liang-Fang; Hsiang, Hsing-I.; Hung, Jia-Jing

2018-03-01

It is difficult to achieve homogeneous phosphatized iron powder dispersion in organic resins during the preparation of soft magnetic composites (SMCs). Inhomogeneous iron powder mixing in organic resins generally leads to the formation of micro-structural defects in SMCs and hence causes the magnetic properties to become worse. Phosphatized iron powder dispersion in organic resins can be improved by coating the phosphatized iron powder surfaces with a coupling agent. This study investigated the (3-aminopropyl) triethoxysilane (APTES) surface modification effects on the electromagnetic properties of phosphatized iron-based soft magnetic composites (SMCs). The results showed that the phosphatized iron powder surface can be modified using APTES to improve the phosphatized iron powder and epoxy resin compatibility and hence enhance phosphate iron powder epoxy mixing. The tensile strength, initial permeability, rated current under DC-bias superposition and magnetic loss in SMCs prepared using phosphatized iron powders can be effectively improved using APTES surface modification, which provides a promising candidate for power chip inductor applications.

Preparation of Si and O co-solution strengthened Ti alloys by using rice husks as SiO2 resource and quantitative descriptions on their strengthening effects

NASA Astrophysics Data System (ADS)

Jia, Lei; Chen, Jiang-xian; Lu, Zhen-lin; Li, Shu-feng; Umeda, Junko; Kondoh, Katsuyoshi

2018-04-01

Ti alloys strengthened by both Si and O solutes were prepared by powder metallurgy method from pure Ti and amorphous SiO2 powder obtained by combusting rice husks. At the same time, Ti alloys singly strengthened by Si or O were also prepared for studying the strengthening effect of Si and O solutes. Results showed that amorphous SiO2 powder originated from rice husks could almost fully dissolve into pure Ti matrix when the content was not higher than 1.0 wt%, while higher content of SiO2 addition resulted in the formation of Ti5Si3 intermetallics. Si and O elements leaded to negative and positive distortion of Ti lattice, and the influencing degrees were ‑0.02 and +0.014 Å/wt% for lattice constant a, while ‑0.05 and +0.046 Å/wt% for constant c, respectively. Solid solution of Si and O would also result in the increase of hardness, which was 98.5 and 209.43 HV/wt%, respectively. When Si and O were co-exsited in Ti matrix, the negative and positive distortion cancelled each other, while the strengthening effect did not cancel but enhance each other.

Preparing and Study the effects of Composite Coatings in Protection of Oil Pipes from the Risk of Corrosion that resulting from Associated water with Petroleum Products

NASA Astrophysics Data System (ADS)

– Sarraf, A. R. Al; Yaseen, M. A.

2018-05-01

In order to inhibit the metallic corrosion in the oil pipelines,the protection method with composite coating of unsaturated polyester and reinforced by Caolin at weight percentage (20%) was studied. Where, the work samples were classified into two groups according to internal composite coatings layers for all groups of these samples. The first group is nitrocellulose coating reinforced by nano and micro powder of Mgo, the second group is sodium silicate coating reinforced by nano powder of Mgo. The following weight percentages (0%, 1%, 3% and 5%) were adopted as reinforcement ratios for nano powders, as well as the weight percentages (0%, 3%, 5% and 7%) as reinforcement ratios for micro powders Tribology properties and Electrochemical Corrosion Resistance by Polarization method (Tafel) and Adhesion Strength were studied. The results showed an improvement in the corrosion resistance of protected steel by coatings compare with uncoated steel, as well as improvement in mechanical properties and adhesion strength of composite coatings.

Synthesization and magnetic properties of Ba1-xYxFe12O19 hexaferrites prepared by solid-state reaction method

NASA Astrophysics Data System (ADS)

Rehman, Khalid Mehmood Ur; Liu, Xiansong; Li, Mingling; Jiang, Shuai; Wu, Yingchun; Zhang, Cong; Liu, Chaocheng; Meng, Xiangyu; Li, Haohao

2017-03-01

M-type hexaferrite Ba(1-x)YxFe12O19 (x=0.00, 0.02, 0.05, 0.08, 0.10, 0.13) magnetic powder and magnets existed to ready according to the conventional ceramic reaction method. X-ray difractometer was used to study the phase compositions of the calcites powder samples. There was a single magnetoplumbite segment in the calcanei magnetic powder with the intensification of x=0.00, 0.02, 0.05, 0.08, 0.10, 0.13. The influence of yttrium aggregation on attractive possessions of the magnets was studied scientifically. The magnetic properties of the magnets were measured by a magnetic properties test instrument (VSM). The saturation magnetization (σs) and coercivity (Hcj) of the Ba(1-x)YxFe12O19 (x=0.00, 0.02, 0.05, 0.08, 0.10, 0.13) magnetic powders with different Yttrium aggregation (x) were determined. The saturation magnetization (σs) was decreased whereas coercivity (Hcj) was increased. The magnetic properties of the magnet at x=0.13 reached the maximum values.

The Importance of the Solids Loading on Confirming the Dielectric Nanosize Dependence of BaTiO3 Powders by Slurry Method

PubMed Central

Zhou, Wei; Nie, Yi Mei; Li, Shu Jing; Liang, Hai Yan

2013-01-01

The dielectric nanosize dependence of BaTiO3 powders was investigated by the slurry method, where two series of BaTiO3 slurries with 10 vol% and 30 vol% solids loadings were prepared as model samples. Applying the Bruggeman-Hanai equation, the high-frequency limiting permittivity (ε h) of the slurries was extracted from the dielectric spectra. The ε h of the 10 vol% slurry showed abnormal size independence in the range from 100 nm to 700 nm, and the ε h of the 30 vol% slurry exhibited good agreement with the previous prediction. Through analysing quantitatively the response of ε h to the changing permittivity of the powders under different solids loading, it was found that the ε h of the slurry with lower solids loading is more inclined to be interfered by the systematic and random errors. Furthermore, a high permittivity value was found in the BaTiO3 powders with 50 nm particle size. PMID:23844376

Production of fine calcium powders by centrifugal atomization with rotating quench bath

DOE PAGES

Tian, Liang; Ames Lab. and Iowa State Univ., Ames, IA; Anderson, Iver; ...

2016-02-08

Recently, a novel Al/Ca composite was produced by severe plastic deformation of Al powders and Ca granules for possible use as a high-voltage power transmission conductor. Since the strength of such composites is inversely proportional to the Ca filament size, fine Ca powders (less than ~250 μm) are needed to achieve the desired high strength for the powder metallurgy production of an Al-matrix composite reinforced by nano-scale Ca filaments. However, fine Ca powders are not commercially available. Therefore, we have developed a method to produce fine Ca powders via centrifugal atomization to supply Ca powder for prototype development of Al/Camore » composite conductor. A secondary goal of the project was to demonstrate that Ca powder can be safely prepared, stored, and handled and could potentially be scaled for commercial production. Our results showed that centrifugal atomization can yield as much as 83 vol. % Ca powder particles smaller than 250 μm. The mean particle size sometimes matches, sometimes deviates substantially from the predictions of the Champagne & Anger equation likely due to unexpected secondary atomization. The particle size distribution is typical for a ligament-disintegration atomization mode. Scanning electron micrographs showed that the morphology of these Ca powders varied with powder size. Spark testing and auto-ignition tests indicated that the atomized powders were difficult to ignite, providing confidence that this material can be handled safely in air.« less

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.

Large scale synthesis of nanostructured zirconia-based compounds from freeze-dried precursors

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

Gomez, A.; Villanueva, R.; Vie, D.

2013-01-15

Nanocrystalline zirconia powders have been obtained at the multigram scale by thermal decomposition of precursors resulting from the freeze-drying of aqueous acetic solutions. This technique has equally made possible to synthesize a variety of nanostructured yttria or scandia doped zirconia compositions. SEM images, as well as the analysis of the XRD patterns, show the nanoparticulated character of those solids obtained at low temperature, with typical particle size in the 10-15 nm range when prepared at 673 K. The presence of the monoclinic, the tetragonal or both phases depends on the temperature of the thermal treatment, the doping concentration and themore » nature of the dopant. In addition, Rietveld refinement of the XRD profiles of selected samples allows detecting the coexistence of the tetragonal and the cubic phases for high doping concentration and high thermal treatment temperatures. Raman experiments suggest the presence of both phases also at relatively low treatment temperatures. - Graphical abstract: Zr{sub 1-x}A{sub x}O{sub 2-x/2} (A=Y, Sc; 0{<=}x{<=}0.12) solid solutions have been prepared as nanostructured powders by thermal decomposition of precursors obtained by freeze-drying, and this synthetic procedure has been scaled up to the 100 g scale. Highlights: Black-Right-Pointing-Pointer Zr{sub 1-x}A{sub x}O{sub 2-x/2} (A=Y, Sc; 0{<=}x{<=}0.12) solid solutions have been prepared as nanostructured powders. Black-Right-Pointing-Pointer The synthetic method involves the thermal decomposition of precursors obtained by freeze-drying. Black-Right-Pointing-Pointer The temperature of the thermal treatment controls particle sizes. Black-Right-Pointing-Pointer The preparation procedure has been scaled up to the 100 g scale. Black-Right-Pointing-Pointer This method is appropriate for the large-scale industrial preparation of multimetallic systems.« less

Microstructure transformation of Cr-Al coating on carbon steel prepared by ball milling method as a function of tungsten doping

NASA Astrophysics Data System (ADS)

Wismogroho, A. S.; Sudiro, T.; Didik, A.; Ciswandi

2018-03-01

In present work, Cr-Al coatings containing 0, 1, 2, 3, and 5% W have been prepared on the surface of low carbon steel by mechanical alloying technique. The composition of each powder was milled for 2 hour in a stainless steel crucible with a ball to powder ratio of 10:1. Afterward, the Cr-Al-W powder and substrate were mechanically alloyed in air for 1 hour. The heat treatment of coated samples was carried out at 800 °C in a vacuum furnace for 2 hour. In order to characterize the phase composition and microstructure of the coating before and after heat treatment, XRD and SEM-EDX were used. The analysis results reveal that the ball milling process induces the formation of homogeneous Cr-Al-W coating structure with a thickness of about 80 μm. The phase observation shows individual peaks of each starting elements, along with the occurrence of powder refinement and solid solution formation. After heat treatment, AlCr2 and Al8Cr5 phases were formed. The addition of W accelerates the formation of AlCr2, but inhibits the formation of Al8Cr5. The detail of the results was presented in this paper.

A Direct Ultrasound Irradiation Method Synthesis of Monodisperse ZnO Microspheres for Varistors Ceramics Application

NASA Astrophysics Data System (ADS)

Chen, Tao; Wang, Mao-Hua; Zhang, Han-Ping; Liu, Jin-Ran; Yao, Da-Chuan

2016-08-01

Monodisperse and uniform ZnO microspheres were synthesized via an ultrasound irradiation method. The microstructure and morphology of the as-prepared sample were characterized by x-ray powder diffraction, Fourier transformation infrared spectra and scanning electron microscopy. The results indicate that the size of ZnO microspheres was strongly affected by the Zn(NO3)2·6H2O. As the amount of the precursor increased, the diameters of the ZnO microspheres can be turned from ˜500 nm to ˜2 μm. The electrical properties of the varistors ceramics prepared from the as-obtained ZnO powders were investigated. The results show that the varistors ceramics made from ZnO with a size of ˜500 nm and sintered in air at 1150°C for 2 h possess a density of 5.50 g/cm3 corresponding to 95.1% of the theoretical density, with breakdown voltage of 280.9 V/mm and nonlinear coefficient of ˜61.3.

The Influence of Conditions on Synthesis Hydroxyapatite By Chemical Precipitation Method

NASA Astrophysics Data System (ADS)

Zhu, Jianping; Kong, Deshuang; Zhang, Yin; Yao, Nengjian; Tao, Yaqiu; Qiu, Tai

2011-10-01

Particles of Hydroxyapatite (HAp) were synthesized by means of chemical precipitation method, under atmosphere pressure. The starting solution with the Ca/P ratio of 1.67 was prepared by mixing 0.167 mol·dm-3 Ca(NO3)2·4H2O, 0.100 mol·dm-3 (NH4)2HPO4, 0.500 mol·dm-3 (NH2)2CO and 0.10 mol·dm-3 HNO3 aqueous solutions. The hydroxyapatite were prepared by heating the solution at 80 °C for 24 hour and then at 90°C for 72 hour. Then followed, the dry powers were heat treatment at 660°C temperatures for 8 hour. The obtained powder was analyzed using XRD, XRF, FT-IR, SEM, TG-DTA. The results showed that obtained HAp powers were greatly influenced by synthetic conditions. HAp powders with various morphologies, such as sphere, rod, layered, dumbbell, fibre, scaly, were obtained by controlling the synthetic conditions.

Preparation of Three-Dimensional Graphene Foams Using Powder Metallurgy Templates.

PubMed

Sha, Junwei; Gao, Caitian; Lee, Seoung-Ki; Li, Yilun; Zhao, Naiqin; Tour, James M

2016-01-26

A simple and scalable method which combines traditional powder metallurgy and chemical vapor deposition is developed for the synthesis of mesoporous free-standing 3D graphene foams. The powder metallurgy templates for 3D graphene foams (PMT-GFs) consist of particle-like carbon shells which are connected by multilayered graphene that shows high specific surface area (1080 m(2) g(-1)), good crystallization, good electrical conductivity (13.8 S cm(-1)), and a mechanically robust structure. The PMT-GFs did not break under direct flushing with DI water, and they were able to recover after being compressed. These properties indicate promising applications of PMT-GFs for fields requiring 3D carbon frameworks such as in energy-based electrodes and mechanical dampening.

A Spatially Offset Raman Spectroscopy Method for Non-Destructive Detection of Gelatin-Encapsulated Powders

PubMed Central

Chao, Kuanglin; Dhakal, Sagar; Qin, Jianwei; Peng, Yankun; Schmidt, Walter F.; Kim, Moon S.; Chan, Diane E.

2017-01-01

Non-destructive subsurface detection of encapsulated, coated, or seal-packaged foods and pharmaceuticals can help prevent distribution and consumption of counterfeit or hazardous products. This study used a Spatially Offset Raman Spectroscopy (SORS) method to detect and identify 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. As the offset distance was increased, the spectral contribution from the subsurface powder gradually outweighed that of the surface capsule layers, allowing for detection of the encapsulated powders. Containing mixed contributions from the powder and capsule, the SORS spectra for each sample were resolved into pure component spectra using self-modeling mixture analysis (SMA) and the corresponding components were identified using spectral information divergence values. As demonstrated here for detecting chemicals contained inside thick capsule layers, this SORS measurement technique coupled with SMA has the potential to be a reliable non-destructive method for subsurface inspection and authentication of foods, health supplements, and pharmaceutical products that are prepared or packaged with semi-transparent materials. PMID:28335453

Method of manufacturing metallic products such as sheet by cold working and flash anealing

DOEpatents

Hajaligol, Mohammad R.; Sikka, Vinod K.

2001-01-01

A metallic alloy composition is manufactured into products such as press formed or stamped products or rolled products such as sheet, strip, rod, wire or band by one or more cold working steps with intermediate or final flash annealing. The method can include cold rolling an iron, nickel or titanium aluminide alloy and annealing the cold worked product in a furnace by infrared heating. The flash annealing is preferably carried out by rapidly heating the cold worked product to an elevated temperature for less than one minute. The flash annealing is effective to reduce surface hardness of the cold worked product sufficiently to allow further cold working. The product to be cold worked can be prepared by casting the alloy or by a powder metallurgical technique such as tape casting a mixture of metal powder and a binder, roll compacting a mixture of the powder and a binder or plasma spraying the powder onto a substrate. In the case of tape casting or roll compaction, the initial powder product can be heated to a temperature sufficient to remove volatile components. The method can be used to form a cold rolled sheet which is formed into an electrical resistance heating element capable of heating to 900.degree. C. in less than 1 second when a voltage up to 10 volts and up to 6 amps is passed through the heating element.

Method of manufacturing metallic products such as sheet by cold working and flash annealing

DOEpatents

Hajaligol, Mohammad R.; Sikka, Vinod K.

2000-01-01

A metallic alloy composition is manufactured into products such as press formed or stamped products or rolled products such as sheet, strip, rod, wire or band by one or more cold working steps with intermediate or final flash annealing. The method can include cold rolling an iron, nickel or titanium aluminide alloy and annealing the cold worked product in a furnace by infrared heating. The flash annealing is preferably carried out by rapidly heating the cold worked product to an elevated temperature for less than one minute. The flash annealing is effective to reduce surface hardness of the cold worked product sufficiently to allow further cold working. The product to be cold worked can be prepared by casting the alloy or by a powder metallurgical technique such as tape casting a mixture of metal powder and a binder, roll compacting a mixture of the powder and a binder or plasma spraying the powder onto a substrate. In the case of tape casting or roll compaction, the initial powder product can be heated to a temperature sufficient to remove volatile components. The method can be used to form a cold rolled sheet which is formed into an electrical resistance heating element capable of heating to 900.degree. C. in less than 1 second when a voltage up to 10 volts and up to 6 amps is passed through the heating element.

Studies on aluminium leaching from cookware in tea and coffee and estimation of aluminium content in toothpaste, baking powder and paan masala.

PubMed

Rajwanshi, P; Singh, V; Gupta, M K; Kumari, V; Shrivastav, R; Ramanamurthy, M; Dass, S

1997-01-30

Studies were conducted in order to assess the level of aluminium (Al) in samples of Indian tea, coffee, toothpaste, paan masala (mouth freshener) and baking powder. Leaching of Al from cookware while preparing tea and coffee was also studied. Experiments were also conducted to study the sequential leaching of Al from cookware by preparing tea and coffee in the presence of standard size Al sheets (coupons). A small amount of Al was found to have leached from coupons during preparation of tea. Tea leaves, were found to be a rich source of Al and a maximum of 2.2% Al is extracted in tea infusions. Coffee powder on the other hand was not found to be a rich source of Al. Baking powder was found to be a rich source of Al and 1 kg of cake prepared with 1-3 teaspoon of baking powder may contain 2-12.7 mg of Al in each serving (25 g). Toothpaste also contains a significant quantity of Al, more so, when packed in Al tubes. Ingestion pattern of Al from these items by humans is also discussed.

Storage stability of cauliflower soup powder: The effect of lipid oxidation and protein degradation reactions.

PubMed

Raitio, Riikka; Orlien, Vibeke; Skibsted, Leif H

2011-09-15

Soups based on cauliflower soup powders, prepared by dry mixing of ingredients and rapeseed oil, showed a decrease in quality, as evaluated by a sensory panel, during the storage of the soup powder in the dark for up to 12weeks under mildly accelerated conditions of 40°C and 75% relative humidity. Antioxidant, shown to be effective in protecting the rapeseed bulk oil, used for the powder preparation, had no effect on storage stability of the soup powder. The freshly prepared soup powder had a relatively high concentration of free radicals, as measured by electron spin resonance spectroscopy, which decreased during storage, and most remarkably during the first two weeks of storage, with only marginal increase in lipid hydroperoxides as primary lipid oxidation products, and without any increase in secondary lipid oxidation products. Analyses of volatiles by SPME-GC-MS revealed a significant increase in concentrations of 2-methyl- and 3-methyl butanals, related to Maillard reactions, together with an increase in 2-acetylpyrrole concentration. The soup powders became more brown during storage, as indicated by a decreasing Hunter L-value, in accord with non-enzymatic browning reactions. A significant increase in the concentrations of dimethyl disulfide in soup powder headspace indicated free radical-initiated protein oxidation. Protein degradation, including Maillard reactions and protein oxidation, is concluded to be more important than lipid oxidation in determining the shelf-life of dry cauliflower soup powder. Copyright © 2011 Elsevier Ltd. All rights reserved.

Preparation of lead-zirconium-titanium film and powder by electrodeposition

DOEpatents

Bhattacharya, Raghu N.; Ginley, David S.

1995-01-01

A process for the preparation of lead-zirconium-titanium (PZT) film and powder compositions. The process comprises the steps of providing an electrodeposition bath, providing soluble salts of lead, zirconium and titanium metals to this bath, electrically energizing the bath to thereby direct ions of each respective metal to a substrate electrode and cause formation of metallic particles as a recoverable film of PZT powder on the electrode, and also recovering the resultant film as a powder. Recovery of the PZT powder can be accomplished by continually energizing the bath to thereby cause powder initially deposited on the substrate-electrode to drop therefrom into the bath from which it is subsequently removed. A second recovery alternative comprises energizing the bath for a period of time sufficient to cause PZT powder deposition on the substrate-electrode only, from which it is subsequently recovered. PZT film and powder so produced can be employed directly in electronic applications, or the film and powder can be subsequently oxidized as by an annealing process to thereby produce lead-zirconium-titanium oxide for use in electronic applications.

Preparation of lead-zirconium-titanium film and powder by electrodeposition

DOEpatents

Bhattacharya, R.N.; Ginley, D.S.

1995-10-31

A process is disclosed for the preparation of lead-zirconium-titanium (PZT) film and powder compositions. The process comprises the steps of providing an electrodeposition bath, providing soluble salts of lead, zirconium and titanium metals to this bath, electrically energizing the bath to thereby direct ions of each respective metal to a substrate electrode and cause formation of metallic particles as a recoverable film of PZT powder on the electrode, and also recovering the resultant film as a powder. Recovery of the PZT powder can be accomplished by continually energizing the bath to thereby cause powder initially deposited on the substrate-electrode to drop therefrom into the bath from which it is subsequently removed. A second recovery alternative comprises energizing the bath for a period of time sufficient to cause PZT powder deposition on the substrate-electrode only, from which it is subsequently recovered. PZT film and powder so produced can be employed directly in electronic applications, or the film and powder can be subsequently oxidized as by an annealing process to thereby produce lead-zirconium-titanium oxide for use in electronic applications. 4 figs.

Solution combustion method for synthesis of nanostructured hydroxyapatite, fluorapatite and chlorapatite

NASA Astrophysics Data System (ADS)

Zhao, Junjie; Dong, Xiaochen; Bian, Mengmeng; Zhao, Junfeng; Zhang, Yao; Sun, Yue; Chen, JianHua; Wang, XuHong

2014-09-01

Hydroxyapatite (HAP), fluorapatite (Fap) and chlorapatite (Clap) were prepared by solution combustion method with further annealing at 800 °C. The characterization and structural features of the synthesized powders were evaluated by the powder X-ray diffraction (XRD, Fourier transform infrared spectroscopy (FT-IR), scanning electron microscope (SEM) and transmission electron microscopy (TEM) techniques. Characterization results from XRD and Rietveld analysis revealed that OH- in the HAP lattice were gradually substituted with the increase of F- and Cl- content and totally substituted at the molar concentration of 0.28 and 0.6, respectively. The results from FI-IR have also confirmed the incorporation of substituted anions in the apatite structure.

Porous titanium obtained by a new powder metallurgy technique: Preliminary results of human osteoblast adhesion on surface polished substrates.

PubMed

Biasotto, M; Ricceri, R; Scuor, N; Schmid, C; Sandrucci, M A; Di Lenarda, R; Matteazzi, P

2003-01-01

This study concerns a novel powder metallurgy method for producing porous titanium (pTi) exhibiting high mechanical properties. The preparation procedure consisted of the following stages: first, the preparation of Ti and titanium hydride (TiH2) powder mixtures and their consolidation with a cold isostatic press, followed by a sintering of the green bodies performed with hot isostatic press (HIP) equipment. Thermal decomposition in controlled environment of the TiH2 phase results in the foam structure. The resulting porosity percolates with a volume fraction of approximately 20%. The final material exhibits interesting mechanical properties, comparable to those of full density titanium (between grade 2 and grade 3), with the advantage of a minor density. The samples produced were tested to verify their biological response by studying the effectiveness of osteoblast adhesion and growth. In this preliminary study, osteoblastic cell morphology was investigated and compared to that observed on fully dense commercially pure titanium (Ti-cp) (ASTM, grade 3). The preliminary results were promising regarding cellular adhesion and spreading. (Journal of Applied Biomaterials & Biomechanics 2003; 1: 172-7).

Fabrication of carbonate apatite block based on internal dissolution-precipitation reaction of dicalcium phosphate and calcium carbonate.

PubMed

Daitou, Fumikazu; Maruta, Michito; Kawachi, Giichiro; Tsuru, Kanji; Matsuya, Shigeki; Terada, Yoshihiro; Ishikawa, Kunio

2010-05-01

In this study, we investigated a novel method for fabrication of carbonate apatite block without ionic movement between precursor and solution by using precursor that includes all constituent ions of carbonate apatite. A powder mixture prepared from dicalcium phosphate anhydrous and calcite at appropriate Ca/P ratios (1.5, 1.67, and 1.8) was used as starting material. For preparation of specimens, the slurry made from the powder mixture and distilled water was packed in a split stainless steel mold and heat - treated, ranging from 60 degrees C to 100 degrees C up to 48 hours at 100% humidity. It appeared that carbonate apatite could be obtained above 70 degrees C and monophasic carbonate apatite could be obtained from the powder mixture at Ca/P ratio of 1.67. Carbonate content of the specimen was about 5-7%. Diametral tensile strength of the carbonate apatite blocks slightly decreased with increasing treatment temperature. The decrease in diametral tensile strength is thought to be related to the crystal size of the carbonate apatite formed.

Structure of Al-Fe alloys prepared by different methods after severe plastic deformation under pressure

NASA Astrophysics Data System (ADS)

Dobromyslov, A. V.; Taluts, N. I.

2017-06-01

Al-Fe alloys prepared by casting, rapid quenching from the melt, and mechanical alloying from elemental powders have been studied using X-ray diffraction analysis, optical metallography, transmission electron microscopy, and microhardness measurements in the initial state and after severe plastic deformation by high-pressure torsion using Bridgman anvils. The relationship between the phase composition, microstructure, and the microhardness of the investigated alloys has been established.

Method of preparing thermal insulation for high temperature microwave sintering operations

DOEpatents

Holcombe, C.E.; Dykes, N.L.; Morrow, M.S.

1996-07-16

Superior microwave transparent thermal insulations for high temperature microwave sintering operations were prepared. One embodiment of the thermal insulation comprises granules of boron nitride coated with a very thin layer of glassy carbon made by preparing a glassy carbon precursor and blending it with boron nitride powder to form a mixture. The blended mixture is granulated to form a grit which is dried and heated to form the granules of boron nitride coated with a glassy carbon. Alternatively, grains of glassy carbon are coated with boron nitride by blending a mixture of a slurry comprising boron nitride, boric acid binder, and methyl alcohol with glassy carbon grains to form a blended mixture. The blended mixture is dried to form grains of glassy carbon coated with boron nitride. In addition, a physical mixture of boron nitride powder and glassy carbon grains has also been shown to be an excellent thermal insulation material for microwave processing and sintering. 1 fig.

Fabrication of PbFe12O19 nanoparticles and study of their structural, magnetic and dielectric properties

NASA Astrophysics Data System (ADS)

Mousavi Ghahfarokhi, S. E.; Rostami, Z. A.; Kazeminezhad, I.

2016-02-01

In this study, M-type Lead hexaferrite (PbFe12O19) nanoparticles were prepared by a sol-gel method and the prepared powders were annealed at 700-1000 °C for 1, 1.5, 2, 2.5 and 3 h. The Lead hexaferrite powders were characterized using thermogravimetry-differential thermal analysis, X-ray diffraction, scanning electron microscopy, LCR meter, vibrating sample magnetometer, and Fourier transforms infrared spectroscopy. The size of the nanoparticles was increased with the annealing temparature. The results reveal that the best annealing temperature and annealing time for preparing PbFe12O19 nanoparticles at 800 °C and 3 h are obtained. The infrared spectra measured in range of 4000-400 cm-1 exhibit stretching modes of metal ions in tetrahedral site at 580-550 cm-1 and octahedral site at 470-430 cm-1. The variation in ac conductivity (σac) with frequency shows that the electrical conductivity in these ferrites is mainly attributed to the electron hopping mechanism.

Synthesis of monodisperse spherical nanometer ZrO{sub 2} (Y{sub 2}O{sub 3}) powders via the coupling route of w/o emulsion with urea homogenous precipitation

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

Chang, Ying; Dong, Shijie, E-mail: dongsjsj@163.com; Wang, Huihu

2012-03-15

Graphical abstract: In this paper, the weight loss and reaction evolution of ZrO{sub 2} precursor powders are determined by TG-DTA, and 600 Degree-Sign C is the most reasonable calcination temperature of precursor according to the TG-DTA. At the same time, we study the effect of reaction conditions upon the particle sizes, such as concentration of zirconium nitrate solution, reaction temperature and urea content. TEM micrographs of zirconia powders indicated that ZrO{sub 2} nano-powders prepared via the coupling route of w/o emulsion with homogenous precipitation possess spherical shape and excellent dispersing. Highlights: Black-Right-Pointing-Pointer The monodisperse spherical nanometer ZrO{sub 2} (Y{sub 2}O{submore » 3}) powders have been prepared via the coupling route of w/o emulsion with urea homogenous precipitation. Black-Right-Pointing-Pointer The principle of the coupling route of emulsion with homogenous precipitation has been studied. Black-Right-Pointing-Pointer The concentration of zirconium nitrate, reaction temperature of water bath and the quantity of urea effect regularly on the average particle size of products. -- Abstract: Using xylol as the oil phase, span-80 as the surfactant, and an aqueous solution containing zirconium (3 mol% Y{sub 2}O{sub 3}) and urea as the water phase, tetragonal phase ZrO{sub 2} nano-powders have been prepared via the coupling route of w/o emulsion with urea homogenous precipitation. The effects of the zirconium concentration, the reaction temperature and the urea content on the average size of the products have been examined. The as-prepared ZrO{sub 2} powders and the precursor powders were characterized by TGA-DTA, XRD, TEM and BET. Experimental results indicate that ZrO{sub 2} powders prepared via the coupling route of w/o emulsion with urea homogenous precipitation possess some excellent characteristics, such as well-rounded spherical shape and excellent dispersing.« less

Low-Pressure and Low-Temperature Hydriding-Pulverization-Dehydriding Method for Producing Shape Memory Alloy Powders

NASA Astrophysics Data System (ADS)

Murguia, Silvia Briseño; Clauser, Arielle; Dunn, Heather; Fisher, Wendy; Snir, Yoav; Brennan, Raymond E.; Young, Marcus L.

2018-04-01

Shape memory alloys (SMAs) are of high interest as active, adaptive "smart" materials for applications such as sensors and actuators due to their unique properties, including the shape memory effect and pseudoelasticity. Binary NiTi SMAs have shown the most desirable properties, and consequently have generated the most commercial success. A major challenge for SMAs, in particular, is their well-known compositional sensitivity. Therefore, it is critical to control the powder composition and morphology. In this study, a low-pressure, low-temperature hydriding-pulverization-dehydriding method for preparing well-controlled compositions, size, and size distributions of SMA powders from wires is presented. Starting with three different diameters of as-drawn martensitic NiTi SMA wires, pre-alloyed NiTi powders of various well-controlled sizes are produced by hydrogen charging the wires in a heated H3PO4 solution. After hydrogen charging for different charging times, the wires are pulverized and subsequently dehydrided. The wires and the resulting powders are characterized using scanning electron microscopy, differential scanning calorimetry, and X-ray diffraction. The relationship between the wire diameter and powder size is investigated as a function of hydrogen charging time. The rate of diameter reduction after hydrogen charging of wire is also examined. Finally, the recovery behavior due to the shape memory effect is investigated after dehydriding.

Mg(1 + x)Ir(1 - x) (x = 0, 0.037 and 0.054), a binary intermetallic compound with a new orthorhombic structure type determined from powder and single-crystal X-ray diffraction.

PubMed

Cerný, Radovan; Renaudin, Guillaume; Favre-Nicolin, Vincent; Hlukhyy, Viktor; Pöttgen, Rainer

2004-06-01

The new binary compound Mg(1 + x)Ir(1 - x) (x = 0-0.054) was prepared by melting the elements in the Mg:Ir ratio 2:3 in a sealed tantalum tube under an argon atmosphere in an induction furnace (single crystals) or by annealing cold-pressed pellets of the starting composition Mg:Ir 1:1 in an autoclave under an argon atmosphere (powder sample). The structure was independently solved from high-resolution synchrotron powder and single-crystal X-ray data: Pearson symbol oC304, space group Cmca, lattice parameters from synchrotron powder data a = 18.46948 (6), b = 16.17450 (5), c = 16.82131 (5) A. Mg(1 + x)Ir(1 - x) is a topologically close-packed phase, containing 13 Ir and 12 Mg atoms in the asymmetric unit, and has a narrow homogeneity range. Nearly all the atoms have Frank-Kasper-related coordination polyhedra, with the exception of two Ir atoms, and this compound contains the shortest Ir-Ir distances ever observed. The solution of a rather complex crystal structure from powder diffraction, which was fully confirmed by the single-crystal method, shows the power of powder diffraction in combination with the high-resolution data and the global optimization method.

[Preparation of nano-nacre artificial bone].

PubMed

Chen, Jian-ting; Tang, Yong-zhi; Zhang, Jian-gang; Wang, Jian-jun; Xiao, Ying

2008-12-01

To assess the improvements in the properties of nano-nacre artificial bone prepared on the basis of nacre/polylactide acid composite artificial bone and its potential for clinical use. The compound of nano-scale nacre powder and poly-D, L-lactide acid (PDLLA) was used to prepare the cylindrical hollow artificial bone, whose properties including raw material powder scale, pore size, porosity and biomechanical characteristics were compared with another artificial bone made of micron-scale nacre powder and PDLLA. Scanning electron microscope showed that the average particle size of the nano-nacre powder was 50.4-/+12.4 nm, and the average pore size of the artificial bone prepared using nano-nacre powder was 215.7-/+77.5 microm, as compared with the particle size of the micron-scale nacre powder of 5.0-/+3.0 microm and the pore size of the resultant artificial bone of 205.1-/+72.0 microm. The porosities of nano-nacre artificial bone and the micron-nacre artificial bone were (65.4-/+2.9)% and (53.4-/+2.2)%, respectively, and the two artificial bones had comparable compressive strength and Young's modulus, but the flexural strength of the nano-nacre artificial bone was lower than that of the micro-nacre artificial bone. The nano-nacre artificial bone allows better biodegradability and possesses appropriate pore size, porosity and biomechanical properties for use as a promising material in bone tissue engineering.

Pharmaceutical and analytical evaluation of triphalaguggulkalpa tablets

PubMed Central

Savarikar, Shreeram S.; Barbhind, Maneesha M.; Halde, Umakant K.; Kulkarni, Alpana P.

2011-01-01

Aim of the Study: Development of standardized, synergistic, safe and effective traditional herbal formulations with robust scientific evidence can offer faster and more economical alternatives for the treatment of disease. The main objective was to develop a method of preparation of guggulkalpa tablets so that the tablets meet the criteria of efficacy, stability, and safety. Materials and Methods: Triphalaguggulkalpa tablet, described in sharangdharsanhita and containing guggul and triphala powder, was used as a model drug. Preliminary experiments on marketed triphalaguggulkalpa tablets exhibited delayed in vitro disintegration that indicated probable delayed in vivo disintegration. The study involved preparation of triphalaguggulkalpa tablets by Ayurvedic text methods and by wet granulation, dry granulation, and direct compression method. The tablets were evaluated for loss on drying, volatile oil content, % solubility, and steroidal content. The tablets were evaluated for performance tests like weight variation, disintegration, and hardness. Results: It was observed that triphalaguggulkalpa tablets, prepared by direct compression method, complied with the hardness and disintegration tests, whereas tablets prepared by Ayurvedic text methods failed. Conclusion: Direct compression is the best method of preparing triphalaguggulkalpa tablets. PMID:21731383

Physico-chemical characteristics and protein adsorption potential of hydroxyapatite particles: influence on in vitro biocompatibility of ceramics after sintering.

PubMed

Rouahi, M; Champion, E; Gallet, O; Jada, A; Anselme, K

2006-01-15

Through the example of two HA ceramics prepared from two HA powders (HAD and HAL), we explored the relation between the physico-chemical qualities of the initial HA powder and the final HA ceramic and their influence on the protein adsorption and cell response to the final HA ceramics. The powders were characterized by XRD, FT-IR, zeta potential, and specific surface area (SSA). Their protein adsorption potential was tested after immersion in culture medium +15% of fetal calf serum. These results were correlated with the protein adsorption potential of the two ceramics (cHAD and cHAL) prepared from the HAD and HAL powders respectively and to the cell attachment after 4, 24 and 72 h on the ceramics. From our results, it appears that a relation can be established between the physico-chemical characteristics of the initial HA powders and the final biological response to the sintered ceramics prepared from these powders. An inverse relation exists between the SSA and the protein adsorption capacity of HA powders and the protein adsorption and cell attachment on HA ceramics. This inverse relation is related to phenomenon occurring during the sintering phase and the formation of inter-granular micro-porosity.

21 CFR 522.1085 - Guaifenesin powder for injection.

Code of Federal Regulations, 2014 CFR

2014-04-01

... 21 Food and Drugs 6 2014-04-01 2014-04-01 false Guaifenesin powder for injection. 522.1085 Section... § 522.1085 Guaifenesin powder for injection. (a) Specifications. The product is a sterile powder containing guaifenesin. A solution is prepared by dissolving the drug in sterile water for injection to make...

21 CFR 176.350 - Tamarind seed kernel powder.

Code of Federal Regulations, 2014 CFR

2014-04-01

... 21 Food and Drugs 3 2014-04-01 2014-04-01 false Tamarind seed kernel powder. 176.350 Section 176... Paperboard § 176.350 Tamarind seed kernel powder. Tamarind seed kernel powder may be safely used as a component of articles intended for use in producing, manufacturing, packing, processing, preparing, treating...

Effects of N precursor on the agglomeration and visible light photocatalytic activity of N-doped TiO2 nanocrystalline powder.

PubMed

Hu, Yulong; Liu, Hongfang; Rao, Qiuhua; Kong, Xiaodong; Sun, Wei; Guo, Xingpeng

2011-04-01

N-doped TiO2 nanocrystalline powders were prepared by the sol-gel method using various N precursors, including triethylamine, hydrazine hydrate, ethylenediamine, ammonium hydroxide, and urea. The samples were characterized by X-ray diffraction, N2 adsorption isotherms, transmission electron microscopy, ultraviolet-visible diffuse reflectance spectroscopy, Fourier transform infrared spectroscopy, and X-ray photoelectron spectroscopy. The photocatalytic activities of as-prepared samples under irradiation of visible light (lambda > 405 nm) were evaluated by photodecomposition of methyl orange. The alkalinity of N precursor was found to play a key role in the gel process. The N precursor with moderate alkalinity causes TiO2 nanoparticles to be sol-transformed into a loosely agglomerated gel. This transformation facilitates the preparation of an N-doped TiO2 powder with small nanocrystal size, large specific surface area, and high N doping level and results in high visible light photocatalytic activity. The N in TiO2 with N is binding energy at 399-400 eV may be assigned to the N-H species located in interstitial sites of TiO2 lattice which is the active N species responsible for the visible light photocatalytic activity. The N species of N 1s peak at 402 and 405 eV are ineffective to the visible light photocatalytic activity and may inhibit the photocatalytic activity. Moreover, a TiO2 nanoparticle powder with large specific area can be achieved by using urea as a template and then by using ammonium hydroxide to transform the sol into gel.

Enhanced oral bioavailability of silymarin using liposomes containing a bile salt: preparation by supercritical fluid technology and evaluation in vitro and in vivo

PubMed Central

Yang, Gang; Zhao, Yaping; Zhang, Yongtai; Dang, Beilei; Liu, Ying; Feng, Nianping

2015-01-01

The aim of this investigation was to develop a procedure to improve the dissolution and bioavailability of silymarin (SM) by using bile salt-containing liposomes that were prepared by supercritical fluid technology (ie, solution-enhanced dispersion by supercritical fluids [SEDS]). The process for the preparation of SM-loaded liposomes containing a bile salt (SM-Lip-SEDS) was optimized using a central composite design of response surface methodology with the ratio of SM to phospholipids (w/w), flow rate of solution (mL/min), and pressure (MPa) as independent variables. Particle size, entrapment efficiency (EE), and drug loading (DL) were dependent variables for optimization of the process and formulation variables. The particle size, zeta potential, EE, and DL of the optimized SM-Lip-SEDS were 160.5 nm, −62.3 mV, 91.4%, and 4.73%, respectively. Two other methods to produce SM liposomes were compared to the SEDS method. The liposomes obtained by the SEDS method exhibited the highest EE and DL, smallest particle size, and best stability compared to liposomes produced by the thin-film dispersion and reversed-phase evaporation methods. Compared to the SM powder, SM-Lip-SEDS showed increased in vitro drug release. The in vivo AUC0−t of SM-Lip-SEDS was 4.8-fold higher than that of the SM powder. These results illustrate that liposomes containing a bile salt can be used to enhance the oral bioavailability of SM and that supercritical fluid technology is suitable for the preparation of liposomes. PMID:26543366

Effect of reductant and PVP on morphology and magnetic property of ultrafine Ni powders prepared via hydrothermal route

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

Zhang, Jun, E-mail: j-zhang@126.com; Wang, Xiucai; Li, Lili

2013-10-15

Graphical abstract: The ultrafine Ni powders with the shapes including sphere, pearl-string, leaf, fish-bone, hexagonal sheet and silknet were prepared through one-step hydrothermal reduction using different reductants. Their saturation magnetization, remanent magnetization and coercivity sequentially increase, and the coercivity of hexagonal sheet-like Ni powders increases by 25% compared with the Ni bulk counterpart. - Highlights: • The ultrafine Ni powders with various shapes of sphere, fish-bone, hexagonal sheet, etc. • Facile and one-step hydrothermal reduction using three reductants and PVP additive was developed. • Magnetic properties of the ultrafine Ni powders with different shapes were measured. • Compared with bulkmore » Ni material, coercivity of hexagonal sheet Ni increases by 25%. • The formation mechanism of the shapes was suggested. - Abstract: The ultrafine nickel particles with different shapes including sphere, pearl-string, leaf, fish-bone, hexagonal sheet and silknet were prepared through one-step hydrothermal reduction using hydrazine hydrate, sodium hypophosphite and ethylene glycol as reductants, polyvinylpyrrolidone as structure-directing agent. It has been verified with the characterization of X-ray powder diffraction and transmission/scanning electronic microscopy that as-prepared products belong to face-centered cubic structure of nickel microcrystals with high purity and fine dispersity. The magnetic hysteresis loops measured at room temperature reveal that the values of saturation magnetization, remanent magnetization and coercivity rise sequentially from silknet, sphere to hexagonal sheet. In comparison with nickel bulk counterpart, the coercivity of the hexagonal sheet nickel powders increases by 25%.« less

Dry powder process for preparing uni-tape prepreg from polymer powder coated filamentary towpregs

NASA Technical Reports Server (NTRS)

Wilkinson, Steven P. (Inventor); Johnston, Norman J. (Inventor); Marchello, Joseph M. (Inventor)

1997-01-01

A process for preparing uni-tape prepreg from polymer powder coated filamentary towpregs is provided. A plurality of polymer powder coated filamentary towpregs are provided. The towpregs are collimated so that each towpreg is parallel. A material is applied to each side of the towpreg to form a sandwich. The sandwich is heated to a temperature wherein the polymer flows and intimately contacts the filaments and pressure is repeatedly applied perpendicularly to the sandwich with a longitudinal oscillating action wherein the filaments move apart and the polymer wets the filaments forming a uni-tape prepreg. The uni-tape prepreg is subsequently cooled.

Synthesis and Characterization of BaFe12O19 Thin Films Using Suspension of Nano Powders

NASA Astrophysics Data System (ADS)

Salemizadeh, Saman; Seyyed Ebrahimi, S. A.

BaM thin films have been synthesized by dispersing the dried gel nano powders prepared by Sol-Gel method. The solution was made by dissolving iron nitrate Fe(NO3).9H2O, barium nitrate Ba(NO3)2 and citric acid in deyonized water and methanol. This sol was slowly evaporated until a dried gel was formed. This dried gel was then added to ethylene glycol. The final solution was vigorously shaken and mixed in ultrasonic cleaner for 30 min to disperse particles sufficiently. Then the prepared solution spin coated on Si(110) substrate. The obtained thin films were dried at 120 °C and then calcined at 900 °C for 1 h. The films were characterized using X-ray diffraction (XRD) and vibrating sample magnetometer (VSM).

Synthesis and structural characterization of Co2+ ions doped ZnO nanopowders by solid state reaction through sonication

NASA Astrophysics Data System (ADS)

Babu, B.; Rama Krishna, Ch.; Venkata Reddy, Ch.; Pushpa Manjari, V.; Ravikumar, R. V. S. S. N.

2013-05-01

Cobalt ions doped zinc oxide nanopowder was prepared at room temperature by a novel and simple one step solid-state reaction method through sonication in the presence of a suitable surfactant Sodium Lauryl Sulphate (SLS). The prepared powder was characterized by various spectroscopic techniques. Powder XRD data revealed that the crystal structure belongs to hexagonal and its average crystallite size was evaluated. From optical absorption data, crystal fields (Dq), inter-electronic repulsion parameters (B, C) were evaluated. By correlating optical and EPR spectral data, the site symmetry of Co2+ ion in the host lattice was determined as octahedral. Photoluminescence spectra exhibited the emission bands in ultraviolet and blue regions. The CIE chromaticity coordinates are also evaluated from the emission spectrum. FT-IR spectra showed the characteristic vibrational bands of Znsbnd O.

Method of preparing a sintered lithium aluminate structure for containing electrolyte

DOEpatents

Sim, James W.; Kinoshita, Kimio

1981-01-01

A porous sintered tile is formed of lithium aluminate for retaining molten lectrolyte within a fuel cell. The tile is prepared by reacting lithium hydroxide in aqueous solution with alumina particles to form beta lithium aluminate particles. The slurry is evaporated to dryness and the solids dehydrated to form a beta lithium aluminate powder. The powder is compacted into the desired shape and sintered at a temperature in excess of 1200 K. but less than 1900 K. to form a porous integral structure that is subsequently filled with molten electrolyte. A tile of this type is intended for use in containing molten alkali metal carbonates as electolyte for use in a fuel cell having porous metal or metal oxide electrodes for burning a fuel gas such as hydrogen and/or carbon monoxide with an oxidant gas containing oxygen.

Room temperature synthesis of agarose/sol-gel glass pieces with tailored interconnected porosity.

PubMed

Cabañas, M V; Peña, J; Román, J; Vallet-Regí, M

2006-09-01

An original shaping technique has been applied to prepare porous bodies at room temperature. Agarose, a biodegradable polysaccharide, was added as binder of a sol-gel glass in powder form, yielding an easy to mold paste. Interconnected tailored porous bodies can be straightforwardly prepared by pouring the slurry into a polymeric scaffold, previously designed by stereolitography, which is subsequently eliminated by alkaline dissolution at room temperature. The so obtained pieces behave like a hydrogel with an enhanced consistency that makes them machinable and easy to manipulate. These materials generate an apatite-like layer when immersed in a simulated body fluid, indicating a potential in vivo bioactivity. The proposed method can be applied to different powdered materials to produce pieces, at room temperature, with various shapes and sizes and with tailored interconnected porosity.

[The effect of composition and structure of radiological equivalent materials on radiological equivalent].

PubMed

Wang, Y; Lin, D; Fu, T

1997-03-01

Morphology of inorganic material powders before and after being treated by ultrafine crush was observed by transformite electron microscope. The length and diameter of granules were measured. Polymers inorganic material powders before and after being treated by ultrafine crush were used for preparing radiological equivalent materials. Blending compatibility of inorganic meterials with polymer materials was observed by scanning electron microscope. CT values of tissue equivalent materials were measured by X-ray CT. Distribution of inorganic materials was examined. The compactness of materials was determined by the water absorbed method. The elastic module of materials was measured by laser speckle interferementry method. The results showed that the inorganic material powders treated by the ultrafine crush blent well with polymer and the distribution of these powders in the polymer was homogeneous. The equivalent errors of linear attenuation coefficients and CT values of equivalent materials were small. Their elastic modules increased one order of magnitude from 6.028 x 10(2) kg/cm2 to 9.753 x 10(3) kg/cm2. In addition, the rod inorganic material powders having rod granule blent easily with polymer. The present study provides a theoretical guidance and experimental basis for the design and synthesis of radiological equivalent materials.

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.

Preparation of thermally stable nanocrystalline hydroxyapatite by hydrothermal method.

PubMed

Prakash Parthiban, S; Elayaraja, K; Girija, E K; Yokogawa, Y; Kesavamoorthy, R; Palanichamy, M; Asokan, K; Narayana Kalkura, S

2009-12-01

Thermally stable hydroxyapatite (HAp) was synthesized by hydrothermal method in the presence of malic acid. X-ray diffraction (XRD), Fourier transform infra-red spectroscopy (FT-IR), Raman spectroscopy, scanning electron microscopy (SEM), differential thermal analysis (DTA), thermogravimetric analysis (TGA) was done on the synthesized powders. These analyses confirmed the sample to be free from impurities and other phases of calcium phosphates, and were of rhombus morphology along with nanosized particles. IR and Raman analyses indicated the adsorption of malic acid on HAp. Thermal stability of the synthesized HAp was confirmed by DTA and TGA. The synthesized powders were thermally stable upto 1,400 degrees C and showed no phase change. The proposed method might be useful for producing thermally stable HAp which is a necessity for high temperature coating applications.

Polymer Infiltration Studies

NASA Technical Reports Server (NTRS)

Marchello, Joseph M.

1991-01-01

Progress was made on the preparation of carbon fiber composites using advanced polymer resins. Processes reported include powder towpreg process, weaving towpreg made from dry powder prepreg, composite from powder coated towpreg, and toughening of polyimide resin (PMR) composites by semi-interpenetrating networks. Several important areas of polymer infiltration into fiber bundles will be researched. Preparation to towpreg for textile preform weaving and braiding and for automated tow placement is a major goal, as are the continued development of prepregging technology and the various aspects of composite part fabrication.

In-situ Preparation of Polymer-Coated Zirconia Nanoparticles by Decomposition of Zirconium-Tert-Butoxide

DTIC Science & Technology

2003-01-01

coated under conditions C are slightly yellow coloured. The zirconia powders collected at position 1 is white. Table I: Plasma parameters of the...pulsed) 99 1 39 40 2,5 2,5 379 400D. 2000 1000 - 20 0 40 4 140 20 [°1 Figure 2: XRD diffractrogram of zirconia powder coated with polymer Zirconia...wave nunter [crn"] Figure 3: FTIR spectra of plasma treated zirconia powders collected at position 2 (coated) prepared under A) continuous plasma B

Phase transformation of TiO2 powder prepared by TiCl4 hydrolysis-electrolysis

NASA Astrophysics Data System (ADS)

Nur, Adrian; Purwanto, Agus; Jumari, Arif; Dyartanti, Endah R.; A. N., Richard Leonardo; Gultom, Barry Januari

2017-01-01

Metal oxide combined with graphite becomes an interesting composition. TiO2 is a good candidate for Li ion battery anode because of low cost, availability sufficient, and environmentally friendly. The form of TiO2 crystals is highly depended on the synthesis method used. The electrochemical method is beginning to emerge as a valuable option for preparing TiO2 powders. Using the electrochemical method, the particle phase can easily be controlled by simply adjusting the imposed current or potential to the system. The present work aims to investigate the effects of electrode distance in the electrolysis of TiCl4 solution to the phase transformation of anatase to rutile. The homogeneous solution for the electro-synthesis of TiO2 powders was TiCl4 in ethanol solution. The electrolysis was carried out in an electrochemical cell consisting of two carbon electrodes with dimensions of (5×2) cm. The electrodes were set parallel with various distances of 2.6 cm, 3 cm, and 4 cm between the electrodes and were immersed in the electrolytic solution at a depth of 2 cm. The electrodes were connected to the positive and negative terminals of a DC power supply (Zhaoxin PS-3005D). The electro-synthesis was performed galvanostatically at 2.5 hours and a voltage 10 V under constant stirring at room temperature. Phase transformation from anatase to rutile occurred at 2.6 cm to 3 cm electrode distance.

Use of Powder PEG-3350 as a Sole Bowel Preparation: Clinical Case Series of 245 Patients.

PubMed

Arora, Manish; Okolo, Patrick I

2008-07-01

To assess the efficacy of low-volume powder polyethylene glycol (PEG)-3350 as a sole bowel preparation for colonoscopy. This case series examined 245 consecutive patients (a mixture of inpatients and outpatients undergoing screening colonoscopy) at a hospital endoscopy center over a 2-year period. The patients received powder PEG-3350 in the amount of 204 g dissolved in 32 oz of water and taken in 3 divided doses 1 hour apart with 8 oz of water in between each dose. Colon preparation scores (CPS) were used to assess the quality of colon cleansing. The results obtained from the 245 patients were collated and compared to those of patients receiving sodium phosphate, the historical control. The mean CPS was calculated to be 3.43, with a standard deviation of 1.12. Of the 245 patients, 92 were scored with a grade of 4, and 5 patients had incomplete colonoscopies secondary to failure of bowel preparation (CPS=0). Among the remaining patients, 22 and 26 were graded as poor (CPS=1) or fair (CPS=2) bowel preparations, respectively. The low-volume powder PEG-3350 formula used in our case series showed effective colon cleansing and may be considered for use as a sole bowel preparation.

Titania nanotube powders obtained by rapid breakdown anodization in perchloric acid electrolytes

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

Ali, Saima, E-mail: saima.ali@aalto.fi; Hannula, Simo-Pekka

Titania nanotube (TNT) powders are prepared by rapid break down anodization (RBA) in a 0.1 M perchloric acid (HClO{sub 4}) solution (Process 1), and ethylene glycol (EG) mixture with HClO{sub 4} and water (Process 2). A study of the as-prepared and calcined TNT powders obtained by both processes is implemented to evaluate and compare the morphology, crystal structure, specific surface area, and the composition of the nanotubes. Longer TNTs are formed in Process 1, while comparatively larger pore diameter and wall thickness are obtained for the nanotubes prepared by Process 2. The TNTs obtained by Process 1 are converted tomore » nanorods at 350 °C, while nanotubes obtained by Process 2 preserve tubular morphology till 350 °C. In addition, the TNTs prepared by an aqueous electrolyte have a crystalline structure, whereas the TNTs obtained by Process 2 are amorphous. Samples calcined till 450 °C have XRD peaks from the anatase phase, while the rutile phase appears at 550 °C for the TNTs prepared by both processes. The Raman spectra also show clear anatase peaks for all samples except the as-prepared sample obtained by Process 2, thus supporting the XRD findings. FTIR spectra reveal the presence of O-H groups in the structure for the TNTs obtained by both processes. However, the presence is less prominent for annealed samples. Additionally, TNTs obtained by Process 2 have a carbonaceous impurity present in the structure attributed to the electrolyte used in that process. While a negligible weight loss is typical for TNTs prepared from aqueous electrolytes, a weight loss of 38.6% in the temperature range of 25–600 °C is found for TNTs prepared in EG electrolyte (Process 2). A large specific surface area of 179.2 m{sup 2} g{sup −1} is obtained for TNTs prepared by Process 1, whereas Process 2 produces nanotubes with a lower specific surface area. The difference appears to correspond to the dimensions of the nanotubes obtained by the two processes. - Graphical abstract: Titania nanotube powders prepared by Process 1 and Process 2 have different crystal structure and specific surface area. - Highlights: • Titania nanotube (TNT) powder is prepared in low water organic electrolyte. • Characterization of TNT powders prepared from aqueous and organic electrolyte. • TNTs prepared by Process 1 are crystalline with higher specific surface area. • TNTs obtained by Process 2 have carbonaceous impurities in the structure.« less

NanoClusters Enhance Drug Delivery in Mechanical Ventilation

NASA Astrophysics Data System (ADS)

Pornputtapitak, Warangkana

The overall goal of this thesis was to develop a dry powder delivery system for patients on mechanical ventilation. The studies were divided into two parts: the formulation development and the device design. The pulmonary system is an attractive route for drug delivery since the lungs have a large accessible surface area for treatment or drug absorption. For ventilated patients, inhaled drugs have to successfully navigate ventilator tubing and an endotracheal tube. Agglomerates of drug nanoparticles (also known as 'NanoClusters') are fine dry powder aerosols that were hypothesized to enable drug delivery through ventilator circuits. This Thesis systematically investigated formulations of NanoClusters and their aerosol performance in a conventional inhaler and a device designed for use during mechanical ventilation. These engineered powders of budesonide (NC-Bud) were delivered via a MonodoseRTM inhaler or a novel device through commercial endotracheal tubes, and analyzed by cascade impaction. NC-Bud had a higher efficiency of aerosol delivery compared to micronized stock budesonide. The delivery efficiency was independent of ventilator parameters such as inspiration patterns, inspiration volumes, and inspiration flow rates. A novel device designed to fit directly to the ventilator and endotracheal tubing connections and the MonodoseRTM inhaler showed the same efficiency of drug delivery. The new device combined with NanoCluster formulation technology, therefore, allowed convenient and efficient drug delivery through endotracheal tubes. Furthermore, itraconazole (ITZ), a triazole antifungal agent, was formulated as a NanoCluster powder via milling (top-down process) or precipitation (bottom-up process) without using any excipients. ITZ NanoClusters prepared by wet milling showed better aerosol performance compared to micronized stock ITZ and ITZ NanoClusters prepared by precipitation. ITZ NanoClusters prepared by precipitation methods also showed an amorphous state while milled ITZ NanoClusters maintained the crystalline character. Overall, NanoClusters prepared by various processes represent a potential engineered drug particle approach for inhalation therapy since they provide effective aerosol properties and stability due to the crystalline state of the drug powders. Future work will continue to explore formulation and delivery performance in vitro and in vivo..

Phase Stabilization of Zirconia.

DTIC Science & Technology

1997-01-30

preparing stabilized zirconia pursuant to this disclosure, an insoluble alumina powder is mixed with zirconia powder using a liquid dispersant, such...in a drying oven or a furnace. When mixing the alumina and zirconia powders , it is not necessary to have zirconia in any particular phase to achieve...phase stabilization, as disclosed herein. When mixed with alumina powder, zirconia powder can be in cubic, tetragonal or 20 monoclinic phases

Setting Ideal Lubricant Mixing Time for Manufacturing Tablets by Evaluating Powder Flowability.

PubMed

Nakamura, Shohei; Yamaguchi, Saori; Hiraide, Rikiha; Iga, Kumi; Sakamoto, Takatoshi; Yuasa, Hiroshi

2017-10-01

We investigated the effectiveness of using Carr's flowability index (FI) and practical angle of internal friction (Φ) as indexes for setting the target Mg-St mixing time needed for preparing tablets with the target physical properties. We used FI as a measure of flowability under non-loaded conditions, and Φ as a measure of flowability under loaded conditions for pharmaceutical powders undergoing direct compression with varying concentrations of Mg-St and mixing times. We evaluated the relationship between Mg-St mixing conditions and pharmaceutical powder flowability, analyzed the correlation between the physical properties of the tablets (i.e., tablet weight variation, drug content uniformity, hardness, friability, and disintegration time of tablets prepared using the pharmaceutical powder), and studied the effect of Mg-St mixing conditions and pharmaceutical powder flowability on tablet properties. Mg-St mixing time highly correlated with pharmaceutical powder FI (R 2  = 0.883) while Mg-St concentration has low correlation with FI, and FI highly correlated with the physical properties of the tablet (R 2 values: weight variation 0.509, drug content variation 0.314, hardness 0.525, friability 0.477, and disintegration time 0.346). Therefore, using pharmaceutical powder FI as an index could enable prediction of the physical properties of a tablet without the need for tableting, and setting the Mg-St mixing time by using pharmaceutical powder FI could enable preparation of tablets with the target physical properties. Thus, the FI of the intermediate product (i.e., pharmaceutical powder) is an effective index for controlling the physical properties of the finished tablet.

Versatility of Evaporation-Induced Self-Assembly (EISA) Method for Preparation of Mesoporous TiO2 for Energy and Environmental Applications

PubMed Central

Mahoney, Luther; Koodali, Ranjit T.

2014-01-01

Evaporation-Induced Self-Assembly (EISA) method for the preparation of mesoporous titanium dioxide materials is reviewed. The versatility of EISA method for the rapid and facile synthesis of TiO2 thin films and powders is highlighted. Non-ionic surfactants such as Pluronic P123, F127 and cationic surfactants such as cetyltrimethylammonium bromide have been extensively employed for the preparation of mesoporous TiO2. In particular, EISA method allows for fabrication of highly uniform, robust, crack-free films with controllable thickness. Eleven characterization techniques for elucidating the structure of the EISA prepared mesoporous TiO2 are discussed in this paper. These many characterization methods provide a holistic picture of the structure of mesoporous TiO2. Mesoporous titanium dioxide materials have been employed in several applications that include Dye Sensitized Solar Cells (DSSCs), photocatalytic degradation of organics and splitting of water, and batteries. PMID:28788590

Osmotic load from glucose polymers.

PubMed

Koo, W W; Poh, D; Leong, M; Tam, Y K; Succop, P; Checkland, E G

1991-01-01

Glucose polymer is a carbohydrate source with variable chain lengths of glucose units which may result in variable osmolality. The osmolality of two commercial glucose polymers was measured in reconstituted powder infant formulas, and the change in osmolality of infant milk formulas at the same increases in energy density (67 kcal/dL to 81 and 97 kcal/dL) from the use of additional milk powder or glucose polymers was compared. All samples were prepared from powders (to nearest 0.1 mg), and osmolality was measured by freezing point depression. For both glucose polymers the within-batch variability of the measured osmolality was less than 3.5%, and between-batch variability of the measured osmolality was less than 9.6%. The measured osmolality varies linearly with energy density (p less than 0.001) and was highest in infant formula reconstituted from milk powder alone. However, there exist significant differences in the measured osmolality between different glucose polymer preparations. At high energy densities (greater than or equal to 97 kcal/dL), infant milk formulas prepared with milk powder alone or with the addition of certain glucose polymer preparation may have high osmolality (greater than or equal to 450 mosm/kg) and theoretically predispose the infant to complications of hyperosmotic feeds.

Photocatalytic properties of h-WO3 nanoparticles obtained by annealing and h-WO3 nanorods prepared by hydrothermal method

NASA Astrophysics Data System (ADS)

Boyadjiev, Stefan I.; Nagy-Kovács, Teodóra; Lukács, István; Szilágyi, Imre M.

2016-03-01

In the present study, two different methods for preparing hexagonal WO3 (h-WO3) photocatalysts were used - controlled thermal decomposition and hydrothermal synthesis. WO3 nanoparticles with hexagonal structure were obtained by annealing (NH4)xWO3-y at 500 °C in air. WO3 nanorods were prepared by a hydrothermal method using sodium tungstate Na2WO4, HCl, (COOH)2 and NaSO4 precursors at 200 °C. The formation, morphology, structure and composition of the as-prepared nanoparticles and nanorods were studied by powder X-ray diffraction (XRD), transmission electron microscopy (TEM), and scanning electron microscopy combined with energy-dispersive X-ray spectroscopy (SEM-EDX). The photocatalytic activity of the h-WO3 nanoparticles and nanorods was studied by decomposing methyl orange in aqueous solution under UV light irradiation.

Facile synthesis of multi-shell structured binary metal oxide powders with a Ni/Co mole ratio of 1:2 for Li-Ion batteries

NASA Astrophysics Data System (ADS)

Choi, Seung Ho; Park, Sun Kyu; Lee, Jung-Kul; Kang, Yun Chan

2015-06-01

Multi-shell structured binary transition metal oxide powders with a Ni/Co mole ratio of 1:2 are prepared by a simple spray drying process. Precursor powder particles prepared by spray drying from a spray solution of citric acid and ethylene glycol have completely spherical shape, fine size, and a narrow size distribution. The precursor powders turn into multi-shell powders after a post heat-treatment at temperatures between 250 and 800 °C. The multi-shell structured powders are formed by repeated combustion and contraction processes. The multi-shell powders have mixed crystal structures of Ni1-xCo2O4-x and NiO phases regardless of the post-treatment temperature. The reversible capacities of the powders post-treated at 250, 400, 600, and 800 °C after 100 cycles are 584, 913, 808, and 481 mA h g-1, respectively. The low charge transfer resistance and high lithium ion diffusion rate of the multi-shell powders post-treated at 400 °C with optimum grain size result in superior electrochemical properties even at high current densities.

Upconversion luminescence in BaMoO{sub 4}:Pr{sup 3+} phosphor for display devices

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

Soni, Abhishek Kumar; Rai, Vineet Kumar, E-mail: vineetkrrai@yahoo.co.in

2015-08-28

The frequency upconversion is an important nonlinear optical property by which near infrared light is converted into the visible light. The BaMoO{sub 4}:Pr{sup 3+} powder phosphor has been synthesized by solid state reaction method. The upconversion emission bands are recorded under the excitation of 808 nm diode laser. The phase formation of the prepared phosphor has been identified by powder X-ray diffraction (XRD) technique. The upconversion emission mechanism and colour coordinate have been explained by using energy level and CIE (International Commission on Illumination) chromaticity diagram study, respectively.

Eu-Doped BaTiO3 Powder and Film from Sol-Gel Process with Polyvinylpyrrolidone Additive

PubMed Central

García-Hernández, Margarita; García-Murillo, Antonieta; de J. Carrillo-Romo, Felipe; Jaramillo-Vigueras, David; Chadeyron, Geneviève; De la Rosa, Elder; Boyer, Damien

2009-01-01

Transparent BaTiO3:Eu3+ films were prepared via a sol-gel method and dip-coating technique, using barium acetate, titanium butoxide, and polyvinylpyrrolidone (PVP) as modifier viscosity. BaTiO3:Eu3+ films ~500 nm thick, crystallized after thermal treatment at 700 ºC. The powders revealed spherical and rod shape morphology. The optical quality of films showed a predominant band at 615 nm under 250 nm excitation. A preliminary luminescent test provided the properties of the Eu3+ doped BaTiO3. PMID:19865533

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

Rabin, B.H.

A simple modified tape casting procedure has been developed for application to ceramic joining when the joining materials are in powder form. The method involves preparation of a slurry from the powder, solvent, and thermoplastic binder, and then casting directly onto the joining surface using a moving doctor blade. Handling of the tape prior to joining is not necessary: therefore, binder content is minimized, plasticizers are not required, and viscosity is controlled by solvent content. The utility of this technique for producing joints with thin, uniform interlayers is demonstrated for silicon carbide materials joined with TiC + Ni and SiCmore » + Si.« less

Study on the RF inductively coupled plasma spheroidization of refractory W and W-Ta alloy powders

NASA Astrophysics Data System (ADS)

Chenfan, YU; Xin, ZHOU; Dianzheng, WANG; Neuyen VAN, LINH; Wei, LIU

2018-01-01

Spherical powders with good flowability and high stacking density are mandatory for powder bed additive manufacturing. Nevertheless, the preparation of spherical refractory tungsten and tungsten alloy powders is a formidable task. In this paper, spherical refractory metal powders processed by high-energy stir ball milling and RF inductively coupled plasma were investigated. By utilizing the technical route, pure spherical tungsten powders were prepared successfully, the flowability increased from 10.7 s/50 g to 5.5 s/50 g and apparent density increased from 6.916 g cm-3 to 11.041 g cm-3. Alloying element tantalum can reduce the tendency to micro-crack during tungsten laser melting and rapid solidification process. Spherical W-6Ta (%wt) powders were prepared in this way, homogeneous dispersion of tantalum in a tungsten matrix occurred but a small amount of flake-like shape particles appeared after high-energy stir ball milling. The flake-like shape particles can hardly be spheroidized in subsequent RF inductively coupled plasma process, might result from the unique suspended state of flaky particles under complex electric and magnetic fields as well as plasma-particle heat exchange was different under various turbulence models. As a result, the flake-like shape particles cannot pass through the high-temperature area of thermal plasma torch and cannot be spheroidized properly.

Microwave-Assisted Synthesis of High Dielectric Constant CaCu3Ti4O12 from Sol-Gel Precursor

NASA Astrophysics Data System (ADS)

Ouyang, Xin; Cao, Peng; Huang, Saifang; Zhang, Weijun; Huang, Zhaohui; Gao, Wei

2015-07-01

CaCu3Ti4O12 (CCTO) powders derived from sol-gel precursors were calcined and sintered via microwave radiation. The obtained CCTO powders were compared with that obtained via a conventional heating method. For microwave heating, 89.1 wt.% CCTO was achieved from the sol-gel precursor, after only 17 min at 950°C. In contrast, the conventional calcination method required 3 h to generate 87.6 wt.% CCTO content at 1100°C. In addition, the CCTO powders prepared through 17 min of microwave calcination exhibited a small particle size distribution of D50 = 3.826 μm. It was found that a lengthy hold time of 1 h by microwave sintering is required to obtain a high dielectric constant (3.14 × 103 at 102 Hz) and a reasonably low dielectric loss (0.161) in the sintered CCTO ceramic. Based upon the distinct microstructures, the dielectric responses of the CCTO samples sintered by different methods are attributed to space charge polarization and internal barrier layer capacitor mechanism.

Assessment of Japanese Technology in Advanced Glass and Ceramic Fibers

DTIC Science & Technology

1992-06-01

powders and crystals by hydrothermal tech- niques, and they have had their process for the preparation of zirconia powder commercial- ized by the...Masahiro Yoshimura. Whisker-Glass Composites, Hydrothermal Zirconia Powders , Hydrothermal Machining, Super-Conducting Thin Films. Professor Eiichi

Phase transitions of sodium niobate powder and ceramics, prepared by solid state synthesis

NASA Astrophysics Data System (ADS)

Koruza, J.; Tellier, J.; Malič, B.; Bobnar, V.; Kosec, M.

2010-12-01

Phase transitions of sodium niobate, prepared by the solid state synthesis method, were examined using dielectric measurements, differential scanning calorimetry, and high temperature x-ray diffraction, in order to contribute to the clarification of its structural behavior below 400 °C. Four phase transitions were detected in the ceramic sample using dielectric measurements and differential scanning calorimetry and the obtained temperatures were in a good agreement with previous reports for the transitions of the P polymorph. The anomaly observed by dielectric measurements in the vicinity of 150 °C was frequency dependent and could be related to the dynamics of the ferroelectric nanoregions. The phase transitions of the as-synthesized NaNbO3 powder were investigated using differential scanning calorimetry and high temperature x-ray diffraction. The results show the existence of the Q polymorph at room temperature, not previously reported for the powder, which undergoes a transition to the R polymorph upon heating through a temperature region between 265 and 326.5 °C. This transition is mainly related to the displacement of Na into a more symmetric position and a minor change in the tilting system. The structures at room temperature, 250, 300, and 420 °C were refined by the Rietveld method and the evolution of the tilting system of the octahedral network and cationic displacement are reported.

On-line double isotope dilution laser ablation inductively coupled plasma mass spectrometry for the quantitative analysis of solid materials.

PubMed

Fernández, Beatriz; Rodríguez-González, Pablo; García Alonso, J Ignacio; Malherbe, Julien; García-Fonseca, Sergio; Pereiro, Rosario; Sanz-Medel, Alfredo

2014-12-03

We report on the determination of trace elements in solid samples by the combination of on-line double isotope dilution and laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). The proposed method requires the sequential analysis of the sample and a certified natural abundance standard by on-line IDMS using the same isotopically-enriched spike solution. In this way, the mass fraction of the analyte in the sample can be directly referred to the certified standard so the previous characterization of the spike solution is not required. To validate the procedure, Sr, Rb and Pb were determined in certified reference materials with different matrices, including silicate glasses (SRM 610, 612 and 614) and powdered samples (PACS-2, SRM 2710a, SRM 1944, SRM 2702 and SRM 2780). The analysis of powdered samples was carried out both by the preparation of pressed pellets and by lithium borate fusion. Experimental results for the analysis of powdered samples were in agreement with the certified values for all materials. Relative standard deviations in the range of 6-21% for pressed pellets and 3-21% for fused solids were obtained from n=3 independent measurements. Minimal sample preparation, data treatment and consumption of the isotopically-enriched isotopes are the main advantages of the method over previously reported approaches. Copyright © 2014 Elsevier B.V. All rights reserved.

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.

Investigation of nanosized crystalline form to improve the oral bioavailability of poorly water soluble cilostazol.

PubMed

Miao, Xiaoqing; Sun, Changshan; Jiang, Tongying; Zheng, Li; Wang, Tianyi; Wang, Siling

2011-01-01

The aim of this study was to develop cilostazol (CLT) nanocrystals intended to improve its dissolution rate and enhance its bioavailability. In this study, CLT nanosuspension was prepared by the anti-solvent and high-pressure homogenization method. The effects of the production parameters, such as the stabilizer concentration, pressure and number of cycles, were investigated. Characterization of the product was performed by scanning electron microscopy (SEM), Nitrogen adsorption, differential scanning calorimetry (DSC), X-ray powder diffraction analysis (XRPD), X-ray Photoelectron Spectroscopy (XPS), particle size analysis and dissolution testing. Additionally, the comparison studies of oral bioavailability in beagle dogs of three type tables were performed. The images of SEM showed a spherical smooth CLT powder, and Nitrogen adsorption test revealed spray dried powder were porous with high BET surface area compared with that of raw CLT. DSC and XRPD results demonstrated that the combination of preferred polymorph B and C of CLT were prepared successfully, the saturation solubility of the nanosized crystalline powder is about 5 fold greater than that of raw CLT, and the dissolution rate was enhanced 4 fold than that of raw CLT. The Cmax and AUC0-48h of CLT nanosized crystalline tablets were 2.1 fold and 1.9 fold, and 3.0 fold and 2.3 fold compared with those of the nanosized tablets and commercial tablets, respectively. The anti-solvent-high-pressure homogenization technique was employed successfully to produce cilostazol nanosuspensions. The bioavailability of CLT tablets prepared using spray dried nanosized crystalline powder after oral administration to dogs was markedly increased compared with that produced by nanosized tablets and commercial tablets, because of its greater dissolution rate owing to its transition of the crystalline state to form C and form B, reduced particle size and porous structure with increased surface area.

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

Sonocatalytic degradation of some dyestuffs and comparison of catalytic activities of nano-sized TiO2, nano-sized ZnO and composite TiO2/ZnO powders under ultrasonic irradiation.

PubMed

Wang, Jun; Jiang, Zhe; Zhang, Liqun; Kang, Pingli; Xie, Yingpeng; Lv, Yanhui; Xu, Rui; Zhang, Xiangdong

2009-02-01

Here, a novel sonocatalyst, composite TiO2/ZnO powder, was prepared through the combination of nano-sized TiO2 and ZnO powders. Because of the appropriate adsorbability to organic pollutants and special crystal interphase between TiO2 and ZnO particles, the composite TiO2/ZnO powder exhibits a high sonocatalytic activity under ultrasonic irradiation during the degradation of acid red B. Especially, the sonocatalytic activity of composite TiO2/ZnO powder with 4:1 molar proportion treated at 500 degrees C for 50 min showed obvious improvement compared with pure nano-sized TiO2 and ZnO powders. When the experimental conditions such as 10mg/L acid red B concentration, 1.0 g/L catalyst addition amount, pH=7.0, 20 degrees C system temperature, 100 min ultrasonic time and 50 mL total volume were adopted, the satisfactory degradation ratio and rate were obtained. All experiments indicate that the sonocatalytic method using composite TiO2/ZnO powder may be a more advisable choice for the treatments of non- or low-transparent organic wastewaters in future.

Effect of Gallium and Indium Co-Substituting on Upconversion Properties of Er/Yb:Yttrium Aluminum Garnet Powders Prepared by the Co-Precipitation Method.

PubMed

Zhang, Wei; Liang, Yun-Ling; Hu, Zheng-Fa; Feng, Zu-Yong; Lun, Ma; Zhang, Xiu-ping; Sheng, Xia; Liu, Qian; Luo, Jie

2016-04-01

Gallium and Indium co-substituted Yb, Er:YAG was fabricated through the chemical co-precipitation method. The formation process and structure of the Ga3+ and In3+ substituted phosphor powders were characterized by the X-ray diffraction, thermo-gravimetry analyzer, infrared spectra, and X-ray photoelectron spectroscopy, and the effects of Ga3+ and In3+ concentration on the luminescence properties were investigated by spectrum. The results showed that the blue shift occurred after the substitution of Ga3+ and In3+ for Al3+ in matrix, and the intensity of emission spectrum was affected by the concentration of Ga3+ and In3+.

Digital Image Correlation of 2D X-ray Powder Diffraction Data for Lattice Strain Evaluation

PubMed Central

Zhang, Hongjia; Sui, Tan; Daisenberger, Dominik; Fong, Kai Soon

2018-01-01

High energy 2D X-ray powder diffraction experiments are widely used for lattice strain measurement. The 2D to 1D conversion of diffraction patterns is a necessary step used to prepare the data for full pattern refinement, but is inefficient when only peak centre position information is required for lattice strain evaluation. The multi-step conversion process is likely to lead to increased errors associated with the ‘caking’ (radial binning) or fitting procedures. A new method is proposed here that relies on direct Digital Image Correlation analysis of 2D X-ray powder diffraction patterns (XRD-DIC, for short). As an example of using XRD-DIC, residual strain values along the central line in a Mg AZ31B alloy bar after 3-point bending are calculated by using both XRD-DIC and the conventional ‘caking’ with fitting procedures. Comparison of the results for strain values in different azimuthal angles demonstrates excellent agreement between the two methods. The principal strains and directions are calculated using multiple direction strain data, leading to full in-plane strain evaluation. It is therefore concluded that XRD-DIC provides a reliable and robust method for strain evaluation from 2D powder diffraction data. The XRD-DIC approach simplifies the analysis process by skipping 2D to 1D conversion, and opens new possibilities for robust 2D powder diffraction data analysis for full in-plane strain evaluation. PMID:29543728

Investigation of phase evolution of CaCu{sub 3}Ti{sub 4}O{sub 12} (CCTO) by in situ synchrotron high-temperature powder diffraction

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

Ouyang, Xin; Huang, Saifang; School of Materials Science and Technology, China University of Geosciences

2014-03-15

In situ synchrotron X-ray powder diffraction was used to study the high-temperature phase evolution of CaCu{sub 3}Ti{sub 4}O{sub 12} (CCTO) precursors prepared via solid-state and sol–gel methods. After the precursors are heated to 1225 °C, the CCTO phase is the main phase observed in the calcined powder, with the presence of some minor impurities. Comparing the two precursors, we found that the onset temperature for the CCTO phase formation is 800 °C in the sol–gel precursor, lower than that in the solid-state precursor (875 °C). Intermediate phases were only observed in the sol–gel precursor. Both precursors are able to bemore » calcined to sub-micrometric sized powders. Based on the synchrotron data along with differential scanning calorimetry (DSC) and thermal gravimetric analysis (TGA), the phase formation sequence and mechanism during calcination are proposed in this study. -- Graphical abstract: The in situ synchrotron HT-XRD patterns of CCTO sol–gel and solid-state precursor. Highlights: • Phase formation sequence/mechanism in two CCTO precursors has been established. • Formation temperature of CCTO via sol–gel method is lower than solid-state method. • Intermediate phases are only observed in the sol–gel precursor. • Both precursors are able to be calcined into sub-micrometric sized powders.« less

The effect of microwave and conventional heating on a modified sol-gel derived biphasic calcium phosphate

NASA Astrophysics Data System (ADS)

Herradi, S.; Bouhazma, S.; Khaldi, M.; El Hachadi, A.; El Bali, B.; Lachkar, M.

2018-03-01

A facile sol-gel method was used to synthesize either hydroxyapatite (HA) or beta-tricalcium phosphate (β-TCP) as the major phase. Herein, we report, on the one hand, the effect of a very low maturation temperature on the final powder composition after drying step, and on the other hand, we compare the effect of calcination of this powder by microwave or electric furnace. It was found that microwave heating has led to the formation of hydroxyapatite phase upon 180°C for 20 minutes, however, XRD patterns show that the powder becomes less crystallized upon 220°C and amorphous upon 230°C. In contrast, furnace heating at 600°C and 700°C converts the as-synthesized powder to β-TCP as the major phase together with HA as the minor phase. This work shows the possibility to obtain the as-prepared BCP at much lower maturation temperature; it also gives an insight into the role, of either microwave or conventional heating, in controlling the ratio between HA and β-TCP in the sintered powder.

Hydrothermal synthesis and characterization of hydroxyapatite and fluorhydroxyapatite nano-size powders.

PubMed

Montazeri, Leila; Javadpour, Jafar; Shokrgozar, Mohammad Ali; Bonakdar, Shahin; Javadian, Sayfoddin

2010-08-01

Pure hydroxyapatite (HAp) and fluoride-containing apatite powders (FHAp) were synthesized using a hydrothermal method. The powders were assessed by x-ray diffraction (XRD), Fourier transform infrared (FTIR), scanning electron microscope (SEM) and F-selective electrode. X-ray diffraction results revealed the formation of single phase apatite structure for all the compositions synthesized in this work. However, the addition of a fluoride ion led to a systematic shift in the (3 0 0) peak of the XRD pattern as well as modifications in the FTIR spectra. It was found that the efficiency of fluoride ion incorporation decreased with the increase in the fluoride ion content. Fluorine incorporation efficiency was around 60% for most of the FHAp samples prepared in the current study. Smaller and less agglomerated particles were obtained by fluorine substitution. The bioactivity of the powder samples with different fluoride contents was compared by performing cell proliferation, alkaline phosphatase (ALP) and Alizarin red staining assays. Human osteoblast cells were used to assess the cellular responses to the powder samples in this study. Results demonstrated a strong dependence of different cell activities on the level of fluoridation.

Roller compaction of different pseudopolymorphic forms of theophylline: Effect on compressibility and tablet properties.

PubMed

Hadzović, Ervina; Betz, Gabriele; Hadzidedić, Seherzada; El-Arini, Silvia Kocova; Leuenberger, Hans

2010-08-30

The effect of roller compaction on disintegration time, dissolution rate and compressibility of tablets prepared from theophylline anhydrate powder, theophylline anhydrate fine powder and theophylline monohydrate was studied. In addition, the influence of adding microcrystalline cellulose, a commonly used excipient, in mixtures with these materials was investigated. Theophylline anhydrate powder was used as a model drug to investigate the influence of different compaction pressures on the tablet properties. Tablets with same porosity were prepared by direct compaction and by roller compaction/re-compaction. Compressibility was characterized by Heckel and modified Heckel equations. Due to the property of polymorphic materials to change their form during milling and compression, X-ray diffraction analysis of theophylline anhydrate powder, theophylline anhydrate fine powder and theophylline monohydrate powders and granules was carried out. After roller compaction the disintegration time and the dissolution rate of the tablets were significantly improved. Compressibility of theophylline anhydrate powder and theophylline anhydrate fine powder was decreased, while theophylline monohydrate showed higher compressibility after roller compaction. Microcrystalline cellulose affected compressibility of theophylline anhydrate powder, theophylline anhydrate fine powder and theophylline monohydrate whereby the binary mixtures showed higher compressibility than the individual materials. X-ray diffraction analyses confirmed that there were no polymorphic/pseudopolymorphic changes after roller compaction. Copyright 2010 Elsevier B.V. All rights reserved.

Optimal methodologies for terahertz time-domain spectroscopic analysis of traditional pigments in powder form

NASA Astrophysics Data System (ADS)

Ha, Taewoo; Lee, Howon; Sim, Kyung Ik; Kim, Jonghyeon; Jo, Young Chan; Kim, Jae Hoon; Baek, Na Yeon; Kang, Dai-ill; Lee, Han Hyoung

2017-05-01

We have established optimal methods for terahertz time-domain spectroscopic analysis of highly absorbing pigments in powder form based on our investigation of representative traditional Chinese pigments, such as azurite [blue-based color pigment], Chinese vermilion [red-based color pigment], and arsenic yellow [yellow-based color pigment]. To accurately extract the optical constants in the terahertz region of 0.1 - 3 THz, we carried out transmission measurements in such a way that intense absorption peaks did not completely suppress the transmission level. This required preparation of pellet samples with optimized thicknesses and material densities. In some cases, mixing the pigments with polyethylene powder was required to minimize absorption due to certain peak features. The resulting distortion-free terahertz spectra of the investigated set of pigment species exhibited well-defined unique spectral fingerprints. Our study will be useful to future efforts to establish non-destructive analysis methods of traditional pigments, to construct their spectral databases, and to apply these tools to restoration of cultural heritage materials.

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.

Conventional and two step sintering of PZT-PCN ceramics

NASA Astrophysics Data System (ADS)

Keshavarzi, Mostafa; Rahmani, Hooman; Nemati, Ali; Hashemi, Mahdieh

2018-02-01

In this study, PZT-PCN ceramic was made via sol-gel seeding method and effects of conventional sintering (CS) as well as two-step sintering (TSS) were investigated on microstructure, phase formation, density, dielectric and piezoelectric properties. First, high quality powder was achieved by seeding method in which the mixture of Co3O4 and Nb2O5 powder was added to the prepared PZT sol to form PZT-PCN gel. After drying and calcination, pyrochlore free PZT-PCN powder was synthesized. Second, CS and TSS were applied to achieve dense ceramic. The optimum temperature used for 2 h of conventional sintering was obtained at 1150 °C; finally, undesired ZrO2 phase formed in CS procedure was removed successfully with TSS procedure and dielectric and piezoelectric properties were improved compared to the CS procedure. The best electrical properties obtained for the sample sintered by TSS in the initial temperature of T 1 = 1200 °C and secondary temperature of T 2 = 1000 °C for 12 h.

A new approach to synthesize supported ruthenium phosphides for hydrodesulfurization

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

Wang, Qingfang; Key Laboratory of Advanced Energy Materials Chemistry; Wang, Zhiqiang

2016-02-15

Highlights: • We bring out a new method to synthesize noble metal phosphides at low temperature. • Both RuP and Ru{sub 2}P were synthesized using triphenylphosphine as phosphorus sources. • Ru{sub 2}P was the better active phase for HDS than RuP and metal Ru. • RuP/SiO{sub 2} prepared by new method had better HDS activity to that by TPR method. - Abstract: Supported noble metal ruthenium phosphides were synthesized by one-step H{sub 2}-thermal treatment method using triphenylphosphine (TPP) as phosphorus sources at low temperatures. Two phosphides RuP and Ru{sub 2}P can be prepared by this method via varying the molarmore » ratio of metal salt and TPP. The as-prepared phosphides were characterized by X-ray powder diffraction (XRD), low-temperature N{sub 2} adsorption, CO chemisorption and transmission electronic microscopy (TEM). The supported ruthenium phosphides prepared by new method and conventional method together with contradistinctive metallic ruthenium were evaluated in hydrodesulfurization (HDS) of dibenzothiophene (DBT). The catalytic results showed that metal-rich Ru{sub 2}P was the better active phase for HDS than RuP and metal Ru. Besides this, ruthenium phosphide catalyst prepared by new method exhibited superior HDS activity to that prepared by conventional method.« less

Study of colouring effect of herbal hair formulations on graying hair

PubMed Central

Singh, Vijender; Ali, Mohammed; Upadhyay, Sukirti

2015-01-01

Objective: To screen the hair colouring properties of hair colorants/ herbal hair colouring formulations. Materials and Methods: The dried aqueous herbal extracts of Gudhal leaves (Hibiscus rosa-sinensis), Jatamansi rhizome (Nardostachys jatamansi), Kuth roots (Saussurea lappa), Kattha (Acacia catechu), Amla dried fruit (Embelica officinalis), were prepared. Coffee powder (Coffea arabica) and Henna powder (Lowsonia inermis) were taken in the form of powder (# 40). Fourteen herbal hair colorants were prepared from these dried aqueous herbal extracts and powders. Activities of hair colorants were observed on sheep wool fibers. On the basis of the above observation six hair colorants were selected. These six formulations were taken for trials on human beings. Observation: The formulation coded HD-3 gave maximum colouring effect on sheep wool fibers as well as on human beings and percentage of acceptance among the volunteers were in the following order: HD- 3 > HD- 4 > HD-1 > HD-13 > HD-14 > HD-11. Results and Discussion: The remarkable results were obtained from five herbal hair colorants, viz., HD-1, HD- 3, HD- 4, HD-13 and HD-14 on sheep wool fibers and human beings. Formulation HD-3, having gudhal, jatamansi, kuth, kattha, amla, coffee and henna, was the maximum accepted formulation and suggested that these herbs in combination acts synergistically in hair colouring action. It also concluded that jatamansi, present in different hair colorants, was responsible to provide maximum blackening on hair PMID:26130937

Hardness and wear analysis of Cu/Al2O3 composite for application in EDM electrode

NASA Astrophysics Data System (ADS)

Hussain, M. Z.; Khan, U.; Jangid, R.; Khan, S.

2018-02-01

Ceramic materials, like Aluminium Oxide (Al2O3), have high mechanical strength, high wear resistance, high temperature resistance and good chemical durability. Powder metallurgy processing is an adaptable method commonly used to fabricate composites because it is a simple method of composite preparation and has high efficiency in dispersing fine ceramic particles. In this research copper and novel material aluminium oxide/copper (Al2O3/Cu) composite has been fabricated for the application of electrode in Electro-Discharge Machine (EDM) using powder metallurgy technique. Al2O3 particles with different weight percentages (0, 1%, 3% and 5%) were reinforced into copper matrix using powder metallurgy technique. The powders were blended and compacted at a load of 100MPa to produce green compacts and sintered at a temperature of 574 °C. The effect of aluminium oxide content on mass density, Rockwell hardness and wear behaviour were investigated. Wear behaviour of the composites was investigated on Die-Sink EDM (Electro-Discharge Machine). It was found that wear rate is highly depending on hardness, mass density and green protective carbonate layer formation at the surface of the composite.

In situ synthesis of magnesium-substituted biphasic calcium phosphate and in vitro biodegradation

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

Kim, Tae-Wan; Lee, Hyeong-Shin; Kim, Dong-Hyun

Highlights: ► Mg–BCP were successfully prepared through in situ aqueous co-precipitation method. ► The amount of β-TCP phase was changed with the magnesium substitution level. ► The substitution of magnesium led to a decrease in the unit cell volume. ► Mg–BCP could be able to develop a new apatite phase on the surface faster than BCP. -- Abstract: In situ preparation of magnesium (Mg) substituted biphasic calcium phosphate (BCP) of hydroxyapatite (HAp)/β-tricalcium phosphate (β-TCP) were carried out through aqueous co-precipitation method. The concentrations of added magnesium were varied with the calcium in order to obtain constant (Ca + Mg)/P ratiosmore » of 1.602. X-ray diffraction (XRD) and Fourier transformed infrared (FTIR) spectroscopy were used to characterize the structure of synthesized magnesium substituted BCP powders. The results have shown that substitution of magnesium in the calcium deficient apatites revealed the formation of biphasic mixtures of different HAp/β-TCP ratios after heating at 1000 °C. The ratios of the formation of phase mixtures were dependent on the content of magnesium. After immersing in Hanks’ balanced salt solution (HBSS) for 1 week, 1 wt% magnesium substituted BCP powders were degraded and precipitation started to be formed with small granules consisting of number of flake-like crystal onto the surface of synthesized powders. On the other hand, in the case of pure BCP powders, the formation of new precipitates was detected after immersion in HBSS for 2 weeks. On the basis of these results, magnesium substituted BCP could be able to develop a new apatite phase on the surface in contact with physiological fluids faster than BCP does. In addition, the retention time to produce the new apatite phase in implantation operation for the BCP powder could be controlled by the amount of magnesium substitution.« less

[Physical fingerprint for quality control of traditional Chinese medicine extract powders].

PubMed

Zhang, Yi; Xu, Bing; Sun, Fei; Wang, Xin; Zhang, Na; Shi, Xin-Yuan; Qiao, Yan-Jiang

2016-06-01

The physical properties of both raw materials and excipients are closely correlated with the quality of traditional Chinese medicine preparations in oral solid dosage forms. In this paper, based on the concept of the chemical fingerprint for quality control of traditional Chinese medicine products, the method of physical fingerprint for quality evaluation of traditional Chinese medicine extract powders was proposed. This novel physical fingerprint was built by the radar map, and consisted of five primary indexes (i.e. stackablity, homogeneity, flowability, compressibility and stability) and 12 secondary indexes (i.e. bulk density, tap density, particle size<50 μm percentage, relative homogeneity index, hausner ratio, angle of repose, powder flow time, inter-particle porosity, Carr index, cohesion index, loss on drying, hygroscopicity). Panax notoginseng saponins (PNS) extract was taken for an example. This paper introduced the application of physical fingerprint in the evaluation of source-to-source and batch-to-batch quality consistence of PNS extract powders. Moreover, the physical fingerprint of PNS was built by calculating the index of parameters, the index of parametric profile and the index of good compressibility, in order to successfully predict the compressibility of the PNS extract powder and relevant formulations containing PNS extract powder and conventional pharmaceutical excipients. The results demonstrated that the proposed method could not only provide new insights into the development and process control of traditional Chinese medicine solid dosage forms. Copyright© by the Chinese Pharmaceutical Association.

Method of producing high purity zirconia powder from zircon powder

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

Funahashi, T.; Uchimura, R.; Oguchi, Y.

A method is described of producing a zirconia powder from zirconia containing SiO/sub 2/, comprising the steps of: preparing a raw material mixture comprising the zircon powder containing the SiO/sub 2/ and a powdery carbon-containing material such that the mole ratio of C, which is contained in the carbon-containing material and does not gasify at temperatures below 100/sup 0/C. in a nonoxidizing atmosphere, to SiO/sub 2/ contained in the zircon powder is in the range from 0.4 to 2.0; and subjecting the raw material mixture to a desiliconizing heat treatment in a nonoxidizing atmosphere of which the presence is notmore » higher than 0.6 atm, the desiliconizing heat treatment being a combination of a first-stage heat treatment which is performed at a temperature in the range from 1200/sup 0/ to 1550/sup 0/C. for separating silica from the zircon powder and a second-stage heat treatment which is performed at a higher temperature in the range from above 1550/sup 0/C. to 2000/sup 0/C. for completely converting silica in the mixture under heat treatment into gaseous SiO and dissipating the gaseous SiO, wherein the raw material mixture is subjected to the desiliconizing heat treatment in the form of at least one lump whose bulk density is in the range from 0.7 to 2.0.« less

Czochralski growth of LaPd2Al2 single crystals

NASA Astrophysics Data System (ADS)

Doležal, P.; Rudajevová, A.; Vlášková, K.; Kriegner, D.; Václavová, K.; Prchal, J.; Javorský, P.

2017-10-01

The present study is focused on the preparation of single crystalline LaPd2Al2 by the Czochralski method. Differential scanning calorimetry (DSC) and energy dispersive X-ray spectroscopy (EDX) analyses reveal that LaPd2Al2 is an incongruently melting phase which causes difficulties for the preparation of single crystalline LaPd2Al2 by the Czochralski method. Therefore several non-stoichiometric polycrystalline samples were studied for its preparation. Finally the successful growth of LaPd2Al2 without foreign phases has been achieved by using a non-stoichiometric precursor with atomic composition 22:39:39 (La:Pd:Al). X-ray powder diffraction, EDX analysis and DSC were used for the characterisation. A single crystalline sample was separated from the ingot prepared by the Czochralski method using the non-stoichiometric precursor. The presented procedure for the preparation of pure single phase LaPd2Al2 could be modified for other incongruently melting phases.

Enhancement of luminescence emission from GdVO{sub 4}:Er{sup 3+}/Yb{sup 3+} phosphor by Li{sup +} co-doping

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

Gavrilović, Tamara V.; Jovanović, Dragana J., E-mail: draganaj@vinca.rs; Lojpur, Vesna M.

2014-09-15

This paper demonstrates the effects of Li{sup +} co-doping on the structure, morphology, and luminescence properties of GdVO{sub 4}:Er{sup 3+}/Yb{sup 3+} phosphor prepared using a high-temperature solid-state chemistry method. The GdVO{sub 4}:Er{sup 3+}/Yb{sup 3+} powders synthesized with the Li{sup +} co-dopant (in concentrations of 0, 5, 10, and 15 mol%) are characterized by X-ray powder diffraction, scanning electron microscopy, and photoluminescence spectroscopy. Structural analysis showed that powders co-doped with Li{sup +} have larger crystallite sizes and slightly smaller crystal lattice parameters than powders prepared without Li{sup +} ions. Photoluminescence down-conversion (345-nm excitation) and up-conversion (980-nm excitation) spectra show characteristic Er{supmore » 3+} emissions, with the most intense bands peaking at 525 nm ({sup 2}H{sub 11/2}→{sup 4}I{sub 15/2} transition) and 552 nm ({sup 4}S{sub 3/2}→{sup 4}I{sub 15/2}). The intensity of up-conversion emission from GdVO{sub 4}:Er{sup 3+}/Yb{sup 3+} is enhanced (by a factor of four) by co-doping with 5 mol% of Li{sup +} ions. The mechanisms responsible for this emission enhancement are discussed. - Graphical abstract: UC emission spectra for GdVO{sub 4}:1.5-mol% Er{sup 3+}/20-mol% Yb{sup 3+} powders co-doped with different concentrations of Li{sup +} ions, recorded under 980-nm excitation. - Highlights: • 5-mol% Li{sup +} co-doped powders have 400% enhanced up-conversion emission intensity. • 15-mol% Li{sup +} co-doping produces 40% higher emission in down-conversion. • Li{sup +} co-doped powders have larger crystallite size and smaller lattice parameters.« less

Preparation and Characterization of Cabamazepine Cocrystal in Polymer Solution.

PubMed

Zhang, Hao; Zhu, Ying; Qiao, Ning; Chen, Yang; Gao, Linghuan

2017-12-01

In this study, we attempted to prepare carbamazepine (CBZ) cocrystal through the solution method in ethanol-water solvent mixture (volume ratio 1:1) and polyvinyl pyrrolidone (PVP) solution. Nicotinamide (NIC) and saccharin (SAC) were selected as cocrystal coformers. Cocrystal screening products were characterized by Fourier Transform Infrared Spectroscopy (FTIR), Differential Scanning Calorimetry (DSC), and Powder X-ray Diffraction (PXRD) techniques. Characterization results show that in ethanol-water solvent mixture, pure CBZ-NIC cocrystal can be prepared, while CBZ-SAC cocrystal cannot be obtained. The addition of PVP can inhibit CBZ-NIC cocrystal formation and facilitate CBZ-SAC cocrystal formation.

Preparation and Characterization of Carbamazepine Cocrystal in Polymer Solution

PubMed Central

Zhang, Hao; Zhu, Ying; Chen, Yang; Gao, Linghuan

2017-01-01

In this study, we attempted to prepare carbamazepine (CBZ) cocrystal through the solution method in ethanol-water solvent mixture (volume ratio 1:1) and polyvinyl pyrrolidone (PVP) solution. Nicotinamide (NIC) and saccharin (SAC) were selected as cocrystal coformers. Cocrystal screening products were characterized by Fourier Transform Infrared Spectroscopy (FTIR), Differential Scanning Calorimetry (DSC), and Powder X-ray Diffraction (PXRD) techniques. Characterization results show that in ethanol-water solvent mixture, pure CBZ-NIC cocrystal can be prepared, while CBZ-SAC cocrystal cannot be obtained. The addition of PVP can inhibit CBZ-NIC cocrystal formation and facilitate CBZ-SAC cocrystal formation. PMID:29194387

Evaluation of different methods of optical impression making on the marginal gap of onlays created with CEREC 3D.

PubMed

da Costa, Juliana B; Pelogia, Fernanda; Hagedorn, Bradley; Ferracane, Jack L

2010-01-01

This study evaluated the marginal gaps on several surfaces of onlays created with the Cerec 3D system using one intraoral and two extraoral optical impression methods. A human molar (#19) was mounted with its adjacent teeth on a typodont (Frasaco) and prepared for a MODL onlay. The typodont was assembled in the mannequin head in order to simulate clinical conditions. The same operator took 36 individual optical impressions using a CEREC 3D camera. For group 1 (IP), a thin layer of titanium dioxide powder (CEREC powder-VITA) was applied directly onto the surface of the preparation for imaging (n = 12). For group 2 (EP), a sectional impression was taken with hydrocolloid Identic Syringable (Dux Dental), a die made with polyvinylsiloxane KwikkModel Scan (R-dental Dentalerzeugnisse GmbH) and powdered with titanium dioxide for imaging (n = 12). For group 3 (ES), a sectional impression was taken with PVS and a sectional stock tray, a die fabricated in stone (Diamond die- HI-TEC Dental Products) and the die being imaged without powdering (n = 12). One operator designed and machined the onlays in VitaBlocks Mark II for Cerec (VITA) using a CEREC 3D. The marginal gaps (microm) were measured with an optical microscope (50x) at 12 points, three on each surface of the MODL. The results were analyzed by two-way ANOVA/ Tukey's (p = 0.05). The overall mean marginal gaps (microm) for the three methods were: IP = 111.6 (+/- 34.0); EP = 161.4 (+/- 37.6) and ES = 116.8 (+/- 42.3). IP and ES were equal, but both were significantly less than EP. The pooled mean marginal gaps (microm) for the occlusal = 110.5 (+/- 39) and lingual = 111.5 (+/- 30.5) surfaces were equivalent and significantly less than the distal = 136.5 (+/- 42.5) and mesial = 161.1 (+/- 43.3). The marginal gap of CEREC 3D onlay restorations was not different when the optical impression was taken intraorally vs extraorally using a stone cast that does not require powdering. The lingual and occlusal surfaces showed the lowest gaps.

Preparation of refractory cermet structures for lithium compatibility testing

NASA Technical Reports Server (NTRS)

Heestand, R. L.; Jones, R. A.; Wright, T. R.; Kizer, D. E.

1973-01-01

High-purity nitride and carbide cermets were synthesized for compatability testing in liquid lithium. A process was developed for the preparation of high-purity hafnium nitride powder, which was subsequently blended with tungsten powder or tantalum nitride and tungsten powders and fabricated into 3 in diameter billets by uniaxial hot pressing. Specimens were then cut from the billets for compatability testing. Similar processing techniques were applied to produce hafnium carbide and zirconium carbide cermets for use in the testing program. All billets produced were characterized with respect to chemistry, structure, density, and strength properties.

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.

Studies on the preparation and plasma spherodization of yttrium aluminosilicate glass microspheres for their potential application in liver brachytherapy

NASA Astrophysics Data System (ADS)

Sreekumar, K. P.; Saxena, S. K.; Kumar, Yogendra; Thiyagarajan, T. K.; Dash, Ashutosh; Ananthapadmanabhan, P. V.; Venkatesh, Meera

2010-02-01

Plasma spheroidization exploits the high temperature and high enthalpy available in the thermal plasma jet to melt irregularly shaped powder particles and quench them to get dense spherical particles. Plasma spheroidization is a versatile process and can be applied to metals, ceramics, alloys and composites to obtain fine spherical powders. Radioactive microspheres incorporated with high energetic beta emitting radioisotopes have been reported to be useful in the palliative treatment of liver cancer. These powders are to be prepared in closer range of near spherical morphology in the size range 20-35 microns. Inactive glass samples were prepared by heating the pre-calculated amount of glass forming ingredients in a recrystallized alumina crucible. The glass was formed by keeping the glass forming ingredients at 1700°C for a period of three hours to form a homogeneous melt. After cooling, the glass was recovered from the crucible by crushing and was subsequently powdered mechanically with the help of mortar and pestle. This powder was used as the feed stock for plasma spheroidization using an indigenously developed 40 kW plasma spray system. Experiments were carried out at various operating parameters. The operating parameters were optimised to get spheroidised particles. The powder was sieved to get the required size range before irradiation.

A robust quantitative near infrared modeling approach for blend monitoring.

PubMed

Mohan, Shikhar; Momose, Wataru; Katz, Jeffrey M; Hossain, Md Nayeem; Velez, Natasha; Drennen, James K; Anderson, Carl A

2018-01-30

This study demonstrates a material sparing Near-Infrared modeling approach for powder blend monitoring. In this new approach, gram scale powder mixtures are subjected to compression loads to simulate the effect of scale using an Instron universal testing system. Models prepared by the new method development approach (small-scale method) and by a traditional method development (blender-scale method) were compared by simultaneously monitoring a 1kg batch size blend run. Both models demonstrated similar model performance. The small-scale method strategy significantly reduces the total resources expended to develop Near-Infrared calibration models for on-line blend monitoring. Further, this development approach does not require the actual equipment (i.e., blender) to which the method will be applied, only a similar optical interface. Thus, a robust on-line blend monitoring method can be fully developed before any large-scale blending experiment is viable, allowing the blend method to be used during scale-up and blend development trials. Copyright © 2017. Published by Elsevier B.V.

Low-temperature sintering behavior of nanocrystalline indium tin oxide prepared from polymer-containing sols

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

Koroesi, Laszlo, E-mail: l.korosi@chem.u-szeged.hu; Papp, Szilvia; Oszko, Albert

2012-04-15

Highlights: Black-Right-Pointing-Pointer The synthesis of ITO powders and thin films from PVP-containing sols is presented. Black-Right-Pointing-Pointer The nano- and microstructures of ITO are more compact when PVP is used. Black-Right-Pointing-Pointer PVP acts both as a steric stabilizer of the sol and as a pre-sintering agent. Black-Right-Pointing-Pointer The PVP-induced enhanced sintering results in ITO with lower electrical resistance. Black-Right-Pointing-Pointer The surface composition of the ITO films is independent of the initial PVP content. -- Abstract: Indium tin hydroxide (ITH) xerogel powders and thin films with different polyvinylpyrrolidone (PVP) contents (0-22%, w/w) were prepared by a classical sol-gel method. To obtain nanocrystallinemore » indium tin oxide (ITO), the ITH xerogels were calcined at 550 Degree-Sign C. The effect of the initial polymer content on the structure of the ITO powders was studied by means of N{sub 2}-sorption measurements, small-angle X-ray scattering (SAXS), transmission and scanning electron microscopy. The N{sub 2}-sorption measurements revealed that the ITO powders obtained contained micropores and both their porosity and specific surface area decreased with increasing PVP content of the ITH xerogels. The SAXS measurements confirmed the enhanced sintering of the particles in the presence of PVP. The calculated mass fractal dimensions of the ITO powders increased significantly, indicating a significant compaction in structure. The pre-sintered structure could be achieved at relatively low temperature, which induced a significant decreasing (three orders of magnitude) in the electrical resistance of the ITO films.« less

Thermal insulation for high temperature microwave sintering operations and method thereof

DOEpatents

Holcombe, Cressie E.; Dykes, Norman L.; Morrow, Marvin S.

1995-01-01

Superior microwave transparent thermal insulations for high temperature microwave sintering operations were prepared. One embodiment of the thermal insulation comprises granules of boron nitride coated with a very thin layer of glassy carbon made by preparing a glassy carbon precursor and blending it with boron nitride powder to form a mixture. The blended mixture is granulated to form a grit which is dried and heated to form the granules of boron nitride coated with a glassy carbon. Alternatively, grains of glassy carbon are coated with boron nitride by blending a mixture of a slurry comprising boron nitride, boric acid binder, and methyl alcohol with glassy carbon grains to form a blended mixture. The blended mixture is dried to form grains of glassy carbon coated with boron nitride. In addition, a physical mixture of boron nitride powder and glassy carbon grains has also been shown to be an excellent thermal insulation material for microwave processing and sintering.

Method for preparation of textured YBa.sub.2 Cu.sub.3 O.sub.x superconductor

DOEpatents

Selvamanickam, Venkat; Goyal, Amit; Kroeger, Donald M.

1998-01-01

The present invention relate to textured YBa.sub.2 Cu.sub.3 O.sub.x (Y-123) superconductors and a process of preparing them by directional recrystallization of compacts fabricated from quenched YBCO powders at temperatures about 100.degree. C. below the peritectic temperature to provide a superconductor where more than 75% of the YBa.sub.2 Cu.sub.3 O.sub.x phase is obtained without any Y.sub.2 BaCuO.sub.5 .

The influence of the preparation methods on the inclusion of model drugs in a beta-cyclodextrin cavity.

PubMed

Salústio, P J; Feio, G; Figueirinhas, J L; Pinto, J F; Cabral Marques, H M

2009-02-01

The work aims to prove the complexation of two model drugs (ibuprofen, IB and indomethacin, IN) by beta-cyclodextrin (betaCD), and the effect of water in such a process, and makes a comparison of their complexation yields. Two methods were considered: kneading of a binary mixture of the drug, betaCD, and inclusion of either IB or IN in aqueous solutions of betaCD. In the latter method water was removed by air stream, spray-drying and freeze-drying. To prove the formation of complexes in final products, optical microscopy, UV spectroscopy, IR spectroscopy, DSC, X-ray and NMR were considered. Each powder was added to an acidic solution (pH=2) to quantify the concentration of the drug inside betaCD cavity. Other media (pH=5 and 7) were used to prove the existence of drug not complexed in each powder, as the drugs solubility increases with the pH. It was observed that complexation occurred in all powders, and that the fraction of drug inside the betaCD did not depend neither on the method of complexation nor on the processes of drying considered.

Preparation of W–Sc{sub 2}O{sub 3} targets and scandate cathodes with film prepared by pulsed laser deposition

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

Zhang, Xizhu; Wang, Jinshu, E-mail: wangjsh@bjut.edu.cn; Liu, Wei

2013-12-15

Graphical abstract: - Highlights: • W–Sc{sub 2}O{sub 3} film containing 5% Sc{sub 2}O{sub 3} and 95% W were prepared by pulsed laser deposition. • W–Sc{sub 2}O{sub 3} film on scandate cathode surface improves emission property. • The film improves Sc distribution uniformity and is favorable for forming Ba–Sc–O layer. - Abstract: Sub-micrometer Sc{sub 2}O{sub 3}–W powder with a narrow particle size distribution has been obtained by a sol–gel method combined with two-step hydrogen reduction process. Based on the obtained powder, the W–Sc{sub 2}O{sub 3} targets have been sintered via spark plasma sintering (SPS) at 1300 °C. The W–Sc{sub 2}O{sub 3}more » targets have the average grain size of about 1 μm. Both the sintering temperature and holding time are much lower than those of the targets prepared with micrometer sized powders. The obtained W–Sc{sub 2}O{sub 3} targets have a high comparative density of 96.4% and rockwell hardness of 86.4 HRC. Using the target, the scandate cathode deposited with a film containing 5% Sc{sub 2}O{sub 3} and 95% W has been obtained by pulsed laser deposition (PLD) method. This cathode has good emission property, i.e., the highest thermionic emission current density reaches 43.09 A/cm{sup 2} of J{sub div} at 900 °C{sub b} after being activated for 8 h, which is much higher than that of scandate cathode without film. Scandium (Sc) supplied by the film on the surface during the activation forms a Ba–Sc–O active layer, which helps to the emission.« less

Fabrication by Electrophoretic Deposition of Nano-Fe3O4 and Fe3O4@SiO2 3D Structure on Carbon Fibers as Supercapacitor Materials

NASA Astrophysics Data System (ADS)

Hajalilou, Abdollah; Abouzari-Lotf, Ebrahim; Etemadifar, Reza; Abbasi-Chianeh, Vahid; Kianvash, Abbas

2018-05-01

Core-shell nanostructured magnetic Fe3O4@SiO2 with particle size ranging from 3 nm to 40 nm has been synthesized via a facile precipitation method. Tetraethyl orthosilicate was employed as surfactant to prepare core-shell structures from Fe3O4 nanoparticles synthesized from pomegranate peel extract using a green method. X-ray diffraction analysis, Fourier-transform infrared and ultraviolet-visible (UV-Vis) spectroscopies, transmission electron microscopy, and scanning electron microscopy with energy-dispersive spectroscopy were employed to characterize the samples. The prepared Fe3O4 nanoparticles were approximately 12 nm in size, and the thickness of the SiO2 shell was 4 nm. Evaluation of the magnetic properties indicated lower saturation magnetization for Fe3O4@SiO2 powder ( 11.26 emu/g) compared with Fe3O4 powder ( 13.30 emu/g), supporting successful wrapping of the Fe3O4 nanoparticles by SiO2. As-prepared powders were deposited on carbon fibers (CFs) using electrophoretic deposition and their electrochemical behavior investigated. The rectangular-shaped cyclic voltagrams of Fe3O4@CF and Fe3O4@C@CF samples indicated electrochemical double-layer capacitor (EDLC) behavior. The higher specific capacitance of 477 F/g for Fe3O4@C@CF (at scan rate of 0.05 V/s in the potential range of - 1.13 to 0.45 V) compared with 205 F/g for Fe3O4@CF (at the same scan rate in the potential range of - 1.04 to 0.24 V) makes the former a superior candidate for use in energy storage applications.

Spectrochemical analysis of powdered biological samples using transversely excited atmospheric carbon dioxide laser plasma excitation

NASA Astrophysics Data System (ADS)

Zivkovic, Sanja; Momcilovic, Milos; Staicu, Angela; Mutic, Jelena; Trtica, Milan; Savovic, Jelena

2017-02-01

The aim of this study was to develop a simple laser induced breakdown spectroscopy (LIBS) method for quantitative elemental analysis of powdered biological materials based on laboratory prepared calibration samples. The analysis was done using ungated single pulse LIBS in ambient air at atmospheric pressure. Transversely-Excited Atmospheric pressure (TEA) CO2 laser was used as an energy source for plasma generation on samples. The material used for the analysis was a blue-green alga Spirulina, widely used in food and pharmaceutical industries and also in a few biotechnological applications. To demonstrate the analytical potential of this particular LIBS system the obtained spectra were compared to the spectra obtained using a commercial LIBS system based on pulsed Nd:YAG laser. A single sample of known concentration was used to estimate detection limits for Ba, Ca, Fe, Mg, Mn, Si and Sr and compare detection power of these two LIBS systems. TEA CO2 laser based LIBS was also applied for quantitative analysis of the elements in powder Spirulina samples. Analytical curves for Ba, Fe, Mg, Mn and Sr were constructed using laboratory produced matrix-matched calibration samples. Inductively coupled plasma optical emission spectroscopy (ICP-OES) was used as the reference technique for elemental quantification, and reasonably well agreement between ICP and LIBS data was obtained. Results confirm that, in respect to its sensitivity and precision, TEA CO2 laser based LIBS can be successfully applied for quantitative analysis of macro and micro-elements in algal samples. The fact that nearly all classes of materials can be prepared as powders implies that the proposed method could be easily extended to a quantitative analysis of different kinds of materials, organic, biological or inorganic.

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

Peric, A.D.

Powder and granules of the high density polyethylene (PEHD) were used to prepare mortar based matrices for immobilization of radioactive waste materials containing {sup 137}Cs, as well as containers for solidified radioactive waste form. Seven types of matrices, differ due to the percentage of granules and filler material added, were investigated. PEHD powder and granules were added to mortar matrix preparations with the objective of improving physico-chemical characteristics of the radwaste-mortar matrix mixtures, in particular the leach-rate of the immobilized radionuclide, as well as mechanical characteristics either of mortar matrix and container. In this paper, only mechanical strength aspect ofmore » the investigated mortar and concrete container formulations, is presented. The equivalent diameter of the PEHD granules used was 2.0 mm. PEHD granules were used to replace 100 volume percent of stone granules, sifted size of 2.0 mm, normally used in the matrix preparation, in order to decrease the porosity and density of the mortar matrix and to avoid segregation of the stone particles at the bottom of the immobilized radioactive waste cylindrical form. PEHD powder, particle size of 250 micrometer, was added as filler to the mortar formulation, replacing 5, 8 and 10 wt% of the total cement weight in matrix formulation and 15 and 18 wt% of the total cement weight in container formulation. Cured samples were investigated on mechanical strength, using 150 MPa hydraulic press, in order to determine influence of added polyethylene granules and powder on samples resistance to mechanical forces that solidified waste materials and concrete containers may experience at the disposal site. Results of performed investigations have shown that samples prepared with polyethylene granules, replacing 100 wt% of the stone granules, have almost twice as much mechanical strength than samples prepared with stone aggregate. Samples prepared with PEHD granules and powder have mechanical strength resistance up to 13.5% higher than ones prepared with PEHD granules, solely. Improved Mechanical strength resistance of tested samples accommodates trend that functionally depends on the percentage of PEHD powder added in formulation.« less

Glycoalkaloid, phenolic, and flavonoid content and antioxidative activities of conventional (nonorganic) and organic potato peel powders from commercial Gold, Red, and Russet Potatoes

USDA-ARS?s Scientific Manuscript database

The content of glycoalkaloids a-chaconine and a-solanine, individual and total phenolics compounds, and total flavonoids for three peels prepared from conventional and three from organic commercial potatoes as well antioxidant activities using three different methods were evaluated. Glycoalkaloids ...

Preparation of 152Gd targets from a small quantity of gadolinium oxide in a pyrochemical reaction

NASA Astrophysics Data System (ADS)

Lipski, A. R.

1995-02-01

A simple method utilizing small amounts (< 5 mg) of isotopically enriched material for the production of gadolinium targets is discussed. An electrostatically focused e-gun is used in the procedure in which 152Gd 2O 3 powder undergoes reduction-distillation and deposition onto an Fe foil.

Preparation of isotopic molybdenum foils utilizing small quantities of material

NASA Astrophysics Data System (ADS)

Lipski, A. R.; Lee, L. L.; Liang, J. F.; Mahon, J. C.

1993-09-01

A simple method utilizing a small amount of isotopic material for production of molybdenum foils is discussed. An e-gun is used in the procedure. The Mo powder undergoes reduction-sintering and melting-solidifying steps leading to the creation of a metallic droplet suitable for further cold rolling or vacuum deposition.

Preparation of glass-ceramics from molten steel slag using liquid-liquid mixing method.

PubMed

Zhang, Kai; Liu, Jianwen; Liu, Wanchao; Yang, Jiakuan

2011-10-01

A novel approach to prepare glass-ceramics from molten steel slag (MSS) was proposed. In laboratory, the water-quenched steel slag was melted at 1350 °C to simulate the MSS. A mixture of additive powders in wt.% (55 quartz powder, 5 Na2O, 16 emery powder, 15 CaO, 8 MgO, 1 TiO2) were melted into liquid at 1350 °C separately. Then the MSS and the molten additives were mixed homogeneously in order to obtain parent glass melt. The proportion of MSS in the melt was 50 wt.%. The melt was subsequently cast, annealed, heat-treated and transformed into glass-ceramics. Their microstructure and crystallization behavior were analyzed. The samples exhibited excellent properties and displayed bulk crystallization. The major crystallized phase was diopside ((Fe0.35Al0.20Mg0.44)Ca0.96(Fe0.08Si0.70Al0.20)2O6.12), which was uniformly distributed in the microstructure. The novel approach may help iron and steel industry achieve zero disposal of steel slag with utilization of the heat energy of the MSS. Copyright © 2011 Elsevier Ltd. All rights reserved.

Effect of the variation in the ambient moisture on the compaction behavior of powder undergoing roller-compaction and on the characteristics of tablets produced from the post-milled granules.

PubMed

Gupta, Abhay; Peck, Garnet E; Miller, Ronald W; Morris, Kenneth R

2005-10-01

Effect of variation in the ambient moisture levels on the compaction behavior of a 10% acetaminophen (APAP) powder blend in microcrystalline cellulose (MCC) powder was studied by comparing the physical and mechanical properties of ribbons prepared by roller compaction with those of simulated ribbons, i.e., tablets prepared under uni-axial compression. Relative density, moisture content, tensile strength, and Young's modulus were used as key compact properties for comparison. Moisture was found to facilitate the particle rearrangement of both, the APAP and the MCC particles, as well as the deformation of the MCC particles. The tensile strength of the simulated ribbons also showed an increase with increasing moisture content. An interesting observation was that the tensile strength of the roller compacted samples first increased and then decreased with increasing moisture content. Variation in the ambient moisture during roller compaction was also found to influence the characteristics of tablets produced from the granules obtained post-milling the ribbons. A method to study this influence is also reported. Copyright (c) 2005 Wiley-Liss, Inc. and the American Pharmacists Association

Preparation of Cu2ZnSnS4 nano-crystalline powder by mechano-chemical method

NASA Astrophysics Data System (ADS)

Alirezazadeh, Farzaneh; Sheibani, Saeed; Rashchi, Fereshteh

2018-01-01

Copper zinc tin sulfide (Cu2ZnSnS4, CZTS) is one of the most promising ceramic materials as an absorber layer in solar cells due to its suitable band gap, high absorption coefficient and non-toxic and environmental friendly constituent elements. In this work, nano-crystalline CZTS powder was synthesized by mechanical milling. Elemental powders of Cu, Zn, Sn and were mixed in atomic ratio of 2:1:1:4 according to the stoichiometry of Cu2ZnSnS4 and then milled in a planetary high energy ball mill under argon atmosphere. The samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and diffusion reflectance spectroscopy (DRS). XRD results confirm the formation of single-phase CZTS with kesterite structure after 20 h of milling. Also, the mean crystallite size was about 35 nm. SEM results show that after 20 h of milling, the product has a relatively uniform particle size distribution. Optical properties of the product indicate that the band gap of prepared CZTS is 1.6 eV which is near to the optimum value for photovoltaic solar cells showing as a light absorber material in solar energy applications.

Fabrication and Analysis of the Wear Properties of Hot-Pressed Al-Si/SiCp + Al-Si-Cu-Mg Metal Matrix Composite

NASA Astrophysics Data System (ADS)

Bang, Jeongil; Oak, Jeong-Jung; Park, Yong Ho

2016-01-01

The aim of this study was to characterize microstructures and mechanical properties of aluminum metal matrix composites (MMC's) prepared by powder metallurgy method. Consolidation of mixed powder with gas atomized Al-Si/SiCp powder and Al-14Si-2.5Cu-0.5Mg powder by hot pressing was classified according to sintering temperature and sintering time. Sintering condition was optimized using tensile properties of sintered specimens. Ultimate tensile strength of the optimized sintered specimen was 228 MPa with an elongation of 5.3% in longitudinal direction. In addition, wear properties and behaviors of the sintered aluminum-based MMC's were analyzed in accordance with vertical load and linear speed. As the linear speed and vertical load of the wear increased, change of the wear behavior occurred in order of oxidation of Al-Si matrix, formation of C-rich layer, Fe-alloying to matrix, and melting of the specimen

Immobilized TiO2 nanoparticles produced by flame spray for photocatalytic water remediation

NASA Astrophysics Data System (ADS)

Bettini, Luca Giacomo; Diamanti, Maria Vittoria; Sansotera, Maurizio; Pedeferri, Maria Pia; Navarrini, Walter; Milani, Paolo

2016-08-01

Anatase/rutile mixed-phase titanium dioxide (TiO2) photocatalysts in the form of nanostructured powders with different primary particle size, specific surface area, and rutile content were produced from the gas-phase by flame spray pyrolysis (FSP) starting from an organic solution containing titanium (IV) isopropoxide as Ti precursor. Flame spray-produced TiO2 powders were characterized by means of X-ray diffraction, Raman spectroscopy, and BET measurements. As-prepared powders were mainly composed of anatase crystallites with size ranging from 7 to 15 nm according to the synthesis conditions. TiO2 powders were embedded in a multilayered fluoropolymeric matrix to immobilize the nanoparticles into freestanding photocatalytic membranes. The photocatalytic activity of the TiO2-embedded membranes toward the abatement of hydrosoluble organic pollutants was evaluated employing the photodegradation of rhodamine B in aqueous solution as test reaction. The photoabatement rate of best performing membranes significantly overcomes that of membranes produced by the same method and incorporating commercial P25-TiO2.

Investigation of phase evolution of CaCu3Ti4O12 (CCTO) by in situ synchrotron high-temperature powder diffraction

NASA Astrophysics Data System (ADS)

Ouyang, Xin; Huang, Saifang; Zhang, Weijun; Cao, Peng; Huang, Zhaohui; Gao, Wei

2014-03-01

In situ synchrotron X-ray powder diffraction was used to study the high-temperature phase evolution of CaCu3Ti4O12 (CCTO) precursors prepared via solid-state and sol-gel methods. After the precursors are heated to 1225 °C, the CCTO phase is the main phase observed in the calcined powder, with the presence of some minor impurities. Comparing the two precursors, we found that the onset temperature for the CCTO phase formation is 800 °C in the sol-gel precursor, lower than that in the solid-state precursor (875 °C). Intermediate phases were only observed in the sol-gel precursor. Both precursors are able to be calcined to sub-micrometric sized powders. Based on the synchrotron data along with differential scanning calorimetry (DSC) and thermal gravimetric analysis (TGA), the phase formation sequence and mechanism during calcination are proposed in this study.

Ultra High Temperature Ceramics' Processing Routes and Microstructures Compared

NASA Technical Reports Server (NTRS)

Gusman, Michael; Stackpoole, Mairead; Johnson, Sylvia; Gasch, Matt; Lau, Kai-Hung; Sanjurjo, Angel

2009-01-01

Ultra High Temperature Ceramics (UHTCs), such as HfB2 and ZrB2 composites containing SiC, are known to have good thermal shock resistance and high thermal conductivity at elevated temperatures. These UHTCs have been proposed for a number of structural applications in hypersonic vehicles, nozzles, and sharp leading edges. NASA Ames is working on controlling UHTC properties (especially, mechanical properties, thermal conductivity, and oxidation resistance) through processing, composition, and microstructure. In addition to using traditional methods of combining additives to boride powders, we are preparing UHTCs using coat ing powders to produce both borides and additives. These coatings and additions to the powders are used to manipulate and control grain-boundary composition and second- and third-phase variations within the UHTCs. Controlling the composition of high temperature oxidation by-products is also an important consideration. The powders are consolidated by hot-pressing or field-assisted sintering (FAS). Comparisons of microstructures and hardness data will be presented.

[Ultra-Fine Pressed Powder Pellet Sample Preparation XRF Determination of Multi-Elements and Carbon Dioxide in Carbonate].

PubMed

Li, Xiao-li; An, Shu-qing; Xu, Tie-min; Liu, Yi-bo; Zhang, Li-juan; Zeng, Jiang-ping; Wang, Na

2015-06-01

The main analysis error of pressed powder pellet of carbonate comes from particle-size effect and mineral effect. So in the article in order to eliminate the particle-size effect, the ultrafine pressed powder pellet sample preparation is used to the determination of multi-elements and carbon-dioxide in carbonate. To prepare the ultrafine powder the FRITSCH planetary Micro Mill machine and tungsten carbide media is utilized. To conquer the conglomeration during the process of grinding, the wet grinding is preferred. The surface morphology of the pellet is more smooth and neat, the Compton scatter effect is reduced with the decrease in particle size. The intensity of the spectral line is varied with the change of the particle size, generally the intensity of the spectral line is increased with the decrease in the particle size. But when the particle size of more than one component of the material is decreased, the intensity of the spectral line may increase for S, Si, Mg, or decrease for Ca, Al, Ti, K, which depend on the respective mass absorption coefficient . The change of the composition of the phase with milling is also researched. The incident depth of respective element is given from theoretical calculation. When the sample is grounded to the particle size of less than the penetration depth of all the analyte, the effect of the particle size on the intensity of the spectral line is much reduced. In the experiment, when grounded the sample to less than 8 μm(d95), the particle-size effect is much eliminated, with the correction method of theoretical α coefficient and the empirical coefficient, 14 major, minor and trace element in the carbonate can be determined accurately. And the precision of the method is much improved with RSD < 2%, except Na2O. Carbon is ultra-light element, the fluorescence yield is low and the interference is serious. With the manual multi-layer crystal PX4, coarse collimator, empirical correction, X-ray spectrometer can be used to determine the carbon dioxide in the carbonate quantitatively. The intensity of the carbon is increase with the times of the measurement and the time delay even the pellet is stored in the dessicator. So employing the latest pressed powder pellet is suggested.

Influence of deposition and spray pattern of nasal powders on insulin bioavailability.

PubMed

Pringels, E; Callens, C; Vervaet, C; Dumont, F; Slegers, G; Foreman, P; Remon, J P

2006-03-09

The influence of the deposition pattern and spray characteristics of nasal powder formulations on the insulin bioavailability was investigated in rabbits. The formulations were prepared by freeze drying a dispersion containing a physical mixture of drum dried waxy maize starch (DDWM)/Carbopol 974P (90/10, w/w) or a spray-dried mixture of Amioca starch/Carbopol 974P (25/75, w/w). The deposition in the nasal cavity of rabbits and in a silicone human nose model after actuation of three nasal delivery devices (Monopowder, Pfeiffer and experimental system) was compared and related to the insulin bioavailability. Posterior deposition of the powder formulation in the nasal cavity lowered the insulin bioavailability. To study the spray pattern, the shape and cross-section of the emitted powder cloud were analysed. It was concluded that the powder bulk density of the formulation influenced the spray pattern. Consequently, powders of different bulk density were prepared by changing the solid fraction of the freeze dried dispersion and by changing the freezing rate during freeze drying. After nasal delivery of these powder formulations no influence of the powder bulk density and of the spray pattern on the insulin bioavailability was observed.

Synthesis of crystalline Ce-activated garnet phosphor powders and technique to characterize their scintillation light yield

NASA Astrophysics Data System (ADS)

Gordienko, E.; Fedorov, A.; Radiuk, E.; Mechinsky, V.; Dosovitskiy, G.; Vashchenkova, E.; Kuznetsova, D.; Retivov, V.; Dosovitskiy, A.; Korjik, M.; Sandu, R.

2018-04-01

This work reports on a process of preparation of garnet phosphor powders and a technique for light yield evaluation of strongly light scattering samples. Powders of scintillation compounds could be used as individual materials or as samples for express tests of scintillation properties. However, estimation of their light yield (LY) is complicated by strong light scattering of this kind of materials. Ce3+-activated yttrium-aluminum and gallium-gadolinium-aluminum garnet phosphor powders, Y3Al5O12 (YAG:Ce) and Gd3Ga3Al2O12 (GGAG:Ce), were obtained using a modified coprecipitation technique. Ga tends to residue in mother liquor in ammonia media, but the modification allows to avoid the loss of components. We propose an approach for sample preparation and LY measurement setup with alpha particles excitation, allowing to decrease light scattering influence and to estimate a light yield of powder samples. This approach is used to evaluate the obtained powders.

Microstructure and Transparent Super-Hydrophobic Performance of Vacuum Cold-Sprayed Al2O3 and SiO2 Aerogel Composite Coating

NASA Astrophysics Data System (ADS)

Li, Jie; Zhang, Yu; Ma, Kai; Pan, Xi-De; Li, Cheng-Xin; Yang, Guan-Jun; Li, Chang-Jiu

2018-02-01

In this study, vacuum cold spraying was used as a simple and fast way to prepare transparent super-hydrophobic coatings. Submicrometer-sized Al2O3 powder modified by 1,1,2,2-tetrahydroperfluorodecyltriethoxysilane and mixed with hydrophobic SiO2 aerogel was employed for the coating deposition. The deposition mechanisms of pure Al2O3 powder and Al2O3-SiO2 mixed powder were examined, and the effects of powder structure on the hydrophobicity and light transmittance of the coatings were evaluated. The results showed that appropriate contents of SiO2 aerogel in the mixed powder could provide sufficient cushioning to the deposition of submicrometer Al2O3 powder during spraying. The prepared composite coating surface showed rough structures with a large number of submicrometer convex deposited particles, characterized by being super-hydrophobic. Also, the transmittance of the obtained coating was higher than 80% in the range of visible light.

Innovative technologies for powder metallurgy-based disk superalloys: Progress and proposal

NASA Astrophysics Data System (ADS)

Chong-Lin, Jia; Chang-Chun, Ge; Qing-Zhi, Yan

2016-02-01

Powder metallurgy (PM) superalloys are an important class of high temperature structural materials, key to the rotating components of aero engines. In the purview of the present challenges associated with PM superalloys, two novel approaches namely, powder preparation and the innovative spray-forming technique (for making turbine disk) are proposed and studied. Subsequently, advanced technologies like electrode-induction-melting gas atomization (EIGA), and spark-plasma discharge spheroidization (SPDS) are introduced, for ceramic-free superalloy powders. Presently, new processing routes are sought after for preparing finer and cleaner raw powders for disk superalloys. The progress of research in spray-formed PM superalloys is first summarized in detail. The spray-formed superalloy disks specifically exhibit excellent mechanical properties. This paper reviews the recent progress in innovative technologies for PM superalloys, with an emphasis on new ideas and approaches, central to the innovation driving techniques like powder processing and spray forming. Project supported by the National Natural Science Foundation of China (Grant Nos. 50974016 and 50071014).

[Study on Archaeological Lime Powders from Taosi and Yinxu Sites by FTIR].

PubMed

Wei, Guo-feng; Zhang, Chen; Chen, Guo-liang; He, Yu-ling; Gao, Jiang-tao; Zhang, Bing-jian

2015-03-01

Archaeological lime powders samples from Taosi and Yinxu sites, natural limestone and experimentally prepared lime mortar were investigated by means of Fourier transform infrared spectrometry (FTIR) to identify the raw material of lime powders from Taosi and Yinxu sites. Results show that ν2/ν4 ratio of calcite resulted from carbonation reaction of man-made lime is around 6.31, which is higher than that of calcite in natural limestone and reflects the difference in the disorder of calcite crystal structure among the natural limestone and prepared lime mortar. With additional grinding, the values of v2 and ν4 in natural limestone and prepared lime mortar decrease. Meanwhile, the trend lines of ν2 versus ν4 for calcite in experimentally prepared lime mortar have a steeper slope when compared to calcite in natural limestone. These imply that ν2/ν4 ratio and the slope of the trend lines of ν2 versus ν4 can be used to determine the archaeological man-made lime. Based on the experiment results, it is possible that the archaeological lime powder from Taosi and Yinxu sites was prepared using man-made lime and the ancient Chinese have mastered the calcining technology of man-made lime in the late Neolithic period about 4 300 years ago.

Potato powders prepared by successive cooking-process depending on resistant starch content affect the intestinal fermentation in rats.

PubMed

Kawakami, Sakura; Han, Kyu-Ho; Araki, Takahiro; Ohba, Kiyoshi; Wakabayashi, Tatsuya; Shimada, Kenichiro; Fukushima, Michihiro

2017-02-01

The effects of resistant starch (RS) in dry potato powders prepared by various processes on intestinal fermentation in rats were assessed. Rats were fed raw potato powder (RP), blanched potato powder (BP), steamed potato powder (SP), or drum-dried potato powder (DP) for 4 weeks. The cecal RS content was significantly higher in the RP group than in the control diet (CN) group and other dry potato powder groups. Cecum pH was significantly lower in the RP group compared to the CN group, and was also significantly lower than that in the SP, BP, and DP groups. Lactic acid bacteria levels in the RP group were significantly higher than those in the CN group, and levels in the SP group also increased relative to the control group. Lactobacillus levels in the RP group were higher than in the CN and other dry potato powder groups. Cecal short-chain fatty acid (SCFA) concentrations in the RP group followed by the SP group exhibited significantly higher levels relative to the control levels. Dry potato powders containing RS produced during the cooking process may represent a useful food material that increases intestinal concentrations of SCFA and enhances the growth of certain lactic acid bacteria.

Bulk Al-Al3Zr composite prepared by mechanical alloying and hot extrusion for high-temperature applications

NASA Astrophysics Data System (ADS)

Pourkhorshid, E.; Enayati, M. H.; Sabooni, S.; Karimzadeh, F.; Paydar, M. H.

2017-08-01

Bulk Al/Al3Zr composite was prepared by a combination of mechanical alloying (MA) and hot extrusion processes. Elemental Al and Zr powders were milled for up to 10 h and heat treated at 600°C for 1 h to form stable Al3Zr. The prepared Al3Zr powder was then mixed with the pure Al powder to produce an Al-Al3Zr composite. The composite powder was finally consolidated by hot extrusion at 550°C. The mechanical properties of consolidated samples were evaluated by hardness and tension tests at room and elevated temperatures. The results show that annealing of the 10-h-milled powder at 600°C for 1 h led to the formation of a stable Al3Zr phase. Differential scanning calorimetry (DSC) results confirmed that the formation of Al3Zr began with the nucleation of a metastable phase, which subsequently transformed to the stable tetragonal Al3Zr structure. The tension yield strength of the Al-10wt%Al3Zr composite was determined to be 103 MPa, which is approximately twice that for pure Al (53 MPa). The yield stress of the Al/Al3Zr composite at 300°C is just 10% lower than that at room temperature, which demonstrates the strong potential for the prepared composite to be used in high-temperature structural applications.

Robust, heat-resistant and multifunctional superhydrophobic coating of carbon microflowers with molybdenum trioxide nanoparticles.

PubMed

Wu, Yang; Zhao, Meiyun; Guo, Zhiguang

2017-11-15

Superhydrophobic materials have triggered large interest due to their widespread applications, such as self-cleaning, corrosion resistance, anti-icing, and oil/water separation. However, suffering from weak mechanical strength, plenty of superhydrophobic materials are limited in practical application. Herein, we prepared hierarchical carbon microflowers (CMF) dispersed with molybdenum trioxide (MoO 3 ) nanoparticles (MoO 3 /CMF) via a two-step preparation method. Taking advantage of high-adhesion epoxy resin and the modification with 1H,1H,2H,2H-perfluorodecyltriethoxysilane (PDES), the modified MoO 3 /CMF (PDES-MoO 3 /CMF) coating on various substrates shows great waterproof ability, excellent chemical stability, good mechanical durability, and self-cleaning property. More significantly, the prepared PDES-MoO 3 /CMF powder with high thermal stability (250°C) can be used for oil/water separation due to its special flower-like structure and superhydrophobicity/superoleophilicity. All of these advantages endow the superhydrophobic powders with huge potential in the practical applications. Copyright © 2017 Elsevier Inc. All rights reserved.

Preparation and UV-Vis photodegradation of gaseous benzene by TiO2 nanotube arrays supporting V2O5 nanoparticles

NASA Astrophysics Data System (ADS)

Zhao, Chunxia; Song, Yanbao; Yang, Yunxia; Chen, Wen; Li, Xiaoyu; Wang, Zongsheng

2015-07-01

TiO2-based catalysts effective in visible radiation for eliminating organic pollutants have attracted intense research activity as a future generation photocatalytic material. However, recombination of electron-hole pairs through trapping/de-trapping as well as the disadvantages of recycling and separation/filtration of powders lead to the limitation of powder TiO2 materials. TiO2 nanotube array films supporting vanadium pentoxide nanoparticles (VTNTs) were synthesized by electrophoresis deposition method with the prepared TiO2 nanotube arrays as the cathode and V2O5 sol as the electrolyte. The results indicate that the formation of Ti-O-V bonds and intimate interaction between host-guest interfaces help to enhance the hybrids’ photodegradation activity of gaseous benzene. Importantly, hybrid film catalysts prepared with 0.05 mol/L V2O5 sol for 10 min electrophoresis deposition perform a 98% conversion rate of benzene and 1028.8 mg/m3CO2 production in 80 min under UV-Vis irradiation.

Optical, Magnetic and Photocatalytic Activity Studies of Li, Mg and Sr Doped and Undoped Zinc Oxide Nanoparticles.

PubMed

Shanthi, S I; Poovaragan, S; Arularasu, M V; Nithya, S; Sundaram, R; Magdalane, C Maria; Kaviyarasu, K; Maaza, M

2018-08-01

Nanoparticles of Li, Mg and Sr doped and undoped zinc oxide was prepared by simple precipitation method. The structural, optical, and magnetic properties of the samples were investigated by the Powder X-ray Diffraction (XRD), Scanning Electron Microscope (SEM), Transmission Electron Microscope (TEM), Fourier Transform Infrared (FTIR) spectroscopy, Ultra-violet Visible spectroscopy (UV-vis) spectra, Photoluminescence (PL) and Vibrational Sample Magnetometer (VSM). The Powder X-ray diffraction data confirm the formation of hexagonal wurtzite structure of all doped and undoped ZnO. The SEM photograph reveals that the pores availability and particles size in the range of 10 nm-50 nm. FTIR and UV-Visible spectra results confirm the incorporation of the dopant into the ZnO lattice nanostructure. The UV-Visible spectra indicate that the shift of blue region (lower wavelength) due to bandgap widening. Photoluminescence intensity varies with doping due to the increase of oxygen vacancies in prepared ZnO. The pure ZnO exist paramagnetic while doped (Li, Mg and Sr) ZnO exist ferromagnetic property. The photocatalytic activity of the prepared sample also carried out in detail.

Development of a Freeze-Dried Fungal Wettable Powder Preparation Able to Biodegrade Chlorpyrifos on Vegetables

PubMed Central

Chen, Shaohua; Xiao, Ying; Hu, Meiying; Zhong, Guohua

2014-01-01

Continuous use of the pesticide chlorpyrifos has resulted in harmful contaminations in environment and species. Based on a chlorpyrifos-degrading fungus Cladosporium cladosporioides strain Hu-01 (collection number: CCTCC M 20711), a fungal wettable powder preparation was developed aiming to efficiently remove chlorpyrifos residues from vegetables. The formula was determined to be 11.0% of carboxymethyl cellulose-Na, 9.0% of polyethylene glycol 6000, 5.0% of primary alcohol ethoxylate, 2.5% of glycine, 5.0% of fucose, 27.5% of kaolin and 40% of freeze dried fungi by response surface methodology (RSM). The results of quality inspection indicated that the fungal preparation could reach manufacturing standards. Finally, the degradation of chlorpyrifos by this fungal preparation was determined on pre-harvest cabbage. Compared to the controls without fungal preparation, the degradation of chlorpyrifos on cabbages, which was sprayed with the fungal preparation, was up to 91% after 7 d. These results suggested this freeze-dried fungal wettable powder may possess potential for biodegradation of chlorpyrifos residues on vegetables and provide a potential strategy for food and environment safety against pesticide residues. PMID:25061758

Development of a freeze-dried fungal wettable powder preparation able to biodegrade chlorpyrifos on vegetables.

PubMed

Liu, Jie; He, Yue; Chen, Shaohua; Xiao, Ying; Hu, Meiying; Zhong, Guohua

2014-01-01

Continuous use of the pesticide chlorpyrifos has resulted in harmful contaminations in environment and species. Based on a chlorpyrifos-degrading fungus Cladosporium cladosporioides strain Hu-01 (collection number: CCTCC M 20711), a fungal wettable powder preparation was developed aiming to efficiently remove chlorpyrifos residues from vegetables. The formula was determined to be 11.0% of carboxymethyl cellulose-Na, 9.0% of polyethylene glycol 6000, 5.0% of primary alcohol ethoxylate, 2.5% of glycine, 5.0% of fucose, 27.5% of kaolin and 40% of freeze dried fungi by response surface methodology (RSM). The results of quality inspection indicated that the fungal preparation could reach manufacturing standards. Finally, the degradation of chlorpyrifos by this fungal preparation was determined on pre-harvest cabbage. Compared to the controls without fungal preparation, the degradation of chlorpyrifos on cabbages, which was sprayed with the fungal preparation, was up to 91% after 7 d. These results suggested this freeze-dried fungal wettable powder may possess potential for biodegradation of chlorpyrifos residues on vegetables and provide a potential strategy for food and environment safety against pesticide residues.