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.

Synthesis and impurity doping of GaN powders by the two-stage vapor-phase method for phosphor applications

NASA Astrophysics Data System (ADS)

Hara, K.; Okuyama, E.; Yonemura, A.; Uchida, T.; Okamoto, N.

2006-09-01

The analysis of particle formation and the doping of luminescent impurities during the two-stage vapor-phase synthesis of GaN powder were carried. GaN particles were grown very fast during the second stage of this method, and the increment in particle size was larger for higher reaction temperature in the region between 800 and 1000 °C. The analysis on the behaviour of particle growth based on the reaction kinetics suggested that the growth almost finishes in a few seconds with an extremely high rate at the early stage at 1000 °C, whereas the growth lasts with relatively low rates for a time longer than the actual growth duration for the case of lower temperature synthesis. GaN powders doped with various impurity atoms were synthesized by supplying impurity sources with GaCl during the second stage. The samples doped with Zn, Mg and Tb showed emissions characteristic for each doped impurity.

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.

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.

Synthesis and characterization of barium hexaferrite with manganese (Mn) doping material as anti-radar

NASA Astrophysics Data System (ADS)

Susilawati, Doyan, Aris; Khalilurrahman

2017-01-01

Have been successfully synthesized barium powder doping Manganese hexaferrite with the expected potential as anti-radar material. Synthesis was done by using the co-precipitation method, the variation of the variable x concentrations used were 0; 0.2; 0.4; and 0.6 and calcined at temperatures of 400, 600 and 800°C. Characterization powders of hexaferrite have used XRD (X-Ray Diffraction), SEM (Scanning Electron Microscopy), TEM (Transmission Electron Microscopy), LCR (inductance, capacitance, and resistance) meter, and VSM (Vibrating Sample Magnetometer). The higher the concentration and temperature of calcinations given affect the color of the powder. The test results using XRD indicates that it has formed barium hexaferrite phase with a hexagonal crystal structure. Tests using SEM showed that all the constituent elements barium powder hexaferrite by doping Manganese powders have been spread evenly. XRD test results were confirmed by a test using a TEM showing the crystal structure and the powder was sized nano particles. The results from the LCR meter showed that the barium powder hexaferrite by doping Manganese that has been synthesized classified in semiconductor materials. The result from VSM showed that the value of coercivity magnetic powder doped barium hexaferrite Manganese is smaller when compared with barium hexaferrite without doping and belong to the soft magnetic. Based on the results of the synthesis and characterization, we can conclude that the barium powder heksaferrite by doping Manganese potential as a material anti-radar.

Micro structrual characterization and analysis of ball milled silicon carbide

NASA Astrophysics Data System (ADS)

Madhusudan, B. M.; Raju, H. P.; Ghanaraja., S.

2018-04-01

Mechanical alloying has been one of the prominent methods of powder synthesis technique in solid state involving cyclic deformation, cold welding and fracturing of powder particles. Powder particles in this method are subjected to greater mechanical deformation due to the impact of ball-powder-ball and ball-powder-container collisions that occurs during mechanical alloying. Strain hardening and fracture of particles decreases the size of the particles and creates new surfaces. The objective of this Present work is to use ball milling of SiC powder for different duration of 5, 10, 15 and 20 hours by High energy planetary ball milling machine and to evaluate the effect of ball milling on SiC powder. Micro structural Studies using Scanning Electron Microscopy (SEM), X-ray Diffraction (XRD) and EDAX has been investigated.

Synthesis of ultrafine powders by microwave heating

DOEpatents

Meek, T.T.; Sheinberg, H.; Blake, R.D.

1987-04-24

A method of synthesizing ultrafine powders using microwaves is described. A water soluble material is dissolved in water and the resulting aqueous solution is exposed to microwaves until the water has dissolved. The resulting material is an ultrafine powder. This method can be used to make Al/sub 2/O/sub 3/, NiO /plus/ Al/sub 2/O/sub 3/ and NiO as well as a number of other materials including GaBa/sub 2/Cu/sub 3/O/sub x/. 1 tab.

Synthesis of ultrafine powders by microwave heating

DOEpatents

Meek, Thomas T.; Sheinberg, Haskell; Blake, Rodger D.

1988-01-01

A method of synthesizing ultrafine powders using microwaves is described. A water soluble material is dissolved in water and the resulting aqueous solution is exposed to microwaves until the water has been removed. The resulting material is an ultrafine powder. This method can be used to make Al.sub.2 O.sub.3, NiO+Al.sub.2 O.sub.3 and NiO as well as a number of other materials including GaBa.sub.2 Cu.sub.3 O.sub.x.

A new powder production route for transparent spinel windows: powder synthesis and window properties

NASA Astrophysics Data System (ADS)

Cook, Ronald; Kochis, Michael; Reimanis, Ivar; Kleebe, Hans-Joachim

2005-05-01

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. The new powder production method allows fine control over the starting particle size, size distribution, purity and stoichiometry. The new process involves formation of a boehmite sol-gel from the hydrolysis of aluminum alkoxides followed by surface modification of the boehmite nanoparticles using carboxylic acids. The resulting surface modified boehmite nanoparticles can then be metal exchanged at room temperature with magnesium acetylacetonate to make a precursor powder that is readily transformed into pure phase spinel.

Synthesis of LiFePO4/C composites based on natural iron stone using a sol gel method

NASA Astrophysics Data System (ADS)

Angela, Riyan; Islam, Humaatul; Sari, Vamellia; Latif, Chaironi; Zainuri, Mochamad; Pratapa, Suminar

2017-01-01

Synthesis of LiFePO4/C composites has been carried out using a sol gel method. The Fe precursor was made from a natural iron stone of Tanah Laut, South Kalimantan, while the other raw materials were commercial Li2CO3 powder and NH4H2PO4 powder with HCl and water as solvents. Citric acid was used as the carbon source in the synthesis. This study used a molar ratio of 1:1:2 for Li:Fe:P with variation of added citric acid of 1.5 and 2.5 g. The solutions were dried in air at 100°C. The dried powders were characterized using DSC-TGA and then calcined at 600 and 700°C under argon environment for 10 hours. The calcined powders were characterized by X-ray diffractometry (XRD), scanning electron microscopy-energy dispersive x-ray (SEM-EDX), and LCR meter. It was found that the samples contained LiFePO4 as the dominant phase and LiFeP2O7 and Fe2O3 as secondary phases. The analysis showed that the addition of citric acid influenced the electronic conductivity of the composites. A Rietveld relative weight fraction of up to 94.7% was achieved in the synthesis at temperature 600°C. The LFP/C sample exhibited electronic conductivity of 4.56×10-3 Scm-1 which was six times of that of the pure LFP.

Combustion synthesis method and products

DOEpatents

Holt, J.B.; Kelly, M.

1993-03-30

Disclosed is a method of producing dense refractory products, comprising: (a) obtaining a quantity of exoergic material in powder form capable of sustaining a combustion synthesis reaction; (b) removing absorbed water vapor therefrom; (c) cold-pressing said material into a formed body; (d) plasma spraying said formed body with a molten exoergic material to form a coat thereon; and (e) igniting said exoergic coated formed body under an inert gas atmosphere and pressure to produce self-sustained combustion synthesis. Also disclosed are products produced by the method.

Combustion synthesis method and products

DOEpatents

Holt, J. Birch; Kelly, Michael

1993-01-01

Disclosed is a method of producing dense refractory products, comprising: (a) obtaining a quantity of exoergic material in powder form capable of sustaining a combustion synthesis reaction; (b) removing absorbed water vapor therefrom; (c) cold-pressing said material into a formed body; (d) plasma spraying said formed body with a molten exoergic material to form a coat thereon; and (e) igniting said exoergic coated formed body under an inert gas atmosphere and pressure to produce self-sustained combustion synthesis. Also disclosed are products produced by the 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.

Freeze drying vs microwave drying-methods for synthesis of sinteractive thoria powders

NASA Astrophysics Data System (ADS)

Annie, D.; Chandramouli, V.; Anthonysamy, S.; Ghosh, Chanchal; Divakar, R.

2017-02-01

Thoria powders were synthesized by oxalate precipitation from an aqueous solution of the nitrate. The filtered precipitates were freeze dried or microwave dried before being calcined at 1073 K. The thoria powders obtained were characterized for crystallite size, specific surface area, bulk density, particle size distribution and residual carbon. Microstructure of the product was studied using scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Sinterability of the synthesized powders was studied by measuring the density of the sintered compacts. Powders that can be consolidated and sintered to densities ∼96% theoretical density (TD) at 1773 K were obtained.

Surface Coating of Oxide Powders: A New Synthesis Method to Process Biomedical Grade Nano-Composites

PubMed Central

Palmero, Paola; Montanaro, Laura; Reveron, Helen; Chevalier, Jérôme

2014-01-01

Composite and nanocomposite ceramics have achieved special interest in recent years when used for biomedical applications. They have demonstrated, in some cases, increased performance, reliability, and stability in vivo, with respect to pure monolithic ceramics. Current research aims at developing new compositions and architectures to further increase their properties. However, the ability to tailor the microstructure requires the careful control of all steps of manufacturing, from the synthesis of composite nanopowders, to their processing and sintering. This review aims at deepening understanding of the critical issues associated with the manufacturing of nanocomposite ceramics, focusing on the key role of the synthesis methods to develop homogeneous and tailored microstructures. In this frame, the authors have developed an innovative method, named “surface-coating process”, in which matrix oxide powders are coated with inorganic precursors of the second phase. The method is illustrated into two case studies; the former, on Zirconia Toughened Alumina (ZTA) materials for orthopedic applications, and the latter, on Zirconia-based composites for dental implants, discussing the advances and the potential of the method, which can become a valuable alternative to the current synthesis process already used at a clinical and industrial scale. PMID:28788117

Synthesis of TiCx Powder via the Underwater Explosion of an Explosive

NASA Astrophysics Data System (ADS)

Tanaka, Shigeru; Bataev, Ivan; Hamashima, Hideki; Tsurui, Akihiko; Hokamoto, Kazuyuki

2018-05-01

In this study, a novel approach to the explosive synthesis of titanium carbide (TiC) is discussed. Nonstoichiometric TiCx powder was produced via the underwater explosion of a Ti powder encapsulated within a spherical explosive charge. The explosion process, bubble formation, and synthesis process were visualized using high-speed camera imaging. It was concluded that synthesis occurred within the detonation gas during the first expansion/contraction cycle of the bubble, which was accompanied by a strong emission of light. The recovered powders were studied using scanning electron microscopy and X-ray diffraction. Submicron particles were generated during the explosion. An increase in the carbon content of the starting powder resulted in an increase in the carbon content of the final product. No oxide byproducts were observed within the recovered powders.

Combustion of Na 2B 4O 7 + Mg + C to synthesis B 4C powders

NASA Astrophysics Data System (ADS)

Guojian, Jiang; Jiayue, Xu; Hanrui, Zhuang; Wenlan, Li

2009-09-01

Boron carbide powder was fabricated by combustion synthesis (CS) method directly from mixed powders of borax (Na 2B 4O 7), magnesium (Mg) and carbon. The adiabatic temperature of the combustion reaction of Na 2B 4O 7 + 6 Mg + C was calculated. The control of the reactions was achieved by selecting reactant composition, relative density of powder compact and gas pressure in CS reactor. The effects of these different influential factors on the composition and morphologies of combustion products were investigated. The results show that, it is advantageous for more Mg/Na 2B 4O 7 than stoichiometric ratio in Na 2B 4O 7 + Mg + C system and high atmosphere pressure in the CS reactor to increase the conversion degree of reactants to end product. The final product with the minimal impurities' content could be fabricated at appropriate relative density of powder compact. At last, boron carbide without impurities could be obtained after the acid enrichment and distilled water washing.

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.

CTAB-assisted hydrothermal synthesis of YVO 4:Eu 3+ powders in a wide pH range

NASA Astrophysics Data System (ADS)

Wang, Juan; Hojamberdiev, Mirabbos; Xu, Yunhua

2012-01-01

Rhombus-, rod-, soya bean- and aggregated soya bean-like YVO 4:Eu 3+ micro- and nanostructures were synthesized by a cetyltrimethylammonium bromide (CTAB)-assisted hydrothermal method at 180 °C for 24 h in a wide pH range. The as-synthesized powders were characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and photoluminescence spectroscopy (PL). The XRD results confirmed the formation of phase-pure YVO 4:Eu 3+ powders with tetragonal structure under hydrothermal process in a wide pH range. Electron microscopic observations evidenced the morphological transformation of YVO 4:Eu 3+ powders from rhombus-like microstructure to rod-, soya bean, and aggregated soya bean-like nanostructures with an increase in the pH of the synthesis solution. The results from the PL measurements revealed that the intensities of PL emission peaks were significantly affected by the morphologies and crystallinity of samples due to the absence of an inversion symmetry at the Eu 3+ lattice site, and the highest luminescence intensity was observed for rod-like YVO 4:Eu 3+ powders.

Effect of powder compaction on radiation-thermal synthesis of lithium-titanium ferrites

NASA Astrophysics Data System (ADS)

Surzhikov, A. P.; Lysenko, E. N.; Vlasov, V. A.; Malyshev, A. V.; Korobeynikov, M. V.; Mikhailenko, M. A.

2017-01-01

Effect of powder compaction on the efficiency of thermal and radiation-thermal synthesis of lithium-substituted ferrites was investigated by X-Ray diffraction and specific magnetization analysis. It was shown that the radiation-thermal heating of compacted powder reagents mixture leads to an increase in efficiency of lithium-titanium ferrites synthesis.

Rapid and direct synthesis of complex perovskite oxides through a highly energetic planetary milling

PubMed Central

Lee, Gyoung-Ja; Park, Eun-Kwang; Yang, Sun-A; Park, Jin-Ju; Bu, Sang-Don; Lee, Min-Ku

2017-01-01

The search for a new and facile synthetic route that is simple, economical and environmentally safe is one of the most challenging issues related to the synthesis of functional complex oxides. Herein, we report the expeditious synthesis of single-phase perovskite oxides by a high-rate mechanochemical reaction, which is generally difficult through conventional milling methods. With the help of a highly energetic planetary ball mill, lead-free piezoelectric perovskite oxides of (Bi, Na)TiO3, (K, Na)NbO3 and their modified complex compositions were directly synthesized with low contamination. The reaction time necessary to fully convert the micron-sized reactant powder mixture into a single-phase perovskite structure was markedly short at only 30–40 min regardless of the chemical composition. The cumulative kinetic energy required to overtake the activation period necessary for predominant formation of perovskite products was ca. 387 kJ/g for (Bi, Na)TiO3 and ca. 580 kJ/g for (K, Na)NbO3. The mechanochemically derived powders, when sintered, showed piezoelectric performance capabilities comparable to those of powders obtained by conventional solid-state reaction processes. The observed mechanochemical synthetic route may lead to the realization of a rapid, one-step preparation method by which to create other promising functional oxides without time-consuming homogenization and high-temperature calcination powder procedures. PMID:28387324

A novel method for the synthesis of zirconia powder

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

Bohe, A.E.; Pasquevich, D.M.

A novel method for the synthesis of zirconia powder is presented in this paper. The formation of fine particles of zirconia takes place when metallic zirconium and hematite are heated in the presence of gaseous chlorine. The overall process, which can be described by the following reaction: 3 Zr(s) + 2 Fe{sub 2}O{sub 3}(s) {r_arrow} 3 ZrO{sub 2}(s) + 4 Fe(s), occurs by a mass-transport mechanism through the vapor phase between 723 and 1223 K. The vapor-mass transport among the solid species takes place by means of zirconium and iron chlorides. The fundamentals of synthesis are discussed on the basismore » of a detailed thermodynamic analysis of reactions involved in the process, as well as by a characterization of the solid phases formed at various temperatures at XRD and SEM examinations.« less

Effect of Pressing Parameters on the Structure of Porous Materials Based on Cobalt and Nickel Powders

NASA Astrophysics Data System (ADS)

Shustov, V. S.; Rubtsov, N. M.; Alymov, M. I.; Ankudinov, A. B.; Evstratov, E. V.; Zelensky, V. A.

2018-03-01

Porous materials with a bulk porosity of more than 68% were synthesized by powder metallurgy methods from a cobalt-nickel mixture. The effect of the ratio of nickel and cobalt powders used in the synthesis of this porous material (including cases when either nickel or cobalt alone was applied) and the conditions of their compaction on structural parameters, such as open and closed porosities and pose size, was established.

Impact of physical and chemical parameters on the hydroxyapatite nanopowder synthesized by chemical precipitation method

NASA Astrophysics Data System (ADS)

Thu Trang Pham, Thi; Phuong Nguyen, Thu; Pham, Thi Nam; Phuong Vu, Thi; Tran, Dai Lam; Thai, Hoang; Thanh Dinh, Thi Mai

2013-09-01

In this paper, the synthesis of hydroxyapatite (HAp) nanopowder was studied by chemical precipitation method at different values of reaction temperature, settling time, Ca/P ratio, calcination temperature, (NH4)2HPO4 addition rate, initial concentration of Ca(NO3)2 and (NH4)2HPO4. Analysis results of properties, morphology, structure of HAp powder from infrared (IR) spectra, x-ray diffraction (XRD), energy dispersive x-ray (EDX) spectra and scanning electron microscopy (SEM) indicated that the synthesized HAp powder had cylinder crystal shape with size less than 100 nm, single-phase structure. The variation of the synthesis conditions did not affect the morphology but affected the size of HAp crystals.

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.

Sonochemical method for producing titanium metal powder.

PubMed

Halalay, Ion C; Balogh, Michael P

2008-07-01

We demonstrate a sonochemical method for producing titanium metal powder. The method uses low intensity ultrasound in a hydrocarbon solvent at near-ambient temperatures to first create a colloidal suspension of liquid sodium-potassium alloy in the solvent and then to reduce liquid titanium tetrachloride to titanium metal under cavitation conditions. XRD data collected for the reaction products after the solvent removal show only NaCl and KCl, with no diffraction peaks attributable to titanium metal or other titanium compounds, indicating either the formation of amorphous metal or extremely small crystallite size. TEM micrographs show that hollow spheres formed of halide salts and titanium metal, with diameters with diameters ranging from 100 to 500 nm and a shell thickness of 20 to 40 nm form during the synthesis, suggesting that the sonochemical reaction occurs inside the liquid shell surrounding the cavitation bubbles. Metal particle sizes are estimated to be significantly smaller than 40 nm from TEM data. XRD data of the powder after annealing and prior to removal of the alkali chloride salts provides direct evidence that titanium metal was formed during the sonochemical synthesis.

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

Structural Ceramic Nanocomposites: A Review of Properties and Powders’ Synthesis Methods

PubMed Central

Palmero, Paola

2015-01-01

Ceramic nanocomposites are attracting growing interest, thanks to new processing methods enabling these materials to go from the research laboratory scale to the commercial level. Today, many different types of nanocomposite structures are proposed in the literature; however, to fully exploit their exceptional properties, a deep understanding of the materials’ behavior across length scales is necessary. In fact, knowing how the nanoscale structure influences the bulk properties enables the design of increasingly performing composite materials. A further key point is the ability of tailoring the desired nanostructured features in the sintered composites, a challenging issue requiring a careful control of all stages of manufacturing, from powder synthesis to sintering. This review is divided into four parts. In the first, classification and general issues of nanostructured ceramics are reported. The second provides basic structure–property relations, highlighting the grain-size dependence of the materials properties. The third describes the role of nanocrystalline second-phases on the mechanical properties of ordinary grain sized ceramics. Finally, the fourth part revises the mainly used synthesis routes to produce nanocomposite ceramic powders, underlining when possible the critical role of the synthesis method on the control of microstructure and properties of the sintered ceramics. PMID:28347029

Synthesis of cristobalite from silica sands of Tuban and Tanah Laut

NASA Astrophysics Data System (ADS)

Nurbaiti, U.; Pratapa, S.

2018-03-01

Synthesis of SiO2 cristobalite powders has been successfully carried out by a coprecipitation method by making use of local silica sands from districts of Tuban and Tanah Laut, Indonesia. Cristobalite is a phase of SiO2 polymorphs which can be used as a composite filler, a coating material, a surface finishing media, and structural ceramics. In the first stage of the synthesis, the as-received sands were processed by a magnetic separation, grinding, and soaking with HCl to increase the purity of silica content. X-ray fluorescence (XRF) spectroscopy showed that the atomic content of Si (excluding oxygen) in both powders reached 95.3 and 97.4%. A coprecipitation process was then performed by dissolving the silica powders in a 7M NaOH solution followed by a titration with 2M HCl to achieve a normal pH and to form a gel. Furthermore, the silica gel is washed, dried and then calcined at a temperature of between 950-1200 °C with a variation of holding time for 1, 4 dan 10 hrs to produce white powders. X-ray diffraction (XRD) data analyses showed that the powder with calcination temperature of 1150 °C for 4 hrs exhibited the highest cristobalite content of up to 95wt%. Its scanning electron microscopy (SEM) image showed that its grain morphology was relatively homogeneous.

Improvement in synthesis of (K 0.5Na 0.5)NbO 3 powders by Ge 4+ acceptor doping

DOE PAGES

Zhao, Yajing; Chen, Yan; Chen, Kepi

2016-11-17

In this study, the effects of doping with GeO 2 on the synthesis temperature, phase structure and morphology of (K 0.5Na 0.5)NbO 3 (KNN) ceramic powders were studied using XRD and SEM. The results show that KNN powders with good crystallinity and compositional homogeneity can be obtained after calcination at up to 900°C for 2 h. Introducing 0.5 mol.% GeO 2 into the starting mixture improved the synthesis of the KNN powders and allowed the calcination temperature to be decreased to 800°C, which can be ascribed to the formation of the liquid phase during the synthesis.

Synthesis of Nano-Polycrystalline Synroc-B Powders as a High Level Radioactive Wastes Ceramic Forms by a Solution Combustion Synthesis.

PubMed

Han, Young-Min; Lee, Sang-Jin; Kim, Yeon-Ku; Jung, Choong-Hwan

2016-02-01

Synroc (Synthetic Rock) consists of four main titanate phases: peroveskite (CaTiO3), zirconolite (CaZrTi2O7), hollandite (BaAl2Ti6O16) and rutile (TiO2). Nano-polycrystalline synroc powders were made by a synthesis combustion process. The combustion process, an externally initiated reaction is self-sustained owing to the exothermic reaction. A significant volume of gas is evolved during the combustion reaction and leads to loosely agglomerated powders. This exothermic reaction provides necessary heat to further carry the reaction in forward direction to produce nanocrystalline powders as the final product. Glycine is used as a fuel, being oxidized by nitrate ions. It is inexpensive, has high energy efficiency, fast heating rates, short reaction times and high compositional homogeneity. In this study, combustion synthesis of nano-sized synroc-B powder is introduced. The fabrication of synroc-B powder result of observation XRD were prepared for polycrystalline (perovskite, zirconolite, hollandite, rutile) structures. The characterization of the synthesized powders is conducted by using XRD, SEM/EDS and TEM.

Method for synthesizing fine-grained phosphor powders of the type (RE.sub.1- Ln.sub.x)(P.sub.1-y V.sub.y)O.sub.4

DOEpatents

Phillips, Mark L. F.

1998-01-01

A method for generating well-crystallized photo- and cathodoluminescent oxide phosphor powders. The method of this invention uses hydrothermal synthesis and annealing to produce nearly monosized (RE.sub.1-x Ln.sub.x)(P.sub.1-y V.sub.y)O.sub.4 (Ln.dbd.Ce.fwdarw.Lu) phosphor grains with crystallite sizes from 0.04 to 5 .mu.m. Such phosphors find application in cathode-ray tube, flat-panel, and projection displays.

Effect of solution combusted TiO2 nanopowder within commercial BaTiO3 dielectric layer on the photoelectric properties for AC powder electroluminescence devices.

PubMed

Park, Sung; Choi, Gil Rak; Kim, Youn Cheol; Lee, Jae Chun; Lee, Ju Hyeon

2013-05-01

A unique synthesis method was developed, which is called solution combustion method (SCM). TiO2 nanopowder was synthesized by this method. This SCM TiO2 nanopowder (-35 nm) was added to the dielectric layer of AC powder electroluminescence (EL) device. The dielectric layer was made of commercial BaTiO3 powder (-1.2 microm) and binding polymer. 0, 5, 10 and 15 wt% of SCM TiO2 nanopowder was added to the dielectric layer during fabrication of AC powder EL device respectively. Dielectric constant of these four kinds of dielectric layers was measured. The brightness and current density of AC powder EL device were also measured. When 10 wt% of SCM TiO2 nanopowder was added, dielectric constant and brightness were increased by 30% and 101% respectively. Furthermore, the current density was decreased by 71%. This means that the brightness was double and the power consumption was one third.

Lifetime of excess electrons in Cu–Zn–Sn–Se powders

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

Novikov, G. F., E-mail: ngf@icp.ac.ru; Gapanovich, M. V.; Gremenok, V. F.

2017-01-15

The method of time-resolved microwave photoconductivity at a frequency of 36 GHz in the range of temperatures of 200–300 K is used to study the kinetics of the annihilation of charge carriers in Cu–Zn–Sn–Se powders obtained by the solid-phase method of synthesis in cells. The lifetime of excess electrons at room temperature is found to be shorter than 5 ns. The activation energy for the process of recombination amounted to E{sub a} ~ 0.054 eV.

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 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

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.

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 Development of High Transition Temperature Superconducting Ceramic Thick Films and Wire Composites

DTIC Science & Technology

1991-12-02

number of protein or sugar agents were experimented with including Agar, pectin, carboxymethylcellulose, gelatin, alginic acid, xanthan gum , guar gum ...I) Introduction and Description of Scientific Goals 1 II) Material and Powder Synthesis 1 A) Freeze Dried Fabrication of Powders 1 B) Utilization of...composites. II). Material and Powder Synthesis The availability of a reliable technique for producing large quantities of phase pure, submicron powders

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).

Synthesis and characterization of graphene oxide using modified Hummer's method

NASA Astrophysics Data System (ADS)

Kaur, Manpreet; Kaur, Harsimran; Kukkar, Deepak

2018-05-01

In the present study, a simple approach has been followed for the synthesis of graphene oxide (GO) using modified Hummers method in which graphite powder was oxidized in the presence of concentrated H2SO4 and KMnO4. The amount of NaNO3 and KMnO4 was varied to produce sheet like structure. The varied concentrations of NaNO3 and KMnO4 resulted in yielding large amount of the product. Structural, morphological and physicochemical features of the product were studied using UV-Visible spectrophotometer, Fourier Transform infrared spectroscopy (FTIR), and crystal structure was determined using X-ray powder diffraction (XRD). UV-Vis spectra of GO was observed at a maximum absorption of 230 nm due to (π-π*) transition of atomic carbon-carbon bonds. FTIR spectra revealed the presence of oxygen containing functional groups which ensures the complete exfoliation of graphite into graphene oxide X-ray powder diffraction pattern of the product showed the diffraction peak at (2θ = 26.7°) with an interlayer spacing of 0.334 nm. All the above characterizations successfully confirmed the formation of GO.

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.

Synthesis and characterization of nanocrystalline Nd{sup 3+}-doped gadolinium scandium aluminum garnet powders by a gel-combustion method

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

Su, Jing, E-mail: zlj007@126.com; Miao, Ju-hong; Xu, Lin-hua

2012-07-15

Graphical abstract: The graph shows the emission spectra (λ{sub ex} = 808 nm) of 1 at.% Nd:GSAG powders sintered at different temperatures for 3 h. Compared with the powder sintered at 900 °C, the PL intensity of the powder sintered at 1000 °C decreased significantly. The changes in the PL intensity should mainly due to the crystallinity and dispersion of the powders. Highlights: ► We synthesized Nd:GSAG nano-powders by gel-combustion method successfully. ► We analyzed the structure and the morphology of the heat-treated products. ► We studied the optical characteristics of Nd:GSAG nano-powders. -- Abstract: Nd{sup 3+}-doped gadolinium scandium aluminummore » garnet (Nd:GSAG) precursor was synthesized by a gel combustion method using metal nitrates and citric acid as raw materials. The structure and morphology of the precursor and the sintered powders were studied by means of X-ray diffraction (XRD), infrared spectroscopy (IR) and transmission electron microscopy (TEM). The results showed that the precursor transformed into pure GSAG polycrystalline phase at about 800 °C, and the powders sintered at 800–1000 °C were well-dispersed with average particle sizes in the range of 30–80 nm. Optical properties of Nd:GSAG nano-powders were characterized by using photoluminescence spectroscopy. The highest photoluminescence intensity was achieved for the powder sintered at 900 °C.« less

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.

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.

Method for synthesizing fine-grained phosphor powders of the type (RE{sub 1{minus}x}Ln{sub x})(P{sub 1{minus}y}V{sub y})O{sub 4}

DOEpatents

Phillips, M.L.F.

1998-04-28

A method for generating well-crystallized photo- and cathodoluminescent oxide phosphor powders is disclosed. The method of this invention uses hydrothermal synthesis and annealing to produce nearly monosized (RE{sub 1{minus}x}Ln{sub x})(P{sub 1{minus}y}V{sub y}O{sub 4}) (Ln{double_bond}Ce{yields}Lu) phosphor grains with crystallite sizes from 0.04 to 5 {micro}m. Such phosphors find application in cathode-ray tube, flat-panel, and projection displays. 4 figs.

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.

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.

Calcium hydride synthesis of Ti-Nb-based alloy powders

NASA Astrophysics Data System (ADS)

Kasimtsev, A. V.; Shuitsev, A. V.; Yudin, S. N.; Levinskii, Yu. V.; Sviridova, T. A.; Alpatov, A. V.; Novosvetlova, E. E.

2017-09-01

The metallothermic (calcium hydride) synthesis of Ti-Nb alloy powders alloyed with tantalum and zirconium is experimentally studied under various conditions. Chemical, X-ray diffraction, and metallographic analyses of the synthesized products show that initial oxides are completely reduced and a homogeneous β-Ti-based alloy powder forms under the optimum synthesis conditions at a temperature of 1200°C. At a lower synthesis temperature, the end products have a high oxygen content. The experimental results are used to plot the thermokinetic dependences o formation of a bcc solid solution at various times of isothermal holding of Ti-22Nb-6Ta and Ti-22Nb-6Zr (at %) alloys. The physicochemical and technological properties of the Ti-22Nb-6Ta and Ti-22Nb-6Zr alloy powders synthesized by calcium hydride reduction under the optimum conditions are determined.

Synthesis and LPG sensing properties of nano-sized cadmium oxide.

PubMed

Waghulade, R B; Patil, P P; Pasricha, Renu

2007-04-30

This paper reports the synthesis and liquid petroleum gas (LPG) sensing properties of nano-sized cadmium oxide (CdO). The nano-sized CdO powder was successfully synthesized by using a chemical co-precipitation method using cadmium acetate and the ammonium hydroxide, as starting materials and water as a carrier. The resulting nano-sized powder was characterized by X-ray diffraction (XRD) measurements and the transmission electron microscopy (TEM). The LPG sensing properties of the synthesized nano-sized CdO were investigated at different operating temperatures and LPG concentrations. It was found that the calcination temperature and the operating temperature significantly affect the sensitivity of the nano-sized CdO powder to the LPG. The sensitivity is found to be maximum when the calcination temperature was 400 degrees C. The sensitivity to 75ppm of LPG is maximum at an operating temperature 450 degrees C and it was found to be approximately 341%. The response and recovery times were found to be nearly 3-5s and 8-10s, respectively. The synthesized nano-sized CdO powder is able to detect up to 25ppm for LPG with reasonable sensitivity at an operating temperature 450 degrees C and it can be reliably used to monitor the concentration of LPG over the range (25-75ppm). The experimental results of the LPG sensing studies reveal that the nano-sized CdO powder synthesized by a simple co-precipitation method is a suitable material for the fabrication of the LPG sensor.

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.

The result of synthesis analysis of the powder TiO{sub 2}/ZnO as a layer of electrodes for dye sensitized solar cell applications

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

Retnaningsih, Lilis, E-mail: lilisretna@gmail.com; Muliani, Lia

2016-04-19

This study has been conducted synthesis of TiO{sub 2} nanoparticle powders and ZnO nanoparticle powder into a paste to be in this research, dye-sensitive solar cells (DSSC) was produced by TiO{sub 2} nanopowder and ZnO nanopowder synthesis to make paste that is applied as electrode. This electrode works based on photon absorbed by dye and transferred to different composition of TiO{sub 2}/ ZnO particle. Properties of DSSC are affected by fabrication method, parameter and dimension of TiO{sub 2} / ZnO nanoparticles, technique and composition of TiO{sub 2} / ZnO paste preparation is important to get the higher performance of DSSC.more » Doctor blade is a method for electrode coating on glass substrate. The electrode was immersed into dye solution of Z907 and ethanol. From the experiment, the effect of TiO{sub 2} and ZnO nanopowder mixture for electrode was investigated. XRD characterization show anatase and rutile phase, which sintered TiO{sub 2}/ZnO has intensity more than 11,000. SEM characterization shows the composition of 20% TiO{sub 2} / 80% ZnO has better porosity. Higher efficiency that is investigated by I-V measurement using Sun Simulator.« less

Synthesis of attrition-resistant heterogeneous catalysts using templated mesoporous silica

DOEpatents

Pham, Hien N.; Datye, Abhaya K.

2003-04-15

The present invention relates to catalysts in mesoporous structures. In a preferred embodiment, the invention comprises a method for encapsulating a dispersed insoluble compound in a mesoporous structure comprising combining a soluble oxide precursor, a solvent, and a surfactant to form a mixture; dispersing an insoluble compound in the mixture; spray-drying the mixture to produce dry powder; and calcining the powder to yield a porous structure comprising the dispersed insoluble compound.

Synthesis of Nano Sized Cr2AlC Powders by Molten Salt Method.

PubMed

Xiao, Dan; Zhu, Jianfeng; Wang, Fen; Tang, Yi

2015-09-01

Cr2AlC powders were successfully synthesized by molten salt method using Cr, Al and C as starting materials. The effects of the process parameters and amount of Al addition on the purity of the Cr2AlC powders were also investigated in details. The formation mechanism of Cr2AlC powders was investigated by XRD and DSC. The results indicated that intermediates of Cr7C3 and Cr- Al intermetallics, such as CrAl17, Cr2Al, Cr2Al8, were formed by the reactions among the initial elements, then the intermediates gradually transformed to Cr2AlC. From the fixed composition of Cr:Al:C = 2:1.2:1, high purity Cr2AlC powders could be obtained with an inorganic salt KCl as a solvent at 1250 degrees C for 60 min under argon atmosphere which was lower than that (generally 1450 degrees C) of conventional solid state reaction.

Synthesis of Black and Red Mercury Sulfide Nano-Powder by Traditional Indian Method for Biomedical Application

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

Padhi, Payodhar; Sahoo, G.; Das, K.

The use of metals and minerals in the traditional Indian system of medicine known as aired is very common and is practiced since seventh century B.C. Metals were reduced to calcined powder form for medicinal purpose. For detoxification, a further step of purification of the metals and minerals with different vegetable extracts was practiced. The people of East India were using mercury and its sulfide as medicine. Gradually this secret was leaked to Arabic physicians who used mercury in skin ointment. Subsequently Italian Physicians adopted Arabic prescriptions of mercurial ointments for skin diseases. In the olden days, metals and mineralsmore » were impregnated with decoction and juice of vegetables and animal products like milk and fat for purification. These were then reduced to fine particles by milling with a pestle and mortar. It was known by then that the fineness of the powder had a significant influence on the color, texture, and medicinal properties as is cited by Charak. Nagarjun studied in detail the processing of metals and minerals, particularly mercury and the influence of the processing parameters on the medicinal values. Mercury is unique in many aspects. Indian alchemy developed a wide variety a chemical processes for the ostensible transmutation of metals and preparation of elixir of life, in which mercury occupied a prime position .The present investigation attempts to use the traditional methods as prescribed in the ancient texts to prepare mercury sulfide in both red and black form for medicinal use. XRD, SEM and HRTEM investigations of the sulfides obtained shows that the ancient Indians were able to produce nano-sized powders. Possibly this may be taken as the earliest application of the production and use of nano powder. The study proves that even in ancient time the knowledge of nano particle synthesis was prevalent and used to enhance effectiveness of medicines. Further mercury in the free form is not acceptable in medicines. The ancient physicians could get rid of free mercury by milling and proper choice of the ratio of ingredients as is shown in the investigation by X-ray diffraction studies. In the traditional method for synthesis of mercury sulfide, mercury and pure sulfur were taken and milled in a mortar and pastel. During milling process, the white mercury and yellow sulfur yielded to a gray black colored sulfide. Synthesis of red sulfide of mercury required additional steps of heating and subsequent milling. For therapeutically application, the sulfide thus obtained needed detoxification, which was done using organic extracts. In the present investigation, the same method was followed to synthesize the sapphires and the product was characterized using modern methods like XRD, SEM and HRTEM. With increase in milling time the fineness of the powder increases, which increases the efficacy of the medicine, and free mercury, which is not desirable for medicinal application is found to decrease. The powder obtained at the end of 48 hours of milling is found to be of a size finer than l0nm.« less

Synthesis of Black and Red Mercury Sulfide Nano-Powder by Traditional Indian Method for Biomedical Application

NASA Astrophysics Data System (ADS)

Padhi, Payodhar; Sahoo, G.; Das, K.; Ghosh, Sudipto; Panigrahi, S. C.

2008-10-01

The use of metals and minerals in the traditional Indian system of medicine known as aired is very common and is practiced since seventh century B.C. Metals were reduced to calcined powder form for medicinal purpose. For detoxification, a further step of purification of the metals and minerals with different vegetable extracts was practiced. The people of East India were using mercury and its sulfide as medicine. Gradually this secret was leaked to Arabic physicians who used mercury in skin ointment. Subsequently Italian Physicians adopted Arabic prescriptions of mercurial ointments for skin diseases. In the olden days, metals and minerals were impregnated with decoction and juice of vegetables and animal products like milk and fat for purification. These were then reduced to fine particles by milling with a pestle and mortar. It was known by then that the fineness of the powder had a significant influence on the color, texture, and medicinal properties as is cited by Charak. Nagarjun studied in detail the processing of metals and minerals, particularly mercury and the influence of the processing parameters on the medicinal values. Mercury is unique in many aspects. Indian alchemy developed a wide variety a chemical processes for the ostensible transmutation of metals and preparation of elixir of life, in which mercury occupied a prime position .The present investigation attempts to use the traditional methods as prescribed in the ancient texts to prepare mercury sulfide in both red and black form for medicinal use. XRD, SEM and HRTEM investigations of the sulfides obtained shows that the ancient Indians were able to produce nano-sized powders. Possibly this may be taken as the earliest application of the production and use of nano powder. The study proves that even in ancient time the knowledge of nano particle synthesis was prevalent and used to enhance effectiveness of medicines. Further mercury in the free form is not acceptable in medicines. The ancient physicians could get rid of free mercury by milling and proper choice of the ratio of ingredients as is shown in the investigation by X-ray diffraction studies. In the traditional method for synthesis of mercury sulfide, mercury and pure sulfur were taken and milled in a mortar and pastel. During milling process, the white mercury and yellow sulfur yielded to a gray black colored sulfide. Synthesis of red sulfide of mercury required additional steps of heating and subsequent milling. For therapeutically application, the sulfide thus obtained needed detoxification, which was done using organic extracts. In the present investigation, the same method was followed to synthesize the sapphires and the product was characterized using modern methods like XRD, SEM and HRTEM. With increase in milling time the fineness of the powder increases, which increases the efficacy of the medicine, and free mercury, which is not desirable for medicinal application is found to decrease. The powder obtained at the end of 48 hours of milling is found to be of a size finer than l0nm.

Ultrasound-assisted sol-gel synthesis of ZrO2.

PubMed

Guel, Marlene Lariza Andrade; Jiménez, Lourdes Díaz; Hernández, Dora Alicia Cortés

2017-03-01

Synthesis of tetragonal ZrO 2 by both conventional sol-gel and ultrasound-assisted sol-gel methods and using a non-ionic surfactant Tween-20, was performed. A porous microstructure composed of nanometric particles was observed. Tetragonal ZrO 2 was obtained using a low heat treatment temperature of powders, 500°C by both methods. A higher crystallinity and a shorter reaction time were observed when ultrasound was used in the sol-gel method due to the cavitation phenomenon. Copyright © 2016 Elsevier B.V. All rights reserved.

Effects of synthesis techniques on chemical composition, microstructure and dielectric properties of Mg-doped calcium titanate

NASA Astrophysics Data System (ADS)

Jongprateep, Oratai; Sato, Nicha

2018-04-01

Calcium titanate (CaTiO3) has been recognized as a material for fabrication of dielectric components, owing to its moderate dielectric constant and excellent microwave response. Enhancement of dielectric properties of the material can be achieved through doping, compositional and microstructural control. This study, therefore, aimed at investigating effects of powder synthesis techniques on compositions, microstructure, and dielectric properties of Mg-doped CaTiO3. Solution combustion and solid-state reaction were powder synthesis techniques employed in preparation of undoped CaTiO3 and CaTiO3 doped with 5-20 at% Mg. Compositional analysis revealed that powder synthesis techniques did not exhibit a significant effect on formation of secondary phases. When Mg concentration did not exceed 5 at%, the powders prepared by both techniques contained only a single phase. An increase of MgO secondary phase was observed as Mg concentrations increased from 10 to 20 at%. Experimental results, on the contrary, revealed that powder synthesis techniques contributed to significant differences in microstructure. Solution combustion technique produced powders with finer particle sizes, which consequently led to finer grain sizes and density enhancement. High-density specimens with fine microstructure generally exhibit improved dielectric properties. Dielectric measurements revealed that dielectric constants of all samples ranged between 231 and 327 at 1 MHz, and that superior dielectric constants were observed in samples prepared by the solution combustion technique.

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

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

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

2016-02-08

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

Reverse micelle synthesis of oxide nanopowders: mechanisms of precipitate formation and agglomeration effects.

PubMed

Graeve, Olivia A; Fathi, Hoorshad; Kelly, James P; Saterlie, Michael S; Sinha, Kaustav; Rojas-George, Gabriel; Kanakala, Raghunath; Brown, David R; Lopez, Enrique A

2013-10-01

We present an analysis of reverse micelle stability in four model systems. The first two systems, composed of unstable microemulsions of isooctane, water, and Na-AOT with additions of either iron sulfate or yttrium nitrate, were used for the synthesis of iron oxide or yttrium oxide powders. These oxide powders were of nanocrystalline character, but with some level of agglomeration that was dependent on calcination temperature and cleaning procedures. Results show that even though the reverse micellar solutions were unstable, nanocrystalline powders with very low levels of agglomeration could be obtained. This effect can be attributed to the protective action of the surfactant on the surfaces of the powders that prevents neck formation until after all the surfactant has volatilized. A striking feature of the IR spectra collected on the iron oxide powders is the absence of peaks in the ~1715 cm(-1) to 1750 cm(-1) region, where absorption due to the symmetric C=O (carbonyl) stretching occurs. The lack of such peaks strongly suggests the carbonyl group is no longer free, but is actively participating in the surfactant-precipitate interaction. The final two microemulsion systems, containing CTAB as the surfactant, showed that loss of control of the reverse micelle synthesis process can easily occur when the amount of salt in the water domains exceeds a critical concentration. Both model systems eventually resulted in agglomerated powders of broad size distributions or particles that were large compared to the sizes of the reverse micelles, consistent with the notion that the microemulsions were not stable and the powders were precipitated in an uncontrolled fashion. This has implications for the synthesis of nanopowders by reverse micelle synthesis and provides a benchmark for process control if powders of the highest quality are desired. Copyright © 2013 Elsevier Inc. All rights reserved.

Electrochemical synthesis of gold nanoparticles on the surface of multi-walled carbon nanotubes with glassy carbon electrode and their application

NASA Astrophysics Data System (ADS)

Song, Y. Z.; Li, X.; Song, Y.; Cheng, Z. P.; Zhong, H.; Xu, J. M.; Lu, J. S.; Wei, C. G.; Zhu, A. F.; Wu, F. Y.; Xu, J.

2013-01-01

Gold nanoparticles on the surface of multi-walled carbon nanotubes with glassy carbon electrode were prepared using electrochemical synthesis method. The thin films of gold Nanoparticles/multi-walled carbon nanotubes were characterized by scanning electron microscopy, powder X-ray diffraction, and cyclic voltammetry. Electrochemical behavior of adrenaline hydrochloride at gold nanoparticles/multi-walled carbon nanotube modified glassy carbon electrode was investigated. A simple, sensitive, and inexpensive method for determination of adrenaline hydrochloride was proposed.

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

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

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

2009-12-15

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

EXAFS Study on LiFePO4 Powders Produced From Two Sol-Gel Routes

NASA Astrophysics Data System (ADS)

Negara, V. S. I.; Latif, C.; Wongtepa, W.; Pratapa, S.

2018-04-01

The local structure of LiFePO4 powders has been investigated using Fe K-edge Extended X-Ray Absorption Fine Structure (EXAFS) Spectroscopy data. The synthesis of LFP powders was carried out using two different sol-gel methods. The raw materials for Fe source were ironstone and commercial precursor of FeCl2·4H2O. Synthesis using natural materials produced two phases, namely LiFePO4 olivine and Li3Fe2(PO4)3 nasicon, whereas that using a commercial product produced a single phase of LiFePO4 olivine. The EXAFS data for both samples were collected at Synchrotron Light Research Institute (SLRI), Thailand. Fitting of the model on the experimental curve provided parameters that can be interpreted as the distance between Fe as the absorber and the nearest atoms on the LFP materials. The EXAFS data analysis has shown that synthesis of LFPs using different Fe sources gives slightly different nearest-neighbor distances, namely Fe-O of 0.21% -0.23%, Fe-P of 0.14% - 0.16%, Fe-Fe of 0.12% for both samples, respectively.

Effect of ammonium carbonate to metal ions molar ratio on synthesis and sintering of Nd:YAG nanopowders

NASA Astrophysics Data System (ADS)

Liu, Qiang; Chen, Cong; Dai, Jiawei; Hu, Zewang; Chen, Haohong; Li, Jiang

2018-06-01

Using the nanopowders synthesized by a reverse co-precipitation method, neodymium doped yttrium aluminum garnet (Nd:YAG) transparent ceramics were fabricated by vacuum sintering method. The influence of ammonium carbonate to metal ions (NH4HCO3/M3+) molar ratio (R value) on the properties of Nd:YAG precursors and powders, as well as the densification, microstructure, and transmittance of the resultant ceramics was systematically investigated. The results show that the precursors have similar compositions and the calcined powders have pure Y3Al5O12 (YAG) phase. However, the R value is closely related to the morphologies of the precursors and powders. It is found that the powder with R = 3.0 has strongest agglomeration and the powders with R = 3.2-4.0 show better dispersity. Using these powders as starting materials, the corresponding ceramics were sintered at 1720 °C for 20 h in vacuum. As a result, the ceramic with R = 3.2 obtains the best transmittance of about 72% at the wavelength of 1064 nm. The grain growth exponent and activation energy of the Nd:YAG ceramics fabricated from the powder with R = 3.2 were also studied.

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.

Sol-gel synthesis and characterisation of nano-scale hydroxyapatite

NASA Astrophysics Data System (ADS)

Bilton, M.; Brown, A. P.; Milne, S. J.

2010-07-01

Hydroxyapatite (HAp) forms the main mineral component of bone and teeth. This naturally occurring HAp is in the form of nano-metre sized crystallites of Ca10(PO4)6(OH)2 that contain a number of cation and anion impurities, for example CO32-, F-, Na+, Mg2+ and Sr2+. Synthetic nano-sized HAp particles exhibit favourable biocompatibility and bioactivity and in order to better match the composition to natural HAp there is great interest in producing a range of chemically modified powders. In this study, two HAp powders have been synthesised via a water-based low-temperature sol-gel method and a third, commercial powder from Sigma-Aldrich have been analysed. Subsequent powder calcination has been carried out within the temperature range of 500-700 °C and the products characterised by bulk chemical analysis, X-ray diffraction and electron microscopy. Energy dispersive X-ray spectroscopy (EDX) in the TEM has been used to assess the composition of individual HAp particles. In order to do this accurately it is first necessary to account for the sensitivity of the HAp structure and composition to irradiation by the high energy electron beam of the TEM. This was done by monitoring the estimated Ca/P ratio derived from TEM-EDX of stoichiometric HAp under increasing levels of electron fluence. A fluence threshold (at a given beam energy) was established below which the measured Ca/P ratio can be considered to be stable. Subsequent elemental analysis at or below this threshold has enabled the variation in composition between particles both within and between synthesis batches to be accurately assessed. Compositional variability between particles is also evident, even in the commercial powder, but is far greater in the powders prepared by the sol-gel method.

Synthesis of functional materials in combustion reactions

NASA Astrophysics Data System (ADS)

Zhuravlev, V. D.; Bamburov, V. G.; Ermakova, L. V.; Lobachevskaya, N. I.

2015-12-01

The conditions for obtaining oxide compounds in combustion reactions of nitrates of metals with organic chelating-reducing agents such as amino acids, urea, and polyvinyl alcohol are reviewed. Changing the nature of internal fuels and the reducing agent-to-oxidizing agent ratio makes possible to modify the thermal regime of the process, fractal dimensionality, morphology, and dispersion of synthesized functional materials. This method can be used to synthesize simple and complex oxides, composites, and metal powders, as well as ceramics and coatings. The possibilities of synthesis in combustion reactions are illustrated by examples of αand γ-Al2O3, YSZ composites, uranium oxides, nickel powder, NiO and NiO: YSZ composite, TiO2, and manganites, cobaltites, and aluminates of rare earth elements.

The Effect of Time, Temperature and Composition on Boron Carbide Synthesis by Sol-gel Method

NASA Astrophysics Data System (ADS)

Hadian, A. M.; Bigdeloo, J. A.

2008-02-01

To minimize free carbon residue in the boron carbide (B4C) powder, a modified sol-gel process is performed where the starting materials as boric acid and citric acid compositions are adjusted. Because of boron loss in the form of B2O2(g) during the reduction reaction of the stoichiometric starting composition, the final B4C powders contain carbon residues. Thus, an excess H3BO3 is used in the reaction to compensate the loss and to obtain stoichiometric powders. Parameters of production have been determined using x-ray diffraction analysis and particle size analyses. The synthesized B4C powder using an excess boric acid composition shows no trace of carbon.

Synthesis of ITO Powder by Dry Process and Lifetime Characteristics of the ITO Target Fabricated with its Powder

NASA Astrophysics Data System (ADS)

Takahashi, Seiichiro; Itoh, Hironori; Komatsu, Ryuichi

Lifetime of an indium tin oxide (ITO) target is an important characteristic in the production of liquid crystal displays (LCDs). Increasing the sintering density of the ITO target is assumed to lead to an increased lifetime. So far, it has been clarified that the carbon concentration in In2O3 powder, the raw material of ITO targets, influences remarkably the target lifetime. In this study, with the aim of reducing the concentration of carbon in In2O3 powder, the synthesis of In2O3 powder containing dissolved Sn by a dry process was performed.

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

Zhao, Yajing; Chen, Yan; Chen, Kepi

In this study, the effects of doping with GeO 2 on the synthesis temperature, phase structure and morphology of (K 0.5Na 0.5)NbO 3 (KNN) ceramic powders were studied using XRD and SEM. The results show that KNN powders with good crystallinity and compositional homogeneity can be obtained after calcination at up to 900°C for 2 h. Introducing 0.5 mol.% GeO 2 into the starting mixture improved the synthesis of the KNN powders and allowed the calcination temperature to be decreased to 800°C, which can be ascribed to the formation of the liquid phase during the synthesis.

Hydrothermal synthesis of nanostructured Y2O3 and (Y0.75Gd0.25)2O3 based phosphors

NASA Astrophysics Data System (ADS)

Mančić, Lidija; Lojpur, Vesna; Marinković, Bojan A.; Dramićanin, Miroslav D.; Milošević, Olivera

2013-08-01

Examples of (Y2O3-Gd2O3):Eu3+ and Y2O3:(Yb3+/Er3+) rare earth oxide-based phosphors are presented to highlight the controlled synthesis of 1D and 2D nanostructures through simple hydrothermal method. Conversion of the starting nitrates mixture into carbonate hydrate phase is performed with the help of ammonium hydrogen carbonate solution during hydrothermal treatment at 200 °C/3 h. Morphological architectures of rare earth oxides obtained after subsequent powders thermal treatment at 600 and 1100 °C for 3 and 12 h and their correlation with the optical characteristics are discussed based on X-ray powder diffractometry, field emission scanning electron microscopy, infrared spectroscopy and photoluminescence measurements. Strong red and green emission followed by the superior decay times are attributed to the high powders purity and homogeneous dopants distribution over the host lattice matrix.

Sol-gel synthesis and characterizations of crystalline NaGd(WO4)2 powder for anisotropic transparent ceramic laser application

NASA Astrophysics Data System (ADS)

Durairajan, A.; Thangaraju, D.; Balaji, D.; Moorthy Babu, S.

2013-02-01

NaGd(WO4)2 powders were synthesized at different pH (3.5, 4.5, 5.5, 6.5 and 7.5) values by conventional Pechini method. Sodium and gadolinium nitrate salts and ammonium paratungstate are used as starting precursors. Metal cations were chelated by citric acid and individual citrates were bound together with ethylene glycol. Synthesized gel was analyzed using differential thermal analysis (DTA), thermo gravimetric (TG) and FT-IR spectroscopy to understand the degradation of gel and formation of metal citrates. Calcined powders (250, 600, 700 and 800 °C) were characterized by powder XRD, FT-IR, Raman and FE-SEM analysis. The temperature dependent phase formation was examined by powder XRD. The morphological changes at different pH derived powders were observed with FE-SEM micrographs. Stepwise organic liberation with respect to temperature and presence of carbon content in the pre-fired powder were analyzed using FT-IR analysis. Raman spectrum reveals disordered tungstate vibrations in the NGW matrix.

Method for producing titanium aluminide weld rod

DOEpatents

Hansen, Jeffrey S.; Turner, Paul C.; Argetsinger, Edward R.

1995-01-01

A process for producing titanium aluminide weld rod comprising: attaching one end of a metal tube to a vacuum line; placing a means between said vacuum line and a junction of the metal tube to prevent powder from entering the vacuum line; inducing a vacuum within the tube; placing a mixture of titanium and aluminum powder in the tube and employing means to impact the powder in the tube to a filled tube; heating the tube in the vacuum at a temperature sufficient to initiate a high-temperature synthesis (SHS) reaction between the titanium and aluminum; and lowering the temperature to ambient temperature to obtain a intermetallic titanium aluminide alloy weld rod.

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.

Synthesis and structural properties of (Y, Sr)(Ti, Fe, Nb)O3-δ perovskite nanoparticles fabricated by modified polymer precursor method

NASA Astrophysics Data System (ADS)

Miruszewski, T.; Gdaniec, P.; Karczewski, J.; Bochentyn, B.; Szaniawska, K.; Kupracz, P.; Prześniak-Welenc, M.; Kusz, B.

2016-09-01

The yttrium, iron and niobium doped-SrTiO3 powders have been successfully fabricated by a modified low-temperature synthesis method from a polymer complex. The usage of strontium hydroxide precursor instead of conventional strontium nitrate or strontium carbonate provides to the possibility of significant decrease of annealing temperature. It allows to prepare a material with sphere-shape grains of nanometric size (15-70 nm). The results of thermal analysis indicate that the crystallization of precursor takes place at different stages. The product after heat treatment at 600 °C for 3 h in air was also characterized by X-Ray diffraction method (XRD) and Fourier transform - infrared spectroscopy (FT-IR). After the crystallization and the impurity removal process, a single-phase material was obtained in case of all analyzed samples. The morphology of obtained nano-powders was also studied by a scanning electron microscopy (SEM). It can be concluded, that this method allows obtaining a perovskite phase of a metal doped SrTiO3 with nanometric particles.

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.

Gas-Phase Combustion Synthesis of Aluminum Nitride Powder

NASA Technical Reports Server (NTRS)

Axelbaum, R. L.; Lottes, C. R.; Huertas, J. I.; Rosen, L. J.

1996-01-01

Due to its combined properties of high electrical resistivity and high thermal conductivity aluminum nitride (AlN) is a highly desirable material for electronics applications. Methods are being sought for synthesis of unagglomerated, nanometer-sized powders of this material, prepared in such a way that they can be consolidated into solid compacts having minimal oxygen content. A procedure for synthesizing these powders through gas-phase combustion is described. This novel approach involves reacting AlCl3, NH3, and Na vapors. Equilibrium thermodynamic calculations show that 100% yields can be obtained for these reactants with the products being AlN, NaCl, and H2. The NaCl by-product is used to coat the AlN particles in situ. The coating allows for control of AlN agglomeration and protects the powders from hydrolysis during post-flame handling. On the basis of thermodynamic and kinetic considerations, two different approaches were employed to produce the powder, in co-flow diffusion flame configurations. In the first approach, the three reactants were supplied in separate streams. In the second, the AlCl3 and NH3 were premixed with HCl and then reacted with Na vapor. X-ray diffraction (XRD) spectra of as-produced powders show only NaCl for the first case and NaCl and AlN for the second. After annealing at 775 C tinder dynamic vacuum, the salt was removed and XRD spectra of powders from both approaches show only AlN. Aluminum metal was also produced in the co-flow flame by reacting AlCl3 with Na. XRD spectra of as-produced powders show the products to be only NaCl and elemental aluminum.

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.

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.

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.

A new method of nanocrystalline nickel powder formation by magnetron sputtering on the water-soluble substrates

NASA Astrophysics Data System (ADS)

Tučkutė, S.; Urbonavičius, M.; Lelis, M.; Maiorov, M.; Díaz Ordaz, J. R.; Milčius, D.

2018-01-01

Due to the accurate and relatively easy control magnetron sputtering is an attractive technique for the synthesis of metallic particles. This work describes a new method of nickel powder production by depositing nickel on the surface of sodium chloride particles which were used as the template and are soluble in water. Ni powder with flake-like structure was obtained after washing Ni coated salt particles in ultrasonic cleaner. Salt particles and nickel powder were characterized using scanning electron microscope (SEM), energy-dispersive x-ray spectrometer, XRD and X-ray photoelectron spectroscopy (XPS) techniques. SEM images showed that thickness of the received Ni particles varied in the nanoscale and depended on the magnetron deposition time but did not depend on the size of salt particles. On the other hand initial size of the salt particles was successfully employed a measure to control lateral dimensions of Ni powder. XRD and XPS analysis results revealed that Ni particles had metallic core and oxidized shell which was a cause of the slightly deteriorated magnetic properties.

Catalytic and antibacterial properties of silver nanoparticles green biosynthesized using soluble green tea powder

NASA Astrophysics Data System (ADS)

Xu, Wei; Fan, Yapei; Liu, Xinfang; Luo, Denglin; Liu, Huan; Yang, Ningning

2018-04-01

Silver nanoparticles (Ag NPs) were green fabricated using soluble green tea powder (SGTP) as stabilizer and reducing agent. The properties and morphology of Ag NPs were investigated through UV–visible spectroscopy, field emission transmission electron microscope (FE-TEM) and fourier transform infrared (FT-IR). The spectroscopy showed surface plasmon resonance around at 420 nm revealing the synthesis of Ag NPs. FE-TEM results confirmed that the Ag NPs are spherical and face-centered cubic structure. FT-IR spectroscopy identified the role of various functional groups in the nanoparticle synthesis. The one spot biosynthesized Ag NPs showed favourable antibacterial properties on Escherichia coli and Staphyloccocus aureus, and excellent catalytic reduction of 4-nitrophenol. This work provided a feasible, green method to fabricate Ag NPs with promising photocatalytic and antimicrobial activities.

Synthesis of functional materials in combustion reactions

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

Zhuravlev, V. D., E-mail: zhvd@ihim.uran.ru; Bamburov, V. G.; Ermakova, L. V.

2015-12-15

The conditions for obtaining oxide compounds in combustion reactions of nitrates of metals with organic chelating–reducing agents such as amino acids, urea, and polyvinyl alcohol are reviewed. Changing the nature of internal fuels and the reducing agent-to-oxidizing agent ratio makes possible to modify the thermal regime of the process, fractal dimensionality, morphology, and dispersion of synthesized functional materials. This method can be used to synthesize simple and complex oxides, composites, and metal powders, as well as ceramics and coatings. The possibilities of synthesis in combustion reactions are illustrated by examples of αand γ-Al{sub 2}O{sub 3}, YSZ composites, uranium oxides, nickelmore » powder, NiO and NiO: YSZ composite, TiO{sub 2}, and manganites, cobaltites, and aluminates of rare earth elements.« less

Molten salt synthesis of La0.8Sr0.2MnO3 powders for SOFC cathode electrode

NASA Astrophysics Data System (ADS)

Gu, Sin-il; Shin, Hyo-soon; Hong, Youn-woo; Yeo, Dong-hun; Kim, Jong-hee; Nahm, Sahn; Yoon, Sang-ok

2012-08-01

For La0.8Sr0.2MnO3 (LSM) perovskite, used as the cathode material for solid oxide fuel cells (SOFC), it is known that the formation of a triple-phase-boundary is restrained due to the formation of a second phase at the YSZ/electrode interface at high temperature. To decrease the 2nd phase, lowering the sintering temperature has been used. LSM powder was synthesized by molten salt synthesis method to control its particle size, shape, and agglomeration. We have characterized the phase formation, particle size, shape, and sintering behavior of LSM in the synthesis using the variation of KCl, LiCl, KF and its mixed salts as raw materials. In the case of KCl and KCl-KF salts, the particle size and shape of the LSM was well controlled and synthesized. However, in the case of LiCl and KCl-LiCl salts, LiMnOx as 2nd phase and LSM were synthesized simultaneously. In the case of the mixed salt of KCl-KF, the growth mechanism of the LSM particle was changed from `diffusion-controlled' to `reaction-controlled' according to the amount of mixed salt. The sintering temperature can be decreased below 1000 °C by using the synthesized LSM powder.

Photosensitized synthesis of silver nanoparticles using Withania somnifera leaf powder and silver nitrate.

PubMed

Raut, Rajesh Warluji; Mendhulkar, Vijay Damodhar; Kashid, Sahebrao Balaso

2014-03-05

The metal nanoparticle synthesis is highly explored field of nanotechnology. The biological methods seem to be more effective; however, due to slow reduction rate and polydispersity of the resulting products, they are less preferred. In the present study, we report rapid and facile synthesis of silver nanoparticles at room temperature. The exposure of reaction mixtures containing silver nitrate and dried leaf powder of Withania somnifera Linn to direct sunlight resulted in reduction of metal ions within five minutes whereas, the dark exposure took almost 12h. Further studies using different light filters reveal the role of blue light in reduction of silver ions. The synthesized silver nanoparticles were characterized by UV-Vis, Infrared spectroscopy (IR), Transmission Electron Microscopy (TEM), X-ray Diffraction studies (XRD), Nanoparticle Tracking Analysis (NTA), Energy Dispersive Spectroscopy (EDS), and Cyclic Voltammetry (CV). The Antibacterial and antifungal studies showed significant activity as compared to their respective standards. Copyright © 2014 Elsevier B.V. All rights reserved.

Synthesis of nanocrystalline TiO 2 in toluene by a solvothermal route

NASA Astrophysics Data System (ADS)

Kim, Chung-Sik; Moon, Byung Kee; Park, Jong-Ho; Tae Chung, Su; Son, Se-Mo

2003-07-01

A solvothermal synthetic method to TiO 2 nanoparticles has been investigated in toluene solutions with titanium isopropoxide (TIP) as precursor. Weight ratios of precursor to solvent prepared in the mixture are 5/100, 10/100, 20/100, 30/100 and 40/100. At the weight ratio of 10/100, 20/100 and 30/100, TiO 2 nanocrystalline particles were obtained after synthesis at 250°C for 3 h in an autoclave. X-ray diffraction and tranmission electron microscopy shows that the product has uniform anatase structure with average particle size below 20 nm. As the composition of TIP in the solution increases, the particle size of TiO 2 powder tends to increase. At 5/100 and 40/100, however, pale yellow colloidal solution is obtained after synthesis and crystalline phase of TiO 2 is not produced. The specific surface area of the TiO 2 nanocrystalline powder was also investigated using BET surface area analyzer.

Comparison of the surface charge behavior of commercial silicon nitride and silicon carbide powders

NASA Technical Reports Server (NTRS)

Whitman, Pamela K.; Feke, Donald L.

1988-01-01

The adsorption and desorption of protons from aqueous solution onto the surfaces of a variety of commercial silicon carbide and silicon nitride powders has been examined using a surface titration methodology. This method provides information on some colloidal characteristics, such as the point of zero charge (pzc) and the variation of proton adsorption with dispersion pH, useful for the prediction of optimal ceramic-processing conditions. Qualitatively, the magnitude of the proton adsorption from solution reveals small differences among all of the materials studied. However, the results show that the pzc for the various silicon nitride powders is affected by the powder synthesis route. Complementary investigations have shown that milling can also act to shift the pzc exhibited by silicon nitride powder. Also, studies of the role of the electrolyte in the development of surface charge have indicated no evidence of specific adsorption of ammonium ion on either silicon nitride or silicon carbide powders.

Rapid synthesis of barium titanate microcubes using composite-hydroxides-mediated avenue

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

He, Xi; Ouyang, Jing, E-mail: jingouyang@csu.edu.cn; Jin, Jiao

2014-04-01

Highlights: • Barium titanate oxides microcubes can be synthesized within 1 min. • Composite-hydroxides-mediated strategy provided a possible large scale production. • BST obtained in the strategy showed fairly good crystallinity and tetragonality. - Abstract: This paper reports the rapid synthesis of barium titanate (BaTiO{sub 3}, BTO) microcubes via composite-hydroxides-mediated reaction within 1 min. X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersion spectrum (EDS) results confirmed both cubic and tetragonal lattices in the sample and the uniform microcubes with an average size of 1 μm. Ultraviolet–visible (UV–vis) spectrum indicated that the band gap of the BTO powder wasmore » 3.05 eV. Ferroelectric polarization vs. electric field (P–E) tests showed that the ferroelectric domains had formed in the as-synthesized BTO microcubes and sintered ceramics. BTO ceramics sintered at 1100 °C for 3 h showed fairly good tetragonality and possessed a maximum polarization of 0.21 μC/cm{sup 2}, indicating that the sintering temperature for the BTO powders prepared via this method was relatively low. The process and equipment reported herein provided a potential method for the rapid synthesis of titanate based perovskites.« less

Synthesis of CaCu3Ti4O12 by modified Sol-gel method with Hydrothermal process

NASA Astrophysics Data System (ADS)

Masingboon, C.; Rungruang, S.

2017-09-01

CaCu3Ti4O12 powders were synthesized by modified Sol-gel method with Hydrothermal process using Ca(NO3)2· 4H2O, Cu(NO3)2·3H2O, Ti(OC3H7)4 and freshly extracted egg white (ovalbumin) in aqueous medium. The precursor was calcined at 800, 900 and 1000 °C in air for 8 h to obtain nanocrystalline powders of CaCu3Ti4O12. The calcined CaCu3Ti4O12 powders were characterized by XRD, TEM and EDX. The XRD results indicated that all calcined samples have a typical perovskite CaCu3Ti4O12 structure and a small amount of CaTiO3, CuO and TiO2. TEM micrographs showed particle size 100 - 500 nm and EDX results showed elements of CaCu3Ti4O12 powders have calcium, copper, titanium and oxygen.

Bench-scale synthesis of nanoscale materials

NASA Technical Reports Server (NTRS)

Buehler, M. F.; Darab, J. G.; Matson, D. W.; Linehan, J. C.

1994-01-01

A novel flow-through hydrothermal method used to synthesize nanoscale powders is introduced by Pacific Northwest Laboratory. The process, Rapid Thermal Decomposition of precursors in Solution (RTDS), uniquely combines high-pressure and high-temperature conditions to rapidly form nanoscale particles. The RTDS process was initially demonstrated on a laboratory scale and was subsequently scaled up to accommodate production rates attractive to industry. The process is able to produce a wide variety of metal oxides and oxyhydroxides. The powders are characterized by scanning and transmission electron microscopic methods, surface-area measurements, and x-ray diffraction. Typical crystallite sizes are less than 20 nanometers, with BET surface areas ranging from 100 to 400 sq m/g. A description of the RTDS process is presented along with powder characterization results. In addition, data on the sintering of nanoscale ZrO2 produced by RTDS are included.

Method to synthesize bulk iron nitride

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

Monson, Todd; Lavernia, Enrique J.; Zheng, Baolong

Bulk iron nitride can be synthesized from iron nitride powder by spark plasma sintering. The iron nitride can be spark plasma sintered at a temperature of less than 600°C. and a pressure of less than 600 MPa, with 400 MPa or less most often being sufficient. High pressure SPS can consolidate dense iron nitrides at a lower temperature to avoid decomposition. The higher pressure and lower temperature of spark discharge sintering avoids decomposition and limits grain growth, enabling enhanced magnetic properties. The method can further comprise synthesis of nanocrystalline iron nitride powders using two-step reactive milling prior to high-pressure sparkmore » discharge sintering.« less

Hydrothermal synthesis and enhanced photocatalytic activity of mixed-phase TiO2 powders with controllable anatase/rutile ratio

NASA Astrophysics Data System (ADS)

Wang, Qi; Qiao, Zhi; Jiang, Peng; Kuang, Jianlei; Liu, Wenxiu; Cao, Wenbin

2018-03-01

In this study, mixed-phase TiO2 powders were novelly synthesized via a facile and mild hydrothermal method without any post-heat treatment. TiOSO4 and peroxide titanic acid (PTA) were used as inorganic titanium sources, while no special solvent or additive were introduced. The XRD and TEM results showed the mixed-phase TiO2 powders were composed of anatase and rutile phases, and the PTA sol played an important role on forming the rutile nucleus. The proportion of rutile in the mixed-phase TiO2 could be easily controlled in the range of 0%-70.5% by changing the amount of PTA sol used in the synthesis process. The UV-Visible absorption spectra indicated the prepared mixed-phase TiO2 showed enhanced visible light absorption with the increase of rutile ratio. The photodegradation experiments revealed the mixed-phase TiO2 exhibited the best photocatalytic activity at the rutile ratio of 41.5%, while a higher or lower rutile ratio both resulted in the decrease of photocatalytic activity.

Oxidation of Ca-α-SiAlON Powders Prepared by Combustion Synthesis

PubMed Central

Li, Jinfu; Li, Zhongmin; Wang, Enhui; Wang, Zhanjun; Yin, Xiaowei; Zhang, Zuotai

2015-01-01

The oxidation of Ca-α-SiAlON synthesized by the combustion synthesis (CS) method with different additives was investigated in air atmosphere using thermogravimetric (TG) analysis in a temperature range from 1453 K to 1653 K. The experimental results indicated that oxidation was controlled by mixed chemical and diffusion steps. The oxidation products by XRD analysis were composed of SiO2 and CaAl2Si2O8 at low oxidation temperature, whereas the SiO2-Al2O3-CaO ternary glassy phase was formed at elevated temperature. The deviation of oxidation resistance from each sample may be due to the morphological difference brought about by different additive additions. This study reveals the effects of additives on the oxidation resistance of synthesized Ca-α-SiAlON powders. PMID:28793657

Synthesis and characterization of nano-hydroxyapatite using Sapindus Mukorossi extract

NASA Astrophysics Data System (ADS)

Subha, B.; Prasath, P. Varun; Abinaya, R.; Kavitha, R. J.; Ravichandran, K.

2015-06-01

Nano-Hydroxyapatite (HAP) powders were successfully synthesised by hydrothermal method using Sapindus Mukorossi extract as an additive. The structural and morphological analyses of thus synthesised powders were carried out using FT-IR, XRD and FESEM/EDX. The FT-IR spectra confirm the presence of phosphate and hydroxyl groups corresponding to HAP. The XRD analysis reveals the formation of HAP phase and found to reduce the crystallite size with addition of Sapindus Mukorossi extract. The morphology changes from sphere to flake shape by the influence of extract.

Mechanochemical synthesis of fluorescent carbon dots from cellulose powders

NASA Astrophysics Data System (ADS)

Chae, Ari; Ram Choi, Bo; Choi, Yujin; Jo, Seongho; Kang, Eun Bi; Lee, Hyukjin; Park, Sung Young; In, Insik

2018-04-01

A novel mechanochemical method was firstly developed to synthesize carbon nanodots (CNDs) or carbon nano-onions (CNOs) through high-pressure homogenization of cellulose powders as naturally abundant resource depending on the treatment times. While CNDs (less than 5 nm in size) showed spherical and amorphous morphology, CNOs (10-50 nm in size) presented polyhedral shape, and onion-like outer lattice structure, graphene-like interlattice spacing of 0.36 nm. CNOs showed blue emissions, moderate dispersibility in aqueous media, and high cell viability, which enables efficient fluorescence imaging of cellular media.

Recycling of surfactant template in mesoporous MCM-41 synthesis

NASA Astrophysics Data System (ADS)

Lai, J. Y.; Twaiq, F.; Ngu, L. H.

2017-06-01

The recycling of surfactant template is investigated through the reuse of the surfactant template in the mesoporous MCM-41 synthesis process. In the synthesis of MCM-41, tetraethylorthosilicate (TEOS) solution in water was utilized as the silica source while hexadecyltrimethylammonium bromide (CTAB) solution in ethyl alcohol was used as a surfactant template. The synthesized gel is formed thoroughly by mixing the two solutions under acid conditions with a pH value of 0.5 for 1 hour and kept for crystallization for 48 hours. The as-synthesized MCM-41 powder is recovered by filtration while the filtrate (mother liquor) was then reused for the second synthesis cycle. The synthesis procedure was repeated till no further solid product was formed. The synthesized gel was not produced in the unifying solution in the fifth cycle of MCM-41 synthesis. The quality of the calcined MCM-41 powder produced in each synthesis cycle was evaluated by calculating the amount of MCM-41 produced and the surface area of the powder product. The result showed that 1.28, 0.37, 1.64, 1.90 and 0.037 g were obtained in the 1st, 2nd, 3rd, 4th and 5th synthesis cycle, respectively. The surface area of the powder produced was found to be 1170, 916, 728, and 508 m2/g for 1st, 2nd, 3rd and 4th respectively. The concentration of the surfactant template has reached value lower than the critical micelle concentration (CMC) and remained constant after the 4th cycle. There was no further formation of gel due to low availability in the interaction between silicate anions and surfactant cations when the amount of TEOS was fixed for every synthesis cycle.

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

Drryl P. Butt; Brian Jaques

Research conducted for this NERI project has advanced the understanding and feasibility of nitride nuclear fuel processing. In order to perform this research, necessary laboratory infrastructure was developed; including basic facilities and experimental equipment. Notable accomplishments from this project include: the synthesis of uranium, dysprosium, and cerium nitrides using a novel, low-cost mechanical method at room temperature; the synthesis of phase pure UN, DyN, and CeN using thermal methods; and the sintering of UN and (Ux, Dy1-x)N (0.7 ≤ X ≤ 1) pellets from phase pure powder that was synthesized in the Advanced Materials Laboratory at Boise State University.

Aqueous Combustion Synthesis and Characterization of Nanosized Tetragonal Zirconia Single Crystals

NASA Astrophysics Data System (ADS)

Reddy, B. S. B.; Mal, Indrajit; Tewari, Shanideep; Das, Karabi; Das, Siddhartha

2007-08-01

Nanocrystalline zirconia powder has been synthesized by an aqueous combustion synthesis route using glycine as fuel and nitrate as oxidizer. The powders have been prepared by using different glycine to zirconyl nitrate molar ratios (G/N). The powders produced with different G/N ratios have been characterized by X-ray diffraction (XRD), Fourier transformed infrared spectroscopy (FTIR), transmission electron microscopy (TEM), and scanning electron microscopy (SEM) to determine the parameters resulting from powder with attractive properties. The theoretical combustion temperature (T ad ) has been calculated for different G/N ratios, and it is correlated with powder characteristics. An attempt is also made to explain the stability of tetragonal zirconia on the basis of extrinsic factors such as the morphology of nanocrystallites. Nanocrystalline metastable tetragonal zirconia (˜25 nm) powder (TZ) with disc-shaped morphology has been produced with a weak agglomeration in fuel deficient mixtures.

Thermal stability of hexagonal OsB2

NASA Astrophysics Data System (ADS)

Xie, Zhilin; Blair, Richard G.; Orlovskaya, Nina; Cullen, David A.; Andrew Payzant, E.

2014-11-01

The synthesis of novel hexagonal ReB2-type OsB2 ceramic powder was performed by high energy ball milling of elemental Os and B powders. Two different sources of B powder have been used for this mechanochemical synthesis. One B powder consisted of a mixture of amorphous and crystalline phases and a mixture of 10B and 11B isotopes with a fine particle size, while another B powder was a purely crystalline (rhombohedral) material consisting of enriched 11B isotope with coarse particle size. The same Os powder was used for the synthesis in both cases. It was established that, in the first case, the hexagonal OsB2 phase was the main product of synthesis with a small quantity of Os2B3 phase present after synthesis as an intermediate product. In the second case, where coarse crystalline 11B powder was used as a raw material, only Os2B3 boride was synthesized mechanochemically. The thermal stability of hexagonal OsB2 powder was studied by heating under argon up to 876 °C and cooling in vacuo down to -225 °C. During the heating, the sacrificial reaction 2OsB2+3O2→2Os+2B2O3 took place due to presence of O2/water vapor molecules in the heating chamber, resulting in the oxidation of B atoms and formation of B2O3 and precipitation of Os metal out of the OsB2 lattice. As a result of such phase changes during heating, the lattice parameters of hexagonal OsB2 changed significantly. The shrinkage of the a lattice parameter was recorded in 276-426 °C temperature range upon heating, which was attributed to the removal of B atoms from the OsB2 lattice due to oxidation followed by the precipitation of Os atoms and formation of Os metal. While significant structural changes occurred upon heating due to presence of O2, the hexagonal OsB2 ceramic demonstrated good phase stability upon cooling in vacuo with linear shrinkage of the lattice parameters and no phase changes detected during cooling.

Bulk synthesis of monodisperse magnetic FeNi3 nanopowders by flow levitation method.

PubMed

Chen, Shanjun; Chen, Yan; Kang, Xiaoli; Li, Song; Tian, Yonghong; Wu, Weidong; Tang, Yongjian

2013-10-01

In this work, a novel bulk synthesis method for monodisperse FeNi3 nanoparticles was developed by flow levitation method (FL). The Fe and Ni vapours ascending from the high temperature levitated droplet was condensed by cryogenic Ar gas under atmospheric pressure. X-ray diffraction was used to identify and characterize the crystal phase of prepared powders exhibiting a FeNi3 phase. The morphology and size of nanopowders were observed by transmission electron microscopy (TEM). The chemical composition of the nanoparticles was determined with energy dispersive spectrometer (EDS). The results indicated that the FeNi3 permalloy powders are nearly spherical-shaped with diameter about 50-200 nm. Measurement of the magnetic property of nanopowders by a superconducting quantum interference device (SQUID, Quantum Design MPMS-7) showed a symmetric hysteresis loop of ferromagnetic behavior with coercivity of 220 Oe and saturation magnetization of 107.17 emu/g, at 293 K. At 5 K, the obtained saturation magnetization of the sample was 102.16 emu/g. The production rate of FeNi3 nanoparticles was estimated to be about 6 g/h. This method has great potential in mass production of FeNi3 nannoparticles.

Direct synthesis of zirconium powder by magnesium reduction

NASA Astrophysics Data System (ADS)

Lee, Dong-Won; Yun, Jung-Yeul; Yoon, Sung-Won; Wang, Jei-Pil

2013-05-01

The direct synthesis of zirconium powder has been conducted through an analysis of the chemical reaction between evaporated ZrCl4 and molten magnesium over a range of reduction temperatures, concentration of hydrochloric acid, and stirring time. The observed results indicated that the purity of zirconium powder increased with increased stirring time, and Mg and MgCl2 were removed by 10 wt% of hydrochloric acid solution. The pure zirconium powder was obtained by stirring again for 5 h using 5 wt% of hydrochloric acid solution. It was noted that the mean particle size increased when the reaction temperature was increased, and the size of the powder at 1,123 K and 1,173 K was found to be 10 μm and 15 μm, respectively. In addition, the purity of the powder was also improved with temperature, and its purity finally reached up to 99.5% at 1,250 K. Overall, pure zirconium powder was obtained after a stirring stage for 5 hours using 5 wt% of hydrochloric acid solution.

Pressure-reaction synthesis of titanium composite materials

DOEpatents

Oden, Laurance L.; Ochs, Thomas L.; Turner, Paul C.

1993-01-01

A pressure-reaction synthesis process for producing increased stiffness and improved strength-to-weight ratio titanium metal matrix composite materials comprising exothermically reacting a titanium powder or titanium powder alloys with non-metal powders or gas selected from the group consisting of C, B, N, BN, B.sub.4 C, SiC and Si.sub.3 N.sub.4 at temperatures from about 900.degree. to about 1300.degree. C., for about 5 to about 30 minutes in a forming die under pressures of from about 1000 to 5000 psi.

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.

Shielding methods of quasilaminar jets outflowing from plasma torch with interelectrode insert

NASA Astrophysics Data System (ADS)

Solonenko, O. P.; Smirnov, A. V.

2017-05-01

Investigations of two methods of protection against mixing of surrounding air atmosphere with the free lengthy jets outflowing at low Reynolds numbers from plasma torches with interelectrode insertion (IEI) were carried out. The offered methods allow to significantly reduce the mixing of oxygen with plasma jets that gives a possibility of synthesis, treatment and spraying of powder materials, as well as melting of coatings critical to oxidation.

Synthesis of zinc ultrafine powders via the Guen–Miller flow-levitation method

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

Jigatch, A. N., E-mail: jan@chph.ras.ru; Leipunskii, I. O.; Kuskov, M. L.

2015-12-15

Zinc ultrafine powders (UFPs) with the average particle size of 0.175 to 1.24 μm are synthesized via the flow-levitation method. The peculiarities of the formation of zinc UFPs are considered with respect to the carrier gas properties (heat capacity, thermal conductivity, and diffusion coefficient), as well as the gas flow parameters (pressure and flow rate). The obtained zinc particles are studied via scanning electron microscopy and X-ray diffraction. The factors determining the crystal structure of zinc particles and their size distribution are discussed as well. The data on oxidation of zinc stored in unsealed containers under normal conditions are alsomore » presented.« less

Internal Nano Voids in Yttria-Stabilised Zirconia (YSZ) Powder

PubMed Central

Barad, Chen; Shekel, Gal; Shandalov, Michael; Hayun, Hagay; Kimmel, Giora; Shamir, Dror; Gelbstein, Yaniv

2017-01-01

Porous yttria-stabilised zirconia ceramics have been gaining popularity throughout the years in various fields, such as energy, environment, medicine, etc. Although yttria-stabilised zirconia is a well-studied material, voided yttria-stabilised zirconia powder particles have not been demonstrated yet, and might play an important role in future technology developments. A sol-gel synthesis accompanied by a freeze-drying process is currently being proposed as a method of obtaining sponge-like nano morphology of embedded faceted voids inside yttria-stabilised zirconia particles. The results rely on a freeze-drying stage as an effective and simple method for generating nano-voided yttria-stabilised zirconia particles without the use of template-assisted additives. PMID:29258227

Internal Nano Voids in Yttria-Stabilised Zirconia (YSZ) Powder.

PubMed

Barad, Chen; Shekel, Gal; Shandalov, Michael; Hayun, Hagay; Kimmel, Giora; Shamir, Dror; Gelbstein, Yaniv

2017-12-18

Porous yttria-stabilised zirconia ceramics have been gaining popularity throughout the years in various fields, such as energy, environment, medicine, etc. Although yttria-stabilised zirconia is a well-studied material, voided yttria-stabilised zirconia powder particles have not been demonstrated yet, and might play an important role in future technology developments. A sol-gel synthesis accompanied by a freeze-drying process is currently being proposed as a method of obtaining sponge-like nano morphology of embedded faceted voids inside yttria-stabilised zirconia particles. The results rely on a freeze-drying stage as an effective and simple method for generating nano-voided yttria-stabilised zirconia particles without the use of template-assisted additives.

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.

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.

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.

The Scaled-Up Synthesis of Nanostructured Ultra-High-Temperature Ceramics and Resistance Sintering of Tantalum Carbide Nanopowders and Composites

NASA Astrophysics Data System (ADS)

Kelly, James P.

Ultra-high temperature ceramics (UHTCs) are a unique class of materials with the potential to withstand harsh environments due to covalent bonding, which gives these materials high melting temperatures, although decomposition temperatures should also be considered. For example, the melting temperature of TaC is near 4000 K, but may vaporize at lower temperatures. The high melting temperatures also make them difficult to process without high pressures and temperatures and to achieve dense ceramics with a nanostructure. Such materials however are appealing for aerospace technologies. The ability to generate high density compacts and maintain a nanostructure could allow for unprecedented control and improvement to the mechanical properties. The goal of this work is to develop processes for the synthesis and consolidation of nanostructured UHTCs. A self-propagating solvothermal synthesis technique for making UHTC nanopowders is presented. The technique is fast, scalable, and requires minimal external energy input. Synthesis of transition metal boride, carbide, and nitride powders is demonstrated. TaC is synthesized using a range of synthesis conditions and characterized to determine the fundamental mechanisms controlling the nanopowder characteristics. Discussion on purification of the powders is also presented. The sintering of TaC nanopowders produced by the solvothermal synthesis method is performed by resistance sintering. The effects of temperature, heating rate, and dwell time on densification and grain growth is presented. Adequate powder processing, carbon content, volatilization, and additives are found to be critical factors affecting the densification, microstructure, and grain growth. The optimal range of carbon addition for minimizing oxygen content is determined. WC and ZrC are evaluated as additives for reducing grain growth of TaC. Secondary phases and/or solid solutions are capable of suppressing grain growth. A unified approach to solid solution chemistries to control the densification, microstructure, and properties of UHTCs in general is presented. This work has important consequences on advancing the properties of UHTCs.

SHS synthesis of Si-SiC composite powders using Mg and reactants from industrial waste

NASA Astrophysics Data System (ADS)

Chanadee, Tawat

2017-11-01

Si-SiC composite powders were synthesized by self-propagating high-temperature synthesis (SHS) using reactants of fly ash-based silica, sawdust-based activated carbon, and magnesium. Fly ash-based silica and sawdust-based activated carbon were prepared from coal mining fly ash and Para rubber-wood sawdust, respectively. The work investigated the effects of the synthesis atmosphere (air and Ar) on the phase and morphology of the SHS products. The SHS product was leached by a two-step acid leaching processes, to obtain the Si-SiC composite powder. The SHS product and SHS product after leaching were characterized by X-ray diffractometry, scanning electron microscopy and energy dispersive X-ray spectrometry. The results indicated that the SHS product synthesized in air consisted of Si, SiC, MgO, and intermediate phases (SiO2, Mg, Mg2SiO4, Mg2Si), whereas the SHS product synthesized in Ar consisted of Si, SiC, MgO and a little Mg2SiO4. The SiC content in the leached-SHS product was higher when Ar was used as the synthesis atmosphere. As well as affecting the purity, the synthesis atmospheres also affected the average crystalline sizes of the products. The crystalline size of the product synthesized in Ar was smaller than that of the product synthesized in air. All of the results showed that fly ash and sawdust could be effective waste-material reactants for the synthesis of Si-SiC composite powders.

Mechanisms of combustion synthesis and magnetic response of high-surface-area hexaboride compounds.

PubMed

Kanakala, Raghunath; Escudero, Roberto; Rojas-George, Gabriel; Ramisetty, Mohan; Graeve, Olivia A

2011-04-01

We present an analysis of the combustion synthesis mechanisms for the preparation of hexaboride materials using three compounds as model systems: EuB(6), YbB(6), and YB(6). These three hexaborides were chosen because of the differences in ionic radii between Eu(3+), Yb(3+), and Y(3+), which is a factor in their stability. The powders were prepared using metal nitrates, carbohydrazide, and two different boron precursor powders. The resulting materials were analyzed by X-ray diffraction, which showed that combustion synthesis is effective for the synthesis of EuB(6), since the Eu(3+) ion has an ionic radius greater than ∼1 Å. The synthesis of YbB(6) and YB(6) is not as effective because of the small size of the Yb(3+) and Y(3+) ions, making the hexaborides of these metals less stable and resulting in the synthesis of borates due to the presence of oxygen during the combustion process. Scanning electron microscopy and dynamic light scattering of the EuB(6) powders shows that the particle size of the hexaboride product is dependent on the particle size of the boron precursor. The magnetic susceptibility of our EuB(6) powders manifests irreversible behavior at low applied fields, which disappears at higher fields. This behavior can be attributed to the increase in size and number of magnetic polarons with increasing magnetic field. © 2011 American Chemical Society

The Microwave-Assisted Green Synthesis of TiC Powders.

PubMed

Wang, Hui; Zhu, Wencheng; Liu, Yanchun; Zeng, Lingke; Sun, Luyi

2016-11-08

Titanium carbide (TiC) is an important engineering material and has found widespread applications. Currently, TiC is typically synthesized through carbothermal reduction, requiring a high temperature (ca. 1700-2300 °C) and long reaction time (ca. 10-20 h), which is not eco-friendly. During a conventional reaction path, anatase TiO₂ (A-TiO₂) was first converted to rutile TiO₂ (R-TiO₂), which was subsequently reduced to TiC. Herein, we explored the synthesis of TiC powders with the assistance of microwave heating. In particular, we achieved the conversion of A-TiO₂, which was more reactive than R-TiO₂ for the carbothermal reduction, to TiC, which was directly due to quick microwave heating. As such, the carbothermal reduction started at a much lower temperature of ca. 1200 °C and finished within 30 min when reacting at 1400 °C, leading to significant energy saving. This study shows that microwave-assisted synthesis can be an effective and green process for preparing TiC powders, which is promising for future large-scale production. The influence of the reaction temperature, the reaction duration, and the carbon content on the synthesis of TiC powders was investigated.

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 thoria nano-particles at low temperature through base electrogeneration on steel 316L surface: Effect of current density

NASA Astrophysics Data System (ADS)

Yousefi, Taher; Torab-Mostaedi, Meisam; Mobtaker, Hossein Ghasemi; Keshtkar, Ali Reza

2016-10-01

The strategy developed in this study, offers significant advantages (simplicity and cleanness of method and also a product purity and new morphology of the product) over the conventional routes for the synthesis of ThO2 nanostructure. The effect of current density on morphology was studied. The synthesized powder was characterized by means of Powder X-ray Diffraction (PXRD), Transmission Electron Microscopy (TEM, Phillips EM 2085) Brunauer-Emmett-Teller (BET) and Fourier Transform Infrared (FT-IR) spectroscopy. The results show that the current density has a great effect on the morphology of the samples. The average size of the particles decreases as the applied current density increases and the average size of the samples decreases from 50 to 15 nm when the current density increases from 2 to 5 mA cm-2.

Biocomposite Plasma-Sprayed Coatings Based on Zinc-Substituted Hydroxyapatite: Structure, Properties, and Prospects of Application

NASA Astrophysics Data System (ADS)

Lyasnikova, A. V.; Markelova, O. A.; Lyasnikov, V. N.; Dudareva, O. A.

2016-01-01

The method of synthesis of a zinc-substituted hydroxyapatite powder is presented, and the technology of creating coatings by its spraying is described. The results of studies on the morphological, physical, and chemical parameters of a zinc-substituted hydroxyapatite coating by using X-ray analysis, infrared spectroscopy, transmission electron microscopy, optical microscopy, SEM, and other methods are given.

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.

A new sol-gel synthesis of 45S5 bioactive glass using an organic acid as catalyst.

PubMed

Faure, J; Drevet, R; Lemelle, A; Ben Jaber, N; Tara, A; El Btaouri, H; Benhayoune, H

2015-02-01

In this paper a new sol-gel approach was explored for the synthesis of the 45S5 bioactive glass. We demonstrate that citric acid can be used instead of the usual nitric acid to catalyze the sol-gel reactions. The substitution of nitric acid by citric acid allows to reduce strongly the concentration of the acid solution necessary to catalyze the hydrolysis of silicon and phosphorus alkoxides. Two sol-gel powders with chemical compositions very close to that of the 45S5 were obtained by using either a 2M nitric acid solution or either a 5mM citric acid solution. These powders were characterized and compared to the commercial Bioglass®. The surface properties of the two bioglass powders were assessed by scanning electron microscopy (SEM) and by Brunauer-Emmett-Teller method (BET). The Fourier transformed infrared spectroscopy (FTIR) and the X-ray diffraction (XRD) revealed a partial crystallization associated to the formation of crystalline phases on the two sol-gel powders. The in vitro bioactivity was then studied at the key times during the first hours of immersion into acellular Simulated Body Fluid (SBF). After 4h immersion into SBF we clearly demonstrate that the bioactivity level of the two sol-gel powders is similar and much higher than that of the commercial Bioglass®. This bioactivity improvement is associated to the increase of the porosity and the specific surface area of the powders synthesized by the sol-gel process. Moreover, the nitric acid is efficiently substituted by the citric acid to catalyze the sol-gel reactions without alteration of the bioactivity of the 45S5 bioactive glass. Copyright © 2014 Elsevier B.V. All rights reserved.

Effect of synthesis process on the microstructure and electrical conductivity of nickel/yttria-stabilized zirconia powders prepared by urea hydrolysis

NASA Astrophysics Data System (ADS)

Lin, Jyung-Dong; Wu, Zhao-Lun

In this study, NiO/YSZ composite powders were synthesized using hydrolysis on two solutions, one contains YSZ particles and Ni 2+ ion, and the other contains NiO particles, Zr 4+, and Y 3+ ions, with the aid of urea. The microstructure of the powders and sintered bulks was further characterized using X-ray diffraction, scanning electron microscopy, and transmission electron microscopy. The results indicated that various synthesis processes yielded NiO/YSZ powders with different morphologies. The NiO precursors would deposit onto the surface of YSZ particles, and NiO-deposited YSZ composite powders were obtained. Alternatively, it was not observed that YSZ precursors deposited onto the surface of NiO particles, thus, a uniform powder mixture of fine NiO and fine YSZ particles was produced. After sintering and subsequent reduction, these powders would lead to the variations of Ni distribution in the YSZ matrix and conductivity of cermets. Owing to the core-shell structure of the powders and the higher size ratio of YSZ and NiO particles, the conductivity of cermet with NiO-deposited YSZ powders containing 23 wt% NiO is comparable to those with a NiO/YSZ powder mixture containing 50 wt% NiO.

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

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.

Influence of reagents mixture density on the radiation-thermal synthesis of lithium-zinc ferrites

NASA Astrophysics Data System (ADS)

Surzhikov, A. P.; Lysenko, E. N.; Vlasov, V. A.; Malyshev, A. V.; Korobeynikov, M. V.; Mikhailenko, M. A.

2017-01-01

Influence of Li2CO3-ZnO-Fe2O3 powder reagents mixture density on the synthesis efficiency of lithium-zinc ferrites in the conditions of thermal heating or pulsed electron beam heating was studied by X-Ray diffraction and magnetization analysis. The results showed that the including a compaction of powder reagents mixture in ferrite synthesis leads to an increase in concentration of the spinel phase and decrease in initial components content in lithium-substituted ferrites synthesized by thermal or radiation-thermal heating.

Controlling the sol–gel process of nano-crystalline lithium-mica glass-ceramic by its chemical composition and synthesis parameters

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

Tohidifar, M.R., E-mail: tohidifar@znu.ac.ir; Alizadeh, P.; Aghaei, A.R.

2015-01-15

This paper aims to explore the impact of the parameters such as pH of the system, refluxing temperature, water quantity and chemical composition on the sol–gel synthesis of lithium-mica glass-ceramic nano-powder. The synthesis process was accomplished using two chemical composition formula (Li{sub (1+x)}Mg{sub 3}AlSi{sub 3(1+x)}O{sub 10+6.5x}F{sub 2} and LiMg{sub 3}AlSi{sub 3(1+x)}O{sub 10+6x}F{sub 2}). X-ray diffraction, Brunauer–Emmett–Teller surface area measurement and scanning electron microscopy techniques were applied to evaluate a variety of as-synthesized samples. Consequently, a transparent homogeneous sol was obtained under the conditions as pH ≤ 4, synthesis temperature ≤ 50 °C, and mol ratio of water to chemicals ≤more » 2. The prepared nano-powders under such conditions were in the range of 60–100 nm. The results also revealed that the mica glass-ceramics prepared based on the composition Li{sub (1+x)}Mg{sub 3}AlSi{sub 3(1+x)}O{sub 10+6.5x}F{sub 2} possessed finer powders due to their slow hydrolysis process. Moreover, any reduction in the stoichiometric deviation of lithium mica (x) leads to acquiring finer powders. - Highlights: • A transparent homogeneous sol leads to prepare nanopowders in the range of 60–100 nm. • The particles synthesized at lower temperatures possess finer sizes. • The acquired product which is prepared with excessive water offers larger sizes. • Any reduction in stoichiometric deviation leads to acquiring finer powders. • Taking synthesis composition as Li{sub (1+x)}Mg{sub 3}AlSi{sub 3(1+x)}O{sub 10+6.5x}F{sub 2} offers finer powders.« less

One-Step Hydrothermal Synthesis of Zeolite X Powder from Natural Low-Grade Diatomite.

PubMed

Yao, Guangyuan; Lei, Jingjing; Zhang, Xiaoyu; Sun, Zhiming; Zheng, Shuilin

2018-05-28

Zeolite X powder was synthesized using natural low-grade diatomite as the main source of Si but only as a partial source of Al via a simple and green hydrothermal method. The microstructure and surface properties of the obtained samples were characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM), wavelength dispersive X-ray fluorescence (XRF), calcium ion exchange capacity (CEC), thermogravimetric-differential thermal (TG-DTA) analysis, and N₂ adsorption-desorption technique. The influence of various synthesis factors, including aging time and temperature, crystallization time and temperature, Na₂O/SiO₂ and H₂O/Na₂O ratio on the CEC of zeolite, were systematically investigated. The as-synthesized zeolite X with binary meso-microporous structure possessed remarkable thermal stability, high calcium ion exchange capacity of 248 mg/g and large surface area of 453 m²/g. In addition, the calcium ion exchange capacity of zeolite X was found to be mainly determined by the crystallization degree. In conclusion, the synthesized zeolite X using diatomite as a cost-effective raw material in this study has great potential for industrial application such as catalyst support and adsorbent.

Synthesis of high-performance Li2FeSiO4/C composite powder by spray-freezing/freeze-drying a solution with two carbon sources

NASA Astrophysics Data System (ADS)

Fujita, Yukiko; Iwase, Hiroaki; Shida, Kenji; Liao, Jinsun; Fukui, Takehisa; Matsuda, Motohide

2017-09-01

Li2FeSiO4 is a promising cathode active material for lithium-ion batteries due to its high theoretical capacity. Spray-freezing/freeze-drying, a practical process reported for the synthesis of various ceramic powders, is applied to the synthesis of Li2FeSiO4/C composite powders and high-performance Li2FeSiO4/C composite powders are successfully synthesized by using starting solutions containing both Indian ink and glucose as carbon sources followed by heating. The synthesized composite powders have a unique structure, composed of Li2FeSiO4 nanoparticles coated with a thin carbon layer formed by the carbonization of glucose and carbon nanoparticles from Indian ink. The carbon layer enhances the electrochemical reactivity of the Li2FeSiO4, and the carbon nanoparticles play a role in the formation of electron-conducting paths in the cathode. The composite powders deliver an initial discharge capacity of 195 and 137 mAh g-1 at 0.1 C and 1 C, respectively, without further addition of conductive additive. The discharge capacity at 1 C is 72 mAh g-1 after the 100th cycle, corresponding to approximately 75% of the capacity at the 2nd cycle.

[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.

Influence of synthesis and sintering parameters on the characteristics of carbonate apatite.

PubMed

Landi, Elena; Tampieri, Anna; Celotti, Giancarlo; Vichi, Lucia; Sandri, Monica

2004-05-01

A new method to synthesise carbonate-substituted hydroxyapatite (CHA) powder has been set up introducing a CO(2) flux, as a source of carbonate, in the HA synthesis process based on the neutralisation reaction. The reactants are abundant and inexpensive. The yield is good compared to other CHA powder synthesis. The reaction may be performed at low temperature and without pH control and does not produce any by-products. The influence of the synthesis parameters (temperature, H(3)PO(4) solution dropping rate, i.e. reaction time, CO(2) flux, ageing time) has been tested to optimise the process conditions in order to obtain the highest carbonation degree and favour the B-type CHA precipitation with respect to A-type one. The prepared powder (5.8wt% of total carbonate with an A/B ratio of 0.78) was thermally treated at various temperatures in the range 500-1400 degrees C in different atmospheres (air, wet and dry carbon dioxide). The thermal treatments were performed with a double aim, to eliminate selectively the carbonate groups in A-position maintaining the B-type substitution, and to evaluate the thermal stability of the CHA and the total loss of carbonate as a function of temperature. The thermal treatment at 900 degrees C in wet CO(2) gave the best result in terms of a high carbonate residue and a low A/B ratio. We also investigate the use of different techniques (inductively coupled plasma, TGA, Fourier transformed infrared spectroscopy, X-ray diffraction) for characterising CHA and calculating sensitivity and accuracy in the quantification of carbonate ions for each molecular site.

Droplet-based microreactor for synthesis of water-soluble Ag₂S quantum dots.

PubMed

Shu, Yun; Jiang, Peng; Pang, Dai-Wen; Zhang, Zhi-Ling

2015-07-10

A droplet-based microreactor was used for synthesis of water-soluble Ag2S quantum dots (QDs). Monodispersed Ag2S nanoparticles with a surface of carboxylic acid-terminated were synthesized in the droplet microreactor. The x-ray powder diffraction results indicated products were monoclinic Ag2S nanocrystals. Furthermore, different-sized Ag2S QDs that were near-infrared-emitting or visible-emitting were continuously stably synthesized in droplet microreactors at different temperatures. We believe we offer a new method for obtaining different-sized Ag2S nanoparticles.

Droplet-based microreactor for synthesis of water-soluble Ag2S quantum dots

NASA Astrophysics Data System (ADS)

Shu, Yun; Jiang, Peng; Pang, Dai-Wen; Zhang, Zhi-Ling

2015-07-01

A droplet-based microreactor was used for synthesis of water-soluble Ag2S quantum dots (QDs). Monodispersed Ag2S nanoparticles with a surface of carboxylic acid-terminated were synthesized in the droplet microreactor. The x-ray powder diffraction results indicated products were monoclinic Ag2S nanocrystals. Furthermore, different-sized Ag2S QDs that were near-infrared-emitting or visible-emitting were continuously stably synthesized in droplet microreactors at different temperatures. We believe we offer a new method for obtaining different-sized Ag2S nanoparticles.

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.

Cooperative upconversion luminescence in Tb{sup 3+}:Yb{sup 3+} co-doped Y{sub 2}SiO{sub 5} powders prepared by combustion synthesis

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

Rakov, Nikifor, E-mail: nikifor.gomez@univasf.edu.br; Vieira, Simone A.; Guimarães, Renato B.

2014-03-15

Frequency upconversion (UC) luminescence via cooperative energy transfer (CET) process between pairs of Yb{sup 3+} and Tb{sup 3+} ions was investigated in Tb{sup 3+}:Yb{sup 3+}:Y{sub 2}SiO{sub 5} crystalline ceramic powders prepared by combustion synthesis. Surface morphology and structure of the powders were investigated by scanning electronic microscopy and X-ray powder diffraction. Photoluminescence experiments were performed in Tb{sup 3+}-singly doped samples using ultraviolet light (λ=255 nm) and in Tb{sup 3+}:Yb{sup 3+} co-doped samples using a near-infrared (NIR) diode laser (λ=975 nm). Upon excitation with the NIR diode laser, UC luminescence with an intense emission band centered at ∼549 nm, corresponding tomore » the 4f intraband {sup 5}D{sub 4}→{sup 7}F{sub 5} transition of Tb{sup 3+}, along with less intense emission bands at ∼490, ∼590 and ∼620 nm, corresponding to other {sup 5}D{sub 4}→{sup 7}F{sub J} transitions, was detected. The CET rate was estimated by analyzing the dynamics of UC luminescence with rate equations model of the electronic populations. -- Graphical Abstract: Left: Cooperative upconversion luminescence spectra of three powder samples prepared by combustion synthesis. Right: The SEM image of the powder showing that it consists of agglomerated flake-like shaped particles of various sizes. Full scale bar is 20 μm. Highlights: • Yttrium orthosilicate (Y{sub 2}SiO{sub 5}) powders were prepared by combustion synthesis. • Cooperative upconversion is observed for the first time in Tb{sup 3+}–Yb{sup 3+} doped Y{sub 2}SiO{sub 5}. • Energy transfer and back-transfer rates between Tb{sup 3+} and Yb{sup 3+} pairs were estimated.« less

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.

Synthesis of kalsilite from microcline powder by an alkali-hydrothermal process

NASA Astrophysics Data System (ADS)

Su, Shuang-qing; Ma, Hong-wen; Yang, Jing; Zhang, Pan; Luo, Zheng

2014-08-01

The properties of aluminosilicate kalsilite have attracted the interest of researchers in chemical synthesis, ceramic industry, biofuels, etc. In this study, kalsilite was hydrothermally synthesized from microcline powder in a KOH solution. The microcline powder, rich in potassium, aluminum, and silicon, was collected from Mountain Changling in Northwestern China. The effects of temperature, time, and KOH concentration on the decomposition of microcline were investigated. The kalsilite and intermediate products were characterized by means of wet chemistry analysis, X-ray Diffraction (XRD), infrared spectrometry (IR), 29Si magic angle spinning nuclear magnetic resonance (29Si MAS NMR), 27Al MAS NMR, and scanning electron microscope (SEM). With increasing temperature, the microcline powder transforms into a metastable KAlSiO4 polymorph before transforming further into pure kalsilite. A mixture of both kalsilite and metastable KAlSiO4 polymorph is obtained when the hydrothermal reaction is carried out within 2 h; but after 2 h, kalsilite is the predominant product. The concentration of KOH, which needs to be larger than 4.3 M, is an important parameter influencing the synthesis of kalsilite.

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.

Experimental study on the fabrication of advanced materials for energy applications using high energy mechanical milling

NASA Astrophysics Data System (ADS)

Narayana Swamy, Ashvin Kumar

The reaction of aluminum (Al) powder with water has the potential for on demand hydrogen generation. Conventional Al powders, however, react with water slowly due to a highly protective oxide layer on the particle surface. Current methods for Al activation involve harmful and expensive materials. The nano-scale Al powders also remain very expensive and have problems such as a large amount of oxide on the surface. The use of aluminum in an energy generation cycle is also hindered by the fact that, although Al is the most abundant metal in the Earth's crust, its recovery from ore consumes a lot of energy. Recycling aluminum hydroxide, formed as a result of Al reaction with water, would also require large amounts of energy. The energy consumption for production of Al powder and hence its cost could be significantly reduced by using recycled aluminum scrap and waste where aluminum is contained in metallic, non-oxidized form. The research work presented here investigates the preparation of an activated aluminum powder from aluminum foil that is widely available as scrap and waste. The obtained results demonstrate that a highly reactive, fine powder can be obtained from Al foil by high-energy ball milling with sodium chloride (NaCl). The obtained powder readily reacts with hot water, releasing hydrogen. Note that NaCl is an environment-friendly additive that can easily be removed after milling and recycled. After washing NaCl out, the powders retain a high reactivity with respect to hot water. As compared to previously studied activation of commercial Al powders, a major advantage of the investigated process is the feasibility of using secondary aluminum. Another area of research presented here is the synthesis of gallium oxide (Ga2O3) nanostructures for their use as high-temperature sensors. Quasi one-dimensional nanomaterials are of great interest due to increased focus on their importance in physics research and also their applications in the nanodevices industry. Since the mid 1950's, considerable research has been reported on the synthesis of filamentary crystals from alloys and metals. Since the discovery of carbon nanotubes (CNTs), there has been a tremendous surge in research activities for development and characterization of one-dimensional nanostructures. Most of the research is targeted towards the development of semiconductors such ZnO, Si, SnO2, and GaAs. Gallium oxide nanostructures have the ability to withstand high temperatures and also act as high-temperature sensors. In particular, they can be used as oxygen sensors at temperatures over 900 °C. These properties make gallium oxide nanostructures attractive for use in exhaust systems of the combustion chambers in power plants. beta-Ga2O3 nano-rods and nano-sheets were successfully synthesized by a simple method based on heating GaN in inert gas environment with traces of oxygen. Characterization of the obtained products showed nano-belts in the size range from 10 nm to 15 nm. Several other unique nano-structures were also synthesized. The results show a vapor-solid mechanism to be the prevailing growth route for the synthesis of nano-structures.

Sintering and Microstructure of BaTiO3 Nano Particles Synthesized by Molten Salt Method.

PubMed

Lee, Chang-Hyun; Shin, Hyo-Soon; Yeo, Dong-Hun; Ha, Gook-Hyun; Nahm, Sahn

2016-05-01

In order to establish thinner dielectric layers in thick film electronic components such as MLCC (Multilayer ceramic capacitor), BaTiO3 nanoparticles have been utilized. However, studies on the synthesis of nanoparticles smaller than 20 nm, the characteristics of the BaTiO3 powder, and the powder's sintering are lacking. Therefore, this paper aims to synthesize BaTiO3 particles smaller than 20 nm by using the molten salt method and evaluate the microstructure and dielectric properties by varying the sintering temperature from 750 degrees C to 1200 degrees C. Through the molten salt method and by using KOH-KCl mixed salt, 20 nm BaTiO3 powder was synthesized at a low temperature of 150 degrees C. Sintering the pellets formed from the synthesized 20 nm BaTiO3 nano powder led to the observation of an unusual phenomenon where the particles grew to approximate sizes below 850 degrees C where densification progressed. At sintering temperatures above 950 degrees C, particles that expanded into rod shapes were observed and these particles were identified to be unreacted TiO2 based on the results of the EDX (Energy Dispersive X-ray Spectroscopy) analysis and phase analysis results.

Combustion Synthesis of Sm0.5Sr0.5CoO3-x and La0.6Sr0.4CoO3-x Nanopowders for Solid Oxide Fuel Cell Cathodes

NASA Technical Reports Server (NTRS)

Bansal, Narottam P.; Zhong, zhimin

2005-01-01

Nanopowders of Sm0.5Sr0.5CoO(3-x) (SSC) and La0.6Sr0.4CoO(3-x) (LSC) compositions, which are being investigated as cathode materials for intermediate temperature solid oxide fuel cells, were synthesized by a solution-combustion method using metal nitrates and glycine as fuel. Development of crystalline phases in the as-synthesized powders after heat treatments at various temperatures was monitored by x-ray diffraction. Perovskite phase in LSC formed more readily than in SSC. Single phase perovskites were obtained after heat treatment of the combustion synthesized LSC and SSC powders at 1000 and 1200 C, respectively. The as-synthesized powders had an average particle size of 12 nm as determined from x-ray line broadening analysis using the Scherrer equation. Average grain size of the powders increased with increase in calcination temperature. Morphological analysis of the powders calcined at various temperatures was done by scanning electron microscopy.

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.

A Green Protocol for Synthesis of MAl2O4, [M=Cu and Co] Spinels Under Microwave Irradiation Method

NASA Astrophysics Data System (ADS)

Yuvasravana, R.; George, P. P.

Nanosized metal aluminates MAl2O4, [M=Cu and Co] are synthesized from their nitrates solution by using pomegranate peel extract as fuel in microwave combustion. MAl2O4 [M=Cu and Co] nanoparticles are grown in microwave assisted synthesis followed by annealing at 700∘C. The nanoparticles have been characterized by powder X-ray diffraction (PXRD), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), UV-VIS spectroscopy and photoluminescence (PL) spectroscopy. The PXRD analysis has confirmed their spinel composition. The green protocol and microwave combustion route for spinel synthesis are rapid, simple, without any hazardous chemicals as reducing or stabilizing agents and economical.

Synthesis of solid solutions of perovskites

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

Dambekalne, M.Y.; Antonova, M.K.; Perro, I.T.

The authors carry out thermographic studies, using a derivatograph, in order to understand the nature of the processes taking place during the synthesis of solid solutions of perovskites. Based on the detailed studies on the phase transformations occurring in the charges of the PSN-PMN solid solutions and on the selection of the optimum conditions for carrying out their synthesis, the authors obtained a powder containing a minimum quantity of the undesirable pyrochlore phase and by sintering it using the hot pressing method, they produced single phase ceramic specimens containing the perovskite phase alone with a density close to the theoreticalmore » value and showing zero apparent porosity and water absorption.« less

Low Temperature Synthesis, Chemical and Electrochemical Characterization of LiNi(x)Co(1-x)O2 (0 less than x less than 1)

NASA Technical Reports Server (NTRS)

Nanjundaswamy, K. S.; Standlee, D.; Kelly, C. O.; Whiteley, R. V., Jr.

1997-01-01

A new method of synthesis for the solid solution cathode materials LiNi(x)Co(1-x)O2 (0 less than x less than 1) involving enhanced reactions at temperatures less than or equal to 700 deg. C, between metal oxy-hydroxide precursors MOOH (M = Ni, Co) and Li-salts (Li2CO3, LiOH, and LiNO3) has been investigated. The effects of synthesis conditions and sources of Li, on phase purity, microstructure, and theoretical electrochemical capacity (total M(3+) content) are characterized by powder X-ray diffraction analysis, scanning electron microscopy, chemical analysis and room temperature magnetic susceptibility. An attempt has been made to correlate the electrochemical properties with the synthesis conditions and microstructure.

One pot synthesis of pure micro/nano photoactive α-PbO crystals

NASA Astrophysics Data System (ADS)

Bhagat, Dharini; Waldiya, Manmohansingh; Vanpariya, Anjali; Mukhopadhyay, Indrajit

2018-05-01

The present study reports a simple, fast and cost effective precipitation technique for synthesis of pure α-PbO powder. Lead monoxide powder with tetragonal structure was synthesized chemically at an elevated temperature using lead acetate and sodium hydroxide solution bath. XRD powder diffraction was used to find the structural properties as well as phase transition from alpha to beta. Study revealed that synthesized PbO powder was crystalline with tetragonal symmetry, having an average crystallite size of 70 nm and lattice constants; a=3.97Å, b=3.97Å, and c=5.02Å. Phase transition from tetragonal to orthorhombic structure was studied by comparing the XRD data of the annealed samples in the temperature range from 200 °C to 600 °C. UV-Visible spectroscopy was used to find out the optical properties of prepared PbO powder. Diffuse reflectance and absorbance spectra confirmed the formation of α-PbO with obtained direct band gap of 1.9 eV. Synthesized lead monoxide (α-PbO) powder has promising application in energy conversion as well as energy storage applications.

The synthetic activities of TiO2-moringa oleifera seed powder in the treatment of the wastewater of the coal mining industry

NASA Astrophysics Data System (ADS)

Marhaini; Legiso; Trilestari

2018-04-01

To process the coal wastewater, the combination of chemical based technology of Advanced Oxidation Process (AOP) of a strong oxidizer using TiO2 photocatalyst and biological treatment of moringa seed powder (Moringa oleifera) is used in the composite form. AOP can be used as an alternative treatment of coal wastewater which is quite economical and environmentally friendly. The XRD results of TiO2 powder and the synthesis of TiO2 - is moringa seed powder in the form of tetragonal crystals. The degradation results of the quality of the coal wastewater using TiO2 powder reached a decrease of (TSS, Fe, Mn, Zn, Hg, Cu, Co, Cr, Al and Ni) by an average of 70% and the increase of pH value of 7 at 200 minute stirring time. The decrease of the wastewater quality using the synthesis of TiO2- moringa seed powder by using sunlight and without sunlight is detected negative (-) at 200 minute stirring time.

Nonaqueous solution synthesis process for preparing oxide powders of lead zirconate titanate and related materials

DOEpatents

Voigt, J.A.; Sipola, D.L.; Tuttle, B.A.; Anderson, M.T.

1999-06-01

A process is disclosed for producing powders of perovskite-type compounds which comprises mixing a metal alkoxide solution with a lead acetate solution to form a homogeneous, clear metal solution, adding an oxalic acid/n-propanol solution to this metal solution to form an easily filterable, free-flowing precursor powder and then calcining this powder. This process provides fine perovskite-phase powders with ferroelectric properties which are particularly useful in a variety of electronic applications. 4 figs.

Nonaqueous solution synthesis process for preparing oxide powders of lead zirconate titanate and related materials

DOEpatents

Voigt, James A.; Sipola, Diana L.; Tuttle, Bruce A.; Anderson, Mark T.

1999-01-01

A process for producing powders of perovskite-type compounds which comprises mixing a metal alkoxide solution with a lead acetate solution to form a homogeneous, clear metal solution, adding an oxalic acid/n-propanol solution to this metal solution to form an easily filterable, free-flowing precursor powder and then calcining this powder. This process provides fine perovskite-phase powders with ferroelectric properties which are particularly useful in a variety of electronic applications.

Ionic liquid functionalized synthesis of gold nanoparticles in response to Elaise Guineensis (oil palm) leaves amount

NASA Astrophysics Data System (ADS)

Irfan, Muhammad; Ahmad, Tausif; Moniruzzaman, Muhammad; Abdullah, Bawadi

2018-05-01

A modified bio-synthesis method was developed to synthesize gold nanoparticles (AuNPs) using Elaeis Guineensis (oil palm) leaves (OPL) extract prepared in aqueous solution of IL, [EMIM][OAc]. The strong interaction and capping ability of IL at surface of AuNPs was examined through XPS analysis. The effect of OPL powder to liquid (P/L) ratio on absorbance, maximum wavelength (λmax) and size variation of AuNPs was observed through UV-vis. TEM analysis indicated predominantly spherical shape AuNPs with mean diameter of 15.76 nm. This study exhibits a rapid, cheap and efficient method to achieve stable AuNPs using bio-waste material.

A solid phase honey-like channel method for synthesizing urea-ammonium chloride cocrystals on industrial scale

NASA Astrophysics Data System (ADS)

Xue, Bingchun; Mao, Meiling; Liu, Yanhong; Guo, Jinyu; Li, Jing; Liu, Erbao

2016-05-01

Unanticipated a new and simple urea-ammonium chloride cocrystal synthesis method on industrial scale was found during attempts to produce a kind of granulated compound fertilizer. The aggregation of fertilizer powder can make the interaction among particles from loose to close, which generate mechanical pressure and in turn act as the driving force to benefit cocrystal growth. Additionally, the honeycomb-like channels constructed by other coexisting compound make the water evaporates more moderate, which can help the formation of supersaturated solution at suitable rate, further promote the growth of cocrystal. This approach possibly opens a new route toward the developing methodologies for cocrystal synthesis.

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.

Synthesis of ZnO Nanocrystal-Graphene Composite by Mechanical Milling and Sonication-Assisted Exfoliation

NASA Astrophysics Data System (ADS)

Arora, Sweety; Srivastava, Chandan

2017-02-01

A ZnO nanocrystal-graphene composite was synthesized by a two-step method involving mechanical milling and sonication-assisted exfoliation. Zn metal powder was first ball-milled with graphite powder for 30 h in water medium. This ball-milled mixture was then subjected to exfoliation by sonication in the presence of sodium lauryl sulfate surfactant to produce graphene decorated with spherical agglomerates of ultrafine nanocrystalline ZnO. The presence of a few layers of graphene was confirmed by Raman spectroscopy and atomic force microscopy measurements. The size, phase identity and composition of the ZnO nanocrystals was determined by transmission electron microscopy measurements.

Synthesis of Commercial Products from Copper Wire-Drawing Waste

NASA Astrophysics Data System (ADS)

Ayala, J.; Fernández, B.

2014-06-01

Copper powder and copper sulfate pentahydrate were obtained from copper wire-drawing scale. The hydrometallurgical recycling process proposed in this article yields a high-purity copper powder and analytical grade copper sulfate pentahydrate. In the first stage of this process, the copper is dissolved in sulfuric acid media via dismutation of the scale. In the second stage, copper sulfate pentahydrate is precipitated using ethanol. Effects such as pH, reaction times, stirring speed, initial copper concentration, and ethanol/solution volume ratio were studied during the precipitation from solution reaction. The proposed method is technically straightforward and provides efficient recovery of Cu from wire-drawing scale.

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.

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.

(Bi, Pb){sub 2}Sr{sub 2}Ca{sub 2}Cu{sub 3}O{sub x} superconductor and method of making same utilizing sinter-forging

DOEpatents

Chen, N.; Goretta, K.C.; Lanagan, M.T.

1998-10-13

A (BiPb){sub 2}Sr{sub 2}Ca{sub 2}Cu{sub 3}O{sub x}(Bi223) superconductor with high J{sub c}, phase purity, density and mechanical strength is formed from Bi2223 powder which is synthesized from a mixture of Bi{sub 2}O{sub 3}, PbO, SrCO{sub 3}, CaCo{sub 3} and CuO. The mixture is milled, then dried and calcined to synthesize the Bi2223 powder with the desired phase purity. The calcination is performed by heating the dried mixture for 50 hours at 840 C. The partially synthesized powder is then milled for 1--4 hours before calcining further for another 50 hours at 855 C to complete the synthesis. After calcination, the Bi2223 powder is cold pressed to a predetermined density and sinter forged under controlled temperature and time to form a Bi2223 superconductor with the desired superconducting properties. 5 figs.

(Bi, Pb).sub.2, Sr.sub.2 Ca.sub.2 Cu.sub.3 O.sub.x superconductor and method of making same utilizing sinter-forging

DOEpatents

Chen, Nan; Goretta, Kenneth C.; Lanagan, Michael T.

1998-01-01

A (BiPb).sub.2 Sr.sub.2 Ca.sub.2 Cu.sub.3 O.sub.x (Bi223) superconductor with high J.sub.c, phase purity, density and mechanical strength is formed from Bi2223 powder which is synthesized from a mixture of Bi.sub.2 O.sub.3, PbO, SrCO.sub.3, CaCo.sub.3 and CuO. The mixture is milled, then dried and calcined to synthesize the Bi2223 powder with the desired phase purity. The calcination is performed by heating the dried mixture for 50 hours at 840.degree. C. The partially synthesized powder is then milled for 1-4 hours before calcining further for another 50 hours at 855.degree. C. to complete the synthesis. After calcination, the Bi2223 powder is cold pressed to a predetermined density and sinter forged under controlled temperature and time to form a Bi2223 superconductor with the desired superconducting properties.

The synthesis, characterisation and in vivo study of a bioceramic for potential tissue regeneration applications

PubMed Central

Poinern, Gérrard Eddy Jai; Brundavanam, Ravi Krishna; Thi Le, Xuan; Nicholls, Philip K.; Cake, Martin A.; Fawcett, Derek

2014-01-01

Hydroxyapatite (HAP) is a biocompatible ceramic that is currently used in a number of current biomedical applications. Recently, nanometre scale forms of HAP have attracted considerable interest due to their close similarity to the inorganic mineral component of the bone matrix found in humans. In this study ultrafine nanometre scale HAP powders were prepared via a wet precipitation method under the influence of ultrasonic irradiation. The resulting powders were compacted and sintered to form a series of ceramic pellets with a sponge-like structure with varying density and porosity. The crystalline structure, size and morphology of the powders and the porous ceramic pellets were investigated using advanced characterization techniques. The pellets demonstrated good biocompatibility, including mixed cell colonisation and matrix deposition, in vivo following surgical implantation into sheep M. latissimus dorsi. PMID:25168046

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).

The effect of precipitation and calcination parameters on oxalate derived ThO2 pellets

NASA Astrophysics Data System (ADS)

Wangle, Tadeas; Tyrpekl, Vaclav; Cagno, Simone; Delloye, Thierry; Larcher, Olivier; Cardinaels, Thomas; Vleugels, Jozef; Verwerft, Marc

2017-11-01

Thorium oxalate is easy to prepare, but the derived oxide powders retain the platelet morphology of the primary oxalate. This negatively impacts packing and sintering. If powder milling is to be avoided, powder synthesis needs to be optimized. That is the goal of this paper, where different precipitation strategies were used and their effect on powder characteristics and pellet synthesis was investigated. Oxalates prepared by adding a thorium nitrate solution to an oxalic acid solution proved most promising. Further optimizing of the calcination temperature revealed that with increasing calcination temperature the packing density improved significantly. This came at the cost of decreased early stage sintering and a higher frequency of end-capping during compaction. The calcination temperature at which the highest final density can be reached was dependent on the sintering cycle. Furthermore, the ThO2 powders had less surface area and thus adsorbed less gases during storage when calcined at higher temperatures.

Low temperature synthesis of nano alpha-alumina powder by two-step hydrolysis

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

Yan, Ting; Guo, Xiaode, E-mail: guoxiaodenj@sina.com; Zhang, Xiang

Highlights: • The nano α-Al{sub 2}O{sub 3} with good dispersion was prepared by two-step hydrolysis. • α-Al{sub 2}O{sub 3} powders were added as seed particles in the hydrolysis. • This article indicated that the glucose could impel the γ-Al{sub 2}O{sub 3} transformed to α-Al{sub 2}O{sub 3} directly. • This article indicated that the addictive of α-Al{sub 2}O{sub 3} seed could improve the phase transformation rate of γ-Al{sub 2}O{sub 3} to α-Al{sub 2}O{sub 3}. • In this article, the pure α-Al{sub 2}O{sub 3} could be obtained by calcining at 1000 °C for 1.5 h. - Abstract: The ultral fine alpha-alumina powdermore » has been successfully synthesized via two-step hydrolysis of aluminum isopropoxide. Glucose and polyvinyl pyrrolidone were used as surfactants during the appropriate processing step. The alpha-alumina powder was used as seed particles. Several synthesis parameters, such as the amount of seeds, surfactants, and calcination temperature, were studied by X-ray diffraction (XRD), Fourier transform infrared spectra (FTIR), Thermogravimetry-differential scanning calorimetry (TG-DSC), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The experimental results showed that glucose greatly lower the phase transformation temperature of alpha-alumina by impelling the gamma-alumina transformed to alpha-alumina directly, and the seed could improve the phase transformation rate of alpha-alumina, the polyvinylpyrrolidone have an effect on preventing excessive grain growth and agglomeration of alpha-alumina powder. Comparatively well dispersed alpha-alumina powder with particle size less than 50 nm can be synthesized through this method after calcinations at 1000 °C for 2 h.« less

Synthesis and structural property of Si nanosheets connected to Si nanowires using MnCl2/Si powder source

NASA Astrophysics Data System (ADS)

Meng, Erchao; Ueki, Akiko; Meng, Xiang; Suzuki, Hiroaki; Itahara, Hiroshi; Tatsuoka, Hirokazu

2016-08-01

Si nanosheets connected to Si nanowires were synthesized using a MnCl2/Si powder source with an Au catalyst. The synthesis method has benefits in terms of avoiding conventionally used air-sensitive SiH4 or SiCl4. The existence of the Si nanosheets connected to the Si<111> nanowires, like sprouts or leaves with petioles, was observed, and the surface of the nanosheets was Si{111}. The nanosheets were grown in the growth direction of <211> perpendicular to that of the Si nanowires. It was evident from these structural features of the nanosheets that the nanosheets were formed by the twin-plane reentrant-edge mechanism. The feature of the observed lattice fringes, which do not appear for Si bulk crystals, of the Si(111) nanosheets obtained by high resolution transmission electron microscopy was clearly explained due to the extra diffraction spots that arose by the reciprocal lattice streaking effect.

Effect of reducing agents on low-temperature synthesis of nanostructured LiFePO4

NASA Astrophysics Data System (ADS)

Kulka, Andrzej; Walczak, Katarzyna; Zając, Wojciech; Molenda, Janina

2017-09-01

Simple co-precipitation synthesis procedure yielding nanometric LiFePO4 with enhanced electrochemical properties without any post-synthesis heat treatment is presented. XRD, SEM and TEM analysis of the obtained powders revealed platelet crystallites and well crystalized bulk structure. Effective way of decreasing amount of Fe3+ containing phases by addition of reducing agents (KI, (NH4)2S2O3, glucose and the atmosphere of 5%H2-95%Ar) during low-temperature (107 °C) synthesis is described. The traditional analytical chemistry methods or the Mӧssbauer spectroscopy methods revealed that utilization of selected reducing agents diminished Fe3+ concentration from 25 to 12 at%. The constructed cells with optimized LiFePO4 as a cathode material showed superior electrochemical performances, including high reversible capacity up to 162 mAh/g at C/10 current discharge rate, flat voltage plateau with a value close to 3.45 V vs. Li0/+.

Ultrarapid Multimode Microwave Synthesis of Nano/Submicron β-SiC

PubMed Central

Johnson, Michael; He, Wenzhi; Li, Guangming; Zhao, Chen; Yu, Luling; Huang, Juwen; Zhu, Haochen

2018-01-01

This paper presents the design, development and realization of a fast and novel process for the synthesis of 3C silicon carbide (β-SiC) nanorods and submicron powder. Using SiO2 (or Si) and activated carbon (AC), this process allows β-SiC to be synthesized with almost 100% purity in timeframes of seconds or minutes using multimode microwave rotary tube reactors under open-air conditions. The synthesis temperature used was 1460 ± 50 °C for Si + AC and 1660 ± 50 °C for SiO2 + AC. The shortest β-SiC synthesis time achieved was about 20 s for Si + AC and 100 s for SiO2 + AC. This novel synthesis method allows for scaled-up flow processes in the rapid industrial-scale production of β-SiC, having advantages of time/energy saving and carbon dioxide emission reduction over comparable modern processes. PMID:29470417

Synthesis of Bi.sub.1.8 Pb.sub.0.4 Sr.sub.2 Ca.sub.2 Cu.sub.3 O.sub.x superconductor

DOEpatents

Smith, Michael G.

1996-01-01

Two-powder processes for the synthesis of superconducting (Bi, Pb)-2223/Ag-clad wires by the oxide-powder-in-the-robe are provided. The first precursor powder, of nominal stoichiometry CaCuO.sub.x, is a solution-synthesized mixture of Ca.sub.0.45 Cu.sub.0.55 O.sub.2 and CaO. Using these oxide precursor mixtures, superconducting tapes with well-aligned grains and reproducible critical current densities J.sub.c in the range of 20,000 to 26,000 A/cm.sup.2 at 75 K in self-field after annealing less than 200 hours were obtained.

Synthesis of Bi{sub 1.8}Pb{sub 0.4}Sr{sub 2}Ca{sub 2}Cu{sub 3}O{sub x} superconductor

DOEpatents

Smith, M.G.

1996-10-29

Two-powder processes for the synthesis of superconducting (Bi, Pb)-2223/Ag-clad wires by the oxide-powder-in-the-robe are provided. The first precursor powder, of nominal stoichiometry CaCuO{sub x}, is a solution-synthesized mixture of Ca{sub 0.45}Cu{sub 0.55}O{sub 2} and CaO. Using these oxide precursor mixtures, superconducting tapes with well-aligned grains and reproducible critical current densities J{sub c} in the range of 20,000 to 26,000 A/cm{sup 2} at 75 K in self-field after annealing less than 200 hours were obtained. 2 figs.

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.

Novel high pressure hexagonal OsB2 by mechanochemistry

NASA Astrophysics Data System (ADS)

Xie, Zhilin; Graule, Moritz; Orlovskaya, Nina; Andrew Payzant, E.; Cullen, David A.; Blair, Richard G.

2014-07-01

Hexagonal OsB2, a theoretically predicted high-pressure phase, has been synthesized for the first time by a mechanochemical method, i.e., high energy ball milling. X-ray diffraction indicated that formation of hexagonal OsB2 begins after 2.5 h of milling, and the reaction reaches equilibrium after 18 h of milling. Rietveld refinement of the powder data indicated that hexagonal OsB2 crystallizes in the P63/mmc space group (No. 194) with lattice parameters of a=2.916 Å and c=7.376 Å. Transmission electron microscopy confirmed the appearance of the hexagonal OsB2 phase after high energy ball milling. in situ X-ray diffraction experiments showed that the phase is stable from -225 °C to 1050 °C. The hexagonal OsB2 powder was annealed at 1050 °C for 6 days in vacuo to improve crystallinity and remove strain induced during the mechanochemical synthesis. The structure partially converted to the orthorhombic phase (20 wt%) after fast current assisted sintering of hexagonal OsB2 at 1500 °C for 5 min. Mechanochemical approaches to the synthesis of hard boride materials allow new phases to be produced that cannot be prepared using conventional methods.

Structural, microstructural and magnetic evolution in cryo milled carbon doped MnAl.

PubMed

Fang, Hailiang; Cedervall, Johan; Hedlund, Daniel; Shafeie, Samrand; Deledda, Stefano; Olsson, Fredrik; von Fieandt, Linus; Bednarcik, Jozef; Svedlindh, Peter; Gunnarsson, Klas; Sahlberg, Martin

2018-02-06

The low cost, rare earth free τ-phase of MnAl has high potential to partially replace bonded Nd 2 Fe 14 B rare earth permanent magnets. However, the τ-phase is metastable and it is experimentally difficult to obtain powders suitable for the permanent magnet alignment process, which requires the fine powders to have an appropriate microstructure and high τ-phase purity. In this work, a new method to make high purity τ-phase fine powders is presented. A high purity τ-phase Mn 0.55 Al 0.45 C 0.02 alloy was synthesized by the drop synthesis method. The drop synthesized material was subjected to cryo milling and  followed by a flash heating process. The crystal structure and microstructure of the drop synthesized, cryo milled and flash heated samples were studied by X-ray in situ powder diffraction, scanning electron microscopy, X-ray energy dispersive spectroscopy and electron backscatter diffraction. Magnetic properties and magnetic structure of the drop synthesized, cryo milled, flash heated  samples were characterized by magnetometry and neutron powder diffraction, respectively. The results reveal that the 2 and 4 hours cryo milled and flash heated samples both exhibit high τ-phase purity and micron-sized round particle shapes. Moreover, the flash heated samples display high saturation magnetization as well as increased coercivity.

Green synthesis of silver nanoparticles mediated by Pulicaria glutinosa extract

PubMed Central

Khan, Mujeeb; Khan, Merajuddin; Adil, Syed Farooq; Tahir, Muhammad Nawaz; Tremel, Wolfgang; Alkhathlan, Hamad Z; Al-Warthan, Abdulrahman; Siddiqui, Mohammed Rafiq H

2013-01-01

The green synthesis of metallic nanoparticles (NPs) has attracted tremendous attention in recent years because these protocols are low cost and more environmentally friendly than standard methods of synthesis. In this article, we report a simple and eco-friendly method for the synthesis of silver NPs using an aqueous solution of Pulicaria glutinosa plant extract as a bioreductant. The as-prepared silver NPs were characterized using ultraviolet–visible spectroscopy, powder X-ray diffraction, transmission electron microscopy, energy-dispersive X-ray spectroscopy, and Fourier-transform infrared spectroscopy. Moreover, the effects of the concentration of the reductant (plant extract) and precursor solution (silver nitrate), the temperature on the morphology, and the kinetics of reaction were investigated. The results indicate that the size of the silver NPs varied as the plant extract concentration increased. The as-synthesized silver NPs were phase pure and well crystalline with a face-centered cubic structure. Further, Fourier-transform infrared spectroscopy analysis confirmed that the plant extract not only acted as a bioreductant but also functionalized the NPs’ surfaces to act as a capping ligand to stabilize them in the solvent. The developed eco-friendly method for the synthesis of NPs could prove a better substitute for the physical and chemical methods currently used to prepare metallic NPs commonly used in cosmetics, foods, and medicines. PMID:23620666

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

PubMed Central

2011-01-01

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

Low Cost Synthesis Method of Two-Dimensional Titanium Carbide MXene

NASA Astrophysics Data System (ADS)

Rasid, Z. A. M.; Omar, M. F.; Nazeri, M. F. M.; A'ziz, M. A. A.; Szota, M.

2017-06-01

A layered MAX phase of Ti3AlC2 was synthesized through pressureless sintering (PLS) the initial powder of TiH2/Al/C without preliminary dehydrogenation under argon atmosphere at 1350°C. An elegant exfoliations approach was used to prepare a two-dimensional (2D) metal carbide Ti3C2 from layered MAX phase by removing A layer by chemical etching. The use of PLS method instead of any pressure assistance method such as hot isostatic press (HIP) and hot press (HP) lowered the cost of synthesis. Recently, some unique potential of Ti3C2 has been discovered leads to the proposal of potential application, mostly on electronic devices. Morphology and structural analysis was used to confirm the successful of this research.

One-pot synthesis of LaFeO3-NiFe2O4 nanocomposite ceramic by egg-white method and its magnetic and dielectric properties

NASA Astrophysics Data System (ADS)

Muthu, K. Sudalai; Lakshminarasimhan, N.; Perumal, P.

2017-10-01

A facile, one-pot synthesis of nanocomposite of LaFeO3-NiFe2O4 was demonstrated by using egg-white method. The same method was adopted to synthesize the individual component oxide nanoparticles of LaFeO3 (LFO) and NiFe2O4 (NFO). The phase formation of individual components and the nanocomposite was confirmed using powder X-Ray diffraction (XRD) technique. The measured room temperature magnetic properties of LFO, NFO and LFO-NFO nanoparticles revealed an enhancement in the properties of the nanocomposite. The dielectric behaviours of LFO, NFO and LFO-NFO pellets sintered at different temperatures such as 800, 900 and 1000 °C were investigated and correlated with the microstructures.

Combustion synthesis of AlB2-Al2O3 composite powders with AlB2 nanowire structures

NASA Astrophysics Data System (ADS)

Yang, Pan; Xiao, Guoqing; Ding, Donghai; Ren, Yun; Yang, Shoulei; Lv, Lihua; Hou, Xing

2018-05-01

Using of Al and B2O3 powders as starting materials, and Mg-Al alloy as additives, AlB2-Al2O3 composite powders with AlB2 nanowire structures were successfully fabricated via combustion synthesis method in Ar atmosphere at a pressure of 1.5 MPa. The effect of different amount of Mg-Al alloy on the phase compositions and morphology of the combustion products was investigated. The results revealed that AlB2 and Al2O3 increased, whereas Al decreased with the content of Mg-Al alloy increasing. The impurities MgAl2O4 and AlB12 would exist in the sample with adding of 18 wt% Mg-Al alloy. Interestingly, FESEM/TEM/EDS results showed that AlB2 nanowires were observed in the products when the content of Mg-Al alloy is 6 wt% and 12 wt%. The more AlB2 nanowires can be found as the content of Mg-Al alloy increased. And the yield of AlB2 nanowires with the diameter of about 200 nanometers (nm) and the length up to several tens of micrometers (μm) in the combustion product is highest when the content of Mg-Al alloy is 12 wt%. The vapor, such as Mg-Al (g), B2O2 (g), AlO (g) and Al2O (g), produced during the process of combustion synthesis, reacted with each other to yield AlB2 nanowires by vapor-solid (VS) mechanism and the corresponding model was also proposed.

First report on soapnut extract-mediated synthesis of sulphur-substituted nanoscale NdFeB permanent magnets and their characterization

NASA Astrophysics Data System (ADS)

Jayapala Rao, G. V. S.; Prasad, T. N. V. K. V.; Shameer, Syed; Arun, T.; Purnachandra Rao, M.

2017-10-01

Biosynthesis of nanoscale materials has its own advantages over other physical and chemical methods. Using soapnut extract as reducing and stabilizing agent for the synthesis of inorganic nanoscale materials is novel and has not been exploited to its potential so far. Herein, we report for the first time on the effects of sulphur substitution on soapnut extract-mediated synthesis of nanoscale NdFeB (S-NdFeB) permanent magnetic powders (Nd 15%, Fe 77.5%, B 7.5% and S with molar ratios: 0.1, 0.2, 0.3, 0.4, and 0.5). To synthesize, a 10 ml of 10% soapnut extract was added to 90 ml of respective chemical composition and heated to 60 °C for 30 min and aged for 24 h. The dried powder was sintered at 500 °C for 1 h. The characterization of the as-prepared nanoscale S-NdFeB magnetic materials was done using the techniques such as X-ray diffraction (XRD), scanning electron microscopy (SEM) with energy dispersion spectroscopy (EDS), Fourier transform infrared spectroscopy (FT-IR), dynamic light scattering (DLS for size and zeta potential measurements) and vibrating sample magnetometer (VSM)-hysteresis loop studies. The results revealed that particles were highly stable (with a negative zeta potential of 25.7 mV) with irregular and spherical shape (with measured hydrodynamic diameter 6.7 and 63.5 nm). The tetragonal structures of the formed powders were revealed by XRD micrographs. Hysteresis loop studies clearly indicate the effect of S concentration on the enhanced magnetization of the materials.

Plasma dynamic synthesis and obtaining ultrafine powders of iron oxides with high content of ε-Fe2O3

NASA Astrophysics Data System (ADS)

Sivkov, Alexander; Naiden, Evgenii; Ivashutenko, Alexander; Shanenkov, Ivan

2016-05-01

The ultrafine iron oxide powders were successfully synthesized using the plasma dynamic synthesis method, based on the use of a coaxial magnetoplasma accelerator with the iron electrode system. The synthesis was implemented in the high-speed iron-containing plasma jet, flowing into the space of the sealed chamber, filled with the gaseous mixture of oxygen and argon at different ratios. The XRD investigations showed that the synthesized products were heterophase and consisted of three main phases such as magnetite Fe3O4, hematite α-Fe2O3 and ε-Fe2O3. The SEM data confirmed the presence of three particle types: the hollow spheroids with sizes about hundreds of micrometers (magnetite), the particles with sizes up to 100 μm from the porous material of sintered submicron particles (hematite), and nanoscale particles (ε-phase). We found that at the higher oxygen concentration the content of ε-Fe2O3 is increased up to 50% at the same time with decreasing the Fe3O4 phase. The magnetic properties of the products are mainly determined by magnetite characteristics and are significantly reduced with decreasing its content in the powder. In order to investigate the synthesized ε-Fe2O3 on the ability to absorb the electromagnetic radiation in the millimeter wavelength range, we separated the product with the higher ε-phase concentration. The fraction mainly, consisting of ε-Fe2O3, showed the occurrence of the natural resonance at frequencies of 8.3 GHz and 130 GHz.

In Situ Synthesis of Gold Nanoparticles on Wool Powder and Their Catalytic Application.

PubMed

Tang, Bin; Zhou, Xu; Zeng, Tian; Lin, Xia; Zhou, Ji; Ye, Yong; Wang, Xungai

2017-03-15

Gold nanoparticles (AuNPs) were synthesized in situ on wool powder (WP) under heating conditions. Wool powder not only reduced Au ions to AuNPs, but also provided a support for as-synthesized AuNPs. WPs were treated under different concentrations of Au ions, and corresponding optical features and morphologies of the treated WPs were investigated by UV-VIS diffuse reflectance absorption spectroscopy and scanning electron microscopy (SEM). X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and transmission electron microscope (TEM) were also employed to characterize the WP treated with AuNPs. The results demonstrate that AuNPs were produced in the presence of WP and distributed over the wool particles. The porous structure led to the synthesis of AuNPs in the internal parts of WP. Acid conditions and high temperature facilitated the synthesis of AuNPs by WP in aqueous solution. The reducibility of wool was improved after being converted to powder from fibers, due to exposure of more active groups. Moreover, the obtained AuNP-WP complexes showed significant catalytic activity to accelerate the reduction reaction of 4-nitrophenol (4-NP) by sodium borohydride (NaBH₄).

Synthesis of Amorphous Powders of Ni-Si and Co-Si Alloys by Mechanical Alloying

NASA Astrophysics Data System (ADS)

Omuro, Keisuke; Miura, Harumatsu

1991-05-01

Amorphous powders of the Ni-Si and Co-Si alloys are synthesized by mechanical alloying (MA) from crystalline elemental powders using a high energy ball mill. The alloying and amorphization process is examined by X-ray diffraction, differential scanning calorimetry (DSC), and scanning electron microscopy. For the Ni-Si alloy, it is confirmed that the crystallization temperature of the MA powder, measured by DSC, is in good agreement with that of the powder sample prepared by mechanical grinding from the cast alloy ingot products of the same composition.

Synthesis of spherical calcium phosphate particles for dental and orthopedic applications

PubMed Central

Bohner, Marc; Tadier, Solène; van Garderen, Noémie; de Gasparo, Alex; Döbelin, Nicola; Baroud, Gamal

2013-01-01

Calcium phosphate materials have been used increasingly in the past 40 years as bone graft substitutes in the dental and orthopedic fields. Accordingly, numerous fabrication methods have been proposed and used. However, the controlled production of spherical calcium phosphate particles remains a challenge. Since such particles are essential for the synthesis of pastes and cements delivered into the host bone by minimally-invasive approaches, the aim of the present document is to review their synthesis and applications. For that purpose, production methods were classified according to the used reagents (solutions, slurries, pastes, powders), dispersion media (gas, liquid, solid), dispersion tools (nozzle, propeller, sieve, mold), particle diameters of the end product (from 10 nm to 10 mm), and calcium phosphate phases. Low-temperature calcium phosphates such as monetite, brushite or octacalcium phosphate, as well as high-temperature calcium phosphates, such as hydroxyapatite, β-tricalcium phosphate or tetracalcium phosphate, were considered. More than a dozen production methods and over hundred scientific publications were discussed. PMID:23719177

One-Pot Synthesis of CoSex -rGO Composite Powders by Spray Pyrolysis and Their Application as Anode Material for Sodium-Ion Batteries.

PubMed

Park, Gi Dae; Kang, Yun Chan

2016-03-14

A simple one-pot synthesis of metal selenide/reduced graphene oxide (rGO) composite powders for application as anode materials in sodium-ion batteries was developed. The detailed mechanism of formation of the CoSe(x)-rGO composite powders that were selected as the first target material in the spray pyrolysis process was studied. The crumple-structured CoSe(x)-rGO composite powders prepared by spray pyrolysis at 800 °C had a crystal structure consisting mainly of Co0.85 Se with a minor phase of CoSe2. The bare CoSe(x) powders prepared for comparison had a spherical shape and hollow structure. The discharge capacities of the CoSe(x)-rGO composite and bare CoSe(x) powders in the 50th cycle at a constant current density of 0.3 A g(-1) were 420 and 215 mA h g(-1), respectively, and their capacity retentions measured from the second cycle were 80 and 46%, respectively. The high structural stability of the CoSe(x)-rGO composite powders for repeated sodium-ion charge and discharge processes resulted in superior sodium-ion storage properties compared to those of the bare CoSe(x) powders. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Aluminum powder metallurgy processing

NASA Astrophysics Data System (ADS)

Flumerfelt, Joel Fredrick

In recent years, the aluminum powder industry has expanded into non-aerospace applications. However, the alumina and aluminum hydroxide in the surface oxide film on aluminum powder require high cost powder processing routes. A driving force for this research is to broaden the knowledge base about aluminum powder metallurgy to provide ideas for fabricating low cost aluminum powder components. The objective of this dissertation is to explore the hypothesis that there is a strong linkage between gas atomization processing conditions, as-atomized aluminum powder characteristics, and the consolidation methodology required to make components from aluminum powder. The hypothesis was tested with pure aluminum powders produced by commercial air atomization commercial inert gas atomization and gas atomization reaction synthesis (GARS). The commercial atomization methods are bench marks of current aluminum powder technology. The GARS process is a laboratory scale inert gas atomization facility. A benefit of using pure aluminum powders is an unambiguous interpretation of the results without considering the effects of alloy elements. A comparison of the GARS aluminum powders with the commercial aluminum powders showed the former to exhibit superior powder characteristics. The powders were compared in terms of size and shape, bulk chemistry, surface oxide chemistry and structure, and oxide film thickness. Minimum explosive concentration measurements assessed the dependence of explosibility hazard on surface area, oxide film thickness, and gas atomization processing conditions. The GARS aluminum powders were exposed to different relative humidity levels, demonstrating the effect of atmospheric conditions on post-atomization oxidation of aluminum powder. An Al-Ti-Y GARS alloy exposed in ambient air at different temperatures revealed the effect of reactive alloy elements on post-atomization powder oxidation. The pure aluminum powders were consolidated by two different routes, a conventional consolidation process for fabricating aerospace components with aluminum powder and a proposed alternative. The consolidation procedures were compared by evaluating the consolidated microstructures and the corresponding mechanical properties. A low temperature solid state sintering experiment demonstrated that tap densified GARS aluminum powders can form sintering necks between contacting powder particles, unlike the total resistance to sintering of commercial air atomization aluminum powder.

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.

Wet powder processing of sol-gel derived mesoporous silica-hydroxyapatite hybrid powders.

PubMed

Andersson, Jenny; Johannessen, Espen; Areva, Sami; Järn, Mikael; Lindén, Mika

2006-08-01

This paper describes a method by which a porous silica coating layer can be obtained on different apatite particles through a simple sol-gel synthesis route. Sol-gel derived powders of hydroxyapatite (HAP) and beta tricalciumphosphate (beta-TCP) were coated with a mesoporous silica using C16TAB (hexadecyltrimethylammonium bromide) as a template in order to induce mesophase formation. Further calcination of the material removes the template from the mesophase and leaves a highly ordered hexagonal arranged mesoporous silica structure with a core of HAP/beta-TCP. The phase purity of the SiO2/apatite composites has been thoroughly investigated by the means of FT-IR, XRD, and solid state 31P MAS NMR. The phase purity of these materials is shown to be dependent on the solubility properties of the used apatites. The hybrid materials are suitable as a multifunctional biomaterial where osteoconductive properties can be combined with drug delivery.

[Structure determination of three novel bile acids from bear bile powder].

PubMed

Jian, Long-Hai; Mao, Xiu-Hong; Wang, Ke; Ji, Shen

2013-08-01

A method of LC-QTOF/MS combining with chemical synthesis has been used to determine the structures of three novel bile acids from bear bile powder. Reference substances of tauroursodeoxycholic acid and taurochenodeoxycholic acid were oxidized by pyridinium chlorochromate. The products were analyzed by LC-QTOF/MS. Total 4 products including 3 isomers were predicted and identified according to the PCC oxidation theory and LC-QTOF/MS results. Bear bile powder samples were dissolved by methanol and analyzed by LC-QTOF/MS. Three unknown peaks were found and identified as 2-[[(3beta, 5beta)-3-hydroxy-7, 24-dioxocholan-24-yl]amino]-ethanesulfonic acid, 2-[[(5beta)-3, 7, 24-trioxocholan-24-yl]amino]-ethanesulfonic acid and 2-[[(5beta, 7beta)-7-hydroxy-3, 24-dioxocholan-24-yl]amino]-ethanesulfonic acid, separately, by matching their results with that of oxidation products above.

Synthesis of Nano-Crystalline Gamma-TiAl Materials

NASA Technical Reports Server (NTRS)

Hales, Stephen J.; Vasquez, Peter

2003-01-01

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

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.

Low temperature synthesis and characterization of carbonated hydroxyapatite nanocrystals

NASA Astrophysics Data System (ADS)

Anwar, Aneela; Asghar, Muhammad Nadeem; Kanwal, Qudsia; Kazmi, Mohsin; Sadiqa, Ayesha

2016-08-01

Carbonate substituted hydroxyapatite (CHA) nanorods were synthesized via coprecipitation method from aqueous solution of calcium nitrate tetrahydrate and diammonium hydrogen phosphate (with urea as carbonate ion source) in the presence of ammonium hydroxide solution at 70 °C at the conditions of pH 11. The obtained powders were physically characterized using transmission electron microscopy (TEM), X-ray powder diffraction analysis (XRD), and FTIR and Raman spectroscopy. The particle size was evaluated by Dynamic light scattering (DLS). The chemical structural analysis of as prepared sample was performed using X-ray photoelectron spectroscopy (XPS). After ageing for 12 h, and heat treatment at 1000 °C for 1 h, the product was obtained as highly crystalline nanorods of CHA.

Synthesis and characterization of TiC nanopowders via sol-gel and subsequent carbothermal reduction process

NASA Astrophysics Data System (ADS)

Chen, Xu; Fan, Jinglian; Lu, Qiong

2018-06-01

TiC nanocrystalline powders were synthesized by in-situ carbothermic reduction of Ti-O-C precursor under vacuum atmosphere. And the Ti-O-C precursor was formed by sol-gel method from titanium butyrate (TBOT) and sucrose. To obtain stable sol, TBOT was directly added into mixed solution which contains water, sucrose, acetic acid (AcOH) and acetylacetone (ACAC). This procedure is more convenient and economical because it avoids the use of alcohol which is used as solvent in most reports of alkoxide hydrolysis sol-gel method. TG-DSC, XRD, FTIR and SEM/TEM were employed to analyze and characterize the product during the entire process. The phase composition and crystalline structure parameters of powders with different C/Ti molar ratio were investigated by Rietveld refinement method, and elemental quantitative analysis of the samples were performed. Furthermore, the optimal parameters of carbothermal reduction were obtained and the grain growth mechanism was demonstrated. The results show that TiC nanocrystalline powders (C/Ti molar ratio is 3.5 in the precursor) were synthesized at 1300 °C for 2 h, which have near standard lattice parameter, well crystallinity and fine average grain size ( 37.4 nm).

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.

Hierarchical macro-mesoporous structures in the system TiO{sub 2}-Al{sub 2}O{sub 3}, obtained by hydrothermal synthesis using Tween-20 as a directing agent

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

Garcia-Benjume, M.L.; Espitia-Cabrera, M.I.; Contreras-Garcia, M.E., E-mail: eucontre@zeus.umich.mx

2009-12-15

Macro-mesoporous powders of titania, alumina, and mixed titania-20%alumina systems were obtained by hydrothermal synthesis employing surfactant Tween-20 as structural directing agent in order to promote the textural properties of titania. The effect of the alumina in the titania phase and on textural properties was analyzed. The obtained powders presented a macroporous channel structure that was characterized by X-ray diffractometry, scanning and transmission electron microscopy, N{sub 2} adsorption-desorption analysis, pore size distribution, Fourier transform infrared spectrometry, and thermogravimetric analysis. It was found that alumina content retarded the anatase phase crystallization and increased the Brunauer-Emmet-Teller surface area from 136 to 210 m{supmore » 2}/g. The powders calcined at 400 deg. C are thermally stable and possess an interconnected macro-mesoporous hierarchical structure; the results indicate that this synthesis can be employed to prepare mixed titania-alumina with good textural properties.« less

Synthesis of nanostructured vanadium powder by high-energy ball milling: X-ray diffraction and high-resolution electron microscopy characterization

NASA Astrophysics Data System (ADS)

Krishnan, Vinoadh Kumar; Sinnaeruvadi, Kumaran

2016-10-01

Vanadium metal powders, ball milled with different surfactants viz., stearic acid, KCl and NaCl, have been studied by X-ray diffraction and transmission electron microscopy. The surfactants alter the microstructural and morphological characteristics of the powders. Ball milling with stearic acid results in solid-state amorphization, while powders milled with KCl yield vanadium-tungsten carbide nanocomposite mixtures. NaCl proved to be an excellent surfactant for obtaining nanostructured fusion-grade vanadium powders. In order to understand the reaction mechanism behind any interstitial addition in the ball-milled powders, CHNOS analysis was performed.

Sintering of BaCe(sub 0.85)Y(sub 0.15)O(sub 3-delta) with/without SrTiO3 Dopant

NASA Technical Reports Server (NTRS)

Dynys, F.; Sayir, A.; Heimann, P. J.

2004-01-01

The perovskite composition, BaCe(sub 0.85)Y(sub 0.15)O(sub 3-delta), displays excellent protonic conduction at high temperatures making it a desirable candidate for hydrogen separation membranes. This paper reports on the sintering behavior of BaCe(sub 0.85)Y(sub 0.15)O(sub 3-delta) powders doped with SrTiO3. Two methods were used to synthesize BaCe(sub 0.85)Y(sub 0.15)O(sub 3-delta) powders: (1) solid state reaction and (2) wet chemical co-precipitation. Co-precipitated powder crystallized into the perovskite phase at 1000 C for 4 hrs. Complete reaction and crystallization of the perovskite phase by solid state was achieved by calcining at 1200 C for 24 hrs. Solid state synthesis produced a coarser powder with an average particle size of 1.3 microns and surface area of 0.74 sq m/g. Co-precipitation produced a finer powder with a average particle size of 65 nm and surface area of 14.9 sq m/g. Powders were doped with 1, 2, 5, and 10 mole % SrTiO3. Samples were sintered at 1450 C, 1550 C and 1650 C. SrTiO3 enhances sintering, optimal dopant level is different for powders synthesized by solid state and co-precipitation. Both powders exhibit similar grain growth behavior. Dopant levels of 5 and 10 mole % SrTiO3 significantly enhances the grain size.

Synthesis of cerium oxide (CeO 2) by co-precipitation for application as a reference material for X-ray powder diffraction peak widths

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

de Lima Batista, Anderson Márcio; Miranda, Marcus Aurélio Ribeiro; Martins, Fátima Itana Chaves Custódio

Several methods can be used to obtain, from powder diffraction patterns, crystallite size and lattice strain of polycrystalline samples. Some examples are the Scherrer equation, Williamson–Hall plots, Warren/Averbach Fourier decomposition, Whole Powder Pattern Modeling, and Debye function analysis. To apply some of these methods, it is necessary to remove the contribution of the instrument to the widths of the diffraction peaks. Nowadays, one of the main samples used for this purpose is the LaB6 SRM660b commercialized by the National Institute of Standard Technology; the width of the diffraction peak of this sample is caused only by the instrumental apparatus. However,more » this sample can be expensive for researchers in developing countries. In this work, the authors present a simple route to obtain micron-sized polycrystalline CeO 2that have a full width at half maximum comparable with the SRM660b and therefore it can be used to remove instrumental broadening.« less

Structural comparison of sintering products made of "TiC + Ti" composite powders and "Ti + C" powder mixtures

NASA Astrophysics Data System (ADS)

Krinitcyn, Maksim G.; Pribytkov, Gennadii A.; Korosteleva, Elena N.; Firsina, Irina A.; Baranovskii, Anton V.

2017-12-01

In this study, powder composite materials comprised of TiC and Ti with different ratios are processed by sintering of Ti and C powder mixtures and self-propagating high-temperature synthesis (SHS) in "Ti+C" system followed by sintering. The microstructure and porosity of obtained composites are investigated and discussed. The dependence of porosity on sintering time is explained theoretically. Optimal regimes that enable to obtain the most homogeneous structure with the least porosity are described.

Sol-Gel Synthesis of La(0.6)Sr(0.4)CoO(3-x) and Sm(0.5)Sr(0.5)CoO(3-x) Cathode Nanopowders for Solid Oxide Fuel Cells

NASA Technical Reports Server (NTRS)

Bansal, Narottam P.; Wise, Brent

2011-01-01

Nanopowders of La(0.6)Sr(0.4)CoO(3-x) (LSC) and Sm(0.5)Sr(0.5)CoO(3-x) (SSC) compositions, which are being investigated as cathode materials for intermediate temperature solid oxide fuel cells (IT-SOFC) with La(Sr)Ga(Mg)O(3-x) (LSGM) as the electrolyte, were synthesized by low-temperature sol-gel method using metal nitrates and citric acid. Thermal decomposition of the citrate gels was followed by simultaneous DSC/TGA methods. Development of phases in the gels, on heat treatments at various temperatures, was monitored by x-ray diffraction. Solgel powders calcined at 550 to 1000 C consisted of a number of phases. Single perovskite phase La(0.6)Sr(0.4)CoO(3-x) or Sm(0.5)Sr(0.5)CoO(3-x) powders were obtained at 1200 and 1300 C, respectively. Morphological analysis of the powders calcined at various temperatures was done by scanning electron microscopy. The average particle size of the powders was approx.15 nm after 700 C calcinations and slowly increased to 70 to 100 nm after heat treatments at 1300 to 1400 C.

Formation of polycrystalline MgB2 synthesized by powder in sealed tube method with different initial boron phase

NASA Astrophysics Data System (ADS)

Yudanto, Sigit Dwi; Imaduddin, Agung; Kurniawan, Budhy; Manaf, Azwar

2018-04-01

Magnesium diboride, MgB2 is a new high critical temperature superconductor that discovered in the beginning of the 21st century. The MgB2 has a simple crystal structure and a high critical temperature, which can be manufactured in several forms like thin films, tapes, wires including bulk in the large scale. For that reason, the MgB2 has good prospects for various applications in the field of electronic devices. In the current work, we have explored the synthesis of MgB2 polycrystalline using powder in a sealed tube method. Different initial boron phase for the synthesized of MgB2 polycrystalline were used. These were, in addition to magnesium powders, crystalline boron, amorphous boron and combination both of them were respectively fitted in the synthesis. The raw materials were mixed in a stoichiometric ratio of Mg: B=1:2, ground using agate mortar, packed into stainless steel SS304. The pack was then sintered at temperature of 800°C for 2 hours in air atmosphere. Phase formation of MgB2 polycrystalline in difference of initial boron phase was characterized using XRD and SEM. Referring to the diffraction pattern and microstructure observation, MgB2 polycrystalline was formed, and the formation was effective when using the crystalline Mg and fully amorphous B as the raw materials. The critical temperature of the specimen was evaluated by the cryogenic magnet. The transition temperature of the MgB2 specimen synthesized using crystalline magnesium and full amorphous boron is 42.678 K (ΔTc = 0.877 K).

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

One-pot green synthesis of zinc oxide nano rice and its application as sonocatalyst for degradation of organic dye and synthesis of 2-benzimidazole derivatives

NASA Astrophysics Data System (ADS)

Paul, Bappi; Vadivel, Sethumathavan; Dhar, Siddhartha Sankar; Debbarma, Shyama; Kumaravel, M.

2017-05-01

In this paper, we report novel and green approach for one-pot biosynthesis of zinc oxide (ZnO) nanoparticles (NPs). Highly stable and hexagonal phase ZnO nanoparticles were synthesized using seeds extract from the tender pods of Parkia roxburghii and characterized by XRD, FT-IR, EDX, TEM, and N2 adsorption-desorption (BET) studies. The present method of synthesis of ZnO NPs is very efficient and cost effective. The powder XRD pattern furnished evidence for the formation of hexagonal close packing structure of ZnO NPs having average crystallite size 25.6 nm. The TEM image reveals rice shapes ZnO NPs are with an average diameter of 40-60 nm. The as-synthesized ZnO NPs has proved to be an excellent sonocatalysts for degradation of organic dye and synthesis of 2-benzimidazole derivatives.

High-throughput continuous hydrothermal synthesis of nanomaterials (part II): unveiling the as-prepared CexZryYzO2-δ phase diagram.

PubMed

Quesada-Cabrera, Raul; Weng, Xiaole; Hyett, Geoff; Clark, Robin J H; Wang, Xue Z; Darr, Jawwad A

2013-09-09

High-throughput continuous hydrothermal flow synthesis was used to manufacture 66 unique nanostructured oxide samples in the Ce-Zr-Y-O system. This synthesis approach resulted in a significant increase in throughput compared to that of conventional batch or continuous hydrothermal synthesis methods. The as-prepared library samples were placed into a wellplate for both automated high-throughput powder X-ray diffraction and Raman spectroscopy data collection, which allowed comprehensive structural characterization and phase mapping. The data suggested that a continuous cubic-like phase field connects all three Ce-Zr-O, Ce-Y-O, and Y-Zr-O binary systems together with a smooth and steady transition between the structures of neighboring compositions. The continuous hydrothermal process led to as-prepared crystallite sizes in the range of 2-7 nm (as determined by using the Scherrer equation).

Low cost synthesis of TiO2-C nanocomposite powder for high efficiency visible light photocatalysis

NASA Astrophysics Data System (ADS)

Mohapatra, A. K.; Nayak, J.

2018-04-01

Titanium dioxide-carbon nanocomposite powder was synthesized via a low cost chemical route using oleic acid and titanium tetra-isopropoxide. Since the carbon remained mainly on the surface of the TiO2 nanoparticles, the powder had black color. The composition of the powder was analyzed by X-ray photoelectron spectroscopy and the structure was studied with X-ray diffraction and transmission electron microscopy. The visible photocatalytic activity of the black TiO2 powder was investigated by studying the photo-bleaching of methylene blue under visible light. Our experimental observation showed that the black-TiO2 powder had a higher visible photocatalytic activity compared to the commercial TiO2 powder (P25 Degussa).

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

Low-temperature synthesis of actinide tetraborides by solid-state metathesis reactions

DOEpatents

Lupinetti, Anthony J [Los Alamos, NM; Garcia, Eduardo [Los Alamos, NM; Abney, Kent D [Los Alamos, NM

2004-12-14

The synthesis of actinide tetraborides including uranium tetraboride (UB.sub.4), plutonium tetraboride (PuB.sub.4) and thorium tetraboride (ThB.sub.4) by a solid-state metathesis reaction are demonstrated. The present method significantly lowers the temperature required to .ltoreq.850.degree. C. As an example, when UCl.sub.4 is reacted with an excess of MgB.sub.2, at 850.degree. C., crystalline UB.sub.4 is formed. Powder X-ray diffraction and ICP-AES data support the reduction of UCl.sub.3 as the initial step in the reaction. The UB.sub.4 product is purified by washing water and drying.

Microwave assisted combustion synthesis of nanocrystalline CoFe2O4 for LPG sensing

NASA Astrophysics Data System (ADS)

Chaudhari, Prashant; Acharya, S. A.; Darunkar, S. S.; Gaikwad, V. M.

2015-08-01

A microwave-assisted citrate precursor method has been utilized for synthesis of nanocrystalline powders of CoFe2O4. The process takes only a few minutes to obtain as-synthesized CoFe2O4. Structural properties of the synthesized material were investigated by X-ray diffraction; scanning electron microscopy, Thermogravimetric analysis (TGA) and Fourier transform infrared spectroscopy. The gas sensing properties of thick film of CoFe2O4 prepared by screen printing towards Liquid Petroleum Gas (LPG) revealed that CoFe2O4 thick films are sensitive and shows maximum sensitivity at 350°C for 2500 ppm of LPG.

Synthesis and characterization of Mn-Bi alloy

NASA Astrophysics Data System (ADS)

Mishra, Ashutosh; Patil, Harsha; Jain, G.; Mishra, N.

2012-06-01

High purity MnBi low temperature phase has been prepared and analyzed using X-ray diffraction, Lorentz-Polarization Factor and Fourier transforms infrared measurement. After synthesis of samples structural characterization has done on samples by X-ray diffraction, which shows that after making the bulk sample is in no single phase MnBi has been prepared by sintering Mn and Bi powders. By Lorentz-Polarization Factor is affecting the relative intensity of diffraction lines on a powder form. And by FTIR which shows absorption peaks of MnBi alloys.

The microstructure-processing-property relationships in an aluminum matrix composite system reinforced by aluminum-copper-iron alloy particles

NASA Astrophysics Data System (ADS)

Tang, Fei

Solid state vacuum sintering was studied in tap densified Al powder and in hot quasi-isostatically forged samples composed of commercial inert gas atomized or high purity Al powder, generated by a gas atomization reaction synthesis (GARS) technique. The GARS process results in spherical Al powder with a far thinner surface oxide. The overall results indicated the enhanced ability of GARS-processed Al and Al alloy powders for solid state sintering, which may lead to simplification of current Al powder consolidation processing methods. Elemental Al-based composites reinforced with spherical Al-Cu-Fe alloy powders were produced by quasi-isostatic forging and vacuum hot pressing (VHP) consolidation methods. It was proved that spherical Al-Cu-Fe alloy powders can serve as an effective reinforcement particulate for elemental Al-based composites, because of their high hardness and a preferred type of matrix/reinforcement interfacial bonding, with reduced strain concentration around the particles. Ultimate tensile strength and yield strength of the composites were increased over the corresponding Al matrix values, far beyond typical observations. This remarkable strengthening was achieved without precipitation hardening and without severe strain hardening during consolidation because of the matrix choice (elemental Al) and the "low shear" consolidation methods utilized. This reinforcement effectiveness is further evidenced by elastic modulus measurements of the composites that are very close to the upper bound predictions of the rule of mixtures. The load partitioning measurements by neutron diffraction showed that composite samples made from GARS powders present significantly higher load transfer efficiency than the composites made from commercially atomized powders. Further analysis of the load sharing measurements and the calculated values of the mismatch of coefficient of thermal expansion (CTE) and the geometrically necessary dislocation (GND) effects suggest that these strengthening mechanisms can be combined to predict accurately the strength of the composites. By neutron diffraction measurements, it also was found that the composites consolidated from Al and Al63Cu25Fe12 quasicrystal alloy reinforcement powders have compressive residual stress in the Al matrix, contrary to the tensile residual stress in typical Al/SiC composites. The composites made by the quasi-isostatic forging process exhibited higher tensile strengths and much higher compressive residual stresses than the composites made by the VHP process.

Ultrasonic-assisted preparation of nano eggshell powder: a novel catalyst in green and high efficient synthesis of 2-aminochromenes.

PubMed

Mosaddegh, Elaheh

2013-11-01

The nano eggshell powder (NESP) has been prepared by ultrasound irradiation and used as a novel and biodegradable catalyst with high catalytic activity and reusability in green synthesis of 2-aminochromenes via condensation of α- or β-phathol, malononitrile and aromatic aldehydes at 120 °C under solvent-free conditions. The reaction proceeds to completion within 10-35 min in 91-98% yield. Nano eggshell catalyst was characterized by scanning electron microscopy, X-ray powder diffraction, IR spectroscopy and X-ray fluorescence, thermal gravimetric, surface area and elemental analyses. In addition, the catalytic activity and chemical structure of nano-sized eggshell were compared with pure CaCO3. Copyright © 2013 Elsevier B.V. All rights reserved.

Combustion synthesis continuous flow reactor

DOEpatents

Maupin, G.D.; Chick, L.A.; Kurosky, R.P.

1998-01-06

The present invention is a reactor for combustion synthesis of inorganic powders. The reactor includes a reaction vessel having a length and a first end and a second end. The reaction vessel further has a solution inlet and a carrier gas inlet. The reactor further has a heater for heating both the solution and the carrier gas. In a preferred embodiment, the reaction vessel is heated and the solution is in contact with the heated reaction vessel. It is further preferred that the reaction vessel be cylindrical and that the carrier gas is introduced tangentially into the reaction vessel so that the solution flows helically along the interior wall of the reaction vessel. As the solution evaporates and combustion produces inorganic material powder, the carrier gas entrains the powder and carries it out of the reactor. 10 figs.

Combustion synthesis continuous flow reactor

DOEpatents

Maupin, Gary D.; Chick, Lawrence A.; Kurosky, Randal P.

1998-01-01

The present invention is a reactor for combustion synthesis of inorganic powders. The reactor includes a reaction vessel having a length and a first end and a second end. The reaction vessel further has a solution inlet and a carrier gas inlet. The reactor further has a heater for heating both the solution and the carrier gas. In a preferred embodiment, the reaction vessel is heated and the solution is in contact with the heated reaction vessel. It is further preferred that the reaction vessel be cylindrical and that the carrier gas is introduced tangentially into the reaction vessel so that the solution flows helically along the interior wall of the reaction vessel. As the solution evaporates and combustion produces inorganic material powder, the carrier gas entrains the powder and carries it out of the reactor.

Modeling & processing of ceramic and polymer precursor ceramic matrix composite materials

NASA Astrophysics Data System (ADS)

Wang, Xiaolin

Synthesis and processing of novel materials with various advanced approaches have attracted much attention of engineers and scientists for the past thirty years. Many advanced materials display a number of exceptional properties and can be produced with different novel processing techniques. For example, AlN is a promising candidate for electronic, optical and opto-electronic applications due to its high thermal conductivity, high electrical resistivity, high acoustic wave velocity and large band gap. Large bulk AlN crystal can be produced by sublimation of AlN powder. Novel nonostructured multicomponent refractory metal-based ceramics (carbides, borides and nitrides) show a lot of exceptional mechanical, thermal and chemical properties, and can be easily produced by pyrolysis of suitable preceramic precursors mixed with metal particles. The objective of this work is to study sublimation and synthesis of AlN powder, and synthesis of SiC-based metal ceramics. For AlN sublimation crystal growth, we will focus on modeling the processes in the powder source that affect significantly the sublimation growth as a whole. To understand the powder porosity evolution and vapor transport during powder sublimation, the interplay between vapor transport and powder sublimation will be studied. A physics-based computational model will be developed considering powder sublimation and porosity evolution. Based on the proposed model, the effect of a central hole in the powder on the sublimation rate is studied and the result is compared to the case of powder without a hole. The effect of hole size on the sublimation rate will be studied. The effects of initial porosity, particle size and driving force on the sublimation rate are also studied. Moreover, the optimal growth condition for large diameter crystal quality and high growth rate will be determined. For synthesis of SiC-based metal ceramics, we will focus on developing a multi-scale process model to describe the dynamic behavior of filler particle reaction, microstructure evolution, at the microscale as well as transient fluid flow, heat transfer, and species transport at the macroscale. The model comprises of (i) a microscale model and (ii) a macroscale transport model, and aims to provide optimal conditions for the fabrication process of the ceramics. The porous media macroscale model for SiC-based metal-ceramic materials processing will be developed to understand the thermal polymer pyrolysis, chemical reaction of active fillers and transport phenomena in the porous media. The macroscale model will include heat and mass transfer, curing, pyrolysis, chemical reaction and crystallization in a mixture of preceramic polymers and submicron/nano-sized metal particles of uranium, zirconium, niobium, or hafnium. The effects of heating rate, sample size, size and volume ratio of the metal particles on the reaction rate and product uniformity will be studied. The microscale model will be developed for modeling the synthesis of SiC matrix and metal particles. The macroscale model provides thermal boundary conditions to the microscale model. The microscale model applies to repetitive units in the porous structure and describes mass transport, composition changes and motion of metal particles. The unit-cell is the representation unit of the source material, and it consists of several metal particles, SiC matrix and other components produced from the synthesis process. The reactions between different components, the microstructure evolution of the product will be considered. The effects of heating rate and metal particle size on species uniformity and microstructure are investigated.

Morphological evolution of Bi2Se3 nanocrystalline materials synthesized by microwave assisted solvothermal method

NASA Astrophysics Data System (ADS)

Bera, Sumit; Behera, P.; Mishra, A. K.; Krishnan, M.; Patidar, M. M.; Singh, D.; Gangrade, M.; Venkatesh, R.; Deshpande, U. P.; Phase, D. M.; Ganesan, V.

2018-04-01

Structural, morphological and spectroscopic properties of Bi2Se3 nanoparticles synthesized by microwave assisted solvothermal method were investigated systematically. A controlled synthesis of different morphologies by a small variation in synthesis procedure is demonstrated. Powder X-ray diffraction (XRD) confirmed the formation of single phase. Crystallite and particle size reductions were studied with XRD and AFM (Atomic Force Microscopy). Different morphologies such as hexagonal nanoflakes with cross section of around˜6µm, nanoflower and octahedral agglomerated crystals of nearly ˜60 nm size have been observed in scanning electron microscope while varying the microwave assisted synthesis procedures. A significant blue shift observed in diffuse reflectance spectroscopy evidences the energy gap tuning as a result of morphological evolution. The difference in morphology observed in this three fast, facile and scalable synthesis is advantageous for tuning the thermoelectric figure of merit and for probing the surface states of these topological insulators. Low temperature resistivity remains similar for all three variants depicting a 2D character as evidenced by a -lnT term of localization.

Thermal Stability of Milled Nanocrystalline Tungsten Powders

DTIC Science & Technology

2011-05-01

v Acknowledgments This research is supported by mission funding from the Depleted Uranium Replacement Program and is the result of collaborative...L.; Reddy, R. G. Synthesis of Titanium Carbide Nano-powders by Thermal Plasma. Scripta Materialia 2005, 52 (12), 1253–1258. 4. Karagedov, G. R

Processing of laser formed SiC powder

NASA Technical Reports Server (NTRS)

Haggerty, J. S.; Bowen, H. K.

1987-01-01

Processing research was undertaken to demonstrate that superior SiC characteristics could be achieved through the use of ideal constituent powders and careful post-synthesis processing steps. Initial research developed the means to produce approximately 1000 A uniform diameter, nonagglomerated, spherical, high purity SiC powders. Accomplishing this goal required major revision of the particle formation and growth model from one based on classical nucleation and growth to one based on collision and coalescence of Si particles followed by their carburization. Dispersions based on pure organic solvents as well as steric stabilization were investigated. Test parts were made by the colloidal pressing technique; both liquid filtration and consolidation (rearrangement) stages were modeled. Green densities corresponding to a random close packed structure were achieved. After drying, parts were densified at temperatures ranging from 1800 to 2100 C. This research program accomplished all of its major objectives. Superior microstructures and properties were attained by using powders having ideal characteristics and special post-synthesis processing procedures.

Detailed kinetics of titanium nitride synthesis

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

Rode, H.; Hlavacek, V.

1995-02-01

A thermogravimetric analyzer is used to study the synthesis of TiN from Ti powder over a wide range of temperature, conversion and heating rate, and for two Ti precursor powders with different morphologies. Conversions to TiN up to 99% are obtained with negligible oxygen contamination. Nonisothermal initial rate and isothermal data are used in a nonlinear least-squares minimization to determine the most appropriate rate law. The logarithmic rate law offers an excellent agreement between the experimental and calculated conversions to TiN and can predict afterburning, which is an important experimentally observed phenomenon. Due to the form of the logarithmic ratemore » law, the observed activation energy is a function of effective particle size, extent of conversion, and temperature even when the intrinsic activation energy remains constant. This aspect explains discrepancies among activation energies obtained in previous studies. The frequently used sedimentation particle size is a poor measure of the powder reactivity. The BET surface area indicates the powder reactivity much better.« less

JPRS Report, Science & Technology, Japan, 28th Ceramics Science Discussion

DTIC Science & Technology

1990-11-13

U non doped "5 Ag powder A 60 120 180 140 300 Temperature (K) Figure 1. Plots or Resistivity Vs. Temperature for YBa 2 Cu 30Y to Which Different...Yasuharu Kodama, et al.] ........................ 13 -a - Superplasticity of Hydroxyapatite [Fumihiro Wakai, Yasuharu Kodama, et al...67 Synthesis of Ag -Added Bi-Pb-Ca-Cu-O Powder by Spray Drying, Superconductivity of Powder [Hiroko Higuma, Mitsunobu Wakata, et al

Combustion synthesis and structural analysis of nanocrystalline nickel ferrite at low temperature regime

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

Shanmugavel, T., E-mail: gokulrajs@hotmail.com, E-mail: shanmugavelnano@gmail.com; Raj, S. Gokul, E-mail: gokulrajs@hotmail.com, E-mail: shanmugavelnano@gmail.com; Rajarajan, G.

2015-06-24

Combustion synthesis of single phase Nickel ferrite was successfully achieved at low temperature regime. The obtained powders were calcinated to increase the crystallinity and their characterization change due to calcinations is investigated in detail. Citric acid used as a chelating agent for the synthesis of nickel ferrite. Pure single phase nickel ferrites were found at this low temperature. The average crystalline sizes were measured by using powder XRD measurements. Surface morphology was investigated through Transmission Electron Microscope (TEM). Particle size calculated in XRD is compared with TEM results. Magnetic behaviour of the samples is analyzed by using Vibrating Sample Magnetometermore » (VSM). Saturation magnetization, coercivity and retentivity are measured and their results are discussed in detail.« less

Si

NASA Astrophysics Data System (ADS)

Fiameni, S.; Famengo, A.; Agresti, F.; Boldrini, S.; Battiston, S.; Saleemi, M.; Johnsson, M.; Toprak, M. S.; Fabrizio, M.

2014-06-01

Magnesium silicide (Mg2Si)-based alloys are promising candidates for thermoelectric (TE) energy conversion in the middle-high temperature range. The detrimental effect of the presence of MgO on the TE properties of Mg2Si based materials is widely known. For this reason, the conditions used for synthesis and sintering were optimized to limit oxygen contamination. The effect of Bi doping on the TE performance of dense Mg2Si materials was also investigated. Synthesis was performed by ball milling in an inert atmosphere starting from commercial Mg2Si powder and Bi powder. The samples were consolidated, by spark plasma sintering, to a density >95%. The morphology, and the composition and crystal structure of samples were characterized by field-emission scanning electronic microscopy and x-ray diffraction, respectively. Moreover, determination of Seebeck coefficients and measurement of electrical and thermal conductivity were performed for all the samples. Mg2Si with 0.1 mol% Bi doping had a ZT value of 0.81, indicative of the potential of this method for fabrication of n-type bulk material with good TE performance.

Key to enhance thermoelectric performance by controlling crystal size of strontium titanate

NASA Astrophysics Data System (ADS)

Wang, Jun; Ye, Xinxin; Yaer, Xinba; Wu, Yin; Zhang, Boyu; Miao, Lei

2015-09-01

One-step molten salt synthesis process was introduced to fabricate nano to micrometer sized SrTiO3 powders in which effects of synthesis temperature, oxide-to-flux ratios and raw materials on the generation of SrTiO3 powders were examined. 100 nm or above sized pure SrTiO3 particles were obtained at relatively lower temperature of 900∘C. Micro-sized rhombohedral crystals with a maximum size of approximately 12 μm were obtained from SrCO3 or Sr(NO3)2 strontium source with 1:1 O/S ratio. Controlled crystal size and morphology of Nb-doped SrTiO3 particles are prepared by using this method to confirm the performance of thermoelectric properties. The Seebeck coefficient obtained is significantly high when compared with the reported data, and the high ratio of nano particles in the sample has a positive effect on the increase of Seebeck coefficient too, which is likely due to the energy filtering effect at large numbers of grain boundaries resulting from largely distributed structure.

Molecular Design and Synthesis of New Noncrystalline Solids

DTIC Science & Technology

1981-06-01

1. Powder X-ray diffraction pattern obtained have concluded that the crystallinity of the films using CuKa radiation. Sharp lines in is a sensitive ...pattern ;is formned in tile detector plane for each position of thle incident beam onl thre specimen. Thte diameter of the region giving thie...analyzer or over an aperture placed immediately in front of a scintillator-photomultiplier detector . This recording method is so inefficient that

EGCG assisted green synthesis of ZnO nanopowders: Photodegradative, antimicrobial and antioxidant activities

NASA Astrophysics Data System (ADS)

Suresh, D.; Udayabhanu; Nethravathi, P. C.; Lingaraju, K.; Rajanaika, H.; Sharma, S. C.; Nagabhushana, H.

2015-02-01

Zinc oxide nanopowders were synthesized by solution combustion method using Epigallocatechin gallate (EGCG) a tea catechin as fuel. The structure and morphology of the product was characterized by Powder X-ray Diffraction, Scanning Electron Microscopy, photoluminescence and UV-Visible spectroscopy. The nanopowders (Nps) were subjected to photocatalytic and biological activities such as antimicrobial and antioxidant studies. PXRD patterns demonstrate that the formed product belongs to hexagonal wurtzite system. SEM images show that the particles are agglomerated to form sponge like structure and the average crystallite sizes were found to be ∼10-20 nm. PL spectra exhibit broad and strong peak at 590 nm due to the Zn-vacancies, and O-vacancies. The prepared ZnO Nps exhibit excellent photocatalytic activity for the photodegradation of malachite green (MG) and methylene blue (MB) indicating that the ZnO NPs are potential photocatalytic semiconductor materials. ZnO NPs exhibit significant bactericidal activity against Klebsiella aerogenes, Pseudomonas aeruginosa, Escherichia coli and Staphylococcus aureus using the agar well diffusion method. Furthermore, the ZnO nano powders show good antioxidant activity by potentially scavenging DPPH radicals. The study successfully demonstrates synthesis of ZnO NPs by simple ecofriendly route employing EGCG as fuel that exhibit superior photodegradative, antibacterial and antioxidant activities.

Effects of Processing Parameters on the Synthesis of (K0.5Na0.5)NbO3 Nanopowders by Reactive High-Energy Ball Milling Method

PubMed Central

Duc Van, Nguyen

2014-01-01

The effects of ball milling parameters, namely, the ball-to-powder mass ratio and milling speed, on the synthesis of (K0.5Na0.5)NbO3 nanopowders by high-energy ball milling method from a stoichiometric mixture containing Na2CO3, K2CO3, and Nb2O5 were investigated in this paper. The results indicated that the single crystalline phase of (K0.5Na0.5)NbO3 was received in as-milled samples synthesized using optimized ball-to-powder mass ratio of 35 : 1 and at a milling speed of 600 rpm for 5 h. In the optimized as-milled samples, no remaining alkali carbonates that can provide the volatilizable potassium-containing species were found and (K0.5Na0.5)NbO3 nanopowders were readily obtained via the formation of an intermediate carbonato complex. This complex was mostly transformed into (K0.5Na0.5)NbO3 at temperature as low as 350°C and its existence was no longer detected at spectroscopic level when calcination temperature crossed over 700°C. PMID:24592146

Effects of processing parameters on the synthesis of (K0.5Na0.5)NbO3 nanopowders by reactive high-energy ball milling method.

PubMed

Nguyen, Duc Van

2014-01-01

The effects of ball milling parameters, namely, the ball-to-powder mass ratio and milling speed, on the synthesis of (K0.5Na0.5)NbO3 nanopowders by high-energy ball milling method from a stoichiometric mixture containing Na2CO3, K2CO3, and Nb2O5 were investigated in this paper. The results indicated that the single crystalline phase of (K0.5Na0.5)NbO3 was received in as-milled samples synthesized using optimized ball-to-powder mass ratio of 35 : 1 and at a milling speed of 600 rpm for 5 h. In the optimized as-milled samples, no remaining alkali carbonates that can provide the volatilizable potassium-containing species were found and (K0.5Na0.5)NbO3 nanopowders were readily obtained via the formation of an intermediate carbonato complex. This complex was mostly transformed into (K0.5Na0.5)NbO3 at temperature as low as 350°C and its existence was no longer detected at spectroscopic level when calcination temperature crossed over 700°C.

The synthesis of ternary acetylides with tellurium: Li 2 TeC 2 and Na 2 TeC 2

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

Németh, Károly; Unni, Aditya K.; Kalnmals, Christopher

The synthesis of ternary acetylides Li 2TeC 2 and Na 2TeC 2 is presented as the first example of ternary acetylides with metalloid elements instead of transition metals. The synthesis was carried out by the direct reaction of the corresponding bialkali acetylides with tellurium powder in liquid ammonia. Alternatively, the synthesis of Na 2TeC 2 was also carried out by the direct reaction of tellurium powder and two equivalents of NaC 2H in liquid ammonia leading to Na 2TeC 2 and acetylene gas through an equilibrium containing the assumed NaTeC 2H molecules besides the reactants and the products. The resultingmore » disordered crystalline materials were characterized by X-ray diffraction and Raman spectroscopy. Implications of these new syntheses on the synthesis of other ternary acetylides with metalloid elements and transition metals are also discussed.« less

Monte Carlo Simulation of Nanoparticle Encapsulation in Flames

NASA Technical Reports Server (NTRS)

Sun, Z.; Huertas, J. I.; Axelbaum, R. L.

1999-01-01

Gas-phase combustion (flame) synthesis has been an essential industrial process for producing large quantities of powder materials such as carbon black, titanium dioxide, and silicon dioxide. Flames typically produce simple oxides, with carbon black being the noted exception because the oxides of carbon are gaseous and are easily separated from the particulate matter that is formed during fuel pyrolysis. Furthermore, the powders produced in flames are usually agglomerated, nanometer-sized particles (nanoparticles). This composition and morphology is acceptable for many applications. However, the present interest in nanoparticles for advanced materials application has led to efforts to employ flames for the synthesis of unagglomerated nanoparticles (2 to 100 nm) of metals and non-oxide ceramics. Sodium-halide chemistry has proven to be viable for producing metals and non-oxide ceramics in flames. Materials that have been produced to date include Si (Calcote and Felder, 1993), TiN, TiB2, TiC, TiSi2, SiC, B4C (Glassman et al, 1993) Al, W, Ti, TiB2, AlN, and W-Ti and Al-AlN composites (DuFaux and Axelbaum, 1995, Axelbaum et al 1996,1997). Many more materials are possible. The main challenge that faces application of flame synthesis for advanced materials is overcoming formation of agglomerates in flames (Brezinsky, 1997). The high temperatures and high number densities in the flame environment favor the formation of agglomerates. Agglomerates must be avoided for many reasons. For example, when nanopowders are consolidated, agglomerates have a deleterious effect on compaction density, leading to voids in the final part. Efforts to avoid agglomeration in flames without substantially reducing particle number density and, consequently, production rate, have had limited success. Another critical challenge that faces all synthesis routes for nanopowders is ensuring that the powders are high purity and that the process is scaleable. Though the containerless, high temperature environment of a flame is excellent for producing high-purity simple compounds, ultrafine metals and non-oxide ceramic powders are inherently reactive in the presence of oxygen and/or moisture. Thus, the handling of these powders after synthesis poses a challenging problem. Impurities acquired during handling of nanoparticles have plagued the advancement of nanostructured materials technology.

Synthesis of PZT powder by conventional method at various conditions

NASA Astrophysics Data System (ADS)

Necira, Z.; Boutarfaia, A.; Abba, M.; Abdessalem, N.

2012-06-01

In this work, the formation of Pb(Zr1-xTix)O3 solid solutions with composition near the morphotropic phase boundary (MPB) using the conventional ceramic method have been studied by changing the thermal conditions such as temperature ramp rate and isothermal times during the calcination treatment performed between 700 and 900 °C. The perovskite phase formation and morphology of undoped Pb(Zr0.52Ti0.48)O3 (abbreviated PZT) and doped new material Pb0.98Gd0.02[(Zr0.52Ti0.48)0.98 (Mg1/3Nb2/3)0.01 (Ni1/3Sb2/3)0.01]O3 (abbreviated PZT-PGMNNS) specimens have been examined by powder X-ray diffraction (XRD), scanning electron microscopy (SEM) and Fourier Transform Infrared (FTIR) while the thermal evolution of the initial precursor was followed by TG-DTA. So the results of these studies have been discussed.

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

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

Zhang Jianrong; Gao Lian

2004-12-02

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

Comparison of mechanical and friction properties of composite materials based on AlMg2 containing nano-dimensional particles of crystalline graphite and nanofibers of gamma oxide of aluminum

NASA Astrophysics Data System (ADS)

Aborkin, A. V.; Babin, D. M.; Soboĺkov, A. V.

2018-04-01

The method of mechanical synthesis in a planetary ball mill was used for production of composite powders based on the AlMg2 alloy containing 1 wt. % of nanosized particles of crystalline graphite or γ-Al2O3. The resulting powders are consolidated by the sintering under pressure. Using the methods of X-ray diffraction analysis, scanning and transmission electron microscopy, the structural-phase composition of bulk composite materials was studied. Comparative analysis of the microhardness, the conditional yield stress at compression, and the friction coefficient of bulk composite materials is carried out. It has been found out that the mechanical properties of composites reinforced with γ-Al2O3 nanofibers are higher than when reinforcing with nanoscale particles of crystalline graphite.

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.

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

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

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

2015-07-22

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

Plasmachemical synthesis of nanopowders of yttria and zirconia from dispersed water-salt-organic mixtures

NASA Astrophysics Data System (ADS)

Novoselov, Ivan; Karengin, Alexander; Shamanin, Igor; Alyukov, Evgeny; Gusev, Alexander

2018-03-01

Article represents results on theoretical and experimental research of yttria and zirconia plasmachemical synthesis in air plasma from water-salt-organic mixtures "yttrium nitrate-water-acetone" and "zirconyl nitrate-water-acetone". On the basis of thermotechnical calculations the influence of organic component on lower heat value and adiabatic combustion temperature of water-salt-organic mixtures as well as compositions of mixtures providing their energy-efficient plasma treatment were determined. The calculations found the influence of mass fraction and temperature of air plasma supporting gas on the composition of plasma treatment products. It was determined the conditions providing yttria and zirconia plasmachemical synthesis in air plasma. During experiments it was b eing carried out the plasmachemical synthesis of yttria and zirconia powders in air plasma flow from water -salt-organic mixtures. Analysis of the results for obtained powders (scanning electron microscopy, X-ray diffraction analysis, BET analysis) confirm nanostructure of yttria and zirconia.

LiFePO4 Nanostructures Fabricated from Iron(III) Phosphate (FePO4 x 2H2O) by Hydrothermal Method.

PubMed

Saji, Viswanathan S; Song, Hyun-Kon

2015-01-01

Electrode materials having nanometer scale dimensions are expected to have property enhancements due to enhanced surface area and mass/charge transport kinetics. This is particularly relevant to intrinsically low electronically conductive materials such as lithium iron phosphate (LiFePO4), which is of recent research interest as a high performance intercalation electrode material for Li-ion batteries. Many of the reported works on LiFePO4 synthesis are unattractive either due to the high cost of raw materials or due to the complex synthesis technique. In this direction, synthesis of LiFePO4 directly from inexpensive FePO4 shows promise.The present study reports LiFePO4 nanostructures prepared from iron (III) phosphate (FePO4 x 2H2O) by precipitation-hydrothermal method. The sintered powder was characterized by X-ray diffractometry (XRD), X-ray photoelectron spectroscopy (XPS), Inductive coupled plasma-optical emission spectroscopy (ICP-OES), and Electron microscopy (SEM and TEM). Two synthesis methods, viz. bulk synthesis and anodized aluminum oxide (AAO) template-assisted synthesis are reported. By bulk synthesis, micro-sized particles having peculiar surface nanostructuring were formed at precipitation pH of 6.0 to 7.5 whereas typical nanosized LiFePO4 resulted at pH ≥ 8.0. An in-situ precipitation strategy inside the pores of AAO utilizing the spin coating was utilized for the AAO-template-assisted synthesis. The template with pores filled with the precipitate was subsequently subjected to hydrothermal process and high temperature sintering to fabricate compact rod-like structures.

Synthesis of ultrafine Si3N4 powder in RF-RF plasma

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

Sato, Michitaka; Nishio, Hiroaki

1991-10-01

A newly designed plasma-CVD apparatus mounted with the RF-RF type plasma torch was introduced to synthesize ultrafine powders of silicon nitride (Si3N4). The RF-RF plasma system (the combination of a main (lower) and controlling (upper) RF plasma) improved the stability of simple RF plasma and solved the impurity problem of dc-RF hybrid plasma. The reaction of SiCl4 and NH3, which were radially injected into the tail flames of the upper and lower plasmas, respectively, yielded near-stoichiometric amorphous powders of Si3N4. The nitrogen content in the products largely depended on the flow rate of the quenching gas, a mixture of NH3more » (reactant) and H2. The oxygen content and metal impurities are 2-3 wt pct and less than 200 ppm, respectively. The powder particles had an average diameter of about 15 nm with a narrow size distribution, and showed extreme air sensitivity. Conspicuous crystallazation and particle growth occurred when heated at temperatures above 1400 C. These results suggested that the RF-RF system was a potential reactor for the synthesis of ultrafine powders with excellent sinterability at relatively low temperatures. 9 refs.« less

Synthesis of Nano-Size AlN Powders by Carbothermal Reduction from Plasma-Assisted Ball Milling Precursor

NASA Astrophysics Data System (ADS)

Liu, Zhijie; Wang, Wenchun; Yang, Dezheng; Wang, Sen; Dai, Leyang

2016-07-01

Nano-size aluminum nitride (AlN) powders have been successfully synthesized with a high efficiency method through annealing from milling assisted by discharge plasma (p-milling) alumina (Al2O3) precursors. The characterization of the p-milling Al2O3 powders and the synthesized AlN are investigated. Compared to conventional ball milling (c-milling), it can be found that the precursors by p-milling have a finer grain size with a higher specific surface area, which lead to a faster reaction efficiency and higher conversion to AlN at lower temperatures. The activation energy of p-milling Al2O3 is found to be 371.5 kJ/mol, a value that is much less than the reported value of the unmilled and the conventional milled Al2O3. Meanwhile, the synthesized AlN powders have unique features, such as an irregular lamp-like morphology with uniform particle distribution and fine average particle size. The results are attributed to the unique synergistic effect of p-milling, which is the effect of deformation, fracture, and cold welding of Al2O3 powders resulting from ball milling, that will be enhanced due to the introduction of discharge plasma. supported by National Natural Science Foundation of China (No. 51177008)

Influence of pH and europium concentration on the luminescent and morphological properties of Y2O3 powders

NASA Astrophysics Data System (ADS)

Esquivel-Castro, Tzipatly; Carrillo-Romo, Felipe de J.; Oliva-Uc, Jorge; García-Murillo, Antonieta; Hirata-Flores, Gustavo A.; Cayetano-Castro, Nicolás; De la Rosa, Elder; Morales-Ramírez, Angel de J.

2015-10-01

This work reports on the synthesis and characterization of Y2O3:Eu3+ powders obtained by the hydrothermal method. We studied the influence of different pH values (7-12) and Eu3+ concentrations (2.5-25 mol%) on the structural, morphological and luminescent characteristics of Y2O3:Eu3+ powders. The hydrothermal synthesis was performed at 200 °C for 12 h by employing Y2O3, HNO3, H2O and Eu (NO3)3 as precursors, in order to obtain two sets of samples. The first set of powders was obtained with different pH values and named Eu5PHx (x = 7, 8, 9, 10, 11, and 12), and the second set was obtained by using a constant pH = 7 with different Eu concentrations, named EuxPH7 (x = 2.5, 5, 8, 15, 20 and 25). The XRD spectra showed that the Y2O3:Eu3+ powders exhibited a cubic phase, regardless of the pH values and Eu3+ concentrations. The SEM observations indicated that pH influenced the morphology and size of phosphors; for instance, for pH = 7, hexagonal microplatelets were obtained, and microrods at pH values from 8 to 12. Doping Y2O3 with various Eu3+ concentrations (in mol%) also produced changes in morphology, in these cases, hexagonal microplatelets were obtained in the range of 2.5-5 mol%, and non uniform plates were observed at higher doping concentrations ranging from 8 to 25 mol%. According to our results, the microplatelets synthesized with a pH of 7 and an 8 mol% Eu3+ concentration presented the highest luminescence under excitation at 254 nm. All of these results indicate that our phosphors could be useful for applications of controlled drug delivery, photocatalysis and biolabeling.

Synthesis, characteristics and antimicrobial activity of ZnO nanoparticles

NASA Astrophysics Data System (ADS)

Janaki, A. Chinnammal; Sailatha, E.; Gunasekaran, S.

2015-06-01

The utilization of various plant resources for the bio synthesis of metallic nano particles is called green technology and it does not utilize any harmful protocols. Present study focuses on the green synthesis of ZnO nano particles by Zinc Carbonate and utilizing the bio-components of powder extract of dry ginger rhizome (Zingiber officinale). The ZnO nano crystallites of average size range of 23-26 nm have been synthesized by rapid, simple and eco friendly method. Zinc oxide nano particles were characterized by using X-ray diffraction (XRD), Scanning Electron Microscope (SEM), Energy Dispersive X-ray spectroscopy (EDX). FTIR spectra confirmed the adsorption of surfactant molecules at the surface of ZnO nanoparticles and the presence of ZnO bonding. Antimicrobial activity of ZnO nano particles was done by well diffusion method against pathogenic organisms like Klebsiella pneumonia, Staphylococcus aureus and Candida albicans and Penicillium notatum. It is observed that the ZnO synthesized in the process has the efficient antimicrobial activity.

Synthesis and characterization of titanium dioxide (TiO2) nanopowder

NASA Astrophysics Data System (ADS)

Munirah, S.; Nadzirah, Sh.; Khusaimi, Z.; Fazlena, H.; Rusop, M.

2018-05-01

Titanium dioxide (TiO2) powder was synthesized via sol-gel technique using Titanium tetraisopropoxide (TTIP) and ethanol as precursors. Acetylacetone, distilled water, polyethylene glycol (PEG) and stabilizers (glacial acetic acid and nitric acid) were then added to the solution. The solution was left for ageing for 24 hours and then dried into powder. The synthesized powders were characterized by X-ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR) and Thermogravimetric Analysis (TGA).

Metamaterial 3D Gain Nanostructures Fabricated Using Direct Laser Writing

DTIC Science & Technology

2015-07-11

oxide (PdO) and selenium powder. To avoid aggregation of the nanoparticles oleic acid and trioctylphosphine were used as stabilizing agents. The...synthesis of the PbSe quantum dots. The precursors used are CdO (Cadmium oxide) and Selenium powder and as stabilizing agent oleic acid was used. The

Reverse micelle synthesis of nanoscale metal containing catalysts. [Nickel metal (with a nickel oxide surface layer) and iron oxyhydroxide nanoscale powders

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

Darab, J.G.; Fulton, J.L.; Linehan, J.C.

1993-03-01

The need for morphological control during the synthesis of catalyst precursor powders is generally accepted to be important. In the liquefaction of coal, for example, iron-bearing catalyst precursor particles containing individual crystallites with diameters in the 1-100 nanometer range are believed to achieve good dispersion through out the coal-solvent slurry during liquefaction 2 runs and to undergo chemical transformations to catalytically active iron sulfide phases. The production of the nanoscale powders described here employs the confining spherical microdomains comprising the aqueous phase of a modified reverse micelle (MRM) microemulsion system as nanoscale reaction vessels in which polymerization, electrochemical reduction andmore » precipitation of solvated salts can occur. The goal is to take advantage of the confining nature of micelles to kinetically hinder transformation processes which readily occur in bulk aqueous solution in order to control the morphology and phase of the resulting powder. We have prepared a variety of metal, alloy, and metal- and mixed metal-oxide nanoscale powders from appropriate MRM systems. Examples of nanoscale powders produced include Co, Mo-Co, Ni[sub 3]Fe, Ni, and various oxides and oxyhydroxides of iron. Here, we discuss the preparation and characterization of nickel metal (with a nickel oxide surface layer) and iron oxyhydroxide MRM nanoscale powders. We have used extended x-ray absorption fine structure (EXAFS) spectroscopy to study the chemical polymerization process in situ, x-ray diffraction (XRD), scanning and transmission electron microcroscopies (SEM and TEM), elemental analysis and structural modelling to characterize the nanoscale powders produced. The catalytic activity of these powders is currently being studied.« less

Original Synthetic Route To Obtain a SrAl2O4 Phosphor by the Molten Salt Method: Insights into the Reaction Mechanism and Enhancement of the Persistent Luminescence.

PubMed

Rojas-Hernandez, Rocío Estefanía; Rubio-Marcos, Fernando; Gonçalves, Ricardo Henrique; Rodriguez, Miguel Ángel; Véron, Emmanuel; Allix, Mathieu; Bessada, Catherine; Fernandez, José Francisco

2015-10-19

SrAl2O4:Eu(2+), Dy(3+) has been extensively studied for industrial applications in the luminescent materials field, because of its excellent persistent luminescence properties and chemical stability. Traditionally, this strontium aluminate material is synthesized in bulk form and/or fine powder by the classic solid-state method. Here, we report an original synthetic route, a molten salt assisted process, to obtain highly crystalline SrAl2O4 powder with nanometer-scale crystals. The main advantages of salt addition are the increase of the reaction rate and the significant reduction of the synthesis temperature because of much higher mobility of reactants in the liquid medium than in the solid-state method. In particular, the formation mechanism of SrAl2O4, the role of the salt, and the phase's evolution have been explored as a function of temperature and time. Phosphorescent powders based on SrAl2O4:Eu(2+), Dy(3+) with high crystallinity are obtained after 1 h treatment at 900 °C. This work could promote further interest in adopting the molten salt strategy to process high-crystallinity materials with enhanced luminescence to design technologically relevant phosphors.

Reverse micelle synthesis of nanoscale metal containing catalysts

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

Darab, J.G.; Fulton, J.L.; Linehan, J.C.

1993-03-01

The need for morphological control during the synthesis of catalyst precursor powders is generally accepted to be important. In the liquefaction of coal, for example, iron-bearing catalyst precursor particles containing individual crystallites with diameters in the 1-100 nanometer range are believed to achieve good dispersion through out the coal-solvent slurry during liquefaction 2 runs and to undergo chemical transformations to catalytically active iron sulfide phases. The production of the nanoscale powders described here employs the confining spherical microdomains comprising the aqueous phase of a modified reverse micelle (MRM) microemulsion system as nanoscale reaction vessels in which polymerization, electrochemical reduction andmore » precipitation of solvated salts can occur. The goal is to take advantage of the confining nature of micelles to kinetically hinder transformation processes which readily occur in bulk aqueous solution in order to control the morphology and phase of the resulting powder. We have prepared a variety of metal, alloy, and metal- and mixed metal-oxide nanoscale powders from appropriate MRM systems. Examples of nanoscale powders produced include Co, Mo-Co, Ni{sub 3}Fe, Ni, and various oxides and oxyhydroxides of iron. Here, we discuss the preparation and characterization of nickel metal (with a nickel oxide surface layer) and iron oxyhydroxide MRM nanoscale powders. We have used extended x-ray absorption fine structure (EXAFS) spectroscopy to study the chemical polymerization process in situ, x-ray diffraction (XRD), scanning and transmission electron microcroscopies (SEM and TEM), elemental analysis and structural modelling to characterize the nanoscale powders produced. The catalytic activity of these powders is currently being studied.« less

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

PubMed Central

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

2017-01-01

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

Nanostructured aluminium titanate (Al{sub 2}TiO{sub 5}) particles and nanofibers: Synthesis and mechanism of microstructural evolution

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

Azarniya, Abolfazl, E-mail: abolfazl_azarniya@mehr.sharif.ir; Azarniya, Amir, E-mail: a.azarnia91@gmail.com; Hosseini, Hamid Reza Madaah, E-mail: madaah@sharif.ir

In this study, aluminium titanate (AT) particles and nanofibers were synthesized through citrate sol gel and sol gel-assisted electrospinning methods in both nanostructured powder and nanofiber forms. The results of X-ray diffraction analysis, field-emission scanning electron microscopy and differential thermal analysis showed that the synthetic products benefit a nanostructured nature with a grain size less than 70 nm. The optimal values for time and temperature at which a roughly pure AT is attained were determined as 2 h and 900 °C, respectively. It was found that the sol gel precursor bears an amorphous structure till 700 °C and begins tomore » be crystallized to alumina, anatase and AT at higher temperatures. Moreover, AT tends to decompose into rutile and alumina at temperatures higher than 900 °C and its degradation rate reaches a maximum at temperatures near to 1100 °C. In this synthesis, citric acid was used as a chelating agent for Al{sup 3} {sup +} and Ti{sup 4} {sup +} ions and it was shown that a low citric acid-to-metal cation ratio leads to larger numbers of nuclei during crystallization and smaller grain size. Finally, a model was suggested to describe the microstructural evolution of AT compound based on a nucleation and growth regime. - Graphical abstract: Display Omitted - Highlights: • We synthesized aluminium titanate ceramic in both powder and nanofiber forms. • The methods in use were citrate sol gel and sol gel-assisted electrospinning. • Powders and nanofibers bear a nanostructured nature with a grain size less than 70 nm. • A model is suggested to describe microstructural evolution of synthetic products.« less

Surfactant-assisted hydrothermal crystallization of nanostructured lithium metasilicate (Li{sub 2}SiO{sub 3}) hollow spheres: (I) Synthesis, structural and microstructural characterization

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

Ortiz-Landeros, J.; Departamento de Ingenieria Metalurgica, Escuela Superior de Ingenieria Quimica e Industrias Extractivas, IPN, UPALM, Av. Instituto Politecnico Nacional s/n, CP 07738, Mexico DF; Contreras-Garcia, M.E.

Lithium metasilicate (Li{sub 2}SiO{sub 3}) was successfully synthesized using a hydrothermal process in the presence of different surfactants with cationic, non-ionic and anionic characters. The samples obtained were compared to a sample prepared by the conventional solid-state reaction method. The structural and microstructural characterizations of different Li{sub 2}SiO{sub 3} powders were performed using various techniques. Diffraction analyses revealed the successful crystallization of pure Li{sub 2}SiO{sub 3} single phase by hydrothermal technique, even without further heat-treatments and independent of the surfactant used. Electron microscopy analyses revealed that Li{sub 2}SiO{sub 3} powders were composed of uniform micrometric particles with a hollow spheremore » morphology and nanostructured walls. Finally, different thermal analyses showed that Li{sub 2}SiO{sub 3} samples preserved their structure and microstructure after further thermal treatments. Specific aspects regarding the formation mechanism of the spherical aggregates under hydrothermal conditions are discussed, and there is a special emphasis on the effect of the synthesis pathway on the morphological characteristics. -- Graphical abstract: Li{sub 2}SiO{sub 3} was synthesized using a hydrothermal process in the presence of different surfactants. Li{sub 2}SiO{sub 3} powders were composed of uniform micrometric particles with a hollow sphere morphology and nanostructured walls. Display Omitted Highlights: {yields} Pure Li{sub 2}SiO{sub 3} was synthesized by the hydrothermal method. {yields} Surfactant addition produced microstructural and morphological variations. {yields} TEM reveled the generation of nanostructured hollow spheres.« less

Strong upconversion from Er3Al5O12 ceramic powders prepared by low temperature direct combustion synthesis

NASA Astrophysics Data System (ADS)

Maciel, Glauco S.; Rakov, Nikifor; Fokine, Michael; Carvalho, Isabel C. S.; Pinheiro, Carlos B.

2006-08-01

Crystalline ceramic powders of Er3Al5O12 were obtained by low temperature direct combustion synthesis. Irradiating the sample with a low-power continuous-wave infrared (1.48μm) diode laser led to ultraviolet, violet, blue, green, and red (380, 410, 456, 495, 525, 550, and 660nm) emissions. The strong upconversion luminescence appeared to the eyes as an intense green color. The presence of efficient four- and three-photon frequency upconversion processes makes this material an excellent candidate for use in photonic devices based on upconverter phosphors.

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.

Synthesis and characterization of NiO nanopowder by sol-gel process

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

Ningsih, Sherly Kasuma Warda

2015-09-30

Preparation of nickel oxide (NiO) nanopowder by sol-gel process has been studied. NiO nanopowders were obtained by sol-gel method by using nickel nitrate hexahydrate and sodium hydroxide and aquadest were used as precursor, agent precipitator and solvent, respectively. The powders were formed by drying at 110°C and followed by heating in the furnace at 400°C for 1.5 hours. The product was obtained black powder. The product was characterized by Energy Dispesive X-ray Fluorescence (ED-XRF), X-ray diffraction (XRD) and Scanning Electron Microscopy (SEM). The ED-XRF pattern shows the composition of NiO produced was 97.1%. The XRD pattern showed NiO forms weremore » produced generally in monoclinic stucture. The crystalline size of NiO was obtained in the range 40-85 nm. SEM micrograph clearly showed that powder had a spherical with uniform distribution size is 0.1-1.0 µm approximately.« less

Ternary and coupled binary zinc tin oxide nanopowders: Synthesis, characterization, and potential application in photocatalytic processes

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

Ivetić, T.B., E-mail: tamara.ivetic@df.uns.ac.rs; Finčur, N.L.; Đačanin, Lj. R.

2015-02-15

Highlights: • Mechanochemically synthesized nanocrystalline zinc tin oxide (ZTO) powders. • Photocatalytic degradation of alprazolam in the presence of ZTO water suspensions. • Coupled binary ZTO exhibits enhanced photocatalytic activity compared to ternary ZTO. - Abstract: In this paper, ternary and coupled binary zinc tin oxide nanocrystalline powders were prepared via simple solid-state mechanochemical method. X-ray diffraction, scanning electron microscopy, Raman and reflectance spectroscopy were used to study the structure and optical properties of the obtained powder samples. The thermal behavior of zinc tin oxide system was examined through simultaneous thermogravimetric-differential scanning calorimetric analysis. The efficiencies of ternary (Zn{sub 2}SnO{submore » 4} and ZnSnO{sub 3}) and coupled binary (ZnO/SnO{sub 2}) zinc tin oxide water suspensions in the photocatalytic degradation of alprazolam, short-acting anxiolytic of the benzodiazepine class of psychoactive drugs, under UV irradiation were determined and compared with the efficiency of pure ZnO and SnO{sub 2}.« less

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

Synthesis and characterization of CdO nano particles by the sol-gel method

NASA Astrophysics Data System (ADS)

Vadgama, V. S.; Vyas, R. P.; Jogiya, B. V.; Joshi, M. J.

2017-05-01

Cadmium Oxide (CdO) is an inorganic compound and one of the main precursors to other cadmium compounds. It finds applications in cadmium plating, storage batteries, in transparent conducting film, etc. Here, an attempt is made to synthesize CdO nano particles by sol-gel technique. The gel was prepared using cadmium nitrate tetra hydrate (Cd(NO3)2.4H2O) and aqueous ammonium hydroxide (NH4OH) as a precursor. The synthesized powder is further characterized by techniques like Powder X-ray diffraction (XRD), Transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR) and Thermal gravimetric analysis (TGA). Powder XRD analysis suggested the nano-crystalline nature of the sample with the cubic crystal system. Nano scaled particles of spherical morphology with the size ranging from 50-100 nm are observed from TEM images. While, FT-IR study is used to confirm the presence of different functional groups. Thermo-gravimetric analysis suggests the highly thermally stable nature of the samples. The results are discussed.

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.

Optimization of calcium phosphate fine ceramic powders preparation

NASA Astrophysics Data System (ADS)

Sezanova, K.; Tepavitcharova, S.; Rabadjieva, D.; Gergulova, R.; Ilieva, R.

2013-12-01

The effect of biomimetic synthesis method, reaction medium and further precursor treatments on the chemical and phase composition, crystal size and morphology of calcium phosphates was examined. Nanosized calcium phosphate precursors were biomimetically precipitated by the method of continuous precipitation in three types of reaction media at pH 8: (i) SBF as an inorganic electrolyte system; (ii) organic (glycerine) modified SBF (volume ratio of 1:1); (iii) polymer (10 g/l xanthan gum or 10 g/l guar gum) modified SBF (volume ratio of 1:1). After maturation (24 h) the samples were lyophilized, calcinated at 300°C for 3 hours, and washed with water, followed by new gelation, lyophilization and step-wise (200, 400, 600, 800, and 1000°C, each for 3 hours) sintering. The reaction medium influenced the chemical composition and particle size but not the morphology of the calcium phosphate powders. In all studied cases bi-phase calcium phosphate fine powders with well-shaped spherical grains, consisting of β-tricalcium phosphate (β-TCP) and hydroxyapatite (HA) with a Ca/P ratio of 1.3 - 1.6 were obtained. The SBF modifiers decreased the particle size of the product in the sequence guar gum ˜ xanthan gum < glycerin < SBF medium.

Stable carbonous catalyst particles and method for making and utilizing same

DOEpatents

Ganguli, Partha S.; Comolli, Alfred G.

2005-06-14

Stable carbonous catalyst particles composed of an inorganic catalytic metal/metal oxide powder and a carbonaceous binder material are formed having a basic inner substantially uniform-porous carbon coating of the catalytic powder, and may include an outer porous carbon coating layer. Suitable inorganic catalytic powders include zinc-chromite (ZnO/Cr.sub.2 03) and suitable carbonaceous liquid binders having molecular weight of 200-700 include partially polymerized furfuryl alcohol, which are mixed together, shaped and carbonized and partially oxidized at elevated temperature. Such stable carbonous catalyst particles such as 0.020-0.100 inch (0.51-2.54 mm) diameter extrudates, have total carbon content of 2-25 wt. % and improved crush strength of 1.0-5 1b/mn, 50-300 m.sup.2 /g surface area, and can be advantageously utilized in fixed bed or ebullated/fluidized bed reactor operations. This invention also includes method steps for making the stable carbonous catalyst particles having improved particle strength and catalytic activity, and processes for utilizing the active stable carbonous carbon-coated catalysts such as for syn-gas reactions in ebullated/fluidized bed reactors for producing alcohol products and Fischer-Tropsch synthesis liquid products.

Addition of CFCl 3 to Aromatic Aldehydes via in Situ Grignard Reaction

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

Barkakaty, Balaka; Talukdar, Bandana; Lokitz, Bradley

In the case of synthetic modification of trichlorofluoromethane (CFCl 3) to non-volatile and useful fluorinated precursors, we realized that it is a cost-effective and an environmentally benign strategy for the safe consumption/destruction of the ozone depleting potential of the reagent. In our report, we present a novel method for in situ Grignard reaction using magnesium powder and CFCl 3 for synthesis of dichlorofluoromethyl aromatic alcohols.

Addition of CFCl 3 to Aromatic Aldehydes via in Situ Grignard Reaction

DOE PAGES

Barkakaty, Balaka; Talukdar, Bandana; Lokitz, Bradley

2015-08-18

In the case of synthetic modification of trichlorofluoromethane (CFCl 3) to non-volatile and useful fluorinated precursors, we realized that it is a cost-effective and an environmentally benign strategy for the safe consumption/destruction of the ozone depleting potential of the reagent. In our report, we present a novel method for in situ Grignard reaction using magnesium powder and CFCl 3 for synthesis of dichlorofluoromethyl aromatic alcohols.

Synthesis and improved explosion behaviors of aluminum powders coated with nano-sized nickel film

NASA Astrophysics Data System (ADS)

Kim, Kyung Tae; Kim, Dong Won; Kim, Soo Hyung; Kim, Chang Kee; Choi, Yoon Jeong

2017-09-01

Nickel (Ni) materials with a thickness of a few hundred nm were homogeneously coated on the surfaces of aluminum (Al) powders by an electroless plating process. The Ni-coated Al powders show characteristic interfacial structures mixed of Ni, Al and O instead of densely packed Al oxide at the surface. The explosion test of the Ni-coated Al powders utilizing flame ignition showed that the powders had a 3.6 times enhanced pressurization rate of 405 kPa/ms compared to 111 kPa/ms of uncoated Al powders. It was found that this is due to a feasible diffusion of oxygen atoms into the Al powders through the thin and rough interfacial layers present at the Ni/Al interface. These results clearly indicate that nano-sized Ni film introduced instead of surface oxide acts as a very profitable layer to achieve efficient combustion behaviors by a rapid oxidation of Al powders.

Preparation, characterization and catalytic application of CoFe2O4 nanoparticles in the synthesis of benzimidazoles

NASA Astrophysics Data System (ADS)

Borade, Ravikumar M.; Shinde, Pavan R.; Kale, Swati B.; Pawar, Rajendra P.

2018-05-01

A highly efficient magnetically recoverable cobalt ferrite nano-catalyst was prepared by sol-gel autocombustion method using glycine as green fuel. The prepared material has been characterized by X-ray powder diffraction and scanning. An investigation of its catalytic activity showed it to be a heterogeneous Lewis acid catalyst for the synthesis of substituted benzimidazoles. The aqueous ethanol used as green solvent for the reaction. The nm size range of these particles facilitates the catalysis process, as an increased surface area available for the reaction. The easy separation of the catalyst by an external magnet and their recovery and reuse in next cycle reaction are additional benefits.

Synthesis and study of the synthetic hydroxyapatite doped with aluminum

NASA Astrophysics Data System (ADS)

Goldberg, M.; Smirnov, V.; Antonova, O.; Konovalov, A.; Fomina, A.; Komlev, V. S.; Barinov, S.; Rodionov, A.; Gafurov, M.; Orlinskii, S.

2018-05-01

Powders of synthetic hydroxyapatite doped with aluminium (Al) ions in concentrations 0 and 20 mol. % were synthesized by the precipitation method from the nitrate solutions and investigated by atomic emission spectrometry with inductively coupled plasma (AES-ICP), X-ray diffraction (XRD), scanning electron microscopy (SEM), gas absorption and conventional electron paramagnetic resonance (EPR). It is shown that for the chosen synthesis route an introduction of Al provokes formation of highly anisotropic phase, leads to the decrease in the crystallinity while no significant changes in the EPR spectra of the radiation-induced defects is observed. The results could be used for understanding the structural transformations with Al doping of the mineralized materials for geological and biomedical applications.

Low-cost synthesis and physical characterization of thieno[3,4-c]pyrrole-4,6-dione-based polymers.

PubMed

Berrouard, Philippe; Dufresne, Stéphane; Pron, Agnieszka; Veilleux, Justine; Leclerc, Mario

2012-09-21

The improved synthesis of thieno[3,4-c]pyrrole-4,6-dione (TPD) monomers, including Gewald thiophene ring formation, a Sandmeyer-type reaction, and neat condensation with an amine, is presented. This protocol enables faster, cheaper, and more efficient preparation of TPD units in comparison to traditional methods. Furthermore, a series of TPD homo- and pseudohomopolymers bearing various alkyl chains was synthesized via a direct heteroarylation polymerization (DHAP) procedure. UV-visible absorption and powder X-ray diffraction measurements revealed the relationship between the ratio of branched to linear alkyl chains and the optoelectronic properties of the polymers as well as their packing in the solid state.

Improved Synthesis Of Potassium Beta' '-Alumina

NASA Technical Reports Server (NTRS)

Williams, Roger M.; Jeffries-Nakamura, Barbara; Ryan, Margaret A.; O'Connor, Dennis E.; Kisor, Adam; Underwood, Mark

1996-01-01

Improved formulations of precursor materials synthesize nearly-phase-pure potassium beta' '-alumina solid electrolyte (K-BASE) powder. Materials are microhomogeneous powders (or, alternatively, gels) containing K(+,) Mg(2+), and Al(3+). K-BASE powder produced used in potassium-working-fluid alkali-metal thermal-to-electric conversion (K-AMTEC), in which heat-input and heat-rejection temperatures lower than sodium-working-fluid AMTEC (Na-AMTEC). Additional potential use lies in purification of pottassium by removal of sodium and calcium.

Comparative XRPD and XAS study of the impact of the synthesis process on the electronic and structural environments of uranium–americium mixed oxides

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

Prieur, D., E-mail: dam.prieur@gmail.com; Lebreton, F.; Martin, P.M.

2015-10-15

Uranium–americium mixed oxides are potential compounds to reduce americium inventory in nuclear waste via a partitioning and transmutation strategy. A thorough assessment of the oxygen-to-metal ratio is paramount in such materials as it determines the important underlying electronic structure and phase relations, affecting both thermal conductivity of the material and its interaction with the cladding and coolant. In 2011, various XAS experiments on U{sub 1−x}Am{sub x}O{sub 2±δ} samples prepared by different synthesis methods have reported contradictory results on the charge distribution of U and Am. This work alleviates this discrepancy. The XAS results confirm that, independently of the synthesis process,more » the reductive sintering of U{sub 1−x}Am{sub x}O{sub 2±δ} leads to the formation of similar fluorite solid solution indicating the presence of Am{sup +III} and U{sup +V} in equimolar proportions. - Graphical abstract: Formation of (U{sup IV/V},Am{sup III})O{sup 2} solid solution by sol–gel and by powder metallurgy. - Highlights: • Uranium–americium mixed oxides were synthesized by sol–gel and powder metallurgy. • Fluorite solid solutions with similar local environment have been obtained. • U{sup V} and Am{sup III} are formed in equimolar proportions.« less

Synthesis of ferrite and nickel ferrite nanoparticles using radio-frequency thermal plasma torch

NASA Astrophysics Data System (ADS)

Son, S.; Taheri, M.; Carpenter, E.; Harris, V. G.; McHenry, M. E.

2002-05-01

Nanocrystalline (NC) ferrite powders have been synthesized using a 50 kW-3 MHz rf thermal plasma torch for high-frequency soft magnet applications. A mixed powder of Ni and Fe (Ni:Fe=1:2), a NiFe permalloy powder with additional Fe powder (Ni:Fe=1:2), and a NiFe permalloy powder (Ni:Fe=1:1) were used as precursors for synthesis. Airflow into the reactor chamber was the source of oxygen for oxide formation. XRD patterns clearly show that the precursor powders were transformed into NC ferrite particles with an average particle size of 20-30 nm. SEM and TEM studies indicated that NC ferrite particles had well-defined polygonal growth forms with some exhibiting (111) faceting and many with truncated octahedral and truncated cubic shapes. The Ni content in the ferrite particles was observed to increase in going from mixed Ni and Fe to mixed permalloy and iron and finally to only permalloy starting precursor. The plasma-torch synthesized ferrite materials using exclusively the NiFe permalloy precursor had 40%-48% Ni content in the Ni-ferrite particle, differing from the NiFe2O4 ideal stoichiometry. EXAFS was used to probe the cation coordination in low Ni magnetite species. The coercivity and Neel temperature of the high Ni content ferrite sample were 58 Oe and ˜590 °C, respectively.

Structural development and kinetic analysis of PbTiO3 powders processed at low-temperature via new sol-gel approach

NASA Astrophysics Data System (ADS)

Bel-Hadj-Tahar, Radhouane; Abboud, Mohamed

2018-04-01

The synthesis of crystalline lead titanate powder by a generic low-temperature sol-gel approach is developed. Acetoin was added as ligand, instead of the commonly used alkanolamines, to ensure total dissolution of the precursor compounds. The feasibility of the acetoin-Ti isopropoxide complex as a new precursor of PbTiO3 perovskite particles via sol-gel method has been demonstrated. No excess lead has been introduced. Nanometric PbTiO3 crystallites have been formed at 400 °C under atmospheric pressure from titanium isopropoxide and lead acetate in alcoholic solution by remarkably low activation energy of crystallization process of 90 kJ mol-1. The powders show tetragonal lattice and dendritic morphology. In addition to the effect of heat-treatment temperature, time, and atmosphere, the sol chemistry particularly influenced the phase composition, particle size, and particle morphology. The use of different ligands significantly modified powder morphology. The extent of the crystallization was quantitatively evaluated by differential thermal analysis and analyzed by Johnson-Mehl-Avrami approach. The crystallization followed two rate regimes depending on the interval of the crystallized fraction.

Green biosynthesis of silver nanoparticles using Curcuma longa tuber powder

PubMed Central

Shameli, Kamyar; Ahmad, Mansor Bin; Zamanian, Ali; Sangpour, Parvanh; Shabanzadeh, Parvaneh; Abdollahi, Yadollah; Zargar, Mohsen

2012-01-01

Green synthesis of noble metal nanoparticles is a vastly developing area of research. Metallic nanoparticles have received great attention from chemists, physicists, biologists, and engineers who wish to use them for the development of a new-generation of nanodevices. In this study, silver nanoparticles were biosynthesized from aqueous silver nitrate through a simple and eco-friendly route using Curcuma longa tuber-powder extracts, which acted as a reductant and stabilizer simultaneously. Characterizations of nanoparticles were done using different methods, which included ultraviolet-visible spectroscopy, powder X-ray diffraction, transmission electron microscopy, scanning electron microscopy, energy-dispersive X-ray fluorescence spectrometry, and Fourier-transform infrared spectroscopy. The ultraviolet-visible spectrum of the aqueous medium containing silver nanoparticles showed an absorption peak at around 415 nm. Transmission electron microscopy showed that mean diameter and standard deviation for the formation of silver nanoparticles was 6.30 ± 2.64 nm. Powder X-ray diffraction showed that the particles are crystalline in nature, with a face-centered cubic structure. The most needed outcome of this work will be the development of value-added products from C. longa for biomedical and nanotechnology-based industries. PMID:23341739

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.

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

PubMed

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

2013-03-21

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

NRL Review - 2009

DTIC Science & Technology

2009-01-01

for a fundamental physical understanding of electronic properties . The Materials Processing Facility includes appa- ratuses for powder production by...situ. Facilities to process powder into bulk specimens by hot and cold isostatic pressing permit a variety of consolidation possibilities. The iso...Synthesis/ Property Measurement Facility has special emphasis on polymers, surface-film processing , and directed self-assembly. The Chemical Vapor

Synthesis and optical properties of Mg-Al layered double hydroxides precursor powders

NASA Astrophysics Data System (ADS)

Lin, Chia-Hsuan; Chu, Hsueh-Liang; Hwang, Weng-Sing; Wang, Moo-Chin; Ko, Horng-Huey

2017-12-01

The synthesis and optical properties of Mg-Al layered double hydroxide (LDH) precursor powders were investigated using X-ray diffraction (XRD), Fourier transform-infrared (FT-IR) spectroscopy, transmission electron microscopy (TEM), selected area electron diffraction (SAED), high-resolution TEM (HRTEM), UV-transmission spectrometer, and fluorescence spectrophotometer. The FT-IR results show that the intense absorption at around 1363-1377 cm-1 can be assigned to the antisymmetric ν3 mode of interlayer carbonate anions because the LDH phase contains some CO32-. The XRD results show that all of the Mg-Al LDH precursor powders contain only a single phase of [Mg0.833Al0.167(OH)2](CO3)0.083.(H2O)0.75 but have broad and weak intensities of peaks. All of Mg-Al LDHs precursor powders before calcination have the same photoluminescence (PL) spectra. Moreover, these spectra were excited at λex = 235 nm, and the broad emission band was in the range 325-650 nm. In the range, there were relatively strong intensity at around 360, 407 and 510 nm, respectively.

Stimulation of processes of self-propagating high temperature synthesis in system Ti + Al at low temperatures by influence of γ-quanta

NASA Astrophysics Data System (ADS)

Sobachkin, A. V.; Loginova, M. V.; Sitnikov, A. A.; Yakovlev, V. I.; Filimonov, V. Yu; Gradoboev, A. V.

2018-03-01

In the present work, the influence of the irradiation with gamma-quanta 60Co upon the structural and phase state of the components of the mechanically activated powder composition of Ti+Al is investigated. The phase composition, structural parameters, and crystallinity are examined by means of X-ray diffractometry. It is found out that the irradiation with gamma-quanta changes the structure of the mechanically activated powder composition. The higher irradiation dose, the higher the structure crystallinity of both components with no change in phase state. At the same time, the parameters of Ti and Al crystal lattices approach to the initial parameters observed before the mechanical activation. The irradiation with gammaquanta leads to decrease of internal stresses in the mechanically activated powder composition while nanocrystallinity of the structure remains unchanged. Using of powder compositions exposed to the irradiation with gamma-quanta for the SH-synthesis helps to increase speed of the reaction, decrease the peak firing temperature and improve homogeneity, as well as the main phase of the produced material is TiAl.

The effects of fuel type in synthesis of NiFe2O4 nanoparticles by microwave assisted combustion method

NASA Astrophysics Data System (ADS)

Karcıoğlu Karakaş, Zeynep; Boncukçuoğlu, Recep; Karakaş, İbrahim H.

2016-04-01

In this study, it was investigated the effects of the used fuels on structural, morphological and magnetic properties of nanoparticles in nanoparticle synthesis with microwave assisted combustion method with an important method in quick, simple and low cost at synthesis of the nanoparticles. In this aim, glycine, urea and citric acid were used as fuel, respectively. The synthesised nanoparticles were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), Brunauer-Emmet-Teller surface area (BET), and vibrating sample magnetometry (VSM) techniques. We observed that fuel type is quite effective on magnetic properties and surface properties of the nanoparticles. X-ray difractograms of the obtained nanoparticles were compared with standard powder diffraction cards of NiFe2O4 (JCPDS Card Number 54-0964). The results demonstrated that difractograms are fully compatible with standard reflection peaks. According to the results of the XRD analysis, the highest crystallinity was observed at nanoparticles synthesized with glycine. The results demonstrated that the nanoparticles prepared with urea has the highest surface area. The micrographs of SEM showed that all of the nanoparticles have nano-crystalline behaviour and particles indication cubic shape. VSM analysis demonstrated that the type of fuel used for synthesis is highly effective a parameter on magnetic properties of nanoparticles.

Synthesis, characterization and biological activity of Rhein-cyclodextrin conjugate

NASA Astrophysics Data System (ADS)

Liu, Manshuo; Lv, Pin; Liao, Rongqiang; Zhao, Yulin; Yang, Bo

2017-01-01

Cyclodextrin conjugate complexation is a useful method to enhance the solubility and absorption of poorly soluble drugs. A series of new Rhein-β-cyclodextrin conjugates (Rh-CD conjugates) have been synthesized and examined. Rhein is covalently linked with the β-CD by amido linkage in a 1:1 molar ratio. The conjugates were characterized by 1H NMR, 13C NMR, HRMS, powder X-ray diffraction (powder XRD) as well as thermogravimetric analysis (TGA). The results reveal that incorporation of β-CD could improve the aqueous solubility of Rhein and the cytotoxicity against hepatocellular carcinoma (HepG2) cell line as well as antibacterial activity against three organisms. The improved biological activity and the satisfactory water solubility of the conjugates will be potentially useful for developing novel drug-cyclodextrin conjugates, such as herbal medicine.

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.

Synthesis and characterization of β-Sialon powders from Si, halloysite clay and AlN powders

NASA Astrophysics Data System (ADS)

Yin, Li; Jones, Mark Ian

2017-07-01

Two β-Sialons, with z-values of 1 and 4, respectively, were successfully synthesized by silicothermal reduction and nitridation method under 0.4 MPa nitrogen pressure. The effect of firing temperatures on the phase transformations and morphologies of β-Sialons were analyzed by XRD and SEM. For β-Sialons (z = 1), the product was finally composed of targeted β-Sialon (z = 1) and secondary phase α-Si3N4; for z = 4, β-Sialon (z = 4) was the main phase, and 15R-Sialon and α-Al2O3 co-existed as secondary phases. A higher firing temperature is more beneficial for the phase transformations and crystal growth of β-Sialons, however, the most suitable firing temperature was 1400∘C.

Structural and Magnetic Properties of {Eu}(3+) Eu 3 + -Doped {CdNb}_{2} {O}_{6} CdNb 2 O 6 Powders

NASA Astrophysics Data System (ADS)

Topkaya, Ramazan; Boyraz, Cihat; Ekmekçi, Mete Kaan

2018-03-01

Europium-doped CdNb2O6 powders with the molar concentration of Eu^{3+} (0.5, 3 and 6 mol%) were successfully prepared at 900°C by using molten salt synthesis method. The effect of europium (Eu) molar concentration on the structural and temperature-dependent magnetic properties of CdNb2O6 powders has been investigated by using X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX), vibrating sample magnetometer (VSM) and ferromagnetic resonance (FMR) techniques in the temperature range of 10-300 K. XRD results confirm that all the powders have orthorhombic crystal structure. It has been confirmed from VSM and FMR measurements that Eu^{3+}-doped CdNb2O6 powders have ferromagnetic behaviour for each Eu^{3+} molar concentration between 10 and 300 K. XRD and EDX analyses indicate that there is no magnetic impurity in Eu^{3+}-doped CdNb_2O_6 powders, supporting that the ferromagnetic behaviour of the powders arises from Eu^{3+} ions. The observed ferromagnetism was elucidated with the intrinsic exchange interactions between the magnetic moments associated with the unpaired 4 f electrons in Eu^{3+} ions. The saturation magnetization decreases with increasing Eu^{3+} molar concentration. The temperature-dependent magnetization behaviour was observed not to agree with Curie-Weiss law because europium obeys Van Vleck paramagnetism. Broad FMR spectra and a g-value higher than 2 were observed from FMR measurements, indicating the ferromagnetic behaviour of the powders. It was found that while the resonance field of FMR spectra decreases, the linewidth increases as a function of Eu^{3+} molar concentration.

Research on self-propagating high temperature synthesis prepared ZrC-ZrB2 composite ceramic

NASA Astrophysics Data System (ADS)

Yong, Cheng; Xunjia, Su; Genliang, Hou; YaKun, Xing

2013-03-01

ZrC-ZrB2 composite ceramic material is prepared by self-propagating high temperature synthesis, using Zr powders, CrO2 powders and Al powders as raw materials. Samples are studied by XRD and SEM, the results show that: ZrC-ZrB2 composite ceramic is attained after self-propagating high-temperature reaction, with Zr+ B4C as the main reactive system, and which is added respectively different content (CrO3 + Al) system. The study finds that the ceramic composite products are mainly composed of ZrC and ZrB2 phase, and other subphase. Compared to the main reactive system composite ceramic, composite ceramic grains grow up obviously, after introduction of the highly exothermic system (CrO3 + Al) in the main reactive system, and with the gradual increase of the content (CrO3 + Al).

Synthesis of nano-titanium dioxide by sol-gel route

NASA Astrophysics Data System (ADS)

Kaler, Vandana; Duchaniya, R. K.; Pandel, U.

2016-04-01

Nanosized titanium dioxide powder was synthesised via sol-gel route by hydrolysis of titanium tetraisopropoxide with ethanol and water mixture in high acidic medium. The synthesized nanopowder was further characterized by X-ray Diffraction, Scanning Electron Microscopy, Fourier Transform Infrared Spectroscopy, and Ultraviolet Visible Spectroscopy in order to determine size, morphology and crystalline structure of the material. The synthesis of nano-TiO2 powder in anatase phase was realized by XRD. The optical studies of nano-TiO2 powder was carried out by UV-Vis spectroscopy and band gap was calculated as 3.5eV, The SEM results with EDAX confirmed that prepared nano-TiO2 particles were in nanometer range with irregular morphology. The FTIR analysis showed that only desired functional groups were present in sample. These nano-TiO2 particles have applications in solar cells, chemical sensors and paints, which are thrust areas these days.

Sources of Chemical Toxics and Their Precursors in Pharmaceutical Industry

DTIC Science & Technology

2001-09-01

includes a lot of independent units specialized in synthesis of active substances, their processing as pharmaceutical forms, control of intermediate and...materials (ingredients), synthesis intermediates, intermediate forms (solutions, powders), analytical reactives, drugs itself, residues etc. Secondary...specialist scenario The simplest idea is to orient the attack against chemical synthesis facilities friom where a lot of volatile solvents could be spread

Monte Carlo Simulation of Nanoparticle Encapsulation in Flames

NASA Technical Reports Server (NTRS)

Sun, Z.; Huertas, J. I.; Axelbaum, R. L.

1999-01-01

Two critical challenges facing the application of flames for synthesis of nanopowder materials are: (1) overcoming formation of agglomerates and (2) ensuring that the highly reactive nanopowders that are synthesized in flames can be produced in such a manner that their purity is maintained during subsequent processing. Agglomerates are produced in flames because particle formation occurs in a high temperature and high number density environment. They are undesirable in most advanced applications of powders. For example, agglomerates have a deleterious effect on compaction density, leading to voids when nanopowders are consolidated. Efforts to avoid agglomeration in flames without substantially reducing particle number density and, consequently, production rate, have had limited success. Powder purity must also be maintained during subsequent handling of nanopowders and this poses a significant challenge for any synthesis route because nanopowders, particularly metals and non-oxide ceramic powders, are inherently reactive. Impurities acquired during handling of nanopowders have slowed the advancement of the nanostructured materials industry. One promising approach that has been proposed to address these problems is nano-encapsulation. In this approach, the core particles are encapsulated in a removable material while they are within the flame but before excessive agglomeration has occurred. Condensation can be very rapid so that core particles are trapped within the condensed material and agglomeration is limited. Nano-encapsulation also addresses the handling concerns for post-synthesis processing. Results have shown that when nano-encapsulated powders are exposed to atmosphere the core particles are protected from oxidation and/or hydrolysis. Thus, handling of the powders does not require extreme care. If, for example, at the time of consolidation the encapsulation material is removed by vacuum annealing, the resulting powder remains unagglomerated and free of impurities. In this work, we described a novel aerosol model that has been developed to simulate particle encapsulation in flames. The model will ultimately be coupled to a one-dimensional spherical flame code and compared to results from microgravity flame experiments.

The effect of Li2CO3 substitution on synthesis of LiBOB compounds as salt of electrolyte battery lithium ion

NASA Astrophysics Data System (ADS)

Lestariningsih, Titik; Wigayati, Etty Marty; Sabrina, Qolby; Prihandoko, Bambang; Priyono, Slamet

2018-04-01

Development of the synthesis of LiB(C2O4)2 compounds continues to evolve along with the need for electrolyte salts to support the research of the manufacture of lithium ion batteries. A study had been conducted on the effect of Li2CO3 substitution on the synthesis of LiB(C2O4)2 or LiBOB compounds. LiBOB was a major candidate to replace LiPF6 as a highly toxic lithium battery electrolyte and harmful to human health. Synthesis of Lithium bis(oxalato) borate used powder metallurgy method. The raw materials used are H2C2O4.2H2O, Li2CO3 or LiOH and H2BO3 from Merck Germany products. The materials are mixed with 2: 1: 1 mol ratio until homogeneous. The synthesis of LiBOB refers to previous research, where the heating process was done gradually. The first stage heating is carried out at 120°C for 4 hours, then the next stage heating is carried out at 240°C for 7 hours. The sample variation in this study was to distinguish the lithium source from Li2CO3 and LiOH. Characterization was done by XRD to know the phase formed, FTIR to confirm that functional group of LiB(C2O4)2 compound, SEM to know the morphological structure, and TG/DTA to know the thermal properties. The results of the analysis shows that LiBOB synthesis using Lithium source from Li2CO3 has succeeded to form LiBOB compound with more LiBOB phase composition is 59.1% and 40.9% LiBOB hydrate phase, SEM morphology shows powder consist of elongated round particle porous and similar to LiBOB commercial and show higher thermal stability.

Continuous Polyol Synthesis of Metal and Metal Oxide Nanoparticles Using a Segmented Flow Tubular Reactor (SFTR).

PubMed

Testino, Andrea; Pilger, Frank; Lucchini, Mattia Alberto; Quinsaat, Jose Enrico Q; Stähli, Christoph; Bowen, Paul

2015-06-08

Over the last years a new type of tubular plug flow reactor, the segmented flow tubular reactor (SFTR), has proven its versatility and robustness through the water-based synthesis of precipitates as varied as CaCO3, BaTiO3, Mn(1-x)NixC2O4·2H2O, YBa oxalates, copper oxalate, ZnS, ZnO, iron oxides, and TiO2 produced with a high powder quality (phase composition, particle size, and shape) and high reproducibility. The SFTR has been developed to overcome the classical problems of powder production scale-up from batch processes, which are mainly linked with mass and heat transfer. Recently, the SFTR concept has been further developed and applied for the synthesis of metals, metal oxides, and salts in form of nano- or micro-particles in organic solvents. This has been done by increasing the working temperature and modifying the particle carrying solvent. In this paper we summarize the experimental results for four materials prepared according to the polyol synthesis route combined with the SFTR. CeO2, Ni, Ag, and Ca3(PO4)2 nanoparticles (NPs) can be obtained with a production rate of about 1-10 g per h. The production was carried out for several hours with constant product quality. These findings further corroborate the reliability and versatility of the SFTR for high throughput powder production.

Natural precursor based hydrothermal synthesis of sodium carbide for reactor applications

NASA Astrophysics Data System (ADS)

Swapna, M. S.; Saritha Devi, H. V.; Sebastian, Riya; Ambadas, G.; Sankararaman, S.

2017-12-01

Carbides are a class of materials with high mechanical strength and refractory nature which finds a wide range of applications in industries and nuclear reactors. The existing synthesis methods of all types of carbides have problems in terms of use of toxic chemical precursors, high-cost, etc. Sodium carbide (Na2C2) which is an alkali metal carbide is the least explored one and also that there is no report of low-cost and low-temperature synthesis of sodium carbide using the eco-friendly, easily available natural precursors. In the present work, we report a simple low-cost, non-toxic hydrothermal synthesis of refractory sodium carbide using the natural precursor—Pandanus. The formation of sodium carbide along with boron carbide is evidenced by the structural and morphological characterizations. The sample thus synthesized is subjected to field emission scanning electron microscopy (FESEM), x-ray powder diffraction (XRD), ultraviolet (UV)—visible spectroscopy, Fourier transform infrared spectroscopy (FTIR), Raman, and photoluminescent (PL) spectroscopic techniques.

Zinc oxide nanoleaves: A scalable disperser-assisted sonochemical approach for synthesis and an antibacterial application.

PubMed

Gupta, Anadi; Srivastava, Rohit

2018-03-01

Current study reports a new and highly scalable method for the synthesis of novel structure Zinc oxide nanoleaves (ZnO-NLs) using disperser-assisted sonochemical approach. The synthesis was carried out in different batches from 50mL to 1L to ensure the scalability of the method which produced almost similar results. The use of high speed (9000rpm) mechanical dispersion while bath sonication (200W, 33kHz) yield 4.4g of ZnO-NLs powder in 1L batch reaction within 2h (>96% yield). The ZnO-NLs shows an excellent thermal stability even at a higher temperature (900°C) and high surface area. The high antibacterial activity of ZnO-NLs against diseases causing Gram-positive bacteria Staphylococcus aureus shows a reduction in CFU, morphological changes like eight times reduction in cell size, cell burst, and cellular leakage at 200µg/mL concentration. This study provides an efficient, cost-effective and an environmental friendly approach for the synthesis of ZnO-NLs at industrial scale as well as new technique to increase the efficiency of the existing sonochemical method. We envisage that this method can be applied to various fields where ZnO is significantly consumed like rubber manufacturing, ceramic industry and medicine. Copyright © 2017 Elsevier B.V. All rights reserved.

Synthesis of magnesium diboride by magnesium vapor infiltration process (MVIP)

DOEpatents

Serquis, Adriana C.; Zhu, Yuntian T.; Mueller, Frederick M.; Peterson, Dean E.; Liao, Xiao Zhou

2003-01-01

A process of preparing superconducting magnesium diboride powder by heating an admixture of solid magnesium and amorphous boron powder or pellet under an inert atmosphere in a Mg:B ratio of greater than about 0.6:1 at temperatures and for time sufficient to form said superconducting magnesium diboride. The process can further include exposure to residual oxygen at high synthesis temperatures followed by slow cooling. In the cooling process oxygen atoms dissolved into MgB.sub.2 segregated to form nanometer-sized coherent Mg(B,O) precipitates in the MgB.sub.2 matrix, which can act as flux pinning centers.

Time-resolved in situ powder X-ray diffraction reveals the mechanisms of molten salt synthesis.

PubMed

Moorhouse, Saul J; Wu, Yue; Buckley, Hannah C; O'Hare, Dermot

2016-11-24

We report the first use of high-energy monochromatic in situ X-ray powder diffraction to gain unprecedented insights into the chemical processes occurring during high temperature, lab-scale metal oxide syntheses. During the flux synthesis of the n = 4 Aurivillius phase, Bi 5 Ti 3 Fe 0.5 Cr 0.5 O 15 at 950 °C in molten Na 2 SO 4 we observe the progression of numerous metastable phases. Using sequential multiphase Rietveld refinement of the time-dependent in situ XRD data, we are able to obtain mechanistic understanding of this reaction under a range of conditions.

Flash microwave synthesis and sintering of nanosized La{sub 0.75}Sr{sub 0.25}Cr{sub 0.93}Ru{sub 0.07}o{sub 3-{delta}} for fuel cell application

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

Combemale, L., E-mail: lionel.combemale@u-bourgogne.f; Caboche, G.; Stuerga, D.

2009-10-15

Perovskite-oxide nanocrystals of La{sub 0.75}Sr{sub 0.25}Cr{sub 0.93}Ru{sub 0.07}O{sub 3-{delta}} with a mean size around 10 nm were prepared by microwave flash synthesis. This reaction was performed in alcoholic solution using metallic salts, sodium ethoxide and microwave autoclave. The obtained powder was characterised after purification by energy dispersive X-ray analysis (EDX), X-ray powder diffraction (XRD), BET adsorption technique, photon correlation spectroscopy (PCS) and transmission electron microscopy (TEM). The results show that integrated perovskite-type phase and uniform particle size were obtained in the microwave treated samples. At last the synthesised powder was directly used in a sintering process. A porous solid, inmore » accordance with the expected applications, was then obtained at low sintering temperature (1000 deg. C) without use of pore forming agent. - Graphical abstract: TEM photograph of La{sub 0.75}Sr{sub 0.25}Cr{sub 0.93}Ru{sub 0.07}O{sub 3-{delta}} obtained by microwave flash synthesis. This picture confirms the nanometric size of the ceramic particles.« less

Solvent- and catalyst-free mechanochemical synthesis of alkali metal monohydrides

DOE PAGES

Hlova, Ihor Z.; Castle, Andra; Goldston, Jennifer F.; ...

2016-07-06

Alkali metal monohydrides, AH (A = Li–Cs) have been synthesized in quantitative yields at room temperature by reactive milling of alkali metals in the presence of hydrogen gas at 200 bar or less. The mechanochemical approach reported here eliminates problems associated with the malleability of alkali metals — especially Li, Na, and K — and promotes effective solid–gas reactions, ensuring their completion. This is achieved by incorporating a certain volume fraction of the corresponding hydride powder as a process control agent, which allows continuous and efficient milling primarily by coating the surface of metal particles, effectively blocking cold welding. Formationmore » of high-purity crystalline monohydrides has been confirmed by powder X-ray diffraction, solid-state NMR spectroscopy, and volumetric analyses of reactively desorbed H 2 from as-milled samples. The proposed synthesis method is scalable and particularly effective for extremely air-sensitive materials, such as alkali and alkaline earth metal hydrides. Furthermore, the technique may also be favorable for production in continuous reactors operating at room temperature, thereby reducing the total processing time, energy consumption and, hence, the cost of production of these hydrides or their derivatives and composites.« less

Operando Synchrotron X-ray Powder Diffraction and Modulated-Excitation Infrared Spectroscopy Elucidate the CO2 Promotion on a Commercial Methanol Synthesis Catalyst.

PubMed

Martin, Oliver; Mondelli, Cecilia; Cervellino, Antonio; Ferri, Davide; Curulla-Ferré, Daniel; Pérez-Ramírez, Javier

2016-09-05

Optimal amounts of CO2 are added to syngas to boost the methanol synthesis rate on Cu-ZnO-Al2 O3 in the industrial process. The reason for CO2 promotion is not sufficiently understood at the particle level due to the catalyst complexity and the high demands of characterization under true reaction conditions. Herein, we applied operando synchrotron X-ray powder diffraction and modulated-excitation infrared spectroscopy on a commercial catalyst to gain insights into its morphology and surface chemistry. These studies unveiled that Cu and ZnO agglomerate and ZnO particles flatten under CO/H2 and/or CO2 /H2 . Under the optimal CO/CO2 /H2 mixture, sintering is prevented and ZnO crystals adopt an elongated shape due to the minimal presence of the H2 O byproduct, enhancing the water-gas shift activity and thus the methanol production. Our results provide a rationale to the CO2 promotion emphasizing the importance of advanced analytical methods to establish structure-performance relations in heterogeneous catalysis. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

β-Dicalcium silicate-based cement: synthesis, characterization and in vitro bioactivity and biocompatibility studies.

PubMed

Correa, Daniel; Almirall, Amisel; García-Carrodeguas, Raúl; dos Santos, Luis Alberto; De Aza, Antonio H; Parra, Juan; Delgado, José Ángel

2014-10-01

β-dicalcium silicate (β-Ca₂ SiO₄, β-C₂ S) is one of the main constituents in Portland cement clinker and many refractory materials, itself is a hydraulic cement that reacts with water or aqueous solution at room/body temperature to form a hydrated phase (C-S-H), which provides mechanical strength to the end product. In the present investigation, β-C₂ S was synthesized by sol-gel process and it was used as powder to cement preparation, named CSiC. In vitro bioactivity and biocompatibility studies were assessed by soaking the cement samples in simulated body fluid solutions and human osteoblast cell cultures for various time periods, respectively. The results showed that the sol-gel process is an available synthesis method in order to obtain a pure powder of β-C₂ S at relatively low temperatures without chemical stabilizers. A bone-like apatite layer covered the material surface after soaking in SBF and its compressive strength (CSiC cement) was comparable with that of the human trabecular bone. The extracts of this cement were not cytotoxic and the cell growth and relative cell viability were comparable to negative control. © 2013 Wiley Periodicals, Inc.

Facile solvothermal synthesis of cube-like Ag@AgCl: a highly efficient visible light photocatalyst

NASA Astrophysics Data System (ADS)

Han, Lei; Wang, Ping; Zhu, Chengzhou; Zhai, Yueming; Dong, Shaojun

2011-07-01

In this paper, a stable and highly efficient plasmonic photocatalyst, Ag@AgCl, with cube-like morphology, has been successfully prepared via a simple hydrothermal method. Using methylene dichloride as chlorine source in the synthesis can efficiently control the morphology of Ag@AgCl, due to the low release rate of chloride ions. Scanning electron microscopy (SEM), X-ray powder diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and UV-vis diffuse reflectance spectra were used to characterize the obtained product. The photocatalytic activity of the obtained product was evaluated by the photodegradation of methyl orange (MO) under visible light irradiation, and it was found, interestingly, that Ag@AgCl exhibits high visible light photocatalytic activity and good stability.In this paper, a stable and highly efficient plasmonic photocatalyst, Ag@AgCl, with cube-like morphology, has been successfully prepared via a simple hydrothermal method. Using methylene dichloride as chlorine source in the synthesis can efficiently control the morphology of Ag@AgCl, due to the low release rate of chloride ions. Scanning electron microscopy (SEM), X-ray powder diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and UV-vis diffuse reflectance spectra were used to characterize the obtained product. The photocatalytic activity of the obtained product was evaluated by the photodegradation of methyl orange (MO) under visible light irradiation, and it was found, interestingly, that Ag@AgCl exhibits high visible light photocatalytic activity and good stability. Electronic supplementary information (ESI) available: SEM images of the AgCl samples synthesized by changing the addition amount of PVP and AgNO3. See DOI: 10.1039/c1nr10247h

Synthesis of two-dimensional titanium nitride Ti4N3 (MXene)

NASA Astrophysics Data System (ADS)

Urbankowski, Patrick; Anasori, Babak; Makaryan, Taron; Er, Dequan; Kota, Sankalp; Walsh, Patrick L.; Zhao, Mengqiang; Shenoy, Vivek B.; Barsoum, Michel W.; Gogotsi, Yury

2016-06-01

We report on the synthesis of the first two-dimensional transition metal nitride, Ti4N3-based MXene. In contrast to the previously reported MXene synthesis methods - in which selective etching of a MAX phase precursor occurred in aqueous acidic solutions - here a molten fluoride salt is used to etch Al from a Ti4AlN3 powder precursor at 550 °C under an argon atmosphere. We further delaminated the resulting MXene to produce few-layered nanosheets and monolayers of Ti4N3Tx, where T is a surface termination (F, O, or OH). Density functional theory calculations of bare, non-terminated Ti4N3 and terminated Ti4N3Tx were performed to determine the most energetically stable form of this MXene. Bare and functionalized Ti4N3 are predicted to be metallic. Bare Ti4N3 is expected to show magnetism, which is significantly reduced in the presence of functional groups.We report on the synthesis of the first two-dimensional transition metal nitride, Ti4N3-based MXene. In contrast to the previously reported MXene synthesis methods - in which selective etching of a MAX phase precursor occurred in aqueous acidic solutions - here a molten fluoride salt is used to etch Al from a Ti4AlN3 powder precursor at 550 °C under an argon atmosphere. We further delaminated the resulting MXene to produce few-layered nanosheets and monolayers of Ti4N3Tx, where T is a surface termination (F, O, or OH). Density functional theory calculations of bare, non-terminated Ti4N3 and terminated Ti4N3Tx were performed to determine the most energetically stable form of this MXene. Bare and functionalized Ti4N3 are predicted to be metallic. Bare Ti4N3 is expected to show magnetism, which is significantly reduced in the presence of functional groups. Electronic supplementary information (ESI) available. See DOI: 10.1039/c6nr02253g

Green synthesis of silver nanoparticles using cranberry powder aqueous extract: characterization and antimicrobial properties

PubMed Central

Ashour, Asmaa A; Raafat, Dina; El-Gowelli, Hanan M; El-Kamel, Amal H

2015-01-01

Background The growing threat of microbial resistance against traditional antibiotics has prompted the development of several antimicrobial nanoparticles (NPs), including silver NPs (AgNPs). In this article, a simple and eco-friendly method for the synthesis of AgNPs using the cranberry powder aqueous extract is reported. Materials and methods Cranberry powder aqueous extracts (0.2%, 0.5%, and 0.8% w/v) were allowed to interact for 24 hours with a silver nitrate solution (10 mM) at 30°C at a ratio of 1:10. The formation of AgNPs was confirmed by ultraviolet-visible spectroscopy and their concentrations were determined using atomic absorption spectroscopy. The prepared NPs were evaluated by transmission electron microscopy, measurement of ζ-potential, and Fourier-transform infrared spectroscopy. The in vitro antimicrobial properties of AgNPs were then investigated against several microbial strains. Finally, in vivo appraisal of both wound-healing and antimicrobial properties of either plain AgNPs (prepared using 0.2% extract) or AgNP-Pluronic F-127 gel was conducted in a rat model after induction of a Staphylococcus aureus ATCC 6538P wound infection. Results The formation of AgNPs was confirmed by ultraviolet-visible spectroscopy, where a surface-plasmon resonance absorption peak was observed between 432 and 438 nm. Both size and concentration of the formed AgNPs increased with increasing concentration of the extracts. The developed NPs were stable, almost spherical, and polydisperse, with a size range of 1.4–8.6 nm. The negative ζ-potential values, as well as Fourier-transform infrared spectroscopy analysis, indicated the presence of a capping agent adsorbed onto the surface of the particles. In vitro antimicrobial evaluation revealed a size-dependent activity of the AgNPs against the tested organisms. Finally, AgNPs prepared using 0.2% extract exhibited a substantial in vivo healing potential for full-thickness excision wounds in rats. Conclusion AgNPs were successfully synthesized from a silver nitrate solution through a simple green route, using cranberry powder aqueous extract as a reducing as well as capping agent. PMID:26664112

Synthesis of Cu-W nanocomposite by high-energy ball milling.

PubMed

Venugopal, T; Rao, K Prasad; Murty, B S

2007-07-01

The Cu-W bulk nanocomposites of different compositions were successfully synthesized by high-energy ball milling of elemental powders. The nanocrystalline nature of the Cu-W composite powder is confirmed by X-ray diffraction analysis, transmission electron microscopy, and atomic force microscopy. The Cu-W nanocomposite powder could be sintered at 300-400 degrees C below the sintering temperature of the un-milled Cu-W powders. The Cu-W nanocomposites showed superior densification and hardness than that of un-milled Cu-W composites. The nanocomposites also have three times higher hardness to resistivity ratio in comparison to Oxygen free high conductivity copper.

Fabrication of high-alloy powders consisting of spherical particles from ultradispersed components

NASA Astrophysics Data System (ADS)

Samokhin, A. V.; Fadeev, A. A.; Sinayskiy, M. A.; Alekseev, N. V.; Tsvetkov, Yu. V.; Arzhatkina, O. A.

2017-07-01

It is shown that powders of a model high alloy consisting of spherical particles 25-50 μm in size can be synthesized from a starting ultradispersed powder, which is made of a mixture of the alloy components and is fabricated by the magnesiothermal reduction of metal chlorides in the potassium chloride melt. The synthesis includes the stages of microgranulation of an ultradispersed powder, heat treatment of microgranules, classification of the microgranules with the separation of microgranule fraction of 25-50 μm, spheroidization of the separated fraction in a thermal plasma flow, and classification with the separation of a fraction of micro- and submicrometer-sized particles.

Study the effect of mechanical alloying parameters on synthesis of Cr{sub 2}Nb–Al{sub 2}O{sub 3} nanocomposite

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

Shayesteh, Payam, E-mail: shayesteh.payam@gmail.com; Mirdamadi, Shamseddin; Razavi, Hossein

2014-01-01

Graphical abstract: - Highlights: • Cr{sub 2}Nb–Al{sub 2}O{sub 3} nanocomposite synthesized through MA. • Effect of BPR, rotating speed, milling time and PCA concentration investigated. • After annealing at 1100 °C crystalline phase were appeared. • Williamson–Hall analysis was used in order to study the grain size of nano composite. - Abstract: In this study, Cr{sub 2}Nb–20 vol.% Al{sub 2}O{sub 3} nanocomposite was prepared successfully by mechanochemical reaction between Al, Nb and Cr{sub 2}O{sub 3} powders. Amorphization of powder occurred during mechanical alloying because of high energy collisions between powders and steel balls in milling container which transfer high degreemore » of energy to powders. Therefore, annealing was needed to form crystalline phases. The influence of different mechanical alloying parameters such as BPR, rotating speed, milling time and PCA concentration on synthesis of composite material were investigated. After mechanical alloying, the powder was encapsulated in quartz and then annealed at 1100 °C for 3 h. After annealing, 3 different phases were appeared (Cr{sub 2}Nb (cubic), Cr{sub 2}Nb (hexagonal) and α-Al{sub 2}O{sub 3}). The structural changes of powder particles during mechanical alloying were studied by X-ray diffractometry (XRD), atomic force microscopy (AFM), scanning electron microscopy (SEM) and transmission electron microscopy (TEM)« less

Application of core-shell-structured CdTe@SiO2 quantum dots synthesized via a facile solution method for improving latent fingerprint detection

NASA Astrophysics Data System (ADS)

Gao, Feng; Han, Jiaxing; Lv, Caifeng; Wang, Qin; Zhang, Jun; Li, Qun; Bao, Liru; Li, Xin

2012-10-01

Fingerprint detection is important in criminal investigation. This paper reports a facile powder brushing technique for improving latent fingerprint detection using core-shell-structured CdTe@SiO2 quantum dots (QDs) as fluorescent labeling marks. Core-shell-structured CdTe@SiO2 QDs are prepared via a simple solution-based approach using NH2NH2·H2O as pH adjustor and stabilizer, and their application for improving latent fingerprint detection is explored. The obtained CdTe@SiO2 QDs show spherical shapes with well-defined core-shell structures encapsulating different amounts of QDs depending on the type of the pH adjustor and stabilizer. Moreover, the fluorescence of CdTe@SiO2 QDs is largely enhanced by surface modification of the SiO2 shell. The CdTe@SiO2 QDs overcome the oxidation problem of pure CdTe QDs in air, thus affording better variability with strong adhesive ability, better resolution, and bright emission colors for practical application in latent fingerprint detection. In comparison with the conventional fluorescence powders, silver powders, and others, the effectiveness of CdTe@SiO2 QD powders for detection of latent fingerprints present on a large variety of object surfaces is greatly improved. The synthesis method for CdTe@SiO2 QDs is simple, cheap, and easy for large-scale production, and thus offers many advantages in the practical application of fingerprint detection.

High-Throughput Synthesis and Structure of Zeolite ZSM-43 with Two-Directional 8-Ring Channels.

PubMed

Willhammar, Tom; Su, Jie; Yun, Yifeng; Zou, Xiaodong; Afeworki, Mobae; Weston, Simon C; Vroman, Hilda B; Lonergan, William W; Strohmaier, Karl G

2017-08-07

The aluminosilicate zeolite ZSM-43 (where ZSM = Zeolite Socony Mobil) was first synthesized more than 3 decades ago, but its chemical structure remained unsolved because of its poor crystallinity and small crystal size. Here we present optimization of the ZSM-43 synthesis using a high-throughput approach and subsequent structure determination by the combination of electron crystallographic methods and powder X-ray diffraction. The synthesis required the use of a combination of both inorganic (Cs + and K + ) and organic (choline) structure-directing agents. High-throughput synthesis enabled a screening of the synthesis conditions, which made it possible to optimize the synthesis, despite its complexity, in order to obtain a material with significantly improved crystallinity. When both rotation electron diffraction and high-resolution transmission electron microscopy imaging techniques are applied, the structure of ZSM-43 could be determined. The structure of ZSM-43 is a new zeolite framework type and possesses a unique two-dimensional channel system limited by 8-ring channels. ZSM-43 is stable upon calcination, and sorption measurements show that the material is suitable for adsorption of carbon dioxide as well as methane.

Green synthesis of Pd/CuO nanoparticles by Theobroma cacao L. seeds extract and their catalytic performance for the reduction of 4-nitrophenol and phosphine-free Heck coupling reaction under aerobic conditions.

PubMed

Nasrollahzadeh, Mahmoud; Sajadi, S Mohammad; Rostami-Vartooni, Akbar; Bagherzadeh, Mojtaba

2015-06-15

We report the green synthesis of palladium/CuO nanoparticles (Pd/CuO NPs) using Theobroma cacao L. seeds extract and their catalytic activity for the reduction of 4-nitrophenol and Heck coupling reaction under aerobic conditions. The catalyst was characterized using the powder XRD, TEM, EDS, UV-vis and FT-IR. This method has the advantages of high yields, elimination of surfactant, ligand and homogeneous catalysts, simple methodology and easy work up. The catalyst can be recovered from the reaction mixture and reused several times without any significant loss of catalytic activity. Copyright © 2015 Elsevier Inc. All rights reserved.

Synthesis and characterization of Ni doped ZnO nanoparticles

NASA Astrophysics Data System (ADS)

Tamgadge, Y. S.; Gedam, P. P.; Ganorkar, R. P.; Mahure, M. A.; Pahurkar, V. G.; Muley, G. G.

2018-05-01

In this paper, we present synthesis of L-valine assisted surface modification of Ni doped ZnO nanoparticles (NPs) using chemical precipitation method. Samples were calcined at 500oC for 2h. Uncalcined and calcined samples were characterized by powder X-ray diffraction (XRD), transmission electron microscopy (TEM) and ultraviolet-visible (UV-vis) spectroscopy. Ni doped ZnO NPs with average particle size of 8 nm have been successfully obtained using L-valine as surface modifying agent. Increase in the particle size was observed after the calcination. XRD and TEM studies confirmed the purity, surface morphology and hexagonal wurtzite crystal structure of ZnO NPs. UV-vis spectroscopy indicated the blue shift of excitons absorption wavelength and surface modification by L-valine.

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.

Molten salt synthesis, visible and near-IR region spectral properties of europium or neodymium doped CoNb2O6 columbite niobate.

PubMed

Ekmekçi, Mete Kaan; Erdem, Murat; Başak, Ali Sadi

2015-03-28

Pure Nd(3+)- or Eu(3+)-doped CoNb2O6 powders have been prepared by a molten salt synthesis method using a Li2SO4-Na2SO4 or NaCl-KCl salt mixture as a flux at relatively low temperatures as compared to the solid state reaction method. X-ray diffraction patterns of pure CoNb2O6 samples indicated an orthorhombic single phase. For Eu(3+)-doped CoNb2O6 samples, the luminescence of Eu(3+) was observed at 615 nm as red emission while the Nd(3+) doped sample showed a typical emission at 1064 nm varying with the Eu(3+) or Nd(3+) doping concentrations. These luminescence characteristics of the doped samples may be attributed to the energy transfer between rare earth ions and CoO6 octahedral groups in the columbite structure.

Synthesis, characterization and electrocatalytic properties of delafossite CuGaO2

NASA Astrophysics Data System (ADS)

Ahmed, Jahangeer; Mao, Yuanbing

2016-10-01

Delafossite CuGaO2 has been employed as photocatalysts for solar cells, but their electrocatalytic properties have not been extensively studied, especially no comparison among samples made by different synthesis routes. Herein, we first reported the successful synthesis of delafossite CuGaO2 particles with three different morphologies, i.e. nanocrystalline hexagons, sub-micron sized plates and micron-sized particles by a modified hydrothermal method at 190 °C for 60 h [1-3], a sono-chemical method followed by firing at 850 °C for 48 h, and a solid state route at 1150 °C, respectively. Morphology, composition and phase purity of the synthesized samples was confirmed by powder X-ray diffraction and Raman spectroscopic studies, and then their electrocatalytic performance as active and cost effective electrode materials to the oxygen and hydrogen evolution reactions in 0.5 M KOH electrolyte versus Ag/AgCl was investigated and compared under the same conditions for the first time. The nanocrystalline CuGaO2 hexagons show enhanced electrocatalytic activity than the counterpart sub-micron sized plates and micron-sized particles.

In situ X-ray powder diffraction studies of the synthesis of graphene oxide and formation of reduced graphene oxide

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

Storm, Mie Møller, E-mail: mmst@dtu.dk; Johnsen, Rune E.; Norby, Poul

2016-08-15

Graphene oxide (GO) and reduced graphene oxide (rGO) are important materials in a wide range of fields. The modified Hummers methods, for synthesizing GO, and subsequent thermal reduction to rGO, are often employed for production of rGO. However, the mechanism behinds these syntheses methods are still unclear. We present an in situ X-ray diffraction study of the synthesis of GO and thermal reduction of GO. The X-ray diffraction revealed that the Hummers method includes an intercalation state and finally formation of additional crystalline material. The formation of GO is observed during both the intercalation and the crystallization stage. During thermalmore » reduction of GO three stages were observed: GO, a disordered stage, and the rGO stage. The appearance of these stages depends on the heating ramp. The aim of this study is to provide deeper insight into the chemical and physical processes during the syntheses. - Graphical abstract: In situ X-ray diffraction results for of the modified Hummers synthesis and the thermal reduction of graphene oxide, revealing three stages for both syntheses as well as new GO diffraction peaks and unidentified crystalline material for the Hummers synthesis and a disordered stage for the thermal reduction of graphene oxide. Display Omitted - Highlights: • Hummers synthesis consists of three stages: dissolution, intercalation and crystal. • GO is produced early on during the synthesis and display new diffraction peaks. • An unidentified triclinic phase is observed for the Hummers synthesis. • Thermal reduction of GO display three stages: GO, a disordered stage and rGO. • In situ XRD indicate reformation of rGO even for fast heated thermal reduction.« less

Adsorption dynamics of methyl violet onto granulated mesoporous carbon: Facile synthesis and adsorption kinetics.

PubMed

Kim, Yohan; Bae, Jiyeol; Park, Hosik; Suh, Jeong-Kwon; You, Young-Woo; Choi, Heechul

2016-09-15

A new and facile one-step synthesis method for preparing granulated mesoporous carbon (GMC) with three-dimensional spherical mesoporous symmetry is prepared to remove large molecular weight organic compounds in aqueous phase. GMC is synthesized in a single step using as-synthesized mesoporous carbon particles and organic binders through a simple and economical synthesis approach involving a simultaneous calcination and carbonization process. Characterization results obtained from SEM, XRD, as well as surface and porosity analysis indicate that the synthesized GMC has similar physical properties to those of the powdered mesoporous carbon and maintains the Brunauer-Emmett-Teller (BET) surface area and pore volume because the new synthesis method prevents the collapse of the pores during the granulation process. Batch adsorption experiments revealed GMC showed a substantial adsorption capacity (202.8 mg/g) for the removal of methyl violet as a target large molecular contaminant in aqueous phase. The mechanisms and dynamics modeling of GMC adsorption were also fully examined, which revealed that surface diffusion was rate limiting step on adsorption process of GMC. Adsorption kinetics of GMC enables 3 times faster than that of granular activated carbon in terms of surface diffusion coefficient. This is the first study, to the best of our knowledge, to synthesize GMC as an adsorbent for water purification by using facile granulation method and to investigate the adsorption kinetics and characteristics of GMC. This study introduces a new and simple method for the synthesis of GMC and reveals its adsorption characteristics for large molecular compounds in a water treatment. Copyright © 2016 Elsevier Ltd. All rights reserved.

Synthesis of Al4SiC4 powders from kaolin grog, aluminum and carbon black by carbothermal reaction

NASA Astrophysics Data System (ADS)

Yuan, Wenjie; Yu, Chao; Deng, Chengji; Zhu, Hongxi

2013-12-01

In this paper, the synthesis of Al4SiC4 used as natural oxide materials by carbothermal reduction was investigated in order to explore the synthesis route with low costs. The samples were calcined by using kaolin grog, aluminum and carbon black as raw materials with the selected proportion at the temperature from 1500 to 1800 ° C for 2 hours under flow argon atmosphere. The phase composition of reaction products were determined by X-ray diffraction. The microstructure and elemental composition of different phases were observed and identified by scanning electron microscopy and energy dispersive spectroscopy. The mechanism of reaction processing was discussed. The results show that Al4SiC4 powders composed of hexagonal plate-like particulates with various sizes and the thickness of less than 20 μm are obtained when the temperature reaches 1800 °C.

Characterization and microstructure of HPMC/Gly:AgNO3 polymer composites

NASA Astrophysics Data System (ADS)

Ananda, H. T.; Urs, G. Thejas; Somashekar, R.

2018-04-01

This study reports the synthesis and characterization of AgNo3 doped HPMC/Glycerol blend films. The microstructural parameters of these composites were evaluated employing whole powder pattern fitting method (WPPF) and the results obtained are related with other physical properties. AC conductivity results and optical band gap evaluated from UV/Vis studies are focused to establish structure property relations. These composite films are bio-degradable in nature and non-hazardous, this makes them very suitable candidates for applications in appropriate fields.

Starch-based polyurethane/CuO nanocomposite foam: Antibacterial effects for infection control.

PubMed

Ashjari, Hamid Reza; Dorraji, Mir Saeed Seyed; Fakhrzadeh, Vahid; Eslami, Hosein; Rasoulifard, Mohammad Hossein; Rastgouy-Houjaghan, Mehrdad; Gholizadeh, Pourya; Kafil, Hossein Samadi

2018-05-01

In the present study, a new method for the synthesis of the open cell flexible polyurethane foams (PUFs) was developed by using starch powder and the modification of closed cell foam formulation. Starch is the second largest polymeric carbohydrate as a macromolecule on this planet with a large number of glucose units. Copper oxide nanoparticles (CuO NPs) were synthesized by thermal degradation method at different temperatures of 400, 600 and 800 °C as antimicrobial agents. The antimicrobial activity of CuO NPs and commercial CuO powder against the main causes of hospital infections were tested. CuO 600 was the most effective antimicrobial agent and enhanced polymer matrix tensile strength with starch powder as new polyurethane foams (PUFs) cell opener with high tensile strength. The effects of parameters on tensile strength were optimized using response surface methodology (RSM). CuO NPs and PUF had optimal conditions and were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FT-IR). Foam synthesized at the optimal conditions had an open cell structure with high tensile strength and efficient antimicrobial activity that made them suitable to be used as an antimicrobial hospital mattress to control hospital infections. Copyright © 2018 Elsevier B.V. All rights reserved.

Low Power Resistive Oxygen Sensor Based on Sonochemical SrTi0.6Fe0.4O2.8 (STFO40)

PubMed Central

Stratulat, Alisa; Serban, Bogdan-Catalin; de Luca, Andrea; Avramescu, Viorel; Cobianu, Cornel; Brezeanu, Mihai; Buiu, Octavian; Diamandescu, Lucian; Feder, Marcel; Ali, Syed Zeeshan; Udrea, Florin

2015-01-01

The current paper reports on a sonochemical synthesis method for manufacturing nanostructured (typical grain size of 50 nm) SrTi0.6Fe0.4O2.8 (Sono-STFO40) powder. This powder is characterized using X ray-diffraction (XRD), Mössbauer spectroscopy and Scanning Electron Microscopy (SEM), and results are compared with commercially available SrTi0.4Fe0.6O2.8 (STFO60) powder. In order to manufacture resistive oxygen sensors, both Sono-STFO40 and STFO60 are deposited, by dip-pen nanolithography (DPN) method, on an SOI (Silicon-on-Insulator) micro-hotplate, employing a tungsten heater embedded within a dielectric membrane. Oxygen detection tests are performed in both dry (RH = 0%) and humid (RH = 60%) nitrogen atmosphere, varying oxygen concentrations between 1% and 16% (v/v), at a constant heater temperature of 650 °C. The oxygen sensor, based on the Sono-STFO40 sensing layer, shows good sensitivity, low power consumption (80 mW), and short response time (25 s). These performance are comparable to those exhibited by state-of-the-art O2 sensors based on STFO60, thus proving Sono-STFO40 to be a material suitable for oxygen detection in harsh environments. PMID:26205267

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

NASA Astrophysics Data System (ADS)

Ahmad, Atiqah; Razak, Khairunisak Abdul

2017-07-01

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

Synthesis of nano-sized ZnO particles by co-precipitation method with variation of heating time

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

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

Zinc oxide powders have been synthesized by a co-precipitation method at low temperature (85 °C), using zinc acetate dihydrate, ammonia, hydrochloric acid solutions as the reactants. A number of process parameters such as reaction temperature, solution basicity or pH and heating time are the main factors affecting the morphology and physical properties of the ZnO nanostructures. In this work the effect of heating time on the morphology and particles size were studied. The as-synthesized ZnO powders were characterized using transmission electron microscopy (TEM) and X-ray diffraction (XRD) techniques. The samples were also analyzed using Fourier transform infrared (FTIR). Rietveld refinementmore » of XRD data confirms that ZnO crystallizes in the hexagonal wurtzite structure with high degree of purity and the (101) plane predominant. The XRD results show that the average crystallite sizes were about 66, 27 and 12 nm for 3, 4 and 5 h of heating times, respectively. The XRD analysis indicated that a fraction of nano-sized ZnO powders were in the form of aggregates, which was also verified by TEM image. The TEM photograph demonstrated that the nano-sized ZnO particles were a pseudo-spherical shape.« less

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.

Synthesis and characterization of a prominent NLO active MOF of lead with 1,5-naphthalenedisulfonic acid

NASA Astrophysics Data System (ADS)

Prasad, S. Shibu; Sudarsanakumar, M. R.; Dhanya, V. S.; Suma, S.; Kurup, M. R. Prathapachandra

2018-09-01

A new metal-organic framework of lead, [Pb(1,5-nds)(H2O)3]n (1,5-nds = 1,5-naphthalenedisulfonate) having prominent nonlinear optical property has been prepared by single gel diffusion technique at ambient condition using sodium metasilicate. The second harmonic generation efficiency was analyzed using Kurtz and Perry powder method and was found to be 30 times as large as potassium dihydrogen phosphate (KDP). Single crystal X-ray diffraction studies reveal the crystal structure. The grown crystals were further characterized by elemental analysis, powder XRD study, thermogravimetry, FT-IR and UV-visible spectral studies. The Pb2S2O4 rings in the crystal structure form a 1D channel. Hydrogen bonding and π-π interactions provide additional stability to the compound. Photoluminescence studies were also carried out.

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.

Alternative route for the preparation of CoSb{sub 3} and Mg{sub 2}Si derivatives

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

Godlewska, E., E-mail: godlewsk@agh.edu.pl; Mars, K.; Zawadzka, K.

2012-09-15

An alternative manufacturing route has been developed for cobalt triantimonide and magnesium disilicide derivatives. Elemental powders were mixed in stoichiometric proportions, cold pressed into cylindrical preforms and heated in oxygen-free environment to initiate the exothermic reaction. According to DTA/TG measurements and observations under high-temperature microscope, the onset of reaction occurred at a temperature not exceeding the melting point of the more volatile component, i.e. antimony in the case of CoSb{sub 3} and magnesium in the case of Mg{sub 2}Si. The reaction products were additionally heat treated to secure homogenization. Dense sinters were obtained by hot uniaxial pressing of the obtainedmore » powders in moderate temperature-and-pressure conditions. Several advantages were identified in the proposed technology: absence of liquid phases, relatively short time of the synthesis, possibility of in-situ or ex-situ doping and grain size control. - Graphical abstract: (1) Manufacturing flow sheet for CoSb{sub 3} (milling included) and Mg{sub 2}Si (no milling). (2) Micrographs of CoSb{sub 3} product. (3) Micrographs of Mg{sub 2}Si product. Highlights: Black-Right-Pointing-Pointer The combustion synthesis followed by HP was used for the manufacturing of CoSb{sub 3} or Mg{sub 2}Si. Black-Right-Pointing-Pointer The time of reaction is shorter compared with many other synthesis methods. Black-Right-Pointing-Pointer The process is scalable and practically wasteless.« less

The properties of LaSrМnO3 powders synthesized at various regimes

NASA Astrophysics Data System (ADS)

Mikhailov, M.; Sokolovskiy, A.; Vlasov, V.; Smolin, A.

2017-09-01

For the first time the concentration of ferromagnetic and paramagnetic phases in LaSrMnO3 compounds has been defined using diffuse reflection and absorption spectra in the visible and near-infrared regions. The compounds as powders were synthesized by heating La2O3/SrCO3/МnСO3 mixtures at 1200 °C which is less than their sintering temperature. The possibility to obtain LaSrMnO3 powders by solid state synthesis for smart coatings was shown.

Nonequiatomic NiTi Alloy Produced by Self Propagating High Temperature Synthesis

NASA Astrophysics Data System (ADS)

Bassani, P.; Bassani, E.; Tuissi, A.; Giuliani, P.; Zanotti, C.

2014-07-01

Shape memory alloy NiTi in porous form is of high interest as implantable material, as low apparent elastic modulus, comparable to that of bone, can be achieved. This condition, combined with proper pore size, allows good osteointegration. Porous NiTi can be produced by self propagating high temperature synthesis (SHS), starting from mixed powders of pure Ni and Ti. Process parameters, among which powder compaction degree and preheating temperature, strongly influence the reaction temperature and the resulting product: at low reaction temperatures, high quantity of secondary phases are formed, which are generally considered detrimental for biocompatibility. On the contrary, at higher reaction temperatures, the powders melt and crystallize in ingots. The porous structure is lost and huge pores are formed. Mechanical activation of powders through ball milling and addition of TiH x are investigated as means to reduce reaction temperature and overheating, in order to preserve high porosity and limit secondary phases content. Both processes affect SHS reaction, and require adjustment of parameters such as heating rate. Changes in porous shape and size were observed especially for TiH x additions: the latter could be a promising route to obtain shaped porous products of improved quality.

Environmentally friendly ultrosound synthesis and antibacterial activity of cellulose/Ag/AgCl hybrids.

PubMed

Dong, Yan-Yan; Deng, Fu; Zhao, Jin-Jin; He, Jing; Ma, Ming-Guo; Xu, Feng; Sun, Run-Cang

2014-01-01

This study aims to investigate the fabrication and property of cellulose/Ag/AgCl hybrids. In this article, preparation of cellulose/Ag/AgCl hybrids was reported using the cellulose solution, AgNO₃, AlCl₃·6H₂O with ultrasound agitation method. The cellulose solution was synthesized by the dissolution of the microcrystalline cellulose in NaOH/urea aqueous solution. Influences of the experimental parameters of ultrasound treatment time and ultrasonic intermittent on the hybrids were investigated. The phase, microstructure, thermal stability, and morphology of the hybrids were characterized by X-ray powder diffraction (XRD), Fourier transform infrared (FTIR) spectrometry, thermogravimetric analysis (TGA), differential thermal analysis (DTA), and scanning electron microscopy (SEM). Results showed the successful synthesis of cellulose/Ag/AgCl hybrids with good thermal stability. Moreover, the hybrids displayed desirable antimicrobial activities. Compared with other conventional methods, the rapid, green, and environmentally friendly ultrasound agitation method opens a new window to the high value-added applications of biomass. Copyright © 2013 Elsevier Ltd. All rights reserved.

Preparation and characterization of hydroxyapatite/sodium alginate biocomposites for bone implant application

NASA Astrophysics Data System (ADS)

Kanasan, Nanthini; Adzila, Sharifah; Suid, Mohd Syafiq; Gurubaran, P.

2016-07-01

In biomedical fields, synthetic scaffolds are being improved by using the ceramics, polymers and composites materials to avoid the limitations of allograft. Ceramic-polymer composites are appearing to be the most successful bone graft substitute in human body. The natural bones itself are well-known as composite of collagen and hydroxyapatite. In this research, precipitation method was used to synthesis hydroxyapatite (HA)/sodium alginate (SA) in various parameters. This paper describes the hydroxyapatite/sodium alginate biocomposite which suitable for use in bone defects or regeneration of bone through the characterizations which include FTIR, FESEM, EDS and DTA. In FTIR, the characteristi peaks of PO4-3 and OH- groups which corresponding to hydroxyapatite are existed in the mixing powders. The needle-size particle of hydroxyapatite/ alginate (HA/SA) are observed in FESEM in the range of 15.8nm-38.2nm.EDS confirmed the existence of HA/SA composition in the mixing powders. There is an endothermic peak which corresponds to the dehydration and the loss of physically adsorbed water molecules of the hydroxyapatite (HA)/sodium alginate (SA) powder which are described in DTA.

Synthesis of TiO{sub 2} by electrochemical method from TiCl{sub 4} solution as anode material for lithium-ion batteries

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

Nur, Adrian, E-mail: adriannur@staff.uns.ac.id; Purwanto, Agus; Jumari, Arif

Metal oxide combined with graphite becomes interesting composition. TiO{sub 2} is a good candidate for Li ion battery anode because of cost, availability of sufficient materials, and environmentally friendly. TiO{sub 2} gravimetric capacity varied within a fairly wide range. TiO{sub 2} crystals form highly depends on the synthesis method used. The electrochemical method is beginning to emerge as a valuable option for preparing TiO{sub 2} powders. Using the electrochemical method, the particle can easily be controlled by simply adjusting the imposed current or potential to the system. In this work, the effects of some key parameters of the electrosynthesis onmore » the formation of TiO{sub 2} have been investigated. The combination of graphite and TiO{sub 2} particle has also been studied for lithium-ion batteries. The homogeneous solution for the electrosynthesis of TiO{sub 2} powders was TiCl{sub 4} 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 a distance of 2.6 cm between the electrodes and 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. The electrosynthesis was performed galvanostatically at 0.5 to 2.5 hours and voltages were varied from 8 to 12 V under constant stirring at room temperature. The resulted suspension was aged at 48 hrs, filtered, dried directly in an oven at 150°C for 2 hrs, washed 2 times, and dried again 60 °C for 6 hrs. The particle product has been used to lithium-ion battery as anode. Synthesis of TiO{sub 2} particle by electrochemical method at 10 V for 1 to 2.5 hrs resulted anatase and rutile phase.« less

Hydrothermal Synthesis and Characterization of a Metal-Organic Framework by Thermogravimetric Analysis, Powder X-Ray Diffraction, and Infrared Spectroscopy: An Integrative Inorganic Chemistry Experiment

ERIC Educational Resources Information Center

Crane, Johanna L.; Anderson, Kelly E.; Conway, Samantha G.

2015-01-01

This advanced undergraduate laboratory experiment involves the synthesis and characterization of a metal-organic framework with microporous channels that are held intact via hydrogen bonding of the coordinated water molecules. The hydrothermal synthesis of Co[subscript 3](BTC)[subscript 2]·12H[subscript 2]O (BTC = 1,3,5-benzene tricarboxylic acid)…

Effect of acidity on the citrate-nitrate combustion synthesis of alumina-zirconia composite powder

NASA Astrophysics Data System (ADS)

Chandradass, J.; Kim, Ki Hyeon

2009-12-01

Alumina-zirconia composite powders were produced by sol-gel autocombustion. 20 wt.% ZrO2-Al2O3 mixture precursor solutions were chelated by citric acid ions at different pH. DTA analysis shows sluggish decomposition at low pH, whereas there was rapid decomposition at high pH = 9. XRD patterns of the calcined powders showed that well crystallized powder with 100 % tetragonal phase and α-alumina phase is produced when pH = 0.58 (without ammonia addition). TEM characterization of composite powders revealed homogenous distribution of nanosized zirconia particles in the alumina matrix. FTIR analysis shows peaks at 590 cm-1 and 454 cm-1, which are identified as the characteristic absorption bands of Zr-O and Al-O.

Magnetically responsive enzyme powders

NASA Astrophysics Data System (ADS)

Pospiskova, Kristyna; Safarik, Ivo

2015-04-01

Powdered enzymes were transformed into their insoluble magnetic derivatives retaining their catalytic activity. Enzyme powders (e.g., trypsin and lipase) were suspended in various liquid media not allowing their solubilization (e.g., saturated ammonium sulfate and highly concentrated polyethylene glycol solutions, ethanol, methanol, 2-propanol) and subsequently cross-linked with glutaraldehyde. Magnetic modification was successfully performed at low temperature in a freezer (-20 °C) using magnetic iron oxides nano- and microparticles prepared by microwave-assisted synthesis from ferrous sulfate. Magnetized cross-linked enzyme powders were stable at least for two months in water suspension without leakage of fixed magnetic particles. Operational stability of magnetically responsive enzymes during eight repeated reaction cycles was generally without loss of enzyme activity. Separation of magnetically modified cross-linked powdered enzymes from reaction mixtures was significantly simplified due to their magnetic properties.

Microgravity Production of Nanoparticles of Novel Materials Using Plasma Synthesis

NASA Technical Reports Server (NTRS)

Frenklach, Michael; Fernandez-Pello, Carlos

2001-01-01

The research goal is to study the formation in reduced gravity of high quality nanoparticulate of novel materials using plasma synthesis. Particular emphasis will be placed on the production of powders of non-oxide materials like diamond, SiC, SiN, c-BN, etc. The objective of the study is to investigate the effect of gravity on plasma synthesis of these materials, and to determine how the microgravity synthesis can improve the quality and yield of the nanoparticles. It is expected that the reduced gravity will aid in the understanding of the controlling mechanisms of plasma synthesis, and will increase the yield, and quality of the synthesized powder. These materials have properties of interest in several industrial applications, such as high temperature load bearings or high speed metal machining. Furthermore, because of the nano-meter size of the particulate produced in this process, they have specific application in the fabrication of MEMS based combustion systems, and in the development and growth of nano-systems and nano-structures of these materials. These are rapidly advancing research areas, and there is a great need for high quality nanoparticles of different materials. One of the primary systems of interest in the project will be gas-phase synthesis of nanopowder of non-oxide materials.

Synthesis of platinum nanoparticles using dried Anacardium occidentale leaf and its catalytic and thermal applications.

PubMed

Sheny, D S; Philip, Daizy; Mathew, Joseph

2013-10-01

An environment friendly approach for the synthesis of Pt nanoparticles (NPs) using dried leaf powder of Anacardium occidentale is reported. The formation of Pt NPs is monitored using UV-Vis spectrophotometer. FTIR spectra reveal that proteins are bound to Pt nanoparticles. TEM images show irregular rod shaped particles which are crystalline. The quantity of leaf powder plays a vital role in determining the size of particles. Synthesized NPs exhibit good catalytic activity in the reduction of aromatic nitrocompound. The effective thermal conductivity of synthesized Pt/water nanofluid has been measured and found to be enhanced to a good extent. Copyright © 2013 Elsevier B.V. All rights reserved.

Magnetic and magneto elastic properties of cobalt ferrite ceramic compacted through cold isostatic pressing

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

Indla, Srinivas; Das, Dibakar, E-mail: ddse@uohyd.ernet.in; Chelvane, Arout

2016-05-06

Nano crystalline CoFe{sub 2}O{sub 4} powder was prepared by combustion synthesis method. As synthesized powder was calcined at an appropriate condition to remove the impurities and to promote phase formation. Phase pure CoFe{sub 2}O{sub 4} powder was pressed into cylindrical rod at an applied pressure of 200 MPa using a cold isostatic pressing. Sintering of the green compact at 1350°c for 12 hrs resulted in sintered cylindrical rod with ~85% of the theoretical density. Single phase cubic spinel structure was observed in the powder x-ray diffraction pattern of the sintered pellet. Scanning electron micrographs (SEM) of the as sintered pelletmore » revealed the microstructure to be composed of ferrite grains of average size ~4 µm. Saturation magnetization of 72 emu/g and coercivity of 355 Oe were observed for cobalt ferrite sample. The magnetostriction was measured on a circular disc (12 mm diameter and 12 mm length) with the strain gauge (350 Ω) mounted on the flat surface of the circular disc. Magnetostriciton of 180 ppm and strain derivative of 1 × 10{sup −9} m/A were observed for the sintered CoFe{sub 2}O{sub 4} sample.« less

Synthesis of fluorapatite–hydroxyapatite nanoparticles and toxicity investigations

PubMed Central

Montazeri, N; Jahandideh, R; Biazar, Esmaeil

2011-01-01

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

Solid-state synthesis of YAG powders through microwave coupling of oxide/carbon particulate mixtures

DOE PAGES

Wildfire, Christina; Sabolsky, Edward M.; Spencer, Michael J.; ...

2017-06-14

The rapid synthesis of yttrium aluminum garnet (Y 3Al 15O 12, YAG) powder was investigated through the use of microwave irradiation of the oxide precursor system. For this investigation, an external hybrid heating source was not used. Instead, the rapid heating of the precursor materials (yttria and alumina powders, which are typically transparent to 2.45 GHz microwaves) was initiated by mixing an intrinsic absorbing material (carbon) into the original oxide precursors. The effect of the carbon characteristics, such as carbon source, concentration, particle size, and agglomerate microstructure were evaluated on the efficiency of coupling and resultant oxide reaction. The microwavemore » power was varied to optimize the YAG conversion and eliminate intermediate phase formation. Interactions between the conductive carbon particles and the dielectric oxides within the microwave exposure produced local arching and micro-plasma formation within the powder bed, resulting in the rapid formation of the refractory YAG composition. This optimal conduction led to temperatures of 1000°C that could be achieved in less than 5 min resulting in the formation of > 90 vol% YAG. The understanding of a conductor/dielectric particulate system here, provided insight into possible application of similar systems where microwave irradiation could be used for enhanced solid-state formation, local melting events, and gas phase reactions with a composite powder media.« less

Gas-to-particle conversion in the particle precipitation-aided chemical vapor deposition process II. Synthesis of the perovskite oxide yttrium chromite

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

Dieten, V.E.J. van; Dekker, J.P.; Hurkmans, E.J.

1993-11-01

In the particle precipitation-aided chemical vapor deposition process, an aerosol is formed in the gas phase at elevated temperatures. The particles are deposited on a cooled substrate. Coherent layers with a controlled porosity can be obtained by a simultaneous heterogeneous reaction, which interconnects the deposited particles. The synthesis of submicrometer powder of the perovskite oxide yttrium chromite (YCrO[sub 3]) by gas to particle conversion, which is the first step of the PP-CVD process, has been investigated, and preliminary results are shown. The powders have been synthesized using yttrium trichloride vapor (YCl[sub 3]), chromium trichloride vapor (CrCl[sub 3]), and steam andmore » oxygen as reactants. The influence of the input molar ratio of the elements on the composition and characteristics of the powders has been investigated. Phase composition has been determined by X-ray diffraction (XRD). The powders have been characterized by transmission electron microscopy (TEM) and sedimentation field flow fractionation (SF[sup 3]). At a reaction temperature of 1283 K the powders consist of the chromium sesquioxide (Cr[sub 2]O[sub 3]), or a mixture of Cr[sub 2]O[sub 3] and YCrO[sub 3]. At stoichiometeric input amounts of metal chlorides and steam the formation of YCrO[sub 3] seems to be favored. 19 refs., 6 figs., 3 tabs.« less

Orthogonal test design for optimization of synthesis of MTX/LDHs hybrids by ion-exchange method

NASA Astrophysics Data System (ADS)

Liu, Su-Qing; Dai, Chao-Fan; Wang, Lin; Li, Shu-Ping; Li, Xiao-Dong

2015-04-01

Based on orthogonal test design, the factors influencing the synthesis of methotrexate intercalated magnesium-aluminum layered double hydroxides (MTX/LDHs for short) by ion-exchange method, such as weight ratio of pristine LDHs to MTX (R for short), exchange temperature, time and pH value were investigated. Of the four controllable independent variables, R had the strongest effect on the crystallinity and the drug-loading capacity and the optimum synthesis conditions considered from the crystallinity and the drug-loading capacity both pointed to the same values, i.e., R=2:1, pH=9.5, temperature of 80 °C and exchange time of 3 day. The XRD diffractions indicated that high MTX content was in favor of the formation of intercalated hybrids, while low content lead to the failure of it. TEM photos indicated that the intercalated hybrids all exhibited aggregated hexagonal plates. In order to improve the morphology, two different states of pristine LDHs, i.e., powder and colloid, were chosen to prepare MTX/LDHs hybrids and the results indicated that colloid state of pristine was advantageous to obtain regular particles. The study also revealed that the properties of hybrids obtained at optimum conditions by ion-exchange were superior to that obtained from standard methods, such as co-precipitation method.

Direct and continuous synthesis of VO2 nanoparticles

NASA Astrophysics Data System (ADS)

Powell, M. J.; Marchand, P.; Denis, C. J.; Bear, J. C.; Darr, J. A.; Parkin, I. P.

2015-11-01

Monoclinic VO2 nanoparticles are of interest due to the material's thermochromic properties, however, direct synthesis routes to VO2 nanoparticles are often inaccessible due to the high synthesis temperatures or long reaction times required. Herein, we present a two-step synthesis route for the preparation of monoclinic VO2 nanoparticles using Continuous Hydrothermal Flow Synthesis (CHFS) followed by a short post heat treatment step. A range of particle sizes, dependent on synthesis conditions, were produced from 50 to 200 nm by varying reaction temperatures and the residence times in the process. The nanoparticles were characterised by powder X-ray diffraction, Raman and UV/Vis spectroscopy, transmission electron microscopy (TEM), scanning electron microscopy (SEM) and differential scanning calorimetry (DSC). The nanoparticles were highly crystalline with rod and sphere-like morphologies present in TEM micrographs, with the size of both the rod and spherical particles being highly dependent on both reaction temperature and residence time. SEM micrographs showed the surface of the powders produced from the CHFS process to be highly uniform. The samples were given a short post synthesis heat treatment to ensure that they were phase pure monoclinic VO2, which led to them exhibiting a large and reversible switch in optical properties (at near-IR wavelengths), which suggests that if such materials can be incorporated into coatings or in composites, they could be used for fenestration in architectural applications.

Direct and continuous synthesis of VO2 nanoparticles.

PubMed

Powell, M J; Marchand, P; Denis, C J; Bear, J C; Darr, J A; Parkin, I P

2015-11-28

Monoclinic VO2 nanoparticles are of interest due to the material's thermochromic properties, however, direct synthesis routes to VO2 nanoparticles are often inaccessible due to the high synthesis temperatures or long reaction times required. Herein, we present a two-step synthesis route for the preparation of monoclinic VO2 nanoparticles using Continuous Hydrothermal Flow Synthesis (CHFS) followed by a short post heat treatment step. A range of particle sizes, dependent on synthesis conditions, were produced from 50 to 200 nm by varying reaction temperatures and the residence times in the process. The nanoparticles were characterised by powder X-ray diffraction, Raman and UV/Vis spectroscopy, transmission electron microscopy (TEM), scanning electron microscopy (SEM) and differential scanning calorimetry (DSC). The nanoparticles were highly crystalline with rod and sphere-like morphologies present in TEM micrographs, with the size of both the rod and spherical particles being highly dependent on both reaction temperature and residence time. SEM micrographs showed the surface of the powders produced from the CHFS process to be highly uniform. The samples were given a short post synthesis heat treatment to ensure that they were phase pure monoclinic VO2, which led to them exhibiting a large and reversible switch in optical properties (at near-IR wavelengths), which suggests that if such materials can be incorporated into coatings or in composites, they could be used for fenestration in architectural applications.

Synthesis and Characterization of Functionalized Metal-organic Frameworks

PubMed Central

Karagiaridi, Olga; Bury, Wojciech; Sarjeant, Amy A.; Hupp, Joseph T.; Farha, Omar K.

2014-01-01

Metal-organic frameworks have attracted extraordinary amounts of research attention, as they are attractive candidates for numerous industrial and technological applications. Their signature property is their ultrahigh porosity, which however imparts a series of challenges when it comes to both constructing them and working with them. Securing desired MOF chemical and physical functionality by linker/node assembly into a highly porous framework of choice can pose difficulties, as less porous and more thermodynamically stable congeners (e.g., other crystalline polymorphs, catenated analogues) are often preferentially obtained by conventional synthesis methods. Once the desired product is obtained, its characterization often requires specialized techniques that address complications potentially arising from, for example, guest-molecule loss or preferential orientation of microcrystallites. Finally, accessing the large voids inside the MOFs for use in applications that involve gases can be problematic, as frameworks may be subject to collapse during removal of solvent molecules (remnants of solvothermal synthesis). In this paper, we describe synthesis and characterization methods routinely utilized in our lab either to solve or circumvent these issues. The methods include solvent-assisted linker exchange, powder X-ray diffraction in capillaries, and materials activation (cavity evacuation) by supercritical CO2 drying. Finally, we provide a protocol for determining a suitable pressure region for applying the Brunauer-Emmett-Teller analysis to nitrogen isotherms, so as to estimate surface area of MOFs with good accuracy. PMID:25225784

Sol-gel synthesis of red-phosphors [Na xGd 1-x/3-zEu z]Mo yW 1-yO 4 powers and luminescence properties

NASA Astrophysics Data System (ADS)

Cao, Fa-Bin; Li, Liao-Sha; Tian, Yan-Wen; Gao, Zhi-Fang; Chen, Yong-Jie; Xiao, Lin-Jiu; Wu, Xing-Rong

2011-04-01

In this work, we report on the sol-gel synthesis of red-phosphors [Na xGd 1-x/3-zEu z]Mo yW 1-yO 4 powders doped with several dopants and its luminescence properties at room temperature. X-ray diffraction patters indicated that red-phosphors powders present tetragonal symmetry and cubic structure. The red-phosphors [Na xGd 1-x/3-zEu z]Mo yW 1-yO 4 powders doped exhibit characteristic of a ultraviolet visible-light emission diode. The SEM images for [ NaGdEu0.043+]Mo 0.4W 0.6O 4 phosphor exhibits irregular morphology and cottonlike shape. The size of the particles is estimated to be about 1 μm. Luminescence properties showed that the maximum emission in red region lies in the arrange of 613 nm and 617 nm.

Synthesis of nano-titanium dioxide by sol-gel route

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

Kaler, Vandana, E-mail: vandana.kaler@gmail.com; Duchaniya, R. K.; Pandel, U.

Nanosized titanium dioxide powder was synthesised via sol-gel route by hydrolysis of titanium tetraisopropoxide with ethanol and water mixture in high acidic medium. The synthesized nanopowder was further characterized by X-ray Diffraction, Scanning Electron Microscopy, Fourier Transform Infrared Spectroscopy, and Ultraviolet Visible Spectroscopy in order to determine size, morphology and crystalline structure of the material. The synthesis of nano-TiO{sub 2} powder in anatase phase was realized by XRD. The optical studies of nano-TiO{sub 2} powder was carried out by UV-Vis spectroscopy and band gap was calculated as 3.5eV, The SEM results with EDAX confirmed that prepared nano-TiO{sub 2} particles weremore » in nanometer range with irregular morphology. The FTIR analysis showed that only desired functional groups were present in sample. These nano-TiO{sub 2} particles have applications in solar cells, chemical sensors and paints, which are thrust areas these days.« less

Synthesis and characterization of thermally evaporated Cu2SnSe3 ternary semiconductor

NASA Astrophysics Data System (ADS)

Hamdani, K.; Chaouche, M.; Benabdeslem, M.; Bechiri, L.; Benslim, N.; Amara, A.; Portier, X.; Bououdina, M.; Otmani, A.; Marie, P.

2014-11-01

Copper Tin Selenide (CuSnSe) powder was mechanically alloyed by high energy planetary ball milling, starting from elemental powders. Synthesis time and velocity have been optimized to produce Cu2SnSe3 materials. Thin films were prepared by thermal evaporation on Corning glass substrate at Ts = 300 °C. The structural, compositional, morphological and optical properties of the synthesized semiconductor have been analyzed by X-ray diffraction (XRD), energy dispersive X-ray analysis (EDAX), scanning electron microscopy (SEM) and transmission electron microscopy. The analyzed powder exhibited a cubic crystal structure, with the presence of Cu2Se as a secondary phase. On the other hand, the deposited films showed a cubic Cu2SnSe3 ternary phase and extra peaks belonging to some binary compounds. Furthermore, optical measurements showed that the deposited layers have a relatively high absorption coefficient of 105 cm-1 and present a band gap of 0.94 eV.

Synthesis of nanoscale magnesium diboride powder

NASA Astrophysics Data System (ADS)

Finnemore, D. K.; Marzik, J. V.

2015-12-01

A procedure has been developed for the preparation of small grained magnesium diboride (MgB2) powder by reacting nanometer size boron powder in a magnesium vapor. Plasma synthesized boron powder that had particle sizes ranging from 20 to 300nm was mixed with millimeter size chunks of Mg by rolling stoichiometric amounts of the powders in a sealed cylindrical container under nitrogen gas. This mixture then was placed in a niobium reaction vessel, evacuated, and sealed by e-beam welding. The vessel was typically heated to approximately 830°C for several hours. The resulting MgB2 particles have a grain size in the 200 nm to 800 nm range. Agglomerates of loosely bound particles could be broken up by light grinding in a mortar and pestle. At 830°C, many particles are composed of several grains grown together so that the average particle size is about twice the average grain size. Experiments were conducted primarily with undoped boron powder, but carbon-doped boron powder showed very similar results.

Preparation of Mo-Re-C samples containing Mo7Re13C with the β-Mn-type structure by solid state reaction of planetary-ball-milled powder mixtures of Mo, Re and C, and their crystal structures and superconductivity

NASA Astrophysics Data System (ADS)

Oh-ishi, Katsuyoshi; Nagumo, Kenta; Tateishi, Kazuya; Takafumi, Ohnishi; Yoshikane, Kenta; Sugiyama, Machiko; Oka, Kengo; Kobayashi, Ryota

2017-01-01

Mo-Re-C compounds containing Mo7Re13C with the β-Mn structure were synthesized with high-melting-temperature metals Mo, Re, and C powders using a conventional solid state method with a planetary ball milling machine instead of the arc melting method. Use of the ball milling machine was necessary to obtain Mo7Re13C with the β-Mn structure using the solid state method. Almost single-phase Mo7Re13C with a trace of impurity were obtained using the synthesis method. By XRF and lattice parameter measurements on the samples, Fe element existed in the compound synthesized using the planetary ball milling machine with a pot and balls made of steel, though Fe element was not detected in the compound synthesized using a pot and balls made of tungsten carbide. The former compound containg the Fe atom did not show superconductivity but the latter compound without the Fe atom showed superconductivity at 6.1 K.

Properties of TiNi intermetallic compound industrially produced by combustion synthesis

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

Kaieda, Yoshinari

Most TiNi shape memory intermetallic compounds are conventionally produced by the process including high frequency induction vacuum melting and casting. A gravity segregation occurs in a cast TiNi ingot because of the big difference in the specific gravity between Ti and Ni. It is difficult to control accurately the phase transformation temperature of TiNi shape memory intermetallic compound produced by the conventional process, because the martensitic transformation temperature shifts by 10K due to the change in 0.1 % of Ni content. Homogeneous TiNi intermetallic compound is produced by the industrial process including combustion synthesis method, which is a newly developedmore » manufacturing process. In the new process, phase transformation temperatures of TiNi can be controlled accurately by controlling the ratio of Ti and Ni elemental starting powders. The chemical component, the impurities and the phase transformation temperatures of the TiNi products industrially produced by the process are revealed. These properties are vitally important when combustion synthesis method is applied to an industrial mass production process for producing TiNi shape memory intermetallic compounds. TiNi shape memory products are industrially and commercially produced today the industrial process including combustion synthesis. The total production weight in a year is 30 tins in 1994.« less

Synthesis and Characterization of Aluminum-Nanodiamond Composite Powders by High Energy Ball Milling

DTIC Science & Technology

2011-12-01

al , “ Cold - spray processing of high density nanocrystalline aluminum alloy 2009...2980, 1996. [21] L. Ajdelsztajn, et al , “ Cold spray deposition of nanocrystalline aluminum alloys ,” Metallurgical and Materials Transactions, vol...form the coating or deposit [9]. Figure 2. Diagram of a typical cold spray system [9] It has been proven that pure metals or composite powders

Combustion and Plasma Synthesis of High Temperature Materials

DTIC Science & Technology

1989-10-01

photodetectors were constructed having tin oxide electrodes deposited under more and less severe condi- tions. The relative quantum efficiencies of these de ...PROPAGATING REACTION PROCESS 19 N. Sata, N. Sanada, T. Hirano, and M. Nilno COMBUSTION SYNTHESIS OF OXIDE -CARBIDE COMPOSITES L. L. Wang, Z. A. Munir, and J...SYNTHESIS OF CERAMIC POWDERS J. S. McFeaters and J. J. Moore 46 DEVELOPMENT OF TIN OXIDE COATINGS FOR USE AS ELECTRODES IN MERCURIC IODIDE

Obtaining aluminas from the thermal decomposition of their different precursors: An {sup 27}Al MAS NMR and X-ray powder diffraction studies

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

Chagas, L.H.; De Carvalho, G.S.G.; San Gil, R.A.S.

2014-01-01

Graphical abstract: - Highlights: • We synthesized three precursors of alumina from different methods. • The calcination of the precursors generated several alumina polymorphs. • XRD and NMR were used for structural investigation of the polymorphs. • The synthesis route determines the structural and textural properties of the solids. - Abstract: A commercial sample of Boehmite was used as precursor of alumina polymorphs. For comparison, three other precursors were synthesized from different methods. Particularly, the use of excess of urea promoted a very crystalline form of basic aluminum carbonate. The characteristics of the four precursors were investigated by thermal, vibrationalmore » and X-ray powder diffraction (XRD) analysis. Additionally, the nuclear magnetic resonance, with magic angle spinning ({sup 27}Al MAS NMR), was used to verify the coordination of aluminum cations. Each precursor was calcined at various temperatures generating alumina polymorphs, which were structurally analyzed by XRD and {sup 27}Al MAS NMR. Due to interest in catalysis supports, special attention was given to the γ-Al{sub 2}O{sub 3} phase, which in addition to structural investigation was subjected to textural analysis. The results showed that, from different synthesis procedures and common route of calcination, one can obtain materials with the same composition but with different structural and textural properties, which in turn can significantly influence the performance of a supported catalyst.« less

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

Thermoelectric Properties of Silicon Germanium: An In-depth Study to the Reduction of Lattice Thermal Conductivity

NASA Astrophysics Data System (ADS)

Thompson, Daniel Ross

The goal of this dissertation will be to demonstrate a new synthesis technique for the current state of the art thermoelectric material for high temperature power generation, silicon germanium (SiGe). This technique is referred to as the single element (SE) spark plasma sintering (SPS) technique because the single elements of silicon, germanium, and their n and p type dopants are alloyed together during the SPS consolidation process. This novel synthesis technique is two orders of magnitude faster than the original technique for alloying this material and one order of magnitude faster than the current technique used for alloying this material. In order to fully demonstrate that the SE SPS technique alloys SiGe several scientific studies and investigations are performed. First, SiGe is alloyed using the current state of the art method, mechanical alloying (MA). Powders of MA SiGe are traditionally consolidated by a conventional hot press (HP). These materials are employed by NASA for deep space power generation on radio-isotope thermoelectric generators (RTGs). Hence, there is readily available published data for MA+HP SiGe used in RTGs. The SiGe powder that is MA by the author is consolidated using the SPS process, MA+SPS. Therefore, an initial study was conducted to ensure that the SPS consolidation process was not having any adverse effects SiGe as compared to the HP technique. Essentially it will be shown that SiGe produced by the MA+HP method and the MA+SPS method are equivalent. This guarantees that the synthesis and characterization techniques used at the complex and advanced materials laboratory (CAML) by the author agree with published standards. Second, once the first study has demonstrated that no adverse effects occur by using the SPS to consolidate SiGe, a study was conducted to show that undoped single elements of silicon and germanium can be alloyed in the SPS. To confirm that undoped SiGe is truly alloyed using the SE SPS technique, the structural properties of the resulting materials were investigated. Based on the densities, x-ray diffraction patterns, derived lattice constants, and Vegard's law it will be shown that the SE SPS method does successfully alloy multiple compositions of undoped SiGe. The third and most important study demonstrated that SiGe alloyed using the SE SPS synthesis technique can be successfully doped to a n and p type thermoelectric (TE) material. This required an investigation of all of the TE transport properties of these materials. A significant investigation and commentary will be provided for the lattice thermal conductivity of SiGe. The need for this investigation arises from the difference in synthesis processes between the traditional MA and the novel SE SPS techniques. The MA powder is already alloyed into micron sized powders that are consolidated by the HP for an extended time (>1 hour), which allows for grain growth. The SE SPS method relies on diffusion being promoted by the electric field assisted sintering technique and occurs over a very short period of time (<30 minutes). Therefore it can not be assumed that grain growth is not affected by the time dependent processes of sintering and diffusion with the SE SPS process. As will be discussed grain size plays a role in the lattice thermal conductivity of SiGe. It is surprising and physically interesting that the MA+HP standards and the SE SPS samples have lattice thermal conductivities that indicate the dominant scattering mechanism is the same. The physical insight provided by the fourth study is made possible by the existence of the new SE SPS synthesis method for SiGe. The MA method is optimized by the addition of GaP to the n-type SiGe materials during processing. The explanation for this optimization is a subject of debate within the community. Although, a staunch conclusion can not be made due to the need for more samples and carrier concentration data, this initial study does indicate that one physical explanation within the debate for the improvement of n-type SiGe with GaP additions is more coherent with scientific experimentation. The fifth study is aimed to provide suggestions for future studies for improving this material. This includes brief investigations on the effects of various nano-structure inclusions on lattice thermal conductivity of SiGe alloys. The study is meant to be used as a tool for future students who wish to investigate the interesting physical properties of this system. (Abstract shortened by UMI.)

Influence of the modulated two-step synthesis of biogenic hydroxyapatite on biomimetic products' surface

NASA Astrophysics Data System (ADS)

Miculescu, Florin; Mocanu, Aura Cătălina; Stan, George E.; Miculescu, Marian; Maidaniuc, Andreea; Cîmpean, Anisoara; Mitran, Valentina; Voicu, Stefan Ioan; Machedon-Pisu, Teodor; Ciocan, Lucian Toma

2018-04-01

Processing calcium-rich natural resources, such as marble and mussel seashells, into biomimetic products could constitute an environmentally-friendly and economically sustainable alternative given their geographical widespread. Hitherto, their value for biomedicine was demonstrated only for seashells, with the technological exploitation approaches still facing challenges with respect to the identification of generic synthesis parameters capable to allow the reproducible and designed synthesis of calcium phosphate at an industrial-ready level. In this study was targeted the optimization of Rathje synthesis method for the fabrication of biogenic calcium phosphates, by conveniently adjusting the chemical composition of employed reagents. It was shown that post-synthesis heat-treatment of compacted powders is the key step for inducing structural transformations suitable to attain biomimetic products for reconstructive orthopedic applications. The sintered materials have been multi-parametricallyevaluated from morpho-compositional, structural, wettability, mechanical and cytocompatibility points of view and the results have been cross-examined and discussed. Convenient and efficient preparation routes to produce biogenic hydroxyapatite have been identified. The functional performances of the as-prepared biogenic ceramics endorse their use as a solid and inexpensive alternative source material for the fabrication of various bone regenerative products and implant coatings.

Shape-controlled solvothermal synthesis of bismuth subcarbonate nanomaterials

NASA Astrophysics Data System (ADS)

Cheng, Gang; Yang, Hanmin; Rong, Kaifeng; Lu, Zhong; Yu, Xianglin; Chen, Rong

2010-08-01

Much effort has been devoted to the synthesis of novel nanostructured materials because of their unique properties and potential applications. Bismuth subcarbonate ((BiO) 2CO 3) is one of commonly used antibacterial agents against Helicobacter pylori ( H. pylori). Different (BiO) 2CO 3 nanostructures such as cube-like nanoparticles, nanobars and nanoplates, were fabricated from bismuth nitrate via a simple solvothermal method. The nanostructures were characterized by powder X-ray diffraction (XRD), scanning electron microscope (SEM), transmission electron microscopy (TEM) and high-resolution transmission electron microscopy (HRTEM). It was found that the solvents and precursors have an influence on the morphologies of (BiO) 2CO 3 nanostructures. The possible formation mechanism of different (BiO) 2CO 3 nanostructures fabricated under different conditions was also discussed.

NaF-assisted combustion synthesis of MoSi2 nanoparticles and their densification behavior

NASA Astrophysics Data System (ADS)

Nersisyan, Hayk H.; Lee, Tae Hyuk; Ri, Vladislav; Lee, Jong Hyeon; Suh, Hoyoung; Kim, Jin-Gyu; Son, Hyeon Taek; Kim, Yong-Ho

2017-03-01

The exothermic reduction of oxides mixture (MoO3+2SiO2) by magnesium in NaF melt enables the synthesis of nanocrystalline MoSi2 powders in near-quantitative yields. The combustion wave with temperature of about 1000-1200 °C was recorded in highly diluted by NaF starting mixtures. The by-products of combustion reaction (NaF and MgO) were subsequently removed by leaching with acid and washing with water. The as-prepared MoSi2 nanopowder composed of spherical and dendritic shape particles was consolidated using the spark plasma sintering method at 1200-1500 °C and 50 MPa for 10 min. The result was dense compacts (98.6% theoretical density) possessing submicron grains and exhibiting hardness of 8.74-12.92 GPa.

Synthesis, characterization and antibacterial property of ZnO:Mg nanoparticles

NASA Astrophysics Data System (ADS)

Kompany, A.; Madahi, P.; Shahtahmasbi, N.; Mashreghi, M.

2012-09-01

Sol-gel method was successfully used for the synthesis of ZnO nanoparticles (NPs) doped with different concentrations of Mg and the structural, optical and antibacterial properties of the nanoparticles were studied. The synthesized ZnO:Mg powders were characterized using x-ray diffraction (XRD), transmission electron microscopy (TEM), Fourier transformation Infrared (FTIR) and UV-Vis spectroscopy. It was revealed that the samples have hexagonal Wurtzite structure, and the phase segregation takes place for 15% Mg content. TEM images show that the average size of the particles is about 50 nm. Also, the antibacterial activities of the nanoparticles were tested against Escherichia coli (Gram negative) cultures. ZnO:Mg nanofluid showed good antibacterial activity which increases with the increase of NPs concentration, and decreases slightly with the amount of Mg.

Grain orientation in high Tc superconductors by molten salt powder synthesis

NASA Technical Reports Server (NTRS)

Gopalakrishnan, Sudhakar; Schulze, Walter A.

1991-01-01

The molten salt or the flux method is used to fabricate a grain oriented YBa2Cu3O(7-x) (123) superconductor. Here we suggest a two-stage approach in using the 'green phase', Y2BaCuO5 (211), as seed crystals in the formation of YBa2Cu3O(7-x). The process uses Y2BaCuO5 formed by molten salt synthesis. The Y2BaCuO5 phase was observed to be stable in water and in most of the salt systems. Salt processing can form a small quantity of anisotropic particles of Y2BaCuO5. This material can form the 123 phase when tape cast and sintered in the presence of the required levels of Ba and Cu.

Preparation of the highly dispersed powder of titanium carbonitride by SHS azide technology with previous partial nitriding

NASA Astrophysics Data System (ADS)

Amosov, A. P.; Markov, Yu M.; Dobrovolskaya, R. A.; Nikolaeva, E. N.

2017-02-01

It is shown that the powder of very hard refractory titanium carbonitride (TiC0.5N0.5) is the basis of tungsten-free hard alloys which are prospective for application as inexpensive cutting tools. The finer the powder of titanium carbonitrideis, the moreenhanced properties of hard alloys, sintered from the powder, are. An opportunity to reduce the particle size of the titanium carbonitride powder obtained by energy-saving azide technology of self-propagating high-temperature synthesis at the cost of reducing the particle size of the initial titanium powderwas investigated. To ensure the safety of the grinding process of the initial metal titanium powder, it was offered to nitride a Ti powder partially into a TiN0.2 compound. Such partial nitriding was performed by the azidetechnology with lack of sodium azide (NaN3) as a nitriding reagent. After intensive grinding in the planetary ball mill, the TiN0.2 powder turned into a superfine powder with an ultrafine structure. This powder was capable of nitriding and carburizing in the azide technology with formation of superfine pure powder agglomerates which are composed of ultrafine and nano-particles of TiC0.5N0.5.

Synthesis of nano anatase for titanosilicate ETS-10 synthesis

NASA Astrophysics Data System (ADS)

Shafeque, Shihara

Functionalized textiles present a vast and growing niche in the global textile market at US $400 billion [1, 2]. Engelhard Titanium Silicate 10 (ETS-10), a photocatalytic zeo-type material if coated on textiles, is expected to impart useful properties similar to TiO2, such as stain-resistant, odor repellant, bactericidal and enhanced UV protection [3, 4]. Typically, small ETS-10 crystals of size ˜300-800 nm are synthesized using solid titania (e.g., anatase or P25) sources [5, 6, 7]. However, smaller ETS-10 crystals are required for a uniform surface coating with highly effective surface area. The dissolution of titania particles (i.e., their size) is hypothesized to be important in small ETS-10 crystal formation [5, 6, 7]. Nano anatase was synthesized by modification of two methods: direct precipitation [7] and sol-gel synthesis [3]. Analysis by XRD confirmed that both methods produced nano anatase of crystallite size ˜4-5 nm. However, FE-SEM analysis showed that product from direct precipitation, existed as intergrown spheroidal particles with size ˜1.0 mum. These particles dispersed poorly in deionized water. Therefore, the best nano anatase samples were from sol-gel synthesis in two forms, dry powder and colloidal anatase. ETS-10 synthesis was investigated using two methods adopted from literature [6, 7]. The method of Yoon and co-workers [7], with nano anatase in a molar composition of 5.5TEOS: TiO2: 8.4NaOH: 1.43KF: 350H2O: 2.2H2SO4 produced unknown phase(s) with some ETS-10 and quartz. Using colloidal anatase with molar composition 5.5TEOS:1.0TiO 2:8.4NaOH:1.43KF:400H2O:2.2H2SO4 also produced unknown phase(s). The method of Anderson and co-workers [6] with nano anatase powder in a molar composition of 5.5SiO2: TiO 2: 5.2Na2O: 0.5K2O: 113H2O produced quartz with ETS-10 impurity. When colloidal anatase was used, with molar composition TiO2:5.5SiO2:5.2Na2O:0.5K2O:332H 2O, unreacted anatase and quartz were formed. It was hypothesized that the very low reaction mixture pH of ˜4.1 was responsible for the absence of ETS-10. Therefore, pH of this mixture was modified between ˜6.55-12.75.At low pH of ˜6.55 unreacted anatase was present, while, pH higher than ˜11.24 formed ETS-4 crystals. At an "optimum" pH of ˜11.24 nearly phase-pure ETS-10 crystals were formed. However, these ETS-10 crystals were not small but ˜10-20 mum. This is the first time, that colloidal anatase has been utilized for ETS-10 synthesis.

Titanium nitride plasma-chemical synthesis with titanium tetrachloride raw material in the DC plasma-arc reactor

NASA Astrophysics Data System (ADS)

Kirpichev, D. E.; Sinaiskiy, M. A.; Samokhin, A. V.; Alexeev, N. V.

2017-04-01

The possibility of plasmochemical synthesis of titanium nitride is demonstrated in the paper. Results of the thermodynamic analysis of TiCl4 - H2 - N2 system are presented; key parameters of TiN synthesis process are calculated. The influence of parameters of plasma-chemical titanium nitride synthesis process in the reactor with an arc plasmatron on characteristics on the produced powders is experimentally investigated. Structure, chemical composition and morphology dependencies on plasma jet enthalpy, stoichiometric excess of hydrogen and nitrogen in a plasma jet are determined.

Coriandrum sativum mediated synthesis of silver nanoparticles and evaluation of their biological characteristics

NASA Astrophysics Data System (ADS)

Senthilkumar, N.; Aravindhan, V.; Ruckmani, K.; Vetha Potheher, I.

2018-05-01

Silver (Ag) nanoparticles (NPs) were prepared by percolated green synthesis method using Coriandrum sativum leaf, root, seed and stem extracts and reported its antibacterial activity. The synthesized Ag NPs were confirmed by UV–visible Spectroscopy, Powder x-ray Diffraction (PXRD), Fourier Transform Infra Red (FT-IR) Spectroscopy analyzes. The Maximum absorbance observed around 400–450 nm reveal the characteristic absorbance of Ag NPs. The Dynamic Light Scattering (DLS) analysis shows the stability of synthesized NPs with average size varying from 35 to 53 nm and also zeta potential stability varying from ‑20 to ‑30 mV. The cubic structure, crystalline nature and purity of the material was confirmed by powder x-ray diffraction studies. FT-IR spectrum shows the presence of various functional groups in the resultant material. The Field Emission Scanning Electron Microscopy (FESEM) image shows the surface morphology of the synthesized NPs and the Energy Dispersive x-ray Analysis (EDAX) confirms the presence of silver metal ions. The Coriandrum sativum aqueous extract exhibited excellent antimicrobial activity against Klebsiella pneumoniae (Gram -ve) bacteria. Numerous studies have been made previously in our field of study but optimization has not been carried out by both extract (different parts like leaf, root, seed and stem) and without addition of any external source such as chemicals, heat etc.

New Approach for Gas Phase Synthesis and Growth Mechanism of MoS2 Fullerene-like Nanoparticles

NASA Astrophysics Data System (ADS)

Zak, Alla; Feldman, Yishay; Alperovich, Vladimir; Rosentsveig, Rita; Tenne, Reshef

2002-10-01

Inorganic fullerene-like (hollow onion-like) nanoparticles (IF) and nanotubes are of significant interest over the past few years due to their unusual crystallographic morphology and their interesting physical properties. The synthesis of inorganic fullerene-like spherical MoS2 nanoparticles (IF-MoS2) of 5-300nm in diameter was studied in the present work. This process is based on the previous formation of suboxide (MoO3-x) 5-300nm nanoparticles and their subsequent sulfidization. During the sulfidization process the overall geometrical parameters of the suboxide nanoparticles are preserved. The oxide nanoparticles were obtained in-situ by the condensation of the evaporated MoO3 powder precursor. The condensation was provoked not by cooling (conventional method for nano-size particle formation), but by a chemical reaction (partial reduction of the MoO3 vapor by hydrogen). In this case the vapor pressure of the product (MoO2) was much lower than that of the precursor (MoO3). Based on the comprehensive understanding of the IF-MoS2 growth mechanism from MoO3 powder, a gas phase reactor, which allowed reproducible preparation of a pure IF-MoS2 phase (up to 100mg/batch) with controllable sizes, is demonstrated. Further scale-up of this production is underway.

The analysis of thermal stability of detonation nanodiamond

NASA Astrophysics Data System (ADS)

Efremov, V. P.; Zakatilova, E. I.

2016-11-01

The detonation nanodiamond is a new perspective material. Ammunition recycling with use of high explosives and obtaining nanodiamond as the result of the detonation synthesis have given a new motivation for searching of their application areas. In this work nanodiamond powder has been investigated by the method of synchronous thermal analysis. Experiments have been carried out at atmospheric pressure in the environment of argon. Nanodiamond powder has been heated in the closed corundum crucible at the temperature range of 30-1500 °C. The heating rates were varied from 2 K/min to 20 K/min. After the heat treatment, the samples have been studied by the x-ray diffraction and the electron microscopy. As one of the results of this work, it has been found that the detonation nanodiamond has not started the transition into graphite at the temperature below 800 °C.

Hexagonal pencil-like CdS nanorods: Facile synthesis and enhanced visible light photocatalytic performance

NASA Astrophysics Data System (ADS)

An, Liang; Wang, Guanghui; Zhao, Lei; Zhou, Yong; Gao, Fang; Cheng, Yang

2015-07-01

In the present study, hexagonal pencil-like CdS nanorods have been successfully synthesized through a typical facile and economical one-step hydrothermal method without using any surfactant or template. The product was characterized by X-ray powder diffraction (XRD), field-emission scanning electron microscopy (FE-SEM) and energy dispersive analysis of X-ray (EDX). The results revealed that the prepared CdS photocatalyst consisted of a large quantity of straight and smooth solid hexagonal nanorods and a few nanoparticles. The photocatalytic activities of CdS nanorods and commercial CdS powders were investigated by the photodegradation of Orange II (OII) in aqueous solution under visible light, and the CdS nanorods presented the highest photocatalytic activity. Its photocatalytic efficiency enhancement was attributed to the improved transmission of photogenerated electron-hole pairs in the CdS nanostructures. The present findings may provide a facile approach to synthesize high efficient CdS photocatalysts.

Synthesis, growth and characterization of 3-nitroacetanilide—A new organic nonlinear optical crystal by Bridgman technique

NASA Astrophysics Data System (ADS)

Lenin, M.; Ramasamy, P.

2008-10-01

Single crystals of 3-nitroacetanilide, an organic nonlinear optical material has been grown by the Bridgman-Stockbarger method. The single crystal X-ray diffraction (XRD) data revealed the noncentrosymmetric crystal structure, which is an essential criterion for second harmonic generation. The crystalline nature of the grown crystals was confirmed using powder XRD techniques. The functional group of the compound is identified by FTIR spectrum. The thermal stability and its tendency to grow as single crystal in solution and in melt have been identified for the new title compound. The UV-vis spectrum of mNAA shows the lower optical cut off at 400 nm and was transparent in the visible region. The second harmonic generation efficiency was found using Kurtz powder technique. The dielectric constant and dielectric loss of the crystal were measured as a function of frequency and temperature, and the results are discussed.

Novel perovskite coating of strontium zirconate in Inconel substrate

NASA Astrophysics Data System (ADS)

Venkatesh, G.; Blessto, B.; Rao, C. Santhosh Kumar; Subramanian, R.; Berchmans, L. John

2018-02-01

Thermal Barrier Coatings (TBC) provides a low thermal conductivity barrier to heat transfer from the hot gas in the engine to the surface of the coated alloy component. SrZrO3 powder are prepared by Sol Gel synthesis method. The synthesized powder sample is characterized by X Ray Diffraction Technique (XRD), Scanning Electron Microscope (SEM) and Transmission Electron Microscope (TEM) and the results are interpreted. The Polycrystalline nature of SrZrO3 is confirmed and lattice spacing are determined in XRD. SEM shows sub-micron sized particles and a fringed pattern is observed in TEM. The IN718 specimen is Wire Cut and Sand Blasted. A SrZrO3 double layer is coated over the Inconel specimen through a Bond Coat made of NiCoCrAlY by Plasma spraying Process and also characterized. SEM analysis of the Coating shows diffusion of Fe, Sr into the substrate.

Synthesis optimisation and characterisation of the organic-inorganic layered materials ZnS(m-xylylenediamine){sub 1/2} and ZnS(p-xylylenediamine){sub 1/2}

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

Luberda-Durnaś, K.; Guillén, A. González; Łasocha, W., E-mail: lasocha@chemia.uj.edu.pl

2016-06-15

Hybrid organic-inorganic layered materials of the type ZnS(amine){sub 1/2}, where amine=m-xylylenediamine (MXDA) or p-xylylenediamine (PXDA), were synthesised using a simple solvothermal method. Since the samples crystallised in the form of very fine powder, X-ray powder diffraction techniques were used for structural characterisation. The crystal structure studies, involving direct methods, show that both compounds crystallised in the orthorhombic crystal system, but in different space groups: ZnS(MXDA){sub 1/2} in non-centrosymmetric Ccm2{sub 1}, ZnS(PXDA){sub 1/2} in centrosymmetric Pcab. The obtained materials are built according to similar orders: semiconducting monolayers with the formula ZnS, parallel to the (010) plane, are separated by diamines. Themore » organic and inorganic fragments are connected by covalent bonds between metal atoms of the layers and nitrogen atoms of the amino groups. The optical properties of the hybrid materials differ from those of their bulk counterpart. In both compounds a blue-shift of about 0.8 or 0.9 eV was observed with reference to the bulk phase of ZnS. - Highlights: • New hybrid compounds: ZnS(MXDA){sub 1/2} and ZnS(PXDA){sub 1/2} were obtained. • Hybrids were studied using XRD, TG/DSC, XRK, SEM, UV–vis spectroscopy. • Structures of both materials were solved by powder diffraction methods.« less

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.

Synthesis and characterization of nanocrystalline Al 2024-B4C composite powders by mechanical alloying

NASA Astrophysics Data System (ADS)

Varol, T.; Canakci, A.

2013-06-01

In the present work, the effect of milling parameters on the morphology and microstructure of nanostructure Al2024-B4C composite powders obtained by mechanical alloying (MA) was studied. The effects of milling time and B4C content on the morphology, microstructure and particle size of nanostructure Al2024-B4C composite powders have been investigated. Different amounts of B4C particles (0, 5, 10 and 20 wt.%) were mixed with Al2024 powders and milled in a planetary ball mill for 30, 60, 120, 300, 420 and 600 min. Al 2024-B4C composite powders were characterized using a scanning electron microscope (SEM), laser particle-size analyzer, X-ray diffraction analysis (XRD) and the Vickers microhardness test. The results showed that the nanostructure Al2024-B4C composite powders were produced when they were milled for 600 min. The size of composite powder in the milled powder mixture was affected by the milling time and content of B4C particles. Moreover, it was observed that when MA reached a steady state, the properties of composite powders were stabilized.

Nd³⁺-Yb³⁺ doped powder for near-infrared optical temperature sensing.

PubMed

Rakov, Nikifor; Maciel, Glauco S

2014-07-01

Er³⁺ doped powders are generally used for fluorescence-based temperature sensing application when near-infrared lasers are the excitation sources of choice. The fluorescence of Er³⁺ is produced by nonlinear (upconversion) processes, which generate strong internal heat. Lowering the excitation power causes drastic reduction of the fluorescence signal, and as a consequence the sensor applicability of Er³⁺ doped powders becomes compromised. Here we propose the use of the downconverted fluorescence of Yb³⁺ produced by efficient energy transfer from Nd³⁺ as an alternative temperature sensing system. Our results are presented for yttrium silicate powders prepared by combustion synthesis.

Synthesis of multi-hierarchical structured yttria-stabilized zirconia powders and their enhanced thermophysical properties

NASA Astrophysics Data System (ADS)

Cao, Fengmei; Gao, Yanfeng; Chen, Hongfei; Liu, Xinling; Tang, Xiaoping; Luo, Hongjie

2013-06-01

Multi-hierarchical structured yttria-stabilized zirconia (YSZ) powders were successfully synthesized by a hydrothermal-calcination process. The morphology, crystallinity, and microstructure of the products were characterized by SEM, XRD, TEM, and BET. A possible formation mechanism of the unique structure formed during hydrothermal processing was also investigated. The measured thermophysical results indicated that the prepared YSZ powders had a low thermal conductivity (0.63-1.27 W m-1 K-1), good short-term high-temperature stability up to 1300 °C. The influence of the morphology and microstructure on their thermophysical properties was briefly discussed. The unique multi-hierarchical structure makes the prepared YSZ powders candidates for use in enhanced applications involving thermal barrier coatings.

USE OF COMBUSTION SYNTHESIS IN PREPARING CERAMIC-MATRIX AND METAL-MATRIX COMPOSITE POWDERS

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

Weil, K. Scott; Hardy, John S.

A standard combustion-based approach typically used to synthesize nanosize oxide powders has been modified to prepare composite oxide-metal powders for subsequent densification via sintering or hot-pressing into ceramic- or metal-matrix composites. Copper and cerium nitrate salts were dissolved in the appropriate ratio in water and combined with glycine, then heated to cause autoignition. The ratio of glycine-to-total nitrate concentration was found to have the largest effect on the composition, agglomerate size, crystallite size, and dispersivity of phases in the powder product. After consolidation and sintering under reducing conditions, the resulting composite compact consists of a well-dispersed mixture of sub-micron sizemore » reinforcement particles in a fine-grained matrix.« less

New Approach to Synthesis of Powder and Composite Materials by Electron Beam. Part 1. Technological Features of the Process

NASA Astrophysics Data System (ADS)

Rudskoy, A. I.; Kondrat'ev, S. Yu.; Sokolov, Yu. A.

2016-05-01

Possibilities of electron beam synthesis of structural and tool composite materials are considered. It is shown that a novel process involving mathematical modeling of each individual operation makes it possible to create materials with programmable structure and predictable properties from granules of various specified chemical compositions and sizes.

Rational synthesis of zerovalent iron/bamboo charcoal composites with high saturation magnetization

Treesearch

Mingshan Wu; Jianfeng Ma; Zhiyong Cai; Genlin Tian; Shumin Yang; Youhong Wang; Xing' e Liu

2015-01-01

The synthesis of magnetic biochar composites is a major new research area in advanced materials sciences. A series of magnetic bamboo charcoal composites (MBC800, MBC1000 and MBC1200) with high saturation magnetization (Ms) was fabricated in this work by mixing bamboo charcoal powder with an aqueous ferric chloride solution and subsequently...

Bio-inorganic synthesis of ZnO powders using recombinant His-tagged ZnO binding peptide as a promoter.

PubMed

Song, Lei; Liu, Yingying; Zhang, Zhifang; Wang, Xi; Chen, Jinchun

2010-10-01

Inorganic-binding peptides termed as genetically engineered polypeptides for inorganics (GEPIs), are small peptide sequences selected via combinatorial biology-based protocols of phage or cell surface display technologies. Recent advances in nanotechnology and molecular biology allow the engineering of these peptides with specific affinity to inorganics, often used as molecular linkers or assemblers, to facilitate materials synthesis, which provides a new insight into the material science and engineering field. As a case study on this biomimetic application, here we report a novel biosynthetic ZnO binding protein and its application in promoting bio-inorganic materials synthesis. In brief, the gene encoding a ZnO binding peptide(ZBP) was genetically fused with His(6)-tag and GST-tag using E.coli expression vector pET-28a (+) and pGEX-4T-3. The recombinant protein GST-His-ZBP was expressed, purified with Ni-NTA system, identified by SDS-PAGE electrophoresis and Western blot analysis and confirmed by liquid chromatography-mass spectrometry/mass spectrometry (LC-MS/MS) analysis. Affinity adsorption test demonstrated that the fusion protein had a specific avidity for ZnO nanoparticles (NPs). Results from the bio-inorganic synthesis experiment indicated that the new protein played a promoting part in grain refinement and accelerated precipitation during the formation of the ultra-fine precursor powders in the Zn(OH)(2) sol. X-ray diffraction (XRD) analysis on the final products after calcining the precursor powders showed that hexagonal wurtzite ZnO crystals were obtained. Our work suggested a novel approach to the application about the organic-inorganic interactions.

Short communication: Development of a rapid laboratory method to polymerize lactose to nondigestible carbohydrates.

PubMed

Kuechel, A F; Schoenfuss, T C

2018-04-01

Nondigestible carbohydrates with a degree of polymerization between 3 and 10 (oligosaccharides) are commonly used as dietary fiber ingredients in the food industry, once they have been confirmed to have positive effects on human health by regulatory authorities. These carbohydrates are produced through chemical or enzymatic synthesis. Polylactose, a polymerization product of lactose and glucose, has been produced by reactive extrusion using a twin-screw extruder, with citric acid as the catalyst. Trials using powdered cheese whey permeate as the lactose source for this reaction were unsuccessful. The development of a laboratory method was necessary to investigate the effect of ingredients present in permeate powder that could be inhibiting polymerization. A Mars 6 Microwave Digestion System (CEM Corp., Matthews, NC) was used to heat and polymerize the sugars. The temperatures had to be lowered from extrusion conditions to produce a caramel-like product and not decompose the sugars. Small amounts of water had to be added to the reaction vessels to allow consistent heating of sugars between vessels. Elevated levels of water (22.86 and 28.57%, vol/wt) and calcium phosphate (0.928 and 1.856%, wt/wt) reduced the oligosaccharide yield in the laboratory method. Increasing the citric acid (catalyst) concentration increased the oligosaccharide yield for the pure sugar blend and when permeate powder was used. The utility of the laboratory method to predict oligosaccharide yields was confirmed during extrusion trials of permeate when this increased acid catalyst concentration resulted in similar oligosaccharide concentrations. Copyright © 2018 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

Synthesis of the zeolitic imidazolate framework ZIF-4 from the ionic liquid 1-butyl-3-methylimidazolium imidazolate

NASA Astrophysics Data System (ADS)

Hovestadt, Maximilian; Schwegler, Johannes; Schulz, Peter S.; Hartmann, Martin

2018-05-01

A new synthesis route for the zeolitic imidazolate framework ZIF-4 using imidazolium imidazolate is reported. Additionally, the ionic liquid-derived material is compared to conventional ZIF-4 with respect to the powder X-ray diffraction pattern pattern, nitrogen uptake, particle size, and separation potential for olefin/paraffin gas mixtures. Higher synthesis yields were obtained, and the different particle size affected the performance in the separation of ethane and ethylene.

Fabrication of high temperature materials by exothermic synthesis and subsequent dynamic consolidation

DOEpatents

Rabin, Barry H.; Korth, Gary E.; Wright, Richard N.; Williamson, Richard L.

1992-01-01

An apparatus for synthesizing a composite material such as titanium carbide and alumina from exothermic reaction of a sample followed by explosive induced consolidation of the reacted sample. The apparatus includes a lower base for holding a powdered composite sample, an igniter and igniter powder for igniting the sample to initiate an exothermic reaction and a piston for dynamically compressing the sample utilizing an explosive reaction.

Pulsed current activated synthesis and rapid consolidation of a nanostructured Mg2Al4Si5O18 and its mechanical properties

NASA Astrophysics Data System (ADS)

Shon, In-Jin; Kang, Hyun-Su; Doh, Jung-Mann; Yoon, Jin-Kook

2015-03-01

Nanocrystalline materials have received much attention as advanced engineering materials, with improved mechanical properties. Attention has been directed to the application of nanomaterials, as they possess excellent mechanical properties (high strength, high hardness, excellent ductility and toughness). A singlestep synthesis and consolidation of nanostructured Mg2Al4Si5O18 was achieved by pulsed current heating, using the stoichiometric mixture of MgO, Al2O3 and SiO2 powders. Before sintering, the powder mixture was high-energy ball milled for 10 h. From the milled powder mixture, a highly dense nanostructured Mg2Al4Si5O18 compound could be obtained within one minute, under the simultaneous application of 80 MPa pressure, and a pulsed current. The advantage of this process is that it allows an instant densification to the near theoretical density, while sustaining the nanosized microstructure of raw powders. The sintering behavior, microstructure and mechanical properties of Mg2Al4Si5O18 were evaluated. The fracture toughness of a nanostructured Mg2Al4Si5O18 compound was higher than that of sub-micron Mg2Al4Si5O18 compound.

Synthesis and characterization of CaCO3 (calcite) nano particles from cockle shells (Anadara granosa Linn) by precipitation method

NASA Astrophysics Data System (ADS)

Widyastuti, Sri; Intan Ayu Kusuma, P.

2017-06-01

Calcium supplements can reduce the risk of osteoporosis, but they are not automatically absorbed in the gastrointestinal tract. Nanotechnology is presumed to have a capacity in resolving this problem. The preparation and characterization of calcium carbonate nano particle to improve the solubility was performed. Calcium carbonate nano particles were synthesized using precipitation method from cockle shells (Anadara granosa Linn). Samples of the cockle shells were dried in an oven at temperature of 50°C for 7 (seven) days and subsequently they were crushed and blended into fine powder that was sieved through 125-μm sieve. The synthesis of calcium carbonate nanocrystals was done by extracting using hydro chloride acid and various concentrations of sodium hydroxide were used to precipitate the calcium carbonate nano particles. The size of the nano particles was determined by SEM, XRD data, and Fourier transform infrared spectroscopy (FT-IR). The results of XRD indicated that the overall crystalline structure and phase purity of the typical calcite phase CaCO3 particles were approximately 300 nm in size. The method to find potential applications in industry to yield the large scale synthesis of aragonite nano particles by a low cost but abundant natural resource such as cockle shells is required.

Simple mass production of zinc oxide nanostructures via low-temperature hydrothermal synthesis

NASA Astrophysics Data System (ADS)

Ghasaban, Samaneh; Atai, Mohammad; Imani, Mohammad

2017-03-01

The specific properties of zinc oxide (ZnO) nanoparticles have attracted much attention within the scientific community as a useful material for biomedical applications. Hydrothermal synthesis is known as a useful method to produce nanostructures with certain particle size and morphology however, scaling up the reaction is still a challenging task. In this research, large scale hydrothermal synthesis of ZnO nanostructures (60 g) was performed in a 5 l stainless steel autoclave by reaction between anionic (ammonia or sodium hydroxide) and cationic (zinc acetate dehydrate) precursors in low temperature. Hydrothermal reaction temperature and time were decreased to 115 °C and 2 or 6 h. In batch repetitions, the same morphologies (plate- and needle-like) with reproducible particle size were obtained. The nanostructures formed were analyzed by powder x-ray diffraction, Fourier-transform infrared spectroscopy, energy dispersive x-ray analysis, scanning electron microscopy and BET analysis. The nanostructures formed were antibacterially active against Staphylococcus aureus.

Custom-designed nanomaterial libraries for testing metal oxide toxicity

PubMed Central

Pokhrel, Suman; Nel, André E.; Mädler, Lutz

2014-01-01

Conspectus Advances in aerosol technology over the past 10 years have provided methods that enable the generation and design of ultrafine nanoscale materials for different applications. The particles are produced combusting a precursor solution and its chemical reaction in the in the gas phase. Flame spray pyrolysis (FSP) is a highly versatile technique for single step and scalable synthesis of nanoscale materials. New innovations in particle synthesis using FSP technology and its precursor chemistry have enabled flexible dry synthesis of loosely-agglomerated highly crystalline ultrafine powders (porosity ≥ 90%) of binary, ternary and mixed binary or ternary oxides. The flame spray pyrolysis lies at the intersection of combustion science, aerosols technology and materials chemistry. The interdisciplinary research is not only inevitable but is becoming increasingly crucial in the design of nanoparticles (NPs) made in the gas phase. The increasing demand especially in the bio-applications for particles with specific material composition, high purity and crystallinity can be often fulfilled with the fast, single step FSP technique. PMID:23194152

Green synthesis of Pd NPs from Pimpinella tirupatiensis plant extract and their application in photocatalytic activity dye degradation

NASA Astrophysics Data System (ADS)

Narasaiah, Palajonna; Mandal, Badal Kumar; Sarada, N. C.

2017-11-01

The present report the synthesis of palladium nanoparticles through the green method route offers few advantages over the common chemical and physical procedures, as it is an easy and fast, eco-friendly and does not involve any costly chemicals as well as hazardous chemicals. In this study, we reported synthesis of Pd NPs by using the Pimpinella tirupatiensis plant Extract (PTPE). The synthesized Pd NPs was characterization using different technique such as UV-Visible for the formation of Pd NPs. FT-IR spectroscopy was performed to detect the bio-active molecules liable for reduction and capping of biogenic Pd NPs. Crystallinity of Pd NPs conformed by powder - XRD. In the present study performed photo catalytic activity of synthesized Pd NPs using organic dye such as Congo red (CR). Hence, this study concludes the PTPE aqueous extract produced Pd NPs can be act as promising material for the degradation of organic pollutants.

Microstructure and phase analysis of Zirconia-ODS (Oxide Dispersion Strengthen) alloy sintered by APS with milling time variation

NASA Astrophysics Data System (ADS)

Sugeng, Bambang; Bandriyana, B.; Sugeng, Bambang; Salam, Rohmad; Sumariyo; Sujatno, Agus; Dimyati, Arbi

2018-03-01

Investigation on the relationship between the process conditions of milling time and the microstructure on the synthesis of the zirconia-ODS steel alloy has been performed. The elemental composition of the alloy was determined on 20 wt% Cr and zirconia dispersoid of 0.50 wt%. The synthesis was carried out by powder metallurgy method with milling time of 3, 5 and 7 hours, static compression of 20 Ton and sintering process for 4 minutes using the APS (Arc Plasma Sintering) equipment. SEM-EDX and XRD test was carried out to characterize the phase and morphology of the alloy and the effect to the mechanical properties was evaluated by the Vickers Hardness testing. The synthesis produced sample of ODS steel with good dense and very little porous with the Fe-Cr phase that clearly observed in the XRD peak pattern. In addition milling time increased the homogeneously of Fe-Cr phase formulation, enhanced the grain refinement of the structure and increase the hardness of the alloy.

One-pot hydrothermal synthesis of an assembly of magnetite nanoneedles on a scaffold of cyclic-diphenylalanine nanorods

NASA Astrophysics Data System (ADS)

Togashi, Takanari; Umetsu, Mitsuo; Naka, Takashi; Ohara, Satoshi; Hatakeyama, Yoshiharu; Adschiri, Tadafumi

2011-09-01

The assembly of metal oxide nanoparticles (NPs) on a biomolecular template by a one-pot hydrothermal synthesis method is achieved for the first time. Magnetite (Fe3O4) nanoneedles (length: 100 nm; width: 10 nm) were assembled on cyclic-diphenylalanine (cFF) nanorods (length: 2-10 μm; width: 200 nm). The Fe3O4 nanoneedles and cFF nanorods were simultaneously synthesized from FeSO4 and l-phenylalanine by hydrothermal synthesis (220 °C and 22 MPa), respectively. The samples were analyzed by powder X-ray diffraction (XRD), Fourier transform infrared spectroscopy (IR), transmission electron microscopy (TEM), and superconducting quantum interference device (SQUID) magnetometry. Experimental results indicate that Fe3O4 nanoneedles were assembled on cFF nanorods during the hydrothermal reaction. The composite contained 3.3 wt% Fe3O4 nanoneedles without any loss of the original magnetic properties of Fe3O4.

Mechanochemical synthesis of bumetanide-4-aminobenzoic acid molecular cocrystals: a facile and green approach to drug optimization.

PubMed

Bruni, Giovanna; Maietta, Mariarosa; Berbenni, Vittorio; Mustarelli, Piercarlo; Ferrara, Chiara; Freccero, Mauro; Grande, Vincenzo; Maggi, Lauretta; Milanese, Chiara; Girella, Alessandro; Marini, Amedeo

2014-08-07

Molecular cocrystals are of growing interest in pharmaceutics for their improved physicochemical properties. Their mechanochemical synthesis is very promising, being easy, cheap, and "green". Here, for the first time, we report on cocrystallization of bumetanide, a diuretic and natriuretic active principle, and 4-aminobenzoic acid. The synthesis is performed both by wet and dry grinding. The cocrystal formation was investigated with a wide range of techniques, including solid-state NMR, IR, XRD, microscopy, and thermal analysis. Wet and dry grinding procedures led to different cocrystal polymorphs. In particular, the dry method gave a cocrystal by powder amorphization and subsequent crystallization. DFT calculations at the B3LYP/6-31+G(d,p) level of theory shed light on the H-bond scheme at the basis of cocrystal formation. The cocrystals showed improved solubility and dissolution rate with respect to the drug alone. This could guarantee a faster absorption and a better bioavailability of the active principle.

Forming a single layer of a composite powder based on the Ti-Nb system via selective laser melting (SLM)

NASA Astrophysics Data System (ADS)

Saprykin, A. A.; Sharkeev, Yu P.; Ibragimov, E. A.; Babakova, E. V.; Dudikhin, D. V.

2016-07-01

Alloys based on the titanium-niobium system are widely used in implant production. It is conditional, first of all, on the low modulus of elasticity and bio-inert properties of an alloy. These alloys are especially important for tooth replacement and orthopedic surgery. At present alloys based on the titanium-niobium system are produced mainly using conventional metallurgical methods. The further subtractive manufacturing an end product results in a lot of wastes, increasing, therefore, its cost. The alternative of these processes is additive manufacturing. Selective laser melting is a technology, which makes it possible to synthesize products of metal powders and their blends. The point of this technology is laser melting a layer of a powdered material; then a sintered layer is coated with the next layer of powder etc. Complex products and working prototypes are made on the base of this technology. The authors of this paper address to the issue of applying selective laser melting in order to synthesize a binary alloy of a composite powder based on the titanium-niobium system. A set of 10x10 mm samples is made in various process conditions. The samples are made by an experimental selective laser synthesis machine «VARISKAF-100MB». The machine provides adjustment of the following process variables: laser emission power, scanning rate and pitch, temperature of powder pre-heating, thickness of the layer to be sprinkled, and diameter of laser spot focusing. All samples are made in the preliminary vacuumized shielding atmosphere of argon. The porosity and thickness of the sintered layer related to the laser emission power are shown at various scanning rates. It is revealed that scanning rate and laser emission power are adjustable process variables, having the greatest effect on forming the sintered layer.

Plasma synthesis and HPHT consolidation of BN nanoparticles, nanospheres, and nanotubes to produce nanocrystalline cubic boron nitride

NASA Astrophysics Data System (ADS)

Stout, Christopher

Plasma methods offer a variety of advantages to nanomaterials synthesis. The process is robust, allowing varying particle sizes and phases to be generated simply by modifying key parameters. The work here demonstrates a novel approach to nanopowder synthesis using inductively-coupled plasma to decompose precursor, which are then quenched to produce a variety of boron nitride (BN)-phase nanoparticles, including cubic phase, along with short-range-order nanospheres (e.g., nano-onions) and BN nanotubes. Cubic BN (c-BN) powders can be generated through direct deposition onto a chilled substrate. The extremely-high pyrolysis temperatures afforded by the equilibrium plasma offer a unique particle growth environment, accommodating long deposition times while exposing resulting powders to temperatures in excess of 5000K without any additional particle nucleation and growth. Such conditions can yield short-range ordered amorphous BN structures in the form of 20nm diameter nanospheres. Finally, when introducing a rapid-quenching counter-flow gas against the plasma jet, high aspect ratio nanotubes are synthesized, which are collected on substrate situated radially. The benefits of these morphologies are also evident in high-pressure/high-temperature consolidation experiments, where nanoparticle phases can offer a favorable conversion route to super-hard c-BN while maintaining nanocrystallinity. Experiments using these morphologies are shown to begin to yield c-BN conversion at conditions as low as 2.0 GPa and 1500°C when using micron sized c-BN seeding to create localized regions of high pressures due to Hertzian forces acting on the nanoparticles.

Nanoscale octahedral molecular sieves: Syntheses, characterization, and applications

NASA Astrophysics Data System (ADS)

Liu, Jia

The major part of this research consists of studies on novel synthesis methods, characterization, and catalytic applications of nanoscale manganese oxide octahedral molecular sieves. The second part involves studies of new applications of bulk porous molecular sieve and layered materials (MSLM), zeolites, and inorganic powder materials for diminishing wound bleeding. Manganese oxide octahedral molecular sieves (OMS) are very important microporous materials. They have been used widely as bulk materials in catalysis, separations, chemical sensors, and batteries, due to their unique tunnel structures and useful properties. Novel methods have been developed to synthesize novel nanoscale octahedral molecular sieve manganese oxides (OMS) and metal-substituted OMS materials in order to modify their physical and chemical properties and to improve their catalytic applications. Different synthetic routes were investigated to find better, faster, and cheaper pathways to produce nanoscale or metal-substituted OMS materials. In the synthetic study of nanosize OMS materials, a combination of sol-gel synthesis and hydrothermal reaction was used to prepare pure crystalline nanofibrous todorokite-type (OMS-1) and cryptomelane-typed (OMS-2) manganese oxides using four alkali cations (Li+, K+, Na +, Rb+) and NH4+ cations. In the synthesis study of nanoscale and metal-substituted OMS materials, a combination of sol-gel synthesis and solid-state reaction was used to prepare transition metal-substituted OMS-2 nanorods, nanoneedles, and nanowires. Preparative parameters of syntheses, such as cation templates, heating temperature and time, were investigated in these syntheses of OMS-1 and OMS-2 materials. The catalytic activities of the novel synthetic nanoscale OMS materials has been evaluated on green oxidation of alcohols and toluene and were found to be much higher than their correspondent bulk materials. New applications of bulk manganese oxide molecular sieve and layered materials (MSLM), zeolites, and several inorganic powder materials have also been studied for diminishing bleeding via in vitro tests using horse blood and in vivo tests on rat organs. MSLM, as well as several types of zeolite, and several inorganic compounds, have been found to have excellent ability to clot blood and arrest wound bleeding. Effects of properties of these porous materials on the efficiency of blood coagulation have been discussed.

Sol-gel synthesis of fine Gd{sub 2}CuO{sub 4} particles: Influence of synthesis variables

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

Mahia, J.; Vazquez-Vazquez, C.; Basadre-Pampin, M.I.

1996-02-01

Fine particles of Gd{sub 2}CuO{sub 4} were prepared by a sol-gel reaction of an aqueous solution of metal nitrates in the presence of urea, which leads to high-homogeneity polycrystalline powders of Gd{sub 2}CuO{sub 4}. The authors have studied the synthesis conditions, demonstrating the existence of a relationship between the calcination temperature and the heating time needed to attain the pure phase. Gd{sub 2}CuO{sub 4} was obtained at temperatures of the order of 650 C, lower than temperatures employed in the conventional ceramic technique. The influence of the [urea]/[salts] ratio and an excess of Cu(II) in the starting solution was alsomore » studied and discussed. X-ray powder diffraction inductively coupled plasma atomic emission spectroscopy (ICPAES), photon correlation spectroscopy (PCS), and transmission electron microscopy (TEM) were used to characterize the Gd{sub 2}CuO{sub 4} samples obtained.« less

Synthesis of K2SiF6:Mn4+ phosphor for LED lamp

NASA Astrophysics Data System (ADS)

Takarkhede, M. G.; Patil, R. R.; Moharil, S. V.; Joshi, C. P.; Talewar, Rupesh

2018-05-01

Now a days red emitting Mn4+ activated dialkali fluorosilicate phosphors have found applications in solid state lighting and displays. In this paper we describe development of K2SiF6 phosphor doped with Mn synthesized by simple method using Si metal powder with addition of oxidizing agent KMnO4. The photoluminescence spectra of K2SiF6:Mn show that emission is in the red region. In addition to this we studied LED spectra by coating the LED with phosphor mixed in different proportions with epoxy.

Synthesis, characterization and electrical properties of a lead sodium vanadate apatite

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

Chakroun-Ouadhour, E.; Ternane, R.; Hassen-Chehimi, D. Ben

2008-08-04

The lacunary lead sodium vanadate apatite Pb{sub 8}Na{sub 2}(VO{sub 4}){sub 6} was synthesized by the solid-state reaction method. The compound was characterized by X-ray powder diffraction, infrared (IR) absorption spectroscopy and Raman scattering spectroscopy. By comparing the effect of vanadate and phosphate ions on electrical properties, it was concluded that Pb{sub 8}Na{sub 2}(VO{sub 4}){sub 6} apatite is better conductor than Pb{sub 8}Na{sub 2}(PO{sub 4}){sub 6} apatite.

Two-step iron(0)-mediated N-demethylation of N-methyl alkaloids.

PubMed

Kok, Gaik B; Pye, Cory C; Singer, Robert D; Scammells, Peter J

2010-07-16

A mild and simple two-step Fe(0)-mediated N-demethylation of a number of tertiary N-methyl alkaloids is described. The tertiary N-methylamine is first oxidized to the corresponding N-oxide, which is isolated as the hydrochloride salt. Subsequent treatment of the N-oxide hydrochloride with iron powder readily provides the N-demethylated amine. Representative substrates include a number of opiate and tropane alkaloids. Key intermediates in the synthesis of semisynthetic 14-hydroxy pharmaceutical opiates such as oxycodone and oxymorphone are also readily N-demethylated using this method.

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.

Phase analysis of ZrO2-SiO2 systems synthesized through Ball milling mechanical activations

NASA Astrophysics Data System (ADS)

Nurlaila, Rizka; Musyarofah, Muwwaqor, Nibras Fuadi; Triwikantoro, Kuswoyo, Anton; Pratapa, Suminar

2017-01-01

Zircon powders have been produced from raw materials of amorphous zirconia and amorphous silica powders obtained from natural zircon sand of Kalimantan Tengah, Indonesia. Synthesis process was started with the extraction of zircon powder to produce sodium silicate solution and pure zircon powder. The amorphous zirconia and silica powders were prepared by alkali fusion and co-precipitation techniques. The powders were mixed using a planetary ball mill, followed by a calcination of various holding time of 3, 10, and 15 h. Phase characterization was done using X-Ray Diffraction (XRD) technique and analysis of the diffraction data was carried out using Rietica and MAUD software. The identified phases after the calcination were zircon, tetragonal zirconia, and cristobalite. The highest zircon content was obtained in the sample calcinated for15 hours - reaching 99.66 %wt. Crystallite size analysis revealed that the samples calcinated for 3, 10, and 15 h exhibited zircon crystal size of 176 (1) nm, 191 (1) nm and 233 (1) nm respectively.

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

Structure-property relationships of iron-hydroxyapatite ceramic matrix nanocomposite fabricated using mechanosynthesis method.

PubMed

Nordin, Jamillah Amer; Prajitno, Djoko Hadi; Saidin, Syafiqah; Nur, Hadi; Hermawan, Hendra

2015-06-01

Hydroxyapatite (HAp) is an attractive bioceramics due to its similar composition to bone mineral and its ability to promote bone-implant interaction. However, its low strength has limited its application as load bearing implants. This paper presented a work focusing on the improvement of HAp mechanical property by synthesizing iron (Fe)-reinforced bovine HAp nanocomposite powders via mechanosynthesis method. The synthesis process was performed using high energy milling at varied milling time (3, 6, 9, and 12h). The samples were characterized by X-ray diffraction (XRD), Fourier transform infrared (FT-IR), and scanning electron microscopy (SEM). Its mechanical properties were investigated by micro-Vicker's hardness and compression tests. Results showed that milling time directly influenced the characteristics of the nanocomposite powders. Amorphous BHAp was formed after 9 and 12h milling in the presence of HPO4(2-) ions. Continuous milling has improved the crystallinity of Fe without changing the HAp lattice structure. The nanocomposite powders were found in spherical shape, agglomerated and dense after longer milling time. The hardness and Young's modulus of the nanocomposites were also increased at 69% and 66%, respectively, as the milling time was prolonged from 3 to 12h. Therefore, the improvement of the mechanical properties of nanocomposite was attributed to high Fe crystallinity and homogenous, dense structure produced by mechanosynthesis. Copyright © 2015 Elsevier B.V. All rights reserved.

The synthesis and characterization of Mg-Zn-Ca alloy by powder metallurgy process

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

Annur, Dhyah; Franciska, P.L.; Erryani, Aprilia

Known for its biodegradation and biocompatible properties, magnesium alloys have gained many interests to be researched as implant material. In this study, Mg-3Zn-1Ca, Mg-29Zn-1Ca, and Mg-53Zn-4.3Ca (in wt%) were synthesized by means of powder metallurgy method. The compression strength and corrosion resistance of magnesium alloy were thoroughly examined. The microstructures of the alloy were characterized using optical microscopy, Scanning Electron Microscope, and also X-ray diffraction analysis. The corrosion resistance were evaluated using electrochemical analysis. The result indicated that Mg- Zn- Ca alloy could be synthesized using powder metallurgy method. This study showed that Mg-29Zn-1Ca would make the highest mechanical strengthmore » up to 159.81 MPa. Strengthening mechanism can be explained by precipitation hardening and grain refinement mechanism. Phase analysis had shown the formation of α Mg, MgO, and intermetallic phases: Mg2Zn11 and also Ca2Mg6Zn3. However, when the composition of Zn reach 53% weight, the mechanical strength will be decreasing. In addition, all of Mg-Zn-Ca alloy studied here had better corrosion resistance (Ecorr around -1.4 VSCE) than previous study of Mg. This study indicated that Mg- 29Zn- 1Ca alloy can be further analyzed to be a biodegradable implant material.« less

Graphene: powder, flakes, ribbons, and sheets.

PubMed

James, Dustin K; Tour, James M

2013-10-15

Graphene's unique physical and electrical properties (high tensile strength, Young's modulus, electron mobility, and thermal conductivity) have led to its nickname of "super carbon." Graphene research involves the study of several different physical forms of the material: powders, flakes, ribbons, and sheets and others not yet named or imagined. Within those forms, graphene can include a single layer, two layers, or ≤10 sheets of sp² carbon atoms. The chemistry and applications available with graphene depend on both the physical form of the graphene and the number of layers in the material. Therefore the available permutations of graphene are numerous, and we will discuss a subset of this work, covering some of our research on the synthesis and use of many of the different physical and layered forms of graphene. Initially, we worked with commercially available graphite, with which we extended diazonium chemistry developed to functionalize single-walled carbon nanotubes to produce graphitic materials. These structures were soluble in common organic solvents and were better dispersed in composites. We developed an improved synthesis of graphene oxide (GO) and explored how the workup protocol for the synthesis of GO can change the electronic structure and chemical functionality of the GO product. We also developed a method to remove graphene layers one-by-one from flakes. These powders and sheets of GO can serve as fluid loss prevention additives in drilling fluids for the oil industry. Graphene nanoribbons (GNRs) combine small width with long length, producing valuable electronic and physical properties. We developed two complementary syntheses of GNRs from multiwalled carbon nanotubes: one simple oxidative method that produces GNRs with some defects and one reductive method that produces GNRs that are less defective and more electrically conductive. These GNRs can be used in low-loss, high permittivity composites, as conductive reinforcement coatings on Kevlar fibers and in the fabrication of large area transparent electrodes. Using solid carbon sources such as polymers, food, insects, and waste, we can grow monolayer and bilayer graphene directly on metal catalysts, and carbon-sources containing nitrogen can produce nitrogen-doped graphene. The resulting graphene can be transferred to other surfaces, such as metal grids, for potential use in transparent touch screens for applications in personal electronics and large area photovoltaic devices. Because the transfer of graphene from one surface to another can lead to defects, low yields, and higher costs, we have developed methods for growing graphene directly on the substrates of interest. We can also produce patterned graphene to make GNRs or graphane/graphene superlattices within a single sheet. These superlattices could have multiple functions for use in sensors and other devices. This Account only touches upon this burgeoning area of materials chemistry, and the field will continue to expand as researchers imagine new forms and applications of graphene.

Plasma-Chemical Synthesis of Oxide Powders Using Transformer-Coupled Discharge

NASA Astrophysics Data System (ADS)

M. Ulanov, I.; V. Isupov, M.; Yu Litvinsev, A.; A. Mischenko, P.

2013-04-01

An experimental investigation of transformer-coupled discharge in an Ar-O2 mixture with the addition of SiCl4, TiCl4 and ZrCl4 has been carried out under the atmospheric pressure of plasma-forming gases. Discharge power and discharge heat losses have been determined, and the dispersion and phase composition of reaction products (oxide powders) has been analyzed with SEM and X-ray diffraction analysis. Investigations reveal the formation of ultrafine oxide powders in the case of vaporized chloride (SiCl4 and TiCl4) injecting into the transformer coupled discharge. In the case of fine powder (ZrCl4) injection, full oxidation was not observed and reaction products consisted of a mixture of ZrO2 and ZrOCl2. A conclusion has been made regarding the perspectives of using transformer-coupled discharge to produce ultrafine oxide powders.

Preparation of TbCu7-type Sm-Fe powders by low-temperature HDDR treatment

NASA Astrophysics Data System (ADS)

Takagi, Kenta; Jinno, Miho; Ozaki, Kimihiro

2018-05-01

Low-temperature hydrogen-disproportionation-desorption-recombination (HDDR) treatment of Sm-Fe alloy powder was conducted to prepare a metastable TbCu7 type Sm-Fe alloy powder with a grain size of more than a few hundreds of nanometers. While a treatment temperature above 700 °C produced the familiar Th2Zn17 type alloy, one below 600 °C resulted in successful synthesis of the TbCu7 type Sm-Fe alloy with submicron-size grains. This TbCu7 type alloy powder, however, showed no significant improvement in magnetic properties compared to the Th2Zn17 type, as its composition was estimated to be near SmFe8.5 and thus did not achieve the expected Fe-rich composition. Therefore, cross-sectional transmission electron microscope observation of the unfinished TbCu7 type alloy powder was conducted in order to explore means of forming the Fe-rich phase.

Sol-gel auto-combustion synthesis and properties of Co2Z-type hexagonal ferrite ultrafine powders

NASA Astrophysics Data System (ADS)

Liu, Junliang; Yang, Min; Wang, Shengyun; Lv, Jingqing; Li, Yuqing; Zhang, Ming

2018-05-01

Z-type hexagonal ferrite ultrafine powders with chemical formulations of (BaxSr1-x)3Co2Fe24O41 (x varied from 0.0 to 1.0) have been synthesized by a sol-gel auto-combustion technique. The average particle sizes of the synthesized powders ranged from 2 to 5 μm. The partial substitution of Ba2+ by Sr2+ led to the shrinkage of the crystal lattices and resulted in changes in the magnetic sub-lattices, which tailored the static and dynamic magnetic properties of the as-synthesized powders. As the substitution ratio of Ba2+ by Sr2+, the saturation magnetization of the synthesized powders almost consistently increased from 43.3 to 56.1 emu/g, while the real part of permeability approached to a relatively high value about 2.2 owing to the balance of the saturation magnetization and magnetic anisotropy field.

Hydrothermal recrystallization of transition metal nitroprussides. Formation of the most stable phases

NASA Astrophysics Data System (ADS)

Echevarría, F.; Reguera, L.; González M, M.; Galicia, J.; Ávila, M.; Reguera, E.

2018-02-01

Hydrothermal recrystallization appears to be an appropriate treatment to explore the structural diversity of porous coordination polymers. In this contribution, such a post-synthesis treatment is applied to divalent transition metal nitroprussides, T[Fe(CN)5NO]•xH2O with T =Mn, Fe, Co, Ni, Cu, Zn, Cd. This family of compounds forms an interesting series of nanoporous coordination polymers with a wide structural diversity, related to the synthesis route used and the solid hydration degree (x). The effect of a hydrothermal recrystallization of previously prepared fine powders using the precipitation method, on their crystal structure and related properties is herein discussed. In this series of coordination polymers, for Fe, Co, Ni the precipitated powders are obtained as cubic phase, with a high porosity related to presence of systematic vacancies for building unit [Fe(CN)5NO]. For Fe and Co a structural transition, from cubic to orthorhombic, was observed, which is associated to formation of a most compact structure. The crystal structure for the new orthorhombic phases was refined from the collected powder HR-XRD patterns. For Ni, the cubic phase remains stable even for large heating time, which is ascribed to the high polarizing power of this metal. The high porosity for the cubic phase allows an easy accommodation for the local deformations around the Ni atom coordination sphere. The structural information from XRD was complemented with CO2 and H2 adsorption and TG data, IR and UV-vis spectra, and magnetic measurements. The magnetic data, through the presence of spin-orbit coupling for Fe and Co in the two phases, provide fine details on the coordination environment for the metal linked at the N ends of the CN group.

Synthesis of nanoscale magnesium diboride powder

DOE PAGES

Finnemore, D. K.; Marzik, J. V.

2015-12-18

A procedure has been developed for the preparation of small grained magnesium diboride (MgB 2) powder by reacting nanometer size boron powder in a magnesium vapor. Plasma synthesized boron powder that had particle sizes ranging from 20 to 300nm was mixed with millimeter size chunks of Mg by rolling stoichiometric amounts of the powders in a sealed cylindrical container under nitrogen gas. This mixture then was placed in a niobium reaction vessel, evacuated, and sealed by e-beam welding. The vessel was typically heated to approximately 830°C for several hours. The resulting MgB 2 particles have a grain size in themore » 200 nm to 800 nm range. Agglomerates of loosely bound particles could be broken up by light grinding in a mortar and pestle. At 830°C, many particles are composed of several grains grown together so that the average particle size is about twice the average grain size. Furthermore, experiments were conducted primarily with undoped boron powder, but carbon-doped boron powder showed very similar results.« less

Synthesis of MSnO{sub 3} (M = Ba, Sr) nanoparticles by reverse micelle method and particle size distribution analysis by whole powder pattern modeling

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

Ahmed, Jahangeer; Blakely, Colin K.; Bruno, Shaun R.

2012-09-15

Highlights: ► BaSnO{sub 3} and SrSnO{sub 3} nanoparticles synthesized using the reverse micelle method. ► Particle size and size distribution studied by whole powder pattern modeling. ► Nanoparticles are of optimal size for investigation in dye-sensitized solar cells. -- Abstract: Light-to-electricity conversion efficiency in dye-sensitized solar cells critically depends not only on the dye molecule, semiconducting material and redox shuttle selection but also on the particle size and particle size distribution of the semiconducting photoanode. In this study, nanocrystalline BaSnO{sub 3} and SrSnO{sub 3} particles have been synthesized using the microemulsion method. Particle size distribution was studied by whole powdermore » pattern modeling which confirmed narrow particle size distribution with an average size of 18.4 ± 8.3 nm for SrSnO{sub 3} and 15.8 ± 4.2 nm for BaSnO{sub 3}. These values are in close agreement with results of transmission electron microscopy. The prepared materials have optimal microstructure for successive investigation in dye-sensitized solar cells.« less

Influence of sodium fluoride on the synthesis of hydroxyapatite by gel method

NASA Astrophysics Data System (ADS)

Kanchana, P.; Sekar, C.

2010-03-01

Hydroxyapatite (HA) is a good candidate for bone substitutes due to its chemical and structural similarity to bone mineral. Hydroxyapatite has been grown by the gel method using sodium fluoride (NaF) as additive. The growth was carried out at room temperature under the physiological pH of 7.4. The addition of NaF has significantly reduced growth rate and the yield was much less when compared to pure system. The samples of pure and fluoride doped HA were sintered at 600, 900 and 1200 °C in ambient atmosphere. Scanning electron microscopy (SEM), powder X-ray diffraction (XRD), thermogravimetric analysis (TG) and Fourier transform infrared spectroscopy (FTIR) were adopted to investigate the influence of NaF on the morphology, crystallinity, stability and phase purity of HA. EDAX and FTIR studies confirm that the fluoride is doped into the hydroxyapatite. Powder XRD and TGA results suggested that the incorporation of fluorine into the HA matrix improves the phase formation and crystallinity. SEM studies show that the microstructural morphology of HA changes from the fibers for pure to granular structure for the fluoride doped.

Synthesis of transparent Lu3Al5O12 ceramic by solid-state reaction method

NASA Astrophysics Data System (ADS)

Basyrova, L. R.; Maksimov, R. N.; Shitov, V. A.; Aleksandrov, E. O.

2017-09-01

Transparent polycrystalline Lu3Al5O12 (LuAG) ceramic was fabricated by solid-state reactive sintering a mixture of Lu2O3 nanoparticles synthesized by laser ablation and commercial Al2O3 powder. The obtained Lu2O3 nanoparticles exhibited a metastable monoclinic phase and were fully converted into a main cubic phase after calcination at 1100 °C for 1 h in air. The powders were mixed in ethanol with the addition of 0.5 wt% tetraethoxysilane (TEOS), dried in a rotary evaporator, and uniaxially pressed into pellet at 200 MPa. Transparent 2 mm thick LuAG ceramic sample with an average grain size of 9.6 µm and an optical transmittance of 30 % at a wavelength of 1080 nm was obtained after sintering at 1780 °C for 20 h under vacuum. The average volume of the scattering centers (380 ppm) in the obtained LuAG ceramic and their distribution along the sample depth was evaluated by the direct count method using an optical microscope.

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.

Fast synthesis of La-substituted apatite by the dry mechanochemical method and analysis of its structure

NASA Astrophysics Data System (ADS)

Bulina, Natalia V.; Chaikina, Marina V.; Prosanov, Igor Yu.; Dudina, Dina V.; Solovyov, Leonid A.

2017-08-01

Compared to pure apatite, La-substituted apatites have improved thermal, mechanical and biological characteristics. In this article, a fast synthesis of La-substituted apatites by a dry mechanochemical method is presented. Structural studies by X-ray diffraction and Fourier transform infrared spectroscopy indicated the formation of a single-phase nanosized product after 30 min of high-energy ball milling of the reaction mixtures. The dry mechanochemical method is technologically attractive for the preparation of La-substituted apatites, as it allows reducing the processing time down to half an hour and does not require prolonged high-temperature annealing normally used in the synthesis practice of the substituted apatite. As the mechanochemically synthesized samples are nanosized, it is difficult to determine the details of their crystal structure by the Rietveld refinement method. Therefore, a series of the mechanochemically synthesized samples with different concentrations of lanthanum were annealed at 1000°C for 5 h. It was found that the annealed powders are microcrystalline La-substituted apatites Ca10-xLax(PO4)6Ox(OH)2-x, where 0 ≤ x ≤2. In their structure, the Ca2+ ions are replaced by the La3+ ions localized near the Ca2 sites, and the OH- groups are replaced by the O2- ions in the hexagonal channels.

Microwave-assisted rapid synthesis and characterization of CaF₂ particles-filled cellulose nanocomposites in ionic liquid.

PubMed

Deng, Fu; Fu, Lian-Hua; Ma, Ming-Guo

2015-05-05

In this article, we try to compound cellulose/alkali earth metal fluorides (MF2, M=Ca, Mg, Sr, Ba) nanocomposites via microwave-assisted ionic liquid method, wherein cellulose/CaF2 and cellulose/MgF2 were successfully synthesized through this method while cellulose/SrF2 and cellulose/BaF2 could not be synthesized. We focused on the synthesis of cellulose/CaF2 and investigated the influences of the different time and different temperature for the synthesis of cellulose/CaF2 nanocomposites. The influence of different heating methods such as oil-bath heating method was also studied. Ionic liquid ([Bmim][BF4]) was used for dissolving microcrystalline cellulose and providing the source of fluoride ionic and the alkali earth metal nitrate (Ca(NO3)2, Mg(NO3)2, Sr(NO3)2, and Ba(NO3)2) was used as the reaction initiator. They were investigated by X-ray powder diffraction (XRD), Fourier transform infrared spectrometry (FTIR), scanning electron microscopy (SEM), thermogravimetric analysis (TG), derivative thermogravimetric (DTG), and energy-dispersive X-ray spectra (EDS). The different heating modes have influence on the morphology and property. The different temperature and heating time also have a certain influence on the morphology and crystallinity of calcium fluoride. Copyright © 2014 Elsevier Ltd. All rights reserved.

Irreversible Phase-Changes in Nanophase RE-doped M2O3 and their Optical Signatures

DTIC Science & Technology

2015-12-01

T.; Eilers, H. Synthesis of silver /SiO2/Eu:Lu2O3 core- shell nanoparticles and their polymer nanocomposites. Powder Technol. 2011, 210, 157-166...Schwartz, J. Surface modification of Y2O3 nanoparticles . Langmuir 2007, 23, 9158-9161 (11) Imanaka, N.; Masui, T.; Mayama, Y.; Koyabu, K. Synthesis ... Synthesis and luminescence characteristics of Eu3+-doped ZrO2 nanoparticles . J. Lumin. 2007, 122, 855-857 (32) Ray, J. C.; Park, D. W.; Ahn, W. S

SnO2 Nanostructures: Effect of Processing Parameters on Their Structural and Functional Properties

NASA Astrophysics Data System (ADS)

Dontsova, Tetiana A.; Nagirnyak, Svitlana V.; Zhorov, Vladyslav V.; Yasiievych, Yuriy V.

2017-05-01

Zero- and 1D (one-dimensional) tin (IV) oxide nanostructures have been synthesized by thermal evaporation method, and a comparison of their morphology, crystal structure, sorption properties, specific surface area, as well as electrical characteristics has been performed. Synthesized SnO2 nanomaterials were studied by X-ray diffraction, scanning and transmission electron microscopy (SEM and TEM), N2 sorption/desorption technique, IR spectroscopy and, in addition, their current-voltage characteristics have also been measured. The single crystalline structures were obtained both in case of 0D (zero-dimensional) SnO2 powders and in case of 0D nanofibers, as confirmed by electron diffraction of TEM. It was found that SnO2 synthesis parameters significantly affect materials' properties by contributing to the difference in morphology, texture formation, changes in IR spectra of 1D structure as compared to 0D powders, increases in the specific surface area of nanofibers, and the alteration of current-voltage characteristics 0D and 1D SnO2 nanostructures. It was established that gas sensors utilizing of 1D nanofibers significantly outperform those based on 0D powders by providing higher specific surface area and ohmic I-V characteristics.

Template-free synthesis of ZnWO{sub 4} powders via hydrothermal process in a wide pH range

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

Hojamberdiev, Mirabbos, E-mail: mirabbos_uz@yahoo.com; Zhu, Gangqiang; Xu, Yunhua

ZnWO{sub 4} powders with different morphologies were fabricated through a template-free hydrothermal method at 180 {sup o}C for 8 h in a wide pH range. X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), UV-visible and luminescence spectrophotometers were applied to study the effects of pH values on crystallinity, morphology, optical and luminescence properties. The XRD results showed that the WO{sub 3} + ZnWO{sub 4}, ZnWO{sub 4}, and ZnO phases could form after hydrothermal processing at 180 {sup o}C for 8 h with the pH values of 1, 3-11, and 13, respectively. The SEM and TEM observation revealedmore » that the morphological transformation of ZnWO{sub 4} powders occurred with an increase in pH values as follows: star anise-, peony-, and desert rose-like microstructures and soya bean- and rod-like nanostructures. The highest luminescence intensity was found to be in sample consisting of star anise-like crystallites among all the samples due to the presence of larger particles with high crystallinity resulted from the favorable pH under the current hydrothermal conditions.« less

Solvent-Based Synthesis of Nano-Bi0.85Sb0.15 for Low-Temperature Thermoelectric Applications

NASA Astrophysics Data System (ADS)

Kaspar, K.; Fritsch, K.; Habicht, K.; Willenberg, B.; Hillebrecht, H.

2017-01-01

In this study we show a preparation method for nanostructured Bi0.85Sb0.15 powders via a chemical reduction route in a polyol medium, yielding material with particle sizes of 20-150 nm in scalable amounts. The powders were consolidated by spark plasma sintering (SPS) in order to maintain the nanostructure. To investigate influence of the sinter process, the powders were characterized by x-ray diffraction (XRD), energy dispersive x-ray spectroscopy (EDX), and scanning electron microscopy (SEM) measurements before and after SPS. Transport properties, Seebeck effect, and thermal conductivity were determined in the low temperature range below 300 K. The samples showed excellent thermal conductivity of 2.3-2.6 W/m × K at 300 K and Seebeck coefficients from -97 μV/K to -107 μV/K at 300 K with a maximum of -141 μV/K at 110 K, thus leading to ZT values of up to 0.31 at room temperature. The results show that Bi-Sb-alloys are promising materials for low-temperature applications. Our wet chemical approach gives access to scalable amounts of nano-material with increased homogeneity and good thermoelectric properties after SPS.

Synthesis of Carbon-Coated ZnO Composite and Varistor Properties Study

NASA Astrophysics Data System (ADS)

Sun, Wei-Jie; Liu, Jin-Ran; Yao, Da-Chuan; Chen, Yong; Wang, Mao-Hua

2017-03-01

In this article, monodisperse ZnO composite nanoparticles were successfully prepared by sol-gel mixed precursor method. Subsequently, carbon as the shell was homogeneously coated on the surface of the ZnO composite nanoparticles via a simple adsorption and calcination process. Microstructural studies of the as-obtained powders were carried out using the techniques of the x-ray powder diffraction, scanning electron microscopy, field emission scanning electron microscopy, transmission electron microscopy with energy dispersive x-ray spectroscopy, and Fourier transform infrared spectroscopy. The results show that the pink ZnO composite powders were fully coated by carbon. Based on the results, the effect of glucose content on the microstructure of the synthesized composites and the electrical properties of the ZnO varistors sintered in air at 1150°C for 2 h were also fully studied. As the amount of glucose increased, the thickness of carbon can be increased from 2.5 nm to 5 nm. In particular, the ZnO varistor fabricated with the appropriate thickness of the carbon coating (5 nm) leads to the superior electrical performance, with present high breakdown voltage ( V b = 420 V/mm) and excellent nonlinear coefficient ( α = 61.7), compared with the varistors obtained without carbon coating.

New reactor for production of tungsten disulfide hollow onion-like (inorganic fullerene-like) nanoparticles

NASA Astrophysics Data System (ADS)

Feldman, Y.; Zak, A.; Popovitz-Biro, R.; Tenne, R.

2000-10-01

MS 2 (M=Mo, W) hollow onion-like nanoparticles were the first inorganic fullerene-like ( IF) materials, found in 1992. Understanding of the IF-MS 2 growth mechanism in 1996 enabled us to build a rather simple reactor, which produced about 0.4 g per batch, of an almost pure IF-WS 2 powder. Soon after, it was found that the new powder showed better tribological properties compared with the regular MS 2 (M=Mo, W) powder, which is a well-known solid lubricant. The present work shows a new synthetic approach, which allows for a scale-up of IF-WS 2 production by more than two orders of magnitude. The falling-bed and, especially, fluidized-bed methods, which are presented here, pave the way for an almost ideal growth condition of the IF synthesis from an oxide precursor. As a result, the presently produced IF has a more uniform (spherical) shape and can grow to a larger size (up to 0.5 μm). It is expected that the relatively spherical IF-WS 2 nanoparticles, which are produced by the falling (fluidized) bed reactor, will exhibit superior tribological properties, than reported before.

Synthesis of ZnSnO{sub 3} nanostructure by sol gel method

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

Para, Touseef Ahmad; Reshi, Hilal Ahmad; Shelke, Vilas, E-mail: drshelke@gmail.com

2016-05-23

Zinc Stannate (ZST) with composition ZnSnO{sub 3} is known for high electron mobility, optical, piezoelectric and charge storage properties. ZST crystalizes in different lattice structures, which allows a wide range of tunablity. We demonstrate successful synthesis of ZnSnO{sub 3} nanomaterial by sol-gel method. ZnSnO{sub 3} nanomaterials were calcined and sintered at different temperatures. Powder X-ray diffraction confirmed the single phase of the nanomaterial with rhombohedral R-3 space group. The Rietveld refinement of diffraction pattern yielded lattice parameter values a=5.26Å, c=14.09Å. Raman spectroscopy revealed higher activity towards higher wavenumbers. Raman shift around 530cm{sup −1} was found to be highly structure dependent,more » most probably due to anharmonic atomic vibrations in ZnO{sub 6}/SnO{sub 6} octahedra around center of mass. Sharp Peak around 650cm{sup −1} is characteristic of ZnSnO{sub 3} molecule.« less

Green synthesis of magnetite (Fe3O4) nanoparticles using Graptophyllum pictum leaf aqueous extract

NASA Astrophysics Data System (ADS)

Sari, I. P.; Yulizar, Y.

2017-04-01

Magnetite nanoparticles (MNPs) attracted the attention of many researchers due to their unique properties. In this research, nanoscale magnetite particles have been successfully synthesized through an environmentally friendly method using aqueous extract of Graptophyllum pictum leaf (GPLE). In MNPs formation, GPLE acted as a base source and capping agent. Alkaloids in GPLE were hydrolyzed in water and hydroxilated Fe2+ to form Fe3O4 nanoparticles powder through calcination. After the addition of leaf extract, MNPs formation was observed by color change from pale yellow to dark brown. The synthesized nanoparticles were characterized using UV-Vis spectrophotometer, X-Ray diffraction (XRD), and Fourier transform infra red (FTIR) spectroscopy. The results confirmed that MNPs formation indicated the surface plasmon resonance at a maximum wavelength, λmax 291 nm. The average crystallite size is 23.17 nm. The formed MNPs through green synthesis method promise in various medical applications such as drug carrier and targeted therapy.

Ultrasound-Assisted Synthesis of Titania Nanoparticles, Characterization of Their Thin Films, and Activity in Photooxidation of β-Naphthol

NASA Astrophysics Data System (ADS)

Hurain, Syyeda Sana; Habib, Amir; Hussain, Syed Muzammil; Ul-Haq, Noaman

2015-11-01

Nanosized titania (TiO2) films and powders were prepared from titanium isopropoxide by ultrasonication then ultrasonic aerosol-assisted chemical vapor deposition (UAACVD). X-ray diffraction (XRD), used to study the crystal structure, phase, and crystallite size of TiO2 samples annealed at 500°C, revealed anatase was the main crystalline phase. Scanning electron microscopy and atomic force microscopy revealed the quasi-spherical morphology of the TiO2 nanoparticles; average size distribution was in the range 20-35 nm. Ultraviolet-visible spectroscopy was used to evaluate the photocatalytic activity of the anatase TiO2, on the basis of efficiency of degradation of β-naphthol. Pure TiO2 nanoparticles synthesized by use of sonication-UAACVD then calcination at 500°C enabled effective photodegradation under UV light. This method of synthesis of TiO2 is superior to the reflux-UAACVD method with titanium isopropoxide as precursor.

The Complex Sol-Gel Process for producing small ThO2 microspheres

NASA Astrophysics Data System (ADS)

Brykala, Marcin; Rogowski, Marcin

2016-05-01

Thorium based fuels offer several benefits compared to uranium based fuels thus they might be an attractive alternative to conventional fuel types. This study is devoted to the synthesis and the characterization of small thorium dioxide microspheres (Ø <50 μm). Their application involves using powder-free process, called the Complex Sol-Gel Process. The source sols used for the processes were prepared by the method where in the starting ascorbic acid solution the solid thorium nitrate was dissolved and partially neutralized by aqueous ammonia under pH control. The microspheres of thorium-ascorbate gel were obtained using the ICHTJ Process (INCT in English). Studies allowed to determine an optimal heat treatment with calcination temperature of 700 °C and temperature rate not higher than 2 °C/min which enabled us to obtain a crack-free surface of microspheres. The main parameters which have a strong influence on the synthesis method and features of the spherical particles of thorium dioxide are described in this article.

SPS-RS technique for solid-phase “in situ” synthesis of biocompatible ZrO2 porous ceramics

NASA Astrophysics Data System (ADS)

Shichalin, O. O.; Medkov, M. A.; Grishchenko, D. N.; Mayorov, V. Yu; Fedorets, A. N.; Belov, A. A.; Golub, A. V.; Gridasova, E. A.; Papynov, E. K.

2018-02-01

The prospective method of spark plasma sintering-reaction synthesis (SPS-RS) for fabrication of ceramics based on ZrO2 and biocompatible with living tissue is presented. Nanostructured ceramics has high mechanical strength (more than 400 MPa) and controlled porosity depending on specified sintering conditions. Biocompatible phases Ca10(PO4)6(OH)2 are formed “in situ” during SPS sintering of ZrO2 powder due to chemical interaction of phosphate precursors preliminary introduced into the mixture. The effective method to improve (to develop) porous structure of bioceramics obtained by SPS or SPS-RS techniques using poreforming agent (carbon black) is proposed. Suggested original SPS-RS “in situ” technique provides fabrication of new ZrO2 ceramics containing biocompatible phosphate components and possessing unique structural and mechanical characteristics. Such ceramics is indispensable for bone-ceramic implants that are able to activate processes of osteogenesis during bone tissue recovery.

Antibacterial studies of novel Cu2WS4 ternary chalcogenide synthesized by hydrothermal process

NASA Astrophysics Data System (ADS)

Kannan, Selvaraj; Vinitha, Perumal; Mohanraj, Kannusamy; Sivakumar, Ganesan

2018-02-01

This is the first report for the synthesis of L-cysteine mediated Cu2WS4 nanoparticles for different temperatures by an inexpensive and less pollutive hydrothermal method. The as-synthesized particles were characterized by XRD, FTIR, FESEM, UV-vis diffuse reflectance and PL spectra technique respectively. The phase purity and structural confirmation were studied by X-ray powder diffraction technique. It is observed that the synthesis temperature affecting the crystalline size. The optical analysis of the Cu2WS4 nanoparticles showed direct band gap in the range of 2.1-2.3 eV. The intensity of the PL emission spectra decreases with increase of reaction temperature. The antibacterial performance of Cu2WS4 nanoparticles were investigated by agar well diffusion method and the results confirm that the antibacterial activity of Cu2WS4 against Gram-positive (B. subtilis, M. luteus) and Gram-negative (E. coli, P. aeruginosa and K. pneumoniae) bacteria.

Two chain gallium fluorodiphosphates: synthesis, structure solution, and their transient presence during the hydrothermal crystallisation of a microporous gallium fluorophosphate.

PubMed

Millange, Franck; Walton, Richard I; Guillou, Nathalie; Loiseau, Thierry; O'Hare, Dermot; Férey, Gérard

2002-04-21

Two novel gallium fluorodiphosphates have been isolated and their structures solved ab initio from powder X-ray diffraction data; the materials readily interconvert under hydrothermal conditions, and are metastable with respect to an open-framework zeolitic gallium fluorophosphate, during the synthesis of which they are present as transient intermediates.

Cermet materials prepared by combustion synthesis and metal infiltration

DOEpatents

Holt, Joseph B.; Dunmead, Stephen D.; Halverson, Danny C.; Landingham, Richard L.

1991-01-01

Ceramic-metal composites (cermets) are made by a combination of self-propagating high temperature combustion synthesis and molten metal infiltration. Solid-gas, solid-solid and solid-liquid reactions of a powder compact produce a porous ceramic body which is infiltrated by molten metal to produce a composite body of higher density. AlN-Al and many other materials can be produced.

An alternative gas sensor material: Synthesis and electrical characterization of SmCoO{sub 3}

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

Michel, Carlos Rafael; Delgado, Emilio; Santillan, Gloria

2007-01-18

Single-phase perovskite SmCoO{sub 3} was prepared by a wet-chemical synthesis technique using metal-nitrates and citric acid; after its characterization by thermal analyses and X-ray diffraction, sintering at 900 deg. C in air, gave single phase and well crystallized powders. The powders were mixed with an organic solvent to prepare a slurry, which was deposited on alumina substrates as thick films, using the screen-printing technique. Electrical and gas sensing properties of sintered SmCoO{sub 3} films were investigated in air, O{sub 2} and CO{sub 2}, the results show that sensitivity reached a maximum value at 420 deg. C, for both gases. Dynamicmore » tests revealed a better behavior of SmCoO{sub 3} in CO{sub 2} than O{sub 2}, due to a fast response and a larger electrical resistance change to this gas. X-ray diffraction made on powders after electrical characterization in gases, showed that perovskite-type structure was preserved.« less

Synthesis of Cobalt Powder by Reduction of Cobalt Oxide with Ethanol

NASA Astrophysics Data System (ADS)

Cetinkaya, S.; Eroglu, S.

2018-03-01

In this study, ethanol (C2H5OH) was used as a reducing agent for Co powder synthesis from Co3O4. It aimed to investigate the effects of temperature (700-900 K), reaction time (0-60 min), and gas flow rate on the reaction behavior of Co3O4 in ethanol flow. Mass measurement, x-ray diffraction, and scanning electron microscopy techniques were used to characterize the products. Single-phase Co powders with mean particle sizes of 0.51 μm and 0.70 μm were obtained within 10 min at 800 K and 900 K, respectively. Above 800 K, external mass transfer controlled the reduction process (Q a = 0.52 kJ/mole). Below 800 K, the process (Q a = 20.17 kJ/mole) was partly controlled by external mass transfer and partly by intrinsic chemical reaction kinetics. Significant C uptake was observed at 700 K and 750 K within 60 min. The reactions were discussed in the light of thermodynamic results, which predicted Co formation from Co3O4 and C2H5OH.

Enhancement of structural and magnetic properties of M-type hexaferrite permanent magnet based on synthesis temperature

NASA Astrophysics Data System (ADS)

Anjum, Safia; Sehar, Fatima; Mustafa, Zeeshan; Awan, M. S.

2018-01-01

The main purpose of this research work is to develop the single domain magnetic particles of M-type barium hexaferrite (BaFe12O19) using oxide precursors employing conventional powder metallurgy technique. The phase formation and magnetic performance of the powders and magnets will be optimized by adjusting calcination and sintering temperatures. The synthesis of M-type barium hexaferrite was carried out in two sections. A series of four samples have been prepared by initial wet mixed powders calcined at different temperatures, i.e., 750, 850, 950 and 1050 °C. On the basis of structural analysis, the sample calcined at 950 °C has been selected and further divided into four parts to sintered them at 1100, 1150, 1200 and 1250 °C. The structural measurements depict the confirmation of M-type barium hexaferrite structure. SEM micrographs show the hexagonal-shaped grains. The abrupt decrease in coercivity for the sample sintered at 1250 °C has been seen which may be due to high sintering temperature, at which the particles have multi-domain properties.

Synthesis of ultrafine ZrB2 powders by sol-gel process

NASA Astrophysics Data System (ADS)

Yang, Li-Juan; Zhu, Shi-Zhen; Xu, Qiang; Yan, Zhen-Yu; Liu, Ling

2010-09-01

Ultrafine zirconium diboride (ZrB2) powders have been synthesized by sol-gel process using zirconium oxychloride (ZrOCl2·8H2O), boric acid (H3BO3) and phenolic resin as sources of zirconia, boron oxide and carbon, respectively. The effects of the reaction temperature, B/Zr ratio, holding time, and EtOH/H2O ratio on properties of the synthesized ZrB2 powders were investigated. It was revealed that ultrafine (average crystallite size between 100 and 400 nm) ZrB2 powders can be synthesized with the optimum processing parameters as follows: (i) the ratio of B/Zr is 4; (ii) the solvent is pure ethanol; (iii) the condition of carbothermal reduction heat treatment is at 1550°C for 20 min.

Plasma synthesis of lithium based intercalation powders for solid polymer electrolyte batteries

DOEpatents

Kong, Peter C [Idaho Falls, ID; Pink, Robert J [Pocatello, ID; Nelson, Lee O [Idaho Falls, ID

2005-01-04

The invention relates to a process for preparing lithium intercalation compounds by plasma reaction comprising the steps of: forming a feed solution by mixing lithium nitrate or lithium hydroxide or lithium oxide and the required metal nitrate or metal hydroxide or metal oxide and between 10-50% alcohol by weight; mixing the feed solution with O.sub.2 gas wherein the O.sub.2 gas atomizes the feed solution into fine reactant droplets, inserting the atomized feed solution into a plasma reactor to form an intercalation powder; and if desired, heating the resulting powder to from a very pure single phase product.

Features of the structure of a TiB2-based powder material obtained under self-propagating high-temperature synthesis and shear deformation

NASA Astrophysics Data System (ADS)

Bazhin, P. M.; Stolin, A. M.; Konstantinov, A. S.; Mukhina, N. I.; Pazniak, A.

2018-04-01

The results of an experimental study of TiB2-based powder material obtained under the combination of SHS processes with shear deformation are presented. The effects of the rotor velocity and the delay time before shear deformation application upon the structure of the synthesized powder are studied. The grain structure of titanium diboride is shown to become predominantly round with particles size of 1-5 μm with increasing the rotor velocity from 120 to 600 rpm. At the same time, particles of 200-400 nm size can be observed on the surface of the agglomerates.

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

Synthesis and physicochemical characterizations and antimicrobial activity of ZnO nanoparticles

NASA Astrophysics Data System (ADS)

Sharma, Bhumika K.; Patel, Kinjal; Roy, Debesh R.

2018-05-01

Nanoparticles exhibit very interesting and useful physicochemical properties when they interact with substrates and goes through some physicochemical and/or biological processes. ZnO is known to be a highly demanding nanomaterial due to its discreet properties, shapes and sizes. A detail experimental study on the synthesis, characterization and antibacterial activity of ZnO nanoparticles (NPs) is performed. ZnO NPs are synthesized using chemical precipitation method. The understanding of crystal structure, morphology and elemental compositions are explained using Powder X-Ray Diffraction (XRD) and Field Emission Scanning Electron Microscope (FE-SEM) respectively. Fourier transform infrared spectroscopy (FTIR) is performed to achieve the information on the presence of various functional groups. The antibacterial activity of these ZnO NPs is investigated in terms of Zone of Inhibition (ZOI) against Escherichia coli (Gram negative) microorganisms.

Low-temperature synthesis and structural properties of ferroelectric K 3WO 3F 3 elpasolite

NASA Astrophysics Data System (ADS)

Atuchin, V. V.; Gavrilova, T. A.; Kesler, V. G.; Molokeev, M. S.; Aleksandrov, K. S.

2010-06-01

Low-temperature ferroelectric G2 polymorph of K 3WO 3F 3 has been prepared by chemical synthesis. Structural and chemical properties of the final product have been evaluated with X-ray powder diffraction (XRD), scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS). Structure parameters of G2-K 3WO 3F 3 are refined by the Rietveld method from XRD data measured at room temperature (space group Cm, Z = 2, a = 8.7350(3) Å, b = 8.6808(5) Å, c = 6.1581(3) Å, β = 135.124(3) Å, V = 329.46(3) Å 3; RB = 2.47%). Partial ordering of oxygen and fluorine atoms has been found over anion positions. Mechanism of ferroelectric phase transition in A 2BMO 3F 3 oxyfluorides is discussed.

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

PubMed

Ghows, Narjes; Entezari, Mohamad H

2010-06-01

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

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

Synthesis and optical properties modulation of ZnO/Eu2O3 nanocable arrays

NASA Astrophysics Data System (ADS)

Yang, Lei; She, Yajuan; Zhao, Shihua; Yue, Shihai; Wang, Qian; Hu, Aiping; Zhang, Wei

2010-11-01

White-light-emitting materials have attracted considerable attention because of their applications, such as large-surface emitting devices and displays. However, simply mixing nanoparticles would result in uneven color. Nanocables are expected to improve the chemical stability and color uniformity. Herein we demonstrate the synthesis of Eu2O3/ZnO nanocable arrays embedded in anodic alumina template via a versatile, simple, and cheap method. In order to control the composition of the cable with low cost, a two-step synthesis including an electric field deposition and a sol-gel template approach is used to fabricate the nanocable. The product is investigated by x-ray powder diffraction, transmission electron microscopy, selected area electron diffraction, and photoluminescence (PL) spectrum. The results show that ordered Eu2O3/ZnO nanocable arrays with an average inside diameter of 20-40 nm and wall thickness of 20-40 nm were prepared. By adjusting the excitation wavelength, change of the emitting color of the cables from blue to white could be obtained. Energy and charge transfer were found by investigating the electronic transition and recombination in the PL process. These arrays are promising for applications in display, white phosphors, and ultraviolet detectors owing to the special optical properties. And this method may be of much significance in the synthesis of nanocables with the controllable composition.

New catalysts for coal liquefaction and new nanocrystalline catalysts synthesis methods

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

Linehan, J.C.; Matson, D.W.; Darab, J.G.

1994-09-01

The use of coal as a source of transportation fuel is currently economically unfavorable due to an abundant world petroleum supply and the relatively high cost of coal liquefaction. Consequently, a reduction in the cost of coal liquefaction, for example by using less and/or less costly catalysts or lower liquefaction temperatures, must be accomplished if coal is to play an significant role as a source of liquid feedstock for the petrochemical industry. The authors and others have investigated the applicability of using inexpensive iron-based catalysts in place of more costly and environmentally hazardous metal catalysts for direct coal liquefaction. Iron-basedmore » catalysts can be effective in liquefying coal and in promoting carbon-carbon bond cleavage in model compounds. The authors have been involved in an ongoing effort to develop and optimize iron-based powders for use in coal liquefaction and related petrochemical applications. Research efforts in this area have been directed at three general areas. The authors have explored ways to optimize the effectiveness of catalyst precursor species through use of nanocrystalline materials and/or finely divided powders. In this effort, the authors have developed two new nanophase material production techniques, Modified Reverse Micelle (MRM) and the Rapid Thermal Decomposition of precursors in Solution (RTDS). A second effort has been aimed at optimizing the effectiveness of catalysts by variations in other factors. To this, the authors have investigated the effect that the crystalline phase has on the capacity of iron-based oxide and oxyhydroxide powders to be effectively converted to an active catalyst phase under liquefaction conditions. And finally, the authors have developed methods to produce active catalyst precursor powders in quantities sufficient for pilot-scale testing. Major results in these three areas are summarized.« less

Synthesis, characterization, temperature dependent electrical and magnetic properties of Ca3Co4O9 by a starch assisted sol-gel combustion method

NASA Astrophysics Data System (ADS)

Agilandeswari, K.; Ruban Kumar, A.

2014-09-01

In this present work we discussed the synthesis of pure Ca3Co4O9 ceramic powder by a starch assisted sol-gel combustion method. The products were characterized by powder X-ray diffraction (XRD), thermogravimetric and differential thermal analyses (TGA-DTA), Fourier transformation infrared spectroscopy (FTIR), scanning electron microscope (SEM) and UV-visible diffuse reflectance spectroscopy (DRS). X-ray diffraction pattern confirmed the formation of single phase Ca3Co4O9 at a sintering temperature of 1073 K, and it is also confirmed in the thermal analysis. SEM images indicate the presence of diffused microporous sphere like morphology and the grain sizes are in the range of 150-300 nm. Optical properties of Ca3Co4O9 ceramic show a band gap at an energy level of 2.10 eV. A maximum electrical resistivity of 0.002 mΩ cm was exhibited by Ca3Co4O9 that was decreased to 0.0012 mΩ cm, when the temperature increased from 300 K to 473 K. Dielectric studies were conducted at various temperatures from room temperature to 673 K and the results indicate that the space charge polarization contributes to the conduction mechanism. It also shows that the dielectric relaxation with activation energy is 0.96 eV. The magnetic properties as a function of temperature represent the ferri-paramagnetic phase transition at above 50 K. M-H curve shows the hysteresis loop with saturation magnetization (Ms) and confirms the presence of soft magnetic materials.

Particle release and control of worker exposure during laboratory-scale synthesis, handling and simulated spills of manufactured nanomaterials in fume hoods

NASA Astrophysics Data System (ADS)

Fonseca, Ana S.; Kuijpers, Eelco; Kling, Kirsten I.; Levin, Marcus; Koivisto, Antti J.; Nielsen, Signe H.; Fransman, W.; Fedutik, Yijri; Jensen, Keld A.; Koponen, Ismo K.

2018-02-01

Fume hoods are one of the most common types of equipment applied to reduce the potential of particle exposure in laboratory environments. A number of previous studies have shown particle release during work with nanomaterials under fume hoods. Here, we assessed laboratory workers' inhalation exposure during synthesis and handling of CuO, TiO2 and ZnO in a fume hood. In addition, we tested the capacity of a fume hood to prevent particle release to laboratory air during simulated spillage of different powders (silica fume, zirconia TZ-3Y and TiO2). Airborne particle concentrations were measured in near field, far field, and in the breathing zone of the worker. Handling CuO nanoparticles increased the concentration of small particles (< 58 nm) inside the fume hood (up to 1 × 105 cm-3). Synthesis, handling and packaging of ZnO and TiO2 nanoparticles did not result in detectable particle release to the laboratory air. Simulated powder spills showed a systematic increase in the particle concentrations inside the fume hood with increasing amount of material and drop height. Despite powder spills were sometimes observed to eject into the laboratory room, the spill events were rarely associated with notable release of particles from the fume hood. Overall, this study shows that a fume hood generally offers sufficient exposure control during synthesis and handling of nanomaterials. An appropriate fume hood with adequate sash height and face velocity prevents 98.3% of particles release into the surrounding environment. Care should still be made to consider spills and high cleanliness to prevent exposure via resuspension and inadvertent exposure by secondary routes.

Thermoluminescence glow curve analysis and CGCD method for erbium doped CaZrO{sub 3} phosphor

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

Tiwari, Ratnesh, E-mail: 31rati@gmail.com; Chopra, Seema

2016-05-06

The manuscript report the synthesis, thermoluminescence study at fixed concentration of Er{sup 3+} (1 mol%) doped CaZrO{sub 3} phosphor. The phosphors were prepared by modified solid state reaction method. The powder sample was characterized by thermoluminescence (TL) glow curve analysis. In TL glow curve the optimized concentration in 1mol% for UV irradiated sample. The kinetic parameters were calculated by computerized glow curve deconvolution (CGCD) techniaue. Trapping parameters gives the information of dosimetry loss in prepared phosphor and its usability in environmental monitoring and for personal monitoring. CGCD is the advance tool for analysis of complicated TL glow curves.

Synthesis of galium nitride thin films using sol-gel dip coating method

NASA Astrophysics Data System (ADS)

Hamid, Maizatul Akmam Ab; Ng, Sha Shiong

2017-12-01

In this research, gallium nitride (GaN) thin film were grown on silicon (Si) substrate by a low-cost sol-gel dip coating deposition method. The GaN precursor solution was prepared using gallium (III) nitrate hydrate powder, ethanol and diethanolamine as a starting material, solvent and surfactant respectively. The structural, morphological and optical characteristics of the deposited GaN thin film were investigated. Field-emission scanning electron microscopy observations showed that crack free and dense grains GaN thin films were formed. Energy dispersive X-ray analysis confirmed that the oxygen content in the deposited films was low. X-ray diffraction results revealed that deposited GaN thin films have hexagonal wurtzite structure.

Enhancement of Ce/Cr Codopant Solubility and Chemical Homogeneity in TiO2 Nanoparticles through Sol-Gel versus Pechini Syntheses.

PubMed

Chen, Wen-Fan; Mofarah, Sajjad S; Hanaor, Dorian Amir Henry; Koshy, Pramod; Chen, Hsin-Kai; Jiang, Yue; Sorrell, Charles Christopher

2018-06-18

Ce/Cr codoped TiO 2 nanoparticles were synthesized using sol-gel and Pechini methods with heat treatment at 400 °C for 4 h. A conventional sol-gel process produced well-crystallized anatase, while Pechini synthesis yielded less-ordered mixed-phase anatase + rutile; this suggests that the latter method enhances Ce solubility and increases chemical homogeneity but destabilizes the TiO 2 lattice. Greater structural disruption from the decomposition of the Pechini precursor formed more open agglomerated morphologies, while the lower levels of structural disruption from pyrolysis of the dried sol-gel precursor resulted in denser agglomerates of lower surface areas. Codoping and associated destabilization of the lattice reduced the binding energies in both powders. Cr 4+ formation in sol-gel powders and Cr 6+ formation in Pechini powders suggest that these valence changes derive from synergistic electron exchange from intervalence and/or multivalence charge transfer. Since Ce is too large to allow either substitutional or interstitial solid solubility, the concept of integrated solubility is introduced, in which the Ti site and an adjacent interstice are occupied by the large Ce ion. The photocatalytic performance data show that codoping was detrimental owing to the effects of reduced crystallinity from lattice destabilization and surface area. Two regimes of mechanistic behavior are seen, which are attributed to the unsaturated solid solutions at lower codopant levels and supersaturated solid solutions at higher levels. The present work demonstrates that the Pechini method offers a processing technique that is superior to sol-gel because the former facilitates solid solubility and consequent chemical homogeneity.

Solid-state synthesis of nano-sized Ba(Ti1- x Sn x )O3 powders and dielectric properties of corresponding ceramics

NASA Astrophysics Data System (ADS)

Ansaree, Md. Jawed; Kumar, Upendra; Upadhyay, Shail

2017-06-01

Powders of a few compositions of solid solution BaTi1- x Sn x O3 ( x = 0.0, 0.1, 0.2, 0.3 and 0.40) have been synthesized at 800 °C for 8 h using Ba(NO3)2, TiO2 and SnCl4·5H2O as starting materials. The thermogravimetric (TG) and differential scanning calorimetric (DSC) analysis of mixture in the stoichiometric proportion for sample BaTi0.80Sn0.20O3 have been carried out to understand the formation of solid solutions. Single-phase pure compounds (except x = 0.40) of the samples have been obtained at a lower calcination temperature (800 °C) than that of those reported in the literature for traditional solid-state synthesis making use of oxides and or carbonates as starting material (≥1200 °C). Tetragonal symmetry for compositions x = 0.0 and 0.10, cubic for x = 0.2 and 0.30 were found by X-ray diffraction (XRD) analysis. The transmission electron microscopic (TEM) analysis confirmed that calcined powders have a particle size between 30 and 50 nm. Ceramics of these powders were prepared by sintering at 1350 °C for 4 h. Properties of ceramics obtained in this work have been compared with properties reported in the literature.

Effect of organic fuels on surface area and photocatalytic activity of scheelite CaWO4 nanoparticles

NASA Astrophysics Data System (ADS)

Manjunath, Kusuma; Gujjarahalli Thimmanna, Chandrappa

2018-03-01

Discrete nanoscale calcium tungstate (CaWO4) nanoparticles with exquisite photocatalytic activities were synthesized through ultra-rapid solution combustion route. Here, we aim to study the effect of different fuels on the synthesis of CaWO4 nanoparticles which lead to improve the characteristic properties and morphological evolution of the powders. From BET surface area measurement, it is observed that CaWO4 nanoparticles synthesized by using citric acid as fuel exhibits relatively large surface area (31.78 m2 g‑1) as compared to other fuels. The powder x-ray diffraction (PXRD) studies reveal that CaWO4 nanoparticles belong to scheelite type tetragonal system. The morphology of CaWO4 nanoparticles investigated using scanning electron microscopy (SEM) reveals that the powders are highly porous and agglomerated. Transmission electron microscopy (TEM) and high-resolution transmission electron microscopy (HRTEM) images of the CaWO4 nanoparticles show that a well-dispersed nearly oval-shaped nanoparticles with variable dimensions and lattice spacing that depends on the type of fuels used in the synthesis. The selected area electron diffraction (SAED) patterns of CaWO4 nanoparticles exhibit several concentric rings with bright spots indicating the polycrystalline nature of the powders. Investigation on photocatalytic activity of CaWO4 nanoparticles synthesized using citric acid shows highest (∼93%) degradation of methylene blue (MB).

Homogeneous Iron Phosphate Nanoparticles by Combustion of Sprays

PubMed Central

Rudin, Thomas; Pratsinis, Sotiris E.

2013-01-01

Low-cost synthesis of iron phosphate nanostructured particles is attractive for large scale fortification of basic foods (rice, bread, etc.) as well as for Li-battery materials. This is achieved here by flame-assisted and flame spray pyrolysis (FASP and FSP) of inexpensive precursors (iron nitrate, phosphate), solvents (ethanol), and support gases (acetylene and methane). The iron phosphate powders produced here were mostly amorphous and exhibited excellent solubility in dilute acid, an indicator of relative iron bioavailability. The amorphous and crystalline fractions of such powders were determined by X-ray diffraction (XRD) and their cumulative size distribution by X-ray disk centrifuge. Fine and coarse size fractions were obtained also by sedimentation and characterized by microscopy and XRD. The coarse size fraction contained maghemite Fe2O3 while the fine was amorphous iron phosphate. Furthermore, the effect of increased production rate (up to 11 g/h) on product morphology and solubility was explored. Using increased methane flow rates through the ignition/pilot flame of the FSP-burner and inexpensive powder precursors resulted in also homogeneous iron phosphate nanoparticles essentially converting the FSP to a FASP process. The powders produced by FSP at increased methane flow had excellent solubility in dilute acid as well. Such use of methane or even natural gas might be economically attractive for large scale flame-synthesis of nanoparticles. PMID:23407874

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

NASA Astrophysics Data System (ADS)

Kersen, Ü.

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

Cermet materials prepared by combustion synthesis and metal infiltration

DOEpatents

Holt, J.B.; Dunmead, S.D.; Halverson, D.C.; Landingham, R.L.

1991-01-29

Ceramic-metal composites (cermets) are made by a combination of self-propagating high temperature combustion synthesis and molten metal infiltration. Solid-gas, solid-solid and solid-liquid reactions of a powder compact produce a porous ceramic body which is infiltrated by molten metal to produce a composite body of higher density. AlN-Al and many other materials can be produced. 6 figures.

Synthesis of gold nanoparticles on the surface of pyrolytic graphite using penicillin as a stabilizing reagent and the catalytic oxidation of α-naphthylamine

NASA Astrophysics Data System (ADS)

Song, Y. Z.; Song, Y.; Cheng, Z. P.; Zhou, J. F.; Wei, C.

2013-01-01

Electrochemical synthesis of gold nanoparticles on the surface of pyrolytic graphite using penicillin as a stabilizing reagent was proposed. The gold nanoparticles were characterized by scanning electron microscopy, cyclic voltammetry, IR spectra, UV spectra, and powder X-ray diffraction spectra. The electro-chemical catalysis of penicillin for α-naphthylamine was demonstrated.

New mesostructured organosilica with chiral sugar derived structures: nice host for gold nanoparticles stabilisation.

PubMed

Hérault, Damien; Cerveau, Geneviève; Corriu, Robert J P; Mehdi, Ahmad

2011-01-14

In this paper we describe the synthesis of functionalised mesoporous organosilicas containing a mannitol derivative in the framework. For this purpose, a bis-silylated precursor 3,4-Di-O-[3-(triethoxysilylpropyl)carbamate]-1,2:5,6-di-O-isopropylidene-D-mannitol was prepared by coupling of 1,2:5,6-di-O-isopropylidene-D-mannitol with 3-(triethoxysilylpropyl)isocyanate. The framework-functionalised materials were obtained in one step by the "direct synthesis" method which consists of a co-hydrolysis and polycondensation of a bis-silylated mannitol precursor with tetraethylorthosilicate (TEOS) in the presence of a non-ionic triblock co-polymer (P123) as structure-directing agent. Interestingly, deprotection of the 1,2,5,6 OH functional groups occurred during the material synthesis. The obtained solids were characterized by (13)C and (29)Si CP-MAS NMR, N(2) adsorption-desorption, powder X-ray diffraction, TEM and elemental analysis. We have shown that, the OH functional groups, which are released during the synthesis of the mesoporous silica, can be used for chelation of ions and stabilisation of nanoparticles. The subsequent growth of gold (0) nanoparticles in the wall has been investigated and evidenced.

Gold nanoparticles mediated coloring of fabrics and leather for antibacterial activity.

PubMed

Velmurugan, Palanivel; Shim, Jaehong; Bang, Keuk-Soo; Oh, Byung-Taek

2016-07-01

Metal gold nanoparticles (AuNPs) were synthesized in situ onto leather, silk and cotton fabrics by three different modules, including green, chemical, and a composite of green and chemical synthesis. Green synthesis was employed using Ginkgo biloba Linn leaf powder extract and HAuCl4 with the fabrics, and chemical synthesis was done with KBH4 and HAuCl4. For composite synthesis, G. biloba extract and KBH4 were used to color and embed AuNPs in the fabrics. The colored fabrics were tested for color coordination and fastness properties. To validate the green synthesis of AuNPs, various instrumental techniques were used including UV-Vis spectrophotometry, HR-TEM, FTIR, and XRD. The chemical and composite methods reduce Au(+) onto leather, silk and cotton fabrics upon heating, and alkaline conditions are required for bonding to fibers; these conditions are not used in the green synthesis protocol. FE-SEM image revealed the binding nature of the AuNPs to the fabrics. The AuNPs that were synthesized in situ on the fabrics were tested against a skin pathogen, Brevibacterium linens using LIVE/DEAD BacLight Bacterial Viability testing. This study represents an initial route for coloring and bio-functionalization of various fabrics with green technologies, and, accordingly, should open new avenues for innovation in the textile and garment sectors. Copyright © 2016 Elsevier B.V. All rights reserved.

Investigation on synthesis, growth, structure and physical properties of AgGa0.5In0.5S2 single crystals for Mid-IR application

NASA Astrophysics Data System (ADS)

Karunagaran, N.; Ramasamy, P.

2018-02-01

Silver Gallium Indium Sulfide (AgGa0.5In0.5S2) belongs to the family of AIBIIIC2VI ternary compound semiconductors which crystallize in the chalcopyrite structure. Synthesis of the polycrystalline material from the starting elements is achieved using melt temperature oscillation method. The AgGa0.5In0.5S2 single crystals have been grown by the vertical Bridgman technique. The synthesized AgGa0.5In0.5S2 polycrystalline charge was confirmed by powder XRD. The peak positions are in good agreement with the powder diffraction file. Thermal property was analyzed using differential scanning calorimetry (DSC) technique. The melting point of the crystal is 896 °C and freezing point is 862 °C. The unit cell parameters were confirmed by single crystal X-ray. The transmittance of the grown crystal is 55% in the NIR region and 60% in the mid-IR region. The optical band gap was found to be 2.0 eV. The stoichiometric composition of AgGa0.5In0.5S2 was measured using energy dispersive spectrometry (EDS). The photoluminescence behavior of AgGa0.5In0.5S2 has been analyzed. The resistivity of the grown single crystal has been measured.

Thermal analysis, phase equilibria, and superconducting properties in magnesium boride and carbon doped magnesium boride

NASA Astrophysics Data System (ADS)

Bohnenstiehl, Scot David

In this work, the low temperature synthesis of MgB2 from Mg/B and MgH2/B powder mixtures was studied using Differential Scanning Calorimetry (DSC). For the Mg/B powder mixture, two exothermic reaction events were observed and the first reaction event was initiated by the decomposition of Mg(OH)2 on the surface of the magnesium powder. For the MgH 2/B powder mixture, there was an endothermic event at ˜375 °C (the decomposition of MgH2 into H2 and Mg) and an exothermic event ˜600 °C (the reaction of Mg and B). The Kissinger analysis method was used to estimate the apparent activation energy of the Mg and B reaction using DSC data with different furnace ramp rates. The limitations of MgB2 low temperature synthesis led to the development of a high pressure induction furnace that was constructed using a pressure vessel and an induction heating power supply. The purpose was to not only synthesize more homogeneous MgB2 samples, but also to determine whether MgB2 melts congruently or incongruently. A custom implementation of the Smith Thermal Analysis method was developed and tested on aluminum and AlB2, the closest analogue to MgB2. Measurements on MgB2 powder and a high purity Mg/B elemental mixture confirmed that MgB2 melts incongruently and decomposes into a liquid and MgB4 at ˜1445 °C at 10 MPa via peritectic decomposition. Another measurement using a Mg/B elemental mixture with impure boron suggested that ˜0.7 wt% carbon impurity in the boron raised the incongruent melting temperature to ˜1490-1500 °C. Lastly, the solubility limit for carbon in MgB2 was studied by making samples from B4C and Mg at 1530 °C, 1600 °C and 1700 °C in the high pressure furnace. All three samples had three phases: Mg, MgB2C2, and carbon doped MgB2. The MgB 2C2 and carbon doped MgB2 grain size increased with temperature and the 1700 °C sample had needle-like grains for both phases. The presence of the ternary phase, MgB2C2, suggested that the maximum doping limit for carbon in MgB2 had been reached. The 1530 °C sample was characterized by Electron Probe Microanalysis at the University of Oregon and the average carbon concentration was estimated to be ˜5.9 at%. Further investigation using TEM found MgO inclusions in the 1530 °C sample which were not detected with X-ray diffraction.

Stability and rheology of dispersions of silicon nitride and silicon carbide

NASA Technical Reports Server (NTRS)

Feke, Donald L.

1987-01-01

The relationship between the surface and colloid chemistry of commercial ultra-fine silicon carbide and silicon nitride powders was examined by a variety of standard characterization techniques and by methodologies especially developed for ceramic dispersions. These include electrokinetic measurement, surface titration, and surface spectroscopies. The effects of powder pretreatment and modification strategies, which can be utilized to augment control of processing characteristics, were monitored with these technologies. Both silicon carbide and nitride were found to exhibit silica-like surface chemistries, but silicon nitride powders possess an additional amine surface functionality. Colloidal characteristics of the various nitride powders in aqueous suspension is believed to be highly dependent on the relative amounts of the two types of surface groups, which in turn is determined by the powder synthesis route. The differences in the apparent colloidal characteristics for silicon nitride powders cannot be attributed to the specific absorption of ammonium ions. Development of a model for the prediction of double-layer characteristics of materials with a hybrid site interface facilitated understanding and prediction of the behavior of both surface charge and surface potential for these materials. The utility of the model in application to silicon nitride powders was demonstrated.

Synthesis of pentafluorides

DOEpatents

Asprey, L.B.; Paine, R.T. Jr.

1975-12-30

The reactions of uranium, molybdenum, rhenium, osmium and iridium hexafluorides with hydrogen gas in the presence of ultraviolet radiation or with silicon powder in an anhydrous HF slurry provide especially useful, high yield syntheses of pure pentafluorides.

Characterization and thermal behavior of PrMO{sub 3} (M = Co or Ni) ceramic materials obtained from gelatin

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

Aquino, F.M., E-mail: flavyma@hotmail.com; Melo, D.M.A.; Pimentel, P.M.

2012-09-15

Graphical abstract: The micrograph in figure shows sample calcined at temperature 900 °C. The sample exhibits morphology with considerable porosity and the formation of agglomerated nanometric particles. Gelatin provides the system with a large amount of organic matter, which is then removed during calcinations, favoring the appearance of pores in the material. Highlights: ► Oxides with PrNiO{sub 3} and PrCoO{sub 3} were prepared by new method synthesis. ► The gelatin, through its carboxylate groups and amine, is an efficient director. ► The obtained materials have magnetic properties and application in catalysis. ► The decomposition kinetic study of bonding groups ofmore » gelatin with metallic ions that takes part in the synthesis of PrMO{sub 3}. -- Abstract: Metal oxides with perovskite-type structure have attracted considerable interest in recent years due to their magnetic and electrical properties, as well as their catalytic activity. In this study, oxides with PrNiO{sub 3} and PrCoO{sub 3} composition were prepared by using gelatin powder as a precursor agent for its use as a catalyst. The powders obtained were calcined at 700 °C and 900 °C and characterized using the X-ray diffraction, thermal analysis (thermogravimetry and differential thermal analysis), infrared spectroscopy, temperature programed reduction and scanning electron microscopy techniques. Thermogravimetric data using the non-isothermal kinetic models of Flynn and Wall and “Model-free Kinetics” were used to determine the activation energy to study the decomposition kinetics of the ligand groups with system's metallic ions that takes part in the synthesis of PrMO{sub 3} (M = Ni or Co).« less

Combustion synthesis and characterization of blue long lasting phosphor CaAl2O4: Eu2+, Dy3+ and its novel application in latent fingerprint and lip mark detection

NASA Astrophysics Data System (ADS)

Sharma, Vishal; Das, Amrita; Kumar, Vijay; Kumar, Vinay; Verma, Kartikey; Swart, H. C.

2018-04-01

This work investigates the structural, optical and photometric characterization of a Eu2+/Dy3+ doped calcium aluminates phosphor (CaAl2O4: Eu2+/Dy3+) for finger and lip print detections. Synthesis of CaAl2O4: Eu2+/Dy3+ (CAED) phosphors were carried out via a combustion synthesis method with urea as a fuel. Eu2+/Dy3+ doped CaAl2O4 phosphors have been studied with X-ray diffraction (XRD, Energy Dispersive X-Ray Spectroscopy Selected Area Diffraction (SAED) and High resolution Transmission Electron Microscope (HR-TEM). The XRD pattern shows that the synthesized Eu2+/Dy3+ doped CaAl2O4 phosphor have a single monoclinic structure and show that the addition of the dopant/co-dopants didn't change the crystal structure. The formation of monoclinic phase was confirmed by the selected area diffraction pattern. The TEM micrograph displays the morphology of the synthesized Eu2+/Dy3+ doped CaAl2O4 phosphors as spherical particles with an average particle size of 33 nm. The optical band gap was calculated using the diffuse reflectance for the synthesized nanophosphor powders. The photoluminescence emission spectra was recorded for the synthesized powder, with an excitation wavelength of 326 nm and the major bands was recorded at 447 nm corresponding to the blue color and two minor bands were recorded at 577 nm and 616 nm. To the best of our knowledge, this work is the first to show the use of CaAl2O4: Eu2+/Dy3+ nanophosphor in developing latent fingerprint and lip print effectively.

An approach to shortening the timeframe between the emergence of new compounds on the drugs market and the availability of reference standards: The microscale syntheses of nitrazolam and clonazolam for use as reference materials, utilizing polymer-supported reagents.

PubMed

Dowling, Geraldine; Kavanagh, Pierce V; Eckhardt, Hans-Georg; Twamley, Brendan; Hessman, Gary; McLaughlin, Gavin; O'Brien, John; Brandt, Simon D

2018-03-15

Nitrazolam and clonazolam are 2 designer benzodiazepines available from Internet retailers. There is growing evidence suggesting that such compounds have the potential to cause severe adverse events. Information about tolerability in humans is scarce but typically, low doses can be difficult to administer for users when handling bulk material. Variability of the active ingredient in tablet formulations can also be of a concern. Customs, toxicology and forensic laboratories are increasingly encountering designer benzodiazepines, both in tablet and powdered form. The unavailability of reference standards can impact on the ability to identify these compounds. Therefore, the need arises for exploring in-house approaches to the preparation of new psychoactive substances (NPS) that can be carried out in a timely manner. The present study was triggered when samples of clonazolam were received in powdered and tablet form at a time when reference material for this drug was commercially unavailable. Therefore, microscale syntheses of clonazolam and its deschloro analog nitrazolam were developed utilizing polymer-supported reagents starting from 2-amino-2'-chloro-5-nitrobenzophenone (clonazolam) and 2-amino-5-nitrobenzophenone (nitrazolam). The final reaction step forming the 1,2,4-triazole ring moiety was performed within a gas chromatography-mass spectrometry (GC-MS) injector. A comparison with a preparative scale synthesis of both benzodiazepine derivatives showed that microscale synthesis might be an attractive option for a forensic laboratory in terms of time and cost savings when compared with traditional methods of synthesis and when qualitative identifications are needed to direct forensic casework. The reaction by-product profiles for both the micro and the preparative scale syntheses are also presented. Copyright © 2018 John Wiley & Sons, Ltd.

Green synthesis of silver nanoparticles using cranberry powder aqueous extract: characterization and antimicrobial properties.

PubMed

Ashour, Asmaa A; Raafat, Dina; El-Gowelli, Hanan M; El-Kamel, Amal H

2015-01-01

The growing threat of microbial resistance against traditional antibiotics has prompted the development of several antimicrobial nanoparticles (NPs), including silver NPs (AgNPs). In this article, a simple and eco-friendly method for the synthesis of AgNPs using the cranberry powder aqueous extract is reported. Cranberry powder aqueous extracts (0.2%, 0.5%, and 0.8% w/v) were allowed to interact for 24 hours with a silver nitrate solution (10 mM) at 30°C at a ratio of 1:10. The formation of AgNPs was confirmed by ultraviolet-visible spectroscopy and their concentrations were determined using atomic absorption spectroscopy. The prepared NPs were evaluated by transmission electron microscopy, measurement of ζ-potential, and Fourier-transform infrared spectroscopy. The in vitro antimicrobial properties of AgNPs were then investigated against several microbial strains. Finally, in vivo appraisal of both wound-healing and antimicrobial properties of either plain AgNPs (prepared using 0.2% extract) or AgNP-Pluronic F-127 gel was conducted in a rat model after induction of a Staphylococcus aureus ATCC 6538P wound infection. The formation of AgNPs was confirmed by ultraviolet-visible spectroscopy, where a surface-plasmon resonance absorption peak was observed between 432 and 438 nm. Both size and concentration of the formed AgNPs increased with increasing concentration of the extracts. The developed NPs were stable, almost spherical, and polydisperse, with a size range of 1.4-8.6 nm. The negative ζ-potential values, as well as Fourier-transform infrared spectroscopy analysis, indicated the presence of a capping agent adsorbed onto the surface of the particles. In vitro antimicrobial evaluation revealed a size-dependent activity of the AgNPs against the tested organisms. Finally, AgNPs prepared using 0.2% extract exhibited a substantial in vivo healing potential for full-thickness excision wounds in rats. AgNPs were successfully synthesized from a silver nitrate solution through a simple green route, using cranberry powder aqueous extract as a reducing as well as capping agent.

Review of the Methods for Production of Spherical Ti and Ti Alloy Powder

NASA Astrophysics Data System (ADS)

Sun, Pei; Fang, Zhigang Zak; Zhang, Ying; Xia, Yang

2017-10-01

Spherical titanium alloy powder is an important raw material for near-net-shape fabrication via a powder metallurgy (PM) manufacturing route, as well as feedstock for powder injection molding, and additive manufacturing (AM). Nevertheless, the cost of Ti powder including spherical Ti alloy has been a major hurdle that prevented PM Ti from being adopted for a wide range of applications. Especially with the increasing importance of powder-bed based AM technologies, the demand for spherical Ti powder has brought renewed attention on properties and cost, as well as on powder-producing processes. The performance of Ti components manufactured from powder has a strong dependence on the quality of powder, and it is therefore crucial to understand the properties and production methods of powder. This article aims to provide a cursory review of the basic techniques of commercial and emerging methods for making spherical Ti powder. The advantages as well as limitations of different methods are discussed.

Powder lemon juice containing oligosaccharides obtained by dextransucrase acceptor reaction synthesis and dehydrated in sprouted bed.

PubMed

Coelho, Raquel Macedo Dantas; Araújo, Antônia Daiana Andrade; Fontes, Cláudia Patrícia Mourão Lima; da Silva, Ana Raquel Araujo; da Costa, José Maria Correia; Rodrigues, Sueli

2015-09-01

Oligosaccharides can be synthesized using the sugars present in the fruit juices through the dextransucrase acceptor reaction. In the present work, the effect of reducing sugar and sucrose concentration on oligosaccharide formation in lemon juice was evaluated through response surface methodology. The oligosaccharide formation in lemon juice was favored at high concentrations of sucrose (75 g/L) and reducing sugar (75 g/L). At this synthesis conditions, an oligosaccharide concentration of 94.81 g/L was obtained with a conversion of 63.21% of the initial sugars into the target product. Oligosaccharides with degree of polymerization up to 11 were obtained. The lemon juice was dehydrated in spouted bed using maltodextrin as drying adjuvant. The powder obtained at 60°C with 20 % maltodextrin presented low moisture (2.24 %), low water activity (Aw = 0.18) and the lowest reconstitution time (~46 s). The results showed that lemon juice is suitable for oligosaccharides enzyme synthesis and can be dehydrated in spouted bed.

Synthesis of high-oxidation Y-Ba-Cu-O phases in superoxygenated thin films

NASA Astrophysics Data System (ADS)

Zhang, H.; Gauquelin, N.; McMahon, C.; Hawthorn, D. G.; Botton, G. A.; Wei, J. Y. T.

2018-03-01

It is known that solid-state reaction in high-pressure oxygen can stabilize high-oxidation phases of Y-Ba-Cu-O superconductors in powder form. We extend this superoxygenation concept of synthesis to thin films which, due to their large surface-to-volume ratio, are more reactive thermodynamically. Epitaxial thin films of YBa2Cu3O7 -δ grown by pulsed laser deposition are annealed at up to 700 atm O2 and 900 ∘C , in conjunction with Cu enrichment by solid-state diffusion. The films show the clear formation of Y2Ba4Cu7O15 -δ and Y2Ba4Cu8O16 as well as regions of YBa2Cu5O9 -δ and YBa2Cu6O10 -δ phases, according to scanning transmission electron microscopy, x-ray diffraction, and x-ray absorption spectroscopy. Similarly annealed YBa2Cu3O7 -δ powders show no phase conversion. Our results demonstrate a route of synthesis towards discovering more complex phases of cuprates and other superconducting oxides.

Fast synthesis and consolidation of porous FeAl by pressureless Spark Plasma Sintering

NASA Astrophysics Data System (ADS)

Dudina, D. V.; Brester, A. E.; Anisimov, A. G.; Bokhonov, B. B.; Legan, M. A.; Novoselov, A. N.; Skovorodin, I. N.; Uvarov, N. F.

2017-07-01

We report one-step fast synthesis and consolidation of iron aluminide FeAl of high open porosity by pressureless reactive Spark Plasma Sintering (SPS). The starting material of the Fe-40at.%Al composition was a mixture of an iron powder with an average particle diameter of 4 μm and an aluminum powder with an average particle diameter of 6 μm. The rationale behind the choice of the SPS as a processing technique and fine and comparable sizes of the two reactants for the synthesis of high-open porosity FeAl was realization of fast full chemical conversion of Fe and Al into single-phase FeAl reducing the time available for the compact shrinkage. According to the XRD phase analysis, single-phase FeAl compacts formed after SPS at 800 and 900°C. These compacts had open porosities of 41 and 46%, respectively. The transverse rupture strength of the compacts sintered at 700-900°C was found to change little with the sintering temperature in the selected range.

Formation of sodium bismuth titanate-barium titanate during solid-state synthesis

DOE PAGES

Hou, Dong; Aksel, Elena; Fancher, Chris M.; ...

2017-01-12

Phase formation of sodium bismuth titanate (Na 0.5Bi 0.5TiO 3 or NBT) and its solid solution with barium titanate (BaTiO 3 or BT) during the calcination process is studied using in situ high-temperature diffraction. The reactant powders were mixed and heated to 1000°C, while X-ray diffraction patterns were recorded continuously. Phase evolutions from starting materials to final perovskite products are observed, and different transient phases are identified. The formation mechanism of NBT and NBT–xBT perovskite structures is discussed, and a reaction sequence is suggested based on the observations. The in situ study leads to a new processing approach, which ismore » the use of nano-TiO 2, and gives insights to the particle size effect for solid-state synthesis products. Lastly, it was found that the use of nano-TiO 2 as reactant powder accelerates the synthesis process, decreases the formation of transient phases, and helps to obtain phase-pure products using a lower thermal budget.« less

Synthesis, structural and vibrational studies on mixed alkali metal gadolinium double tungstate, K1-xNaxGd(WO4)2

NASA Astrophysics Data System (ADS)

Durairajan, A.; Thangaraju, D.; Moorthy Babu, S.

2013-02-01

Mixed alkali double tungstates K1-xNaxGd(WO4)2 (KNGW) (0 ⩽ x ⩽ 1) were synthesized by solid state reaction using sodium doped monoclinic KGd(WO4)2 (KGW). Synthesized KNGW powders were characterized using powder X-ray diffraction (XRD), differential thermal analysis (DTA), scanning electron microscopy (SEM) and Raman analysis. DTA analysis confirms that the melting point of the KGW matrix increases from 1063 °C to 1255 °C with increasing sodium content. The Powder XRD analyses reveal that mixed phases were observed up to 40 wt.% of Na in the KGW matrix above that percentage there is domination of scheelite structure in the synthesized powder. Polyhedral type, bi-pyramidal shape and spheroid shape morphology was observed for KGW, NKGW and NGW powders respectively. The Raman analysis was carried out to understand the vibrational characteristic changes with mixing of sodium ions in the KGW matrix.

Synthesizing and characterization of titanium diboride for composite bipolar plates in PEM fuel cell

NASA Astrophysics Data System (ADS)

Duddukuri, Ramesh

This research deals with the synthesis and characterization of titanium diboride (TiB2) from novel carbon coated precursors. This work provides information on using different boron sources and their effect on the resulting powders of TiB2. The process has two steps in which the oxide powders were first coated with carbon by cracking of a hydrocarbon gas, propylene (C3H6) and then, mixed with boron carbide and boric acid powders in a stoichiometric ratio. These precursors were treated at temperatures in the range of 1200--1400° C for 2 h in flowing Argon atmosphere to synthesize TiB2. The process utilizes a carbothermic reduction reaction of novel carbon coated precursor that has potential of producing high-quality powders (sub-micrometer and high purity). Single phase TiB2 powders produced, were compared with commercially available titanium diboride using X-ray diffraction and Transmission electron microscopy obtained from boron carbide and boric acid containing carbon coated precursor.

Powder-based adsorbents having high adsorption capacities for recovering dissolved metals and methods thereof

DOEpatents

Janke, Christopher J.; Dai, Sheng; Oyola, Yatsandra

2016-05-03

A powder-based adsorbent and a related method of manufacture are provided. The powder-based adsorbent includes polymer powder with grafted side chains and an increased surface area per unit weight to increase the adsorption of dissolved metals, for example uranium, from aqueous solutions. A method for forming the powder-based adsorbent includes irradiating polymer powder, grafting with polymerizable reactive monomers, reacting with hydroxylamine, and conditioning with an alkaline solution. Powder-based adsorbents formed according to the present method demonstrated a significantly improved uranium adsorption capacity per unit weight over existing adsorbents.

Synthesis of iron based hydrocracking catalysts

DOEpatents

Farcasiu, Malvina; Eldredge, Patricia A.; Ladner, Edward P.

1993-01-01

A method of preparing a fine particle iron based hydrocracking catalyst and the catalyst prepared thereby. An iron (III) oxide powder and elemental sulfur are reacted with a liquid hydrogen donor having a hydroaromatic structure present in the range of from about 5 to about 50 times the weight of iron (III) oxide at a temperature in the range of from about 180.degree. C. to about 240.degree. C. for a time in the range of from about 0 to about 8 hours. Various specific hydrogen donors are disclosed. The catalysts are active at low temperature (<350.degree. C.) and low pressure.

Low-temperature rapid synthesis and superconductivity of Fe-based oxypnictide superconductors.

PubMed

Fang, Ai-Hua; Huang, Fu-Qiang; Xie, Xiao-Ming; Jiang, Mian-Heng

2010-03-17

Fe-based oxypnictide superconductors were successfully synthesized at lower reaction temperatures and with shorter reaction times made possible by starting with less stable compounds, which provide a larger driving force for reactions. Using ball-milled powders of intermediate compounds, phase-pure superconductors with T(c) above 50 K were synthesized at 1173 K in 20 min. This method is particularly advantageous for retaining F, a volatile dopant that enhances superconductivity. Bulk superconductivity and high upper critical fields up to 392 T in Sm(0.85)Nd(0.15)FeAsO(0.85)F(0.15) were demonstrated.

Electroplating lithium transition metal oxides.

PubMed

Zhang, Huigang; Ning, Hailong; Busbee, John; Shen, Zihan; Kiggins, Chadd; Hua, Yuyan; Eaves, Janna; Davis, Jerome; Shi, Tan; Shao, Yu-Tsun; Zuo, Jian-Min; Hong, Xuhao; Chan, Yanbin; Wang, Shuangbao; Wang, Peng; Sun, Pengcheng; Xu, Sheng; Liu, Jinyun; Braun, Paul V

2017-05-01

Materials synthesis often provides opportunities for innovation. We demonstrate a general low-temperature (260°C) molten salt electrodeposition approach to directly electroplate the important lithium-ion (Li-ion) battery cathode materials LiCoO 2 , LiMn 2 O 4 , and Al-doped LiCoO 2 . The crystallinities and electrochemical capacities of the electroplated oxides are comparable to those of the powders synthesized at much higher temperatures (700° to 1000°C). This new growth method significantly broadens the scope of battery form factors and functionalities, enabling a variety of highly desirable battery properties, including high energy, high power, and unprecedented electrode flexibility.

Synthesis on structure and properties of zinc nanocrystal in high ordered 3D nanostructures

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

Sathyaseelan, B., E-mail: bsseelan03@gmail.com; Manigandan, A.; Anbarasu, V.

2015-06-24

The wet impregnation method was employed to prepare ZnO encapsulated in mesoporous silica (ZnO/KIT-6). The prepared ZnO/KIT-6 samples have been studied by X-ray diffraction, transmission electron microscope, and nitrogen adsorption–desorption isotherm. The low angle powder XRD patterns of Calcined ZnO/KIT-6 materials showed a phase that can be indexed to cubic Ia3d. Tem images revealed well ordered cubic 3D nanoporous chennels. The ZnO encapsulated in KIT-6 can be used as light-emitting diodes and ultraviolet nanolasers.

Rotating disk atomization of Gd and Gd-Y for hydrogen liquefaction via magnetocaloric cooling

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

Slinger, Tyler

2016-12-17

In order to enable liquid hydrogen fuel cell technologies for vehicles the cost of hydrogen liquefaction should be lowered. The current method of hydrogen liquefaction is the Claude cycle that has a figure of merit (FOM) of 0.3-0.35. New magnetocaloric hydrogen liquefaction devices have been proposed with a FOM>0.5, which is a significant improvement. A significant hurdle to realizing these devices is the synthesis of spherical rare earth based alloy powders of 200μm in diameter. In this study a centrifugal atomization method that used a rotating disk with a rotating oil quench bath was developed to make gadolinium and gadolinium-yttriummore » spheres. The composition of the spherical powders included pure Gd and Gd 0.91Y 0.09. The effect of atomization parameters, such as superheat, melt properties, disk shape, disk speed, and melt system materials and design, were investigated on the size distribution and morphology of the resulting spheres. The carbon, nitrogen, and oxygen impurity levels also were analyzed and compared with the magnetic performance of the alloys. The magnetic properties of the charge material as well as the resulting powders were measured using a vibrating sample magnetometer. The saturation magnetization and Curie temperature were the target properties for the resulting spheres. These values were compared with measurements taken on the charge material in order to investigate the effect of atomization processing on the alloys.« less

Sealed-tube synthesis and phase diagram of Li{sub x}TiS{sub 2} (0 ≤ x ≤1)

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

Zhang, Ziping; National Laboratory for Superconductivity, Institute of Physics, Chinese Academy of Science, Beijing 100190; Dong, Cheng, E-mail: chengdon@aphy.iphy.ac.cn

2015-01-15

Graphical abstract: We reported a new method to prepare Li{sub x}TiS{sub 2} (0 ≤ x ≤ 1) at 600 °C in sealed tube using Li{sub 2}S aslithium source. A schematic phase diagram of the Li{sub x}TiS{sub 2} system has been constructed based on the DTA and XRD data. - Abstract: We reported a new method to prepare Li{sub x}TiS{sub 2} (0 ≤ x ≤ 1) at 600 °C in sealed tube using Li{sub 2}S as lithium source. The Li{sub x}TiS{sub 2} samples were characterized by powder X-ray diffraction, scanning electron microscopy, energy dispersive X-ray spectroscopy, and differential thermal analysis. Themore » variations of the lattice parameters with lithium content x in Li{sub x}TiS{sub 2} were determined by X-ray powder diffraction analysis for both 1T and 3R phases. The phase transition between low-temperature 1T phase and high-temperature 3R phase was confirmed by the powder X-ray diffraction analysis. Based on the differential thermal analysis and X-ray diffraction results, a schematic phase diagram of the Li{sub x}TiS{sub 2} system has been constructed, providing a guideline to synthesize Li{sub x}TiS{sub 2} in 1T structure or 3R structure.« less

Fabrication of MCM-41 fibers with well-ordered hexagonal mesostructure controlled in acidic and alkaline media

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

Jafarzadeh, A.; Sohrabnezhad, Sh., E-mail: sohrabnezhad@guilan.ac.ir; Zanjanchi, M.A.

In this paper, synthesis and characterization of two type morphologies of the MCM-41mesoporous material, nano and microfibers, were investigated by electrospinning technique. The synthesis was performed in acidic and alkaline media, separately. The MCM-41 morphologies were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), x-ray powder diffraction (XRD), and nitrogen adsorption–desorption measurement. Tetraethylorthosilicate (TEOS) and cetyltrimethylammonium bromide (CTAB) were used as silica and template sources for the synthesis of MCM-41 morphologies, respectively. The SEM results showed that MCM-41 nanofibers were spun in acidic media and microfibers of MCM-41 were produced in alkaline media. The XRD study revealed amore » long range structural ordering of mesoporous materials. The TEM results indicated rough surfaces with uniform average diameter 200 nm for nanofibers and 2 µm for microfibers. The pore diameter and surface area of calcined MCM-41 nanofibers were 2.2 nm and 970 m{sup 2}/g, respectively. For the MCM-41 microfibers, pore sizes of 2.7 nm and surface areas 420 m{sup 2}/g was measured. - Graphical abstract: Electrospinning method was used for fabricating of MCM-41 microfibers from TEOS in alkaline media (top) and MCM-41 nanofibers in acidic media (bottom). - Highlights: • Synthesis of MCM-41 nanofibers and microfibers by electrospinning technique. • MCM-41 nanofibers were synthesized in acidic media. • MCM-41 manofibers spun in alkaline media. • Electrospinning was a simple method for preparing of fibers with respect to chemical method.« less

A study on the production of titanium carbide nano-powder in the nanostate and its properties

NASA Astrophysics Data System (ADS)

Shiryaeva, L. S.; Rudneva, S. V.; Galevsky, G. V.; Garbuzova, A. K.

2016-09-01

The plasma synthesis of titanium carbide nano-powder in the conditions close to industrial was studied. Titanium carbide TiC is a wear- and corrosion-resistant, hard, chemically inert material, demanded in various fields for the production of hard alloys, metal- ceramic tools, heat-resistant products, protective metal coatings. New perspectives for application titanium carbide in the nanostate can be found in the field of alloys modification with different composition and destination.

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

PubMed

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

2010-02-15

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

Reduction Expansion Synthesis of Chromium and Nickel Metal Coatings

DTIC Science & Technology

2017-06-01

to a supersonic speed [24]–[25]. To prevent undesired combustion, an inert gas is required for because the gas temperature increases to 100–500°C in...take place. The metal is added by mechanical means only. In the sputtering process, an inert gas (e.g., argon) is supplied to a vacuum chamber with...technique that uses metal powder and compressed gas to feed the powder to a converging-diverging nozzle [24], as shown in Figure 5. The converging

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

Water dynamics of Ser-His-Glu-Cys-Asn powder and effects of moisture absorption on its chemical properties.

PubMed

Lin, Songyi; Xue, Peiyu; Yang, Shuailing; Li, Xingfang; Dong, Xiuping; Chen, Feng

2017-08-01

This study has elucidated moisture dynamics in the soybean peptide, Ser-His-Glu-Cys-Asn (SHECN) powder by using dynamic vapor sorption (DVS) and nuclear magnetic resonance (NMR). We also tried to investigate the effects of moisture absorption on the biological activity and chemical properties of SHECN with some effective methods such as mid-infrared (MIR) spectroscopy and gas chromatography-mass spectrometry (GC-MS). DVS results showed that the moisture absorption of SHECN could reach a maximum of 33%, and the SHECN powder after synthesis actually existed in a trihydrate state of SHECN.3H 2 O. Low-field NMR revealed that three water proportions including strong combined water, binding water and bulk water were involved in SHECN moisture absorption and absored water dominantly existed in the form of combined water. Magnetic resonance imaging (MRI) and MIR spectroscopy results indicated that moisture absorption could change the morphology and structure of SHECN. After moisture absorption at 50% and 75% relative humidity, 19 volatiles were identified by GC-MS analysis. Additionally, this study showed that a part of reductive groups in SHECN was oxidized and its antioxidant ability declined significantly (P < 0.05) after moisture absorption. Water absorbed into SHECN powder can significantly change its microstructure and cause its activity to decrease. We must prevent SHECN from absorbing moisture during storage because the water can accelerate the oxidation of samples and promote microbial reactions. © 2016 Society of Chemical Industry. © 2016 Society of Chemical Industry.

Synthesis and modification of nano-sized TiO{sub 2} for photo-degradation process under visible light irradiation; a Placket–Burman experimental design

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

Izadyar, Soheila; Fatemi, Shohreh, E-mail: shfatemi@ut.ac.ir; Mousavand, Tahereh

2013-09-01

Graphical abstract: - Highlights: • Nanosized TiO{sub 2} doped with nitrogen and iron was produced by sol-gel method. • Linear models were derived to relate the phase and particle size to synthesis factors. • High photocatalytic activity was observed for acetaldehyde degradation. - Abstract: In this research, nitrogen and iron (III) co-doped nano TiO{sub 2} (N-Fe-TiO{sub 2}) was prepared by sol-gel method using ammonium chloride and iron chloride solutions as nitrogen and iron sources, respectively. The effect of synthesis parameters (weight ratios of N/TiO{sub 2} and Fe/TiO{sub 2}, synthesis temperature, calcination time and temperature) was simultaneously investigated on the qualitymore » of the N-Fe-TiO{sub 2} product by a two-level Placket–Burman experimental design. The synthesized powders were characterized by XRD, XPS and UV–Vis spectroscopy techniques. The mean crystal size and anatase content were determined and evaluated as the linear functions of so-called synthesis parameters by the statistical analysis and regression. The 2%N-1%Fe-TiO{sub 2} product by 11 nm mean crystal size and 78% anatase content, synthesized at 35 °C and calcined at 500 °C during 2 h, exhibited the most significant activity during the photo-degradation of acetaldehyde under visible light irradiation and its efficiency was obtained about four times more than photocatalytic activity of Degussa TiO{sub 2}-P25.« less

Geloina coaxans shell as calcium source on synthesis hydroxyapatite

NASA Astrophysics Data System (ADS)

Yanti, P. H.; Kamiah, A.

2018-04-01

Geloina coaxans shell (GCS) is one of mullusc shell mainly composed by calcium carbonate. In this work, calcium carbonate has been converted to calcium oxide by calcination at 1000°C for 12 hours. The calcined of geloina coaxans shell were treated with HNO3 to produce Ca(NO3)2 as calcium source on synthesis hydroxyapatite. Orthophosphoric acid (H3PO4) was used as phosphate donor. Reaction of Ca/P has been done by precipitation method at molar ratio of precursors of 1.67 and pH adjusted at 10 using NH4OH. The XRD result revealed that hydoxyapatite can be prepared at 3 M of HNO3 and stirring time for 240 minutes. Specific band of hydroxyapatite such as PO4 and OH observed using FTIR instrument. Analysis of crystal size using Schererr equation proved nanosize of powder hydroxyapatite can be produced.

Synthesis of NiO nanotubes for use as negative electrodes in lithium ion batteries

NASA Astrophysics Data System (ADS)

Needham, S. A.; Wang, G. X.; Liu, H. K.

Nickel oxide (NiO) nanotubes have been produced for the first time via a template processing method. The synthesis involved a two step chemical reaction in which nickel hydroxide (Ni(OH) 2) nanotubes were firstly formed within the walls of an anodic aluminium oxide (AAO) template. The template was then dissolved away using concentrated NaOH, and the freed nanotubes were converted to NiO by heat treatment in air at 350 °C. Individual nanotubes measured 60 μm in length with a 200 nm outer diameter and a wall thickness of 20-30 nm. The NiO nanotube powder was used in Li-ion cells for assessment of the lithium storage ability. Preliminary testing indicates that the cells demonstrate controlled and sustainable lithium diffusion after the formation of an SEI. Reversible capacities in the 300 mAh g -1 range were typical.

Synthesis of imine bond containing insoluble polymeric ligand and its transition metal complexes, structural characterization and catalytic activity on esterification reaction.

PubMed

Gönül, İlyas; Ay, Burak; Karaca, Serkan; Saribiyik, Oguz Yunus; Yildiz, Emel; Serin, Selahattin

2017-01-01

In this study, synthesis of insoluble polymeric ligand (L) and its transition metal complexes [Cu(L)Cl 2 ]·2H 2 O (1) , [Co(L)Cl 2 (H 2 O) 2 ] (2) and [Ni(L)Cl 2 (H 2 O) 2 ] (3) , having the azomethine groups, were synthesized by the condensation reactions of the diamines and dialdehydes. The structural properties were characterized by the analytical and spectroscopic methods using by elemental analysis, Fourier Transform Infrared, Thermo Gravimetric Analysis, Powder X-ray Diffraction, magnetic susceptibility and Inductively Coupled Plasma. The solubilities of the synthesized polymeric materials were also investigated and found as insoluble some organic and inorganic solvents. Additionally, their catalytic performance was carried out for the esterification reaction of acetic acid and butyl acetate. The highest conversion rate is 75.75% by using catalyst 1 . The esterification of butanol gave butyl acetate with 100% selectivity.

Synthesis of microspheres of triuranium octaoxide by simultaneous water and nitrate extraction from ascorbate-uranyl sols.

PubMed

Brykala, M; Deptula, A; Rogowski, M; Lada, W; Olczak, T; Wawszczak, D; Smolinski, T; Wojtowicz, P; Modolo, G

A new method for synthesis of uranium oxide microspheres (diameter <100 μm) has been developed. It is a variant of our patented Complex Sol-Gel Process, which has been used to synthesize high-quality powders of a wide variety of complex oxides. Starting uranyl-nitrate-ascorbate sols were prepared by addition of ascorbic acid to uranyl nitrate hexahydrate solution and alkalizing by aqueous ammonium hydroxide and then emulsified in 2-ethylhexanol-1 containing 1v/o SPAN-80. Drops of emulsion were firstly gelled by extraction of water by the solvent. Destruction of the microspheres during thermal treatment, owing to highly reactive components in the gels, requires modification of the gelation step by Double Extraction Process-simultaneously extraction of water and nitrates using Primene JMT, which completely eliminates these problem. Final step was calcination in air of obtained microspheres of gels to triuranium octaoxide.

MOF-5 decorated hierarchical ZnO nanorod arrays and its photoluminescence

NASA Astrophysics Data System (ADS)

Zhang, Yinmin; Lan, Ding; Wang, Yuren; Cao, He; Jiang, Heng

2011-04-01

The strategy to manipulate nanoscale materials into well-organized hierarchical architectures is very important to both material synthesis and nanodevice applications. Here, nanoscale MOF-5 crystallites were successfully fabricated onto ordered hierarchical ZnO arrays based on aqueous chemical synthesis and molecule self-assembly technology guided room temperature diffusion method, which has the advantages of energy saving and simple operation. The structures and morphologies of the samples were performed by X-ray powder diffraction and field emission scanning electronic microscopy. The MOF-5 crystallites have good quality and bind well to the hexagonal-patterned ZnO arrays. The photoluminescence spectrum shows that the emission of hybrid MOF-5-ZnO films displays a blue shift in green emission and intensity reduction in UV emission. This ordered hybrid semiconductor material is expected to exploit the great potentiality in sensors, micro/nanodevices, and screen displays.

Molten Salt Synthesis and Structural Characterization of BaTiO3 Nanocrystal Ceramics

NASA Astrophysics Data System (ADS)

Ahda, S.; Misfadhila, S.; Parikin, P.; Putra, T. Y. S. P.

2017-02-01

A new synthesis route to obtain high-purity barium titanate powder, BaTiO3, using the molten salt method by reacting the raw materials (BaCO3 and TiO2) in an atmosphere of molten NaCl and KCl, has been developed. The synthesized BaTiO3 ceramic particles have been successfully carried out at the sintering temperature 950°C for 4 hours. The Rietveld refinement of the XRD diffraction patterns was employed to characterize the structural information of the nanocrystalline BaTiO3 ceramics. The lattice parameters (a=4.0043 Å, b=4.0308Å with space group P4mm) of tetragonal perovskite structure, as an indication of piezoelectric characteristics, have been successfully determined by the Rietveld refinement. While the crystallitte particle size and strains have been obtained for the values of 110.6 nm and 0.74 % respectively

Bio-green synthesis of Fe doped SnO2 nanoparticle thin film

NASA Astrophysics Data System (ADS)

Gattu, Ketan P.; Ghule, Kalyani; Huse, Nanasaheb P.; Dive, Avinash S.; Bagul, Sagar B.; Digraskar, Renuka V.; Sharma, Ramphal; Ghule, Anil V.

2017-05-01

Herein Fe doped SnO2 nanoparticles have been synthesized using simple, cost effective and ecofriendly biosynthesis method, in which remnant water (ideally kitchen waste) collected from soaked Bengal gram beans (Cicer arietinum L.) was used. This extract consists of different bio-molecules which acted as complexing as well as capping agents for synthesis of Fe-doped SnO2 nanoparticles. The X-ray powder diffraction (XRD) and Field-emission scanning electron microscopy (FE-SEM) revealed uniform size distribution with the average size of 6 nm and confirmed the formation of rutile structure with space group (P42/mnm) and nanocrystalline nature of the products with spherical morphology. Further, the gas sensing properties of the materials have been studied in comparison with other gases. The reported gas sensing results are promising, which suggest that the Fe-dopant is a promising noble metal additives to fabricate low cost SnO2 based sensor.

Synthesis, crystal growth and studies on non-linear optical property of new chalcones

NASA Astrophysics Data System (ADS)

Sarojini, B. K.; Narayana, B.; Ashalatha, B. V.; Indira, J.; Lobo, K. G.

2006-09-01

The synthesis, crystal growth and non-linear optical (NLO) property of new chalcone derivatives are reported. 4-Propyloxy and 4-butoxy benzaldehydes were made to under go Claisen-Schmidt condensation with 4-methoxy, 4-nitro and 4-phenoxy acetophenones to form corresponding chalcones. The newly synthesized compounds were characterized by analytical and spectral data. The Second harmonic generation (SHG) efficiency of these compounds was measured by powder technique using Nd:YAG laser. Among tested compounds three chalcones showed NLO property. The chalcone 1-(4-methoxyphenyl)-3-(4-propyloxy phenyl)-2-propen-1-one exhibited SHG conversion efficiency 2.7 times that of urea. The bulk crystal of 1-(4-methoxyphenyl)-3-(4-butoxyphenyl)-2-propen-1-one (crystal size 65×28×15 mm 3) was grown by slow-evaporation technique from acetone. Microhardness of the crystal was tested by Vicker's microhardness method.