High pressure synthesis and investigations of properties of boron allotropes and boron carbide

Energy Technology Data Exchange (ETDEWEB)

Chuvashova, Irina

2017-06-12

This work aimed at the development of the high-pressure high-temperature (HPHT) synthesis of single crystals of boron allotropes and boron-rich compounds, which could be used further for precise investigations of their structures, properties, and behavior at extreme conditions. To summarize, the present work resulted in the HPHT synthesis of the first previously unknown non-icosahedral boron allotrope ζ-B. This finding confirmed earlier theoretical predictions, which stayed unproven for decades because of experimental challenges which couldn't be overcome until recently. Structural stability of α-B and β-B in the Mbar pressure range and B{sub 13}C{sub 2} up to 68 GPa was experimentally proven. Accurate measurements of the unit cell and B{sub 12} icosahedra volumes of the stoichiometric boron carbide B{sub 13}C{sub 2} as a function of pressure led to conclusion that they undergo a similar reduction upon compression that is typical for covalently bonded solids. Neither 'molecular-like' nor 'inversed molecular-like' solid behavior upon compression was detected that has closed a long-standing scientific dispute. A comparison of the compressional behavior of B{sub 13}C{sub 2} with that of α-B and γ-B allotropes and B{sub 4}C showed that it is determined by the types of bonding involved in the course of compression.

The effect of High Pressure and High Temperature processing on carotenoids and chlorophylls content in some vegetables.

Science.gov (United States)

Sánchez, Celia; Baranda, Ana Beatriz; Martínez de Marañón, Iñigo

2014-11-15

The effect of High Pressure (HP) and High Pressure High Temperature (HPHT) processing on carotenoid and chlorophyll content of six vegetables was evaluated. In general, carotenoid content was not significantly influenced by HP or HPHT treatments (625 MPa; 5 min; 20, 70 and 117 °C). Regarding chlorophylls, HP treatment caused no degradation or slight increases, while HPHT processes degraded both chlorophylls. Chlorophyll b was more stable than chlorophyll a at 70 °C, but both of them were highly degraded at 117 °C. HPHT treatment at 117 °C provided products with a good retention of carotenoids and colour in the case of red vegetables. Even though the carotenoids also remained in the green vegetables, their chlorophylls and therefore their colour were so affected that milder temperatures need to be applied. As an industrial scale equipment was used, results will be useful for future industrial implementation of this technology. Copyright © 2014 Elsevier Ltd. All rights reserved.

Required developments towards ultra high pressure and temperature subsea tree system solutions

Energy Technology Data Exchange (ETDEWEB)

Queseth, Per-Olaf

2010-07-01

For the subsea High Pressure High Temperature oil and gas production systems, the primary challenge is to provide good, reliable solutions for HPHT reservoir exploitation based on an overview of parameters for already discovered potential fields. The paper will present a resume of Aker Solutions' previous development in this area exemplified with experiences from testing and operator observations during production start of HPHT fields in the North Sea. Further improvements are required to comply with the extreme pressures and temperatures sought to overcome. 'The Devil is in the details' is a very relevant proverb. A program to qualify subsea production X-mas trees for Ultra HPHT use will be presented with highlight on sealing systems, feed-through solutions and materials as well as impact on interfacing systems. Preliminary and intermediate analytical and test results will be presented and remaining activities summarised. (Author)

High-pressure high-temperature phase diagram of organic crystal paracetamol

Science.gov (United States)

Smith, Spencer J.; Montgomery, Jeffrey M.; Vohra, Yogesh K.

2016-01-01

High-pressure high-temperature (HPHT) Raman spectroscopy studies have been performed on the organic crystal paracetamol in a diamond anvil cell utilizing boron-doped heating diamond anvil. Isobaric measurements were conducted at pressures up to 8.5 GPa and temperature up to 520 K in five different experiments. Solid state phase transitions from monoclinic Form I  →  orthorhombic Form II were observed at various pressures and temperatures as well as transitions from Form II  →  unknown Form IV. The melting temperature for paracetamol was observed to increase with increasing pressures to 8.5 GPa. This new data is combined with previous ambient temperature high-pressure Raman and x-ray diffraction data to create the first HPHT phase diagram of paracetamol.

High-pressure high-temperature phase diagram of organic crystal paracetamol

International Nuclear Information System (INIS)

Smith, Spencer J; Montgomery, Jeffrey M; Vohra, Yogesh K

2016-01-01

High-pressure high-temperature (HPHT) Raman spectroscopy studies have been performed on the organic crystal paracetamol in a diamond anvil cell utilizing boron-doped heating diamond anvil. Isobaric measurements were conducted at pressures up to 8.5 GPa and temperature up to 520 K in five different experiments. Solid state phase transitions from monoclinic Form I  →  orthorhombic Form II were observed at various pressures and temperatures as well as transitions from Form II  →  unknown Form IV. The melting temperature for paracetamol was observed to increase with increasing pressures to 8.5 GPa. This new data is combined with previous ambient temperature high-pressure Raman and x-ray diffraction data to create the first HPHT phase diagram of paracetamol. (paper)

Synthesis of diamonds in Fe–C systems using nitrogen and hydrogen co-doped impurities under HPHT

International Nuclear Information System (INIS)

Sun Shi-Shuai; Xu Zhi-Hui; Cui Wen; Jia Xiao-Peng; Ma Hong-An

2017-01-01

In this study, we investigate the effect of nitrogen and hydrogen impurities on colors, morphologies, impurity structures and synthesis conditions of diamond crystals in Fe–C systems with C 3 N 6 H 6 additives at pressures in the range 5.0–6.5 GPa and temperatures of 1400–1700 °C in detail. Our results reveal that the octahedron diamond nucleation in a Fe–C system is evidently inhibited by co-doped N–H elements, thereby resulting in the increase of minimum pressure and temperature of diamond synthesis by spontaneous nucleation. The octahedron diamond crystals synthesized from a pure Fe–C system are colorless, while they become green in the system with C 3 N 6 H 6 additive. The surface defects of diamond will deteriorate when the nitrogen and hydrogen atoms simultaneously incorporate in the diamond growth environment in the Fe–C system. We believe that this study will provide some important information and be beneficial for the deep understanding of the crystallization of diamonds from different component systems. (paper)

High-Pressure High-Temperature Phase Diagram of the Organic Crystal Paracetamol

Science.gov (United States)

Smith, Spencer; Montgomery, Jeffrey; Vohra, Yogesh

High-pressure high-temperature (HPHT) Raman spectroscopy studies have been performed on the organic crystal paracetamol in a diamond anvil cell utilizing boron-doped diamond as heating anvil. The HPHT data obtained from boron-doped diamond heater is cross-checked with data obtained using a standard block heater diamond anvil cell. Isobaric measurements were conducted at pressures up to 8.5 GPa and temperature up to 520 K in a number of different experiments. Solid state phase transitions from monoclinic Form I --> orthorhombic Form II were observed at various pressures and temperatures as well as transitions from Form II --> unknown Form IV. The melting temperature for paracetamol was observed to increase with increasing pressures to 8.5 GPa. Our previous angle dispersive x-ray diffraction studies at the Advanced Photon Source has confirmed the existence of two unknown crystal structures Form IV and Form V of paracetamol at high pressure and ambient temperature. The phase transformation from Form II to Form IV occurs at ~8.5 GPa and from Form IV to Form V occurs at ~11 GPa at ambient temperature. Our new data is combined with the previous ambient temperature high-pressure Raman and X- ray diffraction data to create the first HPHT phase diagram of paracetamol. Doe-NNSA Carnegie DOE Alliance Center (CDAC) under Grant Number DE-NA0002006.

Stability of Basalt plus Anhydrite plus Calcite at HP-HT: Implications for Venus, the Earth and Mars

Science.gov (United States)

Martin, A. M.; Righter, K.; Treiman, A. H.

2010-01-01

"Canali" observed at Venus surface by Magellan are evidence for very long melt flows, but their composition and origin remain uncertain. The hypothesis of water-rich flow is not reasonable regarding the temperature at Venus surface. The length of these channels could not be explained by a silicate melt composition but more likely, by a carbonate-sulfate melt which has a much lower viscosity (Kargel et al 1994). One hypothesis is that calcite CaCO3 and anhydrite CaSO4 which are alteration products of basalts melted during meteorite impacts. A famous example recorded on the Earth (Chicxulub) produced melt and gas rich in carbon and sulfur. Calcite and sulfate evaporites are also present on Mars surface, associated with basalts. An impact on these materials might release C- and S-rich melt or fluid. Another type of planetary phenomenon (affecting only the Earth) might provoke a high pressure destabilization of basalt+anhydrite+calcite. Very high contents of C and S are measured in some Earth s magmas, either dissolved or in the form of crystals (Luhr 2008). As shown by the high H content and high fO2 of primary igneous anhydrite-bearing lavas, the high S content in their source may be explained by subduction of an anhydrite-bearing oceanic crust, either directly (by melting followed by eruption) or indirectly (by release of S-rich melt or fluid that metasomatize the mantle) . Calcite is a major product of oceanic sedimentation and alteration of the crust. Therefore, sulfate- and calcite-rich material may be subducted to high pressures and high temperatures (HP-HT) and release S- and C-rich melts or fluids which could influence the composition of subduction zone lavas or gases. Both phenomena - meteorite impact and subduction - imply HP-HT conditions - although the P-T-time paths are different. Some HP experimental/theoretical studies have been performed on basalt/eclogite, calcite and anhydrite separately or on a combination of two. In this study we performed piston

Rheological assessment of nanofluids at high pressure high temperature

Science.gov (United States)

Kanjirakat, Anoop; Sadr, Reza

2013-11-01

High pressure high temperature (HPHT) fluids are commonly encountered in industry, for example in cooling and/or lubrications applications. Nanofluids, engineered suspensions of nano-sized particles dispersed in a base fluid, have shown prospective as industrial cooling fluids due to their enhanced rheological and heat transfer properties. Nanofluids can be potentially utilized in oil industry for drilling fluids and for high pressure water jet cooling/lubrication in machining. In present work rheological characteristics of oil based nanofluids are investigated at HPHT condition. Nanofluids used in this study are prepared by dispersing commercially available SiO2 nanoparticles (~20 nm) in a mineral oil. The basefluid and nanofluids with two concentrations, namely 1%, and 2%, by volume, are considered in this investigation. The rheological characteristics of base fluid and the nanofluids are measured using an industrial HPHT viscometer. Viscosity values of the nanofluids are measured at pressures of 100 kPa to 42 MPa and temperatures ranging from 25°C to 140°C. The viscosity values of both nanofluids as well as basefluid are observed to have increased with the increase in pressure. Funded by Qatar National Research Fund (NPRP 08-574-2-239).

Analysis of the structural stability of the smectite submitted to high pressures and temperatures

International Nuclear Information System (INIS)

Alabarse, Frederico Gil

2009-10-01

The thermal stability of bentonite is of particular interest for containment barrier in nuclear waste disposal facilities. However, very little is known about the stability of smectite (principal component of bentonite) under high-pressure and high-temperature conditions (HPHT). The objective of this work was to investigate the stability of the smectite structure under HP-HT conditions. The HP-HT experiments were performed on toroidal chambers (TC) with pressure up 7.7 GPa and temperatures of 1000 deg C. The samples were characterized by X-ray diffraction after the HP-HT processing. Furthermore, one sample from the original material was analyzed using Fourier transformed infra-red (FTIR) in situ measurements on a diamond anvil cell (DAC) in experiments up to 12 GPa. The original sample of bentonite, calcium dioctahedral montmorillonite with small fraction of quartz, was characterized by FTIR, XRD, X-ray fluorescence (XRF), scanning electron microscopy (SEM), surface area, thermogravimetric analysis (TGA) and differential thermal analysis (DTA). In the experiment performed using the DAC up to 12 GPa, the FTIR in situ measurements analysis showed that the smectite structure is stable with a reversible deformation in the Si-O bond and that the smectite did not loose water. Experiments performed in TC at 7.7 GPa of pressure and 250 deg C of temperature, during 3.5 h showed, after analysis by XRD and FTIR, that the smectite structure is stable and did not loose water. Experiments performed in TC at 7.7 GPa of pressure and 1000 deg C of temperature, during 3.5 h showed, after analysis by XRD and SEM, the transformation of bentonite to the mineral assemblage: Coesite, Quartz, Kyanite and Pyrope. (author)

Plasma synthesis and HPHT consolidation of BN nanoparticles, nanospheres, and nanotubes to produce nanocrystalline cubic boron nitride

Science.gov (United States)

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.

XPS analysis for cubic boron nitride crystal synthesized under high pressure and high temperature using Li3N as catalysis

International Nuclear Information System (INIS)

Guo, Xiaofei; Xu, Bin; Zhang, Wen; Cai, Zhichao; Wen, Zhenxing

2014-01-01

Highlights: • The cBN was synthesized by Li 3 N as catalyst under high pressure and high temperature (HPHT). • The film coated on the as-grown cBN crystals was studied by XPS. • The electronic structure variation in the film was investigated. • The growth mechanism of cubic boron nitride crystal was analyzed briefly. - Abstract: Cubic boron nitride (cBN) single crystals are synthesized with lithium nitride (Li3N) as catalyst under high pressure and high temperature. The variation of electronic structures from boron nitride of different layers in coating film on the cBN single crystal has been investigated by X-ray photoelectron spectroscopy. Combining the atomic concentration analysis, it was shown that from the film/cBN crystal interface to the inner, the sp 2 fractions are decreasing, and the sp 3 fractions are increasing in the film at the same time. Moreover, by transmission electron microscopy, a lot of cBN microparticles are found in the interface. For there is no Li 3 N in the film, it is possible that Li 3 N first reacts with hexagonal boron nitride to produce Li 3 BN 2 during cBN crystals synthesis under high pressure and high temperature (HPHT). Boron and nitrogen atoms, required for cBN crystals growth, could come from the direct conversion from hexagonal boron nitride with the catalysis of Li 3 BN 2 under high pressure and high temperature, but not directly from the decomposition of Li 3 BN 2

Analysis of the structural stability of the smectite submitted to high pressures and temperatures; Analise da estabilidade estrutural da esmectita sob altas pressoes e altas temperaturas

Energy Technology Data Exchange (ETDEWEB)

Alabarse, Frederico Gil

2009-10-15

The thermal stability of bentonite is of particular interest for containment barrier in nuclear waste disposal facilities. However, very little is known about the stability of smectite (principal component of bentonite) under high-pressure and high-temperature conditions (HPHT). The objective of this work was to investigate the stability of the smectite structure under HP-HT conditions. The HP-HT experiments were performed on toroidal chambers (TC) with pressure up 7.7 GPa and temperatures of 1000 deg C. The samples were characterized by X-ray diffraction after the HP-HT processing. Furthermore, one sample from the original material was analyzed using Fourier transformed infra-red (FTIR) in situ measurements on a diamond anvil cell (DAC) in experiments up to 12 GPa. The original sample of bentonite, calcium dioctahedral montmorillonite with small fraction of quartz, was characterized by FTIR, XRD, X-ray fluorescence (XRF), scanning electron microscopy (SEM), surface area, thermogravimetric analysis (TGA) and differential thermal analysis (DTA). In the experiment performed using the DAC up to 12 GPa, the FTIR in situ measurements analysis showed that the smectite structure is stable with a reversible deformation in the Si-O bond and that the smectite did not loose water. Experiments performed in TC at 7.7 GPa of pressure and 250 deg C of temperature, during 3.5 h showed, after analysis by XRD and FTIR, that the smectite structure is stable and did not loose water. Experiments performed in TC at 7.7 GPa of pressure and 1000 deg C of temperature, during 3.5 h showed, after analysis by XRD and SEM, the transformation of bentonite to the mineral assemblage: Coesite, Quartz, Kyanite and Pyrope. (author)

Identification of paramagnetic nitrogen centers (P1) in diamond crystallites synthesized via the sintering of detonation nanodiamonds at high pressure and temperature

Science.gov (United States)

Osipov, V. Yu.; Shakhov, F. M.; Efimov, N. N.; Minin, V. V.; Kidalov, S. V.; Vul', A. Ya.

2017-06-01

Diamond single crystals synthesized from powder detonation nanodiamonds (DNDs) by means of treatment at high pressures ( P 7 GPa) and temperatures ( T > 1300°C) have been studied by electron paramagnetic resonance (EPR). A key feature of treatment (high-pressure high-temperature (HPHT) sintering) is the use of low molecular weight alcohols in the process. The appearance of a hyperfine EPR signal structure due to "paramagnetic nitrogen" (P1 centers) is explained by the growth of submicron and micron diamond single crystals from DND nanocrystals by the oriented attachment and coalescence mechanism. Such growth and coarsening of crystals appreciably decreases the concentration of paramagnetic centers, the presence of which hinders the detection of a hyperfine structure in the EPR signal from P1 centers, in the near-surface areas of coalesced and grown together DND particles. It has been shown that the concentration of paramagnetic defects of all types decreases to 3.1 × 1018 g-1 ( 60 ppm) during HPHT treatment at T = 1650°C. This causes the successful identification of P1 centers, whose fraction is no less than 40% of the total amount of paramagnetic centers in microcrystals synthesized by HPHT sintering.

Low-temperature synthesis of silicon carbide powder using shungite

International Nuclear Information System (INIS)

Gubernat, A.; Pichor, W.; Lach, R.; Zientara, D.; Sitarz, M.; Springwald, M.

2017-01-01

The paper presents the results of investigation the novel and simple method of synthesis of silicon carbide. As raw material for synthesis was used shungite, natural mineral rich in carbon and silica. The synthesis of SiC is possible in relatively low temperature in range 1500–1600°C. It is worth emphasising that compared to the most popular method of SiC synthesis (Acheson method where the temperature of synthesis is about 2500°C) the proposed method is much more effective. The basic properties of products obtained from different form of shungite and in wide range of synthesis temperature were investigated. The process of silicon carbide formation was proposed and discussed. In the case of synthesis SiC from powder of raw materials the product is also in powder form and not requires any additional process (crushing, milling, etc.). Obtained products are pure and after grain classification may be used as abrasive and polishing powders. (Author)

Low-temperature synthesis of silicon carbide powder using shungite

Energy Technology Data Exchange (ETDEWEB)

Gubernat, A.; Pichor, W.; Lach, R.; Zientara, D.; Sitarz, M.; Springwald, M.

2017-07-01

The paper presents the results of investigation the novel and simple method of synthesis of silicon carbide. As raw material for synthesis was used shungite, natural mineral rich in carbon and silica. The synthesis of SiC is possible in relatively low temperature in range 1500–1600°C. It is worth emphasising that compared to the most popular method of SiC synthesis (Acheson method where the temperature of synthesis is about 2500°C) the proposed method is much more effective. The basic properties of products obtained from different form of shungite and in wide range of synthesis temperature were investigated. The process of silicon carbide formation was proposed and discussed. In the case of synthesis SiC from powder of raw materials the product is also in powder form and not requires any additional process (crushing, milling, etc.). Obtained products are pure and after grain classification may be used as abrasive and polishing powders. (Author)

Evaluation des fluides de forage HP/HT pour forages profonds Evaluation of Hp/Ht Drilling Fluid Formulations for Deep Drilling

Directory of Open Access Journals (Sweden)

Argillier J. F.

2006-11-01

Full Text Available Le forage de puits profonds exige la mise au point de fluides de forage dont la formulation est adaptée aux températures élevées de formation : l'une des principales difficultés est la dégradation thermique des additifs chimiques utilisés dans les formulations à base d'eau qui se produit fréquemment lors du forage de puits à température élevée. Cette dégradation peut conduire à des variations importantes des caractéristiques rhéologiques et de filtration et à une perte de propriétés nécessaires à leur performance. De plus, même s'il n'y a pas de dégradation des composants la viscosité des solutions de polymères hydrosolubles couramment utilisés dans les formulations de fluides diminue fortement avec l'augmentation de la température au-dessus de 60°C. Une autre source de difficulté qui apparaît à forte température avec les boues à base d'eau est la gélification des argiles utilisées dans la formulation. Ce phénomène provoque une forte augmentation de la viscosité de la formulation et des pertes de charges, en particulier en cas de reprise de forage. Diverses méthodes ont été mises au point pour étudier le comportement des boues à base d'eau dans des conditions de pression et de température élevées, entre autres : - des expériences de laboratoire, pour étudier par exemple la stabilité en conditions anaérobies des solutions de polymères et le comportement rhéologique des suspensions d'argile dans des conditions de pression et de température élevées afin de simuler les caractéristiques de gélification des argiles à haute température; - des essais sur boucle d'étude HP/HT en utilisant une boucle expérimentale conçue pour étudier les fluides de forage dans des conditions de fond réalistes, c'est-à-dire des températures atteignant 180°C, des pressions atteignant 500 bar et des taux de cisaillement atteignant 10 000 s puissance( -1 Cette méthodologie a permis d'étudier un certain

Vacancy-impurity centers in diamond: prospects for synthesis and applications

Science.gov (United States)

Ekimov, E. A.; Kondrin, M. V.

2017-06-01

The bright luminescence of impurity-vacancy complexes, combined with high chemical and radiation resistance, makes diamond an attractive platform for the production of single-photon emitters and luminescent biomarkers for applications in nanoelectronics and medicine. Two representatives of this kind of defects in diamond, silicon-vacancy (SiV) and germanium-vacancy (GeV) centers, are discussed in this review; their similarities and differences are demonstrated in terms of the more thoroughly studied nitrogen-vacancy (NV) complexes. The recent discovery of GeV luminescent centers opens a unique opportunity for the controlled synthesis of single-photon emitters in nanodiamonds. We demonstrate prospects for the high-pressure high-temperature (HPHT) technique to create single-photon emitters, not only as an auxiliary to chemical vapor deposition (CVD) and ion-implantation methods but also as a primary synthesis tool for producing color centers in nanodiamonds. Besides practical applications, comparative studies of these two complexes, which belong to the same structural class of defects, have a fundamental importance for deeper understanding of shelving levels, the electronic structure, and optical properties of these centers. In conclusion, we discuss several open problems regarding the structure, charge state, and practical application of these centers, which still require a solution.

Prediction and experimental determination of the solubility of exotic scales at high temperatures - Zinc sulfide

DEFF Research Database (Denmark)

Carolina Figueroa Murcia, Diana; Fosbøl, Philip Loldrup; Thomsen, Kaj

2016-01-01

The presence of "exotic" scale such as Zinc Sulfide (ZnS), Lead Sulfide (PbS) and Iron Sulfide (FeS) in HP/HT reservoirs has been identified. "Exotic" scale materials come as a new challenge in HP/HT reservoirs. This has led to the development of more advanced tools to predict their behavior...... at extreme conditions. The aim of this work is to include ZnS into the group of scale materials that can be modeled with the Extended UNIQUAC model. Solubility data for ZnS are scarce in the open literature. In order to improve the available data, we study the experimental behavior of ZnS solubility at high...... temperatures. The determination of the solubility of ZnS is carried out at temperatures up to 250°C. Zinc sulfide (99.99%) and ultra-pure water are placed in a vial in a reduced oxygen atmosphere. The sample is placed in a controlled bath and stirred until equilibrium is attained. The suspension is filtered...

A novel high pressure, high temperature vessel used to conduct long-term stability measurements of silicon MEMS pressure transducers

Science.gov (United States)

Wisniewiski, David

2014-03-01

The need to quantify and to improve long-term stability of pressure transducers is a persistent requirement from the aerospace sector. Specifically, the incorporation of real-time pressure monitoring in aircraft landing gear, as exemplified in Tire Pressure Monitoring Systems (TPMS), has placed greater demand on the pressure transducer for improved performance and increased reliability which is manifested in low lifecycle cost and minimal maintenance downtime through fuel savings and increased life of the tire. Piezoresistive (PR) silicon MEMS pressure transducers are the primary choice as a transduction method for this measurement owing to their ability to be designed for the harsh environment seen in aircraft landing gear. However, these pressure transducers are only as valuable as the long-term stability they possess to ensure reliable, real-time monitoring over tens of years. The "heart" of the pressure transducer is the silicon MEMS element, and it is at this basic level where the long-term stability is established and needs to be quantified. A novel High Pressure, High Temperature (HPHT) vessel has been designed and constructed to facilitate this critical measurement of the silicon MEMS element directly through a process of mechanically "floating" the silicon MEMS element while being subjected to the extreme environments of pressure and temperature, simultaneously. Furthermore, the HPHT vessel is scalable to permit up to fifty specimens to be tested at one time to provide a statistically significant data population on which to draw reasonable conclusions on long-term stability. With the knowledge gained on the silicon MEMS element, higher level assembly to the pressure transducer envelope package can also be quantified as to the build-effects contribution to long-term stability in the same HPHT vessel due to its accommodating size. Accordingly, a HPHT vessel offering multiple levels of configurability and robustness in data measurement is presented, along

High-Pressure-High-Temperature Processing Reduces Maillard Reaction and Viscosity in Whey Protein-Sugar Solutions

NARCIS (Netherlands)

Avila Ruiz, Geraldine; Xi, Bingyan; Minor, Marcel; Sala, Guido; Boekel, van Tiny; Fogliano, Vincenzo; Stieger, Markus

2016-01-01

The aim of the study was to determine the influence of pressure in high-pressure-high-temperature (HPHT) processing on Maillard reactions and protein aggregation of whey protein-sugar solutions. Solutions of whey protein isolate containing either glucose or trehalose at pH 6, 7, and 9 were

Low Temperature Synthesis of Magnesium Aluminate Spinel

International Nuclear Information System (INIS)

Lebedovskaya, E.G.; Gabelkov, S.V.; Litvinenko, L.M.; Logvinkov, D.S.; Mironova, A.G.; Odejchuk, M.A.; Poltavtsev, N.S.; Tarasov, R.V.

2006-01-01

The low-temperature synthesis of magnesium-aluminum spinel is carried out by a method of thermal decomposition in combined precipitated hydrates. The fine material of magnesium-aluminium spinel with average size of coherent dispersion's area 4...5 nanometers is obtained. Magnesium-aluminum spinel and initial hydrates were investigated by methods of the differential thermal analysis, the x-ray phase analysis and measurements of weight loss during the dehydration and thermal decomposition. It is established that synthesis of magnesium-aluminum spinel occurs at temperature 300 degree C by method of the x-ray phase analysis

Industrial Coatings at Extreme Conditions

DEFF Research Database (Denmark)

Subramanian, Srinath; Pérez Hornero, Clara; Pedersen, Lars Thorslund

With the gradual depletion of oil wells operable at relatively lower temperatures and pressures, the upstream oil industry relies on High Pressure High Temperature (HPHT) wells to source crude oil and gas. HPHT well extraction and processing require anticorrosive coatings applied on substrates...

Alcohol synthesis in a high-temperature slurry reactor

Energy Technology Data Exchange (ETDEWEB)

Roberts, G.W.; Marquez, M.A.; McCutchen, M.S. [North Carolina State Univ., Raleigh, NC (United States)

1995-12-31

The overall objective of this contract is to develop improved process and catalyst technology for producing higher alcohols from synthesis gas or its derivatives. Recent research has been focused on developing a slurry reactor that can operate at temperatures up to about 400{degrees}C and on evaluating the so-called {open_quotes}high pressure{close_quotes} methanol synthesis catalyst using this reactor. A laboratory stirred autoclave reactor has been developed that is capable of operating at temperatures up to 400{degrees}C and pressures of at least 170 atm. The overhead system on the reactor is designed so that the temperature of the gas leaving the system can be closely controlled. An external liquid-level detector is installed on the gas/liquid separator and a pump is used to return condensed slurry liquid from the separator to the reactor. In order to ensure that gas/liquid mass transfer does not influence the observed reaction rate, it was necessary to feed the synthesis gas below the level of the agitator. The performance of a commercial {open_quotes}high pressure {close_quotes} methanol synthesis catalyst, the so-called {open_quotes}zinc chromite{close_quotes} catalyst, has been characterized over a range of temperature from 275 to 400{degrees}C, a range of pressure from 70 to 170 atm., a range of H{sub 2}/CO ratios from 0.5 to 2.0 and a range of space velocities from 2500 to 10,000 sL/kg.(catalyst),hr. Towards the lower end of the temperature range, methanol was the only significant product.

Synthesis of nano-sized amorphous boron powders through active dilution self-propagating high-temperature synthesis method

Energy Technology Data Exchange (ETDEWEB)

Wang, Jilin [The State Key Laboratory of Advanced Technology for Materials Synthesis and Processing, Wuhan University of Technology, Wuhan 430070 (China); Gu, Yunle [School of Material Science and Engineering, Wuhan Institute of Technology, Wuhan 430073 (China); Li, Zili [The State Key Laboratory of Advanced Technology for Materials Synthesis and Processing, Wuhan University of Technology, Wuhan 430070 (China); Wang, Weimin, E-mail: wangwm@hotmail.com [The State Key Laboratory of Advanced Technology for Materials Synthesis and Processing, Wuhan University of Technology, Wuhan 430070 (China); Fu, Zhengyi [The State Key Laboratory of Advanced Technology for Materials Synthesis and Processing, Wuhan University of Technology, Wuhan 430070 (China)

2013-06-01

Graphical abstract: Nano-sized amorphous boron powders were synthesized by active dilution self-propagating high-temperature synthesis (SHS) method. The effects of endothermic reaction rate, the possible chemical reaction mechanism and active dilution model for synthesis of the product were also discussed. Highlights: ► Nano-sized amorphous boron powders were synthesized by active dilution self-propagating high-temperature synthesis method. ► The morphology, particle size and purity of the samples could be effectively controlled via changing the endothermic rate. ► The diluter KBH{sub 4} played an important role in active dilution synthesis of amorphous nano-sized boron powders. ► The active dilution method could be further popularized and become a common approach to prepare various inorganic materials. - Abstract: Nano-sized amorphous boron powders were synthesized by active dilution self-propagating high-temperature synthesis (SHS) method at temperatures ranging from 700 °C to 850 °C in a SHS furnace using Mg, B{sub 2}O{sub 3} and KBH{sub 4} as raw materials. Samples were characterized by X-ray powder diffraction (XRD), Laser particle size analyzer, Fourier transform infrared spectra (FTIR), X-ray energy dispersive spectroscopy (EDX), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and high-resolution transmission TEM (HRTEM). The boron powders demonstrated an average particle size of 50 nm with a purity of 95.64 wt.%. The diluter KBH{sub 4} played an important role in the active dilution synthesis of amorphous nano-sized boron powders. The effects of endothermic reaction rate, the possible chemical reaction mechanism and active dilution model for synthesis of the product were also discussed.

Synthesis of nano-sized amorphous boron powders through active dilution self-propagating high-temperature synthesis method

International Nuclear Information System (INIS)

Wang, Jilin; Gu, Yunle; Li, Zili; Wang, Weimin; Fu, Zhengyi

2013-01-01

Graphical abstract: Nano-sized amorphous boron powders were synthesized by active dilution self-propagating high-temperature synthesis (SHS) method. The effects of endothermic reaction rate, the possible chemical reaction mechanism and active dilution model for synthesis of the product were also discussed. Highlights: ► Nano-sized amorphous boron powders were synthesized by active dilution self-propagating high-temperature synthesis method. ► The morphology, particle size and purity of the samples could be effectively controlled via changing the endothermic rate. ► The diluter KBH 4 played an important role in active dilution synthesis of amorphous nano-sized boron powders. ► The active dilution method could be further popularized and become a common approach to prepare various inorganic materials. - Abstract: Nano-sized amorphous boron powders were synthesized by active dilution self-propagating high-temperature synthesis (SHS) method at temperatures ranging from 700 °C to 850 °C in a SHS furnace using Mg, B 2 O 3 and KBH 4 as raw materials. Samples were characterized by X-ray powder diffraction (XRD), Laser particle size analyzer, Fourier transform infrared spectra (FTIR), X-ray energy dispersive spectroscopy (EDX), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and high-resolution transmission TEM (HRTEM). The boron powders demonstrated an average particle size of 50 nm with a purity of 95.64 wt.%. The diluter KBH 4 played an important role in the active dilution synthesis of amorphous nano-sized boron powders. The effects of endothermic reaction rate, the possible chemical reaction mechanism and active dilution model for synthesis of the product were also discussed

Catalytic chemical amide synthesis at room temperature: one more step toward peptide synthesis.

Science.gov (United States)

Mohy El Dine, Tharwat; Erb, William; Berhault, Yohann; Rouden, Jacques; Blanchet, Jérôme

2015-05-01

An efficient method has been developed for direct amide bond synthesis between carboxylic acids and amines via (2-(thiophen-2-ylmethyl)phenyl)boronic acid as a highly active bench-stable catalyst. This catalyst was found to be very effective at room temperature for a large range of substrates with slightly higher temperatures required for challenging ones. This methodology can be applied to aliphatic, α-hydroxyl, aromatic, and heteroaromatic acids as well as primary, secondary, heterocyclic, and even functionalized amines. Notably, N-Boc-protected amino acids were successfully coupled in good yields with very little racemization. An example of catalytic dipeptide synthesis is reported.

Self-sustained high-temperature reactions : Initiation, propagation and synthesis

NARCIS (Netherlands)

Martinez Pacheco, M.

2007-01-01

Self-Propagating High-Temperature Synthesis (SHS), also called combustion synthesis is an exothermic and self-sustained reaction between the constituents, which has assumed significance for the production of ceramics and ceramic-metallic materials (cermets), because it is a very rapid processing

Temperature and Pressure Effects on Drilling Fluid Rheology and ECD in Very Deep Wells

Energy Technology Data Exchange (ETDEWEB)

Rommetveit, R.; Bjoerkvoll, K.S.

1997-12-31

The rheological properties of drilling fluids are usually approximated to be independent of pressure and temperature. In many cases this is a good approximation. However, for wells with small margins between pore and fracture pressure, careful evaluations and analysis of the effects of temperature and pressure on well bore hydraulics and kick probability are needed. In this publication the effects of pressure and temperature are discussed and described for typical HPHT (High Pressure High Temperature) wells. Laboratory measurements show that rheology is very pressure and temperature dependent. The practical implications of these observations are illustrated through a series of calculations with an advanced pressure and temperature simulator. 10 refs., 15 figs.

Low-Temperature Synthesis Routes to Intermetallic Superconductors

Energy Technology Data Exchange (ETDEWEB)

Schaak, Raymond E

2008-01-08

Over the past few years, our group has gained expertise at developing low-temperature solution-based synthetic pathways to complex nanoscale solids, with particular emphasis on nanocrystalline intermetallic compounds. Our synthetic capabilities are providing tools to reproducibly generate intermetallic nanostructures with simultaneous control over crystal structure, composition, and morphology. This DOE-funded project aims to expand these capabilities to intermetallic superconductors. This could represent an important addition to the tools that are available for the synthesis and processing of intermetallic superconductors, which traditionally utilize high-temperature, high-pressure, thin film, or gas-phase vacuum deposition methods. Our current knowledge of intermetallic superconductors suggests that significant enhancements could result from the inherent benefits of low-temperature solution synthesis, e.g. metastable phase formation, control over nanoscale morphology to facilitate size-dependent property studies, robust and inexpensive processability, low-temperature annealing and consolidation, and impurity incorporation (for doping, stoichiometry control, flux pinning, and improving the critical fields). Our focus is on understanding the superconducting properties as a function of synthetic route, crystal structure, crystallite size, and morphology, and developing the synthetic tools necessary to accomplish this. This research program can currently be divided into two classes of superconducting materials: intermetallics (transition metal/post transition metal) and metal carbides/borides. Both involve the development and exploitation of low-temperature synthesis routes followed by detailed characterization of structures and properties, with the goal of understanding how the synthetic pathways influence key superconducting properties of selected target materials. Because of the low-temperature methods used to synthesize them and the nanocrystalline morphologies

Protein synthesis during the initial phase of the temperature-induced bleaching response in Euglena gracilis

International Nuclear Information System (INIS)

Ortiz, W.

1990-01-01

Growing cultures of photoheterotrophic Euglena gracilis experience an increase in chlorophyll accumulation during the initial phase of the temperature-induced bleaching response suggesting an increase in the synthesis of plastid components at the bleaching temperature of 33 degree C. A primary goal of this work was to establish whether an increase in the synthesis of plastid proteins accompanies the observed increase in chlorophyll accumulation. In vivo pulse-labeling experiments with [ 35 S]sodium sulfate were carried out with cells grown at room temperature or at 33 degree C. The synthesis of a number of plastid polypeptides of nucleocytoplasmic origin, including some presumably novel polypeptides, increased in cultures treated for 15 hours at 33 degree C. In contrast, while synthesis of thylakoid proteins by the plastid protein synthesis machinery decreased modestly, synthesis of the large subunit of the enzyme ribulosebisphosphate carboxylase was strongly affected at the elevated temperature. Synthesis of novel plastid-encoded polypeptides was not induced at the bleaching temperature. It is concluded that protein synthesis in plastids declines during the initial phase of the temperature response in Euglena despite an overall increase in cellular protein synthesis and an increase in chlorophyll accumulation per cell

Multi-Temperature Zone, Droplet-based Microreactor for Increased Temperature Control in Nanoparticle Synthesis

KAUST Repository

Erdem, E. Yegân

2013-12-12

Microreactors are an emerging technology for the controlled synthesis of nanoparticles. The Multi-Temperature zone Microreactor (MTM) described in this work utilizes thermally isolated heated and cooled regions for the purpose of separating nucleation and growth processes as well as to provide a platform for a systematic study on the effect of reaction conditions on nanoparticle synthesis. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Ruthenium(V) oxides from low-temperature hydrothermal synthesis

Energy Technology Data Exchange (ETDEWEB)

Hiley, Craig I.; Walton, Richard I. [Department of Chemistry, University of Warwick, Coventry (United Kingdom); Lees, Martin R. [Department of Physics, University of Warwick, Coventry (United Kingdom); Fisher, Janet M.; Thompsett, David [Johnson Matthey Technology Centre, Reading (United Kingdom); Agrestini, Stefano [Max-Planck Institut, CPfS, Dresden (Germany); Smith, Ronald I. [ISIS Neutron and Muon Source, Rutherford Appleton Laboratory, Harwell Oxford, Didcot (United Kingdom)

2014-04-22

Low-temperature (200 C) hydrothermal synthesis of the ruthenium oxides Ca{sub 1.5}Ru{sub 2}O{sub 7}, SrRu{sub 2}O{sub 6}, and Ba{sub 2}Ru{sub 3}O{sub 9}(OH) is reported. Ca{sub 1.5}Ru{sub 2}O{sub 7} is a defective pyrochlore containing Ru{sup V/VI}; SrRu{sub 2}O{sub 6} is a layered Ru{sup V} oxide with a PbSb{sub 2}O{sub 6} structure, whilst Ba{sub 2}Ru{sub 3}O{sub 9}(OH) has a previously unreported structure type with orthorhombic symmetry solved from synchrotron X-ray and neutron powder diffraction. SrRu{sub 2}O{sub 6} exhibits unusually high-temperature magnetic order, with antiferromagnetism persisting to at least 500 K, and refinement using room temperature neutron powder diffraction data provides the magnetic structure. All three ruthenates are metastable and readily collapse to mixtures of other oxides upon heating in air at temperatures around 300-500 C, suggesting they would be difficult, if not impossible, to isolate under conventional high-temperature solid-state synthesis conditions. (copyright 2014 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

Room-temperature Electrochemical Synthesis of Carbide-derived Carbons and Related Materials

Energy Technology Data Exchange (ETDEWEB)

Gogotsi, Yury [Drexel Univ., Philadelphia, PA (United States). Nanomaterials Group. Materials Science and Engineering Dept.

2015-02-28

This project addresses room-temperature electrochemical etching as an energy-efficient route to synthesis of 3D nanoporous carbon networks and layered 2D carbons and related structures, as well as provides fundamental understanding of structure and properties of materials produced by this method. Carbide-derived-carbons (CDCs) are a growing class of nanostructured carbon materials with properties that are desirable for many applications, such as electrical energy and gas storage. The structure of these functional materials is tunable by the choice of the starting carbide precursor, synthesis method, and process parameters. Moving from high-temperature synthesis of CDCs through vacuum decomposition above 1400°C and chlorination above 400°C, our studies under the previous DOE BES support led to identification of precursor materials and processing conditions for CDC synthesis at temperatures as low as 200°C, resulting in amorphous and highly reactive porous carbons. We also investigated synthesis of monolithic CDC films from carbide films at 250-1200°C. The results of our early studies provided new insights into CDC formation, led to development of materials for capacitive energy storage, and enabled fundamental understanding of the electrolyte ions confinement in nanoporous carbons.

Robust Temperature Control of a Thermoelectric Cooler via μ -Synthesis

Science.gov (United States)

Kürkçü, Burak; Kasnakoğlu, Coşku

2018-02-01

In this work robust temperature control of a thermoelectric cooler (TEC) via μ -synthesis is studied. An uncertain dynamical model for the TEC that is suitable for robust control methods is derived. The model captures variations in operating point due to current, load and temperature changes. A temperature controller is designed utilizing μ -synthesis, a powerful method guaranteeing robust stability and performance. For comparison two well-known control methods, namely proportional-integral-derivative (PID) and internal model control (IMC), are also realized to benchmark the proposed approach. It is observed that the stability and performance on the nominal model are satisfactory for all cases. On the other hand, under perturbations the responses of PID and IMC deteriorate and even become unstable. In contrast, the μ -synthesis controller succeeds in keeping system stability and achieving good performance under all perturbations within the operating range, while at the same time providing good disturbance rejection.

Solution-phase synthesis of nanomaterials at low temperature

Science.gov (United States)

Zhu, Yongchun; Qian, Yitai

2009-01-01

This paper reviews the solution-phase synthesis of nanoparticles via some routes at low temperatures, such as room temperature route, wave-assisted synthesis (γ-irradiation route and sonochemical route), directly heating at low temperatures, and hydrothermal/solvothermal methods. A number of strategies were developed to control the shape, the size, as well as the dispersion of nanostructures. Using diethylamine or n-butylamine as solvent, semiconductor nanorods were yielded. By the hydrothermal treatment of amorphous colloids, Bi2S3 nanorods and Se nanowires were obtained. CdS nanowires were prepared in the presence of polyacrylamide. ZnS nanowires were obtained using liquid crystal. The polymer poly (vinyl acetate) tubule acted as both nanoreactor and template for the CdSe nanowire growth. Assisted by the surfactant of sodium dodecyl benzenesulfonate (SDBS), nickel nanobelts were synthesized. In addition, Ag nanowires, Te nanotubes and ZnO nanorod arrays could be prepared without adding any additives or templates.

Towards room temperature, direct, solvent free synthesis of tetraborohydrides

International Nuclear Information System (INIS)

Remhof, A; Yan, Y; Friedrichs, O; Kim, J W; Mauron, Ph; Borgschulte, A; Züttel, A; Wallacher, D; Buchsteiner, A; Hoser, A; Oh, K H; Cho, Y W

2012-01-01

Due to their high hydrogen content, tetraborohydrides are discussed as potential synthetic energy carriers. On the example of lithium borohydride LiBH 4 , we discuss current approaches of direct, solvent free synthesis based on gas solid reactions of the elements or binary hydrides and/or borides with gaseous H 2 or B 2 H 6 . The direct synthesis from the elements requires high temperature and high pressure (700°C, 150bar D 2 ). Using LiB or AlB 2 as boron source reduces the required temperature by more than 300 K. Reactive milling of LiD with B 2 H 6 leads to the formation of LiBD 4 already at room temperature. The reactive milling technique can also be applied to synthesize other borohydrides from their respective metal hydrides.

Self-propagating high temperature synthesis and magnetic

Indian Academy of Sciences (India)

Ni–Zn ferrite powders were synthesized by self-propagating high temperature synthesis (SHS) method. X-ray diffraction, TEM and vibrating sample magnetometry (VSM) were used to characterize the phase composition, microstructure and magnetic properties of the combustion products. The effect of the combustion ...

High pressure sintering (HP-HT) of diamond powders with titanium and titanium carbide

International Nuclear Information System (INIS)

Jaworska, L.

1999-01-01

Polycrystalline diamond compacts for cutting tools are mostly manufactured using high pressure sintering (HP-HT). The standard diamond compacts are prepared by diamond powders sintering with metallic binding phase. The first group of metallic binder are metals able to solve carbon - Co, Ni. The second group of metal binders are carbide forming elements - Ti, Cr, W and others. The paper describes high pressure sintering of diamond powder with titanium and nonstoichiometry titanium carbide for cutting tool application. A type of binding phase has the significant influence on microstructure and mechanical properties of diamond compacts. Very homogeneous structure was achieved in case of compacts obtained from metalized diamond where diamond-TiC-diamond connection were predominant. In the case of compacts prepared by mechanical mixing of diamond with titanium powders the obtained structure was nonhomogeneous with titanium carbide clusters. They had more diamond to diamond connections. These compacts compared to the compact made of metallized diamond have greater wear resistance. In the case of the diamond and TiC 0.92 sintering the strong bonding of TiC diamond grains was obtained. The microstructure observations for diamond with 5% wt. Ti and diamond with 5% wt. TiC 0.92 (the initial composition) compacts were performed in transmission microscope. For two type of compacts the strong bonding phase TiC without defects is creating. (author)

Multi-Temperature Zone, Droplet-based Microreactor for Increased Temperature Control in Nanoparticle Synthesis

KAUST Repository

Erdem, E. Yegâ n; Cheng, Jim C.; Doyle, Fiona M.; Pisano, Albert P.

2013-01-01

Microreactors are an emerging technology for the controlled synthesis of nanoparticles. The Multi-Temperature zone Microreactor (MTM) described in this work utilizes thermally isolated heated and cooled regions for the purpose of separating

Combined Effect of Pressure and Temperature on the Viscous Behaviour of All-Oil Drilling Fluids

Directory of Open Access Journals (Sweden)

Hermoso J.

2014-12-01

Full Text Available The overall objective of this research was to study the combined influence of pressure and temperature on the complex viscous behaviour of two oil-based drilling fluids. The oil-based fluids were formulated by dispersing selected organobentonites in mineral oil, using a high-shear mixer, at room temperature. Drilling fluid viscous flow characterization was performed with a controlled-stress rheometer, using both conventional coaxial cylinder and non-conventional geometries for High Pressure/High Temperature (HPHT measurements. The rheological data obtained confirm that a helical ribbon geometry is a very useful tool to characterise the complex viscous flow behaviour of these fluids under extreme conditions. The different viscous flow behaviours encountered for both all-oil drilling fluids, as a function of temperature, are related to changes in polymer-oil pair solvency and oil viscosity. Hence, the resulting structures have been principally attributed to changes in the effective volume fraction of disperse phase due to thermally induced processes. Bingham’s and Herschel-Bulkley’s models describe the rheological properties of these drilling fluids, at different pressures and temperatures, fairly well. It was found that Herschel-Bulkley’s model fits much better B34-based oil drilling fluid viscous flow behaviour under HPHT conditions. Yield stress values increase linearly with pressure in the range of temperature studied. The pressure influence on yielding behaviour has been associated with the compression effect of different resulting organoclay microstructures. A factorial WLF-Barus model fitted the combined effect of temperature and pressure on the plastic viscosity of both drilling fluids fairly well, being this effect mainly influenced by the piezo-viscous properties of the continuous phase.

Room temperature synthesis of biodiesel using sulfonated ...

Science.gov (United States)

Sulfonation of graphitic carbon nitride (g-CN) affords a polar and strongly acidic catalyst, Sg-CN, which displays unprecedented reactivity and selectivity in biodiesel synthesis and esterification reactions at room temperature. Prepared for submission to Royal Society of Chemistry (RSC) journal, Green Chemistry as a communication.

Kinetics of the ammonia synthesis at low temperatures. II. Sources of discrepancies

International Nuclear Information System (INIS)

Kuchaev, V.L.; Shapatina, E.N.; Temkin, M.I.

1988-01-01

A method is developed for calculating the degree of conversion during the synthesis of ammonia in a continuous flow, tubular reactor, taking longitudinal diffusion into account. Such a calculation shows that the available data in the literature on the rate of ammonia synthesis at low temperatures in a tubular reactor agree with the rate equation based on the idea that the predominant intermediate substance is adsorbed ammonia (and not imide). The seeming conflict between this idea and the ratio of the rates of synthesis of ammonia and deuteroammonia at low temperatures is explained

Room temperature synthesis and high temperature frictional study of silver vanadate nanorods

Energy Technology Data Exchange (ETDEWEB)

Singh, D P; Aouadi, S M [Department of Physics, Southern Illinois University, Carbondale-62901 (United States); Polychronopoulou, K [Department of Chemistry, University of Cyprus, Nicosia, 1678 (Cyprus); Rebholz, C, E-mail: dineshpsingh@gmail.com, E-mail: saouadi@physics.siu.edu [Department of Mechanical and Manufacturing Engineering, University of Cyprus, Nicosia, 1678 (Cyprus)

2010-08-13

We report the room temperature (RT) synthesis of silver vanadate nanorods (consisting of mainly {beta}-AgV O{sub 3}) by a simple wet chemical route and their frictional study at high temperatures (HT). The sudden mixing of ammonium vanadate with silver nitrate solution under constant magnetic stirring resulted in a pale yellow coloured precipitate. Structural/microstructural characterization of the precipitate through x-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) revealed the high yield and homogeneous formation of silver vanadate nanorods. The length of the nanorods was 20-40 {mu}m and the thickness 100-600 nm. The pH variation with respect to time was thoroughly studied to understand the formation mechanism of the silver vanadate nanorods. This synthesis process neither demands HT, surfactants nor long reaction time. The silver vanadate nanomaterial showed good lubrication behaviour at HT (700 deg. C) and the friction coefficient was between 0.2 and 0.3. HT-XRD revealed that AgV O{sub 3} completely transformed into silver vanadium oxide (Ag{sub 2}V{sub 4}O{sub 11}) and silver with an increase in temperature from RT to 700 deg. C.

Room temperature synthesis and high temperature frictional study of silver vanadate nanorods.

Science.gov (United States)

Singh, D P; Polychronopoulou, K; Rebholz, C; Aouadi, S M

2010-08-13

We report the room temperature (RT) synthesis of silver vanadate nanorods (consisting of mainly beta-AgV O(3)) by a simple wet chemical route and their frictional study at high temperatures (HT). The sudden mixing of ammonium vanadate with silver nitrate solution under constant magnetic stirring resulted in a pale yellow coloured precipitate. Structural/microstructural characterization of the precipitate through x-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) revealed the high yield and homogeneous formation of silver vanadate nanorods. The length of the nanorods was 20-40 microm and the thickness 100-600 nm. The pH variation with respect to time was thoroughly studied to understand the formation mechanism of the silver vanadate nanorods. This synthesis process neither demands HT, surfactants nor long reaction time. The silver vanadate nanomaterial showed good lubrication behaviour at HT (700 degrees C) and the friction coefficient was between 0.2 and 0.3. HT-XRD revealed that AgV O(3) completely transformed into silver vanadium oxide (Ag(2)V(4)O(11)) and silver with an increase in temperature from RT to 700 degrees C.

Effect of temperature and time on solvothermal synthesis of ...

Indian Academy of Sciences (India)

Effect of temperature and time study on solvothermal synthesis of BaTiO3 revealed that a moderate reaction temperature i.e. 185◦C and longer reaction time favour tetragonal phase stabiliza- tion. Dissolution–precipitation appears to be the transformation mechanism for the crystallization of BaTiO3 from particulate TiO2 ...

Differential chromosomal and mitochondrial DNA synthesis in temperature-sensitive mutants of Ustilago maydis

Energy Technology Data Exchange (ETDEWEB)

Unrau, P.

1977-01-01

The amount and type of residual DNA synthesis was determined in eight temperature-sensitive mutants of the smut fungus Ustilago maydis after incubation at the restrictive temperature (32/sup 0/C) for eight hours. Mutants ts-220, ts-207, ts-432 and ts-346 were found to have an overall reduction in the synthesis of both nuclear and mitochondrial DNA in comparison to the wild-type. In mutants ts-20, tsd 1-1, ts-84 and pol 1-1 nuclear DNA synthesis was depressed relative to mitochondrial synthesis. The DNA-polymerase mutant pol 1-1 had persistent nuclear synthesis at about 50% of the rate of synthesis of mitochondrial DNA and similar behavior was observed in a diploid homozygous strain. Mutant ts-84 had an initial burst of DNA synthesis which was reduced for nuclear but not mitochondrial synthesis after three hours preincubation at 32/sup 0/C. tsd 1-1 and ts-20 had nuclear residual synthesis amounting to about 25% of the relative rate of mitochondrial synthesis which correlates to increasing UV sensitivity of these strains on incubation at 32/sup 0/C. A pol 1-1 ts-84 double mutant had an additive loss of nuclear DNA synthesis which indicates that the steps of replication involved may be sequential.

Ammonia synthesis at low temperatures

DEFF Research Database (Denmark)

Rod, Thomas Holm; Logadottir, Ashildur; Nørskov, Jens Kehlet

2000-01-01

have been carried out to evaluate its feasibility. The calculations suggest that it might be possible to catalytically produce ammonia from molecular nitrogen at low temperatures and pressures, in particular if energy is fed into the process electrochemically. (C) 2000 American Institute of Physics.......Density functional theory (DFT) calculations of reaction paths and energies for the industrial and the biological catalytic ammonia synthesis processes are compared. The industrial catalyst is modeled by a ruthenium surface, while the active part of the enzyme is modeled by a MoFe6S9 complex...

Temperature lowering in cryogenic chemical-synthesis techniques and system

International Nuclear Information System (INIS)

Martinez, H.E.; Nelson, T.O.; Vikdal, L.N.

1993-01-01

When evaluating a chemical synthesis process for a reaction that occurs on the cryogenically cooled walls, it is sometimes necessary to reduce the wall temperatures to enhance the chemical process. To evaluate the chemical process at lower than atmospheric boiling of liquid nitrogen, we built a system and used it to reduce the temperature of the liquid nitrogen. The technique of lowering the liquid nitrogen temperature by reducing the pressure of the boil-off is established knowledge. This paper presents the engineering aspects of the system, design features, equipment requirements, methods of control, and results of the chemical synthesis. The heat input to the system was ∼400 watts, placing a relatively large demand on the pumping system. Our system is a scale-up of the small laboratory experiment, and it provides the information needed to design an effective system. The major problem encountered was the large quantity of liquid escaping the system during the processing, placing a large gas load on the vacuum system

Temperature Dependence on The Synthesis of Jatropha Biolubricant

International Nuclear Information System (INIS)

Resul, Muhammad Faiz M Gunam; Ghazi, Tinia Idaty Mohd; Idris, Azni

2011-01-01

Jatropha oil has good potential as the renewable energy as well as lubricant feedstock. The synthesis of jatropha biolubricant was performed by transesterification of jatropha methyl ester (JME) with trimethyl-ol-propane (TMP) with sodium methoxide (NaOCH3) catalyst. The effects of temperature on the synthesis were studied at a range between 120 deg. C and 200 deg. C with pressure kept at 10mbar. The conversion of JME to jatropha biolubricant was found to be the highest (47%) at 200 deg. C. However, it was suggested that the optimum temperature of the reaction is at 150 deg. C due to insignificant improvement in biolubricant production. To maintain forward reaction, the excess amount of JME was maintained at 3.9:1 ratios to TMP. Kinetic study was done and compared. The synthesis was found to follow a second order reaction with overall rate constant of 1.49 x 10-1 (%wt/wt.min.deg. C)-1. The estimated activation energy was 3.94 kJ/mol. Pour point for jatropha biolubricant was at -3 deg. C and Viscosity Index (VI) ranged from 178 to 183. The basic properties of jatropha biolubricant, pour point and viscosities are found comparable to other plant based biolubricant, namely palm oil and soybean based biolubricant.

Auger electron spectroscopy analysis for growth interface of cubic boron nitride single crystals synthesized under high pressure and high temperature

Science.gov (United States)

Lv, Meizhe; Xu, Bin; Cai, Lichao; Guo, Xiaofei; Yuan, Xingdong

2018-05-01

After rapid cooling, cubic boron nitride (c-BN) single crystals synthesized under high pressure and high temperature (HPHT) are wrapped in the white film powders which are defined as growth interface. In order to make clear that the transition mechanism of c-BN single crystals, the variation of B and N atomic hybrid states in the growth interface is analyzed with the help of auger electron spectroscopy in the Li-based system. It is found that the sp2 fractions of B and N atoms decreases, and their sp3 fractions increases from the outer to the inner in the growth interface. In addition, Lithium nitride (Li3N) are not found in the growth interface by X-ray diffraction (XRD) experiment. It is suggested that lithium boron nitride (Li3BN2) is produced by the reaction of hexagonal boron nitride (h-BN) and Li3N at the first step, and then B and N atoms transform from sp2 into sp3 state with the catalysis of Li3BN2 in c-BN single crystals synthesis process.

Low Temperature Synthesis and Properties of Gadolinium-Doped Cerium Oxide Nanoparticles

DEFF Research Database (Denmark)

Machado, Marina F. S.; P. R. Moraes, Leticia; Monteiro, Natalia K.

2017-01-01

Gadolinium-doped cerium oxide (GDC) is an attractive ceramic material for solid oxide fuel cells (SOFCs) both as the electrolyte or in composite electrodes. The Ni/GDC cermet can be tuned as a catalytic layer, added to the conventional Ni/yttria-stabilized zirconia (YSZ), for the internal steam...... sintering temperature needed to obtain a fully dense ceramic body, which can result in undesired reactions with YSZ. In this study, a green chemistry route for the synthesis of 10 mol% GDC nanoparticles is proposed. Such a low temperature synthesis provides control over particle size and sinterability...

High temperature bismuth cuprate superconductors synthesis and characterization

International Nuclear Information System (INIS)

Mansori, M.; Satre, P.; Breandon, C.; Roubin, M.; Sebaoun, A.

1993-01-01

High temperature superconductor phases synthesis by coprecipitation in alkaline solution is reported. (Bi 1.6 Pb 0.4 )Sr 2 Ca 1 Cu 2 O 8+x and (Bi 1.6 Pb 0.4 )Sr 2 Ca 2 Cu 3 O 10+y noted (2212) and (2223) have been prepared and studied. From aqueous nitrate solutions of Bi, Pb, Sr, Ca and Cu and oxalic acid aqueous solution as well as ethylene glycol, using an organic base (the triethylamine), the pH was increased up to the path of the precipitation zone (pH = 10.5-11.2). This method assures a good granulometric homogeneity of powders. Thermal analysis and characterization of the different components produced during the synthesis have been studied by DTA (differential thermal analysis)- TGA (thermogravimetric analysis), X-ray diffraction at different temperatures and by Infrared spectroscopy with a Fourier transformation. The measurements of magnetic susceptibility for the 2212 (with and without lead) and 2223 (with lead) phases have permitted us to observe the critical temperatures of 84 K, 87 K and 114 K. (author). 29 refs., 2 figs., 4 tabs

Synthesis of pure ozone by nanosecond discharge at cryogenic temperatures

International Nuclear Information System (INIS)

Amirov, R.H.; Asinovsky, E.I.; Samoilov, I.S.

1996-01-01

Synthesis of pure ozone by nanosecond discharge at cryogenic temperatures was experimentally examined. The average ozone concentration in the volume of the discharge tube was less at cryogenic temperatures than at room temperatures. The production of condensed ozone have been determined by measuring the ozone concentration when the walls was heated and ozone evaporated. The energy yield of ozone generation at cryogenic temperatures has been calculated. The maximum value was 200 g/kWh

Standard practice for evaluation of disbonding of bimetallic stainless alloy/steel plate for use in high-pressure, high-temperature refinery hydrogen service

CERN Document Server

American Society for Testing and Materials. Philadelphia

2001-01-01

1.1 This practice covers a procedure for the evaluation of disbonding of bimetallic stainless alloy/steel plate for use in refinery high-pressure/high-temperature (HP/HT) gaseous hydrogen service. It includes procedures to (1) produce suitable laboratory test specimens, (2) obtain hydrogen charging conditions in the laboratory that are similar to those found in refinery HP/HT hydrogen gas service for evaluation of bimetallic specimens exposed to these environments, and (3) perform analysis of the test data. The purpose of this practice is to allow for comparison of data among test laboratories on the resistance of bimetallic stainless alloy/steels to hydrogen-induced disbonding (HID). 1.2 This practice applies primarily to bimetallic products fabricated by weld overlay of stainless alloy onto a steel substrate. Most of the information developed using this practice has been obtained for such materials. The procedures described herein, may also be appropriate for evaluation of hot roll bonded, explosive bonded...

Room temperature growth of ZnO nanorods by hydrothermal synthesis

Science.gov (United States)

Tateyama, Hiroki; Zhang, Qiyan; Ichikawa, Yo

2018-05-01

The effect of seed layer morphology on ZnO nanorod growth at room temperature was studied via hydrothermal synthesis on seed layers with different thicknesses and further annealed at different temperatures. The change in the thickness and annealing temperature enabled us to control over a diameter of ZnO nanorods which are attributed to the changing of crystallinity and roughness of the seed layers.

Application of low-temperature plasma for the synthesis of hydrogenated graphene (graphane)

Science.gov (United States)

Shavelkina, M. B.; Amirov, R. H.; Katarzhis, V. A.; Kiselev, V. I.

2017-12-01

The possibility of a direct synthesis of hydrogenated graphene in decomposition of methane by means of low-temperature plasma was investigated. A DC plasma torch with an expanding channel-anode, a vortex gas supply and a self-setting arc length was used as a generator of low-temperature plasma. Argon was used as the plasma-forming gas. The temperatures of argon plasma and with methane addition to it were determined on the basis of spectral measurements. The synthesis products were characterized by electron microscopy and thermogravimetry. The effect of hydrogenated graphene as a nanomodifier on the properties of the cubic boron nitride based functional ceramics was investigated.

Development of coating technology for nuclear fuel by self-propagating high temperature synthesis

International Nuclear Information System (INIS)

Choi, Y.; Kim, Bong G.; Lee, Y. W.

1997-01-01

This paper presents experimental results of the preparation of silicon carbide and graphite layers on a nuclear fuel from silane and propane gases by a conventional chemical vapor deposition and combustion synthesis technologies. The direct reaction between silicon and pyrolytic carbon in a high temperature releases sufficient amount of energy to make a synthesis self-sustaining under the preheating of about 1200 deg C. During this high temperature process, lamellar structure with isotropic carbon synthesis. A full characterization of phase composition and final morphology of the coated layers by X-ray diffraction, SEM and AES is presented. (author). 6 refs., 1 tab., 11 figs

Low-temperature synthesis of superconducting nanocrystalline MgB2

International Nuclear Information System (INIS)

Lu, J.; Xiao, Z.; Lin, Q.; Claus, H.; Fang, Z.Z.

2010-01-01

Magnesium diboride (MgB 2 ) is considered a promising material for practical application in superconducting devices, with a transition temperature near 40 K. In the present paper, nanocrystalline MgB 2 with an average particle size of approximately 70 nm is synthesized by reacting LiBH 4 with MgH 2 at temperatures as low as 450 C. This synthesis approach successfully bypasses the usage of either elemental boron or toxic diborane gas. The superconductivity of the nanostructures is confirmed by magnetization measurements, showing a superconducting critical temperature of 38.7 K.

Comparison of the quality of single-crystal diamonds grown on two types of seed substrates by MPCVD

Science.gov (United States)

Zhao, Yun; Guo, Yanzhao; Lin, Liangzhen; Zheng, Yuting; Hei, Lifu; Liu, Jinlong; Wei, Junjun; Chen, Liangxian; Li, Chengming

2018-06-01

Microwave plasma chemical vapor deposition (MPCVD) was used to grow single-crystal diamonds on two types of single-crystal diamond seed substrates prepared by high-pressure, high-temperature (HPHT) and chemical vapor deposition (CVD) methods. The quality of diamonds grown on the different seed substrates was compared. Fluorescence characteristics showed that the sectors of the HPHT seed substrates were obviously partitioned. Raman and absorption spectra showed that the CVD seed substrate produced higher-quality crystals with fewer nitrogen impurities. X-ray topography showed that the HPHT seed substrate had obvious growth sector boundaries, inclusions, dislocations, and stacking faults. The polarization characteristics of HPHT seed substrate were obvious, and the stress distribution was not uniform. When etching HPHT and CVD seed substrates using the same parameters, the etching morphology and extent of different growth sectors of the two substrates differed. Although extended defects were inevitably formed at the interface and propagated in the CVD layer, the dislocation density of a 1 mm-thick CVD layer grown on a CVD seed substrate was only half that of a 1 mm-thick CVD layer grown on an HPHT seed substrate. Therefore, the use of CVD seed substrate enabled the growth of a relatively higher-quality CVD single-crystal diamond.

Development of CaO-swelling cements for cementing of natural gas underground storage wells in field trial (temperature range {<=} 60 C) and composition of CaO and MgO-swelling cements for a temperature range between 60 C-105 C. Final report; Entwicklung von CaO-Quellzementen fuer die Zementation von Erdgasspeicherbohrungen im Feldversuch (Temperaturbereich {<=} 60 C) sowie Formulierung von CaO- und MgO-Quellzementen fuer den Einsatz im Temperaturbereich 60 C-105 C. Abschlussbericht

Energy Technology Data Exchange (ETDEWEB)

Ghofrani, R.; Gheorghiu, A.S.; Radu, G.; Rogojinoiu, E.; Stan, M.; Miehe, H.

2000-11-01

The investigations conducted within the scope of this project are a consistent continuation of the work already performed at ITE, especially DGMK research projects 444-1, 444-2 and 444-3. These investigations should lead to a field trial of selected CaO-swelling cement recipes. Essential parameters examined within the course of this project include the HPHT-consistency behavior, HPHT-expansion behavior and the long-term stability behavior of CaO-swelling cements under similar conditions to those prevailing in the borehole. The swelling cement will be made up in correlation with the appropriate industrial make up method using the ITE-equipment; in accordance to the borehole conditions, the swelling cement slurry will be then treated in the ITE-Circulating Facility with respect to shear, temperature and pressure. The cement slurry treated in the ITE-Circulating Facility in accordance to the borehole conditions will be then experimentally investigated regarding the HPHT-consistency behavior and HPHT-expansion behavior. With respect to the long-term stability the swelling cement slurry treated in the Circulating Facility will be cured in autoclaves under appropriate pT-conditions. After evacuation from the autoclaves the compressive strength, the shear strength and the system permeability of the samples will be measured. With respect to the properties of a CaO-reference swelling cement recipe measured under the same experimental conditions, the ITE-make up method has been correlated to the common industrial make up methods LPHM, LPRM and HPRM; the alignment of the ITE-make up method with the planned industrial make up method for an appropriate cement job should make sure that the properties of a swelling cement measured in lab will be of practice relevance. For filling in and annular cementing of selected boreholes CaO-swelling cement recipes have been composed, optimized after experimental investigation results, and ultimately released to field usage after the results

The flavoprotein Tah18-dependent NO synthesis confers high-temperature stress tolerance on yeast cells

International Nuclear Information System (INIS)

Nishimura, Akira; Kawahara, Nobuhiro; Takagi, Hiroshi

2013-01-01

Highlights: ► NO is produced from L-arginine in response to elevated temperature in yeast. ► Tah18 was first identified as the yeast protein involved in NO synthesis. ► Tah18-dependent NO synthesis confers tolerance to high-temperature on yeast cells. -- Abstract: Nitric oxide (NO) is a ubiquitous signaling molecule involved in the regulation of a large number of cellular functions. In the unicellular eukaryote yeast, NO may be involved in stress response pathways, but its role is poorly understood due to the lack of mammalian NO synthase (NOS) orthologues. Previously, we have proposed the oxidative stress-induced L-arginine synthesis and its physiological role under stress conditions in yeast Saccharomyces cerevisiae. Here, our experimental results indicated that increased conversion of L-proline into L-arginine led to NO production in response to elevated temperature. We also showed that the flavoprotein Tah18, which was previously reported to transfer electrons to the Fe–S cluster protein Dre2, was involved in NO synthesis in yeast. Gene knockdown analysis demonstrated that Tah18-dependent NO synthesis confers high-temperature stress tolerance on yeast cells. As it appears that such a unique cell protection mechanism is specific to yeasts and fungi, it represents a promising target for antifungal activity.

Manufacturing Demonstration Facility: Low Temperature Materials Synthesis

International Nuclear Information System (INIS)

Graham, David E.; Moon, Ji-Won; Armstrong, Beth L.; Datskos, Panos G.; Duty, Chad E.; Gresback, Ryan; Ivanov, Ilia N.; Jacobs, Christopher B.; Jellison, Gerald Earle; Jang, Gyoung Gug; Joshi, Pooran C.; Jung, Hyunsung; Meyer, Harry M.; Phelps, Tommy

2015-01-01

The Manufacturing Demonstration Facility (MDF) low temperature materials synthesis project was established to demonstrate a scalable and sustainable process to produce nanoparticles (NPs) for advanced manufacturing. Previous methods to chemically synthesize NPs typically required expensive, high-purity inorganic chemical reagents, organic solvents and high temperatures. These processes were typically applied at small laboratory scales at yields sufficient for NP characterization, but insufficient to support roll-to-roll processing efforts or device fabrication. The new NanoFermentation processes described here operated at a low temperature (~60 C) in low-cost, aqueous media using bacteria that produce extracellular NPs with controlled size and elemental stoichiometry. Up-scaling activities successfully demonstrated high NP yields and quality in a 900-L pilot-scale reactor, establishing this NanoFermentation process as a competitive biomanufacturing strategy to produce NPs for advanced manufacturing of power electronics, solid-state lighting and sensors.

Manufacturing Demonstration Facility: Low Temperature Materials Synthesis

Energy Technology Data Exchange (ETDEWEB)

Graham, David E. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Moon, Ji-Won [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Armstrong, Beth L. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Datskos, Panos G. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Duty, Chad E. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Gresback, Ryan [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Ivanov, Ilia N. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Jacobs, Christopher B. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Jellison, Gerald Earle [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Jang, Gyoung Gug [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Joshi, Pooran C. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Jung, Hyunsung [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Meyer, III, Harry M. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Phelps, Tommy [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)

2015-06-30

The Manufacturing Demonstration Facility (MDF) low temperature materials synthesis project was established to demonstrate a scalable and sustainable process to produce nanoparticles (NPs) for advanced manufacturing. Previous methods to chemically synthesize NPs typically required expensive, high-purity inorganic chemical reagents, organic solvents and high temperatures. These processes were typically applied at small laboratory scales at yields sufficient for NP characterization, but insufficient to support roll-to-roll processing efforts or device fabrication. The new NanoFermentation processes described here operated at a low temperature (~60 C) in low-cost, aqueous media using bacteria that produce extracellular NPs with controlled size and elemental stoichiometry. Up-scaling activities successfully demonstrated high NP yields and quality in a 900-L pilot-scale reactor, establishing this NanoFermentation process as a competitive biomanufacturing strategy to produce NPs for advanced manufacturing of power electronics, solid-state lighting and sensors.

Studies on synthesis of diamond at high pressure and temperature

Science.gov (United States)

Kailath, Ansu J.

Diamond is an essential material of modern industry and probably the most versatile abrasive available today. It also has many other industrial applications attributable to its unique mechanical, optical, thermal and electrical properties. Its usage has grown to the extent that there is hardly a production process in modern industry in which industrial diamond does not play a part. Bulk diamond production today is a major industry. Diamonds can be produced in its thermodynamically stable regions either by direct static conversion, or shock-wave conversion. The pressures and temperatures required for direct static conversion are very high. In the catalyst-solvent method, the material used establishes a reaction path with lower activation energy than for direct transformation. This helps in a quicker transformation under more benign conditions. Hence, catalyst-solvent synthesis is readily accomplished and is now a viable and successful industrial process. Diamonds produced by shock wave are very small (approximately 60mu). Therefore this diamond is limited to applications such as polishing compounds only. The quality, quantity, size and morphology of the crystals synthesized by catalyst-solvent process depend on different conditions employed for synthesis. These details, because of commercial reasons are not disclosed in published literature. Hence, systematic studies have been planned to investigate the effect of various growth parameters on the synthesized crystals. During the growth of synthetic diamond crystals, some catalyst-solvent is retained into the crystals in some form and behaves like an impurity. Several physico-mechanical properties of the crystals are found to depend on the total quantity and distribution of these inclusions. Thus, detailed investigation of the crystallization medium and inclusions in synthesized diamonds was also undertaken in the present work. The work incorporated in this thesis has been divided into seven chapters. The first

Temperature dependence on the synthesis of Jatropha bio lubricant

International Nuclear Information System (INIS)

Gunam Resul, M.F.M.; Tinia Idaty Mohd Ghazi; Idris, A.

2009-01-01

Full text: Jatropha oil has good potential as the renewable energy as well as lubricant feedstock. The synthesis of jatropha bio lubricant was performed by transesterification of jatropha methyl ester (JME) with trimethyl-ol-propane (TMP) with sodium methoxide (NaOCH 3 ) catalyst. The effects of temperature on the synthesis were studied at a range between 120 degree Celsius and 200 degree Celsius with pressure kept at 10 mbar. The conversion of JME to jatropha bio lubricant was found to be the highest (47 %) at 200 degree Celsius. However, it was suggested that the optimum temperature of the reaction is at 150 degree Celsius due to insignificant improvement in bio lubricant production. To maintain forward reaction, the excess amount of JME was maintained at 3.9:1 ratios to TMP. Kinetic study was done and compared. The synthesis was found to follow a second order reaction with overall rate constant of 1.49 x 10 -1 (% wt/ wt.min.degree Celsius) -1 . The estimated activation energy was 3.94 kJ/mol. Pour point for jatropha bio lubricant was at -3 degree Celsius and Viscosity Index (VI) ranged from 178 to 183. The basic properties of jatropha bio lubricant, pour point and viscosities are found comparable to other plant based bio lubricant, namely palm oil and soybean based bio lubricant. (author)

System for detecting acoustic emissions in multianvil experiments: Application to deep seismicity in the Earth

International Nuclear Information System (INIS)

Jung, Haemyeong; Fei Yingwei; Silver, Paul G.; Green, Harry W.

2006-01-01

One of the major goals in the experimental study of deep earthquakes is to identify slip instabilities at high pressure and high temperature (HPHT) that might be responsible for the occurrence of earthquakes. Detecting acoustic emissions from a specimen during faulting provides unique constraints on the instability process. There are few experimental studies reporting acoustic emissions under HPHT conditions, due to technical challenges. And those studies have used only one or at most two acoustic sensors during the experiments. Such techniques preclude the accurate location of the acoustic emission source region and thus the ability to distinguish real signal from noise that may be coming from outside the sample. We have developed a system for detecting acoustic emissions at HPHT. Here we present a four-channel acoustic emission detecting system working in the HPHT octahedral multianvil apparatus. Each channel has high resolution (12 bits) and a sampling rate of 30 MHz. In experiments at the pressures up to 6 GPa and temperatures up to 770 deg. C, we have observed acoustic emissions under various conditions. Analyzing these signals, we are able to show that this system permits us to distinguish between signal and noise, locate the source of the acoustic emission, and obtain reliable data on the radiation pattern. This system has greatly improved our ability to study faulting instabilities under high pressure and high temperature

Combined laser ultrasonics, laser heating, and Raman scattering in diamond anvil cell system

Science.gov (United States)

Zinin, Pavel V.; Prakapenka, Vitali B.; Burgess, Katherine; Odake, Shoko; Chigarev, Nikolay; Sharma, Shiv K.

2016-12-01

We developed a multi-functional in situ measurement system under high pressure equipped with a laser ultrasonics (LU) system, Raman device, and laser heating system (LU-LH) in a diamond anvil cell (DAC). The system consists of four components: (1) a LU-DAC system (probe and pump lasers, photodetector, and oscilloscope) and DAC; (2) a fiber laser, which is designed to allow precise control of the total power in the range from 2 to 100 W by changing the diode current, for heating samples; (3) a spectrometer for measuring the temperature of the sample (using black body radiation), fluorescence spectrum (spectrum of the ruby for pressure measurement), and Raman scattering measurements inside a DAC under high pressure and high temperature (HPHT) conditions; and (4) an optical system to focus laser beams on the sample and image it in the DAC. The system is unique and allows us to do the following: (a) measure the shear and longitudinal velocities of non-transparent materials under HPHT; (b) measure temperature in a DAC under HPHT conditions using Planck's law; (c) measure pressure in a DAC using a Raman signal; and (d) measure acoustical properties of small flat specimens removed from the DAC after HPHT treatment. In this report, we demonstrate that the LU-LH-DAC system allows measurements of velocities of the skimming waves in iron at 2580 K and 22 GPa.

The flavoprotein Tah18-dependent NO synthesis confers high-temperature stress tolerance on yeast cells

Energy Technology Data Exchange (ETDEWEB)

Nishimura, Akira; Kawahara, Nobuhiro [Graduate School of Biological Sciences, Nara Institute of Science and Technology, 8916-5 Takayama, Ikoma, Nara 630-0192 (Japan); Takagi, Hiroshi, E-mail: hiro@bs.naist.jp [Graduate School of Biological Sciences, Nara Institute of Science and Technology, 8916-5 Takayama, Ikoma, Nara 630-0192 (Japan)

2013-01-04

Highlights: Black-Right-Pointing-Pointer NO is produced from L-arginine in response to elevated temperature in yeast. Black-Right-Pointing-Pointer Tah18 was first identified as the yeast protein involved in NO synthesis. Black-Right-Pointing-Pointer Tah18-dependent NO synthesis confers tolerance to high-temperature on yeast cells. -- Abstract: Nitric oxide (NO) is a ubiquitous signaling molecule involved in the regulation of a large number of cellular functions. In the unicellular eukaryote yeast, NO may be involved in stress response pathways, but its role is poorly understood due to the lack of mammalian NO synthase (NOS) orthologues. Previously, we have proposed the oxidative stress-induced L-arginine synthesis and its physiological role under stress conditions in yeast Saccharomyces cerevisiae. Here, our experimental results indicated that increased conversion of L-proline into L-arginine led to NO production in response to elevated temperature. We also showed that the flavoprotein Tah18, which was previously reported to transfer electrons to the Fe-S cluster protein Dre2, was involved in NO synthesis in yeast. Gene knockdown analysis demonstrated that Tah18-dependent NO synthesis confers high-temperature stress tolerance on yeast cells. As it appears that such a unique cell protection mechanism is specific to yeasts and fungi, it represents a promising target for antifungal activity.

Low-temperature synthesis of graphene on nickel foil by microwave plasma chemical vapor deposition

International Nuclear Information System (INIS)

Kim, Y.; Song, W.; Lee, S. Y.; Jeon, C.; Jung, W.; Kim, M.; Park, C.-Y.

2011-01-01

Microwave plasma chemical vapor deposition (MPCVD) was employed to synthesize high quality centimeter scale graphene film at low temperatures. Monolayer graphene was obtained by varying the gas mixing ratio of hydrogen and methane to 80:1. Using advantages of MPCVD, the synthesis temperature was decreased from 750 deg. C down to 450 deg. C. Optical microscopy and Raman mapping images exhibited that a large area monolayer graphene was synthesized regardless of the temperatures. Since the overall transparency of 89% and low sheet resistances ranging from 590 to 1855 Ω/sq of graphene films were achieved at considerably low synthesis temperatures, MPCVD can be adopted in manufacturing future large-area electronic devices based on graphene film.

Low-temperature synthesis of graphene on nickel foil by microwave plasma chemical vapor deposition

Science.gov (United States)

Kim, Y.; Song, W.; Lee, S. Y.; Jeon, C.; Jung, W.; Kim, M.; Park, C.-Y.

2011-06-01

Microwave plasma chemical vapor deposition (MPCVD) was employed to synthesize high quality centimeter scale graphene film at low temperatures. Monolayer graphene was obtained by varying the gas mixing ratio of hydrogen and methane to 80:1. Using advantages of MPCVD, the synthesis temperature was decreased from 750 °C down to 450 °C. Optical microscopy and Raman mapping images exhibited that a large area monolayer graphene was synthesized regardless of the temperatures. Since the overall transparency of 89% and low sheet resistances ranging from 590 to 1855 Ω/sq of graphene films were achieved at considerably low synthesis temperatures, MPCVD can be adopted in manufacturing future large-area electronic devices based on graphene film.

Synthesis of MIL-100(Fe at Low Temperature and Atmospheric Pressure

Directory of Open Access Journals (Sweden)

Jing Shi

2013-01-01

Full Text Available MIL-100(Fe, a mesoporous metal-organic framework (MOF, has a large BET specific surface area and pore volume with the presence of a significant amount of accessible Lewis acid metal sites upon dehydration. The structural characteristics of MIL-100(Fe make it a good candidate for potential applications in gas storage, separation, and heterogeneous catalysis. Mainly, this MOF is obtained by the hydrothermal synthesis in a Teflon-lined autoclave at high temperature (>150°C under static conditions. However, this method has several disadvantages such as high temperature, high (autogenous pressure, long time, and comparable low MOF yield. Therefore, development of a facile method for synthesis of MIL-100(Fe is vitally important for fundamental understanding and practical application. Herein, MIL-100(Fe is synthesized by a facile low-temperature (90% still could be achieved, suggesting that this simple and energy saving method has the potential to be used practically.

Synthesis and characterization of boron-oxygen-hydrogen thin films at low temperatures

International Nuclear Information System (INIS)

Music, D.; Koelpin, H.; Atiser, A.; Kreissig, U.; Bobek, T.; Hadam, B.; Schneider, J.M.

2005-01-01

We have studied the influence of synthesis temperature on chemical composition and mechanical properties of X-ray amorphous boron-oxygen-hydrogen (B-O-H) films. These B-O-H films have been synthesized by RF sputtering of a B-target in an Ar atmosphere. Upon increasing the synthesis temperature from room temperature to 550 deg. C, the O/B and H/B ratios decrease from 0.73 to 0.15 and 0.28 to 0.07, respectively, as determined by elastic recoil detection analysis. It is reasonable to assume that potential sources of O and H are residual gas and laboratory atmosphere. The elastic modulus, as measured by nanoindentation, increases from 93 to 214 GPa, as the O/B and H/B ratios decreases within the range probed. Hence, we have shown that the effect of impurity incorporation on the elastic properties is extensive and that the magnitude of the incorporation is a strong function of the substrate temperature

Room temperature chemical synthesis of Cu(OH)2 thin films for supercapacitor application

International Nuclear Information System (INIS)

Gurav, K.V.; Patil, U.M.; Shin, S.W.; Agawane, G.L.; Suryawanshi, M.P.; Pawar, S.M.; Patil, P.S.; Lokhande, C.D.; Kim, J.H.

2013-01-01

Highlights: •Cu(OH) 2 is presented as the new supercapacitive material. •The novel room temperature method used for the synthesis of Cu(OH) 2 . •The hydrous, nanograined Cu(OH) 2 shows higher specific capacitance of 120 F/g. -- Abstract: Room temperature soft chemical synthesis route is used to grow nanograined copper hydroxide [Cu(OH) 2 ] thin films on glass and stainless steel substrates. The structural, morphological, optical and wettability properties of Cu(OH) 2 thin films are studied by means of X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), field emission scanning electron microscopy (FESEM), UV–vis spectrophotometer and water contact angle measurement techniques. The results showed that, room temperature chemical synthesis route allows to form the nanograined and hydrophilic Cu(OH) 2 thin films with optical band gap energy of 3.0 eV. The electrochemical properties of Cu(OH) 2 thin films are studied in an aqueous 1 M NaOH electrolyte using cyclic voltammetry. The sample exhibited supercapacitive behavior with 120 F/g specific capacitance

Synthesis of indium nanoparticles at ambient temperature; simultaneous phase transfer and ripening

Energy Technology Data Exchange (ETDEWEB)

Aghazadeh Meshgi, Mohammad; Kriechbaum, Manfred [Graz University of Technology, Institute of Inorganic Chemistry (Austria); Biswas, Subhajit; Holmes, Justin D., E-mail: j.holmes@ucc.ie [University College Cork, Materials Chemistry and Analysis Group, Department of Chemistry and the Tyndall National Institute (Ireland); Marschner, Christoph, E-mail: christoph.marschner@tugraz.at [Graz University of Technology, Institute of Inorganic Chemistry (Austria)

2016-12-15

The synthesis of size-monodispersed indium nanoparticles via an innovative simultaneous phase transfer and ripening method is reported. The formation of nanoparticles occurs in a one-step process instead of well-known two-step phase transfer approaches. The synthesis involves the reduction of InCl{sub 3} with LiBH{sub 4} at ambient temperature and although the reduction occurs at room temperature, fine indium nanoparticles, with a mean diameter of 6.4 ± 0.4 nm, were obtained directly in non-polar n-dodecane. The direct synthesis of indium nanoparticles in n-dodecane facilitates their fast formation and enhances their size-monodispersity. In addition, the nanoparticles were highly stable for more than 2 months. The nanoparticles were characterised by dynamic light scattering (DLS), small angle X-ray scattering (SAXS), transmission electron microscopy (TEM), energy dispersive X-ray spectroscopy (EDS) and Fourier transform infrared (FT-IR) spectroscopy to determine their morphology, structure and phase purity.

Synthesis of ZnO Nanostructures for Low Temperature CO and UV Sensing

Directory of Open Access Journals (Sweden)

Nazar Abbas Shah

2012-10-01

Full Text Available In this paper, synthesis and results of the low temperature sensing of carbon monoxide (CO gas and room temperature UV sensors using one dimensional (1-D ZnO nanostructures are presented. Comb-like structures, belts and rods, and needle-shaped nanobelts were synthesized by varying synthesis temperature using a vapor transport method. Needle-like ZnO nanobelts are unique as, according to our knowledge, there is no evidence of such morphology in previous literature. The structural, morphological and optical characterization was carried out using X-ray diffraction, scanning electron microscopy and diffused reflectance spectroscopy techniques. It was observed that the sensing response of comb-like structures for UV light was greater as compared to the other grown structures. Comb-like structure based gas sensors successfully detect CO at 75 °C while other structures did not show any response.

Synthesis, characterization and magnetic properties of room-temperature nanofluid ferromagnetic graphite

OpenAIRE

Souza, N. S.; Sergeenkov, S.; Speglich, C.; Rivera, V. A. G.; Cardoso, C. A.; Pardo, H.; Mombru, A. W.; Rodrigues, A. D.; de Lima, O. F.; Araujo-Moreira, F. M.

2009-01-01

We report the chemical synthesis route, structural characterization, and physical properties of nanofluid magnetic graphite (NFMG) obtained from the previously synthesized bulk organic magnetic graphite (MG) by stabilizing the aqueous ferrofluid suspension with an addition of active cationic surfactant. The measured magnetization-field hysteresis curves along with the temperature dependence of magnetization confirmed room-temperature ferromagnetism in both MG and NFMG samples. (C) 2009 Americ...

SEM and TEM characterization of microstructure of stainless steel composites reinforced with TiB2

International Nuclear Information System (INIS)

Sulima, Iwona; Boczkal, Sonia; Jaworska, Lucyna

2016-01-01

Steel-8TiB 2 composites were produced by two new sintering techniques, i.e. Spark Plasma Sintering (SPS) and High Pressure-High Temperature (HP-HT) sintering. This study discusses the impact of these sintering methods on the microstructure of steel composites reinforced with TiB 2 particles. Scanning electron microscopy (SEM), wavelength dispersive spectroscopy (WDS), X-ray diffraction, electron backscatter diffraction (EBSD) and transmission electron microscopy (TEM) were used to analyze the microstructure evolution in steel matrix composites. The results of microscopic examinations revealed a close relationship between the composite microstructure and the methods and conditions of sintering. Substantial differences were observed in the grain size of materials sintered by HP-HT and SPS. It has been demonstrated that the composites sintered by HP-HT tend to form a chromium-iron-nickel phase in the steel matrix. In contrast, the microstructure of the composites sintered by SPS is characterized by the presence of complex borides and chromium-iron phase. - Highlights: •The steel-8TiB 2 composites were fabricated by Spark Plasma Sintering (SPS) and High Pressure-High Temperature (HP-HT). •Sintering techniques has an important effect on changes in the microstructure of steel-8TiB 2 composites. •New phases of different size and morphology were identified.

Low temperature solution synthesis of zinc antimonide, manganese antimonide, and strontium ruthenate compounds

Science.gov (United States)

Noblitt, Jennifer Lenkner

2011-12-01

Increasing energy demands are fueling research in the area of renewable energy and energy storage. In particular, Li-ion batteries and superconducting wires are attractive choices for energy storage. Improving safety, simplifying manufacturing processes, and advancing technology to increase energy storage capacity is necessary to compete with current marketed energy storage devices. These advancements are accomplished through the study of new materials and new morphologies. Increasing dependence on and rising demand for portable electronic devices has continued to drive research in the area of Li-ion batteries. In order to compete with existing batteries and be applicable to future energy needs such as powering hybrid vehicles, the drawbacks of Li-ion batteries must be addressed including (i) low power density, (ii) safety, and (iii) high manufacturing costs. These drawbacks can be addressed through new materials and morphologies for the anode, cathode, and electrolyte. New intermetallic anode materials such as ZnSb, MnSb, and Mn2Sb are attractive candidates to replace graphite, the current industry standard anode material, because they are safer while maintaining comparable theoretical capacity. Electrodeposition is an inexpensive method that could be used for the synthesis of these electrode materials. Direct electrodeposition allows for excellent electrical contact to the current collector without the use of a binder. To successfully electrodeposit zinc and manganese antimonides, metal precursors with excellent solubility in water were needed. To promote solubility, particularly for the antimony precursor, coordinating ligands were added to the deposition bath solutions. This work shows that the choice of coordinating ligand and metal-ligand speciation can alter both the electrochemistry and the film composition. This work focuses on the search for appropriate coordinating ligands, solution pH, and bath temperatures so that high quality films of ZnSb, MnSb, and

Effects of novel processing techniques on glucosinolates and membrane associated myrosinases in broccoli

OpenAIRE

Frandsen, Heidi Blok; Markedal, Keld Ejdrup; Martín Belloso, Olga; Sánchez Vega, Rogelio; Soliva-Fortuny, Robert; Sørensen, Hilmer; Sørensen, Susanne; Sørensen, Jens Christian

2014-01-01

High pressure/high temperature (HP/HT) and pulsed electric field (PEF) treatment of food are among the novel processing techniques considered as alternatives to conventional thermal food processing. Introduction of new processing techniques with fast and gentle processing steps may reveal new possibilities for preservation of healthy bioactive compounds in processed food. However, effects on various food components due to autolysis and fast reactions prior to the applied HP/HT or PEF need to ...

A self-propagation high-temperature synthesis and annealing route to synthesis of wave-like boron nitride nanotubes

Energy Technology Data Exchange (ETDEWEB)

Wang, Jilin; Zhang, Laiping [School of Materials Science and Engineering, Wuhan Institute of Technology, Wuhan, Hubei, 430073 (China); Gu, Yunle, E-mail: ncm@mail.wit.edu.cn [School of Materials Science and Engineering, Wuhan Institute of Technology, Wuhan, Hubei, 430073 (China); Pan, Xinye; Zhao, Guowei; Zhang, Zhanhui [School of Materials Science and Engineering, Wuhan Institute of Technology, Wuhan, Hubei, 430073 (China)

2013-03-15

Highlights: ► Large quantities of wave-like BN nanotubes were synthesized by SHS-annealing method. ► The catalytic boron-containing porous precursor was produced by self-propagation high-temperature synthesis method. ► Three growth models were proposed to explain the growth mechanism of the wave-like BN nanotubes. - Abstract: Large quantities of boron nitride (BN) nanotubes were synthesized by annealing a catalytic boron-containing porous precursor in flowing NH{sub 3} gas at 1180 °C. The porous precursor was prepared by self-propagation high-temperature synthesis (SHS) method at 800 °C using Mg, B{sub 2}O{sub 3} and amorphous boron powder (α-B) as the starting materials. The porous precursor played an important role in large quantities synthesis of BN nanotubes. The as-synthesized product was characterized by X-ray diffractometer (XRD), Fourier transform infrared spectrometer (FTIR), Raman, Scanning electron microscopy (SEM), X-ray energy dispersive spectroscopy (EDS), Transmission electron microscopy (TEM) and High-resolution transmission electron microscopy (HRTEM). Characterization results indicated that the BN nanotubes displayed wave-like inner structures with diameters in the range of 50–300 nm and average lengths of more than 10 μm. The possible growth mechanism of the BN nanotubes was also discussed.

Rod-Shaped Magnetite Nano/Microparticles Synthesis at Ambient Temperature

Directory of Open Access Journals (Sweden)

Balaprasad Ankamwar

2013-01-01

Full Text Available Here, we reported room temperature synthesis of Fe3O4 rod-shaped nano/microparticles by chemical reduction method from FeCl3 precursor and NaBH4 as the reducing agent in the presence of the pyrrole as a capping agent. The magnetic Fe3O4 particles were characterized by several methods, such as SEM, XRD, FTIR, and TGA. The average aspect ratio of Fe3O4 rod-shaped particles was ~2.8. These particles were redispersed in deionised water to form a colloidal solution and showed magnetic properties. This economical synthesis route is scalable, and Fe3O4 particles can be exploited for various applications such as MRI contrast enhancement, biodiseperations, Ni-Fe batteries, and as a catalyst.

Numerical investigation of high temperature synthesis gas premixed combustion via ANSYS Fluent

Directory of Open Access Journals (Sweden)

Pashchenko Dmitry

2018-01-01

Full Text Available A numerical model of the synthesis gas pre-mixed combustion is developed. The research was carried out via ANSYS Fluent software. Verification of the numerical results was carried out using experimental data. A visual comparison of the flame contours that obtained by the synthesis gas combustion for Re = 600; 800; 1000 was performed. A comparison of the wall temperature of the combustion chamber, obtained with the help of the developed model, with the results of a physical experiment was also presented. For all cases, good convergence of the results is observed. It is established that a change in the temperature of the syngas/air mixture at the inlet to the combustion chamber does not significantly affect the temperature of the combustion products due to the dissipation of the H2O and CO2 molecules. The obtained results are of practical importance for the design of heat engineering plants with thermochemical heat recovery.

Low Temperature Synthesis and Properties of Gadolinium-Doped Cerium Oxide Nanoparticles

DEFF Research Database (Denmark)

Machado, M. F. S.; Moraes, L. P. R.; Monteiro, N. K.

2017-01-01

Gadolinium-doped cerium oxide (GDC) is an attractive ceramic material for solid oxide fuel cells (SOFCs) both as the electrolyte and in composite electrodes operating at low and intermediate temperatures. GDC exhibits high oxygen ion conductivity at a wide range of temperatures and displays a high...... resistance to carbon deposition when hydrocarbons are used as fuels. However, an inconvenience of ceria-based oxides is the high sintering temperature needed to obtain a fully dense ceramic body. In this study, a green chemistry route for the synthesis of 10 mol% GDC nanoparticles is proposed. The aqueous...

Room temperature chemical synthesis of Cu(OH){sub 2} thin films for supercapacitor application

Energy Technology Data Exchange (ETDEWEB)

Gurav, K.V. [Thin Film Photonic and Electronics Lab, Department of Materials Science and Engineering, Chonnam National University, 300 Yongbong-dong, Puk-Gu, Gwangju 500-757 (Korea, Republic of); Patil, U.M. [Thin Film Physics Laboratory, Department of Physics, Shivaji University, Kolhapur 416 007 (M.S.) (India); Shin, S.W.; Agawane, G.L.; Suryawanshi, M.P.; Pawar, S.M.; Patil, P.S. [Thin Film Photonic and Electronics Lab, Department of Materials Science and Engineering, Chonnam National University, 300 Yongbong-dong, Puk-Gu, Gwangju 500-757 (Korea, Republic of); Lokhande, C.D. [Thin Film Physics Laboratory, Department of Physics, Shivaji University, Kolhapur 416 007 (M.S.) (India); Kim, J.H., E-mail: jinhyeok@chonnam.ac.kr [Thin Film Photonic and Electronics Lab, Department of Materials Science and Engineering, Chonnam National University, 300 Yongbong-dong, Puk-Gu, Gwangju 500-757 (Korea, Republic of)

2013-10-05

Highlights: •Cu(OH){sub 2} is presented as the new supercapacitive material. •The novel room temperature method used for the synthesis of Cu(OH){sub 2}. •The hydrous, nanograined Cu(OH){sub 2} shows higher specific capacitance of 120 F/g. -- Abstract: Room temperature soft chemical synthesis route is used to grow nanograined copper hydroxide [Cu(OH){sub 2}] thin films on glass and stainless steel substrates. The structural, morphological, optical and wettability properties of Cu(OH){sub 2} thin films are studied by means of X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), field emission scanning electron microscopy (FESEM), UV–vis spectrophotometer and water contact angle measurement techniques. The results showed that, room temperature chemical synthesis route allows to form the nanograined and hydrophilic Cu(OH){sub 2} thin films with optical band gap energy of 3.0 eV. The electrochemical properties of Cu(OH){sub 2} thin films are studied in an aqueous 1 M NaOH electrolyte using cyclic voltammetry. The sample exhibited supercapacitive behavior with 120 F/g specific capacitance.

The effect of temperature in flux-assisted synthesis of SnNb2O6

KAUST Repository

Noureldine, Dalal; Takanabe, Kazuhiro

2014-01-01

A flux-assisted method was used to synthesize SnNb2O6 as a visible-light-responsive metal oxide photocatalyst. The role of synthesis temperature was investigated in detail using different reaction temperatures (300, 500, 600, 800, 1000 °C

Room temperature synthesis of protonated layered titanate sheets using peroxo titanium carbonate complex solution.

Science.gov (United States)

Sutradhar, Narottam; Sinhamahapatra, Apurba; Pahari, Sandip Kumar; Bajaj, Hari C; Panda, Asit Baran

2011-07-21

We report the synthesis of peroxo titanium carbonate complex solution as a novel water-soluble precursor for the direct synthesis of layered protonated titanate at room temperature. The synthesized titanates showed excellent removal capacity for Pb(2+) and methylene blue. Based on experimental observations, a probable mechanism for the formation of protonated layered dititanate sheets is also discussed.

Synthesis and characterization of strontium carboxylates at room temperature and at high temperature in autoclave vessels

DEFF Research Database (Denmark)

Christgau, Stephan; Ståhl, Kenny; Andersen, Jens Enevold Thaulov

2006-01-01

A novel method was developed for synthesis of strontium coordination compounds in high yields. The synthesis proceeded along three pathways that provided strontium salts in high purity and high yields, close to 100%, as confirmed by flame atomic absorption spectroscopy (FAAS) and powder x......-ray crystallography. Optimum conditions were found at T = 120-1400C, a base-to-acid ratio of 1.2 and 15 min. of reaction-time in an autoclave vessel. Large crystals were readily obtained within a time period of hours. The crystal structures of strontium D-glutamate hexahydrate (I) and strontium di-(hydrogen L......-glutamate) pentahydrate (II) were confirmed by X-ray powder diffraction at 295 K and Rietveld refinements (I: Space group P212121, Z=4, a=7.3519(2), b=8.7616(2), c=20.2627(5) Å, and II: Space group P21, Z=2, a=8.7243(1), b=7.2635(1), c=14.6840(2) Å, β=100.5414(7) °). Synthesis at room temperature provided four additional...

Foundations of low-temperature plasma enhanced materials synthesis and etching

Science.gov (United States)

Oehrlein, Gottlieb S.; Hamaguchi, Satoshi

2018-02-01

Low temperature plasma (LTP)-based synthesis of advanced materials has played a transformational role in multiple industries, including the semiconductor industry, liquid crystal displays, coatings and renewable energy. Similarly, the plasma-based transfer of lithographically defined resist patterns into other materials, e.g. silicon, SiO2, Si3N4 and other electronic materials, has led to the production of nanometer scale devices that are the basis of the information technology, microsystems, and many other technologies based on patterned films or substrates. In this article we review the scientific foundations of both LTP-based materials synthesis at low substrate temperature and LTP-based isotropic and directional etching used to transfer lithographically produced resist patterns into underlying materials. We cover the fundamental principles that are the basis of successful application of the LTP techniques to technological uses and provide an understanding of technological factors that may control or limit material synthesis or surface processing with the use of LTP. We precede these sections with a general discussion of plasma surface interactions, the LTP-generated particle fluxes including electrons, ions, radicals, excited neutrals and photons that simultaneously contact and modify surfaces. The surfaces can be in the line of sight of the discharge or hidden from direct interaction for structured substrates. All parts of the article are extensively referenced, which is intended to help the reader study the topics discussed here in more detail.

ACBC to Balcite: Bioinspired Synthesis of a Highly Substituted High-Temperature Phase from an Amorphous Precursor

Energy Technology Data Exchange (ETDEWEB)

Whittaker, Michael L.; Joester, Derk (NWU)

2017-04-28

Energy-efficient synthesis of materials locked in compositional and structural states far from equilibrium remains a challenging goal, yet biomineralizing organisms routinely assemble such materials with sophisticated designs and advanced functional properties, often using amorphous precursors. However, incorporation of organics limits the useful temperature range of these materials. Herein, the bioinspired synthesis of a highly supersaturated calcite (Ca0.5Ba0.5CO3) called balcite is reported, at mild conditions and using an amorphous calcium–barium carbonate (ACBC) (Ca1- x Ba x CO3·1.2H2O) precursor. Balcite not only contains 50 times more barium than the solubility limit in calcite but also displays the rotational disorder on carbonate sites that is typical for high-temperature calcite. It is significantly harder (30%) and less stiff than calcite, and retains these properties after heating to elevated temperatures. Analysis of balcite local order suggests that it may require the formation of the ACBC precursor and could therefore be an example of nonclassical nucleation. These findings demonstrate that amorphous precursor pathways are powerfully enabling and provide unprecedented access to materials far from equilibrium, including high-temperature modifications by room-temperature synthesis.

Room temperature synthesis of porous SiO2 thin films by plasma enhanced chemical vapor deposition

OpenAIRE

Barranco Quero, Ángel; Cotrino Bautista, José; Yubero Valencia, Francisco; Espinós, J. P.; Rodríguez González-Elipe, Agustín

2004-01-01

Synthesis of porous SiO2 thin films in room temperature was carried out using plasma enhanced chemical vapor deposition (CVD) in an electron cyclotron resonance microwave reactor with a downstream configuration.The gas adsorption properties and the type of porosity of the SiO2 thin films were assessed by adsorption isotherms of toluene at room temperature.The method could also permit the tailoring synthesis of thin films when both composition and porosity can be simultaneously and independent...

An Investigation of Porous Structure of TiNi-Based SHS-Materials Produced at Different Initial Synthesis Temperatures

Science.gov (United States)

Khodorenko, V. N.; Anikeev, S. G.; Kokorev, O. V.; Yasenchuk, Yu. F.; Gunther, V. É.

2018-02-01

An investigation of structural characteristics and behavior of TiNi-based pore-permeable materials manufactured by the methods of selfpropagating high-temperature synthesis (SHS) at the initial synthesis temperatures T = 400 and 600°C is performed. It is shown that depending on the temperature regime, the resulting structure and properties of the material can differ. It is found out that the SHS-material produced at the initial synthesis temperature T = 400°C possesses the largest number of micropores in the pore wall surface structure due to a high phase inhomogeneity of the alloy. The regime of structure optimization of the resulting materials is described and the main stages of formation of the pore wall microporous surfaces are revealed. It is demonstrated that after optimization of the surface structure of a TiNi-based fine-pore alloy by its chemical etching, the fraction of micropores measuring in size less than 50 nm increased from 59 to 68%, while the number of pores larger than 1 μm increased twofold from 11 to 22%. In addition, peculiar features of interaction between certain cell cultures with the surface of the SHS-material manufactured at different initial synthesis temperatures are revealed. It is found out that the dynamics of the cell material integration depends on the pore wall surface morphology and dimensions of macropores.

Fabrication of Titanium Diboride-Cu Composite by Self-High Temperature Synthesis plus Quick Press

Institute of Scientific and Technical Information of China (English)

Jinyong ZHANG; Zhengyi FU; Weimin WANG

2005-01-01

Titanium diboride based composites, good candidates for contact materials, have high hardness, Young's modulus,high temperature stability, and excellent electrical, thermal conductivity. However a good interface of TiB2/Cu is very difficult to achieve for oxidation of TiB2. To avoid this oxidation behavior, the in situ combusting synthesis technology, SHS, was used to prepare TiB2/Cu composite. Thecharacters of Ti-B-xCu SHS were studied in detail,such as combustion temperature, products phases and grain size. Based on the experimental results a proper technology way of self-high temperature synthesis plus quick press (SHS/QP) was determined and compact TiB2/Cu composites with relative density over than 97 pct of the theoretical were fabricated by this method. The properties and microstructures of these TiB2 based composites were also investigated.

ESR characterization of point defects in amber colored c-BN super abrasive powders

International Nuclear Information System (INIS)

Nistor, S.V.; Ghica, D.; Stefan, M.; Bouwen, A.; Goovaerts, E.

2004-01-01

Cubic boron nitride (c-BN) crystalline superabrasive powder (Borazon ** CBN 400), consisting of 200-300 microns sized amber colored crystallites prepared by HP/HT synthesis, has been examined from 2.1 K to 293 K by X-band ESR spectroscopy. The observed spectrum consists of a component line A1, visible in the whole temperature range, and two component lines A2 and A3, visible at high and low temperatures, respectively. The A1 and A3 lines originate from transitions inside S = 1/2 ground states of distinct paramagnetic species and A2 from transitions inside an excited state of another paramagnetic center. The intensity of the A1 and A3 lines changes differently during in situ low temperature illumination in the UV-VIS range. * Borazon is a registered trademark of Diamond Innovations, Inc. (copyright 2004 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

Mechanically activated self-propagated high-temperature synthesis of nanometer-structured MgB2

International Nuclear Information System (INIS)

Radev, D.D.; Marinov, M.; Tumbalev, V.; Radev, I.; Konstantinov, L.

2005-01-01

Nanometer-sized MgB 2 was prepared via a two-step modification of the mechanically activated self-propagated high-temperature synthesis. The experimental conditions and some structural and phase characteristics of the synthesized product are reported. It is shown that a single-phase material can be prepared after 2 h of intense mechanical treatment of the starting magnesium and boron powders and a synthesis induced at a current-pulse density of 30 A cm -2 . The average size of MgB 2 particles synthesized in this way is 70-80 nm. It is also shown that using the same reagents and the 'classic' high-temperature interaction at 850 deg C with a protective atmosphere of pure Ar, mean particle size of the MgB 2 obtained is 50 μm

Preparation of high temperature superconductor ceramics using cuban reactives. Optimization of the synthesis method

International Nuclear Information System (INIS)

Leyva Fabelo, A.; Cruz, C.; Aragon, B.; Suarez, J.C.; Mora, M.

1991-01-01

Results of the crystallographic characterization of a group of Cuban Products, which are evaluated to be employed in HTSC fabrication are presented in this paper. The first results on the synthesis of HTSC (RBa 2 Cu 3 0 7δ , R= Y, La, Nd) using Cuban reactives, are presented. The so called 'solid state reaction method of synthesis' was optimized, obtaining a critical temperature of more than 93 k

Low temperature synthesis of InP nanocrystals

International Nuclear Information System (INIS)

Ung Thi Dieu Thuy; Tran Thi Thuong Huyen; Nguyen Quang Liem; Reiss, Peter

2008-01-01

We present a simple method for the chemical synthesis of InP nanocrystals, which comprises several advantages: (i) the use of simple reagents, namely InCl 3 .4H 2 O and yellow P as the In and P precursors, respectively, and NaBH 4 as the reducing agent in a mixed solvent of ethanol and toluene; (ii) a short reaction time (1-5 h) and low temperature (<75 deg. C); (iii) a high reaction yield approaching 100%. InP NCs in the zinc-blende structure have been obtained as confirmed by powder X-ray diffraction and Raman scattering measurements. Their mean size of 4 nm has been determined by transmission electron microscopy, Raman scattering and absorption spectroscopy

Exploring the Phase Diagram SiO2-CO2 at High Pressures and Temperatures

Science.gov (United States)

Kavner, A.

2015-12-01

CO2 is an important volatile system relevant for planetary sciences and fundamental chemistry. Molecular CO2 has doubly bonded O=C=O units but high pressure-high temperature (HP-HT) studies have recently shown its transformation into a three-dimensional network of corner-linked [CO4] units analogous to the silica mineral polymorphs, through intermediate non-molecular phases. Here, we report P-V-T data on CO2-IV ice from time-of-flight neutron diffraction experiments, which allow determining the compressibility and thermal expansivity of this intermediate molecular-to-non-molecular phase.1 Aditionally, we have explored the SiO2-CO2 phase diagram and the potential formation of silicon carbonate compounds. New data obtained by laser-heating diamond-anvil experiments in CO2-filled microporous silica polymorphs will be shown. In particular, these HP-HT experiments explore the existence of potential CO2/SiO2 compounds with tetrahedrally-coordinated C/Si atoms by oxygens, which are predicted to be stable (or metastable) by state-of-the-art ab initio simulations.2,3 These theoretical predictions were supported by a recent study that reports the formation of a cristobalite-type Si0.4C0.6O2 solid solution at high-pressures and temperatures, which can be retained as a metastable solid down to ambient conditions.4 Entirely new families of structures could exist based on [CO4]4- units in various degrees of polymerisation, giving rise to a range of chain, sheet and framework solids like those found in silicate chemistry. References[1] S. Palaich et al., Am. Mineral. Submitted (2015) [2] A. Morales-Garcia et al., Theor. Chem. Acc. 132, 1308 (2013) [3] R. Zhou et al., Phys. Rev. X, 4, 011030 (2014) [4] M. Santoro et al. Nature Commun. 5, 3761 (2014)

Synthesis of ammonia directly from air and water at ambient temperature and pressure

Science.gov (United States)

Lan, Rong; Irvine, John T. S.; Tao, Shanwen

2013-01-01

The N≡N bond (225 kcal mol−1) in dinitrogen is one of the strongest bonds in chemistry therefore artificial synthesis of ammonia under mild conditions is a significant challenge. Based on current knowledge, only bacteria and some plants can synthesise ammonia from air and water at ambient temperature and pressure. Here, for the first time, we report artificial ammonia synthesis bypassing N2 separation and H2 production stages. A maximum ammonia production rate of 1.14 × 10−5 mol m−2 s−1 has been achieved when a voltage of 1.6 V was applied. Potentially this can provide an alternative route for the mass production of the basic chemical ammonia under mild conditions. Considering climate change and the depletion of fossil fuels used for synthesis of ammonia by conventional methods, this is a renewable and sustainable chemical synthesis process for future. PMID:23362454

Synthesis of ammonia directly from air and water at ambient temperature and pressure.

Science.gov (United States)

Lan, Rong; Irvine, John T S; Tao, Shanwen

2013-01-01

The N≡N bond (225 kcal mol⁻¹) in dinitrogen is one of the strongest bonds in chemistry therefore artificial synthesis of ammonia under mild conditions is a significant challenge. Based on current knowledge, only bacteria and some plants can synthesise ammonia from air and water at ambient temperature and pressure. Here, for the first time, we report artificial ammonia synthesis bypassing N₂ separation and H₂ production stages. A maximum ammonia production rate of 1.14 × 10⁻⁵ mol m⁻² s⁻¹ has been achieved when a voltage of 1.6 V was applied. Potentially this can provide an alternative route for the mass production of the basic chemical ammonia under mild conditions. Considering climate change and the depletion of fossil fuels used for synthesis of ammonia by conventional methods, this is a renewable and sustainable chemical synthesis process for future.

Room temperature synthesis of an optically and thermally responsive hybrid PNIPAM-gold nanoparticle

International Nuclear Information System (INIS)

Morones, J. Ruben; Frey, Wolfgang

2010-01-01

Composites of metal nanoparticles and environmentally sensitive polymers are useful as nanoactuators that can be triggered externally using light of a particular wavelength. We demonstrate a synthesis route that is easier than grafting techniques and allows for the in situ formation of individual gold nanoparticles encapsulated by an environmentally sensitive polymer, while also providing a strong interaction between the polymer and the metal particle. We present a one-pot, room-temperature synthesis route for gold metal nanoparticles that uses poly-N-isopropyl acrylamide as the capping and stabilizing agent and ascorbic acid as the reducing agent and achieves size control similar to the most common citric acid synthesis. We show that the composite can be precipitated reversibly by temperature or light using the non-radiative decay and conversion to heat of the surface plasmon resonance of the metal nanoparticle. The precipitation is induced by the collapse of the polymer cocoon surrounding each gold nanoparticle, as can be seen by surface plasmon spectroscopy. The experiments agree with theoretical models for the heat generation in a colloidal suspension that support fast switching with low laser power densities. The synthesized composite is a simple nanosized opto-thermal switch.

Superhard nanophase cutter materials for rock drilling applications; FINAL

International Nuclear Information System (INIS)

Voronov, O.; Tompa, G.; Sadangi, R.; Kear, B.; Wilson, C.; Yan, P.

2000-01-01

The Low Pressure-High Temperature (LPHT) System has been developed for sintering of nanophase cutter and anvil materials. Microstructured and nanostructured cutters were sintered and studied for rock drilling applications. The WC/Co anvils were sintered and used for development of High Pressure-High Temperature (HPHT) Systems. Binderless diamond and superhard nanophase cutter materials were manufactured with help of HPHT Systems. The diamond materials were studied for rock machining and drilling applications. Binderless Polycrystalline Diamonds (BPCD) have high thermal stability and can be used in geothermal drilling of hard rock formations. Nanophase Polycrystalline Diamonds (NPCD) are under study in precision machining of optical lenses. Triphasic Diamond/Carbide/Metal Composites (TDCC) will be commercialized in drilling and machining applications

Synthesis of Li2SiO3 at low temperature

International Nuclear Information System (INIS)

Mondragon G, G.

2007-01-01

The main objective of this work is to develop a new synthesis method to obtain one of the more studied ceramics in this field Li 2 SiO 3 ) in a simple and economic way using different solutions (urea and ammonium hydroxide). The particular objectives are first to prepare the Li 2 SiO 3 ceramic, by means of the use of the reaction conventional technique in solid state at temperatures between 800 and 900 C to compare it with the one proposed in this work and this way to observe the advantages that it would gives us the new method. Later on, the same one was synthesized lithium ceramic (Li 2 SiO 3 ) by means of the new method at low temperature (between 80 and 90 C), using silicic acid and lithium hydroxide like precursory reagents and different solutions (urea and ammonium hydroxide) for the optimization in their synthesis. Finally, it was carried out the characterization of these materials by means of X-ray diffraction (XRD), electronic microscopes (SEM and TEM), nitrogen physisorption (method BET) and thermal gravimetric analysis (TGA) to observe the differences that exist among the conventional method and the proposed method and by this way to determine the advantages of the last method. (Author)

Low-temperature synthesis and characterization of helical carbon fibers by one-step chemical vapour deposition

Energy Technology Data Exchange (ETDEWEB)

Jin, Yongzhong [Department of Materials and Chemistry Engineering, Sichuan University of Science and Engineering, 643000 Zigong, Sichuan (China); Chen, Jian, E-mail: wuhangzs@163.com [Department of Materials and Chemistry Engineering, Sichuan University of Science and Engineering, 643000 Zigong, Sichuan (China); Fu, Qingshan [Department of Materials and Chemistry Engineering, Sichuan University of Science and Engineering, 643000 Zigong, Sichuan (China); Li, Binghong [China Rubber Group Carbon Black Industry Research and Design Institute, 643000 Zigong, Sichuan (China); Zhang, Huazhi; Gong, Yong [Department of Materials and Chemistry Engineering, Sichuan University of Science and Engineering, 643000 Zigong, Sichuan (China)

2015-01-01

Graphical abstract: - Highlights: • HCNFs were synthesized by one-step CVD using cupric tartrate as a catalyst at temperature below 500 °C. • The synthesis of HCNFs is highly temperature-dependent at the synthesis temperature of 280–480 °C. • The addition of HCNFs makes a noticeable contribution to the reinforcement of NR/CB system. - Abstract: Helical carbon fibers (HCNFs) were synthesized by one-step chemical vapour deposition using cupric tartrate as a catalyst at temperature below 500 °C. The bound rubber of natural rubber (NR)/HCNFs were also prepared in this study. The results of thermogravimetry–differential scanning calorimetry (TG/DSC) for cupric tartrate nanoparticles show that the transformation of C{sub 4}H{sub 4}CuO{sub 6} → Cu reaction occurs at ∼250–310 °C. The characterization of scanning electron microscopy (SEM), transmission electron microscope (TEM), X-ray diffraction (XRD) and Raman spectrum for the synthesized products confirms that the synthesis of HCNFs is highly temperature-dependent. The straight fibers with the fiber diameter of 100–400 nm are obtained at 280 °C and HCNFs can be synthesized at higher temperature, with the coil diameter of 0.5–1 μm and fiber diameter of 100–200 nm at 380 °C, and the coil diameter of ∼100 nm and fiber diameter of ∼80 nm at 480 °C. The maximum of the bound-rubber content (37%) can be obtained with the addition of 100 wt.% HCNFs in NR, which indicates that the coiled configuration of HCNFs makes a noticeable contribution to the reinforcement of NR/CB system.

Low-temperature synthesis and characterization of helical carbon fibers by one-step chemical vapour deposition

International Nuclear Information System (INIS)

Jin, Yongzhong; Chen, Jian; Fu, Qingshan; Li, Binghong; Zhang, Huazhi; Gong, Yong

2015-01-01

Graphical abstract: - Highlights: • HCNFs were synthesized by one-step CVD using cupric tartrate as a catalyst at temperature below 500 °C. • The synthesis of HCNFs is highly temperature-dependent at the synthesis temperature of 280–480 °C. • The addition of HCNFs makes a noticeable contribution to the reinforcement of NR/CB system. - Abstract: Helical carbon fibers (HCNFs) were synthesized by one-step chemical vapour deposition using cupric tartrate as a catalyst at temperature below 500 °C. The bound rubber of natural rubber (NR)/HCNFs were also prepared in this study. The results of thermogravimetry–differential scanning calorimetry (TG/DSC) for cupric tartrate nanoparticles show that the transformation of C 4 H 4 CuO 6 → Cu reaction occurs at ∼250–310 °C. The characterization of scanning electron microscopy (SEM), transmission electron microscope (TEM), X-ray diffraction (XRD) and Raman spectrum for the synthesized products confirms that the synthesis of HCNFs is highly temperature-dependent. The straight fibers with the fiber diameter of 100–400 nm are obtained at 280 °C and HCNFs can be synthesized at higher temperature, with the coil diameter of 0.5–1 μm and fiber diameter of 100–200 nm at 380 °C, and the coil diameter of ∼100 nm and fiber diameter of ∼80 nm at 480 °C. The maximum of the bound-rubber content (37%) can be obtained with the addition of 100 wt.% HCNFs in NR, which indicates that the coiled configuration of HCNFs makes a noticeable contribution to the reinforcement of NR/CB system

Low temperature synthesis of InP nanocrystals

Energy Technology Data Exchange (ETDEWEB)

Ung Thi Dieu Thuy [Institute of Materials Science (IMS), Vietnamese Academy of Science and Technology (VAST), 18 Hoang Quoc Viet, Cau Giay, Hanoi (Viet Nam); Tran Thi Thuong Huyen [Institute of Materials Science (IMS), Vietnamese Academy of Science and Technology (VAST), 18 Hoang Quoc Viet, Cau Giay, Hanoi (Viet Nam); National University of Thai Nguyen, 2 Luong Ngoc Quyen, Thai Nguyen (Viet Nam); Nguyen Quang Liem [Institute of Materials Science (IMS), Vietnamese Academy of Science and Technology (VAST), 18 Hoang Quoc Viet, Cau Giay, Hanoi (Viet Nam)], E-mail: liemnq@ims.vast.ac.vn; Reiss, Peter [DSM/INAC/SPrAM, UMR 5819 CEA-CNRS-Universite Joseph Fourier/LEMOH, CEA Grenoble, 17 rue des Martyrs, 38054 Grenoble Cedex 9 (France)

2008-12-20

We present a simple method for the chemical synthesis of InP nanocrystals, which comprises several advantages: (i) the use of simple reagents, namely InCl{sub 3}.4H{sub 2}O and yellow P as the In and P precursors, respectively, and NaBH{sub 4} as the reducing agent in a mixed solvent of ethanol and toluene; (ii) a short reaction time (1-5 h) and low temperature (<75 deg. C); (iii) a high reaction yield approaching 100%. InP NCs in the zinc-blende structure have been obtained as confirmed by powder X-ray diffraction and Raman scattering measurements. Their mean size of 4 nm has been determined by transmission electron microscopy, Raman scattering and absorption spectroscopy.

Excitation temperature of a solution plasma during nanoparticle synthesis

Energy Technology Data Exchange (ETDEWEB)

Saito, Genki, E-mail: genki@eng.hokudai.ac.jp; Nakasugi, Yuki; Akiyama, Tomohiro [Center for Advanced Research of Energy and Materials, Hokkaido University, Sapporo 060-8628 (Japan)

2014-08-28

Excitation temperature of a solution plasma was investigated by spectroscopic measurements to control the nanoparticle synthesis. In the experiments, the effects of edge shielding, applied voltage, and electrode material on the plasma were investigated. When the edge of the Ni electrode wire was shielded by a quartz glass tube, the plasma was uniformly generated together with metallic Ni nanoparticles. The emission spectrum of this electrode contained OH, H{sub α}, H{sub β}, Na, O, and Ni lines. Without an edge-shielded electrode, the continuous infrared radiation emitted at the edge created a high temperature on the electrode surface, producing oxidized coarse particles as a result. The excitation temperature was estimated from the Boltzmann plot. When the voltages were varied at the edge-shielded electrode with low average surface temperature by using different electrolyte concentrations, the excitation temperature of current-concentration spots increased with an increase in the voltage. The size of the Ni nanoparticles decreased at high excitation temperatures. Although the formation of nanoparticles via melting and solidification of the electrode surface has been considered in the past, vaporization of the electrode surface could occur at a high excitation temperature to produce small particles. Moreover, we studied the effects of electrodes of Ti, Fe, Ni, Cu, Zn, Zr, Nb, Mo, Pd, Ag, W, Pt, Au, and various alloys of stainless steel and Cu–Ni alloys. With the exception of Ti, the excitation temperatures ranged from 3500 to 5500 K and the particle size depended on both the excitation temperature and electrode-material properties.

Synthesis of titanium carbide from wood by self-propagating high temperature synthesis

Directory of Open Access Journals (Sweden)

Sutham Niyomwas

2010-05-01

Full Text Available Titanium carbide (TiC particles were obtained in situ by a self-propagating high temperature synthesis (SHS of wooddust with TiO2 and Mg. The reaction was carried out in a SHS reactor under static argon gas at the pressure of 0.5 MPa. Thestandard Gibbs energy minimization method was used to calculate the equilibrium composition of the reacting species. Theeffects of increasing Mg mole ratio to the precursor mixture of TiO2 and wood dusts were investigated. XRD and SEManalyses indicate a complete reaction of the precursors to yield TiC-MgO as a product composite. The synthesized compositeswere leached with 0.1M HCl acid solution to obtain TiC particles as final products.

Reduce synthesis temperature and improve dispersion of YAG nanopowders based on the co-crystallization method

Energy Technology Data Exchange (ETDEWEB)

Fan, G.F.; Tang, Y.Q.; Lu, W.Z., E-mail: lwz@mail.hust.edu.cn; Zhang, X.R.; Xu, X.

2015-01-05

Highlights: • YAG nanopowders were synthesized through a co-crystallization method. • A three-layer core–shell structure was made to lower the synthesis temperature. • PAA again reduced the synthesis temperature based on the core–shell structure. • YAG nanopowders were synthesized at 700 °C in normal apparatus. • Agglomeration was greatly improved by PAA. - Abstract: Pure yttrium aluminum garnet (YAG) nanopowders were synthesized at 950 °C from the co-crystallization precursor of Y(NO{sub 3}){sub 3}⋅6H{sub 2}O and Al(NO{sub 3}){sub 3}⋅9H{sub 2}O (nitrate process). When 17 wt.% of Y(NO{sub 3}){sub 3}⋅6H{sub 2}O was replaced by Y{sub 2}O{sub 3} nanopowders, so as to make up a three-layer core–shell structure of the precursor, the synthesis temperature was reduced to 850 °C (Y{sub 2}O{sub 3} process). Based on Y{sub 2}O{sub 3} process, further reducing the synthesis temperature to 700 °C was realized by adding polyacrylic acid (PAA, 50% M), which was used to shorten the distance of the metal ions and provide combustion heat (PAA process). TEM characterizations indicated that the powders produced through nitrate and Y{sub 2}O{sub 3} processes agglomerated, while the powders produced through PAA process were dispersed much better. The agglomerate size analysis results demonstrated that the powders produced through PAA process were with smaller agglomerate size and wider agglomerate size distribution than those through nitrate process or Y{sub 2}O{sub 3} process. And they were more likely to be sintered to YAG transparent ceramics.

SYNTHESIS AND FABRICATION OF MO-W COMPONENTS FOR NEUTRON RESONANCE SPECTROSCOPY TEMPERATURE MEASUREMENT

International Nuclear Information System (INIS)

BINGERT, S.; DESCH, P.; TRUJILLO, E.

1999-01-01

A Molybdenum-- 182 Tungsten (Mo- 182 W) alloy was specified for an application that would ultimately result in the measurement of temperature and particle velocity during the steady state time following the shock loading of various materials. The 182 W isotope provides a tag for the analysis of neutron resonance line shape from which the temperature may be calculated. The material was specified to have 1.8 atom percent W, with W-rich regions no larger than 1 microm in size. Both the composition and W distribution were critical to the experiment. Another challenge to the processing was the very small quantity of 182 W material available for the synthesis of the alloy. Therefore, limited fabrication routes were available for evaluation. Several synthesis and processing routes were explored to fabricate the required alloy components. First, precipitation of W onto Mo powder using ammonium metatungstate was investigated for powder synthesis followed by uniaxial hot pressing. Second, mechanical alloying (MA) followed by hot isostatic pressing (HIP) and warm forging was attempted. Finally, arc-melting techniques followed by either hot rolling or crushing the alloyed button into powder and consolidation were pursued. The results of the processing routes and characterization of the materials produced will be discussed

Experimental and Numerical Studies on Self-Propagating High-Temperature Synthesis of Ta5Si3 Intermetallics

Directory of Open Access Journals (Sweden)

Chun-Liang Yeh

2015-09-01

Full Text Available Formation of Ta5Si3 by self-propagating high-temperature synthesis (SHS from elemental powder compacts of Ta:Si = 5:3 was experimentally and numerically studied. Experimental evidence showed that the increase of either sample density or preheating temperature led to the increase of combustion wave velocity and reaction temperature. The apparent activation energy, Ea ≈ 108 kJ/mol, was determined for the synthesis reaction. Based upon numerical simulation, the Arrhenius factor of the rate function, K0 = 2.5 × 107 s−1, was obtained for the 5Ta + 3Si combustion system. In addition, the influence of sample density on combustion wave kinetics was correlated with the effective thermal conductivity (keff of the powder compact. By adopting 0.005 ≤ keff/kbulk ≤ 0.016 in the computation model, the calculated combustion velocity and temperature were in good agreement with experimental data of the samples with compaction densities between 35% and 45% theoretical maximum density (TMD.

Room temperature synthesis of ReS2 through aqueous perrhenate sulfidation

Science.gov (United States)

Borowiec, Joanna; Gillin, William P.; Willis, Maureen A. C.; Boi, Filippo S.; He, Y.; Wen, J. Q.; Wang, S. L.; Schulz, Leander

2018-02-01

In this study, a direct sulfidation reaction of ammonium perrhenate (NH4ReO4) leading to a synthesis of rhenium disulfide (ReS2) is demonstrated. These findings reveal the first example of a simplistic bottom-up approach to the chemical synthesis of crystalline ReS2. The reaction presented here takes place at room temperature, in an ambient and solvent-free environment and without the necessity of a catalyst. The atomic composition and structure of the as-synthesized product were characterized using several analysis techniques including energy dispersive x-ray spectroscopy, x-ray photoelectron spectroscopy, x-ray diffraction, transmission electron microscopy, Raman spectroscopy, thermogravimetric analysis and differential scanning calorimetry. The results indicated the formation of a lower symmetry (1Tʹ) ReS2 with a low degree of layer stacking.

Synthesis of free standing nanocrystalline Cu by ball milling at cryogenic temperature

Energy Technology Data Exchange (ETDEWEB)

Barai, K. [Department of Metallurgy and Materials Engineering, Bengal Engineering College, Shibpur, Howrah 711103 (India); Tiwary, C.S. [Department of Materials Engineering, Indian Institute of Science, Bangalore 560012 (India); Chattopadhyay, P.P. [Department of Metallurgy and Materials Engineering, Bengal Engineering College, Shibpur, Howrah 711103 (India); Chattopadhyay, K., E-mail: kamanio@materials.iisc.ernet.in [Department of Materials Engineering, Indian Institute of Science, Bangalore 560012 (India)

2012-12-15

This paper reports for the first time synthesis of free standing nano-crystalline copper crystals of a {approx}30-40 nm by ball milling of copper powder at 150 K under Argon atmosphere in a specially designed cryomill. The detailed characterization of these particles using multiple techniques that includes transmission electron microscopy confirms our conclusion. Careful analysis of the chemistry of these particles indicates that these particles are essentially contamination free. Through the analysis of existing models of grain size refinements during ball milling and low temperature deformation, we argue that the suppression of thermal processes and low temperature leads to formation of free nanoparticles as the process of fracture dominates over possible cold welding at low temperatures.

Low temperature synthesis of graphene on arbitrary substrates and its transport properties

Science.gov (United States)

Zhao, Rong; Akhtar, Meysam; Alruqi, Adel; Jasinski, Jacek; Sumanasekera, Gamini; Department of Physics; Astronomy, University of Louisville Collaboration; Conn CenterRenewable Energy, University of Louisville Collaboration

Here we report the direct synthesis of uniform and vertically oriented graphene films on multiple substrates including glass, Si/SiO2, and copper foil by radio-frequency plasma enhanced chemical vapor deposition (PECVD) using methane as the carbon precursor at relatively low temperatures. Raman spectra of all the samples show characteristic Raman peaks of graphene. The temperature dependence of electrical transport properties such as 4-probe resistance, thermo electrical power and hall mobility were measured for graphene grown on glass substrates at varying temperature from 500 ° C to 700 ° C. The morphological and surface characteristics were also studied by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). This work demonstrates the potential of low temperature and transfer-free graphene growth for future graphene-based electronic applications.

Organic titanates: a model for activating rapid room-temperature synthesis of shape-controlled CsPbBr3 nanocrystals and their derivatives.

Science.gov (United States)

Fang, Shaofan; Li, Guangshe; Li, Huixia; Lu, Yantong; Li, Liping

2018-04-12

The application of lead halide perovskite nanocrystals is challenged by the lack of strategies in rapid room-temperature synthesis with controlled morphologies. Here, we report on an initial study of adopting organic titanates as a model activator that promotes rapid room-temperature synthesis of shape-controlled, highly luminescent CsPbBr3 nanocrystals and their derivatives.

Room and low temperature synthesis of carbon nanofibres

International Nuclear Information System (INIS)

Boskovic, Bojan O.

2002-01-01

Carbon nanotubes and nanofibres have attracted attention in recent years as new materials with a number of very promising potential applications. Carbon nanotubes are potential candidates for field emitters in flat panel displays. Carbon nanofibres could also be used as a hydrogen storage material and as a filling material in polymer composites. Carbon nanotubes are already used as tips in scanning probe microscopy due to their remarkable mechanical and electrical properties, and could be soon used as nanotweezers. Use of carbon nanotubes in nanoelectronics will open further miniaturisation prospects. Temperatures ranging from 450 to 1000 deg C have been a required for catalytic growth of carbon nanotubes and nanofibres. Researchers have been trying to reduce the growth temperatures for decades. Low temperature growth conditions will allow the growth of carbon nanotubes on different substrates, such glass (below 650 deg C) and as plastics (below 150 deg C) over relatively large areas, which is especially suitable for fiat panel display applications. Room temperature growth conditions could open up the possibility of using different organic substrates and bio-substrates for carbon nanotubes synthesis. Carbon nanofibres have been synthesised at room temperature and low temperatures below 250 deg C using radio frequency plasma enhanced chemical vapour deposition (r.f. PECVD). Previously, the growth of carbon nanofibres has been via catalytic decomposition of hydrocarbons or carbon monoxide at temperatures above 300 deg C. To the best of our knowledge, this is the first evidence of the growth of carbon nanofibres at temperatures lower than 300 deg C by any method. The use of a transition metal catalyst and r.f.-PECVD system is required for the growth of the carbon nanofibre when a hydrocarbon flows above the catalyst. Within the semiconductor industry r.f.-PECVD is a well established technique which lends itself for the growth of carbon nanofibres for various

Timing matters: the underappreciated role of temperature ramp rate for shape control and reproducibility of quantum dot synthesis

KAUST Repository

Baumgardner, William J.

2012-01-01

Understanding the coupled kinetic and thermodynamics factors governing colloidal nanocrystals nucleation and growth are critical factors in the predictable and reproducible synthesis of advanced nanomaterials. We show that the temporal temperature profile is decisive in tuning the particle shape from pseudo-spherical to monodisperse cubes. The shape of the nanocrystals was characterized by transmission electron microscopy and X-ray diffraction. We introduce a mechanism for the shape controlled synthesis in the context of temperature-dependent nucleation and growth and provide experimental evidence to support it. © 2013 The Royal Society of Chemistry.

The effect of temperature in flux-assisted synthesis of SnNb2O6

KAUST Repository

Noureldine, Dalal

2014-10-03

A flux-assisted method was used to synthesize SnNb2O6 as a visible-light-responsive metal oxide photocatalyst. The role of synthesis temperature was investigated in detail using different reaction temperatures (300, 500, 600, 800, 1000 °C). The obtained products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), Brunauer-Emmett-Teller method (BET). The synthesis with SnCl2 as a flux led to tin niobate particles in the platelet morphology with smooth surfaces. The synthesized crystal showed 2D anisotropic growth along the (600) plane as the flux ratio increased. The particles synthesized with a high reactant to flux ratio (1:10 or higher) exhibited improved photocatalytic activity for hydrogen evolution from an aqueous methanol solution under visible radiation (λ > 420 nm). © (2014) COPYRIGHT Society of Photo-Optical Instrumentation Engineers (SPIE). Downloading of the abstract is permitted for personal use only.

Mechanically activated combustion synthesis of molybdenum borosilicides for ultrahigh-temperature structural applications

Energy Technology Data Exchange (ETDEWEB)

Esparza, Alan A.; Shafirovich, Evgeny, E-mail: eshafirovich2@utep.edu

2016-06-15

The thermal efficiency of gas-turbine power plants could be dramatically increased by the development of new structural materials based on molybdenum silicides and borosilicides, which can operate at temperatures higher than 1300 °C with no need for cooling. A major challenge, however, is to simultaneously achieve high oxidation resistance and acceptable mechanical properties at high temperatures. Materials based on Mo{sub 5}SiB{sub 2} (called T{sub 2}) phase are promising materials that offer favorable combinations of high temperature mechanical properties and oxidation resistance. In the present paper, T{sub 2} phase based materials have been obtained using mechanically activated self-propagating high-temperature synthesis (MASHS). Upon ignition, Mo/Si/B/Ti mixtures exhibited a self-sustained propagation of a spinning combustion wave, but the products were porous, contained undesired secondary phases, and had low oxidation resistance. The “chemical oven” technique has been successfully employed to fabricate denser and stronger Mo{sub 5}SiB{sub 2}–TiC, Mo{sub 5}SiB{sub 2}–TiB{sub 2}, and Mo–Mo{sub 5}SiB{sub 2}–Mo{sub 3}Si materials. Among them, Mo{sub 5}SiB{sub 2}–TiB{sub 2} material exhibits the best oxidation resistance at temperatures up to 1500 °C. - Highlights: • Mechanical activation has enabled combustion synthesis of Mo{sub 5}SiB{sub 2} based materials. • For the first time, the fabrication of Mo{sub 5}SiB{sub 2}–TiB{sub 2} material has been reported. • Among the obtained materials, Mo{sub 5}SiB{sub 2}–TiB{sub 2} exhibits the best oxidation resistance.

ZrC Ceramics Prepared by Self-propagating High-temperature Synthesis/Single Action Pressing

Directory of Open Access Journals (Sweden)

CHENG Yong

2017-01-01

Full Text Available ZrC ceramics were prepared by mechanical axial compression of self-propagating high-temperature synthesis/single action pressing (SHS/SAP.The effects of pressure on microstructure and densification of the products,as well as the relationship between displacement/variation of the load curve and SHS reaction,were studied.The structure and properties of the products were investigated by XRD and SEM.In addition,the density was measured by the drain away liquid method.Meanwhile,universal testing machine was used to record the displacement and load curve alternations.The results indicate that products are mainly composed of ZrC phase,the process of exhaust are accelerated as the increasing of pressure as well,leading to the smaller size of porosity and crystal particles.Density manifested as an increasing pattern by the elevated pressure with no longer change at 80MPa.Due to the strong attenuation of pressure at the peak of temperature,the density of the production is only 65.7% in 120MPa.The end point of the SHS reaction and the plastic time of the products can be monitored by displacement and load curve.The results provide evidence for the application of self-propagating high-temperature synthesis/pseudo-hot isostatic pressing to further improve the density of ceramics.

Effect of the synthesis temperature of sodium nona-titanate on batch kinetics of strontium-ion adsorption from aqueous solution

International Nuclear Information System (INIS)

Merceille, A.; Weinzaepfel, E.; Grandjean, A.; Merceille, A.; Weinzaepfel, E.; Barre, Y.

2011-01-01

Sodium titanate materials are promising inorganic ion exchangers for the adsorption of strontium from aqueous solutions. Sodium nona-titanate exhibits a layered structure consisting of titanate layers and exchangeable sodium ions between the layers. The materials used in this study include samples synthesized by a hydrothermal method at temperatures between 60 degrees C and 200 degrees C. Their structure, composition, and morphology were investigated with X-Ray diffraction measurements; thermogravimetric, compositional and surface area analyses, and scanning electron microscopy. The structure, composition, and morphology depended on the synthesis temperature. Batch kinetics experiments for the removal of strontium from aqueous solutions were performed, and the data were fitted by a pseudo-second-order reaction model and a diffusive model. The strontium extraction capacity also depended on the synthesis temperature and exhibited a maximum for samples synthesized at 100 degrees C. The sorption process occurs in one or two diffusion-controlled steps that also depend on the synthesis temperature. These diffusion-limited steps are the boundary-layer diffusion and intra-particle diffusion in the case of pure nona-titanate synthesized at temperatures lower than 170 degrees C, and only intra-particle diffusion in the case of nona-titanate synthesized at 200 degrees C. (authors)

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

International Nuclear Information System (INIS)

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

2013-01-01

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

Influence of Plasma Jet Temperature Profiles in Arc Discharge Methods of Carbon Nanotubes Synthesis.

Science.gov (United States)

Raniszewski, Grzegorz; Wiak, Slawomir; Pietrzak, Lukasz; Szymanski, Lukasz; Kolacinski, Zbigniew

2017-02-23

One of the most common methods of carbon nanotubes (CNTs) synthesis is application of an electric-arc plasma. However, the final product in the form of cathode deposit is composed of carbon nanotubes and a variety of carbon impurities. An assay of carbon nanotubes produced in arc discharge systems available on the market shows that commercial cathode deposits contain about 10% CNTs. Given that the quality of the final product depends on carbon-plasma jet parameters, it is possible to increase the yield of the synthesis by plasma jet control. Most of the carbon nanotubes are multiwall carbon nanotubes (MWCNTs). It was observed that the addition of catalysts significantly changes the plasma composition, effective ionization potential, the arc channel conductance, and in effect temperature of the arc and carbon elements flux. This paper focuses on the influence of metal components on plasma-jet forming containing carbon nanotubes cathode deposit. The plasma jet temperature control system is presented.

Influence of Plasma Jet Temperature Profiles in Arc Discharge Methods of Carbon Nanotubes Synthesis

Directory of Open Access Journals (Sweden)

Grzegorz Raniszewski

2017-02-01

Full Text Available One of the most common methods of carbon nanotubes (CNTs synthesis is application of an electric-arc plasma. However, the final product in the form of cathode deposit is composed of carbon nanotubes and a variety of carbon impurities. An assay of carbon nanotubes produced in arc discharge systems available on the market shows that commercial cathode deposits contain about 10% CNTs. Given that the quality of the final product depends on carbon–plasma jet parameters, it is possible to increase the yield of the synthesis by plasma jet control. Most of the carbon nanotubes are multiwall carbon nanotubes (MWCNTs. It was observed that the addition of catalysts significantly changes the plasma composition, effective ionization potential, the arc channel conductance, and in effect temperature of the arc and carbon elements flux. This paper focuses on the influence of metal components on plasma-jet forming containing carbon nanotubes cathode deposit. The plasma jet temperature control system is presented.

Instant synthesis of gold nanoparticles at room temperature and SERS applications

International Nuclear Information System (INIS)

Britto Hurtado, R.; Cortez-Valadez, M.; Ramírez-Rodríguez, L.P.; Larios-Rodriguez, Eduardo; Alvarez, Ramón A.B.; Rocha-Rocha, O.; Delgado-Beleño, Y.; Martinez-Nuñez, C.E.; Arizpe-Chávez, H.; Hernández-Martínez, A.R.; Flores-Acosta, M.

2016-01-01

Nowadays, gold nanoparticles (AuNps) can be used in a variety of applications, thus efficient methods to produce them are necessary. Several methods have been proposed in this area, but NPs production time is one limitation of these approaches. In this study, we propose a high competitive method to synthesize gold colloidal nanoparticles, instantaneously, using no-toxic reducing agents. These substances allow the instantaneous synthesis at room temperature, even without magnetic stirrers, ovens or ultrasonic baths. Optic analysis showed two absorption bands, associated with surface Plasmon as function of HAuCl_4 concentration. The nanoparticles synthesized have a 10–20 nm size, seen by the transmission electron microscopy (TEM). Therefore, it was possible to obtain several geometric patterns of AuNps, and the synthesis was performed reducing significantly processing time. Additionally, Mie and Fuchs theories were used to predict the location of the absorption bands linked to the plasmon surface in gold nanoparticles. The Surface Enhanced Raman Spectroscopy (SERS) effect was analyzed considering natural zeolite (Chabazite) as analyte, in order to determinate its possible application in soil analysis. - Highlights: • Cubic and spherical morphologies in AuNp. • Surface plasmon prediction in cubic and spherical AuNp. • Instant synthesis of AuNp. • SERS applications in soil analysis.

Instant synthesis of gold nanoparticles at room temperature and SERS applications

Energy Technology Data Exchange (ETDEWEB)

Britto Hurtado, R. [Departamento de Investigación en Física, Universidad de Sonora, Apdo. Postal 5-88, 83190, Hermosillo, Sonora (Mexico); Cortez-Valadez, M., E-mail: jose.cortez@unison.mx [CONACYT-Departamento de Investigación en Física, Universidad de Sonora, Apdo. Postal 5-88, 83190, Hermosillo, Sonora (Mexico); Ramírez-Rodríguez, L.P. [Departamento de Física, Universidad de Sonora, Apdo. Postal 5-88, 83190, Hermosillo, Sonora (Mexico); Larios-Rodriguez, Eduardo [Departamento de Ingeniería Química y Metalurgia, Universidad de Sonora, Rosales y Luis Encinas S/N, Hermosillo, Sonora (Mexico); Alvarez, Ramón A.B.; Rocha-Rocha, O.; Delgado-Beleño, Y.; Martinez-Nuñez, C.E.; Arizpe-Chávez, H. [Departamento de Investigación en Física, Universidad de Sonora, Apdo. Postal 5-88, 83190, Hermosillo, Sonora (Mexico); Hernández-Martínez, A.R. [Centro de Física Aplicada y Tecnología Avanzada (CFATA), Universidad Nacional Autónoma de México, Campus Juriquilla, Querétaro C.P. 76130 (Mexico); Flores-Acosta, M. [Departamento de Investigación en Física, Universidad de Sonora, Apdo. Postal 5-88, 83190, Hermosillo, Sonora (Mexico)

2016-08-06

Nowadays, gold nanoparticles (AuNps) can be used in a variety of applications, thus efficient methods to produce them are necessary. Several methods have been proposed in this area, but NPs production time is one limitation of these approaches. In this study, we propose a high competitive method to synthesize gold colloidal nanoparticles, instantaneously, using no-toxic reducing agents. These substances allow the instantaneous synthesis at room temperature, even without magnetic stirrers, ovens or ultrasonic baths. Optic analysis showed two absorption bands, associated with surface Plasmon as function of HAuCl{sub 4} concentration. The nanoparticles synthesized have a 10–20 nm size, seen by the transmission electron microscopy (TEM). Therefore, it was possible to obtain several geometric patterns of AuNps, and the synthesis was performed reducing significantly processing time. Additionally, Mie and Fuchs theories were used to predict the location of the absorption bands linked to the plasmon surface in gold nanoparticles. The Surface Enhanced Raman Spectroscopy (SERS) effect was analyzed considering natural zeolite (Chabazite) as analyte, in order to determinate its possible application in soil analysis. - Highlights: • Cubic and spherical morphologies in AuNp. • Surface plasmon prediction in cubic and spherical AuNp. • Instant synthesis of AuNp. • SERS applications in soil analysis.

Optical studies of high quality synthetic diamond

International Nuclear Information System (INIS)

Sharp, S.J.

1999-01-01

This thesis is concerned with the study of fundamental and defect induced optical properties of synthetic diamond grown using high pressure, high temperature (HPHT) synthesis or chemical vapour deposition (CVD). The primary technique used for investigation is cathodoluminescence (including imaging and decay-time measurements) in addition to other forms of optical spectroscopy. This thesis is timely in that the crystallinity and purity of synthetic diamond has increased ten fold over the last few years. The diamond exciton emission, which is easily quenched by the presence of defects, is studied in high quality samples in detail. In addition the ability now exists to engineer the isotopic content of synthetic diamond to a high degree of accuracy. The experimental chapters are divided as follows: Chapter 2: High resolution, low temperature spectra reveal a splitting of the free-exciton phonon recombination emission peaks and the bound-exciton zero phonon line. Included are measurements of the variation in intensity and decay-time as a function of temperature. Chapter 3: The shift in energy of the phonon-assisted free-exciton phonon replicas with isotopic content has been measured. The shift is in agreement with the results of interatomic force model for phonon scattering due to isotope disorder. Chapter 4: A study of the shift in energy with isotopic content of the diamond of the GR1 band due to the neutral vacancy has allowed a verification of the theoretical predictions due to the Jahn Teller effect. Chapter 5: The spatial distribution of the free-exciton luminescence is studied in HPHT synthetic and CVD diamond. A variation in intensity with distance from the surface is interpreted as a significant non-radiative loss of excitons to the surface. Chapter 6: The decay-times of all known self-interstitial related centres have been measured in order to calculate the concentration of these centres present in electron irradiated diamond. (author)

Shock-induced synthesis of high temperature superconducting materials

Science.gov (United States)

Ginley, D.S.; Graham, R.A.; Morosin, B.; Venturini, E.L.

1987-06-18

It has now been determined that the unique features of the high pressure shock method, especially the shock-induced chemical synthesis technique, are fully applicable to high temperature superconducting materials. Extraordinarily high yields are achievable in accordance with this invention, e.g., generally in the range from about 20% to about 99%, often in the range from about 50% to about 90%, lower and higher yields, of course, also being possible. The method of this invention involves the application of a controlled high pressure shock compression pulse which can be produced in any conventional manner, e.g., by detonation of a high explosive material, the impact of a high speed projectile or the effect of intense pulsed radiation sources such as lasers or electron beams. Examples and a discussion are presented.

Synthesis and characterization of nickel oxide particulate annealed at different temperatures

Science.gov (United States)

Sharma, Khem Raj; Thakur, Shilpa; Negi, N. S.

2018-04-01

Nickel oxide has been synthesized by solution combustion technique. The nickel oxide ceramic was annealed at 600°C and 1000°C for 2 hours. Structural, electrical, dielectric and magnetic properties were analyzed which are strongly dependent upon the synthesis method. Structural properties were examined by X-ray diffractometer (XRD), which confirmed the purity and cubic phase of nickel oxide. XRD data reveals the increase in crystallite size and decrease in full width half maximum (FWHM) as the annealing temperature increases. Electrical conductivity is found to increase from 10-6 to 10-5 (Ω-1cm-1) after annealing. Dielectric constant is observed to increase from 26 to 175 when the annealing temperature is increased from 600°C to 1000°C. Low value of coercive field is found which shows weak ferromagnetic behavior of NiO. It is observed that all the properties of NiO particulate improve with increasing annealing temperature.

Room temperature synthesis of ReS2 through aqueous perrhenate sulfidation.

Science.gov (United States)

Borowiec, Joanna; Gillin, William P; Willis, Maureen; Boi, Filippo; He, Yi; Wen, Jiqiu; Wang, Shanling; Schulz, Leander

2017-12-29

In this study, a direct sulfidation reaction of ammonium perrhenate (NH₄ReO₄) leading to a synthesis of rhenium disulfide (ReS₂) is demonstrated. These finding reveal the first example of a simplistic bottom-up approach to the chemical synthesis of crystalline ReS₂. The reaction presented here takes place at room temperature, in an ambient and solvent-free environment and without the necessity of a catalyst. The atomic composition and structure of the as-synthesized product were characterized using several analysis techniques including energy dispersive X-ray (EDX) spectroscopy, X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), transmission electron microscopy (TEM), Raman spectroscopy, thermogravimetric analysis (TGA) and differential scannig calorimetry (DSC). The results indicated the formation of a lower symmetry (1T_d) ReS₂ with a low degree of layer stacking. © 2017 IOP Publishing Ltd.

Room temperature synthesis of Si-MCM-41 using polymeric version of ethyl silicate as a source of silica

International Nuclear Information System (INIS)

Gaydhankar, T.R.; Samuel, V.; Jha, R.K.; Kumar, R.; Joshi, P.N.

2007-01-01

Synthesis of mesoporous MCM-41 materials at room temperature using less expensive polymeric version of ethyl silicate (40 wt% SiO 2 ) as a source of silica was established. The influence of crucial synthesis parameters such as molar ratios of H 2 O/NH 4 OH, NH 4 OH/SiO 2 and CTMABr/SiO 2 in gel on the quality of the phase formed was investigated. Powder X-ray diffraction (XRD), scanning electron microscopy (SEM) and low temperature N 2 adsorption-desorption isotherms have been employed to characterize the products. The magnitude of orderness, textural properties and thermal stability of the Si-MCM-41 samples prepared under identical judiciously pre-controlled synthesis conditions using ethyl silicate and conventional tetraethyl orthosilicate (TEOS) were assessed. Even though, ethyl silicate has proved to be suitable source for the preparation of MCM-41 at room temperature, there exists an optimum value of H 2 O/NH 4 OH for different NH 4 OH/SiO 2 molar ratios in the gel. Changes in the morphology were observed when NH 4 OH/SiO 2 , H 2 O/NH 4 OH molar ratios in the gels were changed

Effect of temperature on synthesis and properties of aluminum-magnesium mechanical alloys

International Nuclear Information System (INIS)

Umbrajkar, Swati M.; Schoenitz, Mirko; Jones, Steven R.; Dreizin, Edward L.

2005-01-01

The synthesis of an Al 0.7 Mg 0.3 mechanical alloy was studied using a planetary mill. Several distinct temperature regimes of mechanical alloying were achieved using milling jars equipped with finned heat sinks and an external air conditioner installed to cool the entire milling chamber. Wireless temperature sensors were attached to the milling jars to monitor the process temperature. Intermediate and final products were collected and were analyzed by electron microscopy and X-ray diffraction. The temperature history of the milling jars exhibited two peaks during mechanical alloying. The first peak occurred when particles of the starting powders deformed to produce flakes. The second peak was observed when the flakes agglomerated and re-fragmented forming layered composites that served as precursors for the mechanical alloy. The temperature of milling affected the magnesium solubility of the produced Al-Mg mechanical alloys. Decreasing the milling temperature from ∼70-80 deg. C to 20-30 deg. C resulted in an increase of the dissolved Mg concentration in Al from 2-3 at.% to ∼25 at.% for the Al 0.7 Mg 0.3 composition. The formation of intermetallic phases was favored at higher milling temperatures, where high solubilities cannot be achieved

Effect of temperature on synthesis and properties of aluminum-magnesium mechanical alloys

Energy Technology Data Exchange (ETDEWEB)

Umbrajkar, Swati M. [New Jersey Institute of Technology, Department of Mechanical Engineering, Newark, NJ 07102-1982 (United States); Schoenitz, Mirko [New Jersey Institute of Technology, Department of Mechanical Engineering, Newark, NJ 07102-1982 (United States); Jones, Steven R. [New Jersey Institute of Technology, Department of Mechanical Engineering, Newark, NJ 07102-1982 (United States); Dreizin, Edward L. [New Jersey Institute of Technology, Department of Mechanical Engineering, Newark, NJ 07102-1982 (United States)]. E-mail: dreizin@njit.edu

2005-10-27

The synthesis of an Al{sub 0.7}Mg{sub 0.3} mechanical alloy was studied using a planetary mill. Several distinct temperature regimes of mechanical alloying were achieved using milling jars equipped with finned heat sinks and an external air conditioner installed to cool the entire milling chamber. Wireless temperature sensors were attached to the milling jars to monitor the process temperature. Intermediate and final products were collected and were analyzed by electron microscopy and X-ray diffraction. The temperature history of the milling jars exhibited two peaks during mechanical alloying. The first peak occurred when particles of the starting powders deformed to produce flakes. The second peak was observed when the flakes agglomerated and re-fragmented forming layered composites that served as precursors for the mechanical alloy. The temperature of milling affected the magnesium solubility of the produced Al-Mg mechanical alloys. Decreasing the milling temperature from {approx}70-80 deg. C to 20-30 deg. C resulted in an increase of the dissolved Mg concentration in Al from 2-3 at.% to {approx}25 at.% for the Al{sub 0.7}Mg{sub 0.3} composition. The formation of intermetallic phases was favored at higher milling temperatures, where high solubilities cannot be achieved.

FORMATE-BASED FLUIDS: FORMULATION AND APPLICATION

Directory of Open Access Journals (Sweden)

Nediljka Gaurina-Međimurec

2008-12-01

Full Text Available Formate-based fluids has been successfully used in over hunders HPHT well operations since they introduced in field practice. They have many advantages when compared with conventional HPHT drilling and completion fluids such as: minimal formation damage, maintenance of additve properties at high temperatures, reduced hydraulic flow resistance, low potential for differential sticking, naturally lubricating, very low corrosion rates, biodegradable and pose little risk to the environment etc. Formate-based fluids can be applied during deep slim hole drilling, shale drilling, reservoir drilling, salt and gas hydrate formations drilling. The laboratory research was carried out to evaluate the rheological behavior of formate-based fluids as a function of temperature. Formate-based fluids were formulated using potassium formate brine, xanthan polymer, PAC, starch and calcium carbonate. Experimental results show that potassium formate improves the thermal stability of polymers.

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

Science.gov (United States)

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/+.

Application of Self-Propagating High Temperature Synthesis to the Fabrication of Actinide Bearing Nitride and Other Ceramic Nuclear Fuels

International Nuclear Information System (INIS)

Moore, John J.; Reigel, Marissa M.; Donohoue, Collin D.

2009-01-01

The project uses an exothermic combustion synthesis reaction, termed self-propagating high-temperature synthesis (SHS), to produce high quality, reproducible nitride fuels and other ceramic type nuclear fuels (cercers and cermets, etc.) in conjunction with the fabrication of transmutation fuels. The major research objective of the project is determining the fundamental SHS processing parameters by first using manganese as a surrogate for americium to produce dense Zr-Mn-N ceramic compounds. These fundamental principles will then be transferred to the production of dense Zr-Am-N ceramic materials. A further research objective in the research program is generating fundamental SHS processing data to the synthesis of (i) Pu-Am-Zr-N and (ii) U-Pu-Am-N ceramic fuels. In this case, Ce will be used as the surrogate for Pu, Mn as the surrogate for Am, and depleted uranium as the surrogate for U. Once sufficient fundamental data has been determined for these surrogate systems, the information will be transferred to Idaho National Laboratory (INL) for synthesis of Zr-Am-N, Pu-Am-Zr-N and U-Pu-Am-N ceramic fuels. The high vapor pressures of americium (Am) and americium nitride (AmN) are cause for concern in producing nitride ceramic nuclear fuel that contains Am. Along with the problem of Am retention during the sintering phases of current processing methods, are additional concerns of producing a consistent product of desirable homogeneity, density and porosity. Similar difficulties have been experienced during the laboratory scale process development stage of producing metal alloys containing Am wherein compact powder sintering methods had to be abandoned. Therefore, there is an urgent need to develop a low-temperature or low-heat fuel fabrication process for the synthesis of Am-containing ceramic fuels. Self-propagating high temperature synthesis (SHS), also called combustion synthesis, offers such an alternative process for the synthesis of Am nitride fuels. Although SHS

Single Crystal Synthesis and STM Studies of High Temperature Superconductors

Science.gov (United States)

Barrientos, Alfonso

1997-01-01

This is a final report for the work initiated in September of 1994 under the grant NAG8-1085 - NASA/OMU, on the fabrication of bulk and single crystal synthesis, specific heat measuring and STM studies of high temperature superconductors. Efforts were made to fabricate bulk and single crystals of mercury based superconducting material. A systematic thermal analysis on the precursors for the corresponding oxides and carbonates were carried out to synthesized bulk samples. Bulk material was used as seed in an attempt to grow single crystals by a two-step self flux process. On the other hand bulk samples were characterized by x-ray diffraction, electrical resistivity and magnetic susceptibility, We studied the specific heat behavior in the range from 80 to 300 K. Some preliminary attempts were made to study the atomic morphology of our samples. As part of our efforts we built an ac susceptibility apparatus for measuring the transition temperature of our sintered samples.

Heat-equilibrium low-temperature plasma decay in synthesis of ammonia via transient components N2H6

International Nuclear Information System (INIS)

Cao Guobin; Song Youqun; Chen Qing; Zhou Qiulan; Cao Yun; Wang Chunhe

2001-01-01

The author introduced a new method of heat-equilibrium low-temperature plasma in ammonia synthesis and a technique of continuous real-time inlet sampling mass-spectrometry to detect the reaction channel and step of the decay of transient component N 2 H 6 into ammonia. The experimental results indicated that in the process of ammonia synthesis by discharge of N 2 and H 2 mixture, the transient component N 2 H 6 is a necessary step

Obtaining low temperature catalysts for methanol synthesis by no-waste process

Energy Technology Data Exchange (ETDEWEB)

Il' ko, E G; Sushchaya, L E; Bondar' , P G

1982-11-01

Low temperature production of catalysts for methanol synthesis involves considerable pollution of the environment as well as formation of side products. The authors propose producing such catalysts from joint precipitates of copper and zinc carbonates includiing stabilizers produced by decomposing solvents, then drying, aging and shaping. This method avoids waste water usually formed in scrubbing to remove ions of alkaline metals. Aluminum hydroxide is suggested as a stabilizer. The catalyst tablets prepared in this way were found to have activity like those produced by other methods, and were suitable for industrial use.

Production of advanced materials by methods of self-propagating high-temperature synthesis

CERN Document Server

Tavadze, Giorgi F

2013-01-01

This translation from the original Russian book outlines the production of a variety of materials by methods of self-propagating high-temperature synthesis (SHS). The types of materials discussed include: hard, refractory, corrosion and wear-resistant materials, as well as other advanced and speciality materials. The authors address the issue of optimal parameters for SHS reactions occurring during processes involving a preliminary metallothermic reduction stage, and they calculate this using thermodynamic approaches. In order to confirm the effectiveness of this approach, the authors describe experiments focussing on the synthesis of elemental crysalline boron, boron carbides and nitrides. Other parts of this brief include theoretical and experimental results on single-stage production of hard alloys on the basis of titanium and zirconium borides, as well as macrokinetics of degassing and compaciton of SHS-products.This brief is suitable for academics, as well as those working in industrial manufacturing com...

Synthesis of monoclinic potassium niobate nanowires that are stable at room temperature.

Science.gov (United States)

Kim, Seungwook; Lee, Ju-Hyuck; Lee, Jaeyeon; Kim, Sang-Woo; Kim, Myung Hwa; Park, Sungnam; Chung, Haegeun; Kim, Yong-Il; Kim, Woong

2013-01-09

We report the synthesis of KNbO(3) nanowires (NWs) with a monoclinic phase, a phase not observed in bulk KNbO(3) materials. The monoclinic NWs can be synthesized via a hydrothermal method using metallic Nb as a precursor. The NWs are metastable, and thermal treatment at ∼450 °C changed the monoclinic phase into the orthorhombic phase, which is the most stable phase of KNbO(3) at room temperature. Furthermore, we fabricated energy-harvesting nanogenerators by vertically aligning the NWs on SrTiO(3) substrates. The monoclinic NWs showed significantly better energy conversion characteristics than orthorhombic NWs. Moreover, the frequency-doubling efficiency of the monoclinic NWs was ∼3 times higher than that of orthorhombic NWs. This work may contribute to the synthesis of materials with new crystalline structures and hence improve the properties of the materials for various applications.

The synthesis of [2-13C]2-nitropropane at room temperature and at atmospheric pressure

NARCIS (Netherlands)

Jacquemijns M; Zomer G

1990-01-01

In this report the synthesis of [2-13C]2-nitropropane at room temperature is described. [2-13C]Acetone was converted into the oxime with hydroxy hydrochloridelamine and sodium carbonate. Treatment with hypobromic acid resulted in 2-13C]2-bromo-2-nitropropane. Hydrogenation with sodium borohydride

Advantage of low-temperature hydrothermal synthesis to grow stoichiometric crednerite crystals

Science.gov (United States)

Poienar, Maria; Martin, Christine; Lebedev, Oleg I.; Maignan, Antoine

2018-06-01

This work reports a new approach for the growth of stoichiometric crednerite CuMnO2 crystals. The hydrothermal reaction, starting from soluble metal sulphates as precursors, is assisted by ethylene glycol and the formation of crednerite is found to depend strongly on pH and temperature. This method allows obtaining small hexagonal platelets with the larger dimension about 1.0-1.5 μm and with a composition characterized by a Cu/Mn ratio of 1. Thus, these crystals differ from the needle-like millimetric ones obtained by the flux technique for which the composition departs from the expected one and is close to Cu1.04Mn0.96. This monitoring of the cationic composition in crednerite, using hydrothermal synthesis, is important as the Cu/Mn ratio controls the low temperature antiferromagnetic ground-state.

In situ probing of temperature in radio frequency thermal plasma using Yttrium ion emission lines during synthesis of yttria nanoparticles

Science.gov (United States)

Dhamale, G. D.; Tiwari, N.; Mathe, V. L.; Bhoraskar, S. V.; Ghorui, S.

2017-07-01

Particle feeding is used in the most important applications of radio frequency (r.f.) thermal plasmas like synthesis of nanoparticles and particle spheroidization. The study reports an in-situ investigation of radial distribution of temperature in such devices using yttrium ion emission lines under different rates of particle loading during synthesis of yttria nanoparticles. A number of interesting facts about the response of r.f. plasma to the rate of particle loading, hitherto unknown, are revealed. Observed phenomena are supported with experimental data from fast photographic experiments and actual synthesis results. The use of the Abel inversion technique together with simultaneous multi-track acquisition of emission spectra from different spatial locations using a CCD based spectrometer allowed us to extract accurate distribution of temperature inside the plasma in the presence of inherent instabilities. The temperature profiles of this type of plasma have been measured possibly for the first time while particles are being fed into the plasma. Observed changes in the temperature profiles as the particle feed rate increases are very significant. Reaction forces resulting from particle evaporation, and increased skin depth owing to the decrease in electrical conductivity in the edge region are proposed as the two different mechanisms to account for the observed changes in the temperature profile as the powder feed rate is increased. Quantitative analyses supporting the proposed mechanisms are presented.

Influence of temperature on the synthesis of calcining cement α--tricalcium phosphate

International Nuclear Information System (INIS)

Vieira, R.S.; Thurmer, M.B.; Coelho, W.T.; Fernandes, J.M.; Santos, L.A.

2011-01-01

The calcium phosphate cement (CFCs) bone substitutes are of great potential use in medical and dental. However, one of the great difficulties of using this type of cement is its low mechanical strength due to the presence of undesirable phases, such as beta-tricalcium phosphate. The step of obtaining this compound is done at high temperature by solid state reaction. With the aim of obtaining calcium phosphate cements more resistant, we studied the conditions for obtaining an alpha-TCP at temperatures of 1300, 1400 and 1500 ° C with time 2h calcination. The samples were analyzed for crystalline phases, density, porosity and mechanical strength. The results show that the synthesis parameters studied strongly influence the obtained phases and the mechanical properties of cement. (author)

Silver nanoparticles: Influence of the temperature synthesis on the particles’ morphology

International Nuclear Information System (INIS)

Piñero, S; Camero, S; Blanco, S

2017-01-01

Silver nanoparticles have a wide range of applications in the medical field, textile and food industries. These and other applications can be found due to the relation between its size and morphology. In this study the influence of bath temperature on the morphology and size of silver nanoparticles are evaluated, which are obtained by chemical reduction of AgNO 3 using three reducing agents: sodium borohydride, ascorbic acid and sodium citrate. The evaluation carried out by the traditional UV-vis Spectrophotometric analysis and with High Resolution Transmission Electron Microscopy. The UV-vis spectrum of the silver colloids obtained by chemical reduction using three different reducing agents shows the effect of the temperature change on the growing and aggregative process. The final effect on the morphology, size and aggregation of the particles was confirmed by TEM. The result suggests a change in the growing mechanism, conducted by aggregation of atoms at 5 and 20°C degrees and aggregation of clusters at higher temperatures. Moreover in this work the main synthesis methods of nanomaterials are described. (paper)

P25-graphene hydrogels: room-temperature synthesis and application for removal of methylene blue from aqueous solution.

Science.gov (United States)

Hou, Chengyi; Zhang, Qinghong; Li, Yaogang; Wang, Hongzhi

2012-02-29

Herein we report a room-temperature synthesis of chemically bonded TiO2 (P25)-graphene composite hydrogels and their use as high performance visible light photocatalysts. The three-dimensional (3D) TiO2-carbon composite exhibits a significant enhancement in the reaction rate in the decontamination of methylene blue, compared to the bare P25. The 3D P25-graphene hydrogel is much easier to prepare and apply as a macroscopic device, compared to the 2D P25-graphene sheets. This work could provide new insights into the room-temperature synthesis of graphene-based materials. As a kind of the novel 3D graphene-based composite, the obtained high performance P25-graphene gel could be widely used in the environmental protection issues. Copyright © 2012. Published by Elsevier B.V.

Novel low temperature synthesis of spinel nano-magnesium chromites from secondary resources

Energy Technology Data Exchange (ETDEWEB)

El-Sheikh, S.M., E-mail: selsheikh2001@gmail.com [Nanostructured Materials Laboratory, Advanced Material Department, Central Metallurgical R and D Institute (CMRDI), P.O. Box 78, Helwan, 11421 Cairo (Egypt); Rabbah, M., E-mail: mahmoud.rabah@ymail.com [Electrochemical and Chemical Treatment Laboratory, Minerals Department, Central Metallurgical R and D Institute (CMRDI), P.O. Box 78, Helwan, 11421 Cairo (Egypt)

2013-09-20

Graphical abstract: FE-SEM micrograph and TEM image of magnesium chromite sample heated at 500 °C. - Highlights: • No study has been reported to prepare spinel magnesium chromite form waste resources. • Novel low synthesis temperature of magnesium chromite. • Selective removal of Ca ions from industrial waste tannery solution is rarely reported. • The method applied is simple and safe. - Abstract: A novel low temperature method for synthesis of nano-crystalline magnesium chromites from the tannery waste solution was investigated. Magnesium and chromium hydroxides gel was co-precipitated at pH 8.5 using ammonia solution. MgCr{sub 2}O{sub 4} was obtained by heating the gel formed at different temperatures 300–500 °C for to 8 h. FT-IR, TG-DTG-DTA, FE-SEM and TEM were used to investigate the produced materials. XRD patterns of the primary oxides revealed the formation of amorphous oxide phase by heating at 300 °C. Heating at 400 °C produces nano-crystallite magnesium chromites partly having the structure MgCrO{sub 4} and mainly MgCr{sub 2}O{sub 4} and traces of Cr{sub 2}O{sub 3}{sup +} 500 °C MgCrO{sub 4} mostly decomposed into MgCr{sub 2}O{sub 4} structure{sub .} After 8 h of heating at 500 °C, Cr{sub 2}O{sub 3} completely disappeared. A high surface area about 42.6 m{sup 2}/g and mesoporous structure was obtained for the produced sample at 500 °C for 8 h. A thermodynamic model has been suggested to explain the findings.

Computer modeling of the process of self-propagating high-temperature synthesis in thin system Ni-Al

International Nuclear Information System (INIS)

Poletayev, G.M.; Starostenkov, M.D.; Denisova, N.F.; Skakov, M.K.

2004-01-01

Full text: The process of synthesis of thermal phases of the system Ni-Al is studied through the method of molecular dynamics. As the object of investigation was chosen two-dimensional crystal, that corresponds to atomic packing laying at the plane of volumetric fcc crystal. Clean Ni was taken as a matrix crystal. A particle of clean Al is packed in the center of matrix block. Beyond the bounds of calculated block crystal packing is repeated with the help of periodical border conditions. The interaction between different pairs of atoms is set by pair potential function of Morse, considering interatomic bonding of the point of the sixth coordinate sphere. The allocation of speeds of atomic function in the system is set through the Boltzmann factor, depending the temperature. When the bicrystal is represented by the ideal atom packing and there are no vacancies , the process of structural adjustment is only observed at the temperature, that is higher than melting point. At that, structural adjustment is observed in circular mechanism of atom allocation, also through the border between phases of clean Ni and Al. As a result, Al particle is transformed, at the border between metals, fields of positional disorder and embryos of intermetallide phases NiAl 2 , Ni 2 Al, Ni 3 Al. The introduction of of free volume through the creation of vacancies significantly lowers the temperature of the beginning of the synthesis process of intermetallide phases. The greatest decrease in temperature to the point of 300 K happens, when the vacancies are located in Ni field of bicrystal, the beginning of the thermo-activation is directly connected with the distance from interphase borders. As the process of thermo-activation continues, vacancies located in Ni matrix right up to seventh neighborhood relatively the border bicrystal. During thermo-activation Al particles enter the field and activate the synthesis process

Low Temperature Synthesis of Li2SiO3: Effect on Its Morphological and Textural Properties

Directory of Open Access Journals (Sweden)

Georgina Mondragón-Gutiérrez

2008-01-01

Full Text Available Synthesis, at low temperature, of Li2SiO3 was investigated using different Li : Si molar ratios and urea, which was used as template. This new synthesis was performed in order to look for different textural and morphological properties than those obtained usually by conventional methods in this kind of ceramics. XRD and SEM analyses showed that Li2SiO3 was obtained pure and with ceramic particle morphology of hollow spheres of 2–6 μm. TEM analysis showed that those spheres were composed by needle-like particles crosslinked among them. This morphology provided a high surface area, probed by N2 adsorption. Therefore, this method of synthesis may be used to obtain other similar ceramics and test them in different applications.

Facile, low temperature synthesis of SnO_2/reduced graphene oxide nanocomposite as anode material for lithium-ion batteries

International Nuclear Information System (INIS)

Hou, Chau-Chung; Brahma, Sanjaya; Weng, Shao-Chieh; Chang, Chia-Chin; Huang, Jow-Lay

2017-01-01

Highlights: • Facile, one-pot, low temperature synthesis of SnO_2-RGO composite. • In-situ reduction of graphene oxide and growth of SnO_2 nanoparticle. • Concentration of reductant during synthesis affects the properties significantly. • SnO_2-RGO composite shows good rate capability and stable capacitance. • Synthesis method is energy efficient and scalable for other metal oxides. - Abstract: We demonstrate a facile, single step, low temperature and energy efficient strategy for the synthesis of SnO_2-reduced graphene oxide (RGO) nanocomposite where the crystallization of SnO_2 nanoparticles and the reduction of graphene oxide takes place simultaneously by an in situ chemical reduction process. The electrochemical property of the SnO_2-RGO composite prepared by using low concentrations of reducing agent shows better Li storage performance, good rate capability (378 mAh g"−"1 at 3200 mA g"−"1) and stable capacitance (522 mAh g"−"1 after 50 cycles). Increasing the reductant concentration lead to crystallization of high concentration of SnO_2 nanoparticle aggregation and degrade the Li ion storage property.

Bright and photostable nitrogen-vacancy fluorescence from unprocessed detonation nanodiamond.

Science.gov (United States)

Reineck, P; Capelli, M; Lau, D W M; Jeske, J; Field, M R; Ohshima, T; Greentree, A D; Gibson, B C

2017-01-05

Bright and photostable fluorescence from nitrogen-vacancy (NV) centers is demonstrated in unprocessed detonation nanodiamond particle aggregates. The optical properties of these particles is analyzed using confocal fluorescence microscopy and spectroscopy, time resolved fluorescence decay measurements, and optically detected magnetic resonance experiments. Two particle populations with distinct optical properties are identified and compared to high-pressure high-temperature (HPHT) fluorescent nanodiamonds. We find that the brightness of one detonation nanodiamond particle population is on the same order as that of highly processed fluorescent 100 nm HPHT nanodiamonds. Our results may open the path to a simple and up-scalable route for the production of fluorescent NV nanodiamonds for use in bioimaging applications.

Graphene synthesis on SiC: Reduced graphitization temperature by C-cluster and Ar-ion implantation

International Nuclear Information System (INIS)

Zhang, R.; Li, H.; Zhang, Z.D.; Wang, Z.S.; Zhou, S.Y.; Wang, Z.; Li, T.C.; Liu, J.R.; Fu, D.J.

2015-01-01

Thermal decomposition of SiC is a promising method for high quality production of wafer-scale graphene layers, when the high decomposition temperature of SiC is substantially reduced. The high decomposition temperature of SiC around 1400 °C is a technical obstacle. In this work, we report on graphene synthesis on 6H–SiC with reduced graphitization temperature via ion implantation. When energetic Ar, C 1 and C 6 -cluster ions implanted into 6H–SiC substrates, some of the Si–C bonds have been broken due to the electronic and nuclear collisions. Owing to the radiation damage induced bond breaking and the implanted C atoms as an additional C source the graphitization temperature was reduced by up to 200 °C

Room-temperature solution synthesis of Ag nanoparticle functionalized molybdenum oxide nanowires and their catalytic applications

International Nuclear Information System (INIS)

Dong Wenjun; Huang Huandi; Zhu Yanjun; Li Xiaoyun; Wang Xuebin; Li Chaorong; Chen Benyong; Wang Ge; Shi Zhan

2012-01-01

A simple chemical solution route for the synthesis of large-scale high-quality Ag nanoparticle functionalized molybdenum oxide nanowire at room temperature has been developed. In the synthesis, the protonated amine was intercalated into the molybdenum bronze layers to reduce the electrostatic force of the lamellar structures, and then the Ag nanoparticle functionalized long nanowires could be easily induced by a redox reaction between a molybdenum oxide–amine intermediate and Ag + at room temperature. The intercalation lamellar structures improved the nucleation and growth of the Ag nanoparticles, with the result that uniform Ag nanoparticles occurred on the surface of the MoO 3 nanowire. In this way Ag nanoparticles with average sizes of around 6 nm, and high-purity nanowires with mean diameter of around 50 nm and with typical lengths of several tens to hundreds of micrometers were produced. The heteronanostructured nanowires were intricately and inseparably connected to each other with hydrogen bonds and/or bridge oxygen atoms and packed together, forming a paper-like porous network film. The Ag–MoO 3 nanowire film performs a promoted catalytic property for the epoxidation of cis-cyclooctene, and the heteronanostructured nanowire film sensor shows excellent sensing performance to hydrogen and oxygen at room temperature. (paper)

Room-temperature solution synthesis of Ag nanoparticle functionalized molybdenum oxide nanowires and their catalytic applications.

Science.gov (United States)

Dong, Wenjun; Huang, Huandi; Zhu, Yanjun; Li, Xiaoyun; Wang, Xuebin; Li, Chaorong; Chen, Benyong; Wang, Ge; Shi, Zhan

2012-10-26

A simple chemical solution route for the synthesis of large-scale high-quality Ag nanoparticle functionalized molybdenum oxide nanowire at room temperature has been developed. In the synthesis, the protonated amine was intercalated into the molybdenum bronze layers to reduce the electrostatic force of the lamellar structures, and then the Ag nanoparticle functionalized long nanowires could be easily induced by a redox reaction between a molybdenum oxide-amine intermediate and Ag(+) at room temperature. The intercalation lamellar structures improved the nucleation and growth of the Ag nanoparticles, with the result that uniform Ag nanoparticles occurred on the surface of the MoO(3) nanowire. In this way Ag nanoparticles with average sizes of around 6 nm, and high-purity nanowires with mean diameter of around 50 nm and with typical lengths of several tens to hundreds of micrometers were produced. The heteronanostructured nanowires were intricately and inseparably connected to each other with hydrogen bonds and/or bridge oxygen atoms and packed together, forming a paper-like porous network film. The Ag-MoO(3) nanowire film performs a promoted catalytic property for the epoxidation of cis-cyclooctene, and the heteronanostructured nanowire film sensor shows excellent sensing performance to hydrogen and oxygen at room temperature.

Mechanical alloying and self-propagating high-temperature synthesis of stable icosahedral quasicrystals

International Nuclear Information System (INIS)

Bokhonov, B.B.

2008-01-01

The phase evolution of the mechanically alloyed ternary 63%Al + 25%Cu + 12%Fe and 65%Al + 20%Cu + 15%Fe powder mixtures with milling time has been studied by X-ray diffraction method. It was found that an icosahedral quasicrystalline phase was formed directly during high-energy ball milling of the Al-Cu-Fe mixtures. The X-ray and scanning electron microscopic investigations demonstrated the possibility to use self-propagating high-temperature synthesis (SHS) in combination with preliminary mechanical activation for the synthesis of stable icosahedral quasicrystals. The typical morphology of the Al 63 Cu 25 Fe 12 icosahedral quasicrystals formed in the SHS process is a pentagonal dodecahedron with a size of 3-5 mm. The phase composition of the SHS products depends on the time of preliminary mechanical activation. The content of cubic intermetallic phase in SHS products increases with the time of preliminary mechanical activation of the 63%Al + 25%Cu + 12%Fe powder mixtures

Facile synthesis of concentrated gold nanoparticles with low size-distribution in water: temperature and pH controls

Directory of Open Access Journals (Sweden)

Li Chunfang

2011-01-01

Full Text Available Abstract The citrate reduction method for the synthesis of gold nanoparticles (GNPs has known advantages but usually provides the products with low nanoparticle concentration and limits its application. Herein, we report a facile method to synthesize GNPs from concentrated chloroauric acid (2.5 mM via adding sodium hydroxide and controlling the temperature. It was found that adding a proper amount of sodium hydroxide can produce uniform concentrated GNPs with low size distribution; otherwise, the largely distributed nanoparticles or instable colloids were obtained. The low reaction temperature is helpful to control the nanoparticle formation rate, and uniform GNPs can be obtained in presence of optimized NaOH concentrations. The pH values of the obtained uniform GNPs were found to be very near to neutral, and the pH influence on the particle size distribution may reveal the different formation mechanism of GNPs at high or low pH condition. Moreover, this modified synthesis method can save more than 90% energy in the heating step. Such environmental-friendly synthesis method for gold nanoparticles may have a great potential in large-scale manufacturing for commercial and industrial demand.

Facile synthesis of concentrated gold nanoparticles with low size-distribution in water: temperature and pH controls

Science.gov (United States)

Li, Chunfang; Li, Dongxiang; Wan, Gangqiang; Xu, Jie; Hou, Wanguo

2011-07-01

The citrate reduction method for the synthesis of gold nanoparticles (GNPs) has known advantages but usually provides the products with low nanoparticle concentration and limits its application. Herein, we report a facile method to synthesize GNPs from concentrated chloroauric acid (2.5 mM) via adding sodium hydroxide and controlling the temperature. It was found that adding a proper amount of sodium hydroxide can produce uniform concentrated GNPs with low size distribution; otherwise, the largely distributed nanoparticles or instable colloids were obtained. The low reaction temperature is helpful to control the nanoparticle formation rate, and uniform GNPs can be obtained in presence of optimized NaOH concentrations. The pH values of the obtained uniform GNPs were found to be very near to neutral, and the pH influence on the particle size distribution may reveal the different formation mechanism of GNPs at high or low pH condition. Moreover, this modified synthesis method can save more than 90% energy in the heating step. Such environmental-friendly synthesis method for gold nanoparticles may have a great potential in large-scale manufacturing for commercial and industrial demand.

Timing matters: the underappreciated role of temperature ramp rate for shape control and reproducibility of quantum dot synthesis

KAUST Repository

Baumgardner, William J.; Quan, Zewei; Fang, Jiye; Hanrath, Tobias

2012-01-01

Understanding the coupled kinetic and thermodynamics factors governing colloidal nanocrystals nucleation and growth are critical factors in the predictable and reproducible synthesis of advanced nanomaterials. We show that the temporal temperature

Synthesis and high (pressure, temperature) stability of ZnTiO3 polymorphs studied by Raman spectroscopy

Science.gov (United States)

Bernert, T.; Ruiz-Fuertes, J.; Bayarjargal, L.; Winkler, B.

2015-05-01

The phase-purity of ilmenite-type ZnTiO3 prepared by the ceramic method was investigated in dependence of the conditions during ball milling. The previously proposed addition of 2 ml ethanol to the starting materials led to a significant contamination of the product phase after a subsequent sintering process at 1073 K. However, by omitting ethanol this synthesis route led to a phase-pure sample of ZnTiO3 as confirmed by X-ray powder diffraction and Raman spectroscopy. High-temperature high-pressure experiments gave an ilmenite-type to perovskite-type phase boundary with a slope of dT/dP∼-135 K GPa-1 crossing ambient temperature conditions at ∼ 24 GPa in good agreement with previous calculations. Room-temperature high-pressure Raman spectroscopy experiments have shown the stability of the ilmenite-type phase up to a pressure of at least 38.5 GPa, the highest pressure applied in this study, indicating the presence of a kinetic barrier in this phase transition. The synthesis of ferroelectric LiNbO3-type ZnTiO3 was confirmed by second harmonic generation.

Low-temperature synthesis of nanocrystalline ZrC coatings on flake graphite by molten salts

Energy Technology Data Exchange (ETDEWEB)

Ding, Jun, E-mail: dingjun@wust.edu.cn; Guo, Ding; Deng, Chengji; Zhu, Hongxi; Yu, Chao

2017-06-15

Highlights: • Uniform ZrC coatings are prepared on flake graphite at 900 °C. • ZrC coatings are composed of nanosized (30–50 nm) particles. • The template growth mechanism is believed to be dominant in the molten salt synthesis process. - Abstract: A novel molten salt synthetic route has been developed to prepare nanocrystalline zirconium carbide (ZrC) coatings on flake graphite at 900 °C, using Zr powder and flake graphite as the source materials in a static argon atmosphere, along with molten salts as the media. The effects of different molten salt media, the sintered temperature, and the heat preservation time on the phase and microstructure of the synthetic materials were investigated. The ZrC coatings formed on the flake graphite were uniform and composed of nanosized particles (30–50 nm). With an increase in the reaction temperature, the ZrC nanosized particles were more denser, and the heat preservation time and thickness of the ZrC coating also increased accordingly. Electron microscopy was used to observe the ZrC coatings on the flake graphite, indicating that a “template mechanism” played an important role during the molten salt synthesis.

Room-temperature Pd-catalyzed C-H chlorination by weak coordination: one-pot synthesis of 2-chlorophenols with excellent regioselectivity.

Science.gov (United States)

Sun, Xiuyun; Sun, Yonghui; Zhang, Chao; Rao, Yu

2014-02-07

A room-temperature Pd(II)-catalyzed regioselective chlorination reaction has been developed for a facile one-pot synthesis of a broad range of 2-chlorophenols. The reaction demonstrates an excellent regioselectivity and reactivity for C-H chlorination. This reaction represents one of the rare examples of mild C-H functionalization at ambient temperature.

Surface-Bound Intermediates in Low-Temperature Methanol Synthesis on Copper. Participants and Spectators

Energy Technology Data Exchange (ETDEWEB)

Yang, Yong; Mei, Donghai; Peden, Charles HF; Campbell, Charles T.; Mims, Charles A.

2015-11-03

The reactivity of surface adsorbed species present on copper catalysts during methanol synthesis at low temperatures was studied by simultaneous infrared spectroscopy (IR) and mass spectroscopy (MS) measurements during “titration” (transient surface reaction) experiments with isotopic tracing. The results show that adsorbed formate is a major bystander species present on the surface under steady-state methanol synthesis reaction conditions, but it cannot be converted to methanol by reaction with pure H₂, nor with H₂ plus added water. Formate-containing surface adlayers for these experiments were produced during steady state catalysis in (a) H₂:CO₂ (with substantial formate coverage) and (b) moist H₂:CO (with no IR visible formate species). Both these reaction conditions produce methanol at steady state with relatively high rates. Adlayers containing formate were also produced by (c) formic acid adsorption. Various "titration" gases were used to probe these adlayers at modest temperatures (T = 410-450K) and 6 bar total pressure. Methanol gas (up to ~1% monolayer equivalent) was produced in "titration" from the H₂:CO₂ catalytic adlayers by H₂ plus water, but not by dry hydrogen. The decay in the formate IR features accelerated in the presence of added water vapor. The H₂:CO:H₂O catalytic adlayer produced similar methanol titration yields in H₂ plus water but showed no surface formate features in IR (less than 0.2% monolayer coverage). Finally, formate from formic acid chemisorption produced no methanol under any titration conditions. Even under (H₂:CO₂) catalytic reaction conditions, isotope tracing showed that pre-adsorbed formate from formic acid did not contribute to the methanol produced. Although non-formate intermediates exist during low temperature methanol synthesis on copper which can be converted to methanol gas

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

Science.gov (United States)

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.

Low-temperature synthesis of allyl dimethylamine by selective heating under microwave irradiation used for water treatment

International Nuclear Information System (INIS)

Tian Binghui; Luan Zhaokun; Li Mingming

2005-01-01

Low-temperature synthesis of allyl dimethylamine (ADA) by selective heating under microwave irradiation (MI) used for water treatment is investigated. The effect of MI, ultrasound irradiation (UI) and conventional heating on yield of ADA, reaction time and the flocculation efficiency of polydiallyl dimethylammunion chloride (PDADMAC) prepared form ADA were studied. The results show that by selective heating at low temperature, MI not only increases yield of ADA and reduces reaction time, but also greatly enhances the flocculation efficiency of PDADMAC

Facile, low temperature synthesis of SnO{sub 2}/reduced graphene oxide nanocomposite as anode material for lithium-ion batteries

Energy Technology Data Exchange (ETDEWEB)

Hou, Chau-Chung; Brahma, Sanjaya; Weng, Shao-Chieh [Department of Materials Science and Engineering, National Cheng Kung University, Tainan 70001, Taiwan, ROC (China); Chang, Chia-Chin [Department of Greenergy, National University of Tainan, Tainan 70005, Taiwan, ROC (China); Huang, Jow-Lay, E-mail: jlh888@mail.ncku.edu.tw [Department of Materials Science and Engineering, National Cheng Kung University, Tainan 70001, Taiwan, ROC (China); Department of Chemical and Materials Engineering, National University of Kaohsiung, Kaohsiung 81148, Taiwan, ROC (China); Center for Micro/Nano Science and Technology, National Cheng Kung University, Tainan 70101, Taiwan, ROC (China)

2017-08-15

Highlights: • Facile, one-pot, low temperature synthesis of SnO{sub 2}-RGO composite. • In-situ reduction of graphene oxide and growth of SnO{sub 2} nanoparticle. • Concentration of reductant during synthesis affects the properties significantly. • SnO{sub 2}-RGO composite shows good rate capability and stable capacitance. • Synthesis method is energy efficient and scalable for other metal oxides. - Abstract: We demonstrate a facile, single step, low temperature and energy efficient strategy for the synthesis of SnO{sub 2}-reduced graphene oxide (RGO) nanocomposite where the crystallization of SnO{sub 2} nanoparticles and the reduction of graphene oxide takes place simultaneously by an in situ chemical reduction process. The electrochemical property of the SnO{sub 2}-RGO composite prepared by using low concentrations of reducing agent shows better Li storage performance, good rate capability (378 mAh g{sup −1} at 3200 mA g{sup −1}) and stable capacitance (522 mAh g{sup −1} after 50 cycles). Increasing the reductant concentration lead to crystallization of high concentration of SnO{sub 2} nanoparticle aggregation and degrade the Li ion storage property.

Synthesis of quinoxaline 1,4-di-n-oxide derivatives on solid support using room temperature and microwave-assisted solvent-free procedures

International Nuclear Information System (INIS)

Gomez-Caro, Lilia C.; Sanchez-Sanchez, Mario; Bocanegra-Garcia, Virgilio; Rivera, Gildardo; Monge, Antonio

2011-01-01

We describe the synthesis of 12 new ethyl and methyl quinoxaline-7-carboxylate 1,4-di-N-oxide derivatives on solid supports with room temperature and microwave-assisted solvent-free procedures. Results show that solid supports have good catalytic activity in the formation of quinoxaline 1,4-di-N-oxide derivatives. We found that florisil and montmorillonite KSF and K10 could be used as new, easily available, inexpensive alternatives of catalysts. Additionally, room temperature and microwave-irradiation solvent-free synthesis was more efficient than a conventional procedure (Beirut reaction), reducing reaction time and increasing yield. (author)

Synthesis of quinoxaline 1,4-di-n-oxide derivatives on solid support using room temperature and microwave-assisted solvent-free procedures

Energy Technology Data Exchange (ETDEWEB)

Gomez-Caro, Lilia C.; Sanchez-Sanchez, Mario; Bocanegra-Garcia, Virgilio; Rivera, Gildardo [Universidad Autonoma de Tamaulipas, Reynosa (Mexico). Dept. de Farmacia y Quimica Medicinal; Monge, Antonio [Universidad de Navarra, Pamplona (Spain). Centro de Investigacion en Farmacobiologia Aplicada. Unidad de Investigacion y Desarrollo de Medicamentos

2011-07-01

We describe the synthesis of 12 new ethyl and methyl quinoxaline-7-carboxylate 1,4-di-N-oxide derivatives on solid supports with room temperature and microwave-assisted solvent-free procedures. Results show that solid supports have good catalytic activity in the formation of quinoxaline 1,4-di-N-oxide derivatives. We found that florisil and montmorillonite KSF and K10 could be used as new, easily available, inexpensive alternatives of catalysts. Additionally, room temperature and microwave-irradiation solvent-free synthesis was more efficient than a conventional procedure (Beirut reaction), reducing reaction time and increasing yield. (author)

Low-temperature direct synthesis of mesoporous vanadium nitrides for electrochemical capacitors

Science.gov (United States)

Lee, Hae-Min; Jeong, Gyoung Hwa; Kim, Sang-Wook; Kim, Chang-Koo

2017-04-01

Mesoporous vanadium nitrides are directly synthesized by a one-step chemical precipitation method at a low temperature (70 °C). Structural and morphological analyses reveal that vanadium nitride consist of long and slender nanowhiskers, and mesopores with diameters of 2-5 nm. Compositional analysis confirms the presence of vanadium in the VN structure, along with oxidized vanadium. The cyclic voltammetry and charge-discharge tests indicate that the obtained material stores charges via a combination of electric double-layer capacitance and pseudocapacitance mechanisms. The vanadium nitride electrode exhibits a specific capacitance of 598 F/g at a current density of 4 A/g. After 5000 charge-discharge cycles, the electrode has an equivalent series resistance of 1.42 Ω and retains 83% of its initial specific capacitance. This direct low-temperature synthesis of mesoporous vanadium nitrides is a simple and promising method to achieve high specific capacitance and low equivalent series resistance for electrochemical capacitor applications.

A rapid room temperature chemical route for the synthesis of graphene: metal-mediated reduction of graphene oxide.

Science.gov (United States)

Dey, Ramendra Sundar; Hajra, Saumen; Sahu, Ranjan K; Raj, C Retna; Panigrahi, M K

2012-02-07

A rapid and facile route for the synthesis of reduced graphene oxide sheets (rGOs) at room temperature by the chemical reduction of graphene oxide using Zn/acid in aqueous solution is demonstrated. This journal is © The Royal Society of Chemistry 2012

BF3.SiO2: an efficient catalyst for the synthesis of azo dyes at room temperature

Directory of Open Access Journals (Sweden)

Bi Bi Fatemeh Mirjalili

2012-07-01

Full Text Available A rapid one-pot method has been developed for the synthesis of azo dyes via ‎sequential diazotization–diazo coupling of aromatic amines with coupling agents at room ‎temperature in the presence of BF3.SiO2 as acidic catalyst. The obtained aryl diazonium salts bearing silica supported boron tri-flouride counter ion‎ was sufficiently stable to be kept at room ‎temperature in the dry state.‎

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

Science.gov (United States)

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.

Low temperature synthesis of Ba1–xSrxSnO3 (x = 0–1) from molten ...

Indian Academy of Sciences (India)

Administrator

first time by molten salt synthesis (MSS) method using KOH as the flux at lower temperature (400°C) compared to other ... chemical methods have been adopted by many research- ers. .... financial support and Technology Business Incubator,.

The synthesis of [2-13C]2-nitropropane at room temperature and at atmospheric pressure

OpenAIRE

Jacquemijns M; Zomer G

1990-01-01

In this report the synthesis of [2-13C]2-nitropropane at room temperature is described. [2-13C]Acetone was converted into the oxime with hydroxy hydrochloridelamine and sodium carbonate. Treatment with hypobromic acid resulted in 2-13C]2-bromo-2-nitropropane. Hydrogenation with sodium borohydride gave [2-13C]2-nitropropane in 14,3% overall yield.

Low-temperature hydrothermal synthesis of ZnO nanorods: Effects of zinc salt concentration, various solvents and alkaline mineralizers

Energy Technology Data Exchange (ETDEWEB)

Edalati, Khatereh, E-mail: kh_ed834@stu.um.ac.ir [Department of Metallurgical Engineering, Faculty of Engineering, Ferdowsi University of Mashhad (FUM) Campus, Azadi Sq., Mashhad, Khorasan Razavi (Iran, Islamic Republic of); Shakiba, Atefeh [Department of Material Science and Metallurgy, Amirkabir University of Technology, Tehran (Iran, Islamic Republic of); Vahdati-Khaki, Jalil; Zebarjad, Seyed Mojtaba [Department of Metallurgical Engineering, Faculty of Engineering, Ferdowsi University of Mashhad (FUM) Campus, Azadi Sq., Mashhad, Khorasan Razavi (Iran, Islamic Republic of)

2016-02-15

Highlights: • We synthesized ZnO nanorods by a simple hydrothermal process at 60 °C. • Effects of zinc salt concentration, solvent and alkaline mineralizer was studied. • Increasing concentration of zinc salt changed ZnO nucleation system. • NaOH yielded better results in the production of nanorods in both solvents. • Methanol performed better in the formation of nanorods using the two mineralizers. - Abstract: ZnO has been produced using various methods in the solid, gaseous, and liquid states, and the hydrothermal synthesis at low temperatures has been shown to be an environmentally-friendly one. The current work utilizes a low reaction temperature (60 °C) for the simple hydrothermal synthesis of ZnO nanorod morphologies. Furthermore, the effects of zinc salt concentration, solvent type and alkaline mineralizer type on ZnO nanorods synthesis at a low reaction temperature by hydrothermal processing was studied. Obtained samples were analyzed using X-ray powder diffraction (XRD) and scanning electron microscopy (SEM). Increasing the concentration of the starting zinc salt from 0.02 to 0.2 M changed ZnO nucleation system from the homogeneous to the heterogeneous state. The XRD results confirmed the production hexagonal ZnO nanostructures of with a crystallite size of 40.4 nm. Varying the experimental parameters (mineralizer and solvent) yielded ZnO nanorods with diameters ranging from 90–250 nm and lengths of 1–2 μm.

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

Science.gov (United States)

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.

Changes in the pattern of protein synthesis of prosopis chilensis induced by high temperatures

Energy Technology Data Exchange (ETDEWEB)

Medina, C.; Cardemil, L. (Univ. de Chile, Santiago (USA))

1989-04-01

Seeds of Prosopis chilensis, a leguminous tree from semi-arid regions of Central Chile, were germinated at temperatures of 25-30-35-40-45 and 50{degree}C. Germination was 100% between 25 and 40{degree}C, being faster at 35{degree}C. The best temperature for root growth was also 35{degree}C. There was not germination at 50{degree}C. However, seedlings coming from seeds germinated at 35{degree}C were capable of growing at higher temperatures of 45 and 50{degree}C. Pattern of protein synthesis was followed in roots incubated with {sup 35}S-methionine at increasing temperatures between 35 and 50{degree}C. SDS-PAGE of the proteins followed by fluorography shows that at temperatures above 35{degree}C, new protein bands appear while others become thicker. Most of the protein bands have decreased at 50{degree}C, with the exception of the new bands. A band of 70 KD, that is present at 35{degree}C, is more prominent at 50{degree}C. These proteins may have an important role in the thermotolerance of Prosopis chilensis to stressing temperatures.

Changes in the pattern of protein synthesis of prosopis chilensis induced by high temperatures

International Nuclear Information System (INIS)

Medina, C.; Cardemil, L.

1989-01-01

Seeds of Prosopis chilensis, a leguminous tree from semi-arid regions of Central Chile, were germinated at temperatures of 25-30-35-40-45 and 50 degree C. Germination was 100% between 25 and 40 degree C, being faster at 35 degree C. The best temperature for root growth was also 35 degree C. There was not germination at 50 degree C. However, seedlings coming from seeds germinated at 35 degree C were capable of growing at higher temperatures of 45 and 50 degree C. Pattern of protein synthesis was followed in roots incubated with 35 S-methionine at increasing temperatures between 35 and 50 degree C. SDS-PAGE of the proteins followed by fluorography shows that at temperatures above 35 degree C, new protein bands appear while others become thicker. Most of the protein bands have decreased at 50 degree C, with the exception of the new bands. A band of 70 KD, that is present at 35 degree C, is more prominent at 50 degree C. These proteins may have an important role in the thermotolerance of Prosopis chilensis to stressing temperatures

Plasma-assisted synthesis of MoS2

Science.gov (United States)

Campbell, Philip M.; Perini, Christopher J.; Chiu, Johannes; Gupta, Atul; Ray, Hunter S.; Chen, Hang; Wenzel, Kevin; Snyder, Eric; Wagner, Brent K.; Ready, Jud; Vogel, Eric M.

2018-03-01

There has been significant interest in transition metal dichalcogenides (TMDs), including MoS2, in recent years due to their potential application in novel electronic and optical devices. While synthesis methods have been developed for large-area films of MoS2, many of these techniques require synthesis temperatures of 800 °C or higher. As a result of the thermal budget, direct synthesis requiring high temperatures is incompatible with many integrated circuit processes as well as flexible substrates. This work explores several methods of plasma-assisted synthesis of MoS2 as a way to lower the synthesis temperature. The first approach used is conversion of a naturally oxidized molybdenum thin film to MoS2 using H2S plasma. Conversion is demonstrated at temperatures as low as 400 °C, and the conversion is enabled by hydrogen radicals which reduce the oxidized molybdenum films. The second method is a vapor phase reaction incorporating thermally evaporated MoO3 exposed to a direct H2S plasma, similar to chemical vapor deposition (CVD) synthesis of MoS2. Synthesis at 400 °C results in formation of super-stoichiometric MoS2 in a beam-interrupted growth process. A final growth method relies on a cyclical process in which a small amount of Mo is sputtered onto the substrate and is subsequently sulfurized in a H2S plasma. Similar results could be realized using an atomic layer deposition (ALD) process to deposit the Mo film. Compared to high temperature synthesis methods, the lower temperature samples are lower quality, potentially due to poor crystallinity or higher defect density in the films. Temperature-dependent conductivity measurements are consistent with hopping conduction in the plasma-assisted synthetic MoS2, suggesting a high degree of disorder in the low-temperature films. Optimization of the plasma-assisted synthesis process for slower growth rate and better stoichiometry is expected to lead to high quality films at low growth temperature.

Synthesis of manganese spinel nanoparticles at room temperature by coprecipitation

Energy Technology Data Exchange (ETDEWEB)

Giovannelli, F., E-mail: fabien.giovannelli@univ-tours.fr [GREMAN, UMR 7347 CNRS-CEA, Universite Francois Rabelais, 15 rue de la chocolaterie, 41000 BLOIS (France); Autret-Lambert, C.; Mathieu, C.; Chartier, T.; Delorme, F. [GREMAN, UMR 7347 CNRS-CEA, Universite Francois Rabelais, 15 rue de la chocolaterie, 41000 BLOIS (France); Seron, A [BRGM, 3 Avenue Claude Guillemin, BP 36009, 45060 ORLEANS Cedex 2 (France)

2012-08-15

This paper is focused on a new route to synthesize Mn{sub 3}O{sub 4} nanoparticles by alkalisation by sodium hydroxide on a manganeous solution at room temperature. The precipitates obtained at different pH values have been characterized by XRD and TEM. Since the first addition of sodium hydroxide, a white Mn(OH){sub 2} precipitate appears. At pH=7, {gamma}-MnOOH phase is predominant with needle like shaped particles. At pH=10, hausmanite nanoparticles, which exhibits well defined cubic shape in the range 50-120 nm are obtained. This new precipitation route is a fast and easy environmentally friendly process to obtain well crystallized hausmanite nanoparticles. - Graphical abstract: TEM image showing Mn{sub 3}O{sub 4} particles after a precipitation at pH=10. Highlights: Black-Right-Pointing-Pointer A new route to synthesize Mn{sub 3}O{sub 4} nanoparticles has been demonstrated. Black-Right-Pointing-Pointer Synthesis has been performed by precipitation at room temperature. Black-Right-Pointing-Pointer The size of the Mn{sub 3}O{sub 4} nanoparticles is between 50 and 120 nm.

Droplet-fused microreactors for room temperature synthesis of nanoscale needle-like hydroxyapatite

International Nuclear Information System (INIS)

Liu Kaiying; Qin Jianhua

2013-01-01

A microfluidic device using droplet-fused microreactors is introduced for room temperature synthesis of nanoscale needle-shaped hydroxyapatite (HAp, Ca 10 (PO 4 ) 6 (OH) 2 ). The device is integrated with multifunctional units, e.g., T-junctions for droplet generation and fusion, winding channels for rapid mixing, and a delay line for simple visualization of the HAp formation process. The necessary conditions such as surfactant and fluid flow rate for an aqueous stream to merge with water-in-oil droplets are investigated. The nanoscale morphologies of the HAp produced by this method are also compared with HAp prepared by conventional bulk mixing. This paper shows that further reaction could be initiated by flowing additional reagent streams directly into the droplets of the initial reaction mixture, which is a novel approach for synthesizing a needle-like morphology of the HAp with a high aspect ratio under room temperature. (paper)

Low-temperature direct synthesis of mesoporous vanadium nitrides for electrochemical capacitors

Energy Technology Data Exchange (ETDEWEB)

Lee, Hae-Min [Institute of NT-IT Fusion Technology, Ajou University, 206 Worldcup-ro, Yeongtong-gu, Suwon 16499 (Korea, Republic of); Jeong, Gyoung Hwa [Department of Chemistry, Ulsan National Institute of Science and Technology (UNIST), Banyeon 100, Ulsan 44919 (Korea, Republic of); Kim, Sang-Wook [Department of Molecular Science and Technology, Ajou University, 206 Worldcup-ro, Yeongtong-gu, Suwon 16499 (Korea, Republic of); Kim, Chang-Koo, E-mail: changkoo@ajou.ac.kr [Department of Chemical Engineering and Department of Energy Systems Research, Ajou University, 206 Worldcup-ro, Yeongtong-gu, Suwon 16499 (Korea, Republic of)

2017-04-01

Highlights: • Vanadium nitrides were directly synthesized by a one-step chemical precipitation method. • This method was carried out at a low temperature of 70 °C. • Vanadium nitrides had a specific capacitance of 598 F/g. • The equivalent series resistance of the vanadium nitride electrode was 1.42 Ω after 5000 cycles. - Abstract: Mesoporous vanadium nitrides are directly synthesized by a one-step chemical precipitation method at a low temperature (70 °C). Structural and morphological analyses reveal that vanadium nitride consist of long and slender nanowhiskers, and mesopores with diameters of 2–5 nm. Compositional analysis confirms the presence of vanadium in the VN structure, along with oxidized vanadium. The cyclic voltammetry and charge-discharge tests indicate that the obtained material stores charges via a combination of electric double-layer capacitance and pseudocapacitance mechanisms. The vanadium nitride electrode exhibits a specific capacitance of 598 F/g at a current density of 4 A/g. After 5000 charge-discharge cycles, the electrode has an equivalent series resistance of 1.42 Ω and retains 83% of its initial specific capacitance. This direct low-temperature synthesis of mesoporous vanadium nitrides is a simple and promising method to achieve high specific capacitance and low equivalent series resistance for electrochemical capacitor applications.

Effect of temperature on the synthesis of silver nanoparticles with polyethylene glycol: new insights into the reduction mechanism

Energy Technology Data Exchange (ETDEWEB)

Fleitas-Salazar, Noralvis; Silva-Campa, Erika; Pedroso-Santana, Seidy; Tanori, Judith; Pedroza-Montero, Martín R.; Riera, Raúl, E-mail: rriera@cifus.uson.mx [Universidad de Sonora (Mexico)

2017-03-15

Polyethylene glycol (PEG) molecules act as a reducing and stabilizing agent in the formation of silver nanoparticles. PEG undergoes thermal oxidative degradation at temperatures over 70 °C in the presence of oxygen. Here, we studied how the temperature and an oxidizing atmosphere could affect the synthesis of silver nanoparticles with PEG. We tested different AgNO{sub 3} concentrations for nanoparticles syntheses using PEG of low molecular weight, at 60 and 100 °C. At the higher temperature, the reducing action of PEG increased and the effect of PEG/Ag{sup +} ratio on nanoparticles aggregation changed. These results suggest that different synthesis mechanisms operate at 60 and 100 °C. Thus, at 60 °C the reduction of silver ions can occur through the oxidation of the hydroxyl groups of PEG, as has been previously reported. We propose that the thermal oxidative degradation of PEG at 100 °C increases the number of both, functional groups and molecules that can reduce silver ions and stabilize silver nanoparticles. This degradation process could explain the enhancement of PEG reducing action observed by other authors when they increase the reaction temperature or use a PEG of higher molecular weight.

Ab Initio Guided Low Temperature Synthesis Strategy for Smooth Face–Centred Cubic FeMn Thin Films

Directory of Open Access Journals (Sweden)

Friederike Herrig

2018-05-01

Full Text Available The sputter deposition of FeMn thin films with thicknesses in the range of hundred nanometres and beyond requires relatively high growth temperatures for the formation of the face-centred cubic (fcc phase, which results in high thin film roughness. A low temperature synthesis strategy, based on local epitaxial growth of a 100 nm thick fcc FeMn film as well as a Cu nucleation layer on an α-Al2O3 substrate at 160 °C, enables roughness values (Ra as low as ~0.6 nm, which is in the same order of magnitude as the pristine substrate (~0.1 nm. The synthesis strategy is guided by ab initio calculations, indicating very strong interfacial bonding of the Cu nucleation layer to an α-Al2O3 substrate (work of separation 5.48 J/m²—which can be understood based on the high Cu coordination at the interface—and between fcc FeMn and Cu (3.45 J/m². Accompanied by small lattice misfits between these structures, the strong interfacial bonding is proposed to enable the local epitaxial growth of a smooth fcc FeMn thin film. Based on the here introduced synthesis strategy, the implementation of fcc FeMn based thin film model systems for materials with interface dominated properties such as FeMn steels containing κ-carbide precipitates or secondary phases appears meaningful.

Direct synthesis of multi-layer graphene film on various substrates by microwave plasma at low temperature

Energy Technology Data Exchange (ETDEWEB)

Park, Hyun Jae [Plasma Technology Research Center, 814-2 Osickdo-dong (SGFEZ), Gunsan, Jeollabuk-do 573-540 (Korea, Republic of); Ahn, Byung Wook; Kim, Tae Yoo; Lee, Jung Woo [School of Advanced Materials Science and Engineering, Advanced Materials and Process Research Center (AMPRC), Sungkyunkwan University, Suwon 440-746 (Korea, Republic of); Jung, Yong Ho; Choi, Yong Sup [Plasma Technology Research Center, 814-2 Osickdo-dong (SGFEZ), Gunsan, Jeollabuk-do 573-540 (Korea, Republic of); Song, Young Il, E-mail: physein01@skku.edu [School of Advanced Materials Science and Engineering, Advanced Materials and Process Research Center (AMPRC), Sungkyunkwan University, Suwon 440-746 (Korea, Republic of); Suh, Su Jeong, E-mail: suhsj@skku.edu [School of Advanced Materials Science and Engineering, Advanced Materials and Process Research Center (AMPRC), Sungkyunkwan University, Suwon 440-746 (Korea, Republic of)

2015-07-31

We introduce a possible route for vertically standing multi-layer graphene films (VMGs) on various substrates at low temperature by electron cyclone resonance microwave plasma. VMG films on various substrates, including copper sheet, glass and silicon oxide wafer, were analyzed by studying their structural, electrical, and optical properties. The density and temperature of plasma were measured using Cylindrical Langmuir probe analysis. The morphologies and microstructures of multi-layer graphene were characterized using field emission scattering electron microscope, high resolution transmission electron microscope, and Raman spectra measurement. The VMGs on different substrates at the same experimental conditions synthesized the wrinkled VMGs with different heights. In addition, the transmittance and electrical resistance were measured using ultra-violet visible near-infrared spectroscopy and 4 probe point surface resistance measurement. The VMGs on glass substrate obtained a transmittance of 68.8% and sheet resistance of 796 Ω/square, whereas the VMGs on SiO{sub 2} wafer substrate showed good sheet resistance of 395 Ω/square and 278 Ω/square. The results presented herein demonstrate a simple method of synthesizing of VMGs on various substrates at low temperature for mass production, in which the VMGs can be used in a wide range of application fields for energy storage, catalysis, and field emission due to their unique orientation. - Highlights: • We present for synthesis method of graphene at low temperature on various substrates. • We grow the graphene films at low temperature under of 432 °C. • Structural information of graphene films were studied upon Raman spectroscopy. • Inter-layer spacing of vertically standing graphene relies on synthesis time. • We measured a transmittance and a resistance for graphene films on difference substrate.

Design approach to sealant selection for the life of the well

NARCIS (Netherlands)

Bosma, M.; Ravi, K.; Driel, W.D. van; Schreppers, G.M.A.

1999-01-01

Recent experience in the field has demonstrated that the mechanical properties of the annular sealant are a critical factor in the success of a well. A demanding operational regime of the well such as High Pressure/High Temperature (HP/HT) and well interventions, e.g. pressure testing stimulation,

A new practical approach towards the synthesis of unsymmetric and symmetric 1,10-phenanthroline derivatives at room temperature.

Science.gov (United States)

Cheng, Yongfeng; Han, Xuesong; Ouyang, Huangche; Rao, Yu

2012-03-18

An efficient method towards synthesis of 1,10-phenanthrolines is described. Through Lewis acid-catalyzed annulation reaction between 3-ethoxycyclobutanones and 8-aminoquinolines, a variety of unsymmetric and symmetric 1,10-phenanthroline derivatives were readily prepared with high regioselectivity at room temperature.

Low Temperature Solid-State Synthesis and Characterization of LaBO3

Directory of Open Access Journals (Sweden)

Azmi Seyhun KIPÇAK

2016-11-01

Full Text Available Rare earth (lanthanide series borates, possess high vacuum ultraviolet (VUV transparency, large electronic band gaps, chemical and environmental stability and exceptionally large optical damage thresholds and used in the development of plasma display panels (PDPs. In this study the synthesis of lanthanum borates via solid-state method is studied. For this purpose, lanthanum oxide (La2O3 and boric acid (H3BO3 are used for as lanthanum and boron sources, respectively. Different elemental molar ratios of La to B (between 3:1 to 1:6 as La2O3:H3BO3 were reacted by solid-state method at the reaction temperatures between 500°C - 700°C with the constant reaction time of 4 h. Following the synthesis, characterizations of the synthesized products are conducted by X-ray diffraction (XRD, Fourier transform infrared spectroscopy (FT-IR, Raman spectroscopy and scanning electron microscope (SEM. From the results of the experiments, three types of lanthanum borates of; La3BO6, LaBO3 and La(BO23 were observed at different reaction parameters. Among these three types of lanthanum borates LaBO3 phase were obtained as a major phase.

High-pressure synthesis and characterizations of the R2Pt2O7 pyrochlores.

Science.gov (United States)

Cai, Yunqi; Cui, Qi; Cheng, Jinguang; Dun, Zhiling; Zhou, Haidong; Ma, Jie; Cruz, C. Dela; Yan, Jiaqiang; Li, Xiang; Zhou, Jianshi

Pyrochlore R2B2O7 where R3 + stands for rear-earth ion and B4 + for a nonmagnetic cation such as Sn4 +or Ti4 +consist of an important family of geometrically frustrated magnets, which have been the focus of extensive investigations over last decades. To further enlarge the R2B2O7, we have chosen to stabilize the Pt-based cubic pyrochlores under HPHT conditions for two reasons: (1) Pt4 + is in a low-spin state which ionic radius is located in between Ti4 + (0.605\\x85) and Sn4 + (0.69\\x85), and (2) Pt4 + has a spatially much more extended 5d orbitals and thus enhanced Pt 5d-O 2p hybridizations that might modify the local anisotropic exchange interactions. Such an effect has never been taken into account in the previous studies. In this work, we will present the detailed characterizations on the pyrochlores R2Pt2O7 obtained under HPHT conditions. This work is supported by the National Science Foundation of China (Grant Nos.11304371, 11574377), part of the work was supported by the CEM, and NSF MRSEC, under Grant DMR-1420451, and Grant No. NSF-DMR-1350002.

Effects of electromagnetic radiation (bright light, extremely low-frequency magnetic fields, infrared radiation) on the circadian rhythm of melatonin synthesis, rectal temperature, and heart rate.

Science.gov (United States)

Griefahn, Barbara; Künemund, Christa; Blaszkewicz, Meinolf; Lerchl, Alexander; Degen, Gisela H

2002-10-01

Electromagnetic spectra reduce melatonin production and delay the nadirs of rectal temperature and heart rate. Seven healthy men (16-22 yrs) completed 4 permuted sessions. The control session consisted of a 24-hours bedrest at infrared radiation (65 degrees C) was applied from 5 pm to 1 am. Salivary melatonin level was determined hourly, rectal temperature and heart rate were continuously recorded. Melatonin synthesis was completely suppressed by light but resumed thereafter. The nadirs of rectal temperature and heart rate were delayed. The magnetic field had no effect. Infrared radiation elevated rectal temperature and heart rate. Only bright light affected the circadian rhythms of melatonin synthesis, rectal temperature, and heart rate, however, differently thus causing a dissociation, which might enhance the adverse effects of shiftwork in the long run.

Environmentally friendly room temperature strecker reaction:one-pot synthesis of α-aminonitriles in ionic liquid

International Nuclear Information System (INIS)

Mojtahedi, M. M.; Abaee, M.S.; Abbasi, H.

2006-01-01

A three component efficient and facile procedure is developed for the synthesis of a-aminonitriles from aromatic-and aliphatic aldehydes, amines, and trimethylsilyl cyanide in 1-butyl-3-methyl-1H-imidazolium perchlorate ([bmim][C1O 4 ]) ionic liquid as the reaction medium at room temperature. Excellent yields are obtained in this one-pot procedure with short reaction times and the ionic liquid medium reused several times in a row

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

Science.gov (United States)

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

2014-01-01

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

The Role of Solvent Polarity on Low-Temperature Methanol Synthesis Catalyzed by Cu Nanoparticles

Energy Technology Data Exchange (ETDEWEB)

Ahoba-Sam, Christian [Department of Process, Energy and Environmental Technology, University College of Southeast Norway, Porsgrunn (Norway); Olsbye, Unni [Department of Chemistry, University of Oslo, Oslo (Norway); Jens, Klaus-Joachim, E-mail: Klaus.J.Jens@usn.no [Department of Process, Energy and Environmental Technology, University College of Southeast Norway, Porsgrunn (Norway)

2017-07-14

Methanol syntheses at low temperature in a liquid medium present an opportunity for full syngas conversion per pass. The aim of this work was to study the role of solvents polarity on low-temperature methanol synthesis reaction using eight different aprotic polar solvents. A “once through” catalytic system, which is composed of Cu nanoparticles and sodium methoxide, was used for methanol synthesis at 100°C and 20 bar syngas pressure. Solvent polarity rather than the 7–10 nm Cu (and 30 nm Cu on SiO{sub 2}) catalyst used dictated trend of syngas conversion. Diglyme with a dielectric constant (ε) = 7.2 gave the highest syngas conversion among the eight different solvents used. Methanol formation decreased with either increasing or decreasing solvent ε value of diglyme (ε = 7.2). To probe the observed trend, possible side reactions of methyl formate (MF), the main intermediate in the process, were studied. MF was observed to undergo two main reactions; (i) decarbonylation to form CO and MeOH and (ii) a nucleophilic substitution to form dimethyl ether and sodium formate. Decreasing polarity favored the decarbonylation side reaction while increasing polarity favored the nucleophilic substitution reaction. In conclusion, our results show that moderate polarity solvents, e.g., diglyme, favor MF hydrogenolysis and, hence, methanol formation, by retarding the other two possible side reactions.

Synthesis and regulation of α-LiZnPO4.H2O via a solid-state reaction at low-heating temperatures

International Nuclear Information System (INIS)

Liao Sen; Chen Zhipeng; Tian Xiaozhen; Wu Wenwei

2009-01-01

A simple and novel route for the synthesis of a lithium zinc phosphate hydrate, α-LiZnPO 4 .H 2 O, was studied, and the target product was obtained with LiH 2 PO 4 .H 2 O and ZnCO 3 as raw materials and polyethylene glycol-400 (PEG-400) as a surfactant via a one step solid-state reaction at room temperature (25 deg. C). The product was characterized with X-ray powder diffraction (XRD), thermogravimetric analysis and the 1st derivativative of thermogravimetric analysis (TG/DTG) and Fourier transform infrared spectroscopy (FTIR). The comparison experimental results suggested that aging temperature controlled the products of the synthesis, that is, the α-LiZnPO 4 .H 2 O was formed when the reaction mixture was aged at room temperature, and the α-LiZnPO 4 was obtained when the reaction mixture was aged at 80 deg. C.

Facile synthesis of improved room temperature gas sensing properties of TiO2 nanostructures: Effect of acid treatment

CSIR Research Space (South Africa)

Tshabalala, Zamaswazi P

2016-03-01

Full Text Available and Actuators B: Chemical Facile synthesis of improved room temperature gas sensing properties of TiO2 nanostructures: Effect of acid treatment Z.P. Tshabalalaa,b, D.E. Motaunga,∗, G.H. Mhlongoa,∗, O.M. Ntwaeaborwab,∗ a DST/CSIR, National Centre...

Zero bias thermally stimulated currents in synthetic diamond

Science.gov (United States)

Mori, R.; Miglio, S.; Bruzzi, M.; Bogani, F.; De Sio, A.; Pace, E.

2009-06-01

Zero bias thermally stimulated currents (ZBTSCs) have been observed in single crystal high pressure high temperature (HPHT) and polycrystalline chemical vapor deposited (pCVD) diamond films. The ZBTSC technique is characterized by an increased sensitivity with respect to a standard TSC analysis. Due to the absence of the thermally activated background current, new TSC peaks have been observed in both HPHT and pCVD diamond films, related to shallow activation energies usually obscured by the emission of the dominant impurities. The ZBTSC peaks are explained in terms of defect discharge in the nonequilibrium potential distribution created by a nonuniform traps filling at the metal-diamond junctions. The electric field due to the charged defects has been estimated in a quasizero bias TSC experiment by applying an external bias.

Room temperature chemical synthesis of lead selenide thin films with preferred orientation

Science.gov (United States)

Kale, R. B.; Sartale, S. D.; Ganesan, V.; Lokhande, C. D.; Lin, Yi-Feng; Lu, Shih-Yuan

2006-11-01

Room temperature chemical synthesis of PbSe thin films was carried out from aqueous ammoniacal solution using Pb(CH3COO)2 as Pb2+ and Na2SeSO3 as Se2- ion sources. The films were characterized by a various techniques including, X-ray diffraction (XRD), energy dispersive X-ray analysis (EDAX), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HR-TEM), selected area electron diffraction (SAED), Fast Fourier transform (FFT) and UV-vis-NIR techniques. The study revealed that the PbSe thin film consists of preferentially oriented nanocubes with energy band gap of 0.5 eV.

Room temperature chemical synthesis of lead selenide thin films with preferred orientation

International Nuclear Information System (INIS)

Kale, R.B.; Sartale, S.D.; Ganesan, V.; Lokhande, C.D.; Lin, Y.-F.; Lu, S.-Y.

2006-01-01

Room temperature chemical synthesis of PbSe thin films was carried out from aqueous ammoniacal solution using Pb(CH 3 COO) 2 as Pb 2+ and Na 2 SeSO 3 as Se 2- ion sources. The films were characterized by a various techniques including, X-ray diffraction (XRD), energy dispersive X-ray analysis (EDAX), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HR-TEM), selected area electron diffraction (SAED), Fast Fourier transform (FFT) and UV-vis-NIR techniques. The study revealed that the PbSe thin film consists of preferentially oriented nanocubes with energy band gap of 0.5 eV

Synthesis and characterization of Cu-MFI catalyst for the direct medium temperature range NO decomposition

Directory of Open Access Journals (Sweden)

Valkaj Karolina Maduna

2016-03-01

Full Text Available In this study the physico-chemical and catalytic properties of copper bearing MFI zeolites (Cu-MFI with different Si/Al and Si/Cu ratios were investigated. Two different methods for incorporation of metal ions into the zeolite framework were used: the ion exchange from the solution of copper acetate and the direct hydrothermal synthesis. Direct synthesis of a zeolite in the presence of copper-phosphate complexes was expected to generate more active copper species necessary for the desired reaction than the conventional ion exchange method. Direct decomposition of NO was used as a model reaction, because this reaction still offers a very attractive approach to NOX removal. The catalytic properties of zeolite samples were studied using techniques, such as XRD, SEM, EPR and nitrogen adsorption/desorption measurements at 77 K. Results of the kinetic investigation revealed that both methods are applicable for the preparation of the catalysts with active sites capable of catalyzing the NO decomposition. It was found out that Cu-MFI zeolites obtained through direct synthesis are promising catalysts for NO decomposition, especially at lower reaction temperatures. The efficiency of the catalysts prepared by both methods is compared and discussed.

Self-propagating high-temperature synthesis of TiC-WC composite materials

International Nuclear Information System (INIS)

Mas-Guindal, M.J.; Contreras, L.; Turrillas, X.; Vaughan, G.B.M.; Kvick, A.; Rodriguez, M.A.

2006-01-01

TiC-WC composites have been obtained in situ by self-propagating high-temperature synthesis (SHS) from a mixture of compacted powders of elemental titanium, tungsten and graphite. The Rietveld method has proved to be a useful tool to quantify the different phases in the reaction and calculate the cell parameters of the solid solution found in the products. The reaction has also been followed in real time by X-ray diffraction at the European Synchrotron Radiation Facility (ESRF ID-11 Materials Science Beamline). The mechanism of the reaction is discussed in terms of the diffusion of liquid titanium to yield titanium carbide with a solid solution of tungsten. The microstructures of the materials obtained by this method are presented

Room temperature chemical synthesis of highly oriented PbSe nanotubes based on negative free energy of formation

Energy Technology Data Exchange (ETDEWEB)

Sankapal, B.R., E-mail: brsankapal@rediffmail.com [Thin Film and Nano Science Laboratory, Department of Physics, School of Physical Sciences, North Maharashtra University, Jalgaon 425 001 (MS) (India); Ladhe, R.D.; Salunkhe, D.B.; Baviskar, P.K. [Thin Film and Nano Science Laboratory, Department of Physics, School of Physical Sciences, North Maharashtra University, Jalgaon 425 001 (MS) (India); Gupta, V.; Chand, S. [Organic and Hybrid Solar Cell, Physics of Energy Harvesting Division, Dr. K.S. Krishnan Marg, National Physical Laboratory, New Delhi 110012 (India)

2011-10-13

Highlights: > Simple, inexpensive and room temperature chemical synthesis route. > Highly oriented PbSe nanotubes from Cd(OH){sub 2} nanowires through lead hydroxination. > The process was template free without the use of any capping agent. > Reaction kinetics was accomplished due to more negative free energy of formation. > The ion exchange mechanism due to difference in the solubility products. - Abstract: The sacrificial template free chemical synthesis of PbSe nanotubes at room temperature has been performed by lead hydroxination from cadmium hydroxide nanowires. This process was based on the ion exchange reaction to replace Cd{sup 2+} with Pb{sup 2+} ions from hydroxyl group followed by replacement of hydroxyl group with selenium ions. The reaction kinetics was accomplished due to more negative free energy of formation and thus the difference in the solubility products. The formed nanotubes were inclusive of Pb and Se with proper inter-chemical bonds with preferred orientations having diameter in tens of nanometer. These nanotubes can have future applications in electronic, optoelectronics and photovoltaic's as well.

Room temperature chemical synthesis of highly oriented PbSe nanotubes based on negative free energy of formation

International Nuclear Information System (INIS)

Sankapal, B.R.; Ladhe, R.D.; Salunkhe, D.B.; Baviskar, P.K.; Gupta, V.; Chand, S.

2011-01-01

Highlights: → Simple, inexpensive and room temperature chemical synthesis route. → Highly oriented PbSe nanotubes from Cd(OH) 2 nanowires through lead hydroxination. → The process was template free without the use of any capping agent. → Reaction kinetics was accomplished due to more negative free energy of formation. → The ion exchange mechanism due to difference in the solubility products. - Abstract: The sacrificial template free chemical synthesis of PbSe nanotubes at room temperature has been performed by lead hydroxination from cadmium hydroxide nanowires. This process was based on the ion exchange reaction to replace Cd 2+ with Pb 2+ ions from hydroxyl group followed by replacement of hydroxyl group with selenium ions. The reaction kinetics was accomplished due to more negative free energy of formation and thus the difference in the solubility products. The formed nanotubes were inclusive of Pb and Se with proper inter-chemical bonds with preferred orientations having diameter in tens of nanometer. These nanotubes can have future applications in electronic, optoelectronics and photovoltaic's as well.

Control of nanoparticle agglomeration through variation of the time-temperature profile in chemical vapor synthesis

Energy Technology Data Exchange (ETDEWEB)

Djenadic, Ruzica; Winterer, Markus, E-mail: markus.winterer@uni-due.de [Universität Duisburg-Essen, Nanoparticle Process Technology, Faculty of Engineering and CENIDE (Germany)

2017-02-15

The influence of the time-temperature history on the characteristics of nanoparticles such as size, degree of agglomeration, or crystallinity is investigated for chemical vapor synthesis (CVS). A simple reaction-coagulation-sintering model is used to describe the CVS process, and the results of the model are compared to experimental data. Nanocrystalline titania is used as model material. Titania nanoparticles are generated from titanium-tetraisopropoxide (TTIP) in a hot-wall reactor. Pure anatase particles and mixtures of anatase, rutile (up to 11 vol.%), and brookite (up to 29 vol.%) with primary particle sizes from 1.7 nm to 10.5 nm and agglomerate particle sizes from 24.3 nm to 55.6 nm are formed depending on the particle time-temperature history. An inductively heated furnace with variable inductor geometry is used as a novel system to control the time-temperature profile in the reactor externally covering a large wall temperature range from 873 K to 2023 K. An appropriate choice of inductor geometry, i.e. time-temperature profile, can significantly reduce the degree of agglomeration. Other particle characteristics such as crystallinity are also substantially influenced by the time-temperature profile.

Synthesis and characterization of CoPt nanoparticles prepared by room temperature chemical reduction with PAMAM dendrimer as template.

Science.gov (United States)

Wan, Haiying; Shi, Shifan; Bai, Litao; Shamsuzzoha, Mohammad; Harrell, J W; Street, Shane C

2010-08-01

We describe an approach to synthesize monodisperse CoPt nanoparticles with dendrimer as template by a simple chemical reduction method in aqueous solution using NaBH4 as reducing agent at room temperature. The as-made CoPt nanoparticles buried in the dendrimer matrix have the chemically disordered fcc structure and can be transformed to the fct phase after annealing at 700 degrees C. This is the first report of dendrimer-mediated room temperature synthesis of monodisperse magnetic nanoparticles in aqueous solution.

Facile Low Temperature Hydrothermal Synthesis of BaTiO3 Nanoparticles Studied by In Situ X-ray Diffraction

Directory of Open Access Journals (Sweden)

Ola G. Grendal

2018-06-01

Full Text Available Ferroelectric materials are crucial for today’s technological society and nanostructured ferroelectric materials are important for the downscaling of devices. Controlled and reproducible synthesis of these materials are, therefore, of immense importance. Hydrothermal synthesis is a well-established synthesis route, with a large parameter space for optimization, but a better understanding of nucleation and growth mechanisms is needed for full utilization and control. Here we use in situ X-ray diffraction to follow the nucleation and growth of BaTiO3 formed by hydrothermal synthesis using two different titanium precursors, an amorphous titania precipitate slurry and a Ti-citric acid complex solution. Sequential Rietveld refinement was used to extract the time dependency of lattice parameters, crystallite size, strain, and atomic displacement parameters. Phase pure BaTiO3 nanoparticles, 10–15 nm in size, were successfully synthesized at different temperatures (100, 125, and 150 °C from both precursors after reaction times, ranging from a few seconds to several hours. The two precursors resulted in phase pure BaTiO3 with similar final crystallite size. Finally, two different growth mechanisms were revealed, where the effect of surfactants present during hydrothermal synthesis is discussed as one of the key parameters.

Facile room-temperature solution-phase synthesis of a spherical covalent organic framework for high-resolution chromatographic separation.

Science.gov (United States)

Yang, Cheng-Xiong; Liu, Chang; Cao, Yi-Meng; Yan, Xiu-Ping

2015-08-07

A simple and facile room-temperature solution-phase synthesis was developed to fabricate a spherical covalent organic framework with large surface area, good solvent stability and high thermostability for high-resolution chromatographic separation of diverse important industrial analytes including alkanes, cyclohexane and benzene, α-pinene and β-pinene, and alcohols with high column efficiency and good precision.

The facile and low temperature synthesis of nanophase hydroxyapatite crystals using wet chemistry

International Nuclear Information System (INIS)

Dhand, Vivek; Rhee, K.Y.; Park, Soo-Jin

2014-01-01

A simple and facile wet chemistry route was used to synthesize nanophase hydroxyapatite (HaP) crystals at low temperature. The synthesis was carried out at a pH of 11.0 and at a temperature of 37 °C. The resulting samples were washed several times and subjected to further analysis. XRD studies revealed that the HaP crystals were polycrystalline in nature with a crystallite size of ∼ 15–60 ± 5 nm. SEM-EDXA images confirmed the presence of calcium (Ca), phosphorous (P), and oxygen (O) peaks. Likewise, FTIR confirmed the presence of characteristic phosphate and hydroxyl peaks in samples. Lastly, HRTEM images clearly showed distinctive lattice fringes positioned in the 100 and 002 planes. TGA analysis shows that HaP crystals can withstand higher calcination temperatures and are thermally stable. - Highlights: • Facile and low temperature nanophase HaP crystals synthesized at pH 11 and 37 °C • Electron microscopy image of HaP shows characteristic rice grain like morphology. • FTIR results show the characteristic and fingerprint functional groups of HaP. • Thermal stability of HaP crystals up to 500 °C • Growth of Hap crystals occur parallel to c-axis and a possible mechanism proposed

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

Science.gov (United States)

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

2018-04-01

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

Lithium-deficient Li YMn2O4 spinels (0.9 ≤ Y < 1): Lithium content, synthesis temperature, thermal behaviour and electrochemical properties

International Nuclear Information System (INIS)

Pascual, Laura; Perez-Revenga, M. Luz; Rojas, Rosa M.; Rojo, Jose M.; Amarilla, J. Manuel

2006-01-01

Lithium-deficient Li Y Mn 2 O 4 spinels (LD-Li Y Mn 2 O 4 ) with nominal composition (0.9 ≤ Y 2 O 3 and LiNO 3 at temperatures ranging from 700 deg. C to 850 deg. C. X-ray diffraction data show that LD-Li Y Mn 2 O 4 spinels are obtained as single phases in the range Y = 0.975-1 at 700 deg. C and 750 deg. C. Morphological characterization by transmission electron microscopy shows that the particle size of LD-Li Y Mn 2 O 4 spinels increases on decreasing the Li-content. The influence of the Li-content and the synthesis temperature on the thermal and electrochemical behaviours has been systematically studied. Thermal analysis studies indicate that the temperature of the first thermal effect in the differential thermal analysis (DTA)/thermogravimetric (TG) curves, T C1 , linearly increases on decreasing the Li-content. The electrochemical properties of LD-Li Y Mn 2 O 4 spinels, determined by galvanostatic cycling, notably change with the synthesis conditions. So, the first discharge capacity, Q disch. , at C rate increases on rising the Li-content and the synthesis temperature. The sample Li 0.975 Mn 2 O 4 synthesized at 700 deg. C has a Q disch. = 123 mAh g -1 and a capacity retention of 99.77% per cycle. This LD-Li Y Mn 2 O 4 sample had the best electrochemical characteristics of the series

Low-temperature synthesis of CuFeO{sub 2} (delafossite) at 70 °C: A new process solely by precipitation and ageing

Energy Technology Data Exchange (ETDEWEB)

John, Melanie, E-mail: melanie.john@min.uni-muenchen.de [Section Mineralogy, Petrology & Geochemistry, Department of Earth and Environmental Sciences, Ludwig-Maximilians-Universität München, Theresienstr. 41, 80333 Munich (Germany); Heuss-Aßbichler, Soraya [Section Mineralogy, Petrology & Geochemistry, Department of Earth and Environmental Sciences, Ludwig-Maximilians-Universität München, Theresienstr. 41, 80333 Munich (Germany); Park, So-Hyun [Section Crystallography, Department of Earth and Environmental Sciences, Ludwig-Maximilians-Universität München, Theresienstr. 41, 80333 Munich (Germany); Ullrich, Aladin [Experimental Physics II, University of Augsburg, Universitätsstr. 1, 86159 Augsburg (Germany); Benka, Georg [Physics Department, Technical University Munich, James-Franck-Straße 1, 85748 Garching (Germany); Petersen, Nikolai [Section Geophysics, Department of Earth and Environmental Sciences, Ludwig-Maximilians-Universität München, Theresienstr. 41, 80333 Munich (Germany); Rettenwander, Daniel [Department of Materials Research & Physics, University of Salzburg, Hellbrunnerstrasse 34, 5020 Salzburg (Austria); Horn, Siegfried R. [Experimental Physics II, University of Augsburg, Universitätsstr. 1, 86159 Augsburg (Germany)

2016-01-15

This study presents a new low temperature synthesis method to obtain pure delafossite (Cu{sup 1+}Fe{sup 3+}O{sub 2}) at a temperature of 70 °C within 24 h. For the first time delafossite is synthesized solely by precipitation and subsequent ageing process and without usage of any additives controlling the oxidation state of copper. The synthesized material, called LT-delafossite, consists of pure Cu{sup 1+}Fe{sup 3+}O{sub 2} exclusive of any side products. Rietveld analysis confirms the presence of both 3R (space group (SG): R-3m) and 2H (SG: P6{sub 3}/mmc) polytypes in LT-delafossite. Electron microscopy images show nanometer-sized hexagonal plates with a diameter <500 nm and a thickness of <30 nm. Measurements of the magnetic susceptibility from 2 K to 350 K in zero-field show one peak ∼18.5 K, which is attributed to an AFM phase transition. Zero-field-cooled magnetization data between −14 T and +14 T at 2 K revealed an s-shape form around the origin having no remanent magnetization. - Highlights: • New process: low temperature synthesis of pure CuFeO{sub 2} nanoparticles. • Synthesis at 70 °C within 24 h solely by precipitation and ageing. • Nanoparticle characterization by XRD, FTIR, SEM, ICP–OES, TEM and Mößbauer. • Special magnetic properties of nano-sized CuFeO{sub 2} synthesized at low temperatures.

Room temperature chemical synthesis of lead selenide thin films with preferred orientation

Energy Technology Data Exchange (ETDEWEB)

Kale, R.B. [Department of Chemical Engineering, National Tsing-Hua University, Hsin-Chu, Taiwan 30043 (China)]. E-mail: rb_kale@yahoo.co.in; Sartale, S.D. [Hahn Meitner Institute, Glienicker Strasse-100, D-14109 Berlin (Germany); Ganesan, V. [UGC-DAE Consortium for Scientific Research, University Campus, Khandwa Road, Indore 452017 (India); Lokhande, C.D. [Thin Film Physics Laboratory, Department of Physics, Shivaji University, Kolhapur 416004 (India); Lin, Y.-F. [Department of Chemical Engineering, National Tsing-Hua University, Hsin-Chu, Taiwan 30043 (China); Lu, S.-Y. [Department of Chemical Engineering, National Tsing-Hua University, Hsin-Chu, Taiwan 30043 (China)]. E-mail: sylu@mx.nthu.edu.tw

2006-11-15

Room temperature chemical synthesis of PbSe thin films was carried out from aqueous ammoniacal solution using Pb(CH{sub 3}COO){sub 2} as Pb{sup 2+} and Na{sub 2}SeSO{sub 3} as Se{sup 2-} ion sources. The films were characterized by a various techniques including, X-ray diffraction (XRD), energy dispersive X-ray analysis (EDAX), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HR-TEM), selected area electron diffraction (SAED), Fast Fourier transform (FFT) and UV-vis-NIR techniques. The study revealed that the PbSe thin film consists of preferentially oriented nanocubes with energy band gap of 0.5 eV.

Ambient temperature aqueous synthesis of ultrasmall copper doped ceria nanocrystals for the water gas shift and carbon monoxide oxidation reactions

Energy Technology Data Exchange (ETDEWEB)

Curran, Christopher D. [Department of Chemical and Biomolecular Engineering; Lehigh University; Bethlehem; USA; Lu, Li [Department of Materials Science and Engineering; Lehigh University; Bethlehem; USA; Kiely, Christopher J. [Department of Chemical and Biomolecular Engineering; Lehigh University; Bethlehem; USA; Department of Materials Science and Engineering; McIntosh, Steven [Department of Chemical and Biomolecular Engineering; Lehigh University; Bethlehem; USA

2018-01-01

Ultra-small Cu_xCe_1-xO_2-δnanocrystals were prepared through a room temperature, aqueous synthesis method, achieving high copper doping and low water gas shift activation energy.

Synthesis and characterization of iron cobalt (FECO) nanorods ...

African Journals Online (AJOL)

Synthesis and characterization of iron cobalt (FECO) nanorods prepared by simple ... shaped by increasing annealing temperature from room temperature to 800 ... Keywords: FeCo nanoparticles, sodium borohydrid, CTAB, chemical synthesis ...

Multipurpose high-pressure high-temperature diamond-anvil cell with a novel high-precision guiding system and a dual-mode pressurization device

Science.gov (United States)

Pippinger, Thomas; Miletich, Ronald; Burchard, Michael

2011-09-01

A novel diamond-anvil cell (DAC) design has been constructed and tested for in situ applications at high-pressure (HP) operations and has proved to be suitable even for HP sample environments at non-ambient temperature conditions. The innovative high-precision guiding mechanism, comparable to a dog clutch, consists of perpendicular planar sliding-plane elements and is integrated directly into the base body of the cylindrically shaped DAC. The combination of two force-generating devices, i.e., mechanical screws and an inflatable gas membrane, allows the user to choose independently between, and to apply individually, two different forcing mechanisms for pressure generation. Both mechanisms are basically independent of each other, but can also be operated simultaneously. The modularity of the DAC design allows for an easy exchange of functional core-element groups optimized not only for various analytical in situ methods but also for HP operation with or without high-temperature (HT) application. For HP-HT experiments a liquid cooling circuit inside the specific inner modular groups has been implemented to obtain a controlled and limited heat distribution within the outer DAC body.

Glucose Synthesis in a Protein-Based Artificial Photosynthesis System.

Science.gov (United States)

Lu, Hao; Yuan, Wenqiao; Zhou, Jack; Chong, Parkson Lee-Gau

2015-09-01

The objective of this study was to understand glucose synthesis of a protein-based artificial photosynthesis system affected by operating conditions, including the concentrations of reactants, reaction temperature, and illumination. Results from non-vesicle-based glyceraldehyde-3-phosphate (GAP) and glucose synthesis showed that the initial concentrations of ribulose-1,5-bisphosphate (RuBP) and adenosine triphosphate (ATP), lighting source, and temperature significantly affected glucose synthesis. Higher initial concentrations of RuBP and ATP significantly enhanced GAP synthesis, which was linearly correlated to glucose synthesis, confirming the proper functions of all catalyzing enzymes in the system. White fluorescent light inhibited artificial photosynthesis and reduced glucose synthesis by 79.2 % compared to in the dark. The reaction temperature of 40 °C was optimum, whereas lower or higher temperature reduced glucose synthesis. Glucose synthesis in the vesicle-based artificial photosynthesis system reconstituted with bacteriorhodopsin, F 0 F 1 ATP synthase, and polydimethylsiloxane-methyloxazoline-polydimethylsiloxane triblock copolymer was successfully demonstrated. This system efficiently utilized light-induced ATP to drive glucose synthesis, and 5.2 μg ml(-1) glucose was synthesized in 0.78-ml reaction buffer in 7 h. Light-dependent reactions were found to be the bottleneck of the studied artificial photosynthesis system.

Low temperature synthesis of Ba1–xSrxSnO3 (x= 0–1) from molten ...

Indian Academy of Sciences (India)

... Lecture Workshops · Refresher Courses · Symposia · Live Streaming. Home; Journals; Bulletin of Materials Science; Volume 33; Issue 1. Low temperature synthesis of Ba1–SrSnO3 ( = 0–1) from molten alkali hydroxide flux. B Ramdas R Vijayaraghavan. Electrical Properties Volume 33 Issue 1 February 2010 pp 75- ...

Low temperature synthesis of silicon quantum dots with plasma chemistry control in dual frequency non-thermal plasmas.

Science.gov (United States)

Sahu, Bibhuti Bhusan; Yin, Yongyi; Han, Jeon Geon; Shiratani, Masaharu

2016-06-21

The advanced materials process by non-thermal plasmas with a high plasma density allows the synthesis of small-to-big sized Si quantum dots by combining low-temperature deposition with superior crystalline quality in the background of an amorphous hydrogenated silicon nitride matrix. Here, we make quantum dot thin films in a reactive mixture of ammonia/silane/hydrogen utilizing dual-frequency capacitively coupled plasmas with high atomic hydrogen and nitrogen radical densities. Systematic data analysis using different film and plasma characterization tools reveals that the quantum dots with different sizes exhibit size dependent film properties, which are sensitively dependent on plasma characteristics. These films exhibit intense photoluminescence in the visible range with violet to orange colors and with narrow to broad widths (∼0.3-0.9 eV). The observed luminescence behavior can come from the quantum confinement effect, quasi-direct band-to-band recombination, and variation of atomic hydrogen and nitrogen radicals in the film growth network. The high luminescence yields in the visible range of the spectrum and size-tunable low-temperature synthesis with plasma and radical control make these quantum dot films good candidates for light emitting applications.

A Novel Practical Synthesis of Phenanthrenes Using Iron(Ⅲ) Chloride Involved Intramolecular Oxidative Coupling at Room Temperature

Institute of Scientific and Technical Information of China (English)

L(U),Mao-Yun; WANG,Kai-Liang; CAI,Fei; WANG,Hai-Ying; WANG,Qing-Min

2008-01-01

Iron(Ⅲ) chloride has been used to prepare the polymethoxy substituted phenanthrene derivatives via in-tramolecular oxidative coupling of (E or Z)-2,3-di(substituted phenyl)acrylate at room temperature in excellent yields. Mild reaction conditions and the use of inexpensive and nontoxic FeCI3 provide a novel practical and large-scaled viable route for the synthesis of the important phenanthrene rings.

Surface decoration through electrostatic interaction leading to enhanced reactivity: Low temperature synthesis of nanostructured chromium borides (CrB and CrB2)

International Nuclear Information System (INIS)

Menaka,; Kumar, Bharat; Kumar, Sandeep; Ganguli, A.K.

2013-01-01

The present study describes a novel low temperature route at ambient pressure for the synthesis of nanocrystalline chromium borides (CrB and CrB 2 ) without using any flux or additives. The favorable and intimate mixing of nanoparticles of chromium acetate (Cr source) and boron forms an active chromium–boron precursor which decomposes at much lower temperature (400 °C) to form CrB (which is ∼1000 °C less than the known ambient pressure synthesis). The chromium acetate nanoparticles (∼5 nm) decorate the larger boron particles (150–200 nm) due to electrostatic interactions resulting from opposing surface charges of boron (zeta potential:+48.101 mV) and chromium acetate (zeta potential:−4.021 mV) in ethanolic medium and is evident in the TEM micrographs. The above method leads to the formation of pure CrB film like structure at 400 °C and nanospheres (40–60 nm) at 600 °C. Also, chromium diboride (CrB 2 ) nanoparticles (25 nm) could be obtained at 1000 °C. - Graphical abstract: Variation of surface charge of reactants, precursor and the products, chromium borides (CrB and CrB 2 ). Highlights: ► Novel borothermal reduction process for synthesis of chromium boride. ► Significant lowering of reaction temperature to obtain nanocrystalline chromium boride. ► Enhanced reactivity due to appropriate surface interactions

Room temperature synthesis of 2D CuO nanoleaves in aqueous solution

International Nuclear Information System (INIS)

Zhao Yan; Li Yunling; Wang Zichen; Zhao Jingzhe; Ma Dechong; Hou Shengnan; Li Linzhi; Hao Xinli

2011-01-01

A simple room temperature method was reported for the synthesis of CuO nanocrystals in aqueous solution through the sequence of Cu 2+ → Cu(OA) 2 → Cu(OH) 2 → Cu(OH) 4 2- → CuO. Sodium oleate (SOA) was used as the surfactant and shape controller. The as-prepared samples were characterized by x-ray diffraction (XRD), scanning electron microscopy (SEM), UV-visible absorption spectroscopy (UV-vis) and differential thermal analysis (DTA). It can be seen that 1D Cu(OH) 2 nanowires were first obtained from Cu(OA) 2 and, at room temperature, converted into 2D CuO nanoleaves (CuO NLs) in a short time under a weakly basic environment. On prolonging the reaction time, the top part of these 2D nanoleaves branched and separated along the long axis to form 1D rod-like nano-CuO because of the assistance of SOA. A possible transformation mechanism of Cu(OH) 2 to CuO nanostructures at room temperature in aqueous solution is discussed. The transformation velocity can be controlled by changing the pH value of the system. The prepared CuO NLs were used to construct an enzyme-free glucose sensor. The detecting results showed that the designed sensor exhibited good amperometric responses towards glucose with good anti-interferent ability.

Low-temperature synthesis and structural properties of ferroelectric K 3WO 3F 3 elpasolite

Science.gov (United States)

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.

Synthesis of ultrasmall CsPbBr3 nanoclusters and their transformation to highly deep-blue-emitting nanoribbons at room temperature.

Science.gov (United States)

Xu, Yibing; Zhang, Qiang; Lv, Longfei; Han, Wenqian; Wu, Guanhong; Yang, Dong; Dong, Angang

2017-11-16

Discretely sized semiconductor clusters have attracted considerable attention due to their intriguing optical properties and self-assembly behaviors. While lead halide perovskite nanostructures have been recently intensively explored, few studies have addressed perovskite clusters and their self-assembled superstructures. Here, we report the room-temperature synthesis of sub-2 nm CsPbBr 3 clusters and present strong evidence that these ultrasmall perovskite species, obtained under a wide range of reaction conditions, possess a specific size, with optical properties and self-assembly characteristics resembling those of well-known II-VI semiconductor magic-sized clusters. Unlike conventional CsPbBr 3 nanocrystals, the as-synthesized CsPbBr 3 nanoclusters spontaneously self-assemble into a hexagonally packed columnar mesophase in solution, which can be further converted to single-crystalline CsPbBr 3 quantum nanoribbons with bright deep-blue emission at room temperature. Such a conversion of CsPbBr 3 nanoclusters to nanoribbons is found to be driven by a ligand-destabilization-induced crystallization and mesophase transition process. Our study will facilitate the investigation of perovskite nanoclusters and offer new possibilities in the low-temperature synthesis of anisotropic perovskite nanostructures.

Influence of Synthesis Temperature on the Growth and Surface Morphology of Co3O4 Nanocubes for Supercapacitor Applications

Science.gov (United States)

Samal, Rashmirekha; Dash, Barsha; Sarangi, Chinmaya Kumar; Subbaiah, Tondepu; Senanayake, Gamini; Minakshi, Manickam

2017-01-01

A facile hydrothermal route to control the crystal growth on the synthesis of Co3O4 nanostructures with cube-like morphologies has been reported and tested its suitability for supercapacitor applications. The chemical composition and morphologies of the as-prepared Co3O4 nanoparticles were extensively characterized using X-ray diffraction (XRD) and transmission electron microscopy (TEM). Varying the temperature caused considerable changes in the morphology, the electrochemical performance increased with rising temperature, and the redox reactions become more reversible. The results showed that the Co3O4 synthesized at a higher temperature (180 °C) demonstrated a high specific capacitance of 833 F/g. This is attributed to the optimal temperature and the controlled growth of nanocubes. PMID:29088061

Synthesis of high luminescent carbon nanoparticles

Science.gov (United States)

Gvozdyuk, Alina A.; Petrova, Polina S.; Goryacheva, Irina Y.; Sukhorukov, Gleb B.

2017-03-01

In this article we report an effective and simple method for synthesis of high luminescent carbon nanodots (CDs). In our work as a carbon source sodium dextran sulfate (DS) was used because it is harmless, its analogs are used in medicine as antithrombotic compounds and blood substitutes after hemorrhage. was used as a substrate We investigated the influence of temperature parameters of hydrothermal synthesis on the photoluminescence (PL) intensity and position of emission maxima. We discovered that the PL intensity can be tuned by changing of synthesis temperature and CD concentration.

Mg(OH){sub 2} nanoparticles produced at room temperature by an innovative, facile, and scalable synthesis route

Energy Technology Data Exchange (ETDEWEB)

Taglieri, Giuliana, E-mail: giuliana.taglieri@univaq.it; Felice, Benito; Daniele, Valeria; Ferrante, Fabiola [University of L’Aquila, Department of Industrial and Information Engineering and Economics (Italy)

2015-10-15

Nanoparticles form the fundamental building blocks for many exciting applications in various scientific disciplines. However, the problem of the large-scale synthesis of nanoparticles remains challenging. An original, eco-friendly, single step, and scalable method to produce magnesium hydroxide nanoparticles in aqueous suspensions is here presented. The method, based on an exchange ion process, is extremely simple and rapid (few minutes). It employs cheap or renewable reactants, operates at room temperature and does not require intermediate steps (washings/purifications) to eliminate undesired compounds. Moreover, it is possible to regenerate the exchange material and to reuse it for new operation of synthesis, according to a cyclic procedure, providing potential aptitudes of scalability of nanoparticles production. Some of the synthesis parameters are varied, and structural and morphological features of the produced nanoparticles, after few seconds from the beginning of the synthesis up to the ending time, are investigated by means of several techniques, such as X-ray diffraction (profile fitting and Rietveld refinement), transmission electron microscopy, infrared spectroscopy, thermal analyses, and surface area measurements. In any case, pure and stable suspensions are produced, characterized by crystalline and mesoporous Mg(OH){sub 2} nanoparticles, with lamellar morphology. In particular, the nanolamellas appeared constituted by a superimposition of hexagonally plated and crystalline nanosized precursors (2–3 nm in dimensions), crystallographically oriented.

A facile synthesis of substituted 2-alkylquinolines through [3+3] annulation between 3-ethoxycyclobutanones and aromatic amines at room temperature.

Science.gov (United States)

Shan, Gang; Sun, Xiuyun; Xia, Qian; Rao, Yu

2011-11-04

An efficient single-step approach toward the synthesis of 2-alkylquinolines is described. Through a Lewis acid mediated [3+3] annulation reaction between 3-ethoxycyclobutanones and aromatic amines, a variety of multisubstituted 2-alkylquinoline derivatives were prepared regioselectively at room temperature. © 2011 American Chemical Society

Mathematical Model of Synthesis Catalyst with Local Reaction Centers

Directory of Open Access Journals (Sweden)

I. V. Derevich

2017-01-01

Full Text Available The article considers a catalyst granule with a porous ceramic passive substrate and point active centers on which an exothermic synthesis reaction occurs. A rate of the chemical reaction depends on the temperature according to the Arrhenius law. Heat is removed from the pellet surface in products of synthesis due to heat transfer. In our work we first proposed a model for calculating the steady-state temperature of a catalyst pellet with local reaction centers. Calculation of active centers temperature is based on the idea of self-consistent field (mean-field theory. At first, it is considered that powers of the reaction heat release at the centers are known. On the basis of the found analytical solution, which describes temperature distribution inside the granule, the average temperature of the reaction centers is calculated, which then is inserted in the formula for heat release. The resulting system of transcendental algebraic equations is transformed into a system of ordinary differential equations of relaxation type and solved numerically to achieve a steady-state value. As a practical application, the article considers a Fischer-Tropsch synthesis catalyst granule with active cobalt metallic micro-particles. Cobalt micro-particles are the centers of the exothermic reaction of hydrocarbons macromolecular synthesis. Synthesis occurs as a result of absorption of the components of the synthesis gas on metallic cobalt. The temperature distribution inside the granule for a single local center and reaction centers located on the same granule diameter is found. It was found that there is a critical temperature of reactor exceeding of which leads to significant local overheating of the centers - thermal explosion. The temperature distribution with the local reaction centers is qualitatively different from the granule temperature, calculated in the homogeneous approximation. It is shown that, in contrast to the homogeneous approximation, the

OMS-2-Supported Cu Hydroxide-Catalyzed Benzoxazoles Synthesis from Catechols and Amines via Domino Oxidation Process at Room Temperature.

Science.gov (United States)

Meng, Xu; Wang, Yanmin; Wang, Yuanguang; Chen, Baohua; Jing, Zhenqiang; Chen, Gexin; Zhao, Peiqing

2017-07-07

In the presence of manganese oxide octahedral molecular sieve (OMS-2) supported copper hydroxide Cu(OH) x /OMS-2, aerobic synthesis of benzoxazoles from catechols and amines via domino oxidation/cyclization at room temperature is achieved. This heterogeneous benzoxazoles synthesis initiated by the efficient oxidation of catechols over Cu(OH) x /OMS-2 tolerates a variety of substrates, especially amines containing sensitive groups (hydroxyl, cyano, amino, vinyl, ethynyl, ester, and even acetyl groups) and heterocycles, which affords functionalized benzoxazoles in good to excellent yields by employing low catalyst loading (2 mol % Cu). The characterization and plausible catalytic mechanism of Cu(OH) x /OMS-2 are described. The notable features of our catalytic protocol such as the use of air as the benign oxidant and EtOH as the solvent, mild conditions, ease of product separation, being scalable up to the gram level, and superior reusability of catalyst (up to 10 cycles) make it more practical and environmentally friendly for organic synthesis.

Low-temperature solid-state synthesis and optical properties of ZnO/CdS nanocomposites

International Nuclear Information System (INIS)

Liu, Jinsong; Zhu, Kongjun; Sheng, Beibei; Li, Ziquan; Tai, Guoan; Qiu, Jinhao; Wang, Jing; Chen, Jiankang; You, Yuncheng; Gu, Qilin; Liu, Pengcheng

2015-01-01

Highlights: • Using a low-temperature solid-state method, ZnO/CdS nanocomposites were obtained • Grain growth kinetics of cubic CdS and hexagonal ZnO phase was described. • Sufficient grinding and heating treatment was a key for formation of composites. • Optical properties could be easily manipulated by reaction temperature and time. - Abstract: A simple low-temperature solid-state reaction in the presence of the surfactant PEG400 was developed to obtain ZnO/CdS nanocomposites. The effects of synthesis temperature and reaction time on crystal structure and optical properties of the nanocomposites were investigated by several technologies. X-ray diffraction (XRD) and high resolution transmission electron microscope (HRTEM) characterizations showed that the products consisted of the nanoparticles, and the grain growth kinetics of the cubic CdS and the hexagonal ZnO phase in the nanocomposites was described. The mechanism analysis suggested that sufficient grinding and heating treatment was a key to form the ZnO/CdS nanocomposites, and the surfactant PEG400 was proved not to involve the reaction and prevent the nanoparticles from aggregating to larger in whole grinding and heat-treatment process. Ultraviolet–visible (UV–vis) spectra revealed that the band gaps of the nanocomposites could be tuned by the reaction temperature and reaction time. Photoluminescence (PL) spectra showed that the changing position and the intensity of the emission peaks resulted from the rate of electron transfer and recombination probability under the different conditions

Radiation chemical synthesis

International Nuclear Information System (INIS)

Zagoretz, P.A.; Poluetkov, V.A.; Shostenko, A.G.

1986-01-01

The authors consider processes in radiation chemical synthesis which are being developed in various scientific-research organizations. The important advantages of radiation chlorination, viz. the lower temperature compared with the thermal method and the absence of dehydrochlorination products are discussed. The authors examine the liquid-phase chlorination of trifluorochloroethyltrichloromethyl ether to obtain the pentachloro-contining ether, trifluorodichloroethyltrichloromethyl ether. The authors discuss radiation synthesis processes that have be used formulated kinetic equations on which models have been based. It is concluded that the possibilities of preparative (micro- and low-tonnage) radiation synthesis are promising

Spectroscopic study of defects and inclusions in bulk poly- and nanocrystalline diamond aggregates

International Nuclear Information System (INIS)

Shiryaev, A A; Iakoubovskii, K; Grambole, D; Dubrovinskaia, N

2006-01-01

Recently, a novel form of nanodiamond exhibiting unusual mechanical properties has been synthesized by high-pressure high-temperature (HPHT) treatment of C 60 fullerene, amorphous carbon and diamond powder. In this study, we have characterized the dominant defects in this nanodiamond by a combination of optical absorption, luminescence, Raman, electron spin resonance and elastic recoil detection techniques. Unusually high concentrations (∼0.4 at.%) of hydrogen and very low concentrations of nitrogen (∼10 -5 at.%) have been detected in diamond grown from C 60 . Although most of hydrogen is shown to originate from inclusions of foreign phases, such as water, significant concentrations (∼0.01 at.%) of hydrogen were also detected as a point defect in the nanodiamond grains. Observed structural differences between the samples made from various carbonaceous materials are attributed to different behaviour of the starting compounds during HPHT treatment. (letter to the editor)

Low-temperature solid-state synthesis and optical properties of CdS-ZnS and ZnS-CdS alloy nanoparticles

International Nuclear Information System (INIS)

Liu Jinsong; Zhao Chuanbao; Li Ziquan; Chen Jiankang; Zhou Hengzhi; Gu Shanqun; Zeng Youhong; Li Yongchan; Huang Yongbing

2011-01-01

Highlights: → Using a simple low-temperature solid-state synthetic method, ZnS-CdS and CdS-ZnS alloy nanoparticles were obtained, respectively. → The size of the nanoparticles increased with increasing reaction temperature, and reaction sequence had no effect on the size of the nanoparticles under the same temperature. → The particle diameters of the CdS-ZnS products decreased gradually with increasing Cd 2+ /Zn 2+ molar ratio, whereas those of the ZnS-CdS products increased gradually with increasing Zn 2+ /Cd 2+ molar ratio. → The study shows that sufficient grinding and crystalline water may be a key in forming the alloy nanoparticles. → Optical properties of the products depend on reaction temperature, reactant addition sequence, and reactant molar ratio. - Abstract: A simple low-temperature solid-state synthetic method was employed to obtain ZnS-CdS and CdS-ZnS alloy nanoparticles. The effects of reaction sequence, reactant molar ratios, and synthesis temperature on the products were investigated. The crystal structure and morphology of the products were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), and fourier transform infrared (FT-IR) spectroscopy. The results show that the products are alloy nanoparticles with a cubic phase structure. The formation mechanism of the alloy nanoparticles is briefly discussed. Sufficient grinding and crystalline water may be essential to form alloy nanoparticles. Ultraviolet-visible (UV-vis) spectra show that the edge absorptions of the CdS-ZnS and ZnS-CdS nanoparticles were located between those of ZnS and CdS bulks, and the absorbance at the peak maximum was practically dependent on reaction temperature, reaction sequence, and molar ratio. Extrinsic deep-level emission resulted in strong peaks in the photoluminescence (PL) spectra. The position and intensity of the emission peaks varied with the conditions during synthesis.

Influence of the synthesis parameters on the physico-chemical and catalytic properties of cerium oxide for application in the synthesis of diethyl carbonate

International Nuclear Information System (INIS)

Leino, Ewelina; Kumar, Narendra; Mäki-Arvela, Päivi; Aho, Atte; Kordás, Krisztián; Leino, Anne-Riikka; Shchukarev, Andrey; Murzin, Dmitry Yu.; Mikkola, Jyri-Pekka

2013-01-01

Synthesis of cerium (IV) oxide by means of room temperature precipitation method was carried out. The effect of preparation variables such as synthesis time, calcination temperature and pH of the solution on resulting CeO 2 properties was discussed. Moreover, the comparison of CeO 2 samples prepared in a static and rotation mode of synthesis is presented. The solid catalysts were characterized by means of X-ray powder diffraction, scanning electron microscopy, transmission electron microscope, nitrogen physisorption, X-ray photoelectron spectroscopy, Fourier transform infrared spectroscopy using pyridine as a probe molecule and temperature programmed desorption of CO 2 . Significant variations in physico-chemical properties of CeO 2 by varying the preparation conditions were observed. Furthermore, the catalytic performances of CeO 2 catalysts were compared in the synthesis of diethyl carbonate starting from ethanol and CO 2 using butylene oxide as a dehydrating agent. The dependence of CeO 2 properties on its catalytic activity is evaluated in detail. - Highlights: • Synthesis of cerium (IV) oxide by precipitation method. • Influence of synthesis time, calcination temperature, mode of stirring and solution pH on properties. • Characterization by XRD, SEM, TEM, nitrogen physisorption, XPS, FTIR. • Catalytic performance diethyl carbonate synthesis from ethanol and CO 2

Room-Temperature Synthesis of Thiostannates from {[Ni(tren)]2[Sn2S6]}n.

Science.gov (United States)

Hilbert, Jessica; Näther, Christian; Weihrich, Richard; Bensch, Wolfgang

2016-08-15

The compound {[Ni(tren)]2[Sn2S6]}n (1) (tren = tris(2-aminoethyl)amine, C6H18N4) was successfully applied as source for the room-temperature synthesis of the new thiostannates [Ni(tren)(ma)(H2O)]2[Sn2S6]·4H2O (2) (ma = methylamine, CH5N) and [Ni(tren)(1,2-dap)]2[Sn2S6]·2H2O (3) (1,2-dap = 1,2-diaminopropane, C3H10N2). The Ni-S bonds in the Ni2S2N8 bioctahedron in the structure of 1 are analyzed with density functional theory calculations demonstrating significantly differing Ni-S bond strengths. Because of this asymmetry they are easily broken in the presence of an excess of ma or 1,2-dap immediately followed by Ni-N bond formation to N donor atoms of the amine ligands thus generating [Ni(tren)(amine)](2+) complexes. The chemical reactions are fast, and compounds 2 and 3 are formed within 1 h. The synthesis concept presented here opens hitherto unknown possibilities for preparation of new thiostannates.

One-step synthesis of lightly doped porous silicon nanowires in HF/AgNO3/H2O2 solution at room temperature

International Nuclear Information System (INIS)

Bai, Fan; Li, Meicheng; Song, Dandan; Yu, Hang; Jiang, Bing; Li, Yingfeng

2012-01-01

One-step synthesis of lightly doped porous silicon nanowire arrays was achieved by etching the silicon wafer in HF/AgNO 3 /H 2 O 2 solution at room temperature. The lightly doped porous silicon nanowires (pNWs) have circular nanopores on the sidewall, which can emit strong green fluorescence. The surface morphologies of these nanowires could be controlled by simply adjusting the concentration of H 2 O 2 , which influences the distribution of silver nanoparticles (Ag NPs) along the nanowire axis. A mechanism based on Ag NPs-induced lateral etching of nanowires was proposed to explain the formation of pNWs. The controllable and widely applicable synthesis of pNWs will open their potential application to nanoscale photoluminescence devices. - Graphical abstract: The one-step synthesis of porous silicon nanowire arrays is achieved by chemical etching of the lightly doped p-type Si (100) wafer at room temperature. These nanowires exhibit strong green photoluminescence. SEM, TEM, HRTEM and photoluminescence images of pNWs. The scale bars of SEM, TEM HRTEM and photoluminescence are 10 μm, 20 nm, 10 nm, and 1 μm, respectively. Highlights: ► Simple one-step synthesis of lightly doped porous silicon nanowire arrays is achieved at RT. ► Etching process and mechanism are illustrated with etching model from a novel standpoint. ► As-prepared porous silicon nanowire emits strong green fluorescence, proving unique property.

Low temperature synthesis of Mo2C/W2C superlattices via ultra-thin modulated reactants

International Nuclear Information System (INIS)

Johnson, C.D.; Johnson, D.C.

1996-01-01

The authors report here a synthesis method of preparing carbide superlattices using ultra-thin modulated reactants. Initial investigations into the synthesis of the binary systems, Mo 2 C and W 2 C using ultra-thin modulated reactants revealed that both can be formed at relatively low temperatures (500 and 600 C respectively). DSC and XRD data suggested a two step reaction pathway involving interdiffusion of the initial modulated reactant followed by crystallization of the final product, if the modulation length is on the order of 10 angstrom. This information was used to form Mo 2 C/W 2 C superlattices using the structure of the ultra-thin modulated reactant to control the final superlattice period. Relatively large superlattice modulations were kinetically trapped by having several repeat units of each binary within the total repeat of the initial reactant. DSC and XRD data again are consistent with a two step reaction pathway leading to the formation of carbide superlattices

Synthesis of high saturation magnetic iron oxide nanomaterials via low temperature hydrothermal method

Energy Technology Data Exchange (ETDEWEB)

Bhavani, P.; Rajababu, C.H. [Department of Materials Science & Nanotechnology, Yogivemana University, Vemanapuram 516003, Kadapa (India); Arif, M.D. [Environmental Magnetism Laboratory, Indian Institute of Geomagnetism (IIG), Navi Mumbai 410218, Mumbai (India); Reddy, I. Venkata Subba [Department of Physics, Gitam University, Hyderabad Campus, Rudraram, Medak 502329 (India); Reddy, N. Ramamanohar, E-mail: manoharphd@gmail.com [Department of Materials Science & Nanotechnology, Yogivemana University, Vemanapuram 516003, Kadapa (India)

2017-03-15

Iron oxide nanoparticles (IONPs) were synthesized through a simple low temperature hydrothermal approach to obtain with high saturation magnetization properties. Two series of iron precursors (sulfates and chlorides) were used in synthesis process by varying the reaction temperature at a constant pH. The X-ray diffraction pattern indicates the inverse spinel structure of the synthesized IONPs. The Field emission scanning electron microscopy and high resolution transmission electron microscopy studies revealed that the particles prepared using iron sulfate were consisting a mixer of spherical (16–40 nm) and rod (diameter ~20–25 nm, length <100 nm) morphologies that synthesized at 130 °C, while the IONPs synthesized by iron chlorides are found to be well distributed spherical shapes with size range 5–20 nm. On other hand, the IONPs synthesized at reaction temperature of 190 °C has spherical (16–46 nm) morphology in both series. The band gap values of IONPs were calculated from the obtained optical absorption spectra of the samples. The IONPs synthesized using iron sulfate at temperature of 130 °C exhibited high saturation magnetization (M{sub S}) of 103.017 emu/g and low remanant magnetization (M{sub r}) of 0.22 emu/g with coercivity (H{sub c}) of 70.9 Oe{sub ,} which may be attributed to the smaller magnetic domains (d{sub m}) and dead magnetic layer thickness (t). - Highlights: • Comparison of iron oxide materials prepared with Fe{sup +2}/Fe{sup +3} sulfates and chlorides at different temperatures. • We prepared super-paramagnetic and soft ferromagnetic magnetite nanoparticles. • We report higher saturation magnetization with lower coercivity.

Fabrication of intermetallic NiAl by self-propagating high-temperature synthesis reaction using aluminium nanopowder under high pressure

CERN Document Server

Dong Shu Shan; Cheng Hai Yong; Yang Hai Bin; Zou Guang Tian

2002-01-01

By using aluminium nanopowder prepared by wire electrical explosion, pure monophase NiAl compound with fine crystallites (<=10 mu m) and good densification (98% of the theoretical green density) was successfully fabricated by means of self-propagating high-temperature synthesis (SHS) under a high pressure of 50 MPa. Investigation shows that, due to the physical and chemical characteristics of the nanoparticles, the SHS reaction mode and mechanism are distinct from those when using conventional coarse-grained reactants. The SHS reaction process depends on the thermal conditions related to pressure and can occur at a dramatically low temperature of 308 sup o C, which cannot be expected in conventional SHS reaction. With increasing pressure, the SHS explosive ignition temperature (T sub i sub g) of forming NiAl decreases due to thermal and kinetic effects.

Synthesis of ammonia using sodium melt

OpenAIRE

Kawamura, Fumio; Taniguchi, Takashi

2017-01-01

Research into inexpensive ammonia synthesis has increased recently because ammonia can be used as a hydrogen carrier or as a next generation fuel which does not emit CO2. Furthermore, improving the efficiency of ammonia synthesis is necessary, because current synthesis methods emit significant amounts of CO2. To achieve these goals, catalysts that can effectively reduce the synthesis temperature and pressure, relative to those required in the Haber-Bosch process, are required. Although severa...

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

Science.gov (United States)

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

2014-09-01

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

Diffusion of Co and W in diamond tool induced by 10.6 µm CO2 laser radiation

CSIR Research Space (South Africa)

Masina, Bathusile N

2011-05-01

Full Text Available www.csir.co.za Experimental setup CO2 laser ZnSe lens, f = 250 mm HPHT diamond sample Infrared camera Slide 8 © CSIR 2009 www.csir.co.za Experimental setup CO2 laser ZnSe lens, f = 250 mm HPHT diamond sample Infrared camera...

Mesoporous Structure Control of Silica in Room-Temperature Synthesis under Basic Conditions

Directory of Open Access Journals (Sweden)

Jeong Wook Seo

2015-01-01

Full Text Available Various types of mesoporous silica, such as continuous cubic-phase MCM-48, hexagonal-phase MCM-41, and layer-phase spherical silica particles, have been synthesized at room temperature using cetyltrimethylammonium bromide as a surfactant, ethanol as a cosurfactant, tetraethyl orthosilicate as a silica precursor, and ammonia as a condensation agent. Special care must be taken both in the filtering of the resultant solid products and in the drying process. In the drying process, further condensation of the silica after filtering was induced. As the surfactant and cosurfactant concentrations in the reaction mixture increased and the NH3 concentration decreased, under given conditions, continuous cubic MCM-48 and layered silica became the dominant phases. A cooperative synthesis mechanism, in which both the surfactant and silica were involved in the formation of mesoporous structures, provided a good explanation of the experimental results.

Low temperature molten salt synthesis of Y(sub2)Sn(sub2)O(sub7) anode material for lithium ion batteries

CSIR Research Space (South Africa)

Nithyadharseni, P

2015-10-01

Full Text Available Acta 182 (2015) 1060–1069 Low temperature molten salt synthesis of Y2Sn2O7 anode material for lithium ion batteries P. Nithyadharsenia,b, M.V. Reddya,c,*, Kenneth I. Ozoemenab,d, R. Geetha Balakrishnae, B.V.R. Chowdaria a Advanced Batteries...

A Comparative Characterization of the HPA-MCM-48 Type Catalysts Produced by the Direct Hydrothermal and Room Temperature Synthesis Methods

International Nuclear Information System (INIS)

Gucbilmez, Y.; Calis, I.; Yargic, A. S.

2012-01-01

MCM-48 type support materials synthesized by the direct hydrothermal synthesis (HTS) and room temperature synthesis (RTS) methods were incorporated with tungstophosphoric acid (TPA) in the range of 10-40 wt% by using a wet impregnation technique in methanol solutions. Resulting HPA-MCM-48 catalysts were characterized by the XRD, Nitrogen Physisorption, SEM, TEM, EDS, and FT-IR methods in order to determine the effects of different initial synthesis conditions on the catalyst properties. RTS samples were found to have better crystalline structures, higher BET surface areas, and higher BJH pore volumes than HTS samples. They also had slightly higher TPA incorporation, except for the 40 wt% samples, as evidenced by the EDS results. Keggin ion structure was preserved, for both methods, even at the highest acid loading of 40 wt%. It was concluded that the simpler and more economical RTS method was more successful than the HTS method for hetero poly acid incorporation into MCM-48 type materials

A green synthesis of a layered titanate, potassium lithium titanate; lower temperature solid-state reaction and improved materials performance

International Nuclear Information System (INIS)

Ogawa, Makoto; Morita, Masashi; Igarashi, Shota; Sato, Soh

2013-01-01

A layered titanate, potassium lithium titanate, with the size range from 0.1 to 30 µm was prepared to show the effects of the particle size on the materials performance. The potassium lithium titanate was prepared by solid-state reaction as reported previously, where the reaction temperature was varied. The reported temperature for the titanate preparation was higher than 800 °C, though 600 °C is good enough to obtain single-phase potassium lithium titanate. The lower temperature synthesis is cost effective and the product exhibit better performance as photocatalysts due to surface reactivity. - Graphical abstract: Finite particle of a layered titanate, potassium lithium titanate, was prepared by solid-state reaction at lower temperature to show modified materials performance. Display Omitted - Highlights: • Potassium lithium titanate was prepared by solid-state reaction. • Lower temperature reaction resulted in smaller sized particles of titanate. • 600 °C was good enough to obtain single phased potassium lithium titanate. • The product exhibited better performance as photocatalyst

Low temperature synthesis of hydroxyapatite nano-rods by a modified sol-gel technique

International Nuclear Information System (INIS)

Jadalannagari, Sushma; More, Sandeep; Kowshik, Meenal; Ramanan, Sutapa Roy

2011-01-01

Hydroxyapatite (HAp) nano-rods were successfully synthesized by a modified sol-gel method using a solution of CaCl 2 .2H 2 O in water, along with a solution of H 3 PO 4 in triethylamine and NH 4 OH as starting materials. The Ca/P molar ratio was maintained at 1.67. The sol obtained was dried in an oven for 2 days at 100 deg. C after being dialyzed for 12 h. Pellets were made from the crystalline powders and immersed in simulated body fluid (SBF) to check its biocompatibility after 15, 45 and 180 days of immersion. The HAp powders and pellets were characterized by X-Ray Diffraction crystallography (XRD), Fourier transform Infrared spectroscopy (FTIR), scanning electron microscopy (SEM), and Transmission electron microscopy (TEM). The HAp nano-rods had an average diameter of 25 nm and length 110-120 nm. Immersion of the HAp pellets in SBF led to the formation of a highly porous interconnecting HAp layer on the surface. The porosity increased with increase in immersion time. Highlights: → Low temperature synthesis of hydroxyapatite nanorods using Ca and P sources and triethylamine. → The synthesis time was only 0.5 hours. → Crystalline material was obtained after drying at 100oC only in air. → SBF studies showed the HAP bodies to be biocompatible.

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

Science.gov (United States)

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

2018-05-08

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

Mg2FeH6 Synthesis Efficiency Map

Directory of Open Access Journals (Sweden)

Katarzyna Witek

2018-02-01

Full Text Available The influences of the processing parameters on the Mg2FeH6 synthesis yield were studied. Mixtures of magnesium hydride (MgH2 and iron (Fe were mechanically milled in a planetary ball mill under argon for 0.5-, 1-, 2- and 3-h periods and subsequently sintered at temperatures from 300–500 ∘ C under hydrogen. The reaction yield, phase content and hydrogen storage properties of the received materials were investigated. The morphologies of the powders after synthesis were studied by SEM. The synthesis effectiveness map was presented. The obtained results prove that synthesis parameters, such as the milling time and synthesis temperature, greatly influence the reaction yield and material properties and show that extended mechanical milling may not be beneficial to the reaction efficiency.

The hemocompatibility of oxidized diamond nanocrystals for biomedical applications.

Science.gov (United States)

Li, Hung-Cheng; Hsieh, Feng-Jen; Chen, Ching-Pin; Chang, Ming-Yao; Hsieh, Patrick C H; Chen, Chia-Chun; Hung, Shain-Un; Wu, Che-Chih; Chang, Huan-Cheng

2013-10-25

Low-dimensional carbon-based nanomaterials have recently received enormous attention for biomedical applications. However, increasing evidence indicates that they are cytotoxic and can cause inflammatory responses in the body. Here, we show that monocrystalline nanodiamonds (NDs) synthesized by high-pressure-high-temperature (HPHT) methods and purified by air oxidation and strong oxidative acid treatments have excellent hemocompatibility with negligible hemolytic and thrombogenic activities. Cell viability assays with human primary endothelial cells suggested that the oxidized HPHT-NDs (dimensions of 35-500 nm) are non-cytotoxic. No significant elevation of the inflammatory cytokine levels of IL-1β and IL-6 was detected in mice after intravenous injection of the nanocrystals in vivo. Using a hindlimb-ischemia mouse model, we demonstrated that 35-nm NDs after covalent conjugation with polyarginine are useful as a drug delivery vehicle of heparin for prolonged anticoagulation treatment. The present study lays a solid foundation for further therapeutic applications of NDs in biomedicine.

Kinetically controlled synthesis of large-scale morphology-tailored silver nanostructures at low temperature

Science.gov (United States)

Zhang, Ling; Zhao, Yuda; Lin, Ziyuan; Gu, Fangyuan; Lau, Shu Ping; Li, Li; Chai, Yang

2015-08-01

Ag nanostructures are widely used in catalysis, energy conversion and chemical sensing. Morphology-tailored synthesis of Ag nanostructures is critical to tune physical and chemical properties. In this study, we develop a method for synthesizing the morphology-tailored Ag nanostructures in aqueous solution at a low temperature (45 °C). With the use of AgCl nanoparticles as the precursor, the growth kinetics of Ag nanostructures can be tuned with the pH value of solution and the concentration of Pd cubes which catalyze the reaction. Ascorbic acid and cetylpyridinium chloride are used as the mild reducing agent and capping agent in aqueous solution, respectively. High-yield Ag nanocubes, nanowires, right triangular bipyramids/cubes with twinned boundaries, and decahedra are successfully produced. Our method opens up a new environmentally-friendly and economical route to synthesize large-scale and morphology-tailored Ag nanostructures, which is significant to the controllable fabrication of Ag nanostructures and fundamental understanding of the growth kinetics.Ag nanostructures are widely used in catalysis, energy conversion and chemical sensing. Morphology-tailored synthesis of Ag nanostructures is critical to tune physical and chemical properties. In this study, we develop a method for synthesizing the morphology-tailored Ag nanostructures in aqueous solution at a low temperature (45 °C). With the use of AgCl nanoparticles as the precursor, the growth kinetics of Ag nanostructures can be tuned with the pH value of solution and the concentration of Pd cubes which catalyze the reaction. Ascorbic acid and cetylpyridinium chloride are used as the mild reducing agent and capping agent in aqueous solution, respectively. High-yield Ag nanocubes, nanowires, right triangular bipyramids/cubes with twinned boundaries, and decahedra are successfully produced. Our method opens up a new environmentally-friendly and economical route to synthesize large-scale and morphology

Enhancement of structural and magnetic properties of M-type hexaferrite permanent magnet based on synthesis temperature

Science.gov (United States)

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.

Single-source-precursor Synthesis and High-temperature Behavior of SiC Ceramics Containing Boron

Science.gov (United States)

Gui, Miaomiao; Fang, Yunhui; Yu, Zhaoju

2014-12-01

In this paper, a hyperbranched polyborocarbosilane (HPBCS) was prepared by a one-pot synthesis with Cl2Si(CH3)CH2Cl, Cl3SiCH2Cl and BCl3 as the starting materials. The obtained HPBCS was characterized by GPC, FT-IR and NMR, and was confirmed to have hyperbranched structures. The thermal property of the resulting HPBCS was investigated by TGA. The ceramic yield of the HPBCS is about 84% and that of the counterpart hyperbranched hydridopolycarbosilane is only 45%, indicating that the introduction of boron into the preceramic polymer significantly improved the ceramic yield. With the polymer-derived ceramic route, the final ceramics were annealed at 1800 °C in argon atmosphere for 2 h in order to characterize the microstructure and to evaluate the high-temperature behavior. The final ceramic microstructure was studied by XRD and SEM, indicating that the introduction of boron dramatically inhibits SiC crystallization. The boron-containing SiC ceramic shows excellent high-temperature behavior against decomposition and crystallization at 1800 °C.

Radiation synthesis of the water-soluble, temperature sensitive polymer, copolymer and study on their properties

International Nuclear Information System (INIS)

Zhai Maolin; Yin Min; Ha Hongfei

1994-01-01

In order to obtain the water-soluble, temperature sensitive polymer and activated copolymer, the radiation polymerization of N-isopropylacrylamide (NIPAAm), radiation copolymerization of NIPAAm and N-acryloxysuccide (NASI) in aqueous solution or in buffer solution (PBS pH = 7.4) have been carried out by γ-rays from 60 Co source at room temperature. The optimum dose range (1-7 kGy), dose rate (>40 Gy/min) and monomer concentration (1%) were chosen through determining the monomer conversion yield and molecular weight (M w = 6.8 x 10 5 ) of product. Synthesis of the reversible linear polymer was performed in tetrahydrofuran (THF) as well. In this way a white powder product could be obtained which possesses of thermally reversible property too, when it was dissolved in water or PBS. The only disadvantages of this method is that the molecular weight of the polymer produced in THF was much lower than that in aqueous solution

Carbon Isotope Systematics in Mineral-Catalyzed Hydrothermal Organic Synthesis Processes at High Temperature and Pressures

Science.gov (United States)

Fu, Qi; Socki, R. A.; Niles, Paul B.

2011-01-01

Observation of methane in the Martian atmosphere has been reported by different detection techniques. Reduction of CO2 and/or CO during serpentization by mineral surface catalyzed Fischer-Tropsch Type (FTT) synthesis may be one possible process responsible for methane generation on Mars. With the evidence a recent study has discovered for serpentinization in deeply buried carbon rich sediments, and more showing extensive water-rock interaction in Martian history, it seems likely that abiotic methane generation via serpentinization reactions may have been common on Mars. Experiments involving mineral-catalyzed hydrothermal organic synthesis processes were conducted at 750 C and 5.5 Kbars. Alkanes, alcohols and carboxylic acids were identified as organic compounds. No "isotopic reversal" of delta C-13 values was observed for alkanes or carboxylic acids, suggesting a different reaction pathway than polymerization. Alcohols were proposed as intermediaries formed on mineral surfaces at experimental conditions. Carbon isotope data were used in this study to unravel the reaction pathways of abiotic formation of organic compounds in hydrothermal systems at high temperatures and pressures. They are instrumental in constraining the origin and evolution history of organic compounds on Mars and other planets.

Calculation of partial molar volume of components in supercritical ammonia synthesis system

Institute of Scientific and Technical Information of China (English)

Cunwen WANG; Chuanbo YU; Wen CHEN; Weiguo WANG; Yuanxin WU; Junfeng ZHANG

2008-01-01

The partial molar volumes of components in supercritical ammonia synthesis system are calculated in detail by the calculation formula of partial molar volume derived from the R-K equation of state under different conditions. The objectives are to comprehend phase beha-vior of components and to provide the theoretic explana-tion and guidance for probing novel processes of ammonia synthesis under supercritical conditions. The conditions of calculation are H2/N2= 3, at a concentra-tion of NH3 in synthesis gas ranging from 2% to 15%, Concentration of medium in supercritical ammonia syn-thesis system ranging from 20% to 50%, temperature ran-ging from 243 K to 699 K and pressure ranging from 0.1 MPa to 187 MPa. The results show that the ammonia synthesis system can reach supercritical state by adding a suitable supercritical medium and then controlling the reaction conditions. It is helpful for the supercritical ammonia synthesis that medium reaches supercritical state under the conditions of the corresponding total pres-sure and components near the normal temperature or near the critical temperature of medium or in the range of tem-perature of industrialized ammonia synthesis.

The Effects of Light and Temperature on Biotin Synthesis in Pea Sprouts.

Science.gov (United States)

Kamiyama, Shin; Ohnuki, Risa; Moriki, Aoi; Abe, Megumi; Ishiguro, Mariko; Sone, Hideyuki

2016-01-01

Biotin is an essential micronutrient, and is a cofactor for several carboxylases that are involved in the metabolism of glucose, fatty acids, and amino acids. Because plant cells can synthesize their own biotin, a wide variety of plant-based foods contains significant amounts of biotin; however, the influence of environmental conditions on the biotin content in plants remains largely unclear. In the present study, we investigated the effects of different cultivation conditions on the biotin content and biotin synthesis in pea sprouts (Pisum sativum). In the experiment, the pea sprouts were removed from their cotyledons and cultivated by hydroponics under five different lighting and temperature conditions (control [25ºC, 12-h light/12-h dark cycle], low light [25ºC, 4-h light/20-h dark cycle], dark [25ºC, 24 h dark], low temperature [12ºC, 12-h light/12-h dark cycle], and cold [6ºC, 12-h light/12-h dark cycle]) for 10 d. Compared to the biotin content of pea sprouts under the control conditions, the biotin contents of pea sprouts under the low-light, dark, and cold conditions had significantly decreased. The dark group showed the lowest biotin content among the groups. Expression of the biotin synthase gene (bio2) was also significantly decreased under the dark and cold conditions compared to the control condition, in a manner similar to that observed for the biotin content. No significant differences in the adenosine triphosphate content were observed among the groups. These results indicate that environmental conditions such as light and temperature modulate the biotin content of pea plant tissues by regulating the expression of biotin synthase.

Tuning the shell thickness-dependent plasmonic absorption of Ag coated Au nanocubes: The effect of synthesis temperature

Energy Technology Data Exchange (ETDEWEB)

Zhu, Jian, E-mail: jianzhusummer@163.com; Zhang, Fan; Chen, Bei-Bei; Li, Jian-Jun; Zhao, Jun-Wu, E-mail: nanoptzhao@163.com

2015-09-15

Graphical abstract: Ag coating leads to great enhancement of SPR absorbance of Au nanocubes, and the Ag coating-dependent non-monotonous SPR shift is greater at lower temperature. - Highlights: • Au nanocubes with more uniform shape can be obtained at lower growth temperature. • Ag coating leads to great enhancement of SPR absorption intensity. • The Ag coating dependent non-monotonous SPR shift is greater at lower temperature. - Abstract: The temperature dependent synthesis and plasmonic optical properties of Ag coated Au nanocubes have been investigated experimentally. It has been found that the Au nanocubes with more uniform morphology and higher yield could be obtained by decreasing the growth temperature. Because of the non-spherical symmetry of the particles shape and the plasmon coupling between Au–Ag interface and outer Ag surface, four absorption peaks at most have been observed. As the Ag coating thickness is increased, the absorbance intensity of these plasmon peaks gets intense greatly, and the absorption peak at longest wavelength blue shifts firstly and then red shifts. The non-monotonous plasmonic shift has been attributed to the competition between the increase of Ag composition and the enlargement of the particle size. What's more, the wavelength region of both blue shift and red shift could also be enhanced by decreasing the temperature.

Tuning the shell thickness-dependent plasmonic absorption of Ag coated Au nanocubes: The effect of synthesis temperature

International Nuclear Information System (INIS)

Zhu, Jian; Zhang, Fan; Chen, Bei-Bei; Li, Jian-Jun; Zhao, Jun-Wu

2015-01-01

Graphical abstract: Ag coating leads to great enhancement of SPR absorbance of Au nanocubes, and the Ag coating-dependent non-monotonous SPR shift is greater at lower temperature. - Highlights: • Au nanocubes with more uniform shape can be obtained at lower growth temperature. • Ag coating leads to great enhancement of SPR absorption intensity. • The Ag coating dependent non-monotonous SPR shift is greater at lower temperature. - Abstract: The temperature dependent synthesis and plasmonic optical properties of Ag coated Au nanocubes have been investigated experimentally. It has been found that the Au nanocubes with more uniform morphology and higher yield could be obtained by decreasing the growth temperature. Because of the non-spherical symmetry of the particles shape and the plasmon coupling between Au–Ag interface and outer Ag surface, four absorption peaks at most have been observed. As the Ag coating thickness is increased, the absorbance intensity of these plasmon peaks gets intense greatly, and the absorption peak at longest wavelength blue shifts firstly and then red shifts. The non-monotonous plasmonic shift has been attributed to the competition between the increase of Ag composition and the enlargement of the particle size. What's more, the wavelength region of both blue shift and red shift could also be enhanced by decreasing the temperature

Radiation synthesis of a water-soluble temperature sensitive polymer, activated copolymer and applications in immobilization of proteins

International Nuclear Information System (INIS)

Zhai Maolin; Ha Hongfei; Wu Jilan

1993-01-01

In this work the radiation polymerization of N-isopropylacrylamide (NIPAAM) in aqueous solutions has been carried out and a water-soluble, temperature sensitive polymer and copolymer were obtained by using γ-rays from Co-60 source at room temperature. We have gained the optimum dose and dose-rate of radiation synthesis of linear polyNIPAAM through determining conversion yield and viscosity. In order to immobilize protein (BSA) and enzyme (HRP) into this water-soluble polymer, we prepared an activated copolymer, poly(N-isopropylacrylamide-co-N-acryloxysuccinimide). The BSA and HRP has been immobilized onto the activated copolymer. The BSA (HRP)/copolymer conjugates still kept the original thermally sensitive properties of the linear polyNIPAAM. The conjugation yield of BSA to the activated copolymer decreased with increasing dose. Immobilized HRP was stable at 0 o C for a long time and has, at least, 4 days stability at room temperature. Immobilized HRP activity was lowered when the temperature was raised. This phenomenon was reversible and the immobilized HRP regained activity. The optimum pH of the immobilized HRP shifted from ca.5 upward to ca. 7. (author)

Low temperature synthesis of carbon encapsulated Fe7S8 nanocrystals as high performance anode for lithium-ion batteries

International Nuclear Information System (INIS)

Liu, Boyang; Zhang, Fuhua; Wu, Qianlin; Wang, Junhua; Li, Wenge; Dong, Lihua; Yin, Yansheng

2015-01-01

A novel method is developed for low temperature synthesis of carbon encapsulated spherical Fe 7 S 8 nanocrystals with core–shell structure (Fe 7 S 8 @C) by the reaction of ferrocene with ammonium persulphate. The phase structure, morphology, specific surface area and composition of the nanocomposite are systematically characterized. It is found that the Fe 7 S 8 nanocrystals with a weight percent of 33.5% have a median size of 25.2 nm. The Fe 7 S 8 @C electrodes retain a reversible capacity of 815 and 539 mAh g −1 after 50 cycles at a current density of 200 and 2284 mA g −1 , respectively. The high capacity, good cycling behavior and rate capability of Fe 7 S 8 @C electrodes are attributed to the good protection and electrical conductivity of carbon shell. - Highlights: • Large scale and low temperature synthesis of Fe 7 S 8 @C with core–shell structure. • The Fe 7 S 8 @C electrodes retain a capacity of 815 mAh g −1 after 50 cycles at 200 mA g −1 . • The Fe 7 S 8 @C electrodes show good cycling behavior and rate capability

Influence of temperature and precursor concentration on the synthesis of HDA-capped Ag{sub 2}Se nanoparticles

Energy Technology Data Exchange (ETDEWEB)

Mlambo, M. [Department of Chemistry, Vaal University of Technology, Private Bag X021, Vanderbijlpark 1900 (South Africa); Molecular Science Institute, School of Chemistry, University of the Witwatersrand, Private Bag 3, Wits 2050 (South Africa); Moloto, M.J., E-mail: makwenam@vut.ac.za [Department of Chemistry, Vaal University of Technology, Private Bag X021, Vanderbijlpark 1900 (South Africa); Moloto, N. [Molecular Science Institute, School of Chemistry, University of the Witwatersrand, Private Bag 3, Wits 2050 (South Africa); Mdluli, P.S. [Nanotechnology Innovation Centre, Advanced Materials Division, Mintek, Private Bag X3015, Randburg 2125 (South Africa)

2013-06-01

Graphical abstract: The temperature effect on the growth and size of silver selenide nanoparticles with the size distribution and XRD patterns. Highlights: ► The HDA-capped Ag{sub 2}Se nanoparticles were synthesized via the colloidal route. ► Temperature and monomer concentration of the reaction were varied. ► The concentration as a factor influenced particles with a decrease observed as the amount of Ag{sup +} ion source is increased. ► Temperature has expected influence on the growth of particles resulting in increase as the temperature is increased. ► TEM images shows spherical particles and their orthorhombic phase from structural analysis by XRD. - Abstract: The size dependent of temperature and precursor concentration on the synthesis of hexadecylamine capped Ag{sub 2}Se nanoparticles via the colloidal route were studied using the combination of optical and structural analysis. The as-prepared Ag{sub 2}Se nanoparticles showed the quantum confinement with all the obtained absorption band edges blue-shifted from the bulk and their corresponding emission maxima displaying a red-shift from band edges characterised by UV–vis absorption and photoluminescence spectroscopy. The particle sizes were obtained from transmission electron microscopy analysis. The increase in precursor concentration resulted in a decrease in nanoparticle sizes. The increase in reaction temperature showed an increase in the nanoparticle sizes, when the critical temperature at 160 °C was reached, the nanoparticle sizes decreased.

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

International Nuclear Information System (INIS)

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

2014-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

Wijesinghe, W.P.S.L.; Mantilaka, M.M.M.G.P.G. [Department of Chemistry, Faculty of Science, University of Peradeniya, Peradeniya 20400 (Sri Lanka); Post-graduate Institute of Science, P.O. Box: 25, University of Peradeniya, Peradeniya 20400 (Sri Lanka); Premalal, E.V.A. [Department of Materials Science, Shizuoka University, Johoku, Naka-ku Hamamatsu, 432-8011 (Japan); Herath, H.M.T.U. [Department of Medical Laboratory Science, Faculty of Allied Health Sciences, University of Peradeniya, Peradeniya 20400 (Sri Lanka); Mahalingam, S.; Edirisinghe, M. [Department of Mechanical Engineering, University College London, London WC1E 7JE (United Kingdom); Rajapakse, R.P.V.J. [Department of Veterinary Pathobiology, Faculty of Veterinary, University of Peradeniya, Peradeniya 20400 (Sri Lanka); Rajapakse, R.M.G., E-mail: rmgr@pdn.ac.lk [Department of Chemistry, Faculty of Science, University of Peradeniya, Peradeniya 20400 (Sri Lanka); Post-graduate Institute of Science, P.O. Box: 25, University of Peradeniya, Peradeniya 20400 (Sri Lanka)

2014-09-01

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

Low-temperature synthesis and characterization of helical carbon fibers by one-step chemical vapour deposition

Science.gov (United States)

Jin, Yongzhong; Chen, Jian; Fu, Qingshan; Li, Binghong; Zhang, Huazhi; Gong, Yong

2015-01-01

Helical carbon fibers (HCNFs) were synthesized by one-step chemical vapour deposition using cupric tartrate as a catalyst at temperature below 500 °C. The bound rubber of natural rubber (NR)/HCNFs were also prepared in this study. The results of thermogravimetry-differential scanning calorimetry (TG/DSC) for cupric tartrate nanoparticles show that the transformation of C4H4CuO6 → Cu reaction occurs at ∼250-310 °C. The characterization of scanning electron microscopy (SEM), transmission electron microscope (TEM), X-ray diffraction (XRD) and Raman spectrum for the synthesized products confirms that the synthesis of HCNFs is highly temperature-dependent. The straight fibers with the fiber diameter of 100-400 nm are obtained at 280 °C and HCNFs can be synthesized at higher temperature, with the coil diameter of 0.5-1 μm and fiber diameter of 100-200 nm at 380 °C, and the coil diameter of ∼100 nm and fiber diameter of ∼80 nm at 480 °C. The maximum of the bound-rubber content (37%) can be obtained with the addition of 100 wt.% HCNFs in NR, which indicates that the coiled configuration of HCNFs makes a noticeable contribution to the reinforcement of NR/CB system.

Room temperature synthesis of Ni-based alloy nanoparticles by radiolysis.

Energy Technology Data Exchange (ETDEWEB)

Nenoff, Tina Maria; Berry, Donald T.; Lu, Ping; Leung, Kevin; Provencio, Paula Polyak; Stumpf, Roland Rudolph; Huang, Jian Yu; Zhang, Zhenyuan

2009-09-01

Room temperature radiolysis, density functional theory, and various nanoscale characterization methods were used to synthesize and fully describe Ni-based alloy nanoparticles (NPs) that were synthesized at room temperature. These complementary methods provide a strong basis in understanding and describing metastable phase regimes of alloy NPs whose reaction formation is determined by kinetic rather than thermodynamic reaction processes. Four series of NPs, (Ag-Ni, Pd-Ni, Co-Ni, and W-Ni) were analyzed and characterized by a variety of methods, including UV-vis, TEM/HRTEM, HAADF-STEM and EFTEM mapping. In the first focus of research, AgNi and PdNi were studied. Different ratios of Ag{sub x}- Ni{sub 1-x} alloy NPs and Pd{sub 0.5}- Ni{sub 0.5} alloy NP were prepared using a high dose rate from gamma irradiation. Images from high-angle annular dark-field (HAADF) show that the Ag-Ni NPs are not core-shell structure but are homogeneous alloys in composition. Energy filtered transmission electron microscopy (EFTEM) maps show the homogeneity of the metals in each alloy NP. Of particular interest are the normally immiscible Ag-Ni NPs. All evidence confirmed that homogeneous Ag-Ni and Pd-Ni alloy NPs presented here were successfully synthesized by high dose rate radiolytic methodology. A mechanism is provided to explain the homogeneous formation of the alloy NPs. Furthermore, studies of Pd-Ni NPs by in situ TEM (with heated stage) shows the ability to sinter these NPs at temperatures below 800 C. In the second set of work, CoNi and WNi superalloy NPs were attempted at 50/50 concentration ratios using high dose rates from gamma irradiation. Preliminary results on synthesis and characterization have been completed and are presented. As with the earlier alloy NPs, no evidence of core-shell NP formation occurs. Microscopy results seem to indicate alloying occurred with the CoNi alloys. However, there appears to be incomplete reduction of the Na{sub 2}WO{sub 4} to form the W

A Peltier thermal cycling unit for radiopharmaceutical synthesis

International Nuclear Information System (INIS)

McKinney, C.J.; Nader, M.W.

2001-01-01

We have investigated the use of Peltier devices to rapidly cycle the temperature of reaction vessels in a radiopharmaceutical synthesis system. Peltier devices have the advantage that they can be actively cooled as well as heated, allowing precise and rapid control of vessel temperatures. Reaction vessel temperatures of between -6 deg. C and 110 deg. C have been obtained with commercially available devices with reasonable cycle times. Two devices have been used as the basis for a general purpose, two-pot synthesis system for production of [ 11 C] compounds such as raclopride

Cuprous Oxide Scale up: Gram Production via Bulk Synthesis using Classic Solvents at Low Temperatures

Energy Technology Data Exchange (ETDEWEB)

Hall, A. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Han, T. Y. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States)

2015-05-07

Cuprous oxide is a p-type semiconducting material that has been highly researched for its interesting properties. Many small-scale syntheses have exhibited excellent control over size and morphology. As the demand for cuprous oxide grows, the synthesis method need to evolve to facilitate large-scale production. This paper supplies a facile bulk synthesis method for Cu₂O on average, 1-liter reaction volume can produce 1 gram of particles. In order to study the shape and size control mechanisms on such a scale, the reaction volume was diminished to 250 mL producing on average 0.3 grams of nanoparticles per batch. Well-shaped nanoparticles have been synthesized using an aqueous solution of CuCl₂, NaOH, SDS surfactant, and NH₂OH-HCl at mild temperatures. The time allotted between the addition of NaOH and NH₂OH-HCl was determined to be critical for Cu(OH)2 production, an important precursor to the final produce The effects of stirring rates on a large scale was also analyzed during reagent addition and post reagent addition. A morphological change from rhombic dodecahedra to spheres occurred as the stirring speed was increased. The effects of NH₂OH-HCl concentration were also studied to control the etching effects of the final product.

Problems of synthesis and thermal treatment of bismuth-strontium-calcium superconducting cuprates

International Nuclear Information System (INIS)

Tret'yakov, Yu.D.; Os'kina, T.E.; Putlyaev, V.I.

1990-01-01

The results, which have recently appeared in literature on synthesis and high-temperature treatment of Bi-Sr-Ca superconducting cuprates, are generalized. The review will contribute to the overcoming of experimental difficulties in the process of synthesis of monophase superconducting materials with a high transition temperature T c , including optimization of cation composition and heat treatment regime. Radional selection of synthesis conditions (component ratio, temperature, time, reactive area geometry, medium, cooling) was realized, taking into account the newest achievements in crystallochemistry of the phases

Lactobacillusassisted synthesis of titanium nanoparticles

Directory of Open Access Journals (Sweden)

Jha Anal

2007-01-01

Full Text Available AbstractAn eco-friendlylactobacillussp. (microbe assisted synthesis of titanium nanoparticles is reported. The synthesis is performed at room temperature. X-ray and transmission electron microscopy analyses are performed to ascertain the formation of Ti nanoparticles. Individual nanoparticles as well as a number of aggregates almost spherical in shape having a size of 40–60 nm are found.

Modified Two-Step Dimethyl Ether (DME Synthesis Simulation from Indonesian Brown Coal

Directory of Open Access Journals (Sweden)

Dwiwahju Sasongko

2016-08-01

Full Text Available A theoretical study was conducted to investigate the performance of dimethyl ether (DME synthesis from coal. This paper presents a model for two-step DME synthesis from brown coal represented by the following processes: drying, gasification, water-gas reaction, acid gas removal, and DME synthesis reactions. The results of the simulation suggest that a feedstock ratio of coal : oxygen : steam of 1 : 0.13 : 0.821 produces the highest DME concentration. The water-gas reactor simulation at a temperature of 400°C and a pressure of 20 bar gave the ratio of H2/CO closest to 2, the optimal value for two-step DME synthesis. As for the DME synthesis reactor simulation, high pressure and low temperature promote a high DME concentration. It is predicted that a temperature of 300°C and a pressure of 140 bar are the optimum conditions for the DME synthesis reaction. This study also showed that the DME concentration produced by the two-step route is higher than that produced by one-step DME synthesis, implying that further improvement and research are needed to apply two-step DME synthesis to production of this liquid fuel.

Direct synthesis of BiCuChO-type oxychalcogenides by mechanical alloying

Energy Technology Data Exchange (ETDEWEB)

Pele, Vincent; Barreteau, Celine [Institut de Chimie Moléculaire et des Matériaux d’Orsay, Univ. Paris-Sud, UMR 8182, Orsay F-91405 (France); CNRS, Orsay F-91405 (France); Berardan, David, E-mail: david.berardan@u-psud.fr [Institut de Chimie Moléculaire et des Matériaux d’Orsay, Univ. Paris-Sud, UMR 8182, Orsay F-91405 (France); CNRS, Orsay F-91405 (France); Zhao, Lidong; Dragoe, Nita [Institut de Chimie Moléculaire et des Matériaux d’Orsay, Univ. Paris-Sud, UMR 8182, Orsay F-91405 (France); CNRS, Orsay F-91405 (France)

2013-07-15

We report on the direct synthesis of BiCuChO based materials by mechanical alloying (Ch=Se, Te). We show that contrary to the synthesis paths used in the previous reports dealing with this family of materials, which use costly annealings in closed silica tubes under controlled atmosphere, this new synthesis route enables the synthesis of pure phase materials at room temperature under air, with reasonable milling time. This synthesis procedure is easily scalable for large scale applications. - Highlights: • Phase pure BiCuSeO doped and undoped prepared by mechanical alloying. • Synthesis performed under air at room temperature. • Electrical properties similar to that of samples synthesized by a classical path.

Synthesis and high temperature stability of amorphous Si(B)CN-MWCNT composite nanowires

Science.gov (United States)

Bhandavat, Romil; Singh, Gurpreet

2012-02-01

We demonstrate synthesis of a hybrid nanowire structure consisting of an amorphous polymer-derived silicon boron-carbonitride (Si-B-C-N) shell with a multiwalled carbon nanotube core. This was achieved through a novel process involving preparation of a boron-modified liquid polymeric precursor through a reaction of trimethyl borate and polyureasilazane under atmospheric conditions; followed by conversion of polymer to glass-ceramic on carbon nanotube surfaces through controlled heating. Chemical structure of the polymer was studied by liquid-NMR while evolution of various ceramic phases was studied by Raman spectroscopy, solid-NMR, Fourier transform infrared and X-ray photoelectron spectroscopy. Electron microscopy and X-ray diffraction confirms presence of amorphous Si(B)CN coating on individual nanotubes for all specimen processed below 1400 degree C. Thermogravimetric analysis, followed by TEM revealed high temperature stability of the carbon nanotube core in flowing air up to 1300 degree C.

Room Temperature Co-Precipitation Synthesis of Magnetite Nanoparticles in a Large pH Window with Different Bases.

Science.gov (United States)

Mascolo, Maria Cristina; Pei, Yongbing; Ring, Terry A

2013-11-28

Magnetite nanoparticles (Fe₃O₄) represent the most promising materials in medical applications. To favor high-drug or enzyme loading on the nanoparticles, they are incorporated into mesoporous materials to form a hybrid support with the consequent reduction of magnetization saturation. The direct synthesis of mesoporous structures appears to be of interest. To this end, magnetite nanoparticles have been synthesized using a one pot co-precipitation reaction at room temperature in the presence of different bases, such as NaOH, KOH or (C₂H₅)₄NOH. Magnetite shows characteristics of superparamagnetism at room temperature and a saturation magnetization (Ms) value depending on both the crystal size and the degree of agglomeration of individual nanoparticles. Such agglomeration appears to be responsible for the formation of mesoporous structures, which are affected by the pH, the nature of alkali, the slow or fast addition of alkaline solution and the drying modality of synthesized powders.

An Efficient Protocol for the Synthesis of Quinoxaline Derivatives at Room Temperature Using Recyclable Alumina-Supported Heteropolyoxometalates

Directory of Open Access Journals (Sweden)

Diego M. Ruiz

2012-01-01

Full Text Available We report a suitable quinoxaline synthesis using molybdophosphovanadates supported on commercial alumina cylinders as catalysts. These catalysts were prepared by incipient wetness impregnation. The catalytic test was performed under different reaction conditions in order to know the performance of the synthesized catalysts. The method shows high yields of quinoxaline derivatives under heterogeneous conditions. Quinoxaline formation was obtained using benzyl, o-phenylenediamine, and toluene as reaction solvent at room temperature. The CuH2PMo11VO40 supported on alumina showed higher activity in the tested reaction. Finally, various quinoxalines were prepared under mild conditions and with excellent yields.

Novel Green Synthesis and Characterization of Nanopolymer ...

African Journals Online (AJOL)

Purpose: To develop a novel approach to green synthesis of nano-polymer porous gold oxide nanoparticles, and examine the effects of the temperatures on their surface. Methods: Green synthesis of nano-polymer porous gold oxide nanoparticles (GONPs) using cetyle trimethylammonium bromide (CTAB) surfactant with a ...

Application of Multiphysics Coupling FEM on Open Wellbore Shrinkage and Casing Remaining Strength in an Incomplete Borehole in Deep Salt Formation

OpenAIRE

Tong, Hua; Guo, Daqiang; Zhu, Xiaohua

2015-01-01

Drilling and completing wells in deep salt stratum are technically challenging and costing, as when serving in an incomplete borehole in deep salt formation, well casing runs a high risk of collapse. To quantitatively calculate casing remaining strength under this harsh condition, a three-dimensional mechanical model is developed; then a computational model coupled with interbed salt rock-defective cement-casing and HPHT (high pressure and high temperature) is established and analyzed using m...

New efficient catalyst for ammonia synthesis: barium-promoted cobalt on carbon

DEFF Research Database (Denmark)

Hagen, Stefan; Barfod, Rasmus; Fehrmann, Rasmus

2002-01-01

Barium-promoted cobalt catalysts supported on carbon exhibit higher ammonia activities at synthesis temperatures than the commercial, multipromoted iron catalyst and also a lower ammonia......Barium-promoted cobalt catalysts supported on carbon exhibit higher ammonia activities at synthesis temperatures than the commercial, multipromoted iron catalyst and also a lower ammonia...

Self-assembled 3D zinc borate florets via surfactant assisted synthesis under moderate pressures: Process temperature dependent morphology study

Science.gov (United States)

Mahajan, Dhiraj S.; Deshpande, Tushar; Bari, Mahendra L.; Patil, Ujwal D.; Narkhede, Jitendra S.

2018-04-01

In the present study, we prepared zinc borates using aqueous phase synthesis under moderate pressures (MP) (ethanol as a co-solvent in the presence of a quaternary ammonium surfactant-Cetyltrimethylammonium bromide (CTAB). 3D morphologies of self-assembled zinc borate (Zn(H2O)B2O4 · 0.12 H2O, Zn3B6O12 · 3.5H2O, ZnB2O4) resembling flower-like structures were obtained by varying temperature under moderate pressure conditions. Synthesized zinc borates’ florets were morphologically characterized by Field Emission Scanning Electron Microscopy. The x-ray diffractions of borate species reveal rhombohydra, monoclinic and cubic phases of zinc borate crystals as a function of process temperature. Additionally, thermal analysis confirms excellent dehydration/degradation behavior for the zinc borate crystals synthesized at moderate pressures and elevated temperatures and could be utilized as potential flame retardant fillers in the polymer matrices.

FeCl3/Egg shell: An Effective Catalytic System for the Synthesis of 2,3-Dihydroquinazolin-4(1H)-ones at Room Temperature

OpenAIRE

Zakaria Benzekri; Houda Serrar; Said Boukhris; Abdelaziz Souizi

2017-01-01

The FeCl3/eggshell has been a new and efficient catalyst for the rapid and simple synthesis of 2,3-dihydroquinazolin-4-ones in ethanol at room temperature. The present method has advantages of low cost, mild reaction conditions, simple workup process, better recovery and reusability of catalyst, excellent yields and environmentally friendly procedure.

Influence of air annealing on the luminescence dynamics of HPHT nanodiamonds

Czech Academy of Sciences Publication Activity Database

Salava, J.; Trojánek, F.; Stehlík, Štěpán; Varga, Marián; Rezek, Bohuslav; Malý, P.

2016-01-01

Roč. 68, Sep (2016), s. 62-65 ISSN 0925-9635 R&D Projects: GA ČR GA15-01809S Institutional support: RVO:68378271 Keywords : nanodiamond * time-resolved spectroscopy * annealing * carrier dynamics * high-pressure high-temperature nanodiamonds Subject RIV: BH - Optics, Masers, Lasers Impact factor: 2.561, year: 2016

Product engineering by high-temperature flame synthesis

DEFF Research Database (Denmark)

Johannessen, Tue; Johansen, Johnny; Mosleh, Majid

product gas can be applied directly in additional product engineering concepts. A brief overview of on-going product developments and product engineering projects is outlined below. These projects, which are all founded on flame synthesis of nano-structured materials, include: • Preparation of catalyzed...... hardware by direct deposition of catalysts on process equipment • Modifications of the substrate surfaces to obtain good adhesion during flame-coating • Formation of membrane layers by gas-phase deposition of nano-particles • Catalyst deposition in micro-reactors for rapid catalyst screening...

Method and apparatus for producing synthesis gas

Science.gov (United States)

Hemmings, John William; Bonnell, Leo; Robinson, Earl T.

2010-03-03

A method and apparatus for reacting a hydrocarbon containing feed stream by steam methane reforming reactions to form a synthesis gas. The hydrocarbon containing feed is reacted within a reactor having stages in which the final stage from which a synthesis gas is discharged incorporates expensive high temperature materials such as oxide dispersed strengthened metals while upstream stages operate at a lower temperature allowing the use of more conventional high temperature alloys. Each of the reactor stages incorporate reactor elements having one or more separation zones to separate oxygen from an oxygen containing feed to support combustion of a fuel within adjacent combustion zones, thereby to generate heat to support the endothermic steam methane reforming reactions.

Immobilization of simulated radioactive soil waste containing cerium by self-propagating high-temperature synthesis

International Nuclear Information System (INIS)

Mao, Xianhe; Qin, Zhigui; Yuan, Xiaoning; Wang, Chunming; Cai, Xinan; Zhao, Weixia; Zhao, Kang; Yang, Ping; Fan, Xiaoling

2013-01-01

A simulated radioactive soil waste containing cerium as an imitator element has been immobilized by a thermite self-propagating high-temperature synthesis (SHS) process. The compositions, structures, and element leaching rates of products with different cerium contents have been characterized. To investigate the influence of iron on the chemical stability of the immobilized products, leaching tests of samples with different iron contents with different leaching solutions were carried out. The results showed that the imitator element cerium mainly forms the crystalline phases CeAl 11 O 18 and Ce 2 SiO 5 . The leaching rate of cerium over a period of 28 days was 10 −5 –10 −6 g/(m 2 day). Iron in the reactants, the reaction products, and the environment has no significant effect on the chemical stability of the immobilized SHS products

Immobilization of simulated radioactive soil waste containing cerium by self-propagating high-temperature synthesis

Science.gov (United States)

Mao, Xianhe; Qin, Zhigui; Yuan, Xiaoning; Wang, Chunming; Cai, Xinan; Zhao, Weixia; Zhao, Kang; Yang, Ping; Fan, Xiaoling

2013-11-01

A simulated radioactive soil waste containing cerium as an imitator element has been immobilized by a thermite self-propagating high-temperature synthesis (SHS) process. The compositions, structures, and element leaching rates of products with different cerium contents have been characterized. To investigate the influence of iron on the chemical stability of the immobilized products, leaching tests of samples with different iron contents with different leaching solutions were carried out. The results showed that the imitator element cerium mainly forms the crystalline phases CeAl11O18 and Ce2SiO5. The leaching rate of cerium over a period of 28 days was 10-5-10-6 g/(m2 day). Iron in the reactants, the reaction products, and the environment has no significant effect on the chemical stability of the immobilized SHS products.

Modelling of flame temperature of solution combustion synthesis of ...

Indian Academy of Sciences (India)

Administrator

The basis of combustion synthesis technique comes from the ... of oxidizer to fuel is calculated using the total oxidizing ..... +. −. ∑. (4) where S/Nm is the mean S/N ratio of all the experimental ..... Minitab Inc., User manual of MINITAB. TM.

Two luminescent frameworks constructed from lead(II) salts with carboxylate ligands containing dinuclear lead(II) units

International Nuclear Information System (INIS)

Zhu Xiandong; Li Xiaoju; Liu Qingyan; Lue Jian; Guo Zhengang; He Jinrun; Li Yafeng; Cao Rong

2007-01-01

Two luminescent Pb(II) coordination frameworks containing dinuclear lead(II) units, [Pb(PYDC)(H 2 O)] n (1) and [Pb(HPHT)] n (2) have been prepared by the self-assembly of lead(II) salts with pyridinecarboxylate and benzenecarboxylate. Single-crystal X-ray diffraction analyses reveal that compound 1 is a three-dimensional architecture consisting of Pb 2 O 2 dimeric building units, whereas compound 2 is a two-dimensional layer structure containing one-dimensional lead-oxide chains. The luminescent properties of 1 and 2 have been investigated in the solid state at room temperature, indicating structure-dependent photoluminescent properties of the coordination frameworks. - Graphical abstract: Two luminescent Pb(II) coordination frameworks, [Pb(PYDC)(H 2 O)] n (1) and [Pb(HPHT)] n (2) have been prepared. Single-crystal analyses reveal that compound 1 is a three-dimensional architecture consisting of Pb 2 O 2 dimeric building units, whereas compound 2 is a two-dimensional layer structure containing one-dimensional lead-oxide chains. The luminescent properties have been investigated, indicating structure-dependent photoluminescent properties of the coordination frameworks

Ionothermal synthesis of β-NH4AlF4 and the determination by single crystal X-ray diffraction of its room temperature and low temperature phases

International Nuclear Information System (INIS)

Parnham, Emily R.; Slawin, Alex M.Z.; Morris, Russell E.

2007-01-01

β-NH 4 AlF 4 has been synthesised ionothermally using 1-ethyl-3-methylimidazolium hexafluorophosphate as solvent and template provider. β-NH 4 AlF 4 crystals were produced which were suitable for single crystal X-ray diffraction analysis. A phase transition occurs between room temperature (298 K) and low temperature (93 K) data collections. At 298 K the space group=I4/mcm (no. 140), α=11.642(5), c=12.661(5) A, Z=2 (10NH 4 AlF 4 ), wR(F 2 )=0.1278, R(F)=0.0453. At 93 K the space group=P4 2 /ncm (no. 138), α=11.616(3), c=12.677(3) A, Z=2 (10NH 4 AlF 4 ), wR(F 2 )=0.1387, R(F)=0.0443. The single crystal X-ray diffraction study of β-NH 4 AlF 4 shows the presence of two different polymorphs at low and room temperature, indicative of a phase transition. The [AlF 4/2 F 2 ] - layers are undisturbed except for a small tilting of the AlF 6 octahedra in the c-axis direction. -Ionothermal synthesis, the use of an ionic liquid as the solvent in materials preparation, has been used to prepare β-NH 4 AlF 4 , and structural characterisation indicates that there are two versions of the structure, a low temperature primitive phase at 93 K and a high temperature body-centered phase at 298 K

Solid-State Synthesis and Effect of Temperature on Optical Properties of CuO Nanoparticles

Institute of Scientific and Technical Information of China (English)

C.C.Vidyasagar; Y.Arthoba Naik; T.G.Venkatesha; R.Viswanatha

2012-01-01

Modulation of band energies through size control offers new ways to control photoresponse and photoconversion efficiency of the solar cell. The P-type semiconductor of copper oxide is an important functional material used for photovoltaic cells. Cu O is attractive as a selective solar absorber since it has high solar absorbance and a low thermal emittance. The present work describes the synthesis and characterization of semiconducting Cu O nanoparticles via one-step, solid-state reaction in the presence of Polyethylene glycol400 as size controlling agent for the preparation of Cu O nanoparticles at different temperatures. Solid-state mechanochemical processing, which is not only a physical size reduction process in conventional milling but also a chemical reaction, is mechanically activated at the nanoscale during grinding. The present method is a simple and efficient method of preparing nanoparticles with high yield at low cost. The structural and chemical composition of the nanoparticles were analyzed by X-ray diffraction, field emission scanning electron microscopy and energy-dispersive spectrometer, respectively. Optical properties and band gap of Cu O nanoparticles were studied by UV-Vis spectroscopy. These results showed that the band gap energy decreased with increase of annealing temperature, which can be attributed to the improvement in grain size of the samples.

Application of self-propagation high-temperature synthesis for immobilization of hard radioactive wastes in ceramet materials

International Nuclear Information System (INIS)

Ilyin, E.; Pashkeev, I.; Senin, A.; Gerasimova, N.

2001-01-01

The possibility of self-propagating high-temperature synthesis (SPHTS) application for an immobilization of solid high level wastes (HLW) in cermet materials is considered. The schemes of multilayer cermet blocks formation are offered. Such blocks consist of a ceramet core with immobilized HLW and a protective cover - ceramet without HLW. The influence of the base components form (pure Ti and Si, ferrotitanium and ferrosilicon), metallic components (Ni, Cu, Cr, Fe, ferrochromium) and nonmetallic components (SiO 2 , Al 2 O 3 , TiO 2 ) on burning rate and cover ceramet structure is investigated in compositions on a basis of Ti+B, Ti+Si, Ti+C systems. Model samples of multilayer cermet blocks are manufactured using of HLW simulators. (authors)

High temperature synthesis of ceramic composition by directed reaction of molten titanium or zirconium with boron carbide

International Nuclear Information System (INIS)

Johnson, W.B.

1990-01-01

Alternative methods of producing ceramics and ceramic composites include sintering, hot pressing and more recently hot isostatic pressing (HIP) and self-propagating high temperature synthesis (SHS). Though each of these techniques has its advantages, each suffers from several restrictions as well. Sintering may require long times at high temperatures and for most materials requires sintering aids to get full density. These additives can, and generally do, change (often degrade) the properties of the ceramic. Hot pressing and hot isostatic pressing are convenient methods to quickly prepare samples of some materials to full density, but generally are expensive and may damage some types of reinforcements during densification. This paper focuses on the preparation and processing of composites prepared by the directed reaction of molten titanium or zirconium with boron carbide. Advantages and disadvantages of this approach when compared to traditional methods are discussed, with reference to specific examples. Examples of microstructure are properties of these materials are reported

Synthesis and Characterization of Si Oxide Coated Nano Ceria by Hydrolysis, and Hydrothermal Treatment at Low Temperature

Directory of Open Access Journals (Sweden)

Kong M.

2017-06-01

Full Text Available The purpose of this work was to the application of Si oxide coatings. This study deals with the preparation of ceria (CeO2 nanoparticles coating with SiO2 by water glass and hydrolysis reaction. First, the low temperature hydro-reactions were carried out at 30~100°C. Second, Silicon oxide-coated Nano compounds were obtained by the catalyzing synthesis. CeO2 Nano-powders have been successfully synthesized by means of the hydrothermal method, in a low temperature range of 100~200°C. In order to investigate the structure and morphology of the Nano-powders, scanning electron microscopy (SEM and X-ray diffraction (XRD were employed. The XRD results revealed the amorphous nature of silica nanoparticles. To analyze the quantity and properties of the compounds coated with Si oxide, transmission electron microscopy (TEM in conjunction with electron dispersive spectroscopy was used. Finally, it is suggested that the simple growth process is more favorable mechanism than the solution/aggregation process.

Room Temperature Co-Precipitation Synthesis of Magnetite Nanoparticles in a Large pH Window with Different Bases

Directory of Open Access Journals (Sweden)

Maria Cristina Mascolo

2013-11-01

Full Text Available Magnetite nanoparticles (Fe3O4 represent the most promising materials in medical applications. To favor high-drug or enzyme loading on the nanoparticles, they are incorporated into mesoporous materials to form a hybrid support with the consequent reduction of magnetization saturation. The direct synthesis of mesoporous structures appears to be of interest. To this end, magnetite nanoparticles have been synthesized using a one pot co-precipitation reaction at room temperature in the presence of different bases, such as NaOH, KOH or (C2H54NOH. Magnetite shows characteristics of superparamagnetism at room temperature and a saturation magnetization (Ms value depending on both the crystal size and the degree of agglomeration of individual nanoparticles. Such agglomeration appears to be responsible for the formation of mesoporous structures, which are affected by the pH, the nature of alkali, the slow or fast addition of alkaline solution and the drying modality of synthesized powders.

Flash pyrolysis at high temperature of ligno-cellulosic biomass and its components - production of synthesis gas

International Nuclear Information System (INIS)

Couhert, C.

2007-11-01

Pyrolysis is the first stage of any thermal treatment of biomass and governs the formation of synthesis gas for the production of electricity, hydrogen or liquid fuels. The objective of this work is to establish a link between the composition of a biomass and its pyrolysis gas. We study experimental flash pyrolysis and fix the conditions in which quantities of gas are maximal, while aiming at a regime without heat and mass transfer limitations (particles about 100 μm): temperature of 950 C and residence time of about 2 s. Then we try to predict gas yields of any biomass according to its composition, applicable in this situation where thermodynamic equilibrium is not reached. We show that an additivity law does not allow correlating gas yields of a biomass with fractions of cellulose, hemi-cellulose and lignin contained in this biomass. Several explanations are suggested and examined: difference of pyrolytic behaviour of the same compound according to the biomass from which it is extracted, interactions between compounds and influence of mineral matter. With the aim of industrial application, we study pyrolysis of millimetric and centimetric size particles, and make a numerical simulation of the reactions of pyrolysis gases reforming. This simulation shows that the choice of biomass affects the quantities of synthesis gas obtained. (author)

Selective recovery of silver from waste low-temperature co-fired ceramic and valorization through silver nanoparticle synthesis.

Science.gov (United States)

Swain, Basudev; Shin, Dongyoon; Joo, So Yeong; Ahn, Nak Kyoon; Lee, Chan Gi; Yoon, Jin-Ho

2017-11-01

Considering the value of silver metal and silver nanoparticles, the waste generated during manufacturing of low temperature co-fired ceramic (LTCC) were recycled through the simple yet cost effective process by chemical-metallurgy. Followed by leaching optimization, silver was selectively recovered through precipitation. The precipitated silver chloride was valorized though silver nanoparticle synthesis by a simple one-pot greener synthesis route. Through leaching-precipitation optimization, quantitative selective recovery of silver chloride was achieved, followed by homogeneous pure silver nanoparticle about 100nm size were synthesized. The reported recycling process is a simple process, versatile, easy to implement, requires minimum facilities and no specialty chemicals, through which semiconductor manufacturing industry can treat the waste generated during manufacturing of LTCC and reutilize the valorized silver nanoparticles in manufacturing in a close loop process. Our reported process can address issues like; (i) waste disposal, as well as value-added silver recovery, (ii) brings back the material to production stream and address the circular economy, and (iii) can be part of lower the futuristic carbon economy and cradle-to-cradle technology management, simultaneously. Copyright © 2017 Elsevier Ltd. All rights reserved.

Simple and Efficient Generation of Aryl Radicals from Aryl Triflates: Synthesis of Aryl Boronates and Aryl Iodides at Room Temperature.

Science.gov (United States)

Liu, Wenbo; Yang, Xiaobo; Gao, Yang; Li, Chao-Jun

2017-06-28

Despite the wide use of aryl radicals in organic synthesis, current methods to prepare them from aryl halides, carboxylic acids, boronic acids, and diazonium salts suffer from limitations. Aryl triflates, easily obtained from phenols, are promising aryl radical progenitors but remain elusive in this regard. Inspired by the single electron transfer process for aryl halides to access aryl radicals, we developed a simple and efficient protocol to convert aryl triflates to aryl radicals. Our success lies in exploiting sodium iodide as the soft electron donor assisted by light. This strategy enables the scalable synthesis of two types of important organic molecules, i.e., aryl boronates and aryl iodides, in good to high yields, with broad functional group compatibility in a transition-metal-free manner at room temperature. This protocol is anticipated to find potential applications in other aryl-radical-involved reactions by using aryl triflates as aryl radical precursors.

Ribulose 1,5-bisphosphate carboxylase synthesis during heat shock

International Nuclear Information System (INIS)

Vierling, E.; Key, J.L.

1985-01-01

Ribulose 1,5-bisphosphate carboxylase (RuBPCase) was chosen as a model protein to study how heat shock (HS) affects both chloroplast protein synthesis and the nuclear-chloroplast interaction in production of chloroplast proteins. Experiments were performed using highly chlorophyllous, soybean (Glycine max L. Merr. var Corsoy) cell suspension cultures active in chloroplast protein synthesis. Synthesis of RuBPCase large (L) and small (S) subunits was followed by in vivo labeling, and corresponding mRNA levels were examined by Northern and dot hybridization analyses. Results demonstrate that L and S synthesis declines with increasing HS temperatures (33-40 0 C) and reaches minimum levels (20-30% of control) at temperatures of maximum HS protein synthesis (39-40 0 C). Recovery of L and S synthesis following a 2-hour HS at 38 or 40 0 C was also studied. The changes in S synthesis during HS and recovery correlate with the steady state levels of S mRNA. In contrast, changes in L synthesis show little relationship to the corresponding mRNA levels; levels of L mRNA remain relatively unchanged by HS. The authors conclude that chloroplast protein synthesis shows no greater sensitivity to HS than is observed for cytoplasmic protein synthesis and that transport of proteins into the chloroplast (e.g.,S subunit) continues during HS. Furthermore, there is no apparent coordination of L and S subunit mNRA levels under the conditions examined

Low-temperature synthesis of Li{sub 7}La{sub 3}Zr{sub 2}O{sub 12} with cubic garnet-type structure

Energy Technology Data Exchange (ETDEWEB)

Xie, Hui [Texas Materials Institute, ETC 9.184, University of Texas at Austin, Austin, TX 78712 (United States); Li, Yutao [Texas Materials Institute, ETC 9.184, University of Texas at Austin, Austin, TX 78712 (United States); State Key Laboratory of New Ceramics and Fine Processing, Department of Materials Science and Engineering, Tsinghua University, Beijing 100084 (China); Goodenough, John B., E-mail: jgoodenough@mail.utexas.edu [Texas Materials Institute, ETC 9.184, University of Texas at Austin, Austin, TX 78712 (United States)

2012-05-15

Highlights: Black-Right-Pointing-Pointer One-step synthesis and its optimization of cubic garnet Li{sub 7}La{sub 3}Zr{sub 2}O{sub 12} at 750 Degree-Sign C. Black-Right-Pointing-Pointer Instability above 800 Degree-Sign C of the Al-free cubic Li{sub 7}La{sub 3}Zr{sub 2}O{sub 12}. Black-Right-Pointing-Pointer Li{sup +}-ion conductivity without adventitious Al{sup 3+}. -- Abstract: In this paper, we report the direct synthesis of Li{sub 7}La{sub 3}Zr{sub 2}O{sub 12} with the cubic garnet-type structure at low temperature with a lattice constant of 13.0035 Angstrom-Sign . The synthesis condition is optimized to be at 750 Degree-Sign C for 8 h with 30 wt% excess lithium salt. No intermediate grinding was involved in this straightforward route. Without the adventitious of Al{sup 3+}, the cubic Li{sub 7}La{sub 3}Zr{sub 2}O{sub 12} is unstable above 800 Degree-Sign C and has an ionic conductivity of the order of 10{sup -6} S cm{sup -1}.

Al2O3 - TiO2-A simple sol-gel strategy to the synthesis of low temperature sintered alumina-aluminium titanate composites through a core-shell approach

International Nuclear Information System (INIS)

Jayasankar, M.; Ananthakumar, S.; Mukundan, P.; Wunderlich, W.; Warrier, K.G.K.

2008-01-01

A simple sol-gel based core-shell approach for the synthesis of alumina-aluminium titanate composite is reported. Alumina is the core and titania is the shell. The coating of titania has been performed in aqueous medium on alumina particle by means of heterocoagulation of titanyl chloride. Further heat treatment results in low temperature formation of aluminium titanate as well as low temperature sintering of alumina-aluminium titanate composites. The lowering of the reaction temperature can be attributed to the maximisation of the contact surface between the reactants due to the core-shell approach involving nanoparticles. The mechanism of formation of aluminium titanate and the observations on densification features in the present process are compared with that of mixture of oxides under identical conditions. The sintered alumina-aluminium titanate composite has an average grain size of 2 μm. - Graphical abstract: The article presents a simple sol-gel process through core-shell approach to the synthesis of low temperature sintered alumina-aluminium titanate. The lowering of the reaction temperature can be attributed to the maximisation of the contact surface between the reactant due to the core-shell approach. This material showed the better microstructure control compared to the standard solid-state mixing route

Influence of the temperature on the synthesis of CdS quantum dots stabilized with poly (vinil alcohol)

International Nuclear Information System (INIS)

Carvalho, Andre L.B. de; Mansur, Alexandra A.P.; Mansur, Herman S.; Gonzalez, Juan C.

2011-01-01

Semiconductor nanoparticles (Quantum Dots, QDs) have been the subject of recent research by presenting quantum properties. This property has stimulated the study of these particles in biological applications such as bookmarks, which creates the necessity of using different synthesis routes resulting in biocompatible systems. Thus, this study aimed to evaluate the effect of temperature on the properties of QDs cadmium sulfide, aqueous route using poly (vinyl alcohol), a biocompatible polymer, such as stabilizing agent. The characterization of particles produced was performed by UV-Vis spectroscopy and photoluminescence (PL) spectra for obtaining the absorption and emission, respectively and Transmission microscopy (TEM) for analysis of the diameter of the nanocrystals. (author)

Cooperation between catalytic and DNA binding domains enhances thermostability and supports DNA synthesis at higher temperatures by thermostable DNA polymerases.

Science.gov (United States)

Pavlov, Andrey R; Pavlova, Nadejda V; Kozyavkin, Sergei A; Slesarev, Alexei I

2012-03-13

We have previously introduced a general kinetic approach for comparative study of processivity, thermostability, and resistance to inhibitors of DNA polymerases [Pavlov, A. R., et al. (2002) Proc. Natl. Acad. Sci. U.S.A.99, 13510-13515]. The proposed method was successfully applied to characterize hybrid DNA polymerases created by fusing catalytic DNA polymerase domains with various sequence-nonspecific DNA binding domains. Here we use the developed kinetic analysis to assess basic parameters of DNA elongation by DNA polymerases and to further study the interdomain interactions in both previously constructed and new chimeric DNA polymerases. We show that connecting helix-hairpin-helix (HhH) domains to catalytic polymerase domains can increase thermostability, not only of DNA polymerases from extremely thermophilic species but also of the enzyme from a faculatative thermophilic bacterium Bacillus stearothermophilus. We also demonstrate that addition of Topo V HhH domains extends efficient DNA synthesis by chimerical polymerases up to 105 °C by maintaining processivity of DNA synthesis at high temperatures. We found that reversible high-temperature structural transitions in DNA polymerases decrease the rates of binding of these enzymes to the templates. Furthermore, activation energies and pre-exponential factors of the Arrhenius equation suggest that the mechanism of electrostatic enhancement of diffusion-controlled association plays a minor role in binding of templates to DNA polymerases.

Cooperation between Catalytic and DNA-binding Domains Enhances Thermostability and Supports DNA Synthesis at Higher Temperatures by Thermostable DNA Polymerases

Science.gov (United States)

Pavlov, Andrey R.; Pavlova, Nadejda V.; Kozyavkin, Sergei A.; Slesarev, Alexei I.

2012-01-01

We have previously introduced a general kinetic approach for comparative study of processivity, thermostability, and resistance to inhibitors of DNA polymerases (Pavlov et. al., (2002) Proc. Natl. Acad. Sci. USA 99, 13510–13515). The proposed method was successfully applied to characterize hybrid DNA polymerases created by fusing catalytic DNA polymerase domains with various non-specific DNA binding domains. Here we use the developed kinetic analysis to assess basic parameters of DNA elongation by DNA polymerases and to further study the interdomain interactions in both previously constructed and new chimeric DNA polymerases. We show that connecting Helix-hairpin-Helix (HhH) domains to catalytic polymerase domains can increase thermostability, not only of DNA polymerases from extremely thermophilic species, but also of the enzyme from a faculatative thermophilic bacterium Bacillus stearothermophilus. We also demonstrate that addition of TopoV HhH domains extends efficient DNA synthesis by chimerical polymerases up to 105°C by maintaining processivity of DNA synthesis at high temperatures. We also found that reversible high-temperature structural transitions in DNA polymerases decrease the rates of binding of these enzymes to the templates. Furthermore, activation energies and pre-exponential factors of the Arrhenius equation suggest that the mechanism of electrostatic enhancement of diffusion-controlled association plays a minor role in binding templates to DNA polymerases. PMID:22320201

Antagonistic effects of high and low temperature pretreatments on the germination and pregermination ethylene synthesis of lettuce seeds.

Science.gov (United States)

Burdett, A N

1972-08-01

Red light-induced germination of Grand Rapids lettuce seeds (Lactuca sativa L.) incubated at 20 C was inhibited if the seeds were first imbibed at 30 C for 36 hours. This effect was counteracted by exogenous ethylene and associated with a reduction in the rate at which the seeds produced ethylene throughout the pregermination period. A chilling treatment reversed the effect of a prior imbibition at 30 C on both germination and ethylene production. The possibility that the pretreatments influence germination through their effects on ethylene production is discussed.Other evidence presented indicates that the inability of seeds to germinate at supraoptimal temperature is not due either to a rapid loss of far red-absorbing phytochrome or to an inadequate capacity for ethylene synthesis. It was also shown that a chilling treatment potentiated germination at high temperature without affecting the ethylene synthetic capacity of the seeds.

Synthesis and thermoelectric properties of Sb{sub 0.20}CoSb{sub 2.80} skutterudite

Energy Technology Data Exchange (ETDEWEB)

Figueirêdo, C.A., E-mail: camila_fig@hotmail.com [Universidade Federal do Rio Grande do Sul, PGCIMAT, Instituto de Física, 91501-970 Porto Alegre, RS (Brazil); Gallas, M.R. [Universidade Federal do Rio Grande do Sul, PGCIMAT, Instituto de Física, 91501-970 Porto Alegre, RS (Brazil); Institute for Multiscale Simulations, Friedrich-Alexander-Universität, Nägelsbachstrasse 49b, 91052 Erlangen (Germany); Zorzi, J.E. [Universidade de Caxias do Sul, Instituto de Materiais Cerâmicos, 95765-000 Bom Princípio, RS (Brazil); Perottoni, C.A. [Universidade Federal do Rio Grande do Sul, PGCIMAT, Instituto de Física, 91501-970 Porto Alegre, RS (Brazil); Universidade de Caxias do Sul, Instituto de Materiais Cerâmicos, 95765-000 Bom Princípio, RS (Brazil)

2014-06-15

Highlights: • A HP-HT Sb{sub 0.20}CoSb{sub 2.80} phase was prepared by processing cobalt antimonide at 7.7 GPa and 550 °C, for (at least) 5 min. • The mechanism of formation of this phase involves (i) decomposition of cobalt antimonide into CoSb{sub 2} and Sb, and (ii) insertion of Sb into the remaining cobalt antimonide. • The mechanism of formation is qualitatively different from that responsible for the formation of the high pressure (greater than 20 GPa) phase. - Abstract: Polycrystalline samples of cobalt antimonide (CoSb{sub 2.79}) were submitted to different conditions of pressure, temperature and processing time, in a high-pressure toroidal-type chamber, aiming to maximize the production of the high pressure phase previously observed in experiments with a diamond anvil cell. Rietveld refinements of X-ray powder diffraction data were performed to determine the phase composition and structural parameters. The maximum yield, 89(2) wt.% of Sb{sub x}CoSb{sub 3−x} phase, was obtained at 7.7 GPa, 550 °C and (at least) 5 min of processing time. The mechanism behind the formation of Sb{sub x}CoSb{sub 3−x} at high pressure and high temperature is actually not the same as that previously inferred from experiments at higher pressures (20 GPa) and room temperature with the diamond anvil cell. Indeed, evidences suggest that, at high pressure and high temperature, Sb{sub x}CoSb{sub 3−x} is formed by insertion of Sb resulting from decomposition of cobalt antimonide. Thermal conductivity, Seebeck coefficient and electrical conductivity were estimated for CoSb{sub 2.79} and Sb{sub 0.20}CoSb{sub 2.80}. The thermoelectric figure of merit at room temperature for Sb{sub 0.20}CoSb{sub 2.80} resulted 33% greater than that for CoSb{sub 2.79}.

Utilization of plasmas for graphene synthesis

Science.gov (United States)

Shashurin, Alexey; Keidar, Michael

2013-10-01

Graphene is a one-atom-thick planar sheet of carbon atoms that are densely packed in a honeycomb crystal lattice. Grapheen has tremendous range of potential applications ranging from high-speed transistors to electrochemical energy storage devices and biochemical sensors. Methods of graphene synthesis include mechanical exfoliation, epitaxial growth on SiC, CVD and colloidal suspensions. In this work the utilization of plasmas in synthesis process is considered. Types of carbonaceous structures produced by the anodic arc and regions of their synthesis were studied. Ultimate role of substrate temperature and transformations occurring with various carbonaceous structures generated in plasma discharge were considered. Formation of graphene film on copper substrate was detected at temperatures around the copper melting point. The film was consisted of several layers graphene flakes having typical sizes of about 200 nm. Time required for crystallization of graphene on externally heated substrates was determined. This work was supported by National Science Foundation (NSF Grant No. CBET-1249213).

Synthesis of POSS-based ionic conductors with low glass transition temperatures for efficient solid-state dye-sensitized solar cells.

Science.gov (United States)

Zhang, Wei; Wang, Zhong-Sheng

2014-07-09

Replacing liquid-state electrolytes with solid-state electrolytes has been proven to be an effective way to improve the durability of dye-sensitized solar cells (DSSCs). We report herein the synthesis of amorphous ionic conductors based on polyhedral oligomeric silsesquioxane (POSS) with low glass transition temperatures for solid-state DSSCs. As the ionic conductor is amorphous and in the elastomeric state at the operating temperature of DSSCs, good pore filling in the TiO2 film and good interfacial contact between the solid-state electrolyte and the TiO2 film can be guaranteed. When the POSS-based ionic conductor containing an allyl group is doped with only iodine as the solid-state electrolyte without any other additives, power conversion efficiency of 6.29% has been achieved with good long-term stability under one-sun soaking for 1000 h.

Optimization of self-propagating high-temperature synthesis using a halogen fluoride as an igniter for reagents

Science.gov (United States)

Gaidar, S. M.; Karelina, M. Yu.; Zhigarev, V. D.

2016-12-01

The minimum quantity of the high-activity chemical reagent (HACR) that is required for the initiation of self-propagating high-temperature synthesis (SHS) is determined. The experimental results show that 1-1.3 mg ClF3 (gravity flow from a dosing device), BrF3 on the end of a filling knife, or a few ClF2 + SbF6 - crystals are sufficient for the initiation of titanium-boron or titanium-carbon high-energy powder charge compositions. Since the quantity of HACR required for SHS initiation is very small, the chemical method of initiation can be used for the development of a mobile ignition device for estimating the ignition of various SHS charge compositions under laboratory conditions and for application in standard reactors.

Controllable synthesis of spindle-like ZnO nanostructures by a simple low-temperature aqueous solution route

International Nuclear Information System (INIS)

Lu Hongxia; Zhao Yunlong; Yu Xiujun; Chen Deliang; Zhang Liwei; Xu Hongliang; Yang Daoyuan; Wang Hailong; Zhang Rui

2011-01-01

Spindle-like ZnO nanostructures were successfully synthesized through direct precipitation of zinc acetate aqueous solution at 60 deg. C. Phase structure, morphology and microstructure of the products were investigated by X-ray diffraction, TG-DTA, FTIR and field emission scanning electron microscopy (FESEM). Result showed that hexagonal wurtzite structure ZnO nanostructures with about 100 nm in diameter and 100-200 nm in length were obtained. HMTA acted as a soft template in the process and played an important role in the formation of spindle-like ZnO nanostructures. Meanwhile, different morphologies were also obtained by altering synthetic temperature, additional agents and the ratios of Zn 2+ /OH - . Possible mechanism for the variations of morphology with synthesis parameters was also discussed in this paper.

Synthesis and studies of Y-Ba-Cu-O high temperature superconductor prepared by sol-gel method

International Nuclear Information System (INIS)

Grigoryan, S.G.; Manukyan, A.L.; Hayrapetyan, A.G.; Arzumanyan, A.M.; Rashidyan, L.H.; Mkrtichyan, N.Y.; Mkrtchyan, A.A.; Kurginyan, K.A.; Trozyan, A.H.; Vardanyan, R.S.

2004-01-01

The method of preparation of Y-Ba-Cu-O high temperature superconducting materials by sol-gel processing technique both for powders and thin films are described. All these methods are based on using yttrium alkoxides as precursors, which are not ready available reagents, besides the majority of these methods use copper alkoxides, which show low solubility in organic solvents, moreover they are very sensitive to hydrolysis in air. The new method of preparation of Y-Ba-Cu-O ceramic materials by sol-gel processing technique based on new and convenient precursors stable in air, having high compatibility with each other is offered. Basic scientific and technological issues related to the synthesis of bulk materials, their structure and electrical conductivity are discussed

Exergy analysis of industrial ammonia synthesis

International Nuclear Information System (INIS)

Kirova-Yordanova, Zornitza

2004-01-01

Exergy consumption of ammonia production plants depends strongly on the ammonia synthesis loop design. Due to the thermodynamically limited low degree of conversion of hydrogen-nitrogen mixture to ammonia, industrial ammonia synthesis is implemented as recycle process (so-called 'ammonia synthesis loop'). Significant quantities of reactants are recycled back to reactor, after the removal of ammonia at low temperatures. Modern ammonia synthesis plants use well-developed heat- and cold recovery to improve the reaction heat utilisation and to reduce the refrigeration costs. In this work, the exergy method is applied to estimate the effect of the most important process parameters on the exergy efficiency of industrial ammonia synthesis. A specific approach, including suitable definitions of the system boundaries and process parameters, is proposed. Exergy efficiency indexes are discussed in order to make the results applicable to ammonia synthesis loops of various designs. The dependence of the exergy losses on properly selected independent process parameters is studied. Some results from detailed exergy analysis of the most commonly used ammonia synthesis loop design configurations at a wide range of selected parameters values are shown

Synthesis of type A zeolite from calcinated kaolin

International Nuclear Information System (INIS)

Rodrigues, E.C.; Neves, R.F.; Souza, J.A.S.; Moraes, C.G.; Macedo, E.N.

2011-01-01

The mineral production has caused great concern in environmental and industrial scenario due to the effects caused to the environment. The industries of processing kaolin for paper are important economically for the state of Para, but produce huge quantities of tailings, which depend on large areas to be stocked. This material is rich in silico-aluminates can be recycled and used as raw material for other industries. The objective is to synthesize zeolite A at different temperatures of calcination and synthesis. The starting materials and synthesis of zeolite A have been identified and characterized through analysis of X-ray diffraction (DRX) and scanning electron microscopy (MEV). The synthesis process of zeolite A, using as source of silica and the aluminum metakaolin, which was calcined at temperatures of 700 ° C and 800 ° C for 2 hours of landing in a burning furnace type muffle. Observed in relation to the calcination of kaolin as the main phase, the metakaolin. This is just a removal of water from its structure, so we opted for the lower temperature, less energy consumption. The synthesis process of zeolite A, produced good results for the formation of zeolites type A, which were characterized with high purities. (author)

New Hybrid Route to Biomimetic Synthesis

National Research Council Canada - National Science Library

Morse, Daniel

2003-01-01

To develop economical low-temperature routes to biomimetic synthesis of high-performance composite materials, with control of composition and structure based on the molecular mechanisms controlling...

Development and optimisation of synthesis, characterisation and physical properties of solid materials for strip conductors; purpose oriented synthesis of novel systems. Final report

International Nuclear Information System (INIS)

Guenther, W.; Schoellhorn, R.

1995-06-01

The project reported is part of studies into the performance of HTSC, and was responsible for the following essential tasks: synthesis, characterisation, and optimisation of oxocuprates of the type (RE)Ba 2 Cu 3 O 7 , examination of the relevant corrosion processes and reactivity of the phases, and synthesis of novel systems guided by special model concepts, applying kinetics-controlled low-temperature synthesis. (orig./MM) [de

Characterization of ceramics and intermetallics fabricated by self-propagating high-temperature synthesis

International Nuclear Information System (INIS)

Hurst, J.B.

1989-05-01

Three efforts aimed at investigating the process of self-propagating high temperature synthesis (SHS) for the fabrication of structural ceramics and intermetallics are summarized. Of special interest was the influence of processing variables such as exothermic dopants, gravity, and green state morphology in materials produced by SHS. In the first effort directed toward the fabrication of SiC, exothermic dopants of yttrium and zirconium were added to SiO2 or SiO2 + NiO plus carbon powder mix and processed by SHS. This approach was unsuccessful since it did not produce the desired product of crystalline SiC. In the second effort, the influence of gravity was investigated by examining Ni-Al microstructures which were produced by SHS combustion waves traveling with and opposite the gravity direction. Although final composition and total porosities of the combusted Ni-Al compounds were found to be gravity independent, larger pores were created in those specimens which were combusted opposite to the gravity force direction. Finally, it was found that green microstructure has a significant effect on the appearance of the combusted piece. Severe pressing laminations were observed to arrest the combustion front for TiC samples

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

International Nuclear Information System (INIS)

Yan, Ting; Guo, Xiaode; Zhang, Xiang; Wang, Zhixiang; Shi, Jinqiu

2016-01-01

Highlights: • The nano α-Al 2 O 3 with good dispersion was prepared by two-step hydrolysis. • α-Al 2 O 3 powders were added as seed particles in the hydrolysis. • This article indicated that the glucose could impel the γ-Al 2 O 3 transformed to α-Al 2 O 3 directly. • This article indicated that the addictive of α-Al 2 O 3 seed could improve the phase transformation rate of γ-Al 2 O 3 to α-Al 2 O 3 . • In this article, the pure α-Al 2 O 3 could be obtained by calcining at 1000 °C for 1.5 h. - Abstract: The ultral fine alpha-alumina powder 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.

Bio-synthesis of triangular and hexagonal gold nanoparticles using palm oil fronds’ extracts at room temperature

Science.gov (United States)

Usman, Adamu Ibrahim; Aziz, Azlan Abdul; Abu Noqta, Osama

2018-01-01

Development of bio-reduction techniques for nanoparticles (NPs) synthesis in medical application remains a challenge to numerous researchers. This work reports a novel technique for the synthesis of triangular and hexagonal gold nanoparticles (AuNP) using palm oil fronds’ (POFs) extracts. The functional groups in the POFs’ extracts operate as a persuasive capping and reducing agent to growth AuNPs. The prepared AuNPs were characterized using UV-vis spectrophotometry, Fourier-transform infrared (FTIR) spectroscopy, dynamic light scattering, energy filtered transmission electron microscopy (EFTEM), and x-ray diffraction (XRD). The analysis of FTIR validates the coating of alkynes and phenolic composites on the AuNPs. This shows a feasible function of biomolecules for efficient stabilization of the AuNPs. EFTEM clearly show the triangular and hexagonal shapes of the prepared AuNPs. The XRD patterns display the peaks of fcc crystal structures at (111), (200), (220), (311) and (222), with average particle sizes of 66.7 and 79.02 nm for 1% and 5% POFs extracts concentrations respectively at room temperature. While at 120 °C the average particles size recorded for 1% and 5% of POFs extract concentrations were 32.17 nm and 45.66 nm respectively, and the reaction completed in less than 2 min. The prepared NPs could be potentially applied in biomedical application, due to their excellent stability and refine morphology without agglomeration.

Vapor Phase Synthesis of Organometal Halide Perovskite Nanowires for Tunable Room-Temperature Nanolasers.

Science.gov (United States)

Xing, Jun; Liu, Xin Feng; Zhang, Qing; Ha, Son Tung; Yuan, Yan Wen; Shen, Chao; Sum, Tze Chien; Xiong, Qihua

2015-07-08

Semiconductor nanowires have received considerable attention in the past decade driven by both unprecedented physics derived from the quantum size effect and strong isotropy and advanced applications as potential building blocks for nanoscale electronics and optoelectronic devices. Recently, organic-inorganic hybrid perovskites have been shown to exhibit high optical absorption coefficient, optimal direct band gap, and long electron/hole diffusion lengths, leading to high-performance photovoltaic devices. Herein, we present the vapor phase synthesis free-standing CH3NH3PbI3, CH3NH3PbBr3, and CH3NH3PbIxCl3(-x) perovskite nanowires with high crystallinity. These rectangular cross-sectional perovskite nanowires have good optical properties and long electron hole diffusion length, which ensure adequate gain and efficient optical feedback. Indeed, we have demonstrated optical-pumped room-temperature CH3NH3PbI3 nanowire lasers with near-infrared wavelength of 777 nm, low threshold of 11 μJ/cm(2), and a quality factor as high as 405. Our research advocates the promise of optoelectronic devices based on organic-inorganic perovskite nanowires.

Thermochemistry of some binary lead and transition metal compounds by high temperature direct synthesis calorimetry

Energy Technology Data Exchange (ETDEWEB)

Meschel, S.V., E-mail: meschel@jfi.uchicago.edu [Illinois Institute of Technology,Thermal Processing Technology Center, 10 W. 32nd Street, Chicago, Illinois 60615 (United States); Gordon Center for Integrated Science, 929 E. 57th Street, Chicago, Illinois 60637 (United States); Nash, P. [Illinois Institute of Technology,Thermal Processing Technology Center, 10 W. 32nd Street, Chicago, Illinois 60615 (United States); Chen, X.Q.; Wei, P. [Materials processing Modeling Division, Shenyang National Laboratory for Materials Science, Institute of Metals Research, 72 Wenhua Road, Shenyang City (China)

2015-06-05

Highlights: • Studied binary lead-transition metal alloys by high temperature calorimetry. • Determined the enthalpies of formation of 8 alloys. • Compared the measurements with predictions by the model of Miedema and by the ab initio method. - Abstract: The standard enthalpies of formation of some binary lead and transition metal compounds have been measured by high temperature direct synthesis calorimetry. The reported results are: Pb{sub 3}Sc{sub 5}(−61.3 ± 2.9); PbTi{sub 4}(−16.6 ± 2.4); Pb{sub 3}Y{sub 5}(−64.8 ± 3.6); Pb{sub 3}Zr{sub 5}(−50.6 ± 3.1); PbNb{sub 3}(−10.4 ± 3.4); PbRh(−16.5 ± 3.3); PbPd{sub 3}(−29.6 ± 3.1); PbPt(−34.7 ± 3.3) kJ/mole of atoms. We will compare our results with previously published measurements. We will also compare the experimental measurements with enthalpies of formation of transition metal compounds with elements in the same vertical column in the periodic table. We will compare our measurements with predicted values on the basis of the semi empirical model of Miedema and coworkers and with ab initio values when available.

Rapid, room-temperature synthesis of amorphous selenium/protein composites using Capsicum annuum L extract

Science.gov (United States)

Li, Shikuo; Shen, Yuhua; Xie, Anjian; Yu, Xuerong; Zhang, Xiuzhen; Yang, Liangbao; Li, Chuanhao

2007-10-01

We describe the formation of amorphous selenium (α-Se)/protein composites using Capsicum annuum L extract to reduce selenium ions (SeO32-) at room temperature. The reaction occurs rapidly and the process is simple and easy to handle. A protein with a molecular weight of 30 kDa extracted from Capsicum annuum L not only reduces the SeO32- ions to Se0, but also controls the nucleation and growth of Se0, and even participates in the formation of α-Se/protein composites. The size and shell thickness of the α-Se/protein composites increases with high Capsicum annuum L extract concentration, and decreases with low reaction solution pH. The results suggest that this eco-friendly, biogenic synthesis strategy could be widely used for preparing inorganic/organic biocomposites. In addition, we also discuss the possible mechanism of the reduction of SeO32- ions by Capsicum annuum L extract.

Rapid, room-temperature synthesis of amorphous selenium/protein composites using Capsicum annuum L extract

Energy Technology Data Exchange (ETDEWEB)

Li Shikuo; Shen Yuhua; Xie Anjian; Yu Xuerong; Zhang Xiuzhen; Yang Liangbao; Li Chuanhao [School of Chemistry and Chemical Engineering, Anhui University, Hefei 230039 (China)

2007-10-10

We describe the formation of amorphous selenium ({alpha}-Se)/protein composites using Capsicum annuum L extract to reduce selenium ions (SeO{sub 3}{sup 2-}) at room temperature. The reaction occurs rapidly and the process is simple and easy to handle. A protein with a molecular weight of 30 kDa extracted from Capsicum annuum L not only reduces the SeO{sub 3}{sup 2-} ions to Se{sup 0}, but also controls the nucleation and growth of Se{sup 0}, and even participates in the formation of {alpha}-Se/protein composites. The size and shell thickness of the {alpha}-Se/protein composites increases with high Capsicum annuum L extract concentration, and decreases with low reaction solution pH. The results suggest that this eco-friendly, biogenic synthesis strategy could be widely used for preparing inorganic/organic biocomposites. In addition, we also discuss the possible mechanism of the reduction of SeO{sub 3}{sup 2-} ions by Capsicum annuum L extract.

Rapid, room-temperature synthesis of amorphous selenium/protein composites using Capsicum annuum L extract

International Nuclear Information System (INIS)

Li Shikuo; Shen Yuhua; Xie Anjian; Yu Xuerong; Zhang Xiuzhen; Yang Liangbao; Li Chuanhao

2007-01-01

We describe the formation of amorphous selenium (α-Se)/protein composites using Capsicum annuum L extract to reduce selenium ions (SeO 3 2- ) at room temperature. The reaction occurs rapidly and the process is simple and easy to handle. A protein with a molecular weight of 30 kDa extracted from Capsicum annuum L not only reduces the SeO 3 2- ions to Se 0 , but also controls the nucleation and growth of Se 0 , and even participates in the formation of α-Se/protein composites. The size and shell thickness of the α-Se/protein composites increases with high Capsicum annuum L extract concentration, and decreases with low reaction solution pH. The results suggest that this eco-friendly, biogenic synthesis strategy could be widely used for preparing inorganic/organic biocomposites. In addition, we also discuss the possible mechanism of the reduction of SeO 3 2- ions by Capsicum annuum L extract

Measured winter and spring-time indoor temperatures in UK homes over the period 1969–2010: A review and synthesis

International Nuclear Information System (INIS)

Vadodaria, K.; Loveday, D.L.; Haines, V.

2014-01-01

This paper presents a review and synthesis of average winter and spring-time indoor temperatures in UK homes measured over the period 1969–2010. Analysis of measured temperatures in a sample of solid wall dwellings in the UK, conducted as part of the CALEBRE research project, is included. The review suggests that, for periods when occupation was likely, there has been little or no increase in winter and spring-time average living room temperatures over the last 40 years, with average recorded living room temperatures having been historically lower than the WHO-recommended value of 21 °C. Correspondingly, for periods of likely occupation, average bedroom temperatures appear to have increased. Compared with non-domestic buildings, there have been fewer investigations of domestic thermal comfort, either in the UK or elsewhere, and hence the paper also calls for further detailed investigations of domestic indoor temperatures during occupied hours together with thermal comfort evaluations in order to better understand domestic thermal environments. Based on suggestions from the limited range of studies available to date, living room temperatures may need to be maintained within the range 20–22 °C for thermal satisfaction, though this requires confirmation through further research. The study also emphasises that improving the energy efficiency of homes should be the primary means to effect any increases in indoor temperatures that are deemed essential. Considerations for future policy are discussed. - Highlights: • We review indoor temperatures measured in UK homes during 1960-2010. • We present analysis of temperature recorded by our study in 20 UK homes. • Little or no increase observed in living room temperatures for the last 40 years. • Occupied bedroom temperatures appear to have increased. • Living room temperatures have been historically lower than the WHO guidelines

A Temperature Window for the Synthesis of Single-Walled Carbon Nanotubes by Catalytic Chemical Vapor Deposition of CH4over Mo2-Fe10/MgO Catalyst

Directory of Open Access Journals (Sweden)

Yu Ouyang

2009-01-01

Full Text Available Abstract A temperature window for the synthesis of single-walled carbon nanotubes by catalytic chemical vapor deposition of CH4over Mo2-Fe10/MgO catalyst has been studied by Raman spectroscopy. The results showed that when the temperature is lower than 750 °C, there were few SWCNTs formed, and when the temperature is higher than 950 °C, mass amorphous carbons were formed in the SWCNTs bundles due to the self-decomposition of CH4. The temperature window of SWCNTs efficient growth is between 800 and 950 °C, and the optimum growth temperature is about 900 °C. These results were supported by transmission electron microscope images of samples formed under different temperatures. The temperature window is important for large-scale production of SWCNTs by catalytic chemical vapor deposition method.

Self-propagating high-temperature synthesis of nonstoichiometric wuestite

Energy Technology Data Exchange (ETDEWEB)

Hiramoto, Maki [Graduate School of Engineering, Hokkaido University, Sapporo 060-8628 (Japan); Okinaka, Noriyuki [Center for Advanced Research of Energy and Materials, Faculty of Engineering, Hokkaido University, Sapporo 060-8628 (Japan); Akiyama, Tomohiro, E-mail: takiyama@eng.hokudai.ac.jp [Center for Advanced Research of Energy and Materials, Faculty of Engineering, Hokkaido University, Sapporo 060-8628 (Japan)

2012-04-15

Highlights: Black-Right-Pointing-Pointer The manuscript describes an SHS method of producing Fe{sub x}O. Black-Right-Pointing-Pointer Focus on the effects of nonstoichiometric Fe content and diluent addition on the phase of the SHS product. Black-Right-Pointing-Pointer Without the NaCl diluent, the lattice parameter of SHS Fe{sub 0.947}O corresponded to the theoretical lattice parameter. Black-Right-Pointing-Pointer Nonstoichiometric compounds of Fe{sub x}O (0.942 {<=} x {<=} 0.952) were obtained through SHS without additional external heating. - Abstract: This paper describes the self-propagating high-temperature synthesis (SHS) of nonstoichiometric Fe{sub x}O (x = 0.833-1), with particular focus on the effects of nonstoichiometric Fe content and diluent addition on the phase of the SHS product. In the SHS process, the raw materials Fe, NaClO{sub 4} (oxidizer), and NaCl (diluent) were thoroughly mixed in the desired ratio by ball milling, and the lower surfaces of the disk-shaped green compacts were subsequently electrically ignited to produce Fe{sub x}O through the propagation of the sustainable exothermic reaction. X-ray diffraction analysis showed that the SHS products comprised double phases of Fe{sub x}O and Fe{sub 3}O{sub 4}. The peaks of products with 0.947 {<=} x {<=} 1.00 shifted to lower angles in comparison to those of the product with x = 0.833 attributed to the lattice parameter distortion of the crystal structure because of the Fe defects. In the presence of the NaCl diluent, the raw materials were converted to high-purity Fe{sub x}O powders during the SHS process. Without the NaCl diluent, the lattice parameter of SHS Fe{sub 0.947}O corresponded to the theoretical lattice parameter. Nonstoichiometric compounds of Fe{sub x}O (0.942 {<=} x {<=} 0.952) were obtained through SHS without additional external heating.

Human proton/oligopeptide transporter (POT) genes

DEFF Research Database (Denmark)

Botka, C. W.; Wittig, T. W.; Graul, R. C.

2000-01-01

The proton-dependent oligopeptide transporters (POT) gene family currently consists of approximately 70 cloned cDNAs derived from diverse organisms. In mammals, two genes encoding peptide transporters, PepT1 and PepT2 have been cloned in several species including humans, in addition to a rat...... histidine/peptide transporter (rPHT1). Because the Candida elegans genome contains five putative POT genes, we searched the available protein and nucleic acid databases for additional mammalian/human POT genes, using iterative BLAST runs and the human expressed sequence tags (EST) database. The apparent...... and introns of the likely human orthologue (termed hPHT2). Northern analyses with EST clones indicated that hPHT1 is primarily expressed in skeletal muscle and spleen, whereas hPHT2 is found in spleen, placenta, lung, leukocytes, and heart. These results suggest considerable complexity of the human POT gene...

Synthesis and Electrical Resistivity of Nickel Polymethacrylate

Science.gov (United States)

Chohan, M. H.; Khalid, A. H.; Zulfiqar, M.; Butt, P. K.; Khan, Farah; Hussain, Rizwan

Synthesis of nickel polymethacrylate was carried out using methanolic solutions of sodium hydroxide and polymethacrylic acid. The electrical resistivity of the pellets made from Ni-polymethacrylate was measured at different voltages and temperatures. Results showed that the electrical resistivity of Ni-polymethacrylate decreases significantly with voltage in high temperature regions but the decrease is insignificant at temperatures nearing room temperature. The activation energy at low temperatures is approximately 0.8 eV whereas at high temperature it is in the range 0.21-0.27 eV.

Microstructure evolution of Mo–Si–Al system during self-propagation high-temperature synthesis

International Nuclear Information System (INIS)

Jia, Lei; Xie, Hui; Lu, Zhen-lin; Zhang, Chao

2013-01-01

Highlights: ► Phase transformation subsequence of the reaction system was given by a sketch. ► Transformation of MoSi 2 to Mo(Si, Al) 2 phase was observed by XRD analysis. ► Variation of diffraction peaks was discussed by lattice parameters calculation. -- Abstract: The microstructure and phase constitution of Mo(Si 1−x , Al x ) 2 alloys (x = 0.03, 0.1 and 0.4) prepared by self-propagation high-temperature synthesis is first investigated using SEM, EDS and XRD analysis. Then the lattice parameters and adiabatic temperature are calculated. Based on the above experimental and calculated results, the variation mechanism of diffraction peaks and phase transformation subsequence of the Mo–MoO 3 –Si–Al powders is discussed. Results show that, when the self-propagation reaction is over, there are a homogeneous Mo–Si–Al alloy melt and a fused Al 2 O 3 with lower density at top. Subsequently, MoSi 2 or Mo(Si, Al) 2 phase nucleates and grows as a primary phase in the Mo–Si–Al alloy melts, and then Al, Si substances are generated from the intergranular residual Al–Si liquid according to Al–Si binary phase diagram. The Al increase in the starting powder mixtures leads to the Al concentration increase in the Mo–Si–Al alloy melt. Consequently, MoSi 2 is transformed to Mo(Si, Al) 2 to phase in which Si is replaced by Al atoms and Al substance in the intergranular zones increased accordingly

Ferroic materials synthesis and applications

CERN Document Server

Virk, Hardev Singh

2015-01-01

Ferroics is the generic name given to the study of ferromagnets, ferroelectrics, and ferroelastics. The basis of this study is to understand the large changes in physical characteristics that occur over a very narrow temperature range. In recent years, a new class of ferroic materials has been attracting increased interest. These multiferroics exhibit more than one ferroic property simultaneously in a single phase. The present volume: ""Ferroic Materials: Synthesis and Applications"" has ten Chapters, spread over areas as diverse as Magnetic Oxide Nanomaterials, Ferrites Synthesis, Hexaferrite

Low temperature synthesis and field emission characteristics of single to few layered graphene grown using PECVD

Energy Technology Data Exchange (ETDEWEB)

Kumar, Avshish; Khan, Sunny; Zulfequar, M.; Harsh; Husain, Mushahid, E-mail: mush_reslab@rediffmail.com

2017-04-30

Highlights: • Graphene was synthesized by PECVD system at a low temperature of 600 °C. • From different characterization techniques, the presence of single and few layered graphene was confirmed. • X-ray diffraction pattern of the graphene showed single crystalline nature of the film. • The as-grown graphene films were observed extremely good field emitters with long term emission current stability. - Abstract: In this work, high-quality graphene has successfully been synthesized on copper (Cu) coated Silicon (Si) substrate at very large-area by plasma enhanced chemical vapor deposition system. This method is low cost and highly effective for synthesizing graphene relatively at low temperature of 600 °C. Electron microscopy images have shown that surface morphology of the grown samples is quite uniform consisting of single layered graphene (SLG) to few layered graphene (FLG). Raman spectra reveal that graphene has been grown with high-quality having negligible defects and the observation of G and G' peaks is also an indicative of stokes phonon energy shift caused due to laser excitation. Scanning probe microscopy image also depicts the synthesis of single to few layered graphene. The field emission characteristics of as-grown graphene samples were studied in a planar diode configuration at room temperature. The graphene samples were observed to be a good field emitter having low turn-on field, higher field amplification factor and long term emission current stability.

Plasma synthesis of nanostructures for improved thermoelectric properties

International Nuclear Information System (INIS)

Petermann, Nils; Hecht, Christian; Schulz, Christof; Wiggers, Hartmut; Stein, Niklas; Schierning, Gabi; Theissmann, Ralf; Stoib, Benedikt; Brandt, Martin S

2011-01-01

The utilization of silicon-based materials for thermoelectrics is studied with respect to the synthesis and processing of doped silicon nanoparticles from gas phase plasma synthesis. It is found that plasma synthesis enables the formation of spherical, highly crystalline and soft-agglomerated materials. We discuss the requirements for the formation of dense sintered bodies, while keeping the crystallite size small. Small particles a few tens of nanometres and below that are easily achievable from plasma synthesis, and a weak surface oxidation, both lead to a pronounced sinter activity about 350 K below the temperature usually needed for the successful densification of silicon. The thermoelectric properties of our sintered materials are comparable to the best results found for nanocrystalline silicon prepared by methods other than plasma synthesis.

Influence of temperature on the formation and encapsulation of gold nanoparticles using a temperature-sensitive template

Directory of Open Access Journals (Sweden)

Noel Peter Bengzon Tan

2015-12-01

Full Text Available This data article describes the synthesis of temperature-sensitive and amine-rich microgel particle as a dual reductant and template to generate smart gold/polymer nanocomposite particle. TEM images illustrate the influence of reaction temperature on the formation and in-site encapsulation of gold nanoparticles using the temperature-sensitive microgel template. Thermal stability of the resultant gold/polymer composite particles was also examined.

High-deposition-rate ceramics synthesis

Energy Technology Data Exchange (ETDEWEB)

Allendorf, M.D.; Osterheld, T.H.; Outka, D.A. [Sandia National Laboratories, Livermore, CA (United States)] [and others

1995-05-01

Parallel experimental and computational investigations are conducted in this project to develop validated numerical models of ceramic synthesis processes. Experiments are conducted in the High-Temperature Materials Synthesis Laboratory in Sandia`s Combustion Research Facility. A high-temperature flow reactor that can accommodate small preforms (1-3 cm diameter) generates conditions under which deposition can be observed, with flexibility to vary both deposition temperature (up to 1500 K) and pressure (as low as 10 torr). Both mass spectrometric and laser diagnostic probes are available to provide measurements of gas-phase compositions. Experiments using surface analytical techniques are also applied to characterize important processes occuring on the deposit surface. Computational tools developed through extensive research in the combustion field are employed to simulate the chemically reacting flows present in typical industrial reactors. These include the CHEMKIN and Surface-CHEMKIN suites of codes, which permit facile development of complex reaction mechanisms and vastly simplify the implementation of multi-component transport and thermodynamics. Quantum chemistry codes are also used to estimate thermodynamic and kinetic data for species and reactions for which this information is unavailable.

Synthesis and thermotolerance of heat shock proteins in Campylobacter jejuni

International Nuclear Information System (INIS)

Kim, C.K.; Kim, H.O.; Lee, K.J.

1991-01-01

The heat shock responses of Campylobacter jejuni were studied by examination of their survival rates and synthesis of heat shock proteins. When C. jejuni cells were treated at the sublethal temperatures of 48C° for 30 minutes, most of the cells maintained their viabilities and synthesized the heat shock proteins of 90, 73, and 66 kD in molecular weight. By the method of two-dimensional electrophoresis, the heat shock proteins of C. jejuni were identified to be Hsp90, Hsp73, and Hsp66. During the heat shock at 48C°, the heat shock proteins were induced from about 5 minutes after the heat shock treatment. Their synthesis was continued upto 30 minutes, but remarkably retarded after 50 minutes. When C. jejune cells were heat shocked at 51C° for 30 minutes, the survival rates of the cells were decreased by about 10 3 fold and synthesis of heat shock proteins and normal proteins was also generally retarded. The cells exposed to 55C° for 30 minutes died off by more than 10 5 cells and the new protein synthesis was not observed. But when C. jejuni cells were heat-shocked at the sublethal temperature of 48C° for 15 to 20 minutes and then were exposed at the lethal temperature of 55C° for 30 minutes, their viabilities were higher than those exposed at 55C° for 30 minutes without pre-heat shock at 48C°. Therefore, the heat shock proteins synthesized at the sublethal temperature of 48C° in C. jejuni were thought to be responsible for thermotolerance. However, when C. jejuni cells heat-shocked at various ranges of sublethal and lethal temperatures were placed back to the optimum temperature of 42C°, the multiplication patterns of the cells pretreated at different temperatures were not much different each other

Synthesis and application of intelligent hydrogels

International Nuclear Information System (INIS)

Kaetsu, I.; Uchida, K.; Sutani, K.; Nakayama, H.; Tamori, A.

2000-01-01

The authors have studied synthesis and application of stimule-sensitive and responsive hydrogels. In this report, two kinds of investigations were carried out on the intelligent hydrogels and the applications with radiation techniques. 1. Synthesis of temperature responsive sol-gel transition polymer and the application to drug delivery systems. Polysopropyl acrylamide is a typical temperature responsive polymers and the copolymers show broad variation of LCST (sol-gel transition temperature). The various copolymers of isopropyl acrylamide were synthesized by UV or radiation. 2. Surface curing of pH and electric field responsive hydrogel and the application to drug delivery systems. Electrolyte monomers such as acrylic acid was coated on the surface of polymer membrane (porous or non-porous) including drugs, and cured by UV or radiation various enzymes were immobilized in the coating layer in many cases. The product showed pH, electro-field and substrate responsive releases of model drug under on-off switching of environmental conditions. (J.P.N.)

Synthesis and application of intelligent hydrogels

Energy Technology Data Exchange (ETDEWEB)

Kaetsu, I.; Uchida, K.; Sutani, K.; Nakayama, H.; Tamori, A. [Kinki Univ., Higashi-Osaka, Osaka (Japan). Faculty of Science and Technology

2000-03-01

The authors have studied synthesis and application of stimule-sensitive and responsive hydrogels. In this report, two kinds of investigations were carried out on the intelligent hydrogels and the applications with radiation techniques. 1. Synthesis of temperature responsive sol-gel transition polymer and the application to drug delivery systems. Polysopropyl acrylamide is a typical temperature responsive polymers and the copolymers show broad variation of LCST (sol-gel transition temperature). The various copolymers of isopropyl acrylamide were synthesized by UV or radiation. 2. Surface curing of pH and electric field responsive hydrogel and the application to drug delivery systems. Electrolyte monomers such as acrylic acid was coated on the surface of polymer membrane (porous or non-porous) including drugs, and cured by UV or radiation various enzymes were immobilized in the coating layer in many cases. The product showed pH, electro-field and substrate responsive releases of model drug under on-off switching of environmental conditions. (J.P.N.)

Room temperature synthesis and optical properties of small diameter (5 nm) ZnO nanorod arrays.

Science.gov (United States)

Cho, Seungho; Jang, Ji-Wook; Lee, Jae Sung; Lee, Kun-Hong

2010-10-01

We report a simple wet-chemical synthesis of ∼5 nm diameter ZnO nanorod arrays at room temperature (20 °C) and normal atmospheric pressure (1 atm) and their optical properties. They were single crystalline in nature, and grew in the [001] direction. These small diameter ZnO nanorod arrays can also be synthesized at 0 °C. Control experiments were also conducted. On the basis of the results, we propose a mechanism for the spontaneous growth of the small diameter ZnO structures. The optical properties of the 5 nm diameter ZnO nanorod arrays synthesized using this method were probed by UV-Visible diffuse reflectance spectroscopy. A clear blue-shift, relative to the absorption band from 50 nm diameter ZnO nanorod arrays, was attributed to the quantum confinement effects caused by the small nanocrystal size in the 5 nm diameter ZnO nanorods.

Room temperature synthesis and characterization of CdO nanowires by chemical bath deposition (CBD) method

International Nuclear Information System (INIS)

Dhawale, D.S.; More, A.M.; Latthe, S.S.; Rajpure, K.Y.; Lokhande, C.D.

2008-01-01

A chemical synthesis process for the fabrication of CdO nanowires is described. In the present work, transparent and conductive CdO films were synthesized on the glass substrate using chemical bath deposition (CBD) at room temperature. These films were annealed in air at 623 K and characterized for the structural, morphological, optical and electrical properties were studied by means of X-ray diffraction (XRD), scanning electron microscopy (SEM), optical and electrical resistivity. The XRD analysis showed that the as-deposited amorphous can be converted in to polycrystalline after annealing. Annealed CdO nanowires are 60-65 nm in diameter and length ranges typically from 2.5 to 3 μm. The optical properties revealed the presence of direct and indirect band gaps with energies 2.42 and 2.04 eV, respectively. Electrical resistivity measurement showed semiconducting behavior and thermoemf measurement showed n-type electrical conductivity

Sol-gel synthesis of hydroxyapatite

International Nuclear Information System (INIS)

Zupanski, M.D.; Lucena, M.P.P.; Bergmann, C.P.

2010-01-01

Hydroxyapatite (HAp) has been established as the calcium phosphate based compound with most applications in the biological field. Among the numerous techniques for synthesis of HAp, the sol-gel processing route affords great control over purity and formed phases using low processing temperatures. In addition, the sol-gel approach offers an option for homogeneous HAp coating on metal substrates, as well as the ability to generate nanocrystalline powders. In this work, the sol-gel synthesis of HAp was investigated employing triethyl phosphate and calcium nitrate tetrahydrate as phosphorous and calcium precursors, respectively. The aging effect on phase composition and powder morphology of the final product was studied in terms of temperature and aging time. The powders were studied by using X-ray diffraction, Fourier transform infrared spectroscopy, particle size distribution by laser diffraction and scanning electron microscopy. (author)

Seed-free synthesis of 1D silver nanowires ink using clove oil (Syzygium Aromaticum) at room temperature.

Science.gov (United States)

Jeevika, Alagan; Ravi Shankaran, Dhesingh

2015-11-15

Silver nanowires (AgNWs) have been demonstrated to be a promising next generation conducting material and an alternative to the traditional electrode (ITO) because of its high conductivity, transparency and stability. Generally, AgNWs are synthesized by chemical method (mainly polyol reduction method) at high temperature in the presence of exotic seeds. The present work aims at the green approach for preparation and characterization of 1D AgNWs ink using clove oil (Syzygium Aromaticum) at room temperature. AgNWs was prepared by green synthesis using clove oil as reducing as well as capping agent at room temperature. The obtained ink was purified, filtered and redissolved in methanol. The prepared AgNWs showed an absorption peaks at 350 and 387nm in the UV-vis spectrum due to transverse SPR mode of silver. From the HR-TEM analysis, it was observed that the AgNWs possess an average diameter and length of ∼39±0.01nm and ∼3μm, respectively. The obtained AgNWs are crystalline in nature and are arranged in a perfect crystal lattice orientation, which was confirmed from the selected area electron diffraction studies. Moreover, the X-ray diffraction analysis confirms the face centered cubic structure. The AgNWs coated glass substrate shows an electrical conductivity of ∼0.48×10(6)S/m. Copyright © 2015 Elsevier Inc. All rights reserved.

Combustion synthesis and structural characterization of Li–Ti mixed

Indian Academy of Sciences (India)

Combustion synthesis and structural characterization of Li–Ti mixed nanoferrites ... were prepared by combustion method at lower temperatures compared to the ... first time at low temperatures, using PEG which acts as a new fuel and oxidant.

Combustion synthesis and structural characterization of Li–Ti mixed ...

Indian Academy of Sciences (India)

pared by combustion method at lower temperatures compared to the conventional high temperature sintering for ... Li–Ti mixed ferrites; combustion synthesis; hysteresis. 1. ... Quantum model - VSM 6000) at an applied field of ±10 kOe.

Synthesis of Polyfunctionalized 4H-Pyrans

Directory of Open Access Journals (Sweden)

Manisha Bihani

2013-01-01

Full Text Available Amberlyst A21 catalyzed one-pot three-component coupling of aldehyde and malononitrile with active methylene compounds such as acetylacetone and ethyl acetoacetate for the synthesis of pharmaceutically important polyfunctionalized 4H-pyrans has been reported. Simple experimental procedure, no chromatographic purification, no hazardous organic solvents, easy recovery and reusability of the catalyst, and room temperature reaction conditions are some of the highlights of this protocol for the synthesis of pharmaceutically relevant focused libraries.

ROOM TEMPERATURE BULK SYNTHESIS OF SILVER NANOCABLES WRAPPED WITH POLYPYRROLE

Science.gov (United States)

Wet chemical synthesis of silver cables wrapped with polypyrrole is reported in aqueous media without use of any surfactant/capping agent and/or template. The method employs direct polymerization of pyrrole of an aqueous solution with AgNO3 as an oxidizing agent. The four probe c...

Detonation Synthesis of Alpha-Variant Silicon Carbide

Science.gov (United States)

Langenderfer, Martin; Johnson, Catherine; Fahrenholtz, William; Mochalin, Vadym

2017-06-01

A recent research study has been undertaken to develop facilities for conducting detonation synthesis of nanomaterials. This process involves a familiar technique that has been utilized for the industrial synthesis of nanodiamonds. Developments through this study have allowed for experimentation with the concept of modifying explosive compositions to induce synthesis of new nanomaterials. Initial experimentation has been conducted with the end goal being synthesis of alpha variant silicon carbide (α-SiC) in the nano-scale. The α-SiC that can be produced through detonation synthesis methods is critical to the ceramics industry because of a number of unique properties of the material. Conventional synthesis of α-SiC results in formation of crystals greater than 100 nm in diameter, outside nano-scale. It has been theorized that the high temperature and pressure of an explosive detonation can be used for the formation of α-SiC in the sub 100 nm range. This paper will discuss in detail the process development for detonation nanomaterial synthesis facilities, optimization of explosive charge parameters to maximize nanomaterial yield, and introduction of silicon to the detonation reaction environment to achieve first synthesis of nano-sized alpha variant silicon carbide.

Viscosity of the oil-in-water Pickering emulsion stabilized by surfactant-polymer and nanoparticle-surfactant-polymer system

Science.gov (United States)

Sharma, Tushar; Kumar, G. Suresh; Chon, Bo Hyun; Sangwai, Jitendra S.

2014-11-01

Information on the viscosity of Pickering emulsion is required for their successful application in upstream oil and gas industry to understand their stability at extreme environment. In this work, a novel formulation of oil-in-water (o/w) Pickering emulsion stabilized using nanoparticle-surfactant-polymer (polyacrylamide) system as formulated in our earlier work (Sharma et al., Journal of Industrial and Engineering Chemistry, 2014) is investigated for rheological stability at high pressure and high temperature (HPHT) conditions using a controlled-strain rheometer. The nanoparticle (SiO2 and clay) concentration is varied from 1.0 to 5.0 wt%. The results are compared with the rheological behavior of simple o/w emulsion stabilized by surfactant-polymer system. Both the emulsions exhibit non-Newtonian shear thinning behavior. A positive shift in this behavior is observed for surfactant-polymer stabilized emulsion at high pressure conditions. Yield stress is observed to increase with pressure for surfactant-polymer emulsion. In addition, increase in temperature has an adverse effect on the viscosity of emulsion stabilized by surfactant-polymer system. In case of nanoparticle-surfactant-polymer stabilized o/w emulsion system, the viscosity and yield stress are predominantly constant for varying pressure and temperature conditions. The viscosity data for both o/w emulsion systems are fitted by the Herschel-Bulkley model and found to be satisfactory. In general, the study indicates that the Pickering emulsion stabilized by nanoparticle-surfactant-polymer system shows improved and stable rheological properties as compared to conventional emulsion stabilized by surfactant-polymer system indicating their successful application for HPHT environment in upstream oil and gas industry.

STABILIZATION OF TEMPERATURE REGIMES WHILE SYNTHESIZING DIAMOND POWDERS

Directory of Open Access Journals (Sweden)

A. I. Dudiak

2012-01-01

Full Text Available The paper considers peculiar features of artificial diamond powder synthesis process and also direct and indirect methods for temperature measurement in a reaction cell of high-pressure apparatus. Differences in temperature regimes of diamond synthesis associated with time fixation of strain and heating power have been analyzed in the paper. The paper  reveals their impracticability.Theoretical methodology for temperature correction in the reaction cell has been proposed in the paper. An algorithm controlling cell material heating has been developed on the basis of a microcontroller and it makes it possible to stabilize temperature in the reaction mixture that permits to improve quality and strength characteristics of the obtained diamond powders. The paper contains a graphic interpretation of calculation results with the help of the proposed algorithm. 

High temperature ceramic-tubed reformer

Science.gov (United States)

Williams, Joseph J.; Rosenberg, Robert A.; McDonough, Lane J.

1990-03-01

The overall objective of the HiPHES project is to develop an advanced high-pressure heat exchanger for a convective steam/methane reformer. The HiPHES steam/methane reformer is a convective, shell and tube type, catalytic reactor. The use of ceramic tubes will allow reaction temperature higher than the current state-of-the-art outlet temperatures of about 1600 F using metal tubes. Higher reaction temperatures increase feedstock conversion to synthesis gas and reduce energy requirements compared to currently available radiant-box type reformers using metal tubes. Reforming of natural gas is the principal method used to produce synthesis gas (primarily hydrogen and carbon monoxide, H2 and CO) which is used to produce hydrogen (for refinery upgrading), methanol, as well as several other important materials. The HiPHES reformer development is an extension of Stone and Webster's efforts to develop a metal-tubed convective reformer integrated with a gas turbine cycle.

Self-propagating high-temperature synthesis of La(Sr)Ga(Mg)O3-δ for electrolyte of solid oxide fuel cells

International Nuclear Information System (INIS)

Ishikawa, Hiroyuki; Enoki, Makiko; Ishihara, Tatsumi; Akiyama, Tomohiro

2007-01-01

This paper describes self-propagating high-temperature synthesis (SHS) of an electrolyte for solid oxide fuel (SOFC), in comparison to a conventional solid-state reaction method (SRM). Doped-lanthanum gallate: La 0.9 Sr 0.1 Ga 0.8 Mg 0.2 O 3-δ (LSGM9182) and LSGM9173 as the SOFC electrolyte, was prepared by the SHS and sintered at different temperatures, for measuring the electrical conductivity of the sintered LSGM and the power generating performance at 1073 K, in comparison to the SRM. In the SHS, the LSGM powders with smaller size were obtained and easily sintered at the 100 K-lower temperature, 1673 K, than in the SRM. Most significantly, the electrical conductivity of the sintered LSGM9182 was as high as 0.11 S cm -1 and its maximum power density was a value of 245 mW cm -2 in the cell configuration of Ni/LSGM9182 (0.501 mm in thickness)/Sm 0.5 Sr 0.5 CoO 3 . The conclusion was that the proposed SHS-sintering method with many benefits of minimizing the energy requirement and the processing time in the production, easing temperature restriction for the sintering, and improving the electrolyte performance up to a conventional level is practicable for producing the LSGM-electrolyte of SOFC at an intermediate-temperature application

One-step synthesis of dimethyl ether from the gas mixture containing CO2 with high space velocity

International Nuclear Information System (INIS)

Chen, Wei-Hsin; Lin, Bo-Jhih; Lee, How-Ming; Huang, Men-Han

2012-01-01

Highlights: ► A bifunctional catalyst for DME synthesis is prepared using a coprecipitation method. ► The DME synthesis from syngas at a high space velocity of is investigated. ► The reaction is dominated by chemical kinetics at lower reaction temperatures. ► Thermodynamic equilibrium governs the reaction at higher temperatures. ► 0.2 g of ZSM5 is sufficient to be blended with 1 g of the catalyst for DME synthesis. -- Abstract: Dimethyl ether (DME) has been considered as a potential hydrogen carrier used in fuel cells; it can also be consumed as a diesel substitute or chemicals. To develop the technique of DME synthesis, a bifunctional Cu–ZnO–Al 2 O 3 /ZSM5 catalyst is prepared using a coprecipitation method. The reaction characteristics of DME synthesis from syngas at a high space velocity of 15,000 mL (g cat h) −1 are investigated and the effects of reaction temperature, pressure, CO 2 concentration and ZSM5 amount on the synthesis are taken into account. The results suggest that an increase in CO 2 concentration in the feed gas substantially decreases the DME formation. The optimum reaction temperature always occurs at 225 °C, regardless of what the pressure is. It is thus recognized that the DME synthesis is governed by two different mechanisms when the reaction temperature varies. At lower reaction temperatures ( 225 °C). For the CO 2 content of 5 vol.% and the pressure of 40 atm, the maximum DME yield is 1.89 g (g cat h) −1 . It is also found that 0.2 g of ZSM5 is sufficient to be blended with 1 g of the catalyst for DME synthesis.

Anomalous enhancement of nanodiamond luminescence upon heating

Science.gov (United States)

Khomich, A. A.; Kudryavtsev, O. S.; Dolenko, T. A.; Shiryaev, A. A.; Fisenko, A. V.; Konov, V. I.; Vlasov, I. I.

2017-02-01

Characteristic photoluminescence (PL) of nanodiamonds (ND) of different origin (detonation, HPHT, extracted from meteorite) was studied in situ at high temperatures in the range 20-450 °C. Luminescence was excited using 473 nm laser and recorded in the range 500-800 nm. In contrast to decrease of point defect PL in bulk diamond with temperature, we found that the ND luminescence related to ND surface defects increases almost an order of magnitude upon heating to 200-250 °C. The observed effect reveals that water adsorbed on ND surfaces efficiently quenches PL; water desorption on heating leads to dramatic increase of the radiative de-excitation.

High pressure direct synthesis of adipic acid from cyclohexene and hydrogen peroxide via capillary microreactors

NARCIS (Netherlands)

Shang, M.; Noël, T.; Su, Y.; Hessel, V.

2016-01-01

The direct synthesis of adipic acid from hydrogen peroxide and cyclohexene was investigated in capillary microreactors at high temperature (up to 115°C ) and pressure (up to 70 bar). High temperature was already applied in micro-flow packed-bed reactors for the direct adipic acid synthesis. In our

Effect of Synthesis Temperature on Structure and Magnetic Properties of (La,Nd)0.7Sr0.3MnO3 Nanoparticles.

Science.gov (United States)

Shlapa, Yulia; Solopan, Sergii; Bodnaruk, Andrii; Kulyk, Mykola; Kalita, Viktor; Tykhonenko-Polishchuk, Yulia; Tovstolytkin, Alexandr; Belous, Anatolii

2017-12-01

Two sets of Nd-doped La 0.7 Sr 0.3 MnO 3 nanoparticles were synthesized via sol-gel method with further heat treatment at 1073 and 1573 K, respectively. Crystallographic and magnetic properties of obtained nanoparticles were studied, and the effect of synthesis conditions on these properties was investigated. According to X-ray data, all particles crystallized in the distorted perovskite structure. Magnetic parameters, such as saturation magnetization, coercivity, Curie temperature, and specific loss power, which is released on the exposure of an ensemble of nanoparticles to AC magnetic field, were determined for both sets of samples. The correlation between the values of Curie temperature and maximal heating temperature under AC magnetic field was found. It was revealed that for the samples synthesized at 1573 K, the dependences of crystallographic and magnetic parameters on Nd content were monotonous, while for the samples synthesized at 1073 K, they were non-monotonous. It was concluded that Nd-doped La 0.7 Sr 0.3 MnO 3 nanoparticles are promising materials for self-controlled magnetic hyperthermia applications, but the researchers should be aware of the unusual behavior of the particles synthesized at relatively low temperatures.

Difunctionalization of alkenes with iodine and tert-butyl hydroperoxide (TBHP) at room temperature for the synthesis of 1-(tert-butylperoxy)-2-iodoethanes.

Science.gov (United States)

Wang, Hao; Chen, Cui; Liu, Weibing; Zhu, Zhibo

2017-01-01

We developed a direct vicinal difunctionalization of alkenes with iodine and TBHP at room temperature. This iodination and peroxidation in a one-pot synthesis produces 1-( tert -butylperoxy)-2-iodoethanes, which are inaccessible through conventional synthetic methods. This method generates multiple radical intermediates in situ and has excellent regioselectivity, a broad substrate scope and mild conditions. The iodine and peroxide groups of 1-( tert -butylperoxy)-2-iodoethanes have several potential applications and allow further chemical modifications, enabling the preparation of synthetically valuable molecules.

Synthesis of mordenite in geothermal wells

Energy Technology Data Exchange (ETDEWEB)

Konoya, M [Geological Survey of Hokkaido, Japan

1970-03-01

A study of the possible synthesis of mordenite in geothermal wells was conducted. In 1966 as part of a series of exploratory geothermal investigations, a 500 m well was drilled which had a temperature at 250 m of 120/sup 0/C. The well has constant temperature and constant pressure and has been used to study alteration. Specimens which were placed in the well were tested for mordenite. Mordenite was synthesized when Benki clay and a 10% KOH solution were placed in a Teflon tube at 250 m (120/sup 0/C and 22.3 kg/cm/sup 2/) for three months. No mordenite was synthesized when obsidian powder was used. These results indicate the possibility of synthesis of zeolite and clay minerals in geothermal wells. Two figures and four tables are provided.

Room-temperature synthesis and enhanced catalytic performance of silver-reduced graphene oxide nanohybrids

International Nuclear Information System (INIS)

Thu, Tran Viet; Ko, Pil Ju; Phuc, Nguyen Huu Huy; Sandhu, Adarsh

2013-01-01

The synthesis of supported, ultrasmall metallic nanoparticles (NPs) is of great importance for catalytic applications. In this study, silver-reduced graphene oxide nanohybrids (Ag–rGO NHs) were prepared by reducing Ag ions and graphene oxide (GO) at room temperature using sodium borohydride (NaBH 4 ) and trisodium citrate. The resulting products were characterized using UV–Vis spectroscopy, X-ray diffraction, Raman spectroscopy, scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM), and X-ray photoelectron spectroscopy. The rich chemistry of GO surface provided many sites for the nucleation of Ag ions and efficiently limited their growth. Ag NPs were uniformly grown on basal planes of rGO with a high density (∼1,700 NPs μm −2 ) and well-defined size (3.6 ± 0.6 nm) as evidenced in SEM and HRTEM studies. The resulting Ag–rGO NHs were readily dispersed in water and exhibited enhanced catalytic activity toward the reduction of 4-nitrophenol by NaBH 4 in comparison to unsupported Ag NPs. The role of rGO as an excellent support for Ag catalyst is discussed

Room-temperature synthesis and enhanced catalytic performance of silver-reduced graphene oxide nanohybrids

Energy Technology Data Exchange (ETDEWEB)

Thu, Tran Viet, E-mail: thu@eiiris.tut.ac.jp; Ko, Pil Ju, E-mail: ko@eiiris.tut.ac.jp [Toyohashi University of Technology, Electronics-Inspired Interdisciplinary Research Institute (Japan); Phuc, Nguyen Huu Huy [Toyohashi University of Technology, Department of Electrical and Electronic Information Engineering (Japan); Sandhu, Adarsh [Toyohashi University of Technology, Electronics-Inspired Interdisciplinary Research Institute (Japan)

2013-10-15

The synthesis of supported, ultrasmall metallic nanoparticles (NPs) is of great importance for catalytic applications. In this study, silver-reduced graphene oxide nanohybrids (Ag-rGO NHs) were prepared by reducing Ag ions and graphene oxide (GO) at room temperature using sodium borohydride (NaBH{sub 4}) and trisodium citrate. The resulting products were characterized using UV-Vis spectroscopy, X-ray diffraction, Raman spectroscopy, scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM), and X-ray photoelectron spectroscopy. The rich chemistry of GO surface provided many sites for the nucleation of Ag ions and efficiently limited their growth. Ag NPs were uniformly grown on basal planes of rGO with a high density ({approx}1,700 NPs {mu}m{sup -2}) and well-defined size (3.6 {+-} 0.6 nm) as evidenced in SEM and HRTEM studies. The resulting Ag-rGO NHs were readily dispersed in water and exhibited enhanced catalytic activity toward the reduction of 4-nitrophenol by NaBH{sub 4} in comparison to unsupported Ag NPs. The role of rGO as an excellent support for Ag catalyst is discussed.

Synthesis of ammonia using sodium melt.

Science.gov (United States)

Kawamura, Fumio; Taniguchi, Takashi

2017-09-14

Research into inexpensive ammonia synthesis has increased recently because ammonia can be used as a hydrogen carrier or as a next generation fuel which does not emit CO 2 . Furthermore, improving the efficiency of ammonia synthesis is necessary, because current synthesis methods emit significant amounts of CO 2 . To achieve these goals, catalysts that can effectively reduce the synthesis temperature and pressure, relative to those required in the Haber-Bosch process, are required. Although several catalysts and novel ammonia synthesis methods have been developed previously, expensive materials or low conversion efficiency have prevented the displacement of the Haber-Bosch process. Herein, we present novel ammonia synthesis route using a Na-melt as a catalyst. Using this route, ammonia can be synthesized using a simple process in which H 2 -N 2 mixed gas passes through the Na-melt at 500-590 °C under atmospheric pressure. Nitrogen molecules dissociated by reaction with sodium then react with hydrogen, resulting in the formation of ammonia. Because of the high catalytic efficiency and low-cost of this molten-Na catalyst, it provides new opportunities for the inexpensive synthesis of ammonia and the utilization of ammonia as an energy carrier and next generation fuel.

Uptake and intracellular accumulation of diamond nanoparticles – a metabolic and cytotoxic study

Directory of Open Access Journals (Sweden)

Antonín Brož

2017-08-01

Full Text Available Diamond nanoparticles, known as nanodiamonds (NDs, possess several medically significant properties. Having a tailorable and easily accessible surface gives them great potential for use in sensing and imaging applications and as a component of cell growth scaffolds. In this work we investigate in vitro interactions of human osteoblast-like SAOS-2 cells with four different groups of NDs, namely high-pressure high-temperature (HPHT NDs (diameter 18–210 nm, oxygen-terminated, photoluminescent HPHT NDs (diameter 40 nm, oxygen-terminated, detonation NDs (diameter 5 nm, H-terminated, and the same detonation NDs further oxidized by annealing at 450 °C. The influence of the NDs on cell viability and cell count was measured by the mitochondrial metabolic activity test and by counting cells with stained nuclei. The interaction of NDs with cells was monitored by phase contrast live-cell imaging in real time. For both types of oxygen-terminated HPHT NDs, the cell viability and the cell number remained almost the same for concentrations up to 100 µg/mL within the whole range of ND diameters tested. The uptake of hydrogen-terminated detonation NDs caused the viability and the cell number to decrease by 80–85%. The oxidation of the NDs hindered the decrease, but on day 7, a further decrease was observed. While the O-terminated NDs showed mechanical obstruction of cells by agglomerates preventing cell adhesion, migration and division, the H-terminated detonation NDs exhibited rapid penetration into the cells from the beginning of the cultivation period, and also rapid cell congestion and a rapid reduction in viability. These findings are discussed with reference to relevant properties of NDs such as surface chemical bonds, zeta potential and nanoparticle types.

Synthesis of deuterium and tritium labelled tyrosine

International Nuclear Information System (INIS)

Kanska, M.; Drabarek, S.

1980-01-01

A new method of synthesis of tyrosine labelled with deuterium and tritium in the aromatic ring has been developed. Deuterated and tritiated tyrosine was obtained by isotope exchange between tyrosine and deuterated or tritiated water at elevated temperature in hydrochloric acid medium using K 2 PtCl 4 as a catalyst. For synthesis of tritiated tyrosine 1 Ci HTO was used; the specific activity of the product was 5 mCi/mMol. (author)

Green synthesis and characterisation of platinum nanoparticles using quail egg yolk

Science.gov (United States)

Nadaroglu, Hayrunnisa; Gungor, Azize Alayli; Ince, Selvi; Babagil, Aynur

2017-02-01

Nanotechnology is extensively used in all parts today. Therefore, nano synthesis is also significant in all explored areas. The results of studies conducted have revealed that nanoparticle synthesis is performed by using both chemical and physical methods. It is well known that these syntheses are carried out at high charge, pressure and temperature in harsh environments. Therefore, this study investigated green synthesis method that sustains more mild conditions. In this study, quail egg yolk having high vitamin and protein content was prepared for green synthesis reaction and used for the synthesis of platinum nanoparticles in the reaction medium. Reaction situations were optimised as a function of pH, temperature, time and concentration by using quail egg yolk. The results showed that the highest platinum nanoparticles were synthesised at 20 °C and pH 6.0 for 4 h. Also, optimal concentration of metal ions was established as 0.5 mM. The synthesised platinum nanoparticles were characterised by using UV spectrum, X-ray diffraction and scanning electron microscope.

Moderate Temperature Synthesis of Mesoporous Carbon

KAUST Repository

Dua, Rubal

2013-01-03

Methods and composition for preparation of mesoporous carbon material are provided. For example, in certain aspects methods for carbonization and activation at selected temperature ranges are described. Furthermore, the invention provides products prepared therefrom.

Moderate Temperature Synthesis of Mesoporous Carbon

KAUST Repository

Dua, Rubal; Wang, Peng

2013-01-01

Methods and composition for preparation of mesoporous carbon material are provided. For example, in certain aspects methods for carbonization and activation at selected temperature ranges are described. Furthermore, the invention provides products prepared therefrom.

Electrochemical Synthesis of Ammonia from Water and Nitrogen using a Pt/GDC/Pt Cell

International Nuclear Information System (INIS)

Kim, Jong Nam; Yoo, Chung-Yul; Joo, Jong Hoon; Yu, Ji Haeng; Sharma, Monika; Yoon, Hyung Chul; Jeoung, Hana; Song, Ki Chang

2014-01-01

Electrochemical ammonia synthesis from water and nitrogen using a Pt/GDC/Pt cell was experimentally investigated. Electrochemical analysis and ammonia synthesis in the moisture-saturated nitrogen environment were performed under the operating temperature range 400-600 .deg. C and the applied potential range OCV (Open Circuit Voltage)-1.2V. Even though the ammonia synthesis rate was augmented with the increase in the operating temperature (i.e.. increase in the applied current) under the constant potential, the faradaic efficiency was decreased because of the limitation of dissociative chemisorption of nitrogen on the Pt electrode. The maximum synthesis rate of ammonia was 3.67x10 -11 mols -1 cm -2 with 0.1% faradaic efficiency at 600 .deg. C

Synthesis of InGaZnO4 nanoparticles using low temperature multistep co-precipitation method

International Nuclear Information System (INIS)

Wu, Ming-Chung; Hsiao, Kai-Chi; Lu, Hsin-Chun

2015-01-01

Indium gallium zinc oxide (InGaZnO 4 , IGZO) has attracted explosive growth in investigations over the last decades as an important material in the thin-film transistor. In this study, the various nitrate precursors, including indium nitrate, gallium nitrate, and zinc nitrate, were prepared from the various metals dissolved in nitric acid. Then, we used these nitrate precursors to synthesize the IGZO precursor powder by the multistep co-precipitation method. The synthesis parameters of the co-precipitation method, such as reaction temperature, pH value and reaction time, were controlled precisely to prepare the high quality IGZO precursor powder. Finally, IGZO precursor powder was calcined at 900 °C. Then, the microstructure, the crystalline structure, the particle size distribution and specific surface area of calcined IGZO precursor powder were characterized by electron transmission microscopy, X-ray diffraction technique, dynamic light scattering method and the surface area and porosimetry analyzer, respectively. The relative density of IGZO tablet sintered at 1200 °C for 12 h is as high as 97.30%, and it showed highly InGaZnO 4 crystalline structure and the large grain size. The IGZO nanoparticles developed in our study has the potential for the high quality target materials used in the application of electronic devices. - Graphical abstract: Display Omitted - Highlights: • InGaZnO 4 (IGZO) nanoparticle was synthesized by multistep co-precipitation method. • The synthesis parameters were controlled precisely to prepare high quality powder. • The relative density of highly crystalline IGZO tablet is as high as 97.30%. • IGZO tablet exhibited highly crystalline structure and the large grain size

Synthesis and properties of Oxasmaragdyrins containing one Five ...

Indian Academy of Sciences (India)

pioneering synthesis of Vitamin B12.2a However, the first synthesis of .... 2.3b Compound 3: Yield 22% (135 mg); 1H NMR. (500 MHz, CDCl3, 25 .... (b). Figure 1. (a) 1H NMR and (b) 1H-1H COSY NMR spectrum of compound 4 recorded in CDCl3 at room temperature. The double crossed peak in (a) and an asterix marked ...

Lanthanide ions doped Y2Sn2O7 nano-particles: low temperature synthesis and photoluminescence study

International Nuclear Information System (INIS)

Nigam, Sandeep; Sudarsan, V.; Vatsa, R.K.

2008-01-01

During the past decade, pyrochlore-type oxides (A 2 B 2 O 7 ) have emerged as important host matrices for lanthanide doped luminescent materials due to their higher thermal stability. Up to now, conventional solid-state reaction is the most commonly used synthetic method for preparation, of rare-earth pyrochlore oxides. This synthesis route employs a solid-state reaction of metal-oxide with appropriate rare-earth oxides at high temperature (>1200 deg C) for a long time (several days). However, in present work, Y 2 Sn 2 O 7 nanoparticles co-doped with lanthanide ions Tb 3+ and Ce 3+ were prepared based on the urea hydrolysis of Y 3+ , Sn 4+ , and Ln 3+ in ethylene glycol medium at 150 deg C followed by heating at 500, 700 and 900 deg C

Synthesis of Li{sub 2}SiO{sub 3} at low temperature; Sintesis de Li{sub 2}SiO{sub 3} a baja temperatura

Energy Technology Data Exchange (ETDEWEB)

Mondragon G, G. [ININ, 52750 La Marquesa, Estado de Mexico (Mexico)

2007-07-01

The main objective of this work is to develop a new synthesis method to obtain one of the more studied ceramics in this field Li{sub 2}SiO{sub 3}) in a simple and economic way using different solutions (urea and ammonium hydroxide). The particular objectives are first to prepare the Li{sub 2}SiO{sub 3} ceramic, by means of the use of the reaction conventional technique in solid state at temperatures between 800 and 900 C to compare it with the one proposed in this work and this way to observe the advantages that it would gives us the new method. Later on, the same one was synthesized lithium ceramic (Li{sub 2}SiO{sub 3}) by means of the new method at low temperature (between 80 and 90 C), using silicic acid and lithium hydroxide like precursory reagents and different solutions (urea and ammonium hydroxide) for the optimization in their synthesis. Finally, it was carried out the characterization of these materials by means of X-ray diffraction (XRD), electronic microscopes (SEM and TEM), nitrogen physisorption (method BET) and thermal gravimetric analysis (TGA) to observe the differences that exist among the conventional method and the proposed method and by this way to determine the advantages of the last method. (Author)

Integrated methanol synthesis

International Nuclear Information System (INIS)

Jaeger, W.

1982-01-01

This invention concerns a plant for methanol manufacture from gasified coal, particularly using nuclear power. In order to reduce the cost of the hydrogen circuits, the methanol synthesis is integrated in the coal gasification plant. The coal used is gasified with hydration by means of hydrogen and the crude gas emerging, after cooling and separating the carbon dioxide and hydrogen sulphide, is mixed with the synthetic gas leaving the methane cracking furnace. This mixture is taken to the methanol synthesis and more than 90% is converted into methanol in one pass. The gas mixture remaning after condensation and separation of methanol is decomposed into three fractions in low temperature gas decomposition with a high proportion of unconverted carbon monoxide. The flow of methane is taken to the cracking furnace with steam, the flow of hydrogen is taken to the hydrating coal gasifier, and the flow of carbon monoxide is taken to the methanol synthesis. The heat required for cracking the methane can either be provided by a nuclear reactor or by the coke left after hydrating gasification. (orig./RB) [de

Synthesis of nanocrystalline Gd doped ceria by combustion technique

DEFF Research Database (Denmark)

Jadhav, L. D.; Chourashiya, M. G.; Subhedar, K. M.

2009-01-01

chemical method of combustion where in the combustion of precursors results in the formation of nanoparticles relatively at lower processing temperature. The thermogravimetric study was carried out to understand the ignition temperature and optimize the fuel-to-oxidant ratio. The successful synthesis...

High-temperature synthesis of highly hydrothermal stable mesoporous silica and Fe-SiO2 using ionic liquid as a template

International Nuclear Information System (INIS)

Liu, Hong; Wang, Mengyang; Hu, Hongjiu; Liang, Yuguang; Wang, Yong; Cao, Weiran; Wang, Xiaohong

2011-01-01

Mesoporous silicas and Fe-SiO 2 with worm-like structures have been synthesized using a room temperature ionic liquid, 1-hexadecane-3-methylimidazolium bromide, as a template at a high aging temperature (150-190 o C) with the assistance of NaF. The hydrothermal stability of mesoporous silica was effectively improved by increasing the aging temperature and adding NaF to the synthesis gel. High hydrothermally stable mesoporous silica was obtained after being aged at 190 o C in the presence of NaF, which endured the hydrothermal treatment in boiling water at least for 10 d or steam treatment at 600 o C for 6 h. The ultra hydrothermal stability could be attributed to its high degree of polymerization of silicate. Furthermore, highly hydrothermal stable mesoporous Fe-SiO 2 has been synthesized, which still remained its mesostructure after being hydrothermally treated at 100 o C for 12 d or steam-treated at 600 o C for 6 h. -- Graphical abstract: Worm-like mesoporous silica and Fe-SiO 2 with high hydrothermal stability have been synthesized using ionic liquid 1-hexadecane-3-methylimidazolium bromide as a template under the assistance of NaF at high temperature. Display Omitted Research highlights: → Increasing aging temperature improved the hydrothermal stability of materials. →Addition of NaF enhanced the polymerization degree of silicates. → Mesoporous SiO 2 and Fe-SiO 2 obtained have remarkable hydrothermal stability.

Effect of heat stress on the pattern of protein synthesis in wheat endosperm

International Nuclear Information System (INIS)

Inwood, W.; Bernardin, J.

1990-01-01

The exposure of detached wheat heads (T. aestivum L. cv Cheyenne) to elevated temperatures resulted not only in the induction of a typical set of high and low molecular weight heat shock proteins (hsps), but also in a differential effect on the synthesis of wheat storage proteins in endosperm tissue when monitored by SDS PAGE of 35 S-labeled polypeptides. The synthesis of hsps in the endosperm had a rapid onset, reached a maximum rate within the first 2 hours at 40 degree C, and then steadily decreased during the next four hours. When heads were returned to 25 degree C after 3 hours at 40 degree C, hsp synthesis did not cease abruptly, but gradually declined over the next several hours. High molecular weight glutenin protein synthesis was drastically reduced with the same time course as heat shock protein synthesis was induced at 40 degree C. Conversely, the synthesis of gliadin proteins remained at a high level at 40 degree C. The synthesis rates for glutenin and gliadin proteins remained at low and high levels, respectively, for as long as the elevated temperature was maintained up to 7 hours

One-pot low-temperature green synthesis of magnetic graphene nanocomposite for the selective reduction of nitrobenzene

Science.gov (United States)

Haridas, Vijayasree; Sugunan, Sankaran; Narayanan, Binitha N.

2018-06-01

In the present study, a green one-pot low-temperature method is adopted for the synthesis of a novel magnetic graphene nanocomposite catalyst. Graphene preparation is performed without employing any oxidizing agents or corrosive chemicals, under mild sonication in isopropyl alcohol - water mixture. Monolayered nanoplatelets of graphene are obtained in the green solvent mixture and the composite material is found to be ferromagnetic in nature, obvious from the vibrating sample magnetometric measurements. Fe in the nanocomposite exists in two different forms i.e., α-Fe2O3 and α-FeOOH, as evident from the material characterization results. The graphene nanocomposite is found to be highly efficient in the selective reduction of nitrobenzene to aniline under solvent free reaction conditions and magnetic separation of this fine nanomaterial from the reaction mixture is successfully carried out. The catalyst is efficiently reusable till five repeated cycles.

ROOM TEMPERATURE BULK AND TEMPLATE-FREE SYNTHESIS OF LEUCOEMARLDINE POLYANILINE NANOFIBERS

Science.gov (United States)

An extremely simple single-step method is described for the bulk synthesis of nanofibers of the electronic polymer polyaniline in fully reduced state (leucoemarldine form) without using any reducing agents, surfactants, and/or large amounts of insoluble templates. Chemical oxida...

Self-propagating high-temperature synthesis of La(Sr)Ga(Mg)O{sub 3-{delta}} for electrolyte of solid oxide fuel cells

Energy Technology Data Exchange (ETDEWEB)

Ishikawa, Hiroyuki [Center for Advanced Research of Energy Conversion Materials, Hokkaido University, Sapporo 060-8628 (Japan); Enoki, Makiko [Department of Applied Chemistry, Faculty of Engineering, Kyusyu University, Fukuoka 812-8581 (Japan); Ishihara, Tatsumi [Department of Applied Chemistry, Faculty of Engineering, Kyusyu University, Fukuoka 812-8581 (Japan); Akiyama, Tomohiro [Center for Advanced Research of Energy Conversion Materials, Hokkaido University, Sapporo 060-8628 (Japan)]. E-mail: takiyama@eng.hokudai.ac.jp

2007-03-14

This paper describes self-propagating high-temperature synthesis (SHS) of an electrolyte for solid oxide fuel (SOFC), in comparison to a conventional solid-state reaction method (SRM). Doped-lanthanum gallate: La{sub 0.9}Sr{sub 0.1}Ga{sub 0.8}Mg{sub 0.2}O{sub 3-{delta}} (LSGM9182) and LSGM9173 as the SOFC electrolyte, was prepared by the SHS and sintered at different temperatures, for measuring the electrical conductivity of the sintered LSGM and the power generating performance at 1073 K, in comparison to the SRM. In the SHS, the LSGM powders with smaller size were obtained and easily sintered at the 100 K-lower temperature, 1673 K, than in the SRM. Most significantly, the electrical conductivity of the sintered LSGM9182 was as high as 0.11 S cm{sup -1} and its maximum power density was a value of 245 mW cm{sup -2} in the cell configuration of Ni/LSGM9182 (0.501 mm in thickness)/Sm{sub 0.5}Sr{sub 0.5}CoO{sub 3}. The conclusion was that the proposed SHS-sintering method with many benefits of minimizing the energy requirement and the processing time in the production, easing temperature restriction for the sintering, and improving the electrolyte performance up to a conventional level is practicable for producing the LSGM-electrolyte of SOFC at an intermediate-temperature application.

Maximization of fructose esters synthesis by response surface methodology.

Science.gov (United States)

Neta, Nair Sampaio; Peres, António M; Teixeira, José A; Rodrigues, Ligia R

2011-07-01

Enzymatic synthesis of fructose fatty acid ester was performed in organic solvent media, using a purified lipase from Candida antartica B immobilized in acrylic resin. Response surface methodology with a central composite rotatable design based on five levels was implemented to optimize three experimental operating conditions (temperature, agitation and reaction time). A statistical significant cubic model was established. Temperature and reaction time were found to be the most significant parameters. The optimum operational conditions for maximizing the synthesis of fructose esters were 57.1°C, 100 rpm and 37.8 h. The model was validated in the identified optimal conditions to check its adequacy and accuracy, and an experimental esterification percentage of 88.4% (±0.3%) was obtained. These results showed that an improvement of the enzymatic synthesis of fructose esters was obtained under the optimized conditions. Copyright © 2011 Elsevier B.V. All rights reserved.

Novel Synthesis of Ultra-Small Dextran Coated Maghemite Nanoparticles for MRI and CT Contrast Agents via a Low Temperature Co-Precipitation Reaction.

Science.gov (United States)

Rabias, Ioannis; Fardis, Michael; Kehagias, Thomas; Kletsas, Dimitris; Pratsinis, Harris; Tsitrouli, Danai; Maris, Thomas G; Papavassiliou, George

2015-01-01

Ultra-small dextran coated maghemite nanoparticles are synthesized via a low temperature modified co-precipitation method. A monoethylene glycol/water solution of 1:1 molar ratios and a fixed apparatus is used at a constant temperature of 5-10 degrees C. The growth of nanoparticles is prohibited due to low temperature synthesis and differs from usual thermal decomposition methods via Ostwald ripening. Strict temperature control and reaction timing of less than 20 minutes are essential to maintain narrow distribution in particle size. These nanoparticles are water-dispersible and biocompatible by capping with polyethylene glycol ligands. The aqueous suspensions are tested for cytotoxic activity on normal human skin fibroblasts. There is no reduction of the cells' viability at any concentration tested, the highest being 1% v/v of the suspension in culture medium, corresponding to the highest concentrations to be administered in vivo. Initial comparison with a T1 MRI contrast agent in sale shows that maghemite nanoparticles exhibit high r1 and r2 relaxivities in MRI tomography and strong contrast in computed tomography, demonstrating that these nanoparticles can be efficient T1, T2 and CT contrast agents.

Microfluidic Reactors for the Controlled Synthesis of Nanoparticles

Science.gov (United States)

Erdem, Emine Yegan

Nanoparticles have attracted a lot of attention in the past few decades due to their unique, size-dependent properties. In order to use these nanoparticles in devices or sensors effectively, it is important to maintain uniform properties throughout the system; therefore nanoparticles need to have uniform sizes -- or monodisperse. In order to achieve monodispersity, an extreme control over the reaction conditions is required during their synthesis. These reaction conditions such as temperature, concentration of reagents, residence times, etc. affect the structure of nanoparticles dramatically; therefore when the conditions vary locally in the reaction vessel, different sized nanoparticles form, causing polydispersity. In widely-used batch wise synthesis techniques, large sized reaction vessels are used to mix and heat reagents. In these types of systems, it is very hard to avoid thermal gradients and to achieve rapid mixing times as well as to control residence times. Also it is not possible to make rapid changes in the reaction parameters during the synthesis. The other drawback of conventional methods is that it is not possible to separate the nucleation of nanoparticles from their growth; this leads to combined nucleation and growth and subsequently results in polydisperse size distributions. Microfluidics is an alternative method by which the limitations of conventional techniques can be addressed. Due to the small size, it is possible to control temperature and concentration of reagents precisely as well as to make rapid changes in mixing ratios of reagents or temperature of the reaction zones. There have been several microfluidic reactors -- (microreactors) in literature that were designed to improve the size distribution of nanoparticles. In this work, two novel microfluidic systems were developed for achieving controlled synthesis of nanoparticles. The first microreactor was made out of a chemically robust polymer, polyurethane, and it was used for low

Silicon carbide production by Self-Propagating High Temperature (SHS) technique

International Nuclear Information System (INIS)

Lima, Eduardo de Souza; Schneider, Pedro Luiz; Mattoso, Irani Guedes; Costa, Carlos Roberto Correia da; Louro, Luis Henrique Leme

1997-01-01

Samples of silicon carbide (SiC) were synthesized from a mixture of silicon and carbon powders, using the Self-Propagating High Temperature Synthesis (SHS) technique. Three mixtures were tried, using silicon particles of the same average size but carbon particles of different average sizes. The method tried is characterized by an ignition temperature of 1450 deg C and the short duration of the synthesis ( 2-3 min). The samples were characterized by X-ray diffraction and scattering electron microscopy. (author)

Honey Mediated Green Synthesis of Nanoparticles: New Era of Safe Nanotechnology

Directory of Open Access Journals (Sweden)

Eranga Roshan Balasooriya

2017-01-01

Full Text Available With the advent of nanotechnology, many related industries rapidly developed over the recent past. Generally, top-down and bottom-up approaches are the two major processes used to synthesize nanoparticles; most of these require high temperatures, vacuum conditions, and harsh/toxic chemicals. As a consequence, adverse effects impacted organisms including humans. Some synthesis methods are expensive and time-consuming. As a corollary, the concept of “green nanotechnology” emerged with the green synthesis of nanoparticles commencing a new epoch in nanotechnology. This involves the synthesis of nanomaterial from microorganisms, macroorganisms, and other biological materials. Honey is documented as the world’s oldest food source with exceptional medical, chemical, physical, and pharmaceutical values. Honey mediated green synthesis is a relatively novel concept used during the past few years to synthesize gold, silver, carbon, platinum, and palladium nanoparticles. Honey acts as both a stabilizing and a reducing agent and importantly functions as a precursor in nanoparticle synthesis. This method usually requires room temperature and does not produce toxic byproducts. In conclusion, honey mediated green synthesis of nanoparticles provides a simple, cost effective, biocompatible, reproducible, rapid, and safe method. The special activity of honey functionalized nanoparticles may provide valuable end products with numerous applications in diverse fields.

Effect of pretreatment temperature on catalytic performance of the catalysts derived from cobalt carbonyl cluster in Fischer-Tropsch Synthesis

Directory of Open Access Journals (Sweden)

Byambasuren O

2017-02-01

Full Text Available The monometallic cobalt-based catalysts were prepared by pretreating the catalysts derived from carbonyl cluster precursor (CO6Co2CC(COOH2 supported on γ-Al2O3 with hydrogen at 180, 220, and 260°C respectively. The temperature effect of the pretreatments on the structure evolution of cluster precursors and the catalytic performance of the Fischer-Tropsch (F-T synthesis was investigated. The pretreated catalyst at 220°C with unique phase structure exhibited best catalytic activity and selectivity among three pretreated catalysts. Moreover, the catalysts exhibited high dispersion due to the formation of hydrogen bonds between the cluster precursor and γ-Al2O3 support.

Electrochemical Synthesis of Ammonia from Water and Nitrogen using a Pt/GDC/Pt Cell

Energy Technology Data Exchange (ETDEWEB)

Kim, Jong Nam; Yoo, Chung-Yul; Joo, Jong Hoon; Yu, Ji Haeng; Sharma, Monika; Yoon, Hyung Chul [Korea Institute of Energy Research, Daejeon (Korea, Republic of); Jeoung, Hana; Song, Ki Chang [Konyang University, Nonsan (Korea, Republic of)

2014-02-15

Electrochemical ammonia synthesis from water and nitrogen using a Pt/GDC/Pt cell was experimentally investigated. Electrochemical analysis and ammonia synthesis in the moisture-saturated nitrogen environment were performed under the operating temperature range 400-600 .deg. C and the applied potential range OCV (Open Circuit Voltage)-1.2V. Even though the ammonia synthesis rate was augmented with the increase in the operating temperature (i.e.. increase in the applied current) under the constant potential, the faradaic efficiency was decreased because of the limitation of dissociative chemisorption of nitrogen on the Pt electrode. The maximum synthesis rate of ammonia was 3.67x10{sup -11} mols{sup -1}cm{sup -2} with 0.1% faradaic efficiency at 600 .deg. C.

Effect of Temperature and Mole Ratio on the Synthesis Yield of Rhenium-Tetrofosmin

Directory of Open Access Journals (Sweden)

Widyastuti

2015-08-01

Full Text Available Technetium-99m (99mTc tetrofosmin is widely used in nuclear medicine as a diagnostic agent for myocardial perfusion and as a tumor imaging agent. As a parenteral preparation it requires an evaluation of its pharmacokinetics and stability in-vivo. Since 99mTc has a short half-life and is only available in very low concentrations, it is impossible to characterize its chemical properties and presence in the body. Due to this reason, only technetium-99 (T1/2 = 5 × 105 years, which is available in macro quantities, or natural rhenium can be used for this purpose. In this study rhenium-188 (188Re tetrofosmin will be synthesized and applied, because non-radioactive Re can be easily obtained. Synthesis and radiochemical purity analysis of carrier-added 188Re-tetrofosmin were carried out as a model to study the in-vivo stability of technetium-99m tetrofosmin. Rhenium-188 was used as a tracer to identify the formation of rhenium tetrofosmin. Rhenium gluconate was synthesized first prior to the formation of rhenium tetrofosmin. The quality of labeling for both rhenium gluconate and rhenium tetrofosmin was analyzed using paper- and thin-layer chromatography, respectively. Rhenium gluconate can be synthesized with high labeling yield within 1 hour, whereas rhenium tetrofosmin was synthesized both in room temperature and in an elevated temperature with various tetrofosmin-to-rhenium mole ratios.The results showed that heating at 95oC led to a higher yield of more than 90% within 30 minutes. Rhenium tetrofosmin could be produced in high radiochemical purity using an excess of tetrofosmin with mole ratio of 2000. It is concluded that rhenium tetrofosmin could be synthesized through the formation of rhenium gluconate, and a higher yield could be obtained in a shorter time by heating process.

Sol-Gel Synthesis Of Aluminoborosilicate Powders

Science.gov (United States)

Bull, Jeffrey; Leiser, Daniel; Selvaduray, Guna

1992-01-01

Application of sol-gel process to synthesis of aluminoborosilicate powders shows potential for control of microstructures of materials. Development of materials having enhanced processing characteristics prove advantageous in extending high-temperature endurance of fibrous refractory composite insulation made from ceramic fibers.

Synthesis of Binary Magnesium-Transition Metal Oxides via Inverse Coprecipitation

Science.gov (United States)

Yagi, Shunsuke; Ichikawa, Yuya; Yamada, Ikuya; Doi, Takayuki; Ichitsubo, Tetsu; Matsubara, Eiichiro

2013-02-01

Synthesis of binary magnesium-transition metal oxides, MgM2O4 (M: Cr, Mn, Fe, Co) and MgNiO2, was performed by calcination at relatively low temperatures of 500 and 750 °C for 24 h through inverse coprecipitation of carbonate hydroxide precursors. The important roles of the precipitation agent, sodium carbonate, were clarified by considering equilibria in an aqueous solution. The structure parameters of the obtained binary magnesium-transition metal oxide powders, specifically the occupancy of atomic sites, were evaluated from synchrotron X-ray diffraction (XRD) profiles by Rietveld refinement in addition to the magnetic properties at room temperature. The present work provides general guidelines for low-cost and high-volume synthesis of complex oxides, which are easily decomposed at high temperatures.

Self-propagating high-temperature synthesis flammable range and dominant parameters for synthesizing several ceramics and intermetallic compounds under heat-loss condition

International Nuclear Information System (INIS)

Makino, Atsushi

1996-01-01

Extensive comparisons have been conducted between experimental and theoretical results for the nonadiabatic self-propagating high-temperature synthesis combustion characteristics of many solid-solid systems subjected to volumetric heat loss. The nonadiabatic flame propagation theory--which describes the premixed mode of bulk flame propagation supported by the nonpremixed reaction of dispersed nonmetal (or higher-melting point metal) particles in the liquid metal, with finite-rate reaction at the particle surface and temperature-sensitive Arrhenius-type condensed-phase mass diffusivity--is used to compare with experimental results with heat loss. Systems examined are ceramics (TiC, TiB 2 , and ZrB 2 ) and intermetallic compounds (NiAl, TiCo, and TiNi). By using a consistent set of physicochemical parameters for these systems, satisfactory quantitative agreement is demonstrated for the flammable range (defined in terms of the mixture ratio, degree of dilution, particle size, and/or compact diameter)

Dielectric response of capacitor structures based on PZT annealed at different temperatures

Energy Technology Data Exchange (ETDEWEB)

Kamenshchikov, Mikhail V., E-mail: Mikhailkamenshchikov@yandex.ru [Tver State University, 170002, Tver (Russian Federation); Solnyshkin, Alexander V. [Tver State University, 170002, Tver (Russian Federation); Pronin, Igor P. [Ioffe Institute, 194021, St. Petersburg (Russian Federation)

2016-12-09

Highlights: • Correlation of the microstructure of PZT films and dielectric response was found. • Difference of dielectric responses under low and high bias is caused by domains. • Internal fields is discussed on the basis of the space charges. • Dependences of PZT films characteristics on synthesis temperature are extremal. - Abstract: Dielectric response of thin-film capacitor structures of Pt/PZT/Pt deposited by the RF magnetron sputtering method and annealed at temperatures of 540–570 °C was investigated. It was found that dielectric properties of these structures depend on the synthesis temperature. Stability of a polarized state is considered on the basis of the analysis of hysteresis loops and capacitance–voltage (C–V) characteristics. The contribution of the domain mechanism in the dielectric response of the capacitor structure comprising a ferroelectric is discussed. Extreme dependences of electrophysical characteristics of PZT films on their synthesis temperature were observed. Correlation of dielectric properties with microstructure of these films is found out.

PVT modeling of reservoir fluids using PC-SAFT EoS and Soave-BWR EoS

DEFF Research Database (Denmark)

Yan, Wei; Varzandeh, Farhad; Stenby, Erling Halfdan

2015-01-01

non-cubic EoS models, such as the Perturbed Chain Statistical Associating Fluid Theory (PC-SAFT) EoS and the Soave modified Benedict-Webb-Rubin (Soave-BWR) EoS, may partly replace the roles of these classical cubic models in the upstream oil industry. Here, we attempt to make a comparative study...... for the four models. For PVT prediction, the non-cubic models show advantages in some high pressure high temperature (HPHT) fluids but no clear advantages in general, indicating the necessity for further improvement of the characterization procedure....

Study of the synthesis of nanocrystalline mixed tantalum–zirconium carbide

Energy Technology Data Exchange (ETDEWEB)

Simonenko, E. P., E-mail: ep-simonenko@mail.ru; Simonenko, N. P.; Ezhov, Yu. S.; Sevastyanov, V. G.; Kuznetsov, N. T. [Russian Academy of Sciences, Kurnakov Institute of General and Inorganic Chemistry (Russian Federation)

2015-12-15

The synthesis conditions of refractory tantalum–zirconium carbide Ta{sub 0.8}Zr{sub 0.2}C on the basis of Ta{sub 2}O{sub 5}–ZrO{sub 2}–C ultrafine initial blend prepared via the sol–gel method are explored. The initial blend is prepared via hydrolysis in the presence of Ta(OC{sub 5}H{sub 11}){sub 5} and [Zr(O{sub 2}C{sub 5}H{sub 7}){sub 4–x}(OC{sub 5}H{sub 11}){sub x}] carbon source polymer solutions, gel drying, and carbonization at a temperature of 450°C. A series of the carbothermal synthesis experiments is implemented at various temperatures and exposure times. The synthesis conditions are shown to affect not only the phase composition of products but also their oxidation resistance related to the particle size.

Biomimetic and Aggregation-Driven Crystallization Route for Room-Temperature Material Synthesis: Growth of β-Ga2O3 Nanoparticles Using Peptide Assemblies as Nanoreactors

Science.gov (United States)

Lee, Sang-Yup; Gao, Xueyun; Matsui, Hiroshi

2008-01-01

The room temperature synthesis of β-Ga2O3 nanocrystal was examined by coupling two biomimetic crystallization techniques, the enzymatic peptide nano-assembly templating and the aggregation-driven crystallization. The catalytic template of peptide assembly nucleated and mineralized primary β-Ga2O3 crystals, and then fused them to grow single-crystalline and monodisperse nanoparticles in the cavity of the peptide assembly at room temperature. In this work, the peptide assembly was exploited as a nano-reactor with an enzymatic functionality catalyzing the hydrolysis of gallium precursors. In addition, the characteristic ring-structure of peptide assembly is expected to provide an efficient dehydration pathway and the crystallization control over the surface tension, which are advantageous for the β-Ga2O3 crystal growth. This multifunctional peptide assembly could be applied for syntheses of a variety of nanomaterials that are kinetically difficult to grow at room temperature. PMID:17302413

Control of DNA synthesis in inhibited and activated Agrostemma githago seeds

Energy Technology Data Exchange (ETDEWEB)

Hecker, M [Sektion Biologie, FG Algemeine Botanik und Pflanzenphysiologie, Universitaet Greifswald (German Democratic Republic)

1975-01-01

The relationships between DNA synthesis and germination capacity of Agrostemma seeds had been studied. Protein synthesis and RNA synthesis were activated at the very beginning of imbibition, whereas DNA synthesis started in the second part of the imbibition phase. Agrostemma seeds inhibited by higher temperature (30 degC), or aged seeds with a low germination capacity were characterized by a significantly reduced protein synthesis. DNA synthesis was also reduced. The inhibition of the protein synthesis of Agrostemma embryos fed with cycloheximide or actinomycin D caused a depression of DNA synthesis. The results indicated that the initiation of DNA synthesis of imbibing Agrostemma seeds depended on the synthesis of special proteins. Abscisic acid inhibited the growth as well as DNA synthesis of isolated Agrostemma embryos. Nitomycin inhibited germination and DNA synthesis to the same extent. Dormant seeds with an undiminished intensity of protein synthesis also showed a reduced incorporation of /sup 3/H-thymidine by DNA. It is suggested that DNA synthesis of imbibed seeds, which is a necessary prerequisite for the radicle protrusion, was involved in the mechanism of ripening of the Agrostemma seeds.

Control of DNA synthesis in inhibited and activated Agrostemma githago seeds

International Nuclear Information System (INIS)

Hecker, M.

1975-01-01

The relationships between DNA synthesis and germination capacity of Agrostemma seeds had been studied. Protein synthesis and RNA synthesis were activated at the very beginning of imbibition, whereas DNA synthesis started in the second part of the imbibition phase. Agrostemma seeds inhibited by higher temperature (30 degC), or aged seeds with a low germination capacity were characterized by a significantly reduced protein synthesis. DNA synthesis was also reduced. The inhibition of the protein synthesis of Agrostemma embryos fed with cycloheximide or actinomycin D caused a depression of DNA synthesis. The results indicated that the initiation of DNA synthesis of imbibing Agrostemma seeds depended on the synthesis of special proteins. Abscisic acid inhibited the growth as well as DNA synthesis of isolated Agrostemma embryos. Nitomycin inhibited germination and DNA synthesis to the same extent. Dormant seeds with an undiminished intensity of protein synthesis also showed a reduced incorporation of 3 H-thymidine by DNA. It is suggested that DNA synthesis of imbibed seeds, which is a necessary prerequisite for the radicle protrusion, was involved in the mechanism of ripening of the Agrostemma seeds. (author)

Process assessment of small scale low temperature methanol synthesis

International Nuclear Information System (INIS)

Hendriyana; Susanto, Herri; Subagjo

2015-01-01

Biomass is a renewable energy resource and has the potential to make a significant impact on domestic fuel supplies. Biomass can be converted to fuel like methanol via several step process. The process can be split into following main steps: biomass preparation, gasification, gas cooling and cleaning, gas shift and methanol synthesis. Untill now these configuration still has a problem like high production cost, catalyst deactivation, economy of scale and a huge energy requirements. These problems become the leading inhibition for biomass conversion to methanol, which should be resolved to move towards the economical. To address these issues, we developed various process and new configurations for methanol synthesis via methyl formate. This configuration combining two reactors: the one reactor for the carbonylation of methanol and CO to form methyl formate, and the second for the hydrogenolysis of methyl formate and H 2 to form two molecule of methanol. Four plant process configurations were compared with the biomass basis is 300 ton/day. The first configuration (A) is equipped with a steam reforming process for converting methane to CO and H 2 for increasing H 2 /CO ratio. CO 2 removal is necessary to avoid poisoning the catalyst. COSORB process used for the purpose of increasing the partial pressure of CO in the feed gas. The steam reforming process in B configuration is not used with the aim of reducing the number of process equipment, so expect lower investment costs. For C configuration, the steam reforming process and COSORB are not used with the aim of reducing the number of process equipment, so expect lower investment costs. D configuration is almost similar to the configuration A. This configuration difference is in the synthesis of methanol which was held in a single reactor. Carbonylation and hydrogenolysis reactions carried out in the same reactor one. These processes were analyzed in term of technical process, material and energy balance and economic

Process assessment of small scale low temperature methanol synthesis

Energy Technology Data Exchange (ETDEWEB)

Hendriyana [Chemical Engineering Department, Faculty of Engineering, Jenderal Achmad Yani Univerity (Indonesia); Chemical Engineering Department, Faculty of Industrial Technology, InstitutTeknologi Bandung (Indonesia); Susanto, Herri, E-mail: herri@che.itb.ac.id; Subagjo [Chemical Engineering Department, Faculty of Industrial Technology, InstitutTeknologi Bandung (Indonesia)

2015-12-29

Biomass is a renewable energy resource and has the potential to make a significant impact on domestic fuel supplies. Biomass can be converted to fuel like methanol via several step process. The process can be split into following main steps: biomass preparation, gasification, gas cooling and cleaning, gas shift and methanol synthesis. Untill now these configuration still has a problem like high production cost, catalyst deactivation, economy of scale and a huge energy requirements. These problems become the leading inhibition for biomass conversion to methanol, which should be resolved to move towards the economical. To address these issues, we developed various process and new configurations for methanol synthesis via methyl formate. This configuration combining two reactors: the one reactor for the carbonylation of methanol and CO to form methyl formate, and the second for the hydrogenolysis of methyl formate and H{sub 2} to form two molecule of methanol. Four plant process configurations were compared with the biomass basis is 300 ton/day. The first configuration (A) is equipped with a steam reforming process for converting methane to CO and H{sub 2} for increasing H{sub 2}/CO ratio. CO{sub 2} removal is necessary to avoid poisoning the catalyst. COSORB process used for the purpose of increasing the partial pressure of CO in the feed gas. The steam reforming process in B configuration is not used with the aim of reducing the number of process equipment, so expect lower investment costs. For C configuration, the steam reforming process and COSORB are not used with the aim of reducing the number of process equipment, so expect lower investment costs. D configuration is almost similar to the configuration A. This configuration difference is in the synthesis of methanol which was held in a single reactor. Carbonylation and hydrogenolysis reactions carried out in the same reactor one. These processes were analyzed in term of technical process, material and energy

Reverse microemulsion synthesis of layered gadolinium hydroxide nanoparticles

Science.gov (United States)

Xu, Yadong; Suthar, Jugal; Egbu, Raphael; Weston, Andrew J.; Fogg, Andrew M.; Williams, Gareth R.

2018-02-01

A reverse microemulsion approach has been explored for the synthesis of layered gadolinium hydroxide (LGdH) nanoparticles in this work. This method uses oleylamine as a multifunctional agent, acting as surfactant, oil phase and base. 1-butanol is additionally used as a co-surfactant. A systematic study of the key reaction parameters was undertaken, including the volume ratio of surfactant (oleylamine) to water, the reaction time, synthesis temperature, and the amount of co-surfactant (1-butanol) added. It proved possible to obtain pristine LGdH materials at temperatures of 120 °C or below with an oleylamine: water ratio of 1:4. Using larger amounts of surfactant or higher temperatures caused the formation of Gd(OH)3, either as the sole product or as a major impurity phase. The LGdH particles produced have sizes of ca. 200 nm, with this size being largely independent of temperature or reaction time. Adjusting the amount of 1-butanol co-surfactant added permits the size to be varied between 200 and 300 nm.

Urea-assisted low temperature green synthesis of graphene nanosheets for transparent conducting film

Science.gov (United States)

Chamoli, Pankaj; Das, Malay K.; Kar, Kamal K.

2018-02-01

Present work demonstrates the fabrication of graphene nanosheet (GN) based transparent conducting film (TCF) using spray coating. Green synthesis of GN is carried out by reduction of graphene oxide (GO) using urea as green reducing agent. The reductive ability of urea with varied concentration is studied for GO at low temperature (i.e., 90 °C). As synthesized graphene nanosheets (GNs) are characterized by Raman spectroscopy, Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), UV-visible spectroscopy, field emission scanning electron microscopy (FESEM), atomic force microscope (AFM), and X-ray Photon spectroscopy (XPS). Raman analysis confirms that the maximum reduction of oxygen species is noticed using 30 mg/ml urea concentration at 90 °C from GO, and found Raman D to G band ratio (ID/IG) of ∼1.30. XPS analysis validates the Raman signature of removal of oxygen functional groups from GO, and obtained C/O ratio of ∼5.28. Further, transparent conducting films (TCFs) are fabricated using synthesized GNs. Thermal graphitization is carried out to enhance the optical and electrical properties of TCFs. TCF shows best performance when it is annealed at 900 °C for 1 h in vacuum, and obtained sheet resistance is ∼1.89 kΩ/□ with transmittance of ∼62.53%.

Synthesis of aluminum oxide by the polymer precursor method (Pechini) in 4: 1 ratio of citric acid: metal cation: calcination temperature effect

International Nuclear Information System (INIS)

Silva, M.C.; Lira, H.L.; Ribeiro, P.C.; Freitas, N.L.

2014-01-01

The technology field is nanopowders prominent in science since these materials fall in various sectors regarding their applications. This work aims at the synthesis of aluminum oxide by polymeric precursors in 4:1 ratio of citric acid:metal cation and evaluate the influence of calcination temperature on their structural and morphological characteristics. The samples after reaction were characterized by XRD and thermal analysis. After calcination 500-1200°C the samples were characterized by XRD, SEM and particle size distribution. The results showed that the variation of the calcination temperature is sufficient to achieve a same material with different structural and morphological characteristics. The most stable phase aluminum oxide arose only after calcination at 1100°C, below 900°C, the amorphous material appeared. As regards the morphology, the change was not as significant as compared to the structure. (author)

Microwave-assisted one-step synthesis of acetate-capped NaYF4

DEFF Research Database (Denmark)

Reddy, Kumbam Lingeshwar; Prabhakar, Neeraj; Arppe, Riikka

2017-01-01

Acetate-capped hydrophilic cubic phase NaYF4:Yb/Er upconversion nanophosphors were effectively synthesized in a single step employing a facile microwave-assisted synthesis route by applying relatively low temperatures in a short span of time compared to the conventional synthetic methods. The nan......Acetate-capped hydrophilic cubic phase NaYF4:Yb/Er upconversion nanophosphors were effectively synthesized in a single step employing a facile microwave-assisted synthesis route by applying relatively low temperatures in a short span of time compared to the conventional synthetic methods...

Solvent-free and room temperature synthesis of 3-arylquinolines from different anilines and styrene oxide in the presence of Al2O3/MeSO3H

Directory of Open Access Journals (Sweden)

Hashem Sharghi

2017-09-01

Full Text Available A highly efficient, simple and environmentally friendly synthesis of 3-arylquinolines has been developed in the presence of Al2O3/MeSO3H via one-pot reaction of anilines and styrene oxide. This methodology provides very rapid access to 3-arylquinolines in good to excellent yields under solvent-free conditions at room temperature in air.

Hydrophilic Graphene Preparation from Gallic Acid Modified Graphene Oxide in Magnesium Self-Propagating High Temperature Synthesis Process

Science.gov (United States)

Cao, Lei; Li, Zhenhuan; Su, Kunmei; Cheng, Bowen

2016-10-01

Hydrophilic graphene sheets were synthesized from a mixture of magnesium and gallic acid (GA) modified graphene oxide (GO) in a self-propagating high-temperature synthesis (SHS) process, and hydrophilic graphene sheets displayed the higher C/O ratio (16.36), outstanding conductivity (~88900 S/m) and excellent water-solubility. GO sheets were connected together by GA, and GA was captured to darn GO structure defects through the formation of hydrogen bonds and ester bonds. In SHS process, the most oxygen ions of GO reacted with magnesium to prevent the escape of carbon dioxide and carbon monoxide to from the structure defects associated with vacancies, and GA could take place the high-temperature carbonization, during which a large-area graphene sheets formed with a part of the structure defects being repaired. When only GO was reduced by magnesium in SHS process, and the reduced GO (rGO) exhibited the smaller sheets, the lower C/O ratio (15.26), the weaker conductivity (4200 S/m) and the poor water-solubility because rGO inevitably left behind carbon vacancies and topological defects. Therefore, the larger sheet, less edge defects and free structure defects associated with vacancies play a key role for graphene sheets good dispersion in water.

Microwave-hydrothermal synthesis of barium strontium titanate nanoparticles

International Nuclear Information System (INIS)

Simoes, A.Z.; Moura, F.; Onofre, T.B.; Ramirez, M.A.; Varela, J.A.; Longo, E.

2010-01-01

Research highlights: → Barium strontium titanate nanoparticles were obtained by the Hydrothemal microwave technique (HTMW) → This is a genuine technique to obtain nanoparticles at low temperature and short times → Barium strontium titanate free of carbonates with tetragonal structure was grown at 130 o C. - Abstract: Hydrothermal-microwave method (HTMW) was used to synthesize crystalline barium strontium titanate (Ba 0.8 Sr 0.2 TiO 3 ) nanoparticles (BST) in the temperature range of 100-130 o C. The crystallization of BST with tetragonal structure was reached at all the synthesis temperatures along with the formation of BaCO 3 as a minor impurity at lower syntheses temperatures. Typical FT-IR spectra for tetragonal (BST) nanoparticles presented well defined bands, indicating a substantial short-range order in the system. TG-DTA analyses confirmed the presence of lattice OH- groups, commonly found in materials obtained by HTMW process. FE/SEM revealed that lower syntheses temperatures led to a morphology that consisted of uniform grains while higher syntheses temperature consisted of big grains isolated and embedded in a matrix of small grains. TEM has shown BST nanoparticles with diameters between 40 and 80 nm. These results show that the HTMW synthesis route is rapid, cost effective, and could serve as an alternative to obtain BST nanoparticles.

Synthesis of graphene by MEVVA source ion implantation

International Nuclear Information System (INIS)

Ying, J.J.; Xiao, X.H.; Dai, Z.G.; Wu, W.; Li, W.Q.; Mei, F.; Cai, G.X.; Ren, F.; Jiang, C.Z.

2013-01-01

Ion implantation provides a new synthesis route for graphene, and few-layered graphene synthesis by ion implantation has been reported. Here we show the synthesis of a single layer of high-quality graphene by Metal Vapor Vacuum Arc (MEVVA) source ion implantation. Polycrystalline nickel and copper thin films are implanted with MEVVA source carbon ions at 40 kV, followed by high-temperature thermal annealing and quenching. A Raman spectrum is applied to probe the quality and thickness of the prepared graphene. A single layer of high-quality graphene is grown on the nickel films, but not on the copper films. The growth mechanisms on the nickel and copper films are explained. MEVVA source ion implantation has been widely applied in industrial applications, demonstrating that this synthesis method can be generalized for industrial production

Synthesis and tribological properties of antimony N, N-diethanoldithiocarbamate

Institute of Scientific and Technical Information of China (English)

李丽; 黄可龙; 瞿龙; 舒万艮

2001-01-01

Antimony N, N-diethanoldithiocarbamate was synthesized with diethanolamine, antimony trioxide and carbon disulfide. The influences of temperature, reaction time, solvents and their dosages were investigated, and the optimum synthesis conditions were: reaction temperature 15～20 ℃, reaction time 2.5 h, 250 mL CH3OH as solvent and the hot CH3OH as recrystallization solvent. Element analysis, IR, 1HNMR and 13CNMR spectra were used to study its chemical composition and molecular structure. Antimony N, N-diethanol-dithiocarbamate was added in the base oil, and its properties of wear resistance and extreme pressure were studied by FB, FD and WSD. The synthesis product behaves per fectly as wear resistance and extreme pressure additive and its extreme pressure property is superior to its wear resistance property. The mechanism of tribological action was discussed by using XPS and AES spectra, and the reason of good wear resistance and extreme pressure properties is that the synthesis product decompose element C, S and N.

Mg-doped VO2 nanoparticles: hydrothermal synthesis, enhanced visible transmittance and decreased metal-insulator transition temperature.

Science.gov (United States)

Zhou, Jiadong; Gao, Yanfeng; Liu, Xinling; Chen, Zhang; Dai, Lei; Cao, Chuanxiang; Luo, Hongjie; Kanahira, Minoru; Sun, Chao; Yan, Liuming

2013-05-28

This paper reports the successful preparation of Mg-doped VO2 nanoparticles via hydrothermal synthesis. The metal-insulator transition temperature (T(c)) decreased by approximately 2 K per at% Mg. The Tc decreased to 54 °C with 7.0 at% dopant. The composite foils made from Mg-doped VO2 particles displayed excellent visible transmittance (up to 54.2%) and solar modulation ability (up to 10.6%). In addition, the absorption edge blue-shifted from 490 nm to 440 nm at a Mg content of 3.8 at%, representing a widened optical band gap from 2.0 eV for pure VO2 to 2.4 eV at 3.8 at% doping. As a result, the colour of the Mg-doped films was modified to increase their brightness and lighten the yellow colour over that of the undoped-VO2 film. A first principle calculation was conducted to understand how dopants affect the optical, Mott phase transition and structural properties of VO2.

High-temperature superconducting oxide synthesis and the chemical doping of the Cu-O planes

International Nuclear Information System (INIS)

Tarascon, J.M.; Barboux, P.; Bagley, B.G.; Greene, L.H.; McKinnon, W.R.; Hull, G.W.

1987-01-01

Different synthesis techniques for the preparation of dense superconducting ceramics are discussed, and a sol-gel process is shown to be very promising. The effect of oxygen content, and the effect of substitution of Ni and Zn for copper, on the structural, transport and superconducting properties of the La-Sr-Cu-O and Y-Ba-Cu-O systems are presented. The authors find that substitution on the copper sites destroys T/sub c/ in the La-Sr-Cu-O system and decreases it in the Y-Ba-Cu-O system, and this effect is insensitive as to whether the 3d metal is magnetic (Ni) or diamagnetic (Zn). A detailed study of the YBa/sub 2/Cu/sub 3/O/sub 7-y/ system as a function of oxygen content (y) shows that superconductivity can be destroyed in these materials by the removal of oxygen and restored by reinjecting oxygen; either thermally at 500 0 C or at temperatures (80 0 C) compatible with device processing by means of a novel plasma oxidation process. Of scientific interest, the plasma process induces bulk superconductivity in the undoped La/sub 2/CuO/sub 4/

Synthesis of nickel nanoparticles by hydrazine reduction: mechanistic study and continuous flow synthesis

International Nuclear Information System (INIS)

Eluri, Ravi; Paul, Brian

2012-01-01

The continuous synthesis of nickel nanoparticles (NiNPs) in a static microchannel T-mixer by the reduction of NiCl 2 ·6H 2 O in the presence of ethylene glycol without a stabilizing/capping agent was investigated. The nanoparticles were formed in accordance with the modified polyol process with hydrazine used as a reducing agent and NaOH as a catalyst for nanoparticle formation. The reaction mechanism for NiNP formation was investigated in batch with the help of Fourier transform infrared spectroscopy and X-ray diffraction (XRD) techniques. Parameters were found for reducing reaction times from 60 to 1 min. The effects of temperature (60–120 °C) and NaOH concentration (0.1 and 0.5 M) on batch-processed particle characteristics were also studied using XRD, transmission electron microscope and electron microprobe analysis. Average particle size was reduced from 9.2 ± 2.9 to 5.4 ± 0.9 nm at higher temperature and NaOH concentration. Adaptation of this chemistry to a static microchannel T-mixer for continuous synthesis resulted in smooth, spherical particles. Increases in the reaction temperature from 120 to 130 °C resulted in a narrow size distribution of 5.3 ± 1 nm and also resulted in magnetic properties of 5.1 emu/g (saturation magnetization), 1.1 emu/g (remanent magnetization), and 62 Oe (coercivity).

Hydrothermal synthesis of sodium titanate nanotubes; Hydrotermalna synteza nanorurok titanatu sodneho

Energy Technology Data Exchange (ETDEWEB)

Miskoci, M.; Jesenak, K. [Univerzita Komenskeho, Prirodovedecka fakulta, Katedra anorganickej chemie, 84215 Bratislava (Slovakia); Caplovicova, M. [Univerzita Komenskeho, Prirodovedecka fakulta, Katedra loziskovej geologie, 84215 Bratislava (Slovakia)

2013-04-16

From suspension of nanoparticles TiO{sub 2} in concentrated water solution of NaOH were prepared by hydrothermal synthesis sodium titanates particles with different shapes. Influence of synthesis duration under temperature 180 grad C on the change of particles shapes was observed. The result of experiment showed that one day synthesis resulted to obtained product with high content of nanotubes, but the extension of this period led to the transformation of product's shape into stripes. From the results of experiment follows that as a precursor for TiO{sub 2} nanotubes preparation may be used only products of hydrothermal synthesis, which duration of pressure synthesis was not longer than 24 hours. (authors)

Fabrication of FeAl Intermetallic Foams by Tartaric Acid-Assisted Self-Propagating High-Temperature Synthesis

Directory of Open Access Journals (Sweden)

Krzysztof Karczewski

2018-04-01

Full Text Available Iron aluminides are intermetallics with interesting applications in porous form thanks to their mechanical and corrosion resistance properties. However, making porous forms of these materials is not easy due to their high melting points. We formed FeAl foams by elemental iron and aluminum powders sintering with tartaric acid additive. Tartaric acid worked as an in situ gas-releasing agent during the self-propagating high-temperature synthesis of FeAl intermetallic alloy, which was confirmed by X-ray diffraction measurements. The porosity of the formed foams was up to 36 ± 4%. In the core of the sample, the average equivalent circle diameter was found to be 47 ± 20 µm, while on the surface, it was 35 ± 16 µm; thus, the spread of the pore size was smaller than reported previously. To investigate functional applications of the formed FeAl foam, the pressure drop of air during penetration of the foam was examined. It was found that increased porosity of the material increased the flow of the air through the metallic foam.

Combustion synthesis: A new approach for preparation of thermoelectric zinc antimonide compounds

Energy Technology Data Exchange (ETDEWEB)

Rouessac, F., E-mail: Florence.Rouessac@univ-montp2.fr [Institut Charles Gerhardt Montpellier, UMR 5253 CNRS-UM2-ENSCM-UM1, C2M Universite Montpellier 2, CC 1504 Place Eugene Bataillon, 34095 Montpellier Cedex 5 (France); Ayral, R.-M. [Institut Charles Gerhardt Montpellier, UMR 5253 CNRS-UM2-ENSCM-UM1, C2M Universite Montpellier 2, CC 1504 Place Eugene Bataillon, 34095 Montpellier Cedex 5 (France)

2012-07-25

Highlights: Black-Right-Pointing-Pointer Reliable preparation method of thermoelectric materials. Black-Right-Pointing-Pointer Formation of zinc antimonide by the combustion synthesis method is investigated. Black-Right-Pointing-Pointer XRD and Raman spectroscopy as a function of temperature. Black-Right-Pointing-Pointer SHS: a new way for synthesizing thermoelectric materials. - Abstract: Due to the interesting properties of Zn{sub 4}Sb{sub 3} thermoelectric material, a reliable preparation method of this material is required. In this study, the formation of zinc antimonides by the combustion synthesis method is investigated and subjected to characterization using X-ray diffraction and Raman spectroscopy as a function of temperature. The results show that combustion synthesis can be a new way for synthesizing these thermoelectric materials.

Synthesis of uniform-sized zeolite from windshield waste

International Nuclear Information System (INIS)

Kim, Jae-Chan; Choi, Mingu; Song, Hee Jo; Park, Jung Eun; Yoon, Jin-Ho; Park, Kyung-Soo; Lee, Chan Gi; Kim, Dong-Wan

2015-01-01

We demonstrate the synthesis of A-type zeolite from mechanically milled windshield waste via acid treatment and a low-temperature hydrothermal method. As-received windshield cullet was crushed to a fine powder and impurities were removed by HNO 3 treatment. The resulting glass powder was used as the source material for the hydrothermal synthesis of A-type zeolite. Crystal structure, morphology, and elemental composition changes of the windshield waste were evaluated at each step of the process through scanning electron microscopy, X-ray diffraction, X-ray fluorescence spectrometry, etc. After a high-energy milling process, the glass had an average particle size of 520 nm; after acid treatment, its composition was over 94% silica. Zeolite was successfully synthesized in the A-type phase with a uniform cubic shape. - Highlights: • Environmental-friendly recycling of windshield waste for high valuable product of zeolite. • Synthesis of zeolite form windshield waste via a low-temperature hydrothermal process. • High-energy milling effect on the uniform cubic shape and high-purity A-type zeolite.

Synthesis of InGaZnO{sub 4} nanoparticles using low temperature multistep co-precipitation method

Energy Technology Data Exchange (ETDEWEB)

Wu, Ming-Chung, E-mail: mingchungwu@mail.cgu.edu.tw; Hsiao, Kai-Chi; Lu, Hsin-Chun

2015-07-15

Indium gallium zinc oxide (InGaZnO{sub 4}, IGZO) has attracted explosive growth in investigations over the last decades as an important material in the thin-film transistor. In this study, the various nitrate precursors, including indium nitrate, gallium nitrate, and zinc nitrate, were prepared from the various metals dissolved in nitric acid. Then, we used these nitrate precursors to synthesize the IGZO precursor powder by the multistep co-precipitation method. The synthesis parameters of the co-precipitation method, such as reaction temperature, pH value and reaction time, were controlled precisely to prepare the high quality IGZO precursor powder. Finally, IGZO precursor powder was calcined at 900 °C. Then, the microstructure, the crystalline structure, the particle size distribution and specific surface area of calcined IGZO precursor powder were characterized by electron transmission microscopy, X-ray diffraction technique, dynamic light scattering method and the surface area and porosimetry analyzer, respectively. The relative density of IGZO tablet sintered at 1200 °C for 12 h is as high as 97.30%, and it showed highly InGaZnO{sub 4} crystalline structure and the large grain size. The IGZO nanoparticles developed in our study has the potential for the high quality target materials used in the application of electronic devices. - Graphical abstract: Display Omitted - Highlights: • InGaZnO{sub 4} (IGZO) nanoparticle was synthesized by multistep co-precipitation method. • The synthesis parameters were controlled precisely to prepare high quality powder. • The relative density of highly crystalline IGZO tablet is as high as 97.30%. • IGZO tablet exhibited highly crystalline structure and the large grain size.

Effects of process parameters on tungsten boride production from WO{sub 3} by self propagating high temperature synthesis

Energy Technology Data Exchange (ETDEWEB)

Yazici, Sertac [Metallurgical and Materials Engineering Department, Istanbul Technical University, Maslak, Istanbul 34469 (Turkey); Derin, Bora, E-mail: bderin@itu.edu.tr [Metallurgical and Materials Engineering Department, Istanbul Technical University, Maslak, Istanbul 34469 (Turkey)

2013-01-01

Highlights: Black-Right-Pointing-Pointer We produced tungsten boride compounds by SHS method. Black-Right-Pointing-Pointer Mg containing byproducts were leached out by using a hot aqueous HCl media. Black-Right-Pointing-Pointer The ratio of W{sub 2}B{sub 5}/WB was found to be {approx}2.0 containing minor phases of W{sub 2}B and W. - Abstract: In the present study, the production parameters of tungsten boride compounds by self-propagating high-temperature synthesis (SHS) method and following leaching process were investigated. In the SHS stage, the products consisting of tungsten borides, magnesium oxide, magnesium borate, and also minor compounds were obtained by using different initial molar ratios of WO{sub 3}, Mg and B{sub 2}O{sub 3} as starting materials. In the leaching step, Mg containing byproducts, i.e. MgO and Mg{sub 3}B{sub 2}O{sub 6}, existed in the selected SHS product synthesized at 1:8:2.5 initial molar ratio of WO{sub 3}:Mg:B{sub 2}O{sub 3} were leached out by using aqueous HCl solution to obtain clean tungsten boride compounds at different experimental parameters which are time, acid concentration and temperature. The acid leaching experiments of the SHS product showed that optimum leaching conditions could be achieved by using 5.8 M HCl at 1/10 S/L ratio and the temperature of 80 Degree-Sign C for 60 min.

Mineralizer-assisted high-pressure high-temperature synthesis and characterization of novel phosphorus nitride imides and luminescent alkaline earth metal (oxo)nitridophosphates

International Nuclear Information System (INIS)

Marchuk, Alexey

2016-01-01

The main objectives of this thesis were the synthesis, identification and structural characterization of new alkaline earth metal (oxo)nitridophopshates and phosphorus nitrides. Furthermore, luminescence properties of the resulting materials should be investigated and a connection between these properties and the respective structures should be established. For this purpose, a range of synthesis strategies was employed, including conventional solid-state syntheses in silica ampoules and high-pressure high-temperature syntheses using the multianvil technique. The emphasis of the synthetic part of this thesis lies on the development of new synthetic strategies in order to increase crystallinity of alkaline earth metal (oxo)nitridophosphates and thus accelerate their structure determination. This involves the selection of a suitable mineralizer and the investigation of its interaction with the respective starting materials. In addition, the analytical methods applied in this thesis in order to identify and characterize the compounds are just as essential as the synthesis strategies. X-ray diffraction on single crystals and on powders was carried out as the main analytical method while being supported by quantitative and qualitative 1 H and 31 P solid-state NMR measurements, FTIR and energy-dispersive X-ray (EDX) spectroscopy, as well as electron microscopy methods including both imaging and diffraction techniques. Implied by the large number of novel structures investigated, theoretical studies including topological analysis, calculations of lattice energies and bond-valence sums also played a major role in this thesis. Optical analysis methods such as reflectance spectroscopy, luminescence microscopy and photoluminescence measurements helped to determine the luminescence properties of some of the presented compounds.

Functional Properties of Porous Ti-48.0 at.% Ni Shape Memory Alloy Produced by Self-Propagating High-Temperature Synthesis

Science.gov (United States)

Resnina, Natalia; Belyaev, Sergey; Voronkov, Andrew

2018-03-01

The functional behavior of the porous shape memory alloy produced by self-propagating high-temperature synthesis from the Ti-48.0 at.% Ni powder mixture was studied. It was found that a large unelastic strain recovered on unloading and it was not attributed to the pseudoelasticity effect. A decrease in deformation temperatures did not influence the value of strain that recovered on unloading, while the effective modulus decreased from 1.9 to 1.44 GPa. It was found that the porous Ti-48.0 at.% Ni alloy revealed the one-way shape memory effect, where the maximum recoverable strain was 5%. The porous Ti-48.0 at.% Ni alloy demonstrated the transformation plasticity and the shape memory effects on cooling and heating under a stress. An increase in stress did not influence the shape memory effect value, which was equal to 1%. It was shown that the functional properties of the porous alloy were determined by the TiNi phase consisted of the two volumes Ti49.3Ni50.7 and Ti50Ni50 where the martensitic transformation occurred at different temperatures. The results of the study showed that the existence of the Ti49.3Ni50.7 volumes in the porous Ti-48.0 at.% Ni alloy improved the functional properties of the alloy.

Synthesis and characterization of actinide metal compounds formed by combustion

International Nuclear Information System (INIS)

Behrens, R.G.; King, M.A.

1985-01-01

This paper briefly describes the results of attempts to synthesize arsenides, phosphides, and antimonides of uranium and thorium using Self-Propagating High-Temperature Synthesis (SHS) techniques. This paper first summarizes the chemistry and thermodynamics of these chemical systems, describes SHS synthesis techniques, and then describes the results of the syntheses using data from powder x-ray diffraction, metallographic, and electron microprobe analyses

Study of Colloidal Gold Synthesis Using Turkevich Method

Science.gov (United States)

Rohiman, Asep; Anshori, Isa; Surawijaya, Akhmadi; Idris, Irman

2011-12-01

The synthesis of colloidal gold or Au-nanoparticles (Au-NPs) by reduction of chloroauric acid (HAuCl4) with sodium citrate was done using Turkevich method. We prepare HAuCl4 solution by dissolving gold wires (99.99%) into aqua regia solution. To initiate the Au-NPs synthesis 0.17 ml of 1 % chloroauric acid solution was heated to the boiling point and then 10 ml of 1 % sodium citrate was added to the boiling solution with a constant stirring in order to maintain a homogenous solution. A color of faint gray was observed in the solution approximately one minute and in a period of 2-3 minutes later, it further darkened to deep wine and red color. It showed that the gold solution has reduced to Au-NPs. The effect of process temperature on the size of Au-NPs prepared by sodium citrate reduction has also been investigated. With increasing temperature of Au-NPs synthesis, smaller-size Au-NPs were obtained. The higher temperatures shorten the time needed to achieve activation energy for reduction process. The resulting Au-NPs has been characterized by scanning Electron Microscope (SEM), showing the size of Au-NPs average diameter is ˜20-27 nm. The resulting colloidal gold will be used as catalyst for Si nanowires growth using VLS method.

Substrate independent approach for synthesis of graphene platelet networks

Science.gov (United States)

Shashurin, A.; Fang, X.; Zemlyanov, D.; Keidar, M.

2017-06-01

Graphene platelet networks (GPNs) comprised of randomly oriented graphene flakes two to three atomic layers thick are synthesized using a novel plasma-based approach. The approach uses a substrate capable of withstanding synthesis temperatures around 800 °C, but is fully independent of the substrate material. The synthesis occurs directly on the substrate surface without the necessity of any additional steps. GPNs were synthesized on various substrate materials including silicon (Si), thermally oxidized Si (SiO2), molybdenum (Mo), nickel (Ni) and copper (Cu), nickel-chromium (NiCr) alloy and alumina ceramics (Al2O3). The mismatch between the atomic structures of sp2 honeycomb carbon networks and the substrate material is fully eliminated shortly after the synthesis initiation, namely when about 100 nm thick deposits are formed on the substrate. GPN structures synthesized on a substrate at a temperature of about 800 °C are significantly more porous in comparison to the much denser packed amorphous carbon deposits synthesized at lower temperatures. The method proposed here can potentially revolutionize the area of electrochemical energy storage by offering a single-step direct approach for the manufacture of graphene-based electrodes for non-Faradaic supercapacitors. Mass production can be achieved using this method if a roll-to-roll system is utilized.

The Microwave-Assisted Green Synthesis of TiC Powders.

Science.gov (United States)

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.

GRINDING TECHNIQUE FOR THE TANDEM SYNTHESIS OF BIS ...

African Journals Online (AJOL)

pot ... reaction of one equivalent of synthesized aldehyde and two equivalent of ... Synthesis of biscoumarinylmethane 3a-k using [BDBDMIm]Brat room temperature.a ... Melting points were measured on an Electrothermal 9100 apparatus.

Room temperature synthesis of PbSe quantum dots in aqueous solution: Stabilization by interactions with ligands

Science.gov (United States)

Primera-Pedrozo, Oliva M.; Arslan, Zikri; Rasulev, Bakhtiyor; Leszczynski, Jerzy

2011-01-01

An aqueous route of synthesis is described for rapid synthesis of lead selenide quantum dots (PbSe QDs) at room temperature in an attempt to produce water-soluble and stable nanocrystals. Several thiol-ligands, including thioglycolic acid (TGA), thioglycerol (TGC), 3-mercaptopropionic acid (MPA), 2-mercaptoethyleamine hydrochloride (MEA), 6-mercaptohexanoic acid (MHA), and L-cysteine (L-cys), were used for capping/stabilization of PbSe QDs. The effects of the ligands on the stability of PbSe QDs were evaluated for a period of two months at room temperature under normal light conditions and at 4 °C in dark. The TGA- and MEA-capped QDs exhibited the highest stability prior to purification, almost two months when kept in dark at 4 °C. However, the stability of TGA-capped QDs was reduced substantially after purification to about 5 days under same conditions, while MEA-capped QDs did not show any significant instability. The stabilization energies of Pb-thiolate complexes determined by theoretical DFT simulations supported the experimental results. The PbSe QDs capped with TGA, MPA and MEA were successfully purified and re-dispersed in water, while those stabilized with TGC, MHA and L-cys aggregated during purification attempts. The purified PbSe QDs possess very susceptible surface resulting in poor stability for about 30 – 45 min after re-dispersion in water. In the presence of an excess of free ligand, the stability increased up to 5 days for TGA-capped QDs at pH 7.19, 9 –12 days for MPA-capped QDs at pH 7.3–7.5 and 45–47 days for MEA-capped QDs at pH 7.35. X-Ray Diffraction (XRD) results showed that the QDs possess a cubic rock salt structure with the most intense peaks located at 2θ = 25.3° (200) and 2θ = 29.2° (100). TEM images showed that the size of the QDs ranges between 5 and 10 nm. ICP-MS results revealed that Pb:Se ratio was 1.26, 1.28, 3.85, 1.18, and 1.31 for the QDs capped with TGA, MPA, MEA, L-Cys, and TGC, respectively. The proposed method

Self-propagating high-temperature synthesis of Sr-doped LaMnO3 perovskite as oxidation catalyst

International Nuclear Information System (INIS)

Hirano, T.; Purwanto, H.; Watanabe, T.; Akiyama, T.

2007-01-01

Sr-doped LaMnO 3 perovskite oxide has been focused on as one of the alternative catalysts to precious metals such as platinum that are used for cleaning automotive emission gas. The conventional Solid-state reaction method is a popular productive process for perovskite oxide, however, it is time and energy consuming process because it requires repeated prolonged heat treatment at high temperatures. Therefore, the purposes of this work are to produce Sr-doped LaMnO 3 perovskite by using Self-propagating high-temperature synthesis (SHS) and experimentally examine the oxidation catalytic activity of the product for cleaning automotive emission gas. In the SHS, powders of La 2 O 3 , SrCO 3 , Mn and NaClO 4 were well mixed at the desired ratio and poured in a graphite crucible, where at one end it was ignited by using an electrically heated carbon foil. The wave of exothermic reaction due to oxidation of manganese propagated to the other end in a short time. The obtained products were characterized by means of XRD, FE-SEM, BET and particle size distribution analysis and then evaluated via catalytic oxidation tests by using propane in a fixed bed reactor at several temperatures. From the XRD analysis, the products had the desired composition of La 1-x Sr x MnO 3 (x = 0, 0.1, 0.2 and 0.4) perovskite, in which the replacing ratio x of La and Sr in the products was easily controlled by changing the mixing ratio of raw materials. The catalytic activity test showed that the samples exhibited good catalytic activity for propane oxidation over 200 deg. C , although the products had a relatively small surface area. SHS showed the potential for the production of a relatively inexpensive catalytic converter

Synthesis and Doping of Silicon Nanocrystals for Versatile Nanocrystal Inks

Science.gov (United States)

Kramer, Nicolaas Johannes

The impact of nanotechnology on our society is getting larger every year. Electronics are becoming smaller and more powerful, the "Internet of Things" is all around us, and data generation is increasing exponentially. None of this would have been possible without the developments in nanotechnology. Crystalline semiconductor nanoparticles (nanocrystals) are one of the latest developments in the field of nanotechnology. This thesis addresses three important challenges for the transition of silicon nanocrystals from the lab bench to the marketplace: A better understanding of the nanocrystal synthesis was obtained, the electronic properties of the nanocrystals were characterized and tuned, and novel silicon nanocrystal inks were formed and applied using simple coating technologies. Plasma synthesis of nanocrystals has numerous advantages over traditional solution-based synthesis methods. While the formation of nanoparticles in low pressure nonthermal plasmas is well known, the heating mechanism leading to their crystallization is poorly understood. A combination of comprehensive plasma characterization with a nanoparticle heating model presented here reveals the underlying plasma physics leading to crystallization. The model predicts that the nanoparticles reach temperatures as high as 900 K in the plasma as a result of heating reactions on the nanoparticle surface. These temperatures are well above the gas temperature and sufficient for complete nanoparticle crystallization. Moving the field of plasma nanoparticle synthesis to atmospheric pressures is important for lowering its cost and making the process attractive for industrial applications. The heating and charging model for silicon nanoparticles was adapted in Chapter 3 to study plasmas maintained over a wide range of pressures (10 -- 105 Pa). The model considers three collisionality regimes and determines the dominant contribution of each regime under various plasma conditions. Strong nanoparticle cooling at

Synthesis of Metal-Oxide/Carbon-Fiber Heterostructures and Their Properties for Organic Dye Removal and High-Temperature CO2 Adsorption

Science.gov (United States)

Shao, Liangzhi; Nie, Shibin; Shao, Xiankun; Zhang, LinLin; Li, Benxia

2018-03-01

One-dimensional metal-oxide/carbon-fiber (MO/CF) heterostructures were prepared by a facile two-step method using the natural cotton as a carbon source the low-cost commercial metal salts as precursors. The metal oxide nanostructures were first grown on the cotton fibers by a solution chemical deposition, and the metal-oxide/cotton heterostructures were then calcined and carbonized in nitrogen atmosphere. Three typical MO/CF heterostructures of TiO2/CF, ZnO/CF, and Fe2O3/CF were prepared and characterized. The loading amount of the metal oxide nanostructures on carbon fibers can be tuned by controlling the concentration of metal salt in the chemical deposition process. Finally, the performance of the as-obtained MO/CF heterostructures for organic dye removal from water was tested by the photocatalytic degradation under a simulated sunlight, and their properties of high-temperature CO2 adsorption were predicted by the temperature programmed desorption. The present study would provide a desirable strategy for the synthesis of MO/CF heterostructures for various applications.

Synthesis of tin monosulfide (SnS) nanoparticles using surfactant free microemulsion (SFME) with the single microemulsion scheme

Science.gov (United States)

Tarkas, Hemant S.; Marathe, Deepak M.; Mahajan, Mrunal S.; Muntaser, Faisal; Patil, Mahendra B.; Tak, Swapnil R.; Sali, Jaydeep V.

2017-02-01

Synthesis of monomorphic, SnS nanoparticles without using a capping agent is a difficult task with chemical route of synthesis. This paper reports on synthesis of tin monosulfide (SnS) nanopartilces with dimension in the quantum-dot regime using surfactant free microemulsion with single microemulsion scheme. This has been achieved by reaction in microreactors in the CME (C: chlorobenzene, M: methanol and E: ethylene glycol) microemulsion system. This is an easy and controllable chemical route for synthesis of SnS nanoparticles. Nanoparticle diameter showed prominent dependence on microemulsion concentration and marginal dependence on microemulsion temperature in the temperature range studied. The SnS nanoparticles formed with this method form stable dispersion in Tolune.

Nanoparticles of Sr(OH)2: synthesis in homogeneous phase at low temperature and application for cultural heritage artefacts

International Nuclear Information System (INIS)

Ciliberto, E.; Condorelli, G.G.; La Delfa, S.; Viscuso, E.

2008-01-01

This paper concerns the synthesis and the characterization of nanometer particles of Sr(OH) 2 , a moderately high water soluble hydroxide (Ksp=3.2 x 10 -4 at 25 C). The reported process yields strontium hydroxide nanoparticles starting from low cost raw materials in aqueous medium (homogeneous phase) at low temperature (below 100 C) by chemical precipitation from salt solutions, involving very simple operational steps and avoiding the use of organic solvents. Observations by X-ray diffraction (XRD), scanning electron microscopy (SEM), electron dispersive X-Ray (EDX) and Fourier transform infrared spectroscopy (FTIR) indicate that the particles are well-crystallized and have nanometer dimensions (∝30 nm in diameter). Moreover, experimental evidence shows the potential use of this material for the protection and the consolidation of wall paintings (frescoes), paper, stone, wood and other artistic artefacts. (orig.)

Two-dimensional tantalum disulfide: controlling structure and properties via synthesis

Science.gov (United States)

Zhao, Rui; Grisafe, Benjamin; Krishna Ghosh, Ram; Holoviak, Stephen; Wang, Baoming; Wang, Ke; Briggs, Natalie; Haque, Aman; Datta, Suman; Robinson, Joshua

2018-04-01

Tantalum disulfide (TaS2) is a transition metal dichalcogenide (TMD) that exhibits phase transition induced electronic property modulation at low temperature. However, the appropriate phase must be grown to enable the semiconductor/metal transition that is of interest for next generation electronic applications. In this work, we demonstrate direct and controllable synthesis of ultra-thin 1T-TaS2 and 2H-TaS2 on a variety of substrates (sapphire, SiO2/Si, and graphene) via powder vapor deposition. The synthesis process leads to single crystal domains ranging from 20 to 200 nm thick and 1-10 µm on a side. The TaS2 phase (1T or 2H) is controlled by synthesis temperature, which subsequently is shown to control the electronic properties. Furthermore, this work constitutes the first demonstration of a metal-insulator phase transition in directly synthesized 1T-TaS2 films and domains by electronic means.

High-temperature Ionization-induced Synthesis of Biologically Relevant Molecules in the Protosolar Nebula

Science.gov (United States)

Bekaert, David V.; Derenne, Sylvie; Tissandier, Laurent; Marrocchi, Yves; Charnoz, Sebastien; Anquetil, Christelle; Marty, Bernard

2018-06-01

Biologically relevant molecules (hereafter biomolecules) have been commonly observed in extraterrestrial samples, but the mechanisms accounting for their synthesis in space are not well understood. While electron-driven production of organic solids from gas mixtures reminiscent of the photosphere of the protosolar nebula (PSN; i.e., dominated by CO–N2–H2) successfully reproduced key specific features of the chondritic insoluble organic matter (e.g., elementary and isotopic signatures of chondritic noble gases), the molecular diversity of organic materials has never been investigated. Here, we report that a large range of biomolecules detected in meteorites and comets can be synthesized under conditions typical of the irradiated gas phase of the PSN at temperatures = 800 K. Our results suggest that organic materials—including biomolecules—produced within the photosphere would have been widely dispersed in the protoplanetary disk through turbulent diffusion, providing a mechanism for the distribution of organic meteoritic precursors prior to any thermal/photoprocessing and subsequent modification by secondary parent body processes. Using a numerical model of dust transport in a turbulent disk, we propose that organic materials produced in the photosphere of the disk would likely be associated with small dust particles, which are coupled to the motion of gas within the disk and therefore preferentially lofted into the upper layers of the disk where organosynthesis occurs.

Facile synthesis of B-type carbonated nanoapatite with tailored microstructure

Energy Technology Data Exchange (ETDEWEB)

Gualtieri, Magdalena Lassinantti, E-mail: magdalena.gualtieri@unimore.it [Dipartimento Ingegneria “Enzo Ferrari”, Università degli studi di Modena e Reggio Emilia, I-41125 Modena (Italy); Romagnoli, Marcello, E-mail: marcello.romagnoli@unimore.it [Dipartimento Ingegneria “Enzo Ferrari”, Università degli studi di Modena e Reggio Emilia, I-41125 Modena (Italy); Hanuskova, Miriam, E-mail: Miriam.hanuskova@unimore.it [Dipartimento Ingegneria “Enzo Ferrari”, Università degli studi di Modena e Reggio Emilia, I-41125 Modena (Italy); Fabbri, Elena, E-mail: Elena.fabbri@unimore.it [Dipartimento Ingegneria “Enzo Ferrari”, Università degli studi di Modena e Reggio Emilia, I-41125 Modena (Italy); Gualtieri, Alessandro F., E-mail: Alessandro.gualtieri@unimore.it [Dipartimento di Scienze Chimiche e Geologiche, Università degli studi di Modena e Reggio Emilia, I-41121 Modena (Italy)

2014-12-15

Nanolime and a phosphate-based chelating agent were used to synthesize B-type carbonated apatite. Developed Rietveld refinement strategies allowed one to determine process yield, product crystallinity as well as structural (unit cell) and microstructural (size, strain) parameters. The effect of synthesis temperature (20–60 °C) as well as Ca/P ratio (1.5–2.5) and solid content (10–30 wt%) of the starting batch on these properties were investigated. FTIR, TEM and gas adsorption data provided supporting evidence. The process yield was 42–60 wt% and found to be governed by the Ca/P ratio. The purified products had high specific surface area (107–186 m{sup 2}/g) and crystallinity (76–97%). The unit cell parameters, correlated to the degree of structural carbonate, were sensitive to the Ca/P ratio. Instead, temperature governed the microstructural parameters. Less strained and larger crystals were obtained at higher temperatures. Long-term aging up to 6 months at 20 °C compensated for higher crystal growth kinetics at higher temperature. - Graphical abstract: Controlled synthesis of carbonated apatite at moderate temperatures using nanolime and sodiumhexametaphosphate as starting reagent. - Highlights: • Chemical synthesis of nano-sized apatite with tailored microstructure was performed. • Colloidal Ca(OH){sub 2} and a phosphorus-based chelating agents were used as reagents. • The method is simple and reproducible which facilitate industrial process scale-up. • Rietveld refinement strategies for product characterization were developed. • Rietveld analyses provided yield, microstructural and structure information.

Facile synthesis of B-type carbonated nanoapatite with tailored microstructure

International Nuclear Information System (INIS)

Gualtieri, Magdalena Lassinantti; Romagnoli, Marcello; Hanuskova, Miriam; Fabbri, Elena; Gualtieri, Alessandro F.

2014-01-01

Nanolime and a phosphate-based chelating agent were used to synthesize B-type carbonated apatite. Developed Rietveld refinement strategies allowed one to determine process yield, product crystallinity as well as structural (unit cell) and microstructural (size, strain) parameters. The effect of synthesis temperature (20–60 °C) as well as Ca/P ratio (1.5–2.5) and solid content (10–30 wt%) of the starting batch on these properties were investigated. FTIR, TEM and gas adsorption data provided supporting evidence. The process yield was 42–60 wt% and found to be governed by the Ca/P ratio. The purified products had high specific surface area (107–186 m 2 /g) and crystallinity (76–97%). The unit cell parameters, correlated to the degree of structural carbonate, were sensitive to the Ca/P ratio. Instead, temperature governed the microstructural parameters. Less strained and larger crystals were obtained at higher temperatures. Long-term aging up to 6 months at 20 °C compensated for higher crystal growth kinetics at higher temperature. - Graphical abstract: Controlled synthesis of carbonated apatite at moderate temperatures using nanolime and sodiumhexametaphosphate as starting reagent. - Highlights: • Chemical synthesis of nano-sized apatite with tailored microstructure was performed. • Colloidal Ca(OH) 2 and a phosphorus-based chelating agents were used as reagents. • The method is simple and reproducible which facilitate industrial process scale-up. • Rietveld refinement strategies for product characterization were developed. • Rietveld analyses provided yield, microstructural and structure information

Nanocrystalline Ni-Co Alloy Synthesis by High Speed Electrodeposition

Directory of Open Access Journals (Sweden)

Jamaliah Idris

2013-01-01

Full Text Available Electrodeposition of nanocrystals is economically and technologically viable production path for the synthesis of pure metals and alloys both in coatings and bulk form. The study presents nanocrystalline Ni-Co alloy synthesis by high speed electrodeposition. Nanocrystalline Ni-Co alloys coatings were prepared by direct current (DC and deposited directly on steel and aluminum substrates without any pretreatment, using high speed electrodeposition method. The influence of the electrolysis parameters, such as cathodic current density and temperature at constant pH, on electrodeposition and microstructure of Ni-Co alloys were examined. A homogeneous surface morphology was obtained at all current densities of the plated samples, and it was evident that the current density and temperature affect the coating thickness of Ni-Co alloy coatings.

Synthesis of nanosized powders of stabilized zirconia

International Nuclear Information System (INIS)

Takodoro, Sandra Kiyoko

2000-01-01

Zirconia solid solutions containing 3 mol % Yttria or 12 mol % ceria have been prepared by the coprecipitation technique followed by azeotropic distillation. The aim of this work is the synthesis of tetragonal zirconia polycrystals nanosized powders that sinter at comparatively lower temperatures attaining high densification, and without using any milling procedure. The main results show that: 1- the dopant cation has a strong influence on the crystallization behavior of the precipitates; 2- the used techniques allowed for obtaining high values of specific surface area (∼130 m 2 .g -1 ); 3- the optimization of the synthesis and processing parameters are responsible for obtaining high densification (≥97% of the theoretical value), at lower temperatures (∼1200 deg C) with average grain sizes lower than 500 nm; 4- impedance spectroscopy results show a strong correlation between the electrical resistivity and the microstructure of sintered ceramics.(author)

Theses of the reports of the XXXI Zvenigorod conference on the plasma physics and controlled thermonuclear synthesis

International Nuclear Information System (INIS)

Kovrizhnykh, L.M.; Ivanov, V.A.; Nagaeva, M.L.; Aleksandrov, A.F.; Vorob'ev, V.S.; Ivanenkov, G.V.; Meshcheryakov, A.I.

2004-01-01

Theses of the reports of the 31th Zvenigorod Conference on the physics and controlled thermonuclear synthesis, presented by Russian and foreign scientists, are published. The total number of reports is 258, namely, summarizing ones 16, magnetic confinement of high temperature plasma - 98, inertial thermonuclear synthesis - 44, physical processes in low temperature plasma - 58, physical bases of plasma and beam technologies - 42 [ru

Localized synthesis, assembly and integration of silicon nanowires

Science.gov (United States)

Englander, Ongi

Localized synthesis, assembly and integration of one-dimensional silicon nanowires with MEMS structures is demonstrated and characterized in terms of local synthesis processes, electric-field assisted self-assembly, and a proof-of-concept nanoelectromechanical system (HEMS) demonstration. Emphasis is placed on the ease of integration, process control strategies, characterization techniques and the pursuit of integrated devices. A top-down followed by a bottom-up integration approach is utilized. Simple MEMS heater structures are utilized as the microscale platforms for the localized, bottom-up synthesis of one-dimensional nanostructures. Localized heating confines the high temperature region permitting only localized nanostructure synthesis and allowing the surroundings to remain at room temperature thus enabling CMOS compatible post-processing. The vapor-liquid-solid (VLS) process in the presence of a catalytic nanoparticle, a vapor phase reactant, and a specific temperature environment is successfully employed locally. Experimentally, a 5nm thick gold-palladium layer is used as the catalyst while silane is the vapor phase reactant. The current-voltage behavior of the MEMS structures can be correlated to the approximate temperature range required for the VLS reaction to take place. Silicon nanowires averaging 45nm in diameter and up to 29mum in length synthesized at growth rates of up to 1.5mum/min result. By placing two MEMS structures in close proximity, 4--10mum apart, localized silicon nanowire growth can be used to link together MEMS structures to yield a two-terminal, self-assembled micro-to-nano system. Here, one MEMS structure is designated as the hot growth structure while a nearby structure is designated as the cold secondary structure, whose role is to provide a natural stopping point for the VLS reaction. The application of a localized electric-field, 5 to 13V/mum in strength, during the synthesis process, has been shown to improve nanowire

Synthesis and characterization of activated lithium fluoride with silver

International Nuclear Information System (INIS)

Encarnacion E, E. K.; Guerrero S, Z.; Reyes A, J.

2017-10-01

The present work shows part of the results obtained in the development of the research that has been carried out since 2015 entitled -Synthesis and characterization of new thermoluminescent materials for the radiation dosimetry and its applications in health-. In the development of this research, the synthesis of crystals of pure lithium fluoride (LiF) and activated with different concentrations of silver (LiF:Ag); synthesized samples are also presented using different temperatures, as well as varying the concentration of the solvent (water-ethanol). The synthesized materials were characterized through different techniques: scanning electron microscopy and X-ray diffraction. Specifically, the results of the calculation of the size of the LiF crystals are presented using the Scherrer equation. Within the results, a dependence on the size of the crystals is highlighted by means of the following factors: the amount of activator in the sample, the temperature at which the sample was synthesized, as well as the amount of solvent in the synthesis. The samples have a simple cubic crystalline phase. (Author)

Synthesis of [18F]-5-fluorouridine (F-18-5-FUR) as a probe for measuring RNA synthesis and tumor growth rates in vivo

International Nuclear Information System (INIS)

Shiue, C.Y.; Fowler, J.S.; MacGregor, R.R.; Wolf, A.P.

1979-01-01

A method for the rapid synthesis of high specific activity of [ 18 F]-5-fluorouridine is described. The 20 Ne(d,α) 18 F nuclear reaction is used to produce high specific activity, anhydrous [ 18 F]-F 2 at the Brookhaven National Laboratory 60'' cyclotron. Fluorination of 2',3',5'-tri-0-acetyluridine with [ 18 F]-F 2 in glacial acetic acid at room temperature followed by hydrolysis with sodium methoxide in methanol gives [ 18 F]-5-fluorouridine with a radiochemical yield of 5 to 7% in a synthesis time of 90 minutes from EOB. The compound is required for the study of RNA synthesis and tumor growth rates in vivo

A novel process for methanol synthesis. Final report

Energy Technology Data Exchange (ETDEWEB)

Tierney, J.W.; Wender, I.

1994-01-25

The use of methanol (MeOH) as a fuel additive and in MTBE production has renewed interest in the search for improved MeOH processes. Commercial processes are characterized by high pressures and temperatures with low per pass conversion (10--12%). Efforts are underway to find improved MeOH synthesis processes. A slurry phase ``concurrent`` synthesis of MeOH/methyl formate (MeF) which operates under relatively mild conditions (100{degrees}C lower than present commercial processes) was the subject of investigation in this work. Evidence for a reaction scheme involving the carbonylation of MeOH to MeF followed by the hydrogenolysis of MeF to two molecules of MeOH -- the net result being the reaction of H{sub 2} with CO to give MeOH via MeF, is presented. Up to 90% per pass conversion and 98% selectivity to methanol at rates comparable to commercial processes have been obtained in spite of the presence of as much as 10,000 ppM CO{sub 2} and 3000 ppM H{sub 2}O in the gas and liquid respectively. The effect of process parameters such as temperature, pressure, H{sub 2}/CO ratio in the reactor, flow rate and catalyst loading were also investigated. The use of temperatures above 170{degrees}C at a pressure of 50 atm results in MeF being the limiting reactant. Small amounts of CH{sub 4} are also formed. Significant MeOH synthesis rates at a pressure in the range of 40--50 atm makes possible the elimination of an upstream shift reactor and the use of an air-blown syngas generator. The nature of the catalysts was studied and correlated with the behavior of the various species in the concurrent synthesis.

Synthesis of metastable A-15 ''Nb3Si'' by ion implantation and on its superconducting transition temperature

International Nuclear Information System (INIS)

Clapp, M.T.; Rose, R.M.

1980-01-01

The authors have found a new technique for the synthesis of metastable compounds of well-defined composition: namely, ion implantation of a selected element into the desired crystal structure. [M.T. Clapp and R.M. Rose, Appl. Phys. Lett. 33, 205 (1978)]. Starting with a substrate material of A-15 Nb 3 Al/sub 0.9/Si/sub 0.1/, two basic approaches were tried towards the formation of A-15 Nb 3 Si by Si implantation: (1) direct replacement of the Al by Si and (2) implantation into a surface layer depleted of Al. This latter approach proved to be the most successful. It consisted of removing the Al by a diffusion anneal and replacing the Al deficiency by sequential Si implantations. Upon subsequent heat treatment a surface layer of A-15 Nb 3 Al/sub 0.2/Si/sub 0.8/ was produced. Details of the experimental procedure and a discussion of the superconducting transition temperature measurements of the implanted surfaces are presented

Formulation and catalytic performance of MOF-derived Fe@C/Al composites for high temperature Fischer–Tropsch synthesis

KAUST Repository

Oar-Arteta, Lide; Valero-Romero, Marí a José ; Wezendonk, Tim; Kapteijn, Freek; Gascon, Jorge

2017-01-01

High productivity towards C-2-C-4 olefins together with high catalyst stability are key for optimum operation in high temperature Fischer-Tropsch synthesis (HT-FTS). Here, we report the fabrication of Fe@C/Al composites that combine both the outstanding catalytic properties of the Fe-BTC MOF-derived Fe catalyst and the excellent mechanical resistance and textural properties provided by the inorganic AlOOH binder. The addition of AlOOH to Fe-BTC followed by pyrolysis in N-2 atmosphere at 500 degrees C results in composites with a large mesoporosity, a high Fe/Fe3O4 ratio, 10-35 nm average Fe crystallite size and coordinatively unsaturated Al3+ sites. In catalytic terms, the addition of AlOOH binder gives rise to enhanced C-2-C-4 selectivity and catalyst mechanical stability in HT-FTS, but at high Al contents the activity decreases. Altogether, the productivity of these Fe@C/Al composites is well above most known Fe catalysts for this process.

Low-temperature synthesis of hexagonal transition metal ion doped ZnS nanoparticles by a simple colloidal method

International Nuclear Information System (INIS)

Wang, Liping; Huang, Shungang; Sun, Yujie

2013-01-01

A general route to synthesize transition metal ions doped ZnS nanoparticles with hexagonal phase by means of a conventional reverse micelle at a low temperature is developed. The synthesis involves N,N-dimethylformamide, Zn(AC) 2 solution, thiourea, ammonia, mercaptoacetic acid, as oil phase, water phase, sulfide source, pH regulator, and surfactant, respectively. Thiourea, ammonia and mercaptoacetic acid are demonstrated crucial factors, whose effects have been studied in detail. In addition, the FT-IR spectra suggest that mercaptoacetic acid may form complex chelates with Zn 2+ in the preparation. In the case of Cu 2+ as a doped ion, hexagonal ZnS:Cu 2+ nanoparticles were synthesized at 95 °C for the first time. The X-ray diffraction (XRD) and transmission electron microscope (TEM) measurements show that the ZnS:Cu 2+ nanoparticles are polycrystalline and possess uniform particle size. The possible formation mechanism of the hexagonal doped ZnS is discussed.

Formulation and catalytic performance of MOF-derived Fe@C/Al composites for high temperature Fischer–Tropsch synthesis

KAUST Repository

Oar-Arteta, Lide

2017-11-15

High productivity towards C-2-C-4 olefins together with high catalyst stability are key for optimum operation in high temperature Fischer-Tropsch synthesis (HT-FTS). Here, we report the fabrication of Fe@C/Al composites that combine both the outstanding catalytic properties of the Fe-BTC MOF-derived Fe catalyst and the excellent mechanical resistance and textural properties provided by the inorganic AlOOH binder. The addition of AlOOH to Fe-BTC followed by pyrolysis in N-2 atmosphere at 500 degrees C results in composites with a large mesoporosity, a high Fe/Fe3O4 ratio, 10-35 nm average Fe crystallite size and coordinatively unsaturated Al3+ sites. In catalytic terms, the addition of AlOOH binder gives rise to enhanced C-2-C-4 selectivity and catalyst mechanical stability in HT-FTS, but at high Al contents the activity decreases. Altogether, the productivity of these Fe@C/Al composites is well above most known Fe catalysts for this process.

Synthesis and Characterization of Novel Quaternary Thioaluminogermanates

KAUST Repository

Al-Bloushi, Mohammed

2013-05-01

Metal chalcogenides form an important class of inorganic materials, which include several technologically important applications. The design of metal chlcogenides is of technological interest and has encouraged recent research into moderate temperature solid-state synthetic methods for the single crystal growth of new materials. The aim of this project is the investigation and development of synthetic methodology for the synthesis of novel metal chlcogenides. The new inorganic compounds of the type “M(AlS2)(GeS2)” (M = Na and K) are new metal-chalcogenides, synthesized by the classical solid state approach. The characterization of these compounds was carried out by Scanning Electron Microscopy (SEM), Energy Dispersive X-ray Spectroscopy (EDS), Single crystal and powder X-ray diffraction, solid state Nuclear Magnetic Resonance (NMR), Ultraviolet-visible (UV-VIS), Infrared (IR) and Raman spectroscopy. These theses study the synthesis of metal chalcogenides through the use of standard chemical techniques. The systematic studies demonstrate the effect of the reactants ratio and reaction temperature on the synthesis and growth of the single crystals. Metal chalcogenides have several potential applications in gas separation, ion exchange, environmental remediation, and energy storage. Especially, the ion exchange materials have found\\tpossible applications in waste-water treatment, water softening, metal separation, and production of high purity water.

Investigations into low pressure methanol synthesis

DEFF Research Database (Denmark)

Sharafutdinov, Irek

The central topic of this work has been synthesis, characterization and optimization of novel Ni-Ga based catalysts for hydrogenation of CO2 to methanol. The overall goal was to search for materials that could be used as a low temperature (and low pressure) methanol synthesis catalyst....... This is required for small scale delocalized methanol production sites, where installation of energy demanding compression units should be avoided. The work was triggered by DFT calculations, which showed that certain bimetallic systems are active towards methanol synthesis from CO2 and H2 at ambient pressure...... containing 5:3 molar ratio of Ni:Ga, the intrinsic activity (methanol production rate per active surface area) is comparable to that of highly optimised Cu/ZnO/Al2O3. Formation of the catalyst was investigated with the aid of in-situ XRD and in-situ XAS techniques. The mechanism of alloying was proposed...

Study of tryptophan assisted synthesis of gold nanoparticles by combining UV-Vis, fluorescence, and SERS spectroscopy