hydrothermal synthesis and characterisation of amine-templated

African Journals Online (AJOL)

PROF EKWUEME

showed that the complexes were insoluble in water, ethanol, DMF and DMSO. KEYWORDS: Hydrothermal synthesis, metal phosphates, p-aminobenzoic acid, ethylacetoacetate, ethylammonium-. 4-aminobenzoate. INTRODUCTION. One of the major areas of materials science is the development of solid state materials with ...

Some peculiarities of zirconium tungstate synthesis by thermal decomposition of hydrothermal precursors

International Nuclear Information System (INIS)

Gubanov, Alexander I.; Dedova, Elena S.; Plyusnin, Pavel E.; Filatov, Eugeny Y.; Kardash, Tatyana Y.; Korenev, Sergey V.; Kulkov, Sergey N.

2014-01-01

Highlights: • Synthesis of ZrW 2 O 8 using hydrothermal method. • On hydrothermal synthesis optimal conc. of HCl in the reaction mixture is 2.3 M. • Thermal decomposition of ZrW 2 O 7 ((OH) 1.5 ,Cl 0.5 )·2H 2 O begins are 200 °S. • Amorphous intermediate crystallizes into cubic single-phase ZrW 2 O 8 above 550 °S. • ZrW 2 O 8 destructed at temperatures above 700 °S. - Abstract: This article discusses some peculiarities of the synthesis of ZrW 2 O 8 (1) using thermal decomposition of the precursor ZrW 2 O 7 ((OH) 1.5 ,Cl 0.5 )·2H 2 O (2) prepared by hydrothermal method. On hydrothermal synthesis of 2 the optimal concentration of hydrochloric acid in the reaction mixture is about 2.3 M. TG approach to determine the chemical composition of the precursor was suggested. It has been found that the precursor for the synthesis of zirconium tungstate has chemical formula 2. Thermal decomposition of the precursor 2 begins at 200 °S and affords an amorphous intermediate, which crystallizes as a cubic phase 1 above 550 °S with an exoeffect. The temperature of the beginning of the transition from amorphous to the crystalline state is 350 ± 25 °S

Hydrothermal synthesis and characterisation of amine-templated ...

African Journals Online (AJOL)

Hydrothermal synthesis and characterisation of amine-templated metal phosphate framework. ... The complexes were thermally stable up to 3000C, after which the organic components starts decomposing. The solubility test in a wide spectrum of solvents (at room temperature) showed that the complexes were insoluble in ...

Studies on the use of supercritical ammonia for ceramic nitride synthesis and fabrication

Science.gov (United States)

Cornell, Linda; Lin, Y. C.; Philipp, Warren H.

1990-01-01

The extractability of ammonia halides (including ammonium thiocyanate) formed as byproducts from the synthesis of Si(NH)2 via ammonolysis of the corresponding silicon tetrahalides using supercritical NH3 as the extraction medium was investigated. It was found that the NH4SCN byproduct of ammonolysis of Si(SCN)4 can be almost completely extracted from the insoluble Si(NH)2 forming a promising system for the synthesis of pure Si(NH)2, one of the best precursors for Si3N4. In addition it was found that Si3N4, AlN, BN, and Si(NH)2 are insoluble in SC ammonia. Also discussed are design considerations for a supercritical ammonia extraction unit.

Analysis of product distribution and characteristics in hydrothermal liquefaction of barley straw in subcritical and supercritical water

DEFF Research Database (Denmark)

Zhu, Zhe; Toor, Saqib; Rosendahl, Lasse

2014-01-01

In this study, hydrothermal liquefaction of barley straw in subcritical and supercritical water with potassium carbonate catalyst was performed in the temperatures range of 280-400°C. The influence of final reaction temperature on products yield was investigated and some physicochemical properties...... yield (35.24 wt %) as well as the maximum energy recovery of 55.33% were obtained at 300°C. The products obtained were characterized in terms of CHNS elemental composition, higher heating values (HHVs), Fourier transform infrared spectroscopy (FTIR) and gas chromatography-mass spectrometer (GC...

Versatile hydrothermal synthesis of one-dimensional composite structures

Science.gov (United States)

Luo, Yonglan

2008-12-01

In this paper we report on a versatile hydrothermal approach developed to fabricate one-dimensional (1D) composite structures. Sulfur and selenium formed liquid and adsorbed onto microrods as droplets and subsequently reacted with metallic ion in solution to produce nanoparticles-decorated composite microrods. 1D composites including ZnO/CdS, ZnO/MnS, ZnO/CuS, ZnO/CdSe, and FeOOH/CdS were successfully made using this hydrothermal strategy and the growth mechanism was also discussed. This hydrothermal strategy is simple and green, and can be extended to the synthesis of various 1D composite structures. Moreover, the interaction between the shell nanoparticles and the one-dimensional nanomaterials were confirmed by photoluminescence investigation of ZnO/CdS.

Some peculiarities of zirconium tungstate synthesis by thermal decomposition of hydrothermal precursors

Energy Technology Data Exchange (ETDEWEB)

Gubanov, Alexander I., E-mail: gubanov@niic.nsc.su [Nikolaev Institute of Inorganic Chemistry, Siberian Branch of the Russian Academy of Sciences, Akad. Lavrentiev Prospekt 3, 630090 Novosibirsk (Russian Federation); Novosibirsk State University, Pirogova str. 2, 630090 Novosibirsk (Russian Federation); Dedova, Elena S. [Institute of Strength Physics and Materials Science, Siberian Branch of the Russian Academy of Sciences, pr. Akademicheskii 2/4, 634021 Tomsk (Russian Federation); Tomsk Polytechnic University, Lenin Avenue 30, 634050 Tomsk (Russian Federation); Plyusnin, Pavel E.; Filatov, Eugeny Y. [Nikolaev Institute of Inorganic Chemistry, Siberian Branch of the Russian Academy of Sciences, Akad. Lavrentiev Prospekt 3, 630090 Novosibirsk (Russian Federation); Novosibirsk State University, Pirogova str. 2, 630090 Novosibirsk (Russian Federation); Kardash, Tatyana Y. [Boreskov Institute of Catalysis, Siberian Branch of the Russian Academy of Sciences, Akad. Lavrentiev Prospekt 5, 630090 Novosibirsk (Russian Federation); Korenev, Sergey V. [Nikolaev Institute of Inorganic Chemistry, Siberian Branch of the Russian Academy of Sciences, Akad. Lavrentiev Prospekt 3, 630090 Novosibirsk (Russian Federation); Novosibirsk State University, Pirogova str. 2, 630090 Novosibirsk (Russian Federation); Kulkov, Sergey N. [Institute of Strength Physics and Materials Science, Siberian Branch of the Russian Academy of Sciences, pr. Akademicheskii 2/4, 634021 Tomsk (Russian Federation); Tomsk Polytechnic University, Lenin Avenue 30, 634050 Tomsk (Russian Federation)

2014-12-10

Highlights: • Synthesis of ZrW{sub 2}O{sub 8} using hydrothermal method. • On hydrothermal synthesis optimal conc. of HCl in the reaction mixture is 2.3 M. • Thermal decomposition of ZrW{sub 2}O{sub 7}((OH){sub 1.5},Cl{sub 0.5})·2H{sub 2}O begins are 200 °S. • Amorphous intermediate crystallizes into cubic single-phase ZrW{sub 2}O{sub 8} above 550 °S. • ZrW{sub 2}O{sub 8} destructed at temperatures above 700 °S. - Abstract: This article discusses some peculiarities of the synthesis of ZrW{sub 2}O{sub 8} (1) using thermal decomposition of the precursor ZrW{sub 2}O{sub 7}((OH){sub 1.5},Cl{sub 0.5})·2H{sub 2}O (2) prepared by hydrothermal method. On hydrothermal synthesis of 2 the optimal concentration of hydrochloric acid in the reaction mixture is about 2.3 M. TG approach to determine the chemical composition of the precursor was suggested. It has been found that the precursor for the synthesis of zirconium tungstate has chemical formula 2. Thermal decomposition of the precursor 2 begins at 200 °S and affords an amorphous intermediate, which crystallizes as a cubic phase 1 above 550 °S with an exoeffect. The temperature of the beginning of the transition from amorphous to the crystalline state is 350 ± 25 °S.

Synthesis of higher diamondoids by pulsed laser ablation plasmas in supercritical CO2

International Nuclear Information System (INIS)

Nakahara, Sho; Stauss, Sven; Kato, Toru; Terashima, Kazuo; Sasaki, Takehiko

2011-01-01

Pulsed laser ablation (wavelength 532 nm; fluence 18 J/cm 2 ; pulse width 7 ns; repetition rate 10 Hz) of highly oriented pyrolytic graphite was conducted in adamantane-dissolved supercritical CO 2 with and without cyclohexane as a cosolvent. Micro-Raman spectroscopy of the products revealed the presence of hydrocarbons possessing sp 3 -hybridized carbons similar to diamond structures. The synthesis of diamantane and other possible diamondoids consisting of up to 12 cages was confirmed by gas chromatography-mass spectrometry. Furthermore, gas chromatography-mass spectrometry measurements of samples before and after pyrolysis treatment indicate the synthesis of the most compact decamantane, namely, superadamantane. It is thought that oxidant species originating from CO 2 during pulsed laser ablation might lead to the selective dissociation of C-H bonds, enabling the synthesis of low H/C ratio molecules. Therefore, laser ablation in supercritical CO 2 is proposed as a practical method for synthesizing diamondoids.

Geological model of supercritical geothermal reservoir related to subduction system

Science.gov (United States)

Tsuchiya, Noriyoshi

2017-04-01

Following the Great East Japan Earthquake and the accident at the Fukushima Daiichi Nuclear power station on 3.11 (11th March) 2011, geothermal energy came to be considered one of the most promising sources of renewable energy for the future in Japan. The temperatures of geothermal fields operating in Japan range from 200 to 300 °C (average 250 °C), and the depths range from 1000 to 2000 m (average 1500 m). In conventional geothermal reservoirs, the mechanical behavior of the rocks is presumed to be brittle, and convection of the hydrothermal fluid through existing network is the main method of circulation in the reservoir. In order to minimize induced seismicity, a rock mass that is "beyond brittle" is one possible candidate, because the rock mechanics of "beyond brittle" material is one of plastic deformation rather than brittle failure. Supercritical geothermal resources could be evaluated in terms of present volcanic activities, thermal structure, dimension of hydrothermal circulation, properties of fracture system, depth of heat source, depth of brittle factures zone, dimension of geothermal reservoir. On the basis of the GIS, potential of supercritical geothermal resources could be characterized into the following four categories. 1. Promising: surface manifestation d shallow high temperature, 2 Probability: high geothermal gradient, 3 Possibility: Aseismic zone which indicates an existence of melt, 4 Potential : low velocity zone which indicates magma input. Base on geophysical data for geothermal reservoirs, we have propose adequate tectonic model of development of the supercritical geothermal reservoirs. To understand the geological model of a supercritical geothermal reservoir, granite-porphyry system, which had been formed in subduction zone, was investigated as a natural analog of the supercritical geothermal energy system. Quartz veins, hydrothermal breccia veins, and glassy veins are observed in a granitic body. The glassy veins formed at 500-550 �

Hydrothermal synthesis of a new ethylenediammonium intercalated ...

Indian Academy of Sciences (India)

Unknown

Vanadyl phosphate; hydrothermal synthesis; intercalation; single crystal ... presence of 'en'.7–15 In all these solids en molecules occur in suitable ... all the cases, the mixture was transferred to a 45 ml Teflon lined Parr acid digestion .... position cannot be fully occupied at the same time as it will lead to a P-P distance of.

A shortcut hydrothermal strategy for the synthesis of zinc nanowires

International Nuclear Information System (INIS)

Hu Jianqiang; Chen Zhiwu; Xie Jingsi; Yu Ying

2008-01-01

Synthesis of metal nanowires has opened many new possibilities for designing ideal building blocks for future nanodevices. In this work, zinc nanowires with lengths of micrometre magnitude were synthesized in high yield by a shortcut hydrothermal strategy. The synthesis involves a template-free, non-seed and catalyst-free solution-phase process to high-quality zinc nanowires, which is low-cost and proceeds at relatively short time. In this process, zinc nanowires were prepared through the reduction of zinc acetate with absolute ethanol in the presence of silver nitrate under hydrothermal atmosphere. The strategy suggests that silver ion plays a vital role in the synthesis of zinc nanowires, without which the substituted product is zinc oxide nanowires. X-ray diffraction and energy-dispersive x-ray spectroscopy measurements confirm the final formation of zinc nanowires and component transformation from zinc oxide nanowires in the introduction of silver ion. We believe that with the efficient synthesis, longer zinc nanowires can be fabricated and may find potential applications for superconductors and nanodevices. (fast track communication)

The rapid size- and shape-controlled continuous hydrothermal synthesis of metal sulphide nanomaterials

OpenAIRE

Dunne, Peter W.; Starkey, Christopher L.; Gimeno-Fabra, Miquel; Lester, Edward

2014-01-01

Continuous flow hydrothermal synthesis offers a cheap, green and highly scalable route for the preparation of inorganic nanomaterials which has predominantly been applied to metal oxide based materials. In this work we report the first continuous flow hydrothermal synthesis of metal sulphide nanomaterials. A wide range of binary metal sulphides, ZnS, CdS, PbS, CuS, Fe₍₁₋ᵪ₎S and Bi₂S₃, have been synthesised. By varying the reaction conditions two different mechanisms may be invoked; a growth d...

Hydrothermal synthesis, off-axis electron holography and magnetic properties of Fe3O4 nanoparticles

DEFF Research Database (Denmark)

Almeida, Trevor P.; Muxworthy, Adrian R.; Williams, Wyn

2014-01-01

The hydrothermal synthesis of Fe3O4 nanoparticles (NPs) (<50 nm) from mixed FeCl3 / FeCl2 precursor solution at pH ~ 12 has been confirmed using complementary characterisation techniques of transmission electron microscopy and X-ray diffractometry. Off-axis electron holography allowed for visuali......The hydrothermal synthesis of Fe3O4 nanoparticles (NPs) (holography allowed...

Sonochemical and hydrothermal synthesis of PbTe nanostructures with the aid of a novel capping agent

International Nuclear Information System (INIS)

Fard-Fini, Shahla Ahmadian; Salavati-Niasari, Masoud; Mohandes, Fatemeh

2013-01-01

Graphical abstract: - Highlights: • PbTe nanostructures were prepared with the aid of Schiff-base compound. • Sonochemical and hydrothermal methods were employed to fabricate PbTe nanostrucrues. • The effect of preparation parameters on the morphology of PbTe was investigated. - Abstract: In this work, a new Schiff-base compound derived from 1,8-diamino-3,6-dioxaoctane and 2-hydroxy-1-naphthaldehyde marked as (2-HyNa)-(DaDo) was synthesized, characterized, and then used as capping agent for the preparation of PbTe nanostructures. To fabricate PbTe nanostructures, two different synthesis methods; hydrothermal and sonochemical routes, were applied. To further investigate, the effect of preparation parameters like reaction time and temperature in hydrothermal synthesis and sonication time in the presence of ultrasound irradiation on the morphology and purity of the final products was tested. The products were analyzed with the aid of SEM, TEM, XRD, FT-IR, and EDS. Based on the obtained results, it was found that pure cubic phased PbTe nanostructures have been obtained by hydrothermal and sonochemical approaches. Besides, SEM images showed that cubic-like and rod-like PbTe nanostructures have been formed by hydrothermal and sonochemical methods, respectively. Sonochemical synthesis of PbTe nanostructures was favorable, because the synthesis time of sonochemical method was shorter than that of hydrothermal method

Rapid synthesis of single-phase bismuth ferrite by microwave-assisted hydrothermal method

Energy Technology Data Exchange (ETDEWEB)

Cao, Wenqian [College of Materials Science and Engineering, China Jiliang University, 258 Xueyuan Street, Xiasha Higher Education District, Hangzhou 310018, Zhejiang Province (China); Chen, Zhi, E-mail: zchen0@gmail.com [College of Materials Science and Engineering, China Jiliang University, 258 Xueyuan Street, Xiasha Higher Education District, Hangzhou 310018, Zhejiang Province (China); Gao, Tong; Zhou, Dantong; Leng, Xiaonan; Niu, Feng [College of Materials Science and Engineering, China Jiliang University, 258 Xueyuan Street, Xiasha Higher Education District, Hangzhou 310018, Zhejiang Province (China); Zhu, Yuxiang [College of Materials Science and Engineering, China Jiliang University, 258 Xueyuan Street, Xiasha Higher Education District, Hangzhou 310018, Zhejiang Province (China); Tianjin Key Laboratory of Marine Resources and Chemistry, Tianjin University of Science and Technology, Tianjin (China); Qin, Laishun, E-mail: qinlaishun@yeah.net [College of Materials Science and Engineering, China Jiliang University, 258 Xueyuan Street, Xiasha Higher Education District, Hangzhou 310018, Zhejiang Province (China); Wang, Jiangying; Huang, Yuexiang [College of Materials Science and Engineering, China Jiliang University, 258 Xueyuan Street, Xiasha Higher Education District, Hangzhou 310018, Zhejiang Province (China)

2016-06-01

This paper describes on the fast synthesis of bismuth ferrite by the simple microwave-assisted hydrothermal method. The phase transformation and the preferred growth facets during the synthetic process have been investigated by X-ray diffraction. Bismuth ferrite can be quickly prepared by microwave hydrothermal method by simply controlling the reaction time, which is further confirmed by Fourier Transform infrared spectroscopy and magnetic measurement. - Graphical abstract: Single-phase BiFeO{sub 3} could be realized at a shortest reaction time of 65 min. The reaction time has strong influences on the phase transformation and the preferred growth facets. - Highlights: • Rapid synthesis (65 min) of BiFeO{sub 3} by microwave-assisted hydrothermal method. • Reaction time has influence on the purity and preferred growth facets. • FTIR and magnetic measurement further confirm the pure phase.

Rapid synthesis of single-phase bismuth ferrite by microwave-assisted hydrothermal method

International Nuclear Information System (INIS)

Cao, Wenqian; Chen, Zhi; Gao, Tong; Zhou, Dantong; Leng, Xiaonan; Niu, Feng; Zhu, Yuxiang; Qin, Laishun; Wang, Jiangying; Huang, Yuexiang

2016-01-01

This paper describes on the fast synthesis of bismuth ferrite by the simple microwave-assisted hydrothermal method. The phase transformation and the preferred growth facets during the synthetic process have been investigated by X-ray diffraction. Bismuth ferrite can be quickly prepared by microwave hydrothermal method by simply controlling the reaction time, which is further confirmed by Fourier Transform infrared spectroscopy and magnetic measurement. - Graphical abstract: Single-phase BiFeO_3 could be realized at a shortest reaction time of 65 min. The reaction time has strong influences on the phase transformation and the preferred growth facets. - Highlights: • Rapid synthesis (65 min) of BiFeO_3 by microwave-assisted hydrothermal method. • Reaction time has influence on the purity and preferred growth facets. • FTIR and magnetic measurement further confirm the pure phase.

Supercritical fluid technologies for ceramic-processing applications

International Nuclear Information System (INIS)

Matson, D.W.; Smith, R.D.

1989-01-01

This paper reports on the applications of supercritical fluid technologies for ceramic processing. The physical and chemical properties of these densified gases are summarized and related to their use as solvents and processing media. Several areas are identified in which specific ceramic processes benefit from the unique properties of supercritical fluids. The rapid expansion of supercritical fluid solutions provides a technique for producing fine uniform powders and thin films of widely varying materials. Supercritical drying technologies allow the formation of highly porous aerogel products with potentially wide application. Hydrothermal processes leading to the formation of large single crystals and microcrystalline powders can also be extended into the supercritical regime of water. Additional applications and potential applications are identified in the areas of extraction of binders and other additives from ceramic compacts, densification of porous ceramics, the formation of powders in supercritical micro-emulsions, and in preceramic polymer processing

Hydrothermal synthesis of titania powders and their photocatalyc properties

Czech Academy of Sciences Publication Activity Database

Štengl, Václav; Bakardjieva, Snejana; Murafa, Nataliya; Houšková, Vendula

2008-01-01

Roč. 52, č. 4 (2008), s. 278-290 ISSN 0862-5468 R&D Projects: GA ČR GA203/08/0334 Institutional research plan: CEZ:AV0Z40320502 Keywords : anatase * rutile * hydrothermal synthesis Subject RIV: CA - Inorganic Chemistry Impact factor: 0.644, year: 2008

Abiotic synthesis of organic compounds from carbon disulfide under hydrothermal conditions.

Science.gov (United States)

Rushdi, Ahmed I; Simoneit, Bernd R T

2005-12-01

Abiotic formation of organic compounds under hydrothermal conditions is of interest to bio, geo-, and cosmochemists. Oceanic sulfur-rich hydrothermal systems have been proposed as settings for the abiotic synthesis of organic compounds. Carbon disulfide is a common component of magmatic and hot spring gases, and is present in marine and terrestrial hydrothermal systems. Thus, its reactivity should be considered as another carbon source in addition to carbon dioxide in reductive aqueous thermosynthesis. We have examined the formation of organic compounds in aqueous solutions of carbon disulfide and oxalic acid at 175 degrees C for 5 and 72 h. The synthesis products from carbon disulfide in acidic aqueous solutions yielded a series of organic sulfur compounds. The major compounds after 5 h of reaction included dimethyl polysulfides (54.5%), methyl perthioacetate (27.6%), dimethyl trithiocarbonate (6.8%), trithianes (2.7%), hexathiepane (1.4%), trithiolanes (0.8%), and trithiacycloheptanes (0.3%). The main compounds after 72 h of reaction consisted of trithiacycloheptanes (39.4%), pentathiepane (11.6%), tetrathiocyclooctanes (11.5%), trithiolanes (10.6%), tetrathianes (4.4%), trithianes (1.2%), dimethyl trisulfide (1.1%), and numerous minor compounds. It is concluded that the abiotic formation of aliphatic straight-chain and cyclic polysulfides is possible under hydrothermal conditions and warrants further studies.

Magma-Hydrothermal Transition: Basalt Alteration at Supercritical Conditions in Drill Core from Reykjanes, Iceland, Iceland Deep Drilling Project.

Science.gov (United States)

Zierenberg, R. A.; Fowler, A. P.; Schiffman, P.; Fridleifsson, G. Ó.; Elders, W. A.

2017-12-01

The Iceland Deep Drilling Project well IDDP-2, drilled to 4,659 m in the Reykjanes geothermal system, the on-land extension of the Mid Atlantic Ridge, SW Iceland. Drill core was recovered, for the first time, from a seawater-recharged, basalt-hosted hydrothermal system at supercritical conditions. The well has not yet been allowed to heat to in situ conditions, but temperature and pressure of 426º C and 340 bar was measured at 4500 m depth prior to the final coring runs. Spot drill cores were recovered between drilling depths of 3648.00 m and 4657.58 m. Analysis of the core is on-going, but we present the following initial observations. The cored material comes from a basaltic sheeted dike complex in the brittle-ductile transition zone. Felsic (plagiogranite) segregation veins are present in minor amounts in dikes recovered below 4300 m. Most core is pervasively altered to hornblende + plagioclase, but shows only minor changes in major and minor element composition. The deepest samples record the transition from the magmatic regime to the presently active hydrothermal system. Diabase near dike margins has been locally recrystallized to granoblastic-textured orthopyroxene-clinopyroxe-plagioclase hornfels. High temperature hydrothermal alteration includes calcic plagioclase (up to An100) and aluminous hornblende (up to 11 Wt. % Al2O3) locally intergrown with hydrothermal biotite, clinopyroxene, orthopyroxene and/or olivine. Hydrothermal olivine is iron-rich (Mg # 59-64) compared to expected values for igneous olivine. Biotite phenocrysts in felsic segregation veins have higher Cl and Fe compared to hydrothermal biotites. Orthopyroxene-clinopyroxene pairs in partially altered quench dike margins give temperature of 955° to 1067° C. Orthopyroxene-clinopyroxene pairs from hornfels and hydrothermal veins and replacements give temperature ranging from 774° to 888° C. Downhole fluid sampling is planned following thermal equilibration of the drill hole. Previous work

Hydrothermal Synthesis of Analcime from Kutingkeng Formation Mudstone

Science.gov (United States)

Hsiao, Yin-Hsiu; Chen, Kuan-Ting; Ray, Dah-Tong

2015-04-01

In southwest of Taiwan, the foothill located in Tainan-Kaohsiung city is the exposed area of Pliocene strata to early Pleistocene strata. The strata are about a depth of five thousand, named as Kutigkeng Formation. The outcrop of Kutigkeng Formation is typical badlands, specifically called 'Moon World.' It is commonly known as no important economic applications of agricultural land. The mineral compositions of Kutingkeng Formation are quartz, clay minerals and feldspar. The clay minerals consist of illite, clinochlore and swelling clays. To study how the phase and morphology of analcime formed by hydrothermal synthesis were affected, analcime was synthesized from the mudstone of Kutinkeng Formation with microwave hydrothermal reaction was investigated. The parameters of the experiment were the reaction temperature, the concentration of mineralizer, solids/liquid ratio and time. The sodium silicate (Na2SiO3) were used as mineralizer. The results showed that the analcime could be synthesized by hydrothermal reaction above 180° from Kutinkeng Formation mudstone samples. At the highest temperature (240°) of this study, the high purity analcime could be produced. When the concentration of Na2SiO3=3~6M, analcime could be synthesized at 240°. The best solids/liquid ratio was approximate 1 to 5. The hydrothermal reaction almost was completed after 4 hours.

Geological Model of Supercritical Geothermal Reservoir on the Top of the Magma Chamber

Science.gov (United States)

Tsuchiya, N.

2017-12-01

We are conducting supercritical geothermal project, and deep drilling project named as "JBBP: Japan Beyond Brittle Project" The temperatures of geothermal fields operating in Japan range from 200 to 300 °C (average 250 °C), and the depths range from 1000 to 2000 m (average 1500 m). In conventional geothermal reservoirs, the mechanical behavior of the rocks is presumed to be brittle, and convection of the hydrothermal fluid through existing network is the main method of circulation in the reservoir. In order to minimize induced seismicity, a rock mass that is "beyond brittle" is one possible candidate, because the rock mechanics of "beyond brittle" material is one of plastic deformation rather than brittle failure. To understand the geological model of a supercritical geothermal reservoir, granite-porphyry system, which had been formed in subduction zone, was investigated as a natural analog of the supercritical geothermal energy system. Quartz veins, hydrothermal breccia veins, and glassy veins are observed in a granitic body. The glassy veins formed at 500-550 °C under lithostatic pressures, and then pressures dropped drastically. The solubility of silica also dropped, resulting in formation of quartz veins under a hydrostatic pressure regime. Connections between the lithostatic and hydrostatic pressure regimes were key to the formation of the hydrothermal breccia veins, and the granite-porphyry system provides useful information for creation of fracture clouds in supercritical geothermal reservoirs. A granite-porphyry system, associated with hydrothermal activity and mineralization, provides a suitable natural analog for studying a deep-seated geothermal reservoir where stockwork fracture systems are created in the presence of supercritical geothermal fluids. I describe fracture networks and their formation mechanisms using petrology and fluid inclusion studies in order to understand this "beyond brittle" supercritical geothermal reservoir, and a geological

Fatty acid methyl esters synthesis from non-edible vegetable oils using supercritical methanol and methyl tert-butyl ether

International Nuclear Information System (INIS)

Lamba, Neha; Modak, Jayant M.; Madras, Giridhar

2017-01-01

Highlights: • FAMEs were synthesized from non-edible oils using supercritical MeOH and MTBE. • Effect of time, temperature, pressure and molar ratio on conversions was studied. • Rate constants of reaction with methanol and MTBE differ by an order of magnitude. • Non-catalytic supercritical reactions are one order faster than acid catalyzed synthesis. - Abstract: Fatty acid methyl esters (FAMEs) are useful as biodiesel and have environmental benefits compared to conventional diesel. In this study, these esters were synthesized non-catalytically from non-edible vegetable oils: neem oil and mahua oil with two different methylating agents: methanol and methyl tert-butyl ether (MTBE). The effects of temperature, pressure, time and molar ratio on the conversion of triglycerides were studied. The temperature was varied in the range of 523–723 K with molar ratios upto 50:1 and a reaction time of upto 150 min. Conversion of neem and mahua oil to FAMEs with supercritical methanol was found to be 83% in 15 min and 99% in 10 min, respectively at 698 K. Further, a conversion of 46% of mahua oil and 59% of neem oil was obtained in 15 min at 723 K using supercritical MTBE. The rate constants evaluated using pseudo first order reaction kinetics were in the range of 4.7 × 10"−"6 to 1.0 × 10"−"3 s"−"1 for the investigated range of temperatures. The activation energies obtained were in the range of 62–113 kJ/mol for the reaction systems investigated. The supercritical synthesis was found to be superior to the catalytic synthesis of the corresponding FAMEs.

Synthesis and characterization of nanosized ceria powders by microwave-hydrothermal method

International Nuclear Information System (INIS)

Bonamartini Corradi, A.; Bondioli, F.; Ferrari, A.M.; Manfredini, T.

2006-01-01

Nanocrystalline ceria powders (CeO 2 ) have been prepared by adding NaOH to a cerium ammonium nitrate aqueous solution under microwave-hydrothermal conditions. In particular the effect of the synthesis conditions (time, pressure and concentration of both the precursor and the precipitant agent solutions) on the physical properties of the crystals have been evaluated. Microwave-hydrothermal treatment of 5 min at 13.4 atm allows to obtain almost crystallized powders (amorphous phase 4%) as underlined by Rietveld-reference intensity ratio (RIR) results

A process to enhance the specific surface area and capacitance of hydrothermally reduced graphene oxide

KAUST Repository

Alazmi, Amira

2016-08-26

The impact of post-synthesis processing in reduced graphene oxide materials for supercapacitor electrodes has been analyzed. A comparative study of vacuum, freeze and critical point drying was carried out for hydrothermally reduced graphene oxide demonstrating that the optimization of the specific surface area and preservation of the porous network are critical to maximize its supercapacitance performance. As described below, using a supercritical fluid as the drying medium, unprecedented values of the specific surface area (364 m2 g−1) and supercapacitance (441 F g−1) for this class of materials have been achieved.

A process to enhance the specific surface area and capacitance of hydrothermally reduced graphene oxide

KAUST Repository

Alazmi, Amira; El Tall, Omar; Rasul, Shahid; Hedhili, Mohamed N.; Patole, Shashikant P.; Da Costa, Pedro M. F. J.

2016-01-01

The impact of post-synthesis processing in reduced graphene oxide materials for supercapacitor electrodes has been analyzed. A comparative study of vacuum, freeze and critical point drying was carried out for hydrothermally reduced graphene oxide demonstrating that the optimization of the specific surface area and preservation of the porous network are critical to maximize its supercapacitance performance. As described below, using a supercritical fluid as the drying medium, unprecedented values of the specific surface area (364 m2 g−1) and supercapacitance (441 F g−1) for this class of materials have been achieved.

FY1995 generic supercritical water technology; 1995 nendo generic technology to shite no chorinkai riyo gijutsu

Energy Technology Data Exchange (ETDEWEB)

NONE

1997-03-01

For the establishment of the basis of supercritical fluid technology, we perform elucidation of the specific feature of the supercritical fluid as a reaction media and development of some new process. In this study, we first studied the fluid structure of SCF through in-situ spectroscopy and MD simulation. As a result, significant hydrogen bonding amongst water molecules and a solvation structure around the solute were observed in the supercritical state. This fluid structure has new features different from that of high temperature steam or liquid water. We found that this is closely related to the difference of bulk properties of SCF and local one around the solute. On the basis of these fundamental findings and with the better understanding of the specific features of SCF as a reaction media, development of some new process had been conducted more efficiently and successfully. The processes being developed in this study include 1) waste biomass and plastic conversion to recover chemicals, 2) hydrogenation of heavy oil for desulphurization through partial oxidation 1 and 3) hydrothermal synthesis of metal oxide fine particles. (NEDO)

Polymer-Assisted Hydrothermal Synthesis of Hierarchically Arranged Hydroxyapatite Nanoceramic

Directory of Open Access Journals (Sweden)

A. Joseph Nathanael

2013-01-01

Full Text Available Flower-like hydroxyapatite (HA nanostructures were synthesized by a polymer-assisted hydrothermal method. The thickness of the petals/plates decreased from 200 nm to 40 nm as the polymer concentration increased. The thickness also decreased as the hydrothermal treatment time increased from 6 to 12 hr. The HRTEM and SAED patterns suggest that the floral-like HA nanostructures are single crystalline in nature. Structural analysis based on XRD and Raman experiments implied that the produced nanostructure is a pure form of HA without any other impurities. The possible formation mechanism was discussed for the formation of flower-like HA nanostructures during polymer-assisted hydrothermal synthesis. Finally, in vitro cellular analysis revealed that the hierarchically arranged HA nanoceramic had improved cell viability relative to other structures. The cells were actively proliferated over these nanostructures due to lower cytotoxicity. Overall, the size and the crystallinity of the nanostructures played a role in improving the cell proliferation.

The rapid size- and shape-controlled continuous hydrothermal synthesis of metal sulphide nanomaterials

Science.gov (United States)

Dunne, Peter W.; Starkey, Chris L.; Gimeno-Fabra, Miquel; Lester, Edward H.

2014-01-01

Continuous flow hydrothermal synthesis offers a cheap, green and highly scalable route for the preparation of inorganic nanomaterials which has predominantly been applied to metal oxide based materials. In this work we report the first continuous flow hydrothermal synthesis of metal sulphide nanomaterials. A wide range of binary metal sulphides, ZnS, CdS, PbS, CuS, Fe(1-x)S and Bi2S3, have been synthesised. By varying the reaction conditions two different mechanisms may be invoked; a growth dominated route which permits the formation of nanostructured sulphide materials, and a nucleation driven process which produces nanoparticles with temperature dependent size control. This offers a new and industrially viable route to a wide range of metal sulphide nanoparticles with facile size and shape control.Continuous flow hydrothermal synthesis offers a cheap, green and highly scalable route for the preparation of inorganic nanomaterials which has predominantly been applied to metal oxide based materials. In this work we report the first continuous flow hydrothermal synthesis of metal sulphide nanomaterials. A wide range of binary metal sulphides, ZnS, CdS, PbS, CuS, Fe(1-x)S and Bi2S3, have been synthesised. By varying the reaction conditions two different mechanisms may be invoked; a growth dominated route which permits the formation of nanostructured sulphide materials, and a nucleation driven process which produces nanoparticles with temperature dependent size control. This offers a new and industrially viable route to a wide range of metal sulphide nanoparticles with facile size and shape control. Electronic supplementary information (ESI) available: Experimental details, refinement procedure, fluorescence spectra of ZnS samples. See DOI: 10.1039/c3nr05749f

Acid-Base Behavior in Hydrothermal Processing of Wastes - Final Report

International Nuclear Information System (INIS)

Johnston, K.; Rossky, P.

2000-01-01

A major obstacle to development of hydrothermal oxidation technology has been a lack of scientific knowledge of chemistry in hydrothermal solution above 350 C, particularly acid-base behavior, and transport phenomena, which is needed to understand corrosion, metal-ion complexation, and salt precipitation and recovery. Our objective has been to provide this knowledge with in situ UV-visible spectroscopic measurements and fully molecular computer simulation. Our recent development of relatively stable organic UV-visible pH indicators for supercritical water oxidation offers the opportunity to characterize buffers and to monitor acid-base titrations. These results have important implications for understanding reaction pathways and yields for decomposition of wastes in supercritical water

Hydrothermal synthesis and physicochemical properties of ruthenium(0) nanoparticles

Energy Technology Data Exchange (ETDEWEB)

Dikhtiarenko, A., E-mail: dikhtiarenkoalla@uniovi.es [Departamento de Quimica Organica e Inorganica, Universidad de Oviedo - CINN, 33006 Oviedo (Spain); Khainakov, S.A.; Garcia, J.R.; Gimeno, J. [Departamento de Quimica Organica e Inorganica, Universidad de Oviedo - CINN, 33006 Oviedo (Spain); Pedro, I. de; Fernandez, J. Rodriguez [CITIMAC, Facultad de Ciencias, Universidad de Cantabria, 39005 Santander (Spain); Blanco, J.A. [Departamento de Fisica, Universidad de Oviedo, 33007 Oviedo (Spain)

2012-09-25

Highlights: Black-Right-Pointing-Pointer Ruthenium nanoparticles were synthesized by hydrothermal technique. Black-Right-Pointing-Pointer The average size of the nanoparticles are depend on the reducing agent used. Black-Right-Pointing-Pointer The magnetic response seems to be dominated by a paramagnetic contribution characteristic of the band electronic magnetism of the ruthenium(0) nanoparticles. - Abstract: The synthesis of ruthenium nanoparticles in hydrothermal conditions using mild reducing agents (succinic acid, ascorbic acid and sodium citrate) is reported. The shape of the nanoparticles depends on the type of the reducing agent, while the size is more influenced by the pH of the medium. The magnetic response seems to be dominated by a paramagnetic contribution characteristic of the band electronic magnetism of the nanoparticles.

Comparative dynamics analysis on xonotlite spherical particles synthesized via hydrothermal synthesis

Science.gov (United States)

Liu, F.; Chen, S.; Lin, Q.; Wang, X. D.; Cao, J. X.

2018-01-01

The xonotlite crystals were synthesized via the hydrothermal synthesis manner from CaO and SiO2 as the raw materials with their Si/Ca molar ratio of 1.0. Comparative dynamics analysis on xonotlite spherical particles synthesized via hydrothermal synthesis process was explored in this paper. The accuracy of the dynamic equation of xonotlite spherical particles was verified by two methods, one was comparing the production rate of the xonotlite products calculated by the dynamic equation with the experimental values, and the other was comparing the apparent activation energies calculated by the dynamic equation with that calculated by the Kondo model. The results indicated that the production rates of the xonotlite spherical particles calculated by the dynamic equation were in good agreement with the experimental values and the apparent activation energy of the xonotlite spherical particles calculated by dynamic equation (84 kJ·mol-1) was close to that calculated by Kondo model (77 kJ·mol-1), verifying the high accuracy of the dynamic equation.

Reaction kinetics of cellulose hydrolysis in subcritical and supercritical water

Science.gov (United States)

Olanrewaju, Kazeem Bode

The uncertainties in the continuous supply of fossil fuels from the crisis-ridden oil-rich region of the world is fast shifting focus on the need to utilize cellulosic biomass and develop more efficient technologies for its conversion to fuels and chemicals. One such technology is the rapid degradation of cellulose in supercritical water without the need for an enzyme or inorganic catalyst such as acid. This project focused on the study of reaction kinetics of cellulose hydrolysis in subcritical and supercritical water. Cellulose reactions at hydrothermal conditions can proceed via the homogeneous route involving dissolution and hydrolysis or the heterogeneous path of surface hydrolysis. The work is divided into three main parts. First, the detailed kinetic analysis of cellulose reactions in micro- and tubular reactors was conducted. Reaction kinetics models were applied, and kinetics parameters at both subcritical and supercritical conditions were evaluated. The second major task was the evaluation of yields of water soluble hydrolysates obtained from the hydrolysis of cellulose and starch in hydrothermal reactors. Lastly, changes in molecular weight distribution due to hydrothermolytic degradation of cellulose were investigated. These changes were also simulated based on different modes of scission, and the pattern generated from simulation was compared with the distribution pattern from experiments. For a better understanding of the reaction kinetics of cellulose in subcritical and supercritical water, a series of reactions was conducted in the microreactor. Hydrolysis of cellulose was performed at subcritical temperatures ranging from 270 to 340 °C (tau = 0.40--0.88 s). For the dissolution of cellulose, the reaction was conducted at supercritical temperatures ranging from 375 to 395 °C (tau = 0.27--0.44 s). The operating pressure for the reactions at both subcritical and supercritical conditions was 5000 psig. The results show that the rate-limiting step in

Hydrothermal synthesis and characterization of zirconia based catalysts

Science.gov (United States)

Caillot, T.; Salama, Z.; Chanut, N.; Cadete Santos Aires, F. J.; Bennici, S.; Auroux, A.

2013-07-01

In this work, three equimolar mixed oxides ZrO2/CeO2, ZrO2/TiO2, ZrO2/La2O3 and a reference ZrO2 have been synthesized by hydrothermal method. The structural and surface properties of these materials have been fully characterized by X-ray diffraction, transmission electron microscopy, surface area measurement, chemical analysis, XPS, infrared spectroscopy after adsorption of pyridine and adsorption microcalorimetry of NH3 and SO2 probe molecules. All investigated mixed oxides are amphoteric and possess redox centers on their surface. Moreover, hydrothermal synthesis leads to catalysts with higher surface area and with better acid-base properties than classical coprecipitation method. Both Lewis and Brønsted acid sites are present on the surface of the mixed oxides. Compared to the other samples, the ZrO2/TiO2 material appears to be the best candidate for further application in acid-base catalysis.

Hydrothermal synthesis of magnetite particles with uncommon crystal facets

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Junki Sato

2014-09-01

Full Text Available Hydrothermal synthesis of Fe3O4 (magnetite particles was carried out using organic compounds as morphology control agents to obtain magnetite crystals with uncommon facets. It was established that the morphology of Fe3O4 crystals obtained by hydrothermal treatment of an aqueous solution containing Fe2+ and organic compounds depended on the organic compound used. The shape of the Fe3O4 particles obtained when no additives were used was quasi-octahedral. In contrast, the addition of picolinic acid, citric acid or pyridine resulted in the formation of polyhedral crystals, indicating the presence of not only {1 1 1}, {1 0 0} and {1 1 0} facets but also high-index facets including at least {3 1 1} and {3 3 1}. When citric acid was used as an additive, octahedral crystals with {1 1 1} facets also appeared, and their size decreased as the amount of citric acid was increased. Thus, control of Fe3O4 particle morphology was achieved by a simple hydrothermal treatment using additives.

Supercritical temperature synthesis of fluorine-doped VO2(M) nanoparticle with improved thermochromic property

Science.gov (United States)

Riapanitra, Anung; Asakura, Yusuke; Cao, Wenbin; Noda, Yasuto; Yin, Shu

2018-06-01

Fluorine-doped VO2(M) nanoparticles have been successfully synthesized using the hydrothermal method at a supercritical temperature of 490 °C. The pristine VO2(M) has the critical phase transformation temperature of 64 °C. The morphology and homogeneity of the monoclinic structure VO2(M) were adopted by the fluorine-doped system. The obtained particle size of the samples is smaller at the higher concentration of anion doping. The best reduction of critical temperature was achieved by fluorine doping of 0.13% up to 48 °C. The thin films of the fluorine-doped VO2(M) showed pronounced thermochromic property and therefore are suitable for smart window applications.

Hydrothermal synthetic strategies of inorganic semiconducting nanostructures.

Science.gov (United States)

Shi, Weidong; Song, Shuyan; Zhang, Hongjie

2013-07-07

Because of their unique chemical and physical properties, inorganic semiconducting nanostructures have gradually played a pivotal role in a variety of research fields, including electronics, chemical reactivity, energy conversion, and optics. A major feature of these nanostructures is the quantum confinement effect, which strongly depends on their size, shape, crystal structure and polydispersity. Among all developed synthetic methods, the hydrothermal method based on a water system has attracted more and more attention because of its outstanding advantages, such as high yield, simple manipulation, easy control, uniform products, lower air pollution, low energy consumption and so on. Precise control over the hydrothermal synthetic conditions is a key to the success of the preparation of high-quality inorganic semiconducting nanostructures. In this review, only the representative hydrothermal synthetic strategies of inorganic semiconducting nanostructures are selected and discussed. We will introduce the four types of strategies based on exterior reaction system adjustment, namely organic additive- and template-free hydrothermal synthesis, organic additive-assisted hydrothermal synthesis, template-assisted hydrothermal synthesis and substrate-assisted hydrothermal synthesis. In addition, the two strategies based on exterior reaction environment adjustment, including microwave-assisted and magnetic field-assisted hydrothermal synthesis, will be also described. Finally, we conclude and give the future prospects of this research area.

Structural archetypes in nickel(II) hybrid vanadates. Towards a directed hydrothermal synthesis

International Nuclear Information System (INIS)

Luis, R. Fernandez de; Urtiaga, M.K.; Mesa, J.L.; Rojo, T.; Arriortua, M.I.

2009-01-01

In the present work, we relate the modifications of the initial synthesis parameters (pH value, stoichiometry and concentration) with the different structural archetypes obtained in the {Ni/Bpy/VO} and {Ni/Bpe/VO} systems (4,4'-bipyridine (Bpy), 1,2-di(4-pyridyl) ethylene (Bpe)). The vanadium coordination is partially controlled by the hydrothermal synthesis conditions, and the final crystal structures depend on the synergetic interaction between the metal-organic subnets and the vanadium oxide subunits.

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.

Hydrothermal synthesis of electrode materials pyrochlore tungsten trioxide film

Science.gov (United States)

Guo, Jingdong; Li, Yingjeng James; Stanley Whittingham, M.

Hydrothermal synthesis methods have been successfully used to prepare new transition-metal oxides for cathodes in electrochemical devices such as lithium batteries and electrochromic windows. The tungsten oxides were the first studied, but the method has been extended to the oxides of molybdenum, vanadium and manganese. Sodium tungsten oxide films with the pyrochlore structure have been prepared on gold/alumina and indium-doped tin oxide substrates. These films reversibly and rapidly intercalate lithium and hydrogen ions.

Hydrothermal synthesis of hydroxyapatite nanorods using pyridoxal-5′-phosphate as a phosphorus source

Energy Technology Data Exchange (ETDEWEB)

Zhao, Xin-Yu; Zhu, Ying-Jie, E-mail: y.j.zhu@mail.sic.ac.cn; Lu, Bing-Qiang; Chen, Feng; Qi, Chao; Zhao, Jing; Wu, Jin

2014-07-01

Graphical abstract: Hydroxyapatite nanorods are synthesized using biocompatible biomolecule pyridoxal-5′-phosphate as a new organic phosphorus source by the hydrothermal method. - Highlights: • Hydrothermal synthesis of hydroxyapatite nanorods is reported. • Biocompatible pyridoxal-5′-phosphate is used as an organic phosphorus source. • This method is simple, surfactant-free and environmentally friendly. - Abstract: Hydroxyapatite nanorods are synthesized by the hydrothermal method using biocompatible biomolecule pyridoxal-5′-phosphate (PLP) as a new organic phosphorus source. In this method, PLP biomolecules are hydrolyzed to produce phosphate ions under hydrothermal conditions, and these phosphate ions react with pre-existing calcium ions to form hydroxyapatite nanorods. The effects of experimental conditions including hydrothermal temperature and time on the morphology and crystal phase of the products are investigated. This method is simple, surfactant-free and environmentally friendly. The products are characterized by X-ray powder diffraction, scanning electron microscopy, transmission electron microscopy, Fourier transform infrared (FTIR) spectroscopy, and thermogravimetric (TG) analysis.

Synthesis of p-Phenylenediamine (PPD) using Supercritical Ammonia

International Nuclear Information System (INIS)

Cho, Hang-Kyu; Lim, Jong Sung

2015-01-01

In this study, investigated the synthesis method of p-Phenylenediamine (PPD) by amination of p-Diiodobenzene (PDIB) under supercritical ammonia and CuI catalyst conditions. We examined the effects of various process variables (e.g., reaction temperature, pressure, amount of ammonia inserted, amount of catalyst inserted, and reaction time) on the production yield of PPD by analyzing the Gas Chromatography (GC). The experimental results demonstrated that PPD was not produced under non-catalyst conditions, and PPD production yield increased with increasing temperature, pressure, amount of catalyst inserted, and reaction time. However, for the reaction temperature case, it was found that 200 .deg. C was the optimal temperature, because thermal degradation of PPD occurred above 250 .deg. C. In addition, we confirmed the structure of PPD and the bonding characteristics of the amine group via FT-IR and H-NMR analysis

Synthesis of p-Phenylenediamine (PPD) using Supercritical Ammonia

Energy Technology Data Exchange (ETDEWEB)

Cho, Hang-Kyu; Lim, Jong Sung [Sogang University, Seoul (Korea, Republic of)

2015-02-15

In this study, investigated the synthesis method of p-Phenylenediamine (PPD) by amination of p-Diiodobenzene (PDIB) under supercritical ammonia and CuI catalyst conditions. We examined the effects of various process variables (e.g., reaction temperature, pressure, amount of ammonia inserted, amount of catalyst inserted, and reaction time) on the production yield of PPD by analyzing the Gas Chromatography (GC). The experimental results demonstrated that PPD was not produced under non-catalyst conditions, and PPD production yield increased with increasing temperature, pressure, amount of catalyst inserted, and reaction time. However, for the reaction temperature case, it was found that 200 .deg. C was the optimal temperature, because thermal degradation of PPD occurred above 250 .deg. C. In addition, we confirmed the structure of PPD and the bonding characteristics of the amine group via FT-IR and H-NMR analysis.

Synthesis and colloidal properties of anisotropic hydrothermal barium titanate

Science.gov (United States)

Yosenick, Timothy James

2005-11-01

Nanoparticles of high dielectric constant materials, especially BaTiO3, are required to achieve decreased layer thickness in multilayer ceramic capacitors (MLCCs). Tabular metal nanoparticles can produce thin metal layers with low surface roughness via electrophoretic deposition (EPD). To achieve similar results with dielectric layers requires the synthesis and dispersion of tabular BaTiO3 nanoparticles. The goal of this study was to investigate the deposition of thin BaTiO3 layers using a colloidal process. The synthesis, interfacial chemistry and colloidal properties of hydrothermal BaTiO3 a model particle system, was investigated. After characterization of the material system particulates were deposited to form thin layers using EPD. In the current study, the synthesis of BaTiO3 has been investigated using a hydrothermal route. TEM and AFM analyses show that the synthesized particles are single crystal with a majority of the particle having a zone axis and {111} large face. The particles have a median thickness of 5.8 +/- 3.1 nm and face diameter of 27.1 +/- 12.3 nm. Particle growth was likely controlled by the formation of {111} twins and the synthesis pH which stabilizes the {111} face during growth. With limited growth in the direction, the particles developed a plate-like morphology. Physical property characterization shows the powder was suitable for further processing with high purity, low hydrothermal defect concentration, and controlled stoichiometry. TEM observations of thermally treated powders indicate that the particles begin to loose the plate-like morphology by 900 °C. The aqueous passivation, dispersion, and doping of nanoscale BaTiO 3 powders was investigated. Passivation BaTiO3 was achieved through the addition of oxalic acid. The oxalic acid selectively adsorbs onto the particle surface and forms a chemically stable 2-3 nm layer of barium oxalate. The negative surface charge of the oxalate effectively passivated the BaTiO3 providing a surface

Synthesis and characterization of nanosized MnZn ferrites via a modified hydrothermal method

Science.gov (United States)

Li, Mingling; Liu, Xiansong; Xu, Taotao; Nie, Yu; Li, Honglin; Zhang, Cong

2017-10-01

Nanosized MnZn ferrite particles, with narrow size distribution, regular morphology and high saturation magnetization have been synthesized via a modified hydrothermal method. This modified hydrothermal method involves a chemical co-precipitation of hydroxides under a vacuum condition using potassium hydroxide as precipitating agent, followed by a separate hydrothermal process. The microstructure and magnetic properties of the synthesized nanoparticles were investigated by X-ray diffraction (XRD), Raman spectroscopy, field emission scanning electron microscopy (FESEM), high resolution transmission electron microscopy (HRTEM) and vibrating sample magnetometer (VSM). The effects of different synthesis conditions (excess ratio of precipitating agent and hydrothermal reaction time) on the microstructure and magnetic properties of the as-synthesized nanoparticles were discussed. The magnetic measurements indicated that the obtained samples were superparamagnetic in nature at room temperature. Moreover, the MnZn ferrite nanoparticles with excellent magnetic performance could be synthesized at 180 °C for a short reaction time (3 h).

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

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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.

Microwave hydrothermal synthesis and characterization of PZT 52/48 powders

International Nuclear Information System (INIS)

Teixeira, G.F.; Gasparotto, G.; Santos, N.A.; Zaghete, M.A.; Varela, J.A.; Longo, E.

2009-01-01

Full text: Lead Zirconate Titanate (PZT) is a ceramic witch has great interest because of their ferroelectric, piezoelectric, and other electrical properties. In this work Pb(ZrxTi1-x)O3 powders were synthesized by microwave hydrothermal synthesis (M-H) at 180°C without excess lead content. This method allows obtaining particles whit nanometer size, good stoichiometric controls, high purity and crystalline degree at low temperatures and short times of synthesis. Powders were synthesized with molar concentration of 0.15 mol.L -1 during different times: 30 min, 2, 4, 6 and 8 h. After that the powders were characterized by X-ray diffraction (XRD), Field Emission Gun (FEG) and photoluminescence (PL). Through analysis it is observed that the crystalline phase of PZT is obtained from 2 hours of synthesis and this same time also presents more intense PL emission. (author)

Hydrothermal synthesis and characterization of polycrystalline gadolinium aluminum perovskite (GdAlO3, GAP

Directory of Open Access Journals (Sweden)

N. Girish H.

2015-06-01

Full Text Available Gadolinium aluminum perovskite (GdAlO3, GAP is a promising high temperature ceramic material, known for its wide applications in phosphors. Polycrystalline gadolinium aluminum perovskites were synthesized using a precursor of co-precipitate gel of GdAlO3 by employing hydrothermal supercritical fluid technique under pressure and temperature ranging from 150 to 200 MPa and 600 to 700 °C, respectively. The resulted products of GAP were studied using the characterization techniques, such as powder X-ray diffraction analysis (XRD, infrared spectroscopy (IR, scanning electron microscopy (SEM and energy dispersive analysis of X-ray (EDX. The X-ray diffraction pattern matched well with the reported orthorhombic GAP pattern (JCPDS-46-0395.

Structural archetypes in nickel(II) hybrid vanadates. Towards a directed hydrothermal synthesis

Energy Technology Data Exchange (ETDEWEB)

Luis, R. Fernandez de; Urtiaga, M.K. [Dpto. Mineralogia y Petrologia, Facultad de Ciencia y Tecnologia, Universidad del Pais Vasco/UPV/EHU, Apdo. 644, 48080 Bilbao (Spain); Mesa, J.L.; Rojo, T. [Dpto. Quimica Inorganica, Facultad de Ciencia y Tecnologia, Universidad del Pais Vasco UPV/EHU, Apdo. 644, 48080 Bilbao (Spain); Arriortua, M.I. [Dpto. Mineralogia y Petrologia, Facultad de Ciencia y Tecnologia, Universidad del Pais Vasco/UPV/EHU, Apdo. 644, 48080 Bilbao (Spain)], E-mail: maribel.arriortua@ehu.es

2009-07-01

In the present work, we relate the modifications of the initial synthesis parameters (pH value, stoichiometry and concentration) with the different structural archetypes obtained in the {l_brace}Ni/Bpy/VO{r_brace} and {l_brace}Ni/Bpe/VO{r_brace} systems (4,4'-bipyridine (Bpy), 1,2-di(4-pyridyl) ethylene (Bpe)). The vanadium coordination is partially controlled by the hydrothermal synthesis conditions, and the final crystal structures depend on the synergetic interaction between the metal-organic subnets and the vanadium oxide subunits.

Synthesis of Mesoporous Nanocrystalline Zirconia by Surfactant-Assisted Hydrothermal Approach.

Science.gov (United States)

Nath, Soumav; Biswas, Ashik; Kour, Prachi P; Sarma, Loka S; Sur, Ujjal Kumar; Ankamwar, Balaprasad G

2018-08-01

In this paper, we have reported the chemical synthesis of thermally stable mesoporous nanocrystalline zirconia with high surface area using a surfactant-assisted hydrothermal approach. We have employed different type of surfactants such as CTAB, SDS and Triton X-100 in our synthesis. The synthesized nanocrystalline zirconia multistructures exhibit various morphologies such as rod, mortar-pestle with different particle sizes. We have characterized the zirconia multistructures by X-ray diffraction study, Field emission scanning electron microscopy, Attenuated total refection infrared spectroscopy, UV-Vis spectroscopy and photoluminescence spectroscopy. The thermal stability of as synthesized zirconia multistructures was studied by thermo gravimetric analysis, which shows the high thermal stability of nanocrystalline zirconia around 900 °C temperature.

Pyrophosphate synthesis in iron mineral films and membranes simulating prebiotic submarine hydrothermal precipitates

Science.gov (United States)

Barge, Laura M.; Doloboff, Ivria J.; Russell, Michael J.; VanderVelde, David; White, Lauren M.; Stucky, Galen D.; Baum, Marc M.; Zeytounian, John; Kidd, Richard; Kanik, Isik

2014-03-01

Cells use three main ways of generating energy currency to drive metabolism: (i) conversion of adenosine diphosphate (ADP) to adenosine triphosphate (ATP) by the proton motive force through the rotor-stator ATP synthase; (ii) the synthesis of inorganic phosphate˜phosphate bonds via proton (or sodium) pyrophosphate synthase; or (iii) substrate-level phosphorylation through the direct donation from an active phosphoryl donor. A mechanism to produce a pyrophosphate bond as “energy currency” in prebiotic systems is one of the most important considerations for origin of life research. Baltscheffsky (1996) suggests that inorganic pyrophosphate (PO74-; PPi) may have preceded ATP/ADP as an energy storage molecule in earliest life, produced by an H+ pyrophosphatase. Here we test the hypothesis that PPi could be synthesized in inorganic precipitates simulating hydrothermal chimney structures transected by thermal and/or ionic gradients. Appreciable yields of PPi were obtained via substrate phosphorylation by acetyl phosphate within the iron sulfide/silicate precipitates at temperatures expected for an alkaline hydrothermal system. The formation of PPi only occurred in the solid phase, i.e. when both Pi and the phosphoryl donor were precipitated with Fe-sulfides or Fe-silicates. The amount of Ac-Pi incorporated into the precipitate was a significant factor in the amount of PPi that could form, and phosphate species were more effectively incorporated into the precipitate at higher temperatures (⩾50 to >85 °C). Thus, we expect that the hydrothermal precipitate would be more enriched in phosphate (and especially, Ac-Pi) near the inner margins of a hydrothermal mound where PPi formation would be at a maximum. Iron sulfide and iron silicate precipitates effectively stabilized Ac-Pi and PPi against hydrolysis (relative to hydrolysis in aqueous solution). Thus it is plausible that PPi could accumulate as an energy currency up to useful concentrations for early life in a

Production of Yttria-doped zirconia by hydrothermal synthesis: thermodynamical analysis

International Nuclear Information System (INIS)

Nascimento Dias, A.J. do; Ogasawara, T.

1993-01-01

After a short review of the literature on Hydrothermal Synthesis of Zirconia, the computation and construction of the Standard Hydrogen Scale Potential versus pH diagrams have been performed starting from data supplied by Thermodynamic Tables. Diagrams have been developed for several temperatures (in the range 298.15 K up to 573.15 K) and for activities of the Y and Zr in the aqueous solution ranging from 0,0001 M up to 1 M. The resultant diagrams have been analyzed and interpreted. The results gotten from the study give good elucidation of the phenomena taking place in the hydrothermal treatment of the Zirconia Powders inside an autoclave at temperatures between 473.15 K and 573.15 K. The conditions for crystallization of the doped zirconia at temperatures lower than 573.15 K are better visualized. (author)

Simulation for scale-up of a confined jet mixer for continuous hydrothermal flow synthesis of nanomaterials

OpenAIRE

Ma, CY; Liu, JJ; Zhang, Y; Wang, XZ

2015-01-01

Reactor performance of confined jet mixers for continuous hydrothermal flow synthesis of nanomaterials is investigated for the purpose of scale-up from laboratory scale to pilot-plant scale. Computational fluid dynamics (CFD) models were applied to simulate hydrothermal fluid flow, mixing and heat transfer behaviours in the reactors at different volumetric scale-up ratios (up to 26 times). The distributions of flow and heat transfer variables were obtained using ANSYS Fluent with the tracer c...

Hydrothermal synthesis of a layered-type W-Ti-O mixed metal oxide and its solid acid activity

NARCIS (Netherlands)

Murayama, T.; Nakajima, K.; Hirata, J.; Omata, K.; Hensen, E.J.M.; Ueda, W.

2017-01-01

A layered-type W–Ti–O mixed oxide was synthesized by hydrothermal synthesis from an aqueous solution of ammonium metatungstate and titanium sulfate. To avoid the formation of titania, oxalic acid was used as a reductant. Optimized synthesis led to rod-like particles comprised of MO6 (M = W, Ti)

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.

PULSE RADIOLYSIS IN SUPERCRITICAL RARE GAS FLUIDS

International Nuclear Information System (INIS)

HOLROYD, R.

2007-01-01

Recently, supercritical fluids have become quite popular in chemical and semiconductor industries for applications in chemical synthesis, extraction, separation processes, and surface cleaning. These applications are based on: the high dissolving power due to density build-up around solute molecules, and the ability to tune the conditions of a supercritical fluid, such as density and temperature, that are most suitable for a particular reaction. The rare gases also possess these properties and have the added advantage of being supercritical at room temperature. Information about the density buildup around both charged and neutral species can be obtained from fundamental studies of volume changes in the reactions of charged species in supercritical fluids. Volume changes are much larger in supercritical fluids than in ordinary solvents because of their higher compressibility. Hopefully basic studies, such as discussed here, of the behavior of charged species in supercritical gases will provide information useful for the utilization of these solvents in industrial applications

Development of Hydrotalcite Based Cobalt Catalyst by Hydrothermal and Co-precipitation Method for Fischer-Tropsch Synthesis

Directory of Open Access Journals (Sweden)

Muhammad Faizan Shareef

2017-10-01

Full Text Available This paper presents the effect of a synthesis method for cobalt catalyst supported on hydrotalcite material for Fischer-Tropsch synthesis. The hydrotalcite supported cobalt (HT-Co catalysts were synthesized by co-precipitation and hydrothermal method. The prepared catalysts were characterized by using various techniques like BET (Brunauer–Emmett–Teller, SEM (Scanning Electron Microscopy, TGA (Thermal Gravimetric Analysis, XRD (X-ray diffraction spectroscopy, and FTIR (Fourier Transform Infrared Spectroscopy. Fixed bed micro reactor was used to test the catalytic activity of prepared catalysts. The catalytic testing results demonstrated the performance of hydrotalcite based cobalt catalyst in Fischer-Tropsch synthesis with high selectivity for liquid products. The effect of synthesis method on the activity and selectivity of catalyst was also discussed. Copyright © 2017 BCREC Group. All rights reserved Received: 3rd November 2016; Revised: 26th February 2017; Accepted: 9th March 2017; Available online: 27th October 2017; Published regularly: December 2017 How to Cite: Sharif, M.S., Arslan, M., Iqbal, N., Ahmad, N., Noor, T. (2017. Development of Hydrotalcite Based Cobalt Catalyst by Hydrothermal and Co-precipitation Method for Fischer-Tropsch Synthesis. Bulletin of Chemical Reaction Engineering & Catalysis, 12(3: 357-363 (doi:10.9767/bcrec.12.3.762.357-363

Microwave-assisted hydrothermal synthesis of CePO4 nanostructures: Correlation between the structural and optical properties

International Nuclear Information System (INIS)

Palma-Ramírez, D.; Domínguez-Crespo, M.A.; Torres-Huerta, A.M.; Dorantes-Rosales, H.; Ramírez-Meneses, E.; Rodríguez, E.

2015-01-01

Highlights: • An enhancement in the hydrothermal synthesis for obtaining of CePO 4 is presented. • Microwave energy can replace the energy by convection for obtaining CePO 4 . • CePO 4 demonstrates to be an option to increase the optical properties of polymers. • Adjusting the pH, the sintering process is not necessary to obtain the desire phase. • CePO 4 morphologies undergo evolution from nanorods to semispherical nanoparticles. - Abstract: In this work, the microwave-assisted hydrothermal method is proposed as an alternative to the synthesis of cerium phosphate (CePO 4 ) nanostructures to evaluate the influence of different synthesis parameters on both the structural and optical properties. In order to reach this goal, two different sets of experiments were designed, varying the reaction temperature (130 and 180 °C), synthesis time (15 and 30 min) and sintering temperature (400 and 600 °C), maintaining a constant pH = 3. Thereafter, two experimental conditions were selected to assess changes in the properties of CePO 4 nanopowders with pH (1, 5, 9 and 11). The crystal structure and morphology of the nanostructures were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and scanning electron microscopy (SEM), respectively. Diffuse reflectance properties of CePO 4 with different microstructures were studied. The results demonstrated that by using the microwave-assisted hydrothermal method, the shape, size and structural phase of CePO 4 can be modulated by using relatively low synthesis temperatures and short reaction times, and depending on pH, a sintering process is not needed to obtain either a desired phase or size. Under the selected experimental conditions, the materials underwent an evolution from nanorods to semispherical nanoparticles, accompanied by a phase transition from hexagonal to monoclinic

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.

Controlled Synthesis of Manganese Dioxide Nano structures via a Facile Hydrothermal

International Nuclear Information System (INIS)

Pang, R.S.C.; Chin, S.F.; Ye, Ch. Ling

2012-01-01

Manganese dioxide nano structures with controllable morphological structures and crystalline phases were synthesized via a facile hydrothermal route at low temperatures without using any templates or surfactants. Both the aging duration and aging temperatures were the main synthesis parameters used to influence and control the rate of morphological and structural evolution of MnO 2 nano structures. MnO 2 nano structures comprise of spherical nano particulate agglomerates and highly amorphous in nature were formed at lower temperature and/or short aging duration. In contrast, MnO 2 nano structures of sea-urchin-like and nano rods-like morphologies and nanocrystalline in nature were prepared at the combined higher aging temperatures and longer aging durations. These nano structures underwent notable phase transformation from d-MnO 2 to a-MnO 2 upon prolonged hydrothermal aging duration and exhibited accelerated rate of phase transformation at higher aging temperature.

Characterization structural and morphology ZSM-5 zeolite by hydrothermal synthesis

International Nuclear Information System (INIS)

Silva, V.J.; Crispim, A.C.; Queiroz, M.B.; Laborde, H.M.; Rodrigues, M.G.F.; Menezes, R.R.

2009-01-01

Solid acids are catalytic materials commonly used in the chemical industry. Among these zeolites are the most important business processes including water treatment, gas separation, and cracking long hydrocarbon chains to produce high octane gasoline. Its synthesis, characterization and applications have been widely studied. The objective this study was to synthesize the ZSM-5 zeolite for future use in separation processes and catalysis. The zeolite ZSM-5 was prepared by hydrothermal synthesis at 170°C, using silica, deionized water and the director of structures (TPABr - tetrapropylammonium bromide). The materials were characterized by X ray diffraction (XRD), scanning electron microscopy (SEM) and semiquantitative chemical analysis by X ray fluorescence (XRF). According to the XRD was possible to observe the formation of ZSM-5 zeolite, with peaks intense and well defined. The SEM showed the formation of individual particles, clean, rounded shapes. (author)

Microwave-Hydrothermal Synthesis and Characterization of High-Purity Nb Doped BaTiO3 Nanocrystals

Directory of Open Access Journals (Sweden)

A. Khanfekr

2014-01-01

Full Text Available The synthesis of Nb doped BaTiO3 has been investigated under Microwave-Hydrothermal (MH conditions in the temperature of 150°C for only 2 h using C16H36O4Ti, BaH2O2.8H2O and NbCl5 as Ba, Ti and  Nb sources, respectively.  Typical experiments performed on MH processing have not yet reported for Nb doped BaTiO3.  In the MH process, the formation of high purity nano tetragonal Nb-BaTiO3 was strongly enhanced. New hydrothermal method was used instead of the previous solid state reaction for the BaTiO3±Nb2O3 system. The new method uses high pressure to create nano dimension particles in a lower time and temperature. In case of the phase evolution studies, the XRD pattern measurements and Raman spectroscopy were performed. TEM and FE-SEM images were taken for the detailed analysis of the particle size, surface and morphology.  Synthesis of Nb doped BaTiO3 with the Microwave-hydrothermal provides an advantage of fast crystallization and reduced crystal size when compared to existing methods.

Pathways for abiotic organic synthesis at submarine hydrothermal fields.

Science.gov (United States)

McDermott, Jill M; Seewald, Jeffrey S; German, Christopher R; Sylva, Sean P

2015-06-23

Arguments for an abiotic origin of low-molecular weight organic compounds in deep-sea hot springs are compelling owing to implications for the sustenance of deep biosphere microbial communities and their potential role in the origin of life. Theory predicts that warm H2-rich fluids, like those emanating from serpentinizing hydrothermal systems, create a favorable thermodynamic drive for the abiotic generation of organic compounds from inorganic precursors. Here, we constrain two distinct reaction pathways for abiotic organic synthesis in the natural environment at the Von Damm hydrothermal field and delineate spatially where inorganic carbon is converted into bioavailable reduced carbon. We reveal that carbon transformation reactions in a single system can progress over hours, days, and up to thousands of years. Previous studies have suggested that CH4 and higher hydrocarbons in ultramafic hydrothermal systems were dependent on H2 generation during active serpentinization. Rather, our results indicate that CH4 found in vent fluids is formed in H2-rich fluid inclusions, and higher n-alkanes may likely be derived from the same source. This finding implies that, in contrast with current paradigms, these compounds may form independently of actively circulating serpentinizing fluids in ultramafic-influenced systems. Conversely, widespread production of formate by ΣCO2 reduction at Von Damm occurs rapidly during shallow subsurface mixing of the same fluids, which may support anaerobic methanogenesis. Our finding of abiogenic formate in deep-sea hot springs has significant implications for microbial life strategies in the present-day deep biosphere as well as early life on Earth and beyond.

Structural study of the controlled hydrothermal synthesis of LiMn2O4 and LixMnyO2

DEFF Research Database (Denmark)

Christiansen, Troels Lindahl; Jensen, Kirsten Marie Ørnsbjerg; Shen, Yanbin

, a layered structure, which can also be described as a defective spinel structure. Here, we show that both LiMn2O4 and LixMnyO2 nanoparticles can be synthesized from a simple, low-temperature hydrothermal synthesis. By tuning a single synthesis parameter (Li-concentration) each of the 2 structures...

Microwave-assisted hydrothermal synthesis of lead zirconate fine powders

Directory of Open Access Journals (Sweden)

Apinpus Rujiwatra

2011-01-01

Full Text Available A rapid synthesis of lead zirconate fine powders by microwave-assisted hydrothermal technique is reported. The influences of type of lead precursor, concentration of potassium hydroxide mineraliser, applied microwave power and irradiation time are described. The synthesised powders were characterised by powder X-ray diffraction, field emission scanning electron microscopy, energy-dispersive X-ray spectroscopic microanalysis and light scattering technique. The merits of the microwave application in reducing reaction time and improving particle mono-dispersion and size uniformity as well as the drawbacks, viz. low purity of the desired phase and increasing demand of mineraliser, are discussed in relation to conventional heating method.

Natural precursor based hydrothermal synthesis of sodium carbide for reactor applications

Science.gov (United States)

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

2017-12-01

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

Microwave-assisted hydrothermal synthesis of CePO{sub 4} nanostructures: Correlation between the structural and optical properties

Energy Technology Data Exchange (ETDEWEB)

Palma-Ramírez, D. [Instituto Politécnico Nacional, CICATA-Unidad Altamira, Km 14.5, Carretera Tampico-Puerto Industrial Altamira, C.P. 89600 Altamira, Tamps (Mexico); Domínguez-Crespo, M.A., E-mail: mdominguezc@ipn.mx [Instituto Politécnico Nacional, CICATA-Unidad Altamira, Km 14.5, Carretera Tampico-Puerto Industrial Altamira, C.P. 89600 Altamira, Tamps (Mexico); Torres-Huerta, A.M. [Instituto Politécnico Nacional, CICATA-Unidad Altamira, Km 14.5, Carretera Tampico-Puerto Industrial Altamira, C.P. 89600 Altamira, Tamps (Mexico); Dorantes-Rosales, H. [Instituto Politécnico Nacional, ESIQIE, Departamento de Metalurgia, C.P. 07300 México D.F. (Mexico); Ramírez-Meneses, E. [Universidad Iberoamericana, Departamento de Ingeniería y Ciencias Químicas, Prolongación Paseo de la Reforma 880, Lomas de Santa Fe, C.P. 01219 México D.F. (Mexico); Rodríguez, E. [Instituto Politécnico Nacional, CICATA-Unidad Altamira, Km 14.5, Carretera Tampico-Puerto Industrial Altamira, C.P. 89600 Altamira, Tamps (Mexico)

2015-09-15

Highlights: • An enhancement in the hydrothermal synthesis for obtaining of CePO{sub 4} is presented. • Microwave energy can replace the energy by convection for obtaining CePO{sub 4}. • CePO{sub 4} demonstrates to be an option to increase the optical properties of polymers. • Adjusting the pH, the sintering process is not necessary to obtain the desire phase. • CePO{sub 4} morphologies undergo evolution from nanorods to semispherical nanoparticles. - Abstract: In this work, the microwave-assisted hydrothermal method is proposed as an alternative to the synthesis of cerium phosphate (CePO{sub 4}) nanostructures to evaluate the influence of different synthesis parameters on both the structural and optical properties. In order to reach this goal, two different sets of experiments were designed, varying the reaction temperature (130 and 180 °C), synthesis time (15 and 30 min) and sintering temperature (400 and 600 °C), maintaining a constant pH = 3. Thereafter, two experimental conditions were selected to assess changes in the properties of CePO{sub 4} nanopowders with pH (1, 5, 9 and 11). The crystal structure and morphology of the nanostructures were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and scanning electron microscopy (SEM), respectively. Diffuse reflectance properties of CePO{sub 4} with different microstructures were studied. The results demonstrated that by using the microwave-assisted hydrothermal method, the shape, size and structural phase of CePO{sub 4} can be modulated by using relatively low synthesis temperatures and short reaction times, and depending on pH, a sintering process is not needed to obtain either a desired phase or size. Under the selected experimental conditions, the materials underwent an evolution from nanorods to semispherical nanoparticles, accompanied by a phase transition from hexagonal to monoclinic.

Fischer-Tropsch synthesis in supercritical phase carbon dioxide: Recycle rates

Science.gov (United States)

Soti, Madhav

With increasing oil prices and attention towards the reduction of anthropogenic CO2, the use of supercritical carbon dioxide for Fischer Tropsch Synthesis (FTS) is showing promise in fulfilling the demand of clean liquid fuels. The evidence of consumption of carbon dioxide means that it need not to be removed from the syngas feed to the Fischer Tropsch reactor after the gasification process. Over the last five years, research at SIUC have shown that FTS in supercritical CO2reduces the selectivities for methane, enhances conversion, reduces the net CO2produces in the coal to liquid fuels process and increase the life of the catalyst. The research has already evaluated the impact of various operating and feed conditions on the FTS for the once through process. We believe that the integration of unreacted feed recycle would enhance conversion, increase the yield and throughput of liquid fuels for the same reactor size. The proposed research aims at evaluating the impact of recycle of the unreacted feed gas along with associated product gases on the performance of supercritical CO2FTS. The previously identified conditions will be utilized and various recycle ratios will be evaluated in this research once the recycle pump and associated fittings have been integrated to the supercritical CO2FTS. In this research two different catalysts (Fe-Zn-K, Fe-Co-Zn-K) were analyzed under SC-FTS in different recycle rate at 350oC and 1200 psi. The use of recycle was found to improve conversion from 80% to close to 100% with both catalysts. The experiment recycle rate at 4.32 and 4.91 was clearly surpassing theoretical recycle curve. The steady state reaction rate constant was increased to 0.65 and 0.8 min-1 for recycle rate of 4.32 and 4.91 respectively. Carbon dioxide selectivity was decreased for both catalyst as it was converting to carbon monoxide. Carbon dioxide consumption was increased from 0.014 to 0.034 mole fraction. This concluded that CO2is being used in the system and

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)

Complexing and hydrothermal ore deposition

CERN Document Server

Helgeson, Harold C

1964-01-01

Complexing and Hydrothermal Ore Deposition provides a synthesis of fact, theory, and interpretative speculation on hydrothermal ore-forming solutions. This book summarizes information and theory of the internal chemistry of aqueous electrolyte solutions accumulated in previous years. The scope of the discussion is limited to those aspects of particular interest to the geologist working on the problem of hydrothermal ore genesis. Wherever feasible, fundamental principles are reviewed. Portions of this text are devoted to calculations of specific hydrothermal equilibriums in multicompone

Hydrothermal synthesis of highly water-dispersible anatase nanocrystals from transparent aqueous sols of titanate colloids

International Nuclear Information System (INIS)

Ban, Takayuki; Tanaka, Yusuke; Ohya, Yutaka

2011-01-01

Transparent colloidal aqueous solutions of anatase nanocrystals were hydrothermally synthesized from aqueous transparent sols with tetramethylammonium titanate colloids, the surfaces of which were modified with citric acid, by structural conversion of the titanate to anatase. This modification hindered coalescence of the titanate colloids during the hydrothermal synthesis. Although the amount of citric acid adsorbed on the colloids was reduced during hydrothermal treatment, a small amount of citric acid was adsorbed on the resulting anatase nanocrystals. Moreover, the use of the titanate colloids as a precursor was compared with the use of a citrato Ti complex, tetramethylammonium citratotitanate. The hydrothermal treatment of the transparent aqueous solutions of the Ti complex yielded opaque solutions with large anatase colloids, suggesting that the titanate colloids were useful for preparing transparent anatase colloidal solutions. Because the shape and size of resulting colloids may be dependent on the size and shape of starting colloids, the use of titanate colloids as a precursor may make it easy to control size and shape of anatase colloids.

Rapid synthesis of nitrogen doped titania with mixed crystal lattice via microwave-assisted hydrothermal method

International Nuclear Information System (INIS)

Zhang Peilin; Liu Bin; Yin Shu; Wang Yuhua; Petrykin, Valery; Kakihana, Masato; Sato, Tsugio

2009-01-01

A microwave-assisted hydrothermal method was employed to synthesize nitrogen doped titania nanoparticles. Due to the high heating efficiency of microwave, rapid synthesis could be achieved in comparison with the conventional oven. Mixed crystal lattice was found existing in the obtained product, and the phase transformation behaviour under calcination was studied by XRD measurement together with Raman spectroscopy in details. The obtained nitrogen doped titania showed high specific surface area, about 300 m 2 g -1 . Photocatalytic activity in destructing NO x gas by the prepared sample exceeded that of commercial titania (P 25) or nitrogen doped titania synthesized by conventional hydrothermal method, under both visible-light and ultraviolet-light irradiation.

Hydrothermal synthesis and sol-gel methods for CdS particle production in different morphologies and their use in wastewater applications

OpenAIRE

Tuncer, Cansel

2018-01-01

In this study, CdSnanoparticles were synthesized in different sizes and morphologies using twodifferent methods. First, the synthesis of both cauliflower-type CdS microspheresand CdS nanoflower-type microstructures by hydrothermal synthesis was carriedout in a steel reactors with teflon chamber. While polyethylene glycol andthioacetamide were used in the synthesis of cauliflower-type CdS microspheres,thiourea was used as a sulfur source in the synthesis of nanoflower CdS microstructures.Spher...

Synthesis and characterization of intercalated polyaniline-clay nanocomposite using supercritical CO2

Science.gov (United States)

Abdelraheem, A.; El-Shazly, A. H.; Elkady, M. F.

2018-05-01

Lately, supercritical CO2 (SCCO2) have been getting great interest. It can be used in numerous applications because it is environmentally friendly, safe, comparatively low cost, and nonflammable. One of its applications is being a solvent in the synthesis of polymeric-clay nanocomposite. In this paper, intercalated polyaniline-clay nanocomposite (PANC) was prepared using SCCO2. The intercalation structure of polyaniline chains between clay layers was verified by various characterization techniques. Scanning electron microscope and transmission electron microscope (SEM-TEM) were used to show the morphology of the synthesized nanocomposite. The molecular structure of PANC nanocomposite was confirmed using Fourier transform infrared spectroscopy (FTIR) and X-ray diffraction (XRD). The BET surface area and the conductivity of the nanocomposite were determined.

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.

Simulation, design and proof-of-concept of a two-stage continuous hydrothermal flow synthesis reactor for synthesis of functionalized nano-sized inorganic composite materials

DEFF Research Database (Denmark)

Zielke, Philipp; Xu, Yu; Simonsen, Søren Bredmose

2016-01-01

Computational fluid dynamics simulations were employed to evaluate several mixer geometries for a novel two-stage continuous hydrothermal flow synthesis reactor. The addition of a second stage holds the promise of allowing the synthesis of functionalized nano-materials as for example core-shell...... or decorated particles. Based on the simulation results, a reactor system employing a confined jet mixer in the first and a counter-flow mixer in the second stage was designed and built. The two-stage functionality and synthesis capacity is shown on the example of single- and two-stage syntheses of pure...... and mixed-phase NiO and YSZ particles....

Radiolytic and electron-transfer reactions in supercritical CO2

International Nuclear Information System (INIS)

Bartels, D. M.; Dimitrijevic, N. M.; Jonah, C. D.; Takahashi, K.

2000-01-01

Using supercritical fluids as solvents is useful for both practical and theoretical reasons. It has been proposed to use supercritical CO 2 as a solvent for synthesis because it eliminates the air pollution arising from other solvents. The properties of supercritical fluids can be easily varied with only modest changes in temperature and density, so they provide a way of testing theories of chemical reactions. It has also been proposed to use supercritical fluids for the treatment of hazardous mixed waste. For these reasons the authors have studied the production of radiolytic species in supercritical CO 2 and have measured their reactivity as a function of density. They have shown that the C 2 O 4 + is formed. They also have shown that the electron transfer reactions of dimethylaniline to C 2 O 4 + and CO 2 (e - ) to benzoquinone are diffusion controlled over a considerable density range

Al-doped SnO2 nanocrystals from hydrothermal systems

International Nuclear Information System (INIS)

Jin Haiying; Xu Yaohua; Pang Guangsheng; Dong Wenjun; Wan Qiang; Sun Yan; Feng Shouhua

2004-01-01

Nanoparticles of Al-doped SnO 2 have been hydrothermally synthesized. The influences of the hydrothermal reaction time, the molar ratio of Sn/Al as well as the pH value of the solution have been studied. During the hydrothermal synthesis, the particle's core is rich in Sn and the surface is rich in Al. The Al-rich surface prevents the particles from further growing up either in the hydrothermal condition or during the calcination at 600 deg. C for a short period of time. The optimal hydrothermal synthesis condition of the nanoparticles is pH 5, Sn/Al=4:1 and 12 h at 160 deg. C. The products have been studied by XRD, TEM and 27 Al solid-state NMR

Microwave radiation hydrothermal synthesis and characterization of micro- and mesoporous composite molecular sieve Y/SBA-15

Directory of Open Access Journals (Sweden)

Wenyuan Wu

2017-05-01

Full Text Available A microwave radiation hydrothermal method to control synthesis of micro- and mesoporous Y/SBA-15 composite molecular sieves was reported. The synthesized SBA-15 and Y/SBA-15 were characterized by scanning electron microscopy (SEM and N2 adsorption–desorption. The three kinds of different concentrations of hydrochloric acid (0.75 M, 2 M and 3.25 M were used to investigate the effect on Y/SBA-15. The analysis results of the composite products indicated that the optimization synthesis condition employed zeolite type Y and TEOS as silicon sources under 0.75 M hydrochloric acid by the microwave radiation hydrothermal synthesis method. The N2 adsorption–desorption test results of micro–mesoporous composite molecular sieve type Y/SBA-15 in mesoporous extent indicated that SBET is 355.529 m2/g, D‾BET is 4.050 nm, and mesoporous aperture focuses on the distribution region of 5.3 nm. It was found that the received composite product has an appropriate proportion of smaller size, larger size pore structure and the thicker pore wall. In addition, its internal channels have a high degree of order and smooth flow in long-range channels.

Synthesis of non-aggregated nicotinic acid coated magnetite nanorods via hydrothermal technique

Energy Technology Data Exchange (ETDEWEB)

Attallah, Olivia A., E-mail: olivia.adly@hu.edu.eg [Center of Nanotechnology, Nile University, 12677 Giza (Egypt); Pharmaceutical Chemistry Department, Heliopolis University, 11777 El Salam, Cairo (Egypt); Girgis, E. [Solid State Physics Department, National Research Center, 12622 Dokki, Giza (Egypt); Advanced Materials and Nanotechnology Lab, CEAS, National Research Center, 12622 Dokki, Giza (Egypt); Abdel-Mottaleb, Mohamed M.S.A. [Center of Nanotechnology, Nile University, 12677 Giza (Egypt)

2016-02-01

Non-aggregated magnetite nanorods with average diameters of 20–30 nm and lengths of up to 350 nm were synthesized via in situ, template free hydrothermal technique. These nanorods capped with different concentrations (1, 1.5, 2 and 2.5 g) of nicotinic acid (vitamin B3); possessed good magnetic properties and easy dispersion in aqueous solutions. Our new synthesis technique maintained the uniform shape of the nanorods even with increasing the coating material concentration. The effect of nicotinic acid on the shape, particle size, chemical structure and magnetic properties of the prepared nanorods was evaluated using different characterization methods. The length of nanorods increased from 270 nm to 350 nm in nicotinic acid coated nanorods. Goethite and magnetite phases with different ratios were the dominant phases in the coated samples while a pure magnetite phase was observed in the uncoated one. Nicotinic acid coated magnetic nanorods showed a significant decrease in saturation magnetization than uncoated samples (55 emu/g) reaching 4 emu/g in 2.5 g nicotinic acid coated sample. The novel synthesis technique proved its potentiality to prepare coated metal oxides with one dimensional nanostructure which can function effectively in different biological applications. - Highlights: • We synthesize nicotinic acid coated magnetite nanorods via hydrothermal technique • Effect of nicotinic acid concentration on the nanorods properties was significant • Nanorods maintained uniform shape with increased concentration of nicotinic acid • Alterations occurred in particle size, mineral phases and magnetics of coated samples.

Synthesis of non-aggregated nicotinic acid coated magnetite nanorods via hydrothermal technique

International Nuclear Information System (INIS)

Attallah, Olivia A.; Girgis, E.; Abdel-Mottaleb, Mohamed M.S.A.

2016-01-01

Non-aggregated magnetite nanorods with average diameters of 20–30 nm and lengths of up to 350 nm were synthesized via in situ, template free hydrothermal technique. These nanorods capped with different concentrations (1, 1.5, 2 and 2.5 g) of nicotinic acid (vitamin B3); possessed good magnetic properties and easy dispersion in aqueous solutions. Our new synthesis technique maintained the uniform shape of the nanorods even with increasing the coating material concentration. The effect of nicotinic acid on the shape, particle size, chemical structure and magnetic properties of the prepared nanorods was evaluated using different characterization methods. The length of nanorods increased from 270 nm to 350 nm in nicotinic acid coated nanorods. Goethite and magnetite phases with different ratios were the dominant phases in the coated samples while a pure magnetite phase was observed in the uncoated one. Nicotinic acid coated magnetic nanorods showed a significant decrease in saturation magnetization than uncoated samples (55 emu/g) reaching 4 emu/g in 2.5 g nicotinic acid coated sample. The novel synthesis technique proved its potentiality to prepare coated metal oxides with one dimensional nanostructure which can function effectively in different biological applications. - Highlights: • We synthesize nicotinic acid coated magnetite nanorods via hydrothermal technique • Effect of nicotinic acid concentration on the nanorods properties was significant • Nanorods maintained uniform shape with increased concentration of nicotinic acid • Alterations occurred in particle size, mineral phases and magnetics of coated samples.

Selective oxidation of propylene to acrolein by hydrothermally synthesized bismuth molybdates

DEFF Research Database (Denmark)

Schuh, Kirsten; Kleist, Wolfgang; Høj, Martin

2014-01-01

Hydrothermal synthesis has been used as a soft chemical method to prepare bismuth molybdate catalysts for the selective oxidation of propylene to acrolein. All obtained samples displayed a plate-like morphology, but their individual aspect ratios varied with the hydrothermal synthesis conditions...... of nitric acid during hydrothermal synthesis enhanced both propylene conversion and acrolein yield, possibly due to a change in morphology. Formation of β-Bi2Mo2O9 was not observed under the applied conditions. In general, the catalytic performance of all samples decreased notably after calcination at 550...

Hydrothermal Synthesis of Nanoclusters of ZnS Comprised on Nanowires

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Magnus Willander

2013-09-01

Full Text Available Cetyltrimethyl ammonium bromide cationic (CTAB surfactant was used as template for the synthesis of nanoclusters of ZnS composed of nanowires, by hydrothermal method. The structural and morphological studies were performed by using X-ray diffraction (XRD, scanning electron microscopy (SEM and high resolution transmission electron microscopy (HRTEM techniques. The synthesized ZnS nanoclusters are composed of nanowires and high yield on the substrate was observed. The ZnS nanocrystalline consists of hexagonal phase and polycrystalline in nature. The chemical composition of ZnS nanoclusters composed of nanowires was studied by X-ray photo electron microscopy (XPS. This investigation has shown that the ZnS nanoclusters are composed of Zn and S atoms.

Hydrothermal Synthesis of Nanoclusters of ZnS Comprised on Nanowires.

Science.gov (United States)

Ibupoto, Zafar Hussain; Khun, Kimleang; Liu, Xianjie; Willander, Magnus

2013-09-09

Cetyltrimethyl ammonium bromide cationic (CTAB) surfactant was used as template for the synthesis of nanoclusters of ZnS composed of nanowires, by hydrothermal method. The structural and morphological studies were performed by using X-ray diffraction (XRD), scanning electron microscopy (SEM) and high resolution transmission electron microscopy (HRTEM) techniques. The synthesized ZnS nanoclusters are composed of nanowires and high yield on the substrate was observed. The ZnS nanocrystalline consists of hexagonal phase and polycrystalline in nature. The chemical composition of ZnS nanoclusters composed of nanowires was studied by X-ray photo electron microscopy (XPS). This investigation has shown that the ZnS nanoclusters are composed of Zn and S atoms.

Gram-scale synthesis of highly crystalline, 0-D and 1-D SnO2 nanostructures through surfactant-free hydrothermal process

International Nuclear Information System (INIS)

Pal, Umapada; Pal, Mou; Sánchez Zeferino, Raul

2012-01-01

We report the synthesis of highly crystalline SnO 2 nanoparticle and nanorod structures with average diameters well within quantum confinement limit (3.5−6.4 nm), through surfactant-free hydrothermal synthesis. The size and shape of the nanostructures could be controlled by controlling the pH (4.5–13.0) of the reaction mixture and the temperature of hydrothermal treatment. Probable mechanisms for the variation of particle size and growth of one-dimensional structures are presented considering the size-dependent crystal solubility at lower pH values of the reaction solution and Ostwald ripening of the quasi-spherical nanoparticles at higher pH values, respectively. Variation of optical band gap energy and hence the effects of quantum confinement in the nanostructures have been studied.

Bismuth molybdate catalysts prepared by mild hydrothermal synthesis: Influence of pH on the selective oxidation of propylene

DEFF Research Database (Denmark)

Schuh, Kirsten; Kleist, Wolfgang; Høj, Martin

2015-01-01

A series of bismuth molybdate catalysts with relatively high surface area was prepared via mild hydrothermal synthesis. Variation of the pH value and Bi/Mo ratio during the synthesis allowed tuning of the crystalline Bi-Mo oxide phases, as determined by X-ray diffraction (XRD) and Raman...... spectroscopy. The pH value during synthesis had a strong influence on the catalytic performance. Synthesis using a Bi/Mo ratio of 1/1 at pH ≥ 6 resulted in γ-Bi2MoO6, which exhibited a better catalytic performance than phase mixtures obtained at lower pH values. However, a significantly lower catalytic...

Hydrothermal Synthesis of Disulfide-Containing Uranyl Compounds. In Situ Ligand Synthesis versus Direct Assembly

Energy Technology Data Exchange (ETDEWEB)

Rowland, Clare E. [George Washington Univ., Washington, DC (United States); Belai, Nebebech [George Washington Univ., Washington, DC (United States); Knope, Karah E. [George Washington Univ., Washington, DC (United States); Cahill, Christopher L. [George Washington Univ., Washington, DC (United States)

2010-01-29

Three disulfide-containing uranyl compounds, [UO₂(C₇H₄O₂S)₃]·H₂O (1), [UO₂(C₇H₄O₂S)₂(C₇H₅O₂S)] (2), and [UO₂(C₇H₄O₂S)₄] (3) have been hydrothermally synthesized. Both in situ disulfide bond formation from 3- and 4-mercaptobenzoic acid (C₇H₅O₂S, MBA) to yield 3,3'- and 4,4'-dithiobisbenzoic acid (C₁₄H₈O₄S₂, DTBA) and direct assembly with the presynthesized dimeric ligands have been explored. While the starting materials 4-MBA and 4,4'-DTBA both yield 2 via in situ ligand synthesis and direct assembly, respectively, we observe the formation of 1 from the starting material 3-MBA via in situ ligand synthesis and of 3 from the direct assembly of the uranyl cation with 3,3'-DTBA. Concurrently with the synthesis of 1 and 2, we have observed the in situ formation of the crystalline dimeric organic species, 3,3'-DTBA, [(C₇H₅O₂S)₂] (4) and 4,4'-DTBA, [(C₇H₅O₂S)₂] (5). Herein we report the synthesis and crystallographic characterization of 1-5, as well as observations regarding the utility of product formation via direct assembly and in situ ligand synthesis.

Properties of ceria doped with gadolinia via microwave-assisted hydrothermal synthesis

International Nuclear Information System (INIS)

Carregosa, J.D.C.; Oliveira, R.M.P.B.; Macedo, D.A.; Nascimento, R.M.

2016-01-01

The solid solution of CeO_2 doped with Gd"3"+ (CGO) is a promising candidate for electrolyte in Solid Oxide Full Cells (SOFCs) operating in intermediate and low temperatures. The reduction of the working temperature of these energy conversion devices is the great technological challenge to its marketing. In this work, nanocrystalline powders of Ce_1_-_xGd_xO_2_-_x_/_2 with x=0, x=0.1 e x=0.2 were obtained via microwave-hydrothermal synthesis at low temperature and times of synthesis (10 and 20 min at 120° C). The powders were analyzed by TG-DTA, DRX and dilatometry. The results showed characteristic peaks of the cubic fluorite-type structure, referring to the cerium oxide (CeO_2), without the presence of secondary peaks. It was also observed that the samples processed at levels of 10 and 20 minutes showed distinct behaviors in contrast to the concentrations of Gd"3"+. (author)

Measurement of the thermal diffusivity and speed of sound of hydrothermal solutions via the laser-induced grating technique

International Nuclear Information System (INIS)

Butenhoff, T.J.

1994-01-01

Hydrothermal processing is being developed as a method for organic destruction for the Hanford Site in Washington. Hydrothermal processing refers to the redox reactions of chemical compounds in supercritical or near-supercritical aqueous solutions. In order to design reactors for the hydrothermal treatment of complicated mixtures found in the Hanford wastes, engineers need to know the thermophysical properties of the solutions under hydrothermal conditions. The author used the laser-induced grating technique to measure the thermal diffusivity and speed of sound of hydrothermal solutions. In this non-invasive optical technique, a transient grating is produced in the hydrothermal solution by optical absorption from two crossed time-coincident nanosecond laser pulses. The grating is probed by measuring the diffraction efficiency of a third laser beam. The grating relaxes via thermal diffusion, and the thermal diffusivity can be determined by measuring the decay of the grating diffraction efficiency as a function of the pump-probe delay time. In addition, intense pump pulses produce counterpropagating acoustic waves that appear as large undulations in the transient grating decay spectrum. The speed of sound in the sample is simply the grating fringe spacing divided by the undulation period. The cell is made from a commercial high pressure fitting and is equipped with two diamond windows for optical access. Results are presented for dilute dye/water solutions with T = 400 C and pressures between 20 and 70 MPa

Microwave-Assisted Hydrothermal Synthesis of Cellulose/Hydroxyapatite Nanocomposites

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Lian-Hua Fu

2016-09-01

Full Text Available In this paper, we report a facile, rapid, and green strategy for the synthesis of cellulose/hydroxyapatite (HA nanocomposites using an inorganic phosphorus source (sodium dihydrogen phosphate dihydrate (NaH2PO4·2H2O, or organic phosphorus sources (adenosine 5′-triphosphate disodium salt (ATP, creatine phosphate disodium salt tetrahydrate (CP, or D-fructose 1,6-bisphosphate trisodium salt octahydrate (FBP through the microwave-assisted hydrothermal method. The effects of the phosphorus sources, heating time, and heating temperature on the phase, size, and morphology of the products were systematically investigated. The experimental results revealed that the phosphate sources played a critical role on the phase, size, and morphology of the minerals in the nanocomposites. For example, the pure HA was obtained by using NaH2PO4·2H2O as phosphorus source, while all the ATP, CP, and FBP led to the byproduct, calcite. The HA nanostructures with various morphologies (including nanorods, pseudo-cubic, pseudo-spherical, and nano-spherical particles were obtained by varying the phosphorus sources or adjusting the reaction parameters. In addition, this strategy is surfactant-free, avoiding the post-treatment procedure and cost for the surfactant removal from the product. We believe that this work can be a guidance for the green synthesis of cellulose/HA nanocomposites in the future.

Hydrothermal synthesis of highly nitrogen-doped few-layer graphene via solid–gas reaction

International Nuclear Information System (INIS)

Liang, Xianqing; Zhong, Jun; Shi, Yalin; Guo, Jin; Huang, Guolong; Hong, Caihao; Zhao, Yidong

2015-01-01

Highlights: • A novel approach to synthesis of N-doped few-layer graphene has been developed. • The high doping levels of N in products are achieved. • XPS and XANES results reveal a thermal transformation of N bonding configurations. • The developed method is cost-effective and eco-friendly. - Abstract: Nitrogen-doped (N-doped) graphene sheets with high doping concentration were facilely synthesized through solid–gas reaction of graphene oxide (GO) with ammonia vapor in a self-designed hydrothermal system. The morphology, surface chemistry and electronic structure of N-doped graphene sheets were investigated by TEM, AFM, XRD, XPS, XANES and Raman characterizations. Upon hydrothermal treatment, up to 13.22 at% of nitrogen could be introduced into the crumpled few-layer graphene sheets. Both XPS and XANES analysis reveal that the reaction between oxygen functional groups in GO and ammonia vapor produces amide and amine species in hydrothermally treated GO (HTGO). Subsequent thermal annealing of the resultant HTGO introduces a gradual transformation of nitrogen bonding configurations in graphene sheets from amine N to pyridinic and graphitic N with the increase of annealing temperature. This study provides a simple but cost-effective and eco-friendly method to prepare N-doped graphene materials in large-scale for potential applications

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.

Generic supercritical water technology; Generic technology to shite no chorinkaisui riyo gijutsu

Energy Technology Data Exchange (ETDEWEB)

Arai, K; Ajiri, M; Inomata, H; Smith, R; Hakuta, Y [Tohoku University, Sendai (Japan). Faculty of Engineering; Yokoyama, C [Tohoku University, Sendai (Japan). The Institute forChemical Reaction Science; Chin, L [New Energy and Industrial Technology Development Organization, Tokyo, (Japan)

1997-02-01

This paper describes the measurement and analysis for clarifying solution structure of supercritical water and exhibition mechanism of solvent functions. It also describes the development of new processes using supercritical water as reaction solvent. The PVT measurements were conducted in the supercritical region using pure water and NaCl aqueous solution, to confirm the reduction of molar volume of the electrolyte solution. The hydration structure was examined in the supercritical aqueous solution by the molecular dynamic simulation. As a result, presence of hydrogen bond structure, where the contribution of two branching hydrogen bond can not be ignored, was suggested under the supercritical condition. Characteristics of supercritical aqueous solutions are analyzed through in-situ Raman and scattered X-ray spectral measurements. Moreover, this paper introduces developments of some processes in the supercritical water, such as decomposition of wasted polymers, recovery of chemical materials, reforming of heavy hydrocarbons by contact hydrogenation, and synthesis of fine powders of metal oxide by reaction crystallization.

Hydrothermal synthesis, characterization and up/down-conversion luminescence of barium rare earth fluoride nanocrystals

International Nuclear Information System (INIS)

Jia, Li-Ping; Zhang, Qiang; Yan, Bing

2014-01-01

Graphical abstract: Lanthanide ions doped bare earth rare earth fluoride nanocrystals are synthesized by hydrothermal technology and characterized. The down/up-conversion luminescence of them are discussed. - Highlights: • Mixed hydrothermal system H 2 O–OA (EDA)–O-A(LO-A) is used for synthesis. • Barium rare earth fluoride nanocrystals are synthesized comprehensively. • Luminescence for down-conversion and up-conversion are obtained for these systems. - Abstract: Mixed hydrothermal system H 2 O–OA (EDA)–O-A(LO-A) is developed to synthesize barium rare earth fluorides nanocrystals (OA = oleylamine, EDA = ethylenediamine, O-A = oleic acid and LO-A = linoleic acid). They are presented as BaREF 5 (RE = Ce, Pr, Nd, Eu, Gd, Tb, Dy, Y, Tm, Lu) and Ba 2 REF 7 (RE = La, Sm, Ho, Er, Yb). The influence of reaction parameters (rare earth species, hydrothermal system and temperature) is checked on the phase and shape evolution of the fluoride nanocrystals. It is found that reaction time and temperature of these nanocrystals using EDA (180 °C, 6 h) is lower than those of them using OA (220 °C, 10 h). The photoluminescence properties of these fluorides activated by some rare earth ions (Nd 3+ , Eu 3+ , Tb 3+ ) are studied, and especially up-conversion luminescence of the four fluoride nanocrystal systems (Ba 2 LaF 7 :Yb, Tm(Er), Ba 2 REF 7 :Yb, Tm(Er) (RE = Gd, Y, Lu)) is observed

Studies on supercritical hydrothermal syntheses of uranium and lanthanide oxide particles and their reaction mechanisms

Science.gov (United States)

Hwang, DongKi; Tsukahara, Takehiko; Tanaka, Kosuke; Osaka, Masahiko; Ikeda, Yasuhisa

2015-11-01

In order to develop preparation method of raw metal oxide particles for low decontaminated MOX fuels by supercritical hydrothermal (SH) treatments, we have investigated behavior of aqueous solutions dissolving U(VI), Ln(III) (Ln: lanthanide = Ce, Pr, Nd, Sm, Tb), Cs(I), and Sr(II) nitrate or chloride compounds under SH conditions (temperature = 400-500 °C, pressure = 30-40 MPa). As a result, it was found that Ln(NO3)3 (Ln = Ce, Pr, Tb) compounds produce LnO2, that Ln(NO3)3 (Ln = Nd, Sm) compounds are hardly converted to their oxides, and that LnCl3 (Ln = Ce, Pr, Nd, Sm, Tb), CsNO3, and Sr(NO3)2 do not form their oxide compounds. Furthermore, HNO2 species were detected in the liquid phase obtained after treating HNO3 aqueous solutions containing Ln(NO3)3 (Ln = Ce, Pr, Tb) under SH conditions, and also NO2 and NO compounds were found to be produced by decomposition of HNO3. From these results, it was proposed that the Ln oxide (LnO2) particles are directly formed with oxidation of Ln(III) to Ln(IV) by HNO3 and HNO2 species in the SH systems. Moreover, the uranyl ions were found to form U3O8 and UO3 depending on the concentration of HNO3. From these results, it is expected that the raw metal oxide particles for low decontaminated MOX fuels are efficiently prepared by the SH method.

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.

Hydrothermal synthesis of carbonyl iron-carbon nanocomposite: Characterization and electromagnetic performance

Directory of Open Access Journals (Sweden)

Hakimeh Pourabdollahi

Full Text Available In this research, the electromagnetic absorption properties of the carbonyl iron-carbon (CI/C nanocomposite prepared via hydrothermal reaction using glucose as carbon precursor was studied in the range of 8.2–12.4 GHz. In hydrothermal reaction, glucose solution containing CI particles, placed in autoclave for 4 h under 453 K. Using surface coating technology is a method that prevents Cl oxidation and improves CI electromagnetic absorption. The structure, morphology and magnetic performances of the prepared nanocomposites were characterized by X-ray diffraction (XRD, energy dispersive spectrometry (EDS, transmission electron microscopy (TEM and vibrating sample magnetometer (VSM. The electromagnetic properties including complex permittivity (εr, the permeability (µr, dielectric loss, magnetic loss, reflection loss, and attenuation constant were investigated using a vector network analyzer. For The CI/C nanocomposite, the bandwidth of −10 dB and −20 dB were obtained in the frequency range of 9.8–12.4 and 11.0–11.8 GHz, respectively. As well as, the reflection loss was −46.69 dB at the matching frequency of 11.5 GHz, when the matching thickness was 1.3 mm. While for CI particles the reflection loss for 4.4 mm thickness was −16.86 dB at the matching frequency of 12.3 GHz. The results indicate that the existence layer of carbon on carbonyl iron enhance the electromagnetic absorbing properties. Therefore, this nanocomposite can be suitable for in the radar absorbing coatings. Keywords: Hydrothermal synthesis, Carbonyl iron-carbon nanocomposite, Microwave absorption, Reflection loss

Hierarchically nanostructured hydroxyapatite: hydrothermal synthesis, morphology control, growth mechanism, and biological activity

Science.gov (United States)

Ma, Ming-Guo

2012-01-01

Hierarchically nanosized hydroxyapatite (HA) with flower-like structure assembled from nanosheets consisting of nanorod building blocks was successfully synthesized by using CaCl2, NaH2PO4, and potassium sodium tartrate via a hydrothermal method at 200°C for 24 hours. The effects of heating time and heating temperature on the products were investigated. As a chelating ligand and template molecule, the potassium sodium tartrate plays a key role in the formation of hierarchically nanostructured HA. On the basis of experimental results, a possible mechanism based on soft-template and self-assembly was proposed for the formation and growth of the hierarchically nanostructured HA. Cytotoxicity experiments indicated that the hierarchically nanostructured HA had good biocompatibility. It was shown by in-vitro experiments that mesenchymal stem cells could attach to the hierarchically nanostructured HA after being cultured for 48 hours. Objective The purpose of this study was to develop facile and effective methods for the synthesis of novel hydroxyapatite (HA) with hierarchical nanostructures assembled from independent and discrete nanobuilding blocks. Methods A simple hydrothermal approach was applied to synthesize HA by using CaCl2, NaH2PO4, and potassium sodium tartrate at 200°C for 24 hours. The cell cytotoxicity of the hierarchically nanostructured HA was tested by MTT (3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide) assay. Results HA displayed the flower-like structure assembled from nanosheets consisting of nanorod building blocks. The potassium sodium tartrate was used as a chelating ligand, inducing the formation and self-assembly of HA nanorods. The heating time and heating temperature influenced the aggregation and morphology of HA. The cell viability did not decrease with the increasing concentration of hierarchically nanostructured HA added. Conclusion A novel, simple and reliable hydrothermal route had been developed for the synthesis of

High performance supercapacitor using N-doped graphene prepared via supercritical fluid processing with an oxime nitrogen source

International Nuclear Information System (INIS)

Balaji, S. Suresh; Elavarasan, A.; Sathish, M.

2016-01-01

Graphical abstract: N-doped graphene prepared via supercritical fluid processing with oxime nitrogen source (DMG) showed enhanced performance in electrochemical supercapacitor application. A maximum specific capacitance of 286 F g"−"1 at a current density of 0.5 A/g was achieved with a high specific capacity retention of 98% after 1000 cycles at 5 A/g. - Highlights: • N-functionalised graphene synthesized via supercritical fluid processing. • DMG, an oxime based nitrogen precursor. • Maximum specific capacitance of 286 F/g at 0.5 A/g in aqueous solution. • Pyridinic as well as quarternary nitrogen for enhanced capacitance. - Abstract: Heteroatom doped graphene has been proved for its promising applications in electrochemical energy storage systems. Here, nitrogen (N) doped graphene was prepared via two different techniques namely supercritical fluid assisted processing and hydrothermal heat treatment using dimethylglyoxime (DMG) as an oxime nitrogen precursor. The FT-IR and Raman spectra showed the N-containing functional group in the graphene. The XRD analysis revealed the complete reduction of graphene oxide during the supercritical fluid processing. The elemental analysis and X-ray photoelectron spectroscopy revealed the amount and nature of N-doping in the graphene, respectively. The surface morphology and physical nature of the samples were analyzed using scanning and transmission electron microscopic analysis. The electrochemical performance of prepared electrode materials was evaluated using cyclic voltammetry, galvanostatic charge-discharge analysis and electrochemical impedance spectroscopy. The N-doped graphene prepared via supercritical fluid assisted processing exhibit enhanced capacitive behaviour with a maximum specific capacitance of 286 F g"−"1 at a current density of 0.5 A/g. The cycling studies showed 98% specific capacity retention with 100% coulombic efficiency over 1000 cycles at 5 A/g. The enhanced specific capacitance of N

Morphology-controlled hydrothermal synthesis of MnCO3 hierarchical superstructures with Schiff base as stabilizer

International Nuclear Information System (INIS)

Hu, He; Xu, Jie-yan; Yang, Hong; Liang, Jie; Yang, Shiping; Wu, Huixia

2011-01-01

Graphical abstract: MnCO3 microcrystals with hierarchical superstructures were synthesized by using the CO2 in atmosphere as carbonate ions source and Schiff base as shape guiding-agent in water/ethanol system under hydrothermal condition. Highlights: → The most interesting in this work is the use of the greenhouse gases CO 2 in atmosphere as carbonate ions source to precipitate with Mn 2+ for producing MnCO 3 crystals. → This work is the first report related to the small organic molecule Schiff base as shape guiding-agent to produce different MnCO 3 hierarchical superstructures. → We are controllable synthesis of the MnCO 3 hierarchical superstructures such as chrysanthemum, straw-bundle, dumbbell and sphere-like microcrystals. → The as-prepared MnCO 3 could be used precursor to fabricate the Mn 2 O 3 hierarchical superstructures after thermal decomposition at high temperature. -- Abstract: MnCO 3 with hierarchical superstructures such as chrysanthemum, straw-bundle, dumbbell and sphere-like were synthesized in water/ethanol system under environment-friendly hydrothermal condition. In the synthesis process, the CO 2 in atmosphere was used as the source of carbonate ions and Schiff base was used as shape guiding-agent. The different superstructures of MnCO 3 could be obtained by controlling the hydrothermal temperature, the molar ratio of manganous ions to the Schiff base, or the volume ratio of water to ethanol. A tentative growth mechanism for the generation of MnCO 3 superstructures was proposed based on the rod-dumbbell-sphere model. Furthermore, the MnCO 3 as precursor could be further successfully transferred to Mn 2 O 3 microstructure after heating in the atmosphere at 500 o C, and the morphology of the Mn 2 O 3 was directly determined by that of the MnCO 3 precursor.

Synthesis and characterization of CuO flower-nanostructure processing by a domestic hydrothermal microwave

International Nuclear Information System (INIS)

Volanti, D.P.; Keyson, D.; Cavalcante, L.S.; Simoes, A.Z.; Joya, M.R.; Longo, E.; Varela, J.A.; Pizani, P.S.; Souza, A.G.

2008-01-01

The synthesis and characterization of CuO flower-nanostructure processed in domestic hydrothermal microwave oven was presented. Phase analysis was carried out using X-ray diffraction (XRD) and micro-Raman scattering (MRS) and the results confirmed the CuO flower-nanostructure as a single-phase. The field-emission scanning electron microscopy (FEG-SEM) was used to estimate the average spheres diameter while transmission electron microscope (TEM) to observe the thorn of the flower-nanostructures. The mechanism of CuO flower-nanostructures formation is proposed and explained

Synthesis and characterization of CuO flower-nanostructure processing by a domestic hydrothermal microwave

Energy Technology Data Exchange (ETDEWEB)

Volanti, D.P. [Laboratorio Interdisciplinar em Ceramica, Departamento de Fisico-Quimica, Instituto de Quimica, Universidade Estadual Paulista, P.O. Box 355, 14801-907 Araraquara, SP (Brazil); Keyson, D. [Laboratorio de Ensino de Ciencias e Laboratorio de Combustiveis e Materiais, Departamento de Quimica, Universidade Federal da Paraiba, 58051-900 Joao Pessoa, PB (Brazil); Cavalcante, L.S. [Laboratorio Interdisciplinar de Eletroquimica e Ceramica, Departamento de Quimica, Universidade Federal de Sao Carlos, P.O. Box 676, 13565-905 Sao Carlos, SP (Brazil)], E-mail: laeciosc@bol.com.br; Simoes, A.Z. [Laboratorio Interdisciplinar em Ceramica, Departamento de Fisico-Quimica, Instituto de Quimica, Universidade Estadual Paulista, P.O. Box 355, 14801-907 Araraquara, SP (Brazil); Joya, M.R. [Departamento de Fisica, Universidade Federal de Sao Carlos, P.O. Box 676, 13565-905 Sao Carlos, SP (Brazil); Longo, E.; Varela, J.A. [Laboratorio Interdisciplinar em Ceramica, Departamento de Fisico-Quimica, Instituto de Quimica, Universidade Estadual Paulista, P.O. Box 355, 14801-907 Araraquara, SP (Brazil); Pizani, P.S. [Departamento de Fisica, Universidade Federal de Sao Carlos, P.O. Box 676, 13565-905 Sao Carlos, SP (Brazil); Souza, A.G. [Laboratorio de Ensino de Ciencias e Laboratorio de Combustiveis e Materiais, Departamento de Quimica, Universidade Federal da Paraiba, 58051-900 Joao Pessoa, PB (Brazil)

2008-07-14

The synthesis and characterization of CuO flower-nanostructure processed in domestic hydrothermal microwave oven was presented. Phase analysis was carried out using X-ray diffraction (XRD) and micro-Raman scattering (MRS) and the results confirmed the CuO flower-nanostructure as a single-phase. The field-emission scanning electron microscopy (FEG-SEM) was used to estimate the average spheres diameter while transmission electron microscope (TEM) to observe the thorn of the flower-nanostructures. The mechanism of CuO flower-nanostructures formation is proposed and explained.

Sb{sub 2}Te{sub 3} nanobelts and nanosheets: Hydrothermal synthesis, morphology evolution and thermoelectric properties

Energy Technology Data Exchange (ETDEWEB)

Dong, Guo-Hui [State Key Laboratory of High Performance Ceramics and Superfine Microstructure, Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 200050 (China); Zhu, Ying-Jie, E-mail: y.j.zhu@mail.sic.ac.cn [State Key Laboratory of High Performance Ceramics and Superfine Microstructure, Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 200050 (China); Cheng, Guo-Feng; Ruan, Yin-Jie [State Key Laboratory of High Performance Ceramics and Superfine Microstructure, Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 200050 (China)

2013-02-15

Graphical abstract: Sb{sub 2}Te{sub 3} nanobelts and nanosheets were synthesized by a hydrothermal method, and the morphology evolution from Sb{sub 2}Te{sub 3} nanobelts to nanosheets with the prolonging hydrothermal time was observed. Highlights: Black-Right-Pointing-Pointer Hydrothermal synthesis of Sb{sub 2}Te{sub 3} nanobelts and nanosheets is demonstrated. Black-Right-Pointing-Pointer The morphology of Sb{sub 2}Te{sub 3} can be adjusted by varying hydrothermal time. Black-Right-Pointing-Pointer The morphology evolution of Sb{sub 2}Te{sub 3} from nanobelts to nanosheets is observed. Black-Right-Pointing-Pointer High Seebeck coefficients (S) of Sb{sub 2}Te{sub 3} nanobelts and nanosheets are attained. - Abstract: Sb{sub 2}Te{sub 3} nanobelts and nanosheets were synthesized by a hydrothermal method using SbCl{sub 3} and TeO{sub 2} as the antimony and tellurium source, hydrazine hydrate as a reducing reagent, polyvinyl alcohol as a surfactant and water as the solvent. The effects of experimental parameters on the product were investigated. The experiments indicated that the elemental Te formed during the reaction, acting as a reactive and self-sacrificial template for the formation of Sb{sub 2}Te{sub 3} nanobelts. The morphology evolution from Sb{sub 2}Te{sub 3} nanobelts to nanosheets with the prolonging hydrothermal time was observed. The products were characterized by X-ray powder diffraction (XRD), transmission electron microscopy (TEM), energy dispersive spectroscopy (EDS), selected area electron diffraction (SAED), Fourier transform infrared (FTIR) spectroscopy and differential scanning calorimetry (DSC). The thermoelectric properties of the tablet samples of Sb{sub 2}Te{sub 3} nanostructured powders with different morphologies prepared by a room-temperature pressurized method were investigated.

Hydrothermally synthesised Fe{sub 2}O{sub 3} nanoparticles as catalyst precursors for the CVD production of graphitic nanofibres

Energy Technology Data Exchange (ETDEWEB)

Edwards, H K [School of Mechanical, Materials and Manufacturing Engineering, University of Nottingham, University Park, Nottingham, NG7 2RD (United Kingdom); Evans, E [School of Chemistry, University of Nottingham, University Park, Nottingham, NG7 2RD (United Kingdom); McCaldin, S [School of Mechanical, Materials and Manufacturing Engineering, University of Nottingham, University Park, Nottingham, NG7 2RD (United Kingdom); Blood, P [School of Chemistry, University of Nottingham, University Park, Nottingham, NG7 2RD (United Kingdom); Gregory, D H [School of Chemistry, University of Nottingham, University Park, Nottingham, NG7 2RD (United Kingdom); Poliakoff, M [School of Chemistry, University of Nottingham, University Park, Nottingham, NG7 2RD (United Kingdom); Lester, E [School of Chemical Engineering and Mining Engineering, University of Nottingham, University Park, Nottingham, NG7 2RD (United Kingdom); Walker, G S [School of Mechanical, Materials and Manufacturing Engineering, University of Nottingham, University Park, Nottingham, NG7 2RD (United Kingdom); Brown, P D [School of Mechanical, Materials and Manufacturing Engineering, University of Nottingham, University Park, Nottingham, NG7 2RD (United Kingdom)

2006-02-22

Graphitic nanofibres (GNFs) have been grown by chemical vapour deposition at 500 deg. C and 700 deg. C, using 6 nm and 20 nm particles of Fe{sub 2}O{sub 3} produced by supercritical water hydrothermal synthesis (scWHS). The morphologies of catalyst and GNFs have been examined using the combined techniques of conventional transmission electron microscopy, high resolution electron microscopy, selected area electron diffraction and powder X-ray diffraction. GNF production varied from well ordered nanofibres with an average diameter of 100 nm, to very large, disordered fibres with diameters ranging from 500 nm to {approx}2 {mu}m. Larger fibres were found to have a compound structure composed of discreet domains of graphite and multiwall nanotubes. 20 nm particles produced by scWHS were associated with significant increases in the yield of GNFs as compared with traditional catalyst precipitation routes.

Oxalic acid induced hydrothermal synthesis of single crystalline tungsten oxide nanorods

International Nuclear Information System (INIS)

Patil, V.B.; Adhyapak, P.V.; Suryavanshi, S.S.; Mulla, I.S.

2014-01-01

Highlights: • We report synthesis of 1D tungsten oxide using a hydrothermal route at 170 °C. • Oxalic acid plays an important role in the formation of 1D nanostructure. • Monoclinic transforms to hexagonal phase with increment in reaction duration. -- Abstract: One-dimensional single-crystalline tungsten oxide nanorods have been synthesized by the hydrothermal technique. The controlled morphology of tungsten oxide was obtained by using sodium tungstate and oxalic acid as an organic inducer. The reaction was carried out at 170 °C for 24, 48 and 72 h. The obtained tungsten oxides were investigated by using XRD, SEM and HRTEM techniques. In order to understand the role of organic inducer on the shape, size and phase formation of WO 3 was prepared with and without organic inducer. On heating of sodium tungstate without organic inducer for 72 h at 170 °C in the hydrothermal unit we obtain nanoparticles of monoclinic WO 3 , however, on addition of oxalic acid a single phase hexagonal WO 3 with distinct nanorods was formed. On addition of oxalic acid a systematic emergence of nanorod-like morphology was obtained with incrementing reaction times from 24 h to 48 h. The 72 h reaction generates self-assembled 20–30 nm diameter and 4–5 μm long h-WO 3 bundles of nanorods. The XRD studies show hexagonal structure of tungsten oxide, while SAED reveals its single crystalline nature. The photoluminescence (PL) emission spectrum shows a characteristic blue emission peak at 3 eV (410 nm). Raman spectra provide the evidence of hexagonal structure with stretching vibrations (830 cm −1 ) for 72 h of heating at 170 °C

Oxalic acid induced hydrothermal synthesis of single crystalline tungsten oxide nanorods

Energy Technology Data Exchange (ETDEWEB)

Patil, V.B. [School of Physical Sciences, Solapur University, Solapur 413255 (India); Adhyapak, P.V. [Centre for Materials for Electronic Technology (C-MET), Pune 411008 (India); Suryavanshi, S.S., E-mail: sssuryavanshi@rediffmail.com [School of Physical Sciences, Solapur University, Solapur 413255 (India); Mulla, I.S., E-mail: ismulla2001@gmail.com [Emeritus Scientist (CSIR), Centre for Materials for Electronic Technology (C-MET), Pune 411008 (India)

2014-03-25

Highlights: • We report synthesis of 1D tungsten oxide using a hydrothermal route at 170 °C. • Oxalic acid plays an important role in the formation of 1D nanostructure. • Monoclinic transforms to hexagonal phase with increment in reaction duration. -- Abstract: One-dimensional single-crystalline tungsten oxide nanorods have been synthesized by the hydrothermal technique. The controlled morphology of tungsten oxide was obtained by using sodium tungstate and oxalic acid as an organic inducer. The reaction was carried out at 170 °C for 24, 48 and 72 h. The obtained tungsten oxides were investigated by using XRD, SEM and HRTEM techniques. In order to understand the role of organic inducer on the shape, size and phase formation of WO{sub 3} was prepared with and without organic inducer. On heating of sodium tungstate without organic inducer for 72 h at 170 °C in the hydrothermal unit we obtain nanoparticles of monoclinic WO{sub 3}, however, on addition of oxalic acid a single phase hexagonal WO{sub 3} with distinct nanorods was formed. On addition of oxalic acid a systematic emergence of nanorod-like morphology was obtained with incrementing reaction times from 24 h to 48 h. The 72 h reaction generates self-assembled 20–30 nm diameter and 4–5 μm long h-WO{sub 3} bundles of nanorods. The XRD studies show hexagonal structure of tungsten oxide, while SAED reveals its single crystalline nature. The photoluminescence (PL) emission spectrum shows a characteristic blue emission peak at 3 eV (410 nm). Raman spectra provide the evidence of hexagonal structure with stretching vibrations (830 cm{sup −1}) for 72 h of heating at 170 °C.

Hydrothermal synthesis of nanostructured titania

International Nuclear Information System (INIS)

Yoshito, Walter Kenji; Ferreira, Nildemar A.M.; Rumbao, Ana Carolina S. Coutinho; Lazar, Dolores R.R.; Ussui, Valter

2009-01-01

Titania ceramics have many applications due to its surface properties and, recently, its nanostructured compounds, prepared by hydrothermal treatments, have been described to improve these properties. In this work, commercial titanium dioxide was treated with 10% sodium hydroxide solution in a pressurized reactor at 150°C for 24 hours under vigorous stirring and then washed following two different procedures. The first one consisted of washing with water and ethanol and the second with water and hydrochloric acid solution (1%). Resulting powders were characterized by X-ray diffraction, N 2 gas adsorption and field emission gun scanning and transmission electronic microscopy. Results showed that from an original starting material with mainly rutile phase, both anatase and H 2 Ti 3 O 7 phase could be identified after the hydrothermal treatment. Surface area of powders presented a notable increase of one order of magnitude and micrographs showed a rearrangement on the microstructure of powders. (author)

Zinc stannate nanostructures: hydrothermal synthesis

International Nuclear Information System (INIS)

Baruah, Sunandan; Dutta, Joydeep

2011-01-01

Nanostructured binary semiconducting metal oxides have received much attention in the last decade owing to their unique properties rendering them suitable for a wide range of applications. In the quest to further improve the physical and chemical properties, an interest in ternary complex oxides has become noticeable in recent times. Zinc stannate or zinc tin oxide (ZTO) is a class of ternary oxides that are known for their stable properties under extreme conditions, higher electron mobility compared to its binary counterparts and other interesting optical properties. The material is thus ideal for applications from solar cells and sensors to photocatalysts. Among the different methods of synthesizing ZTO nanostructures, the hydrothermal method is an attractive green process that is carried out at low temperatures. In this review, we summarize the conditions leading to the growth of different ZTO nanostructures using the hydrothermal method and delve into a few of its applications reported in the literature. (topical review)

Hydrothermal synthesis of nanostructured titania

International Nuclear Information System (INIS)

Yoshito, W.K.; Ferreira, N.A.M.; Lazar, D.R.R.; Ussui, V.; Rumbao, A.C.S.

2011-01-01

Titania ceramics have many applications due to its surface properties and, recently, its nanostructured compounds, prepared by hydrothermal treatments, have been described to improve these properties. In this work, commercial titanium dioxide was treated with 10% sodium hydroxide solution in a pressurized reactor at 150 deg C for 24 hours under vigorous stirring and then washed following two different procedures. The first one consisted of washing with water and ethanol and the second with water and hydrochloric acid solution (1%). Resulting powders were characterized by X-ray diffraction, N 2 gas adsorption and field emission gun scanning and transmission electronic microscopy. Results showed that from an original starting material with mainly rutile phase, both anatase and H 2 Ti 3 O 7 phase could be identified after the hydrothermal treatment. Surface area of powders presented a notable increase of one order of magnitude and micrographs showed a rearrangement on the microstructure of powders. (author)

A catechol-like phenolic ligand-functionalized hydrothermal carbon: One-pot synthesis, characterization and sorption behavior toward uranium

Energy Technology Data Exchange (ETDEWEB)

Li, Bo; Ma, Lijian; Tian, Yin; Yang, Xiaodan; Li, Juan; Bai, Chiyao; Yang, Xiaoyu; Zhang, Shuang; Li, Shoujian, E-mail: sjli000616@scu.edu.cn; Jin, Yongdong, E-mail: jinyongdong@scu.edu.cn

2014-04-01

Highlights: • A new catechol-like ligand-functionalized hydrothermal carbon sorbent is synthesized. • A combination of bayberry tannin and glyoxal is firstly used as starting materials. • Simple, economically viable and environment-friendly synthesis method. • The sorbent exhibits high sorption capacity and distinct selectivity for uranium. - Abstract: We proposed a new approach for preparing an efficient uranium-selective solid phase extractant (HTC-btg) by choosing bayberry tannin as the main building block and especially glyoxal as crosslinking agent via a simple, economic, and green one-pot hydrothermal synthesis. The results of characterization and analysis show that after addition of glyoxal into only bayberry tannin-based hydrothermal reaction system, the as-synthesized HTC-btg displayed higher thermal stability, larger specific surface area and more than doubled surface phenolic hydroxyl groups. The sorption behavior of the sorbents toward uranium under various conditions was investigated in detail and the results indicated that the process is fast, endothermic, spontaneous, and pseudo-second-order chemisorption. The U(VI) sorption capacity reached up to 307.3 mg g{sup −1} under the current experimental conditions. The selective sorption in a specially designed multi-ion solution containing 12 co-existing cations over the range of pH 1.0–4.5 shown that the amount of uranium sorbed accounts for about 53% of the total sorption amount at pH 4.5 and distinctively about 85%, unreported so far to our knowledge, at pH 2.0. Finally, a possible mechanism involving interaction between uranyl ions and phenolic hydroxyl groups on HTC-btg was proposed.

A catechol-like phenolic ligand-functionalized hydrothermal carbon: One-pot synthesis, characterization and sorption behavior toward uranium

International Nuclear Information System (INIS)

Li, Bo; Ma, Lijian; Tian, Yin; Yang, Xiaodan; Li, Juan; Bai, Chiyao; Yang, Xiaoyu; Zhang, Shuang; Li, Shoujian; Jin, Yongdong

2014-01-01

Highlights: • A new catechol-like ligand-functionalized hydrothermal carbon sorbent is synthesized. • A combination of bayberry tannin and glyoxal is firstly used as starting materials. • Simple, economically viable and environment-friendly synthesis method. • The sorbent exhibits high sorption capacity and distinct selectivity for uranium. - Abstract: We proposed a new approach for preparing an efficient uranium-selective solid phase extractant (HTC-btg) by choosing bayberry tannin as the main building block and especially glyoxal as crosslinking agent via a simple, economic, and green one-pot hydrothermal synthesis. The results of characterization and analysis show that after addition of glyoxal into only bayberry tannin-based hydrothermal reaction system, the as-synthesized HTC-btg displayed higher thermal stability, larger specific surface area and more than doubled surface phenolic hydroxyl groups. The sorption behavior of the sorbents toward uranium under various conditions was investigated in detail and the results indicated that the process is fast, endothermic, spontaneous, and pseudo-second-order chemisorption. The U(VI) sorption capacity reached up to 307.3 mg g −1 under the current experimental conditions. The selective sorption in a specially designed multi-ion solution containing 12 co-existing cations over the range of pH 1.0–4.5 shown that the amount of uranium sorbed accounts for about 53% of the total sorption amount at pH 4.5 and distinctively about 85%, unreported so far to our knowledge, at pH 2.0. Finally, a possible mechanism involving interaction between uranyl ions and phenolic hydroxyl groups on HTC-btg was proposed

In situ reduction of as-prepared γ-Iron Oxide Nanoparticles

DEFF Research Database (Denmark)

Garbus, Pelle Gorm; Ahlburg, Jakob; Christensen, Mogens

-ray diffraction measurement. The as-prepared maghemite nanoparticles were synthesized by the continuous decomposition of solutes in supercritical hydrothermal flow synthesis [3, 4]. The reagent used was ferric ammonium citrate (C6H8O7•xFe(III)•yNH3) that under hydrothermal flow synthesis decomposes into the γ......-iron oxide Fe2O3. The reduction of maghemite to body centered cubic (BCC) iron does not go through a detectable intermediate state.1.Jensen, K.M., et al., Mechanisms for iron oxide formation under hydrothermal conditions: an in situ total scattering study. ACS nano, 2014. 8(10): p. 10704-10714.2.Andersen, H...

Hydrothermal synthesis of pollucite, analcime and their solid solutions and analysis of their properties

Energy Technology Data Exchange (ETDEWEB)

Jing, Zhenzi, E-mail: zzjing@tongji.edu.cn [Key Laboratory of Advanced Civil Engineering Materials, Ministry of Education, Tongji University, 4800 Cao' an Road, Shanghai 201804 (China); Cai, Kunchuan; Li, Yan; Fan, Junjie; Zhang, Yi; Miao, Jiajun; Chen, Yuqian [Key Laboratory of Advanced Civil Engineering Materials, Ministry of Education, Tongji University, 4800 Cao' an Road, Shanghai 201804 (China); Jin, Fangming [School of Environmental Science and Engineering, Shanghai Jiao Tong University, 800 Dongchuan Road, Shanghai 200240 (China)

2017-05-15

Pollucite, as a perfect long-term potential host for radioactive Cs immobilization, barely exists in pure form naturally but in an isomorphism form between pollucite and analcime due to coexistence of Cs and Na. Pollucite could be hydrothermally synthesized with Cs-polluted soil or clay minerals which contain Cs and Na, and it is necessary to study the properties of the synthesis if Cs and Na contained. Pure pollucite, analcime and their solid solutions were hydrothermally synthesized with chemicals, and it was found that the most formed pollucite analcime solid solutions with Cs/(Cs + Na) ratios of 2/6–5/6 had very similar properties in mineral composition, morphology and size, structural water (Cs cations) and coordination environment to pollucite. This also suggests that even coexistence of Cs and Na in nature, pollucite favors to form due to site preference for Cs over Na, which leads to the property and the structure of the most solid solutions similar to that of pollucite. - Highlights: •Pure pollucite barely exists in nature due to coexistence of Cs and Na. •Pollucite, analcime and their solid solutions could be hydrothermally synthesized. •Most formed solid solutions were found to have similar properties to pollucite. •Even coexistence in nature, pollucite favors to form due to site preference for Cs over Na.

A review on hydrothermal pre-treatment technologies and environmental profiles of algal biomass processing.

Science.gov (United States)

Patel, Bhavish; Guo, Miao; Izadpanah, Arash; Shah, Nilay; Hellgardt, Klaus

2016-01-01

The need for efficient and clean biomass conversion technologies has propelled Hydrothermal (HT) processing as a promising treatment option for biofuel production. This manuscript discussed its application for pre-treatment of microalgae biomass to solid (biochar), liquid (biocrude and biodiesel) and gaseous (hydrogen and methane) products via Hydrothermal Carbonisation (HTC), Hydrothermal Liquefaction (HTL) and Supercritical Water Gasification (SCWG) as well as the utility of HT water as an extraction medium and HT Hydrotreatment (HDT) of algal biocrude. In addition, the Solar Energy Retained in Fuel (SERF) using HT technologies is calculated and compared with benchmark biofuel. Lastly, the Life Cycle Assessment (LCA) discusses the limitation of the current state of art as well as introduction to new potential input categories to obtain a detailed environmental profile. Copyright © 2015 Elsevier Ltd. All rights reserved.

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

Science.gov (United States)

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

2015-01-01

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

Hydrothermal synthesis of polyethylenimine-protected high luminescent Pt-nanoclusters and their application to the detection of nitroimidazoles

International Nuclear Information System (INIS)

Xu, Na; Li, Hong-Wei; Wu, Yuqing

2017-01-01

A novel one-step hydrothermal synthesis of highly fluorescent platinum nanoclusters protected by polyethylenimine (Pt-NCs@PEI) is described. The products are characterized well by UV–vis absorption, fluorescence spectra, X-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM) imaging. The Pt-NCs@PEI possess high quantum yield at 28%, which is the relatively high one among the reported Pt-NCs; especially, the synthesis is in one-step and the reaction time is much shorter (<1 h) than the related methods. In addition, the Pt-NCs@PEI have large Stocks-shift (∼150 nm), high tolerability to the extreme pH and high ionic strengths, and excellent photo-stability under UV–vis irradiation, lay the foundation for the practical bio-applications. Finally, the obtained Pt-NCs@PEI are used to determine trace amount of metronidazole (MTZ) in buffer solution in showing a linear response over a concentration range of 0.25–300 μM and a low detection limit of 0.1 μM. Furthermore, the related investigation on response mechanism will be helpful to design and synthesize new metal nanoclusters as fluorescent probe to detect the trace amount of harmful medicine residuum as nitroimidazoles in human body. - Highlights: • This paper provides the first hydrothermal synthesis of platinum nanoclusters. • The prepared polyethylenimine-protected platinum nanoclusters possess high quantum yield of 28%. • A new method to detect trace amount of metronidazole in urine is proposed.

Hydrothermal synthesis of polyethylenimine-protected high luminescent Pt-nanoclusters and their application to the detection of nitroimidazoles

Energy Technology Data Exchange (ETDEWEB)

Xu, Na [State Key Laboratory of Supramolecular Structure and Materials, College of Chemistry, Jilin University, Changchun, 130012 (China); College of Materials Science and Engineering, Jilin Institute of Chemical Technology, Jilin, 132022 (China); Li, Hong-Wei, E-mail: lihongwei@jlu.edu.cn [State Key Laboratory of Supramolecular Structure and Materials, College of Chemistry, Jilin University, Changchun, 130012 (China); Wu, Yuqing, E-mail: yqwu@jlu.edu.cn [State Key Laboratory of Supramolecular Structure and Materials, College of Chemistry, Jilin University, Changchun, 130012 (China)

2017-03-15

A novel one-step hydrothermal synthesis of highly fluorescent platinum nanoclusters protected by polyethylenimine (Pt-NCs@PEI) is described. The products are characterized well by UV–vis absorption, fluorescence spectra, X-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM) imaging. The Pt-NCs@PEI possess high quantum yield at 28%, which is the relatively high one among the reported Pt-NCs; especially, the synthesis is in one-step and the reaction time is much shorter (<1 h) than the related methods. In addition, the Pt-NCs@PEI have large Stocks-shift (∼150 nm), high tolerability to the extreme pH and high ionic strengths, and excellent photo-stability under UV–vis irradiation, lay the foundation for the practical bio-applications. Finally, the obtained Pt-NCs@PEI are used to determine trace amount of metronidazole (MTZ) in buffer solution in showing a linear response over a concentration range of 0.25–300 μM and a low detection limit of 0.1 μM. Furthermore, the related investigation on response mechanism will be helpful to design and synthesize new metal nanoclusters as fluorescent probe to detect the trace amount of harmful medicine residuum as nitroimidazoles in human body. - Highlights: • This paper provides the first hydrothermal synthesis of platinum nanoclusters. • The prepared polyethylenimine-protected platinum nanoclusters possess high quantum yield of 28%. • A new method to detect trace amount of metronidazole in urine is proposed.

Hierarchically nanostructured hydroxyapatite: hydrothermal synthesis, morphology control, growth mechanism, and biological activity

Directory of Open Access Journals (Sweden)

Ma MG

2012-04-01

Full Text Available Ming-Guo MaInstitute of Biomass Chemistry and Technology, College of Materials Science and Technology, Beijing Forestry University, Beijing, People's Republic of ChinaAbstract: Hierarchically nanosized hydroxyapatite (HA with flower-like structure assembled from nanosheets consisting of nanorod building blocks was successfully synthesized by using CaCl2, NaH2PO4, and potassium sodium tartrate via a hydrothermal method at 200°C for 24 hours. The effects of heating time and heating temperature on the products were investigated. As a chelating ligand and template molecule, the potassium sodium tartrate plays a key role in the formation of hierarchically nanostructured HA. On the basis of experimental results, a possible mechanism based on soft-template and self-assembly was proposed for the formation and growth of the hierarchically nanostructured HA. Cytotoxicity experiments indicated that the hierarchically nanostructured HA had good biocompatibility. It was shown by in-vitro experiments that mesenchymal stem cells could attach to the hierarchically nanostructured HA after being cultured for 48 hours.Objective: The purpose of this study was to develop facile and effective methods for the synthesis of novel hydroxyapatite (HA with hierarchical nanostructures assembled from independent and discrete nanobuilding blocks.Methods: A simple hydrothermal approach was applied to synthesize HA by using CaCl2, NaH2PO4, and potassium sodium tartrate at 200°C for 24 hours. The cell cytotoxicity of the hierarchically nanostructured HA was tested by MTT (3-(4,5-dimethylthiazol-2-yl-2,5-diphenyltetrazolium bromide assay.Results: HA displayed the flower-like structure assembled from nanosheets consisting of nanorod building blocks. The potassium sodium tartrate was used as a chelating ligand, inducing the formation and self-assembly of HA nanorods. The heating time and heating temperature influenced the aggregation and morphology of HA. The cell viability did

BIOGENIC VS. ABIOGENIC ISOTOPE SIGNATURES OF REDUCED CARBON COMPOUNDS: A LESSON FROM HYDROTHERMAL SYNTHESIS EXPERIMENTS

International Nuclear Information System (INIS)

Horita, J.

2001-01-01

With growing interest in and demonstrated cases of inorganic hydrothermal synthesis of reduced or organic carbon compounds from CO and CO(sub 2), it becomes crucial to establish geochemical criteria to distinguish reduced/organic carbon compounds of abiogenic origin from those of biogenic origin with overwhelming abundances on the surface and in subsurface of the Earth. Chemical and isotopic compositions, particularly(sup 13)C/(sup 12)C ratios, of reduced/organic carbon compounds have been widely utilized for deducing the origins and formation pathways of these compounds. An example is isotopic and C(sub 1)/(C(sub 2)+C(sub 3)) ratios of natural gases, which have been used to distinguish bacterial, thermogenic, and possible abiogenic origins. Another example is that ancient graphitic carbon with(delta)(sup 13)C values c-25per thousand has been considered of biogenic origin. Although these criteria could be largely valid, growing data including those from our hydrothermal experiments suggest that a great caution must be exercised

Diiodination of Alkynes in supercritical Carbon dioxide

Institute of Scientific and Technical Information of China (English)

李金恒; 谢叶香; 尹笃林; 江焕峰

2003-01-01

A general,green and efficient method for the synthesis of transdiiodoalkenes in CO2(sc) has been developed.Trans-diiodoalkenes were obtained stereospecifically in quantitative yields via diiodination of both electron-rich and electron-deficient alkynes in the presence of KI,Ce(SO4)2 and water in supercritical carbon dioxide [CO2(sc)]at 40℃.

Hydrothermal Growth of Polyscale Crystals

Science.gov (United States)

Byrappa, Kullaiah

In this chapter, the importance of the hydrothermal technique for growth of polyscale crystals is discussed with reference to its efficiency in synthesizing high-quality crystals of various sizes for modern technological applications. The historical development of the hydrothermal technique is briefly discussed, to show its evolution over time. Also some of the important types of apparatus used in routine hydrothermal research, including the continuous production of nanosize crystals, are discussed. The latest trends in the hydrothermal growth of crystals, such as thermodynamic modeling and understanding of the solution chemistry, are elucidated with appropriate examples. The growth of some selected bulk, fine, and nanosized crystals of current technological significance, such as quartz, aluminum and gallium berlinites, calcite, gemstones, rare-earth vanadates, electroceramic titanates, and carbon polymorphs, is discussed in detail. Future trends in the hydrothermal technique, required to meet the challenges of fast-growing demand for materials in various technological fields, are described. At the end of this chapter, an Appendix 18.A containing a more or less complete list of the characteristic families of crystals synthesized by the hydrothermal technique is given with the solvent and pressure-temperature (PT) conditions used in their synthesis.

Preparation of minute particle using supercritical fluid; Chorinkai ryutai wo mochiita biryushi no chosei

Energy Technology Data Exchange (ETDEWEB)

Ajiri, T [Tohoku University, Sendai (Japan). Faculty of Engineering

1995-03-05

The metal oxide minute particle synthesis method according to the water-heat reaction in supercritical water was described. Metal salt liquid solution was subjected to hydrolysis when heated to become metal hydroxide but dehydration reaction was generated at a high temperature to generate metal oxide minute particle. Metal salt aqueous solution was supplied to a circulation system unit to contact heated water and was rapidly heated to supercritical state and then was subjected to hydrolysis/dehydration reaction, thus continuously collecting metal oxide minute particles. The hydrolysis speed was in first order for the metal ion concentration and the reaction speed was accelerated by several tens of times when entering supercritical region from subcritical region. When the temperature was rapidly increased to the supercritical state, a radical hydrolysis was generated and a high saturation was instantly reached and minute particles tended to be generated easily since the dissolution force of supercritical water for a product was small. A minute particle with a crystallizability of 5 nm was obtained by synthesizing ceria super-minute particle which was the abrasive of an optical glass material. A single phase of a high magnetization characteristic was synthesized continuously and quickly (faster than a conventional method by two orders or more) in the continuous synthesis of Ba ferrite as a magnetic recording material. 12 refs., 3 figs., 1 tab.

Template-directed synthesis of MS (M=Cd, Zn) hollow microsphere via hydrothermal method

Science.gov (United States)

Wang, Shi-Ming; Wang, Qiong-Sheng; Wan, Qing-Li

2008-05-01

CdS, ZnS hollow microspheres were prepared with chitosan as the synthesis template at 140 and 150 °C, respectively, by hydrothermal method. The resultant products were characterized by X-ray diffraction (XRD) measurements in order to determine the crystalline phase of the products. The structural and morphological features of the nanoparticles were investigated by transmission electron microscopy (TEM) and ultraviolet-visible diffuse reflection spectroscopy (DRS). The experimental results indicated that all the nanoparticles aggregated into hollow microspheres and chitosan as a template played an important role in the formation of hollow microspheres. In addition, an intermediate complex structure-controlling possible reaction mechanism was proposed in this paper.

Continuous Hydrothermal Flow Synthesis of Functional Oxide Nanomaterials Used in Energy Conversion Devices

DEFF Research Database (Denmark)

Xu, Yu

Continuous hydrothermal flow synthesis (CHFS) was used to prepare functional oxide nanoparticles. Materials synthesized include NiO, Y-doped ZrO2, Gd-doped CeO2, LaCrO3 and Ni-substituted CoFe2O4. These types of oxides can be applied in several energy conversion devices, e.g. as active materials...... as materials are continuously produced, and the technology can be scaled-up to an industrial-relevant production capacity. The thesis starts with investigating the most appropriate mixer design for a novel two-stage reactor by computational fluid dynamics modelling. On basis of the modelling results, a two......, dense continuous layers (

Synthesis of flower-like Boehmite (γ-AlOOH) via a one-step ionic liquid-assisted hydrothermal route

International Nuclear Information System (INIS)

Tang, Zhe; Liang, Jilei; Li, Xuehui; Li, Jingfeng; Guo, Hailing; Liu, Yunqi; Liu, Chenguang

2013-01-01

A simple and novel synthesis process, one-step ionic liquid-assisted hydrothermal synthesis route, has been developed in the work to synthesize Bohemithe (γ-AlOOH) with flower-like structure. The samples were characterized by X-ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FT-IR) and Scanning Electron Microscope (SEM). Ionic liquid [Omim] + Cl − , as a template, plays an important role in the morphology and pore structure of the products due to its strong interactions with reaction particles. With the increase in the dosage of ionic liquid [Omim] + Cl − , the morphology of the γ-AlOOH was changed from initial bundles of nanosheets (without ionic liquid) into final well-developed monodispersed 3D flower-like architectures ([Omim] + Cl − =72 mmol). The pore structure was also altered gradually from initial disordered slit-like pore into final relatively ordered ink-bottle pore. Furthermore, the proposed formation mechanism and other influencing factors such as reaction temperature and urea on formation and morphology of the γ-AlOOH have also been investigated. - Graphical abstract: The flower-like γ-AlOOH architectures composed by nanosheets with narrow size distribution (1.6–2.2 μm) and uniform pore size (6.92 nm) have been synthesized via a one-step ionic liquid-assisted hydrothermal route. - Highlights: • The γ-AlOOH microflowers were synthesized via an ionic liquid-assisted hydrothermal route. • Ionic liquid plays an important role on the morphology and porous structure of the products. • Ionic liquid can be easily removed from the products and reused in recycling experiments. • A “aggregation–recrystallization–Ostwald Ripening“formation mechanism may occur

Hydrothermal Synthesis and Mechanism of Unusual Zigzag Ag2Te and Ag2Te/C Core-Shell Nanostructures

Directory of Open Access Journals (Sweden)

Saima Manzoor

2014-01-01

Full Text Available A single step surfactant-assisted hydrothermal route has been developed for the synthesis of zigzag silver telluride nanowires with diameter of 50–60 nm and length of several tens of micrometers. Silver nitrate (AgNO3 and sodium tellurite (Na2TeO3, are the precursors and polyvinylpyrrolidone (PVP is used as surfactant in the presence of the reducing agent, that is, hydrazine hydrate (N2H4·H2O. In addition to the zigzag nanowires a facile hydrothermal reduction-carbonization route is proposed for the preparation of uniform core-shell Ag2Te/C nanowires. In case of Ag2Te/C synthesis process the same precursors are employed for Ag and Te along with the ethylene glycol used as reducing agent and glucose as the carbonizing agent. Morphological and compositional properties of the prepared products are analyzed with the help of scanning electron microscopy, transmission electron microscopy, and energy dispersive X-ray spectroscopy, respectively. The detailed formation mechanism of the zigzag morphology and reduction-carbonization growth mechanism for core-shell nanowires are illustrated on the bases of experimental results.

Chemical environments of submarine hydrothermal systems

Science.gov (United States)

Shock, Everett L.

1992-01-01

Perhaps because black-smoker chimneys make tremendous subjects for magazine covers, the proposal that submarine hydrothermal systems were involved in the origin of life has caused many investigators to focus on the eye-catching hydrothermal vents. In much the same way that tourists rush to watch the spectacular eruptions of Old Faithful geyser with little regard for the hydrology of the Yellowstone basin, attention is focused on the spectacular, high-temperature hydrothermal vents to the near exclusion of the enormous underlying hydrothermal systems. Nevertheless, the magnitude and complexity of geologic structures, heat flow, and hydrologic parameters which characterize the geyser basins at Yellowstone also characterize submarine hydrothermal systems. However, in the submarine systems the scale can be considerably more vast. Like Old Faithful, submarine hydrothermal vents have a spectacular quality, but they are only one fascinating aspect of enormous geologic systems operating at seafloor spreading centers throughout all of the ocean basins. A critical study of the possible role of hydrothermal processes in the origin of life should include the full spectrum of probable environments. The goals of this chapter are to synthesize diverse information about the inorganic geochemistry of submarine hydrothermal systems, assemble a description of the fundamental physical and chemical attributes of these systems, and consider the implications of high-temperature, fluid-driven processes for organic synthesis. Information about submarine hydrothermal systems comes from many directions. Measurements made directly on venting fluids provide useful, but remarkably limited, clues about processes operating at depth. The oceanic crust has been drilled to approximately 2.0 km depth providing many other pieces of information, but drilling technology has not allowed the bore holes and core samples to reach the maximum depths to which aqueous fluids circulate in oceanic crust. Such

Use of supercritical carbon dioxide extraction

Energy Technology Data Exchange (ETDEWEB)

Taniguchi, Masayuki (Niigata Univ., Faculty of Engineering, Niigata, (Japan))

1989-09-25

Supercritical fluid extraction is a novel diffusion and separation technique which exploits simultaneously the increase of vapor pressure and the difference of chemical affinities of fluids near the critical point. A solvent which is used as the supercritical fluid has the following features: the critical point exists in the position of relatively ease of handling, the solvent is applicable to the extraction of a physiological active substance of thermal instability. Carbon dioxide as the solvent is non-flammable, non-corrosive, non-toxic, cheap, and readily available of high purity. The results of studies on the use of supercritical carbon dioxide (SC-CO{sub 2}) as a solvent for natural products in the fermentation and food industries, were collected. SC-CO{sub 2} extraction are used in many fields, examples for the application are as follows: removal of organic solvents from antibiotics; extraction of vegetable oils contained in wheat germ oil, high quality mustard seeds, rice bran and so on; brewing of sake using rice and rice-koji; use as a non-aqueous medium for the synthesis of precursors of the Aspartame; and use in sterilization. 66 refs., 17 figs., 21 tabs.

Hydrothermal synthesis and characterization of novel vanadium oxides and their application as cathodes in lithium secondary batteries

Science.gov (United States)

Chirayil, Thomas George

Novel layered or tunneled vanadium oxides are sought as a substitute for the expensive Lisb{x}CoOsb2 cathode material in lithium rechargeable batteries. The hydrothermal synthesis approach was taken in search of new vanadium oxides in the presence of a structure directing cation, TMA. A systematic study was done on the hydrothermal synthesis of the Vsb{2}Osb{5}-TMAOH-LiOH system. It was determined from this study that the pH of the reaction mixture was very critical in the formation of many compounds. Acetic acid utilized to adjust the pH of the reaction mixture in the presence of TMA behaved as a buffer and maintained a constant pH during the reaction. Hydrothermal synthesis conducted between pH 10 and 2 resulted in the formation of 7 compounds. At the highest pH, a well known compound Lisb3VOsb4, was formed. Between pH 5.2-9, a layered compound, TMAVsb3Osb7 resulted. The thermal treatment of TMAVsb3Osb7 under oxygen lead to an oxidized phase, TMAVsb3Osb8, which increased its lithium capacity significantly. Between pH 5-6, a cluster compound, TMAsb8lbrack Vsb{22}Osb{54}(CHsb3COO)rbrack{*}4Hsb2O with the acetate ion trapped inside the caged Vsb{22}Osb{54} cluster, and a layered vanadium oxide, Lisb{x}Vsb{2-delta}Osb{4-delta}{*}Hsb2O was obtained. The Lisb{x}Vsb{2-delta}Osb{4-delta}{*}Hsb2O compound was dehydrated to form Lisb{x}Vsb{2-delta}Osb{4-delta} and the lithium was removed electrochemically to form a new type of "VOsb2". Several alkylamines, DMSO and an additional water molecule were intercalated to swell the layers of Lisb{x}Vsb{2-delta}Osb{4-delta}{*}Hsb2O. Lowering the pH between 3.0-3.5, resulted in layered compound, TMAVsb4Osb{10}, with TMA residing between the layers. Layered compounds, TMAVsb8Osb{20} and TMAsb{0.17}Hsp+sb{0.1}Vsb2Osb5, were obtained at very acidic conditions. The hydrothermally grown TMAsb{0.17}Hsp+sb{0.1}Vsb2Osb5 is similar to the xerogel Vsb2Osb5 intercalated with TMA synthesized by the sol-gel process. Several trends were observed

One-step hydrothermal synthesis of three-dimensional porous graphene aerogels/sulfur nanocrystals for lithium–sulfur batteries

International Nuclear Information System (INIS)

Jiang, Yong; Lu, Mengna; Ling, Xuetao; Jiao, Zheng; Chen, Lingli; Chen, Lu; Hu, Pengfei; Zhao, Bing

2015-01-01

Highlights: • 3D porous GA/S nanocrystals are prepared by a one-step hydrothermal method. • The structure is affected by hydrothermal temperature and liquid sulfur’s viscosity. • The hybrid delivers a capacity of 716.2 mA h g −1 after 50 cycles at 100 mA g −1 . • The nanosized S, strong adsorbability and intimate contact of GNS are main factors. - Abstract: Lithium–sulfur (Li–S) batteries are receiving significant attention as a new energy source because of its high theoretical capacity and specific energy. However, the low sulfur loading and large particles (usually in submicron dimension) in the cathode greatly offset its advantage in high energy density and lead to the instability of the cathode and rapid capacity decay. Herein, we introduce a one-step hydrothermal synthesis of three-dimensional porous graphene aerogels/sulfur nanocrystals to suppress the rapid fading of sulfur electrode. It is found that the hydrothermal temperature and viscosity of liquid sulfur have significant effects on particle size and loading mass of sulfur nanocrystals, graphitization degree of graphene and chemical bonding between sulfur and oxygen-containing groups of graphene. The hybrid could deliver a specific capacity of 716.2 mA h g −1 after 50 cycles at a current density of 100 mA g −1 and reversible capacity of 517.9 mA h g −1 at 1 A g −1 . The performance we demonstrate herein suggests that Li–S battery may provide an opportunity for development of rechargeable battery systems

Oleic-acid-coated CoFe2O4 nanoparticles synthesized by co-precipitation and hydrothermal synthesis

International Nuclear Information System (INIS)

Gyergyek, Sašo; Drofenik, Miha; Makovec, Darko

2012-01-01

Highlights: ► Synthesis of oleic-acid-coated CoFe 2 O 4 nanoparticles from an aqueous solution. ► During the co-precipitation of Co 2+ /Fe 3+ single-phase spinel forms. ► During the co-precipitation of Co 2+ /Fe 2+ , feroxyhyte forms in addition to spinel. ► Oleic acid increases the spinel formation temperature and limits particle growth. ► Colloidal suspensions of ferrimagnetic CoFe 2 O 4 were prepared. - Abstract: Oleic-acid-coated CoFe 2 O 4 nanoparticles were synthesized by co-precipitation and hydrothermal synthesis. The coprecipitation of the nanoparticles was achieved by the rapid addition of a strong base to an aqueous solution of cations in the presence of the oleic acid surfactant, or without this additive. The nanoparticles were also synthesized by a hydrothermal treatment of suspensions of the precipitates, coprecipitated at room temperature in the presence of the oleic acid, or without it. The influence of the synthesis conditions, such as the valence state of the iron cation in the starting aqueous solution, the temperature of the treatment and the presence of oleic acid, on the particles size was systematically studied. X-ray powder diffractometry (XRD) and transmission electron microscopy (TEM) coupled with energy-dispersive X-ray spectroscopy (EDS) revealed that, although spinel forms at room temperature, a substantial amount of Co was incorporated within the secondary, feroxyhyte-like phase when the iron cation was in the 2+ state. In contrast, when iron was in the 3+ state, the spinel forms at elevated temperatures of approximately 60 °C. The presence of the oleic acid further increased the formation temperature for the stoichiometric spinel. Moreover, the oleic acid impeded the particles’ growth and enabled the preparation of colloidal suspensions of the nanoparticles in non-polar organic solvents. The nanoparticles’ size was successfully controlled by the temperature of the synthesis in the region where superparamagnetism

Hydrothermal synthesis of thiol-capped CdTe nanoparticles and their optical properties.

Science.gov (United States)

Bu, Hang-Beom; Kikunaga, Hayato; Shimura, Kunio; Takahasi, Kohji; Taniguchi, Taichi; Kim, DaeGwi

2013-02-28

Water soluble nanoparticles (NPs) with a high emission property were synthesized via hydrothermal routes. In this report, we chose thiol ligand N-acetyl-L-cysteine as the ideal stabilizer and have successfully employed it to synthesize readily size-controllable CdTe NPs in a reaction of only one step. Hydrothermal synthesis of CdTe NPs has been carried out in neutral or basic conditions so far. We found out that the pH value of precursor solutions plays an important role in the uniformity of the particle size. Actually, high quality CdTe NPs were synthesized under mild acidic conditions of pH 5. The resultant NPs indicated good visible light-emitting properties and stability. Further, the experimental results showed that the reaction temperature influenced significantly the growth rate and the maximum size of the NPs. The CdTe NPs with a high photoluminescence quantum yield (the highest value: 57%) and narrower half width at half maximum (the narrowest value: 33 nm) were attained in very short time, within 40 minutes, reaching diameters of 2.3 to 4.3 nm. The PL intensity was increased with an increase in the reaction time, reflecting the suppression of nonradiative recombination processes. Furthermore, the formation of CdTe/CdS core-shell structures was discussed from the viewpoint of PL dynamics and X-ray diffraction studies.

The design and application of a new Bassett-type diamond anvil cell for spectroscopic analysis of supercritical aqueous solutions

International Nuclear Information System (INIS)

Anderson, A.J.; Meredith, P.R.; Bassett, W.A.; Mayanovic, R.A.; Benmore, C.

2010-01-01

The Bassett-type hydrothermal diamond anvil cell has been modified to facilitate direct x-ray and Raman spectroscopic analysis of aqueous solutions and/or coexisting solid samples at temperatures and pressures above the critical point of water. The new cell provides more sample-detector geometry options for x-ray micro beam analysis and the reduced size of the cell affords a smaller working distance (≥ 14 mm) required for better Raman spectroscopic analysis and microscopic inspection. A shallow recess (300 × 300 × 26.5 μm) milled into one of the diamond anvils is used instead of a metal gasket to contain the aqueous solution. These modifications significantly improve our ability to directly monitor the composition and structure of supercritical fluids and have eliminated the problem of contamination due to the reaction of a metal gasket with supercritical water. The use of the modified hydrothermal diamond anvil cell to characterize the MoO 3 -H 2 O system up to 500 o C will be discussed. (author)

SiC-dopped MCM-41 materials with enhanced thermal and hydrothermal stabilities

International Nuclear Information System (INIS)

Wang, Yingyong; Jin, Guoqiang; Tong, Xili; Guo, Xiangyun

2011-01-01

Graphical abstract: Novel SiC-dopped MCM-41 materials were synthesized by adding silicon carbide suspension in the molecular sieve precursor solvent followed by in situ hydrothermal synthesis. The dopped materials have a wormhole-like mesoporous structure and exhibit enhanced thermal and hydrothermal stabilities. Highlights: → SiC-dopped MCM-41 was synthesized by in situ hydrothermal synthesis of molecular sieve precursor combined with SiC. → The dopped MCM-41 materials show a wormhole-like mesoporous structure. → The thermal stability of the dopped materials have an increment of almost 100 o C compared with the pure MCM-41. → The hydrothermal stability of the dopped materials is also better than that of the pure MCM-41. -- Abstract: SiC-dopped MCM-41 mesoporous materials were synthesized by the in situ hydrothermal synthesis, in which a small amount of SiC was added in the precursor solvent of molecular sieve before the hydrothermal treatment. The materials were characterized by X-ray diffraction, transmission electron microscopy, X-ray photoelectron spectroscopy, N 2 physical adsorption and thermogravimetric analysis, respectively. The results show that the thermal and hydrothermal stabilities of MCM-41 materials can be improved obviously by incorporating a small amount of SiC. The structure collapse temperature of SiC-dopped MCM-41 materials is 100 o C higher than that of pure MCM-41 according to the differential scanning calorimetry analysis. Hydrothermal treatment experiments also show that the pure MCM-41 will losses it's ordered mesoporous structure in boiling water for 24 h while the SiC-dopped MCM-41 materials still keep partial porous structure.

Biomolecule-assisted hydrothermal synthesis of silver bismuth sulfide with nanostructures

International Nuclear Information System (INIS)

Kaowphong, Sulawan

2012-01-01

Silver bismuth sulfide (AgBiS 2 ) nanostructures were successfully prepared via a simple biomolecule-assisted hydrothermal synthesis at 200 °C for 12–72 h. Silver nitrate, bismuth nitrate and L-cysteine were used as starting materials. Here, the biomolecule, L-cysteine, was served as the sulfide source and a complexing agent. The products, characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM), were cubic AgBiS 2 nanoparticles with a diameter range of about 20–75 nm. It was found that their crystallinity and particle size increased with increasing reaction time. The energy dispersive X-ray spectroscopy (EDX) and inductively coupled plasma optical emission spectrophotometry (ICP-OES) analyses were used to confirm the stoichiometry of AgBiS 2 . The optical band gap of the AgBiS 2 nanoparticles, calculated from UV–vis spectra, was 3.0 eV which indicated a strong blue shift because of the quantum confinement effect. A possible formation mechanism of the AgBiS 2 nanoparticles was also discussed. - Graphical abstract: The optical band gap of the as-prepared AgBiS 2 nanoparticles displays a strong blue shift comparing to the 2.46 eV of bulk AgBiS 2 caused by the quantum confinement effects. Highlights: ► A simple biomolecule-assisted hydrothermal method is developed to prepare AgBiS 2 . ► L-Cysteine is served as the sulfide source and a complexing agent. ► Increase in band gap of the AgBiS 2 nanoparticles attributes to the quantum confinement effects.

Improving the circular economy via hydrothermal processing of high-density waste plastics.

Science.gov (United States)

Helmer Pedersen, Thomas; Conti, Federica

2017-10-01

Rising environmental concerns on climate changes are causing an increasing attention on circular economies. The plastic economy, in particular, is in focus due to the accelerating consumption of plastics, mainly derived from virgin feedstock, combined with the lack of plastic recycling strategies. This work presents a novel outlook on the potential of using supercritical hydrothermal processing of waste plastic fractions for tertiary recycling. The study investigates hydrothermal processing of nine different, high-density types of plastics into original resin monomers and other value-added chemical compounds. The outlook presents conversion yields, carbon balances, and chemical details on the products obtained. It is found that all the investigated resins are prone to hydrothermal treatment, and that high yields of monomers and high value compounds (up to nearly 100%), suitable for chemicals and fuels applications, can be obtained. For instance, for polycarbonate, styrene-butadiene, poly(lactic acid), poly(ethylene terephthalate), and poly(butylene terephthalate), original monomeric compounds can be reclaimed for manufacturing new resins. The promising results presented demonstrate that hydrothermal processing of high-density plastics is a prospective technology for increasing the circularity of the plastic economy. Copyright © 2017 Elsevier Ltd. All rights reserved.

Production of Valuables Organic Acids from Organic Wastes with Hydrothermal Treatment Process

Directory of Open Access Journals (Sweden)

Muhammad Faisal

2009-06-01

Full Text Available This article reports production of valuables organic acids from the hydrothermal treatment of representative organic wastes and compounds (i. e. domestic sludge, proteinaceous, cellulosic and plastic wastes with or without oxidant (H2O2. Organic acids such as acetic, formic, propionic, succinic and lactic acids were obtained in significant amounts. At 623 K (16.5 MPa, acetic acid of about 26 mg/g-dry waste fish entrails was obtained. This increased to 42 mg/g dry waste fish entrails in the presence of H2O2. Experiments on glucose to represent cellulosic wastes were also carried out, getting acetic acid of about 29 mg/g-glucose. The study was extended to terephthalic acid and glyceraldehyde, reaction intermediates of hydrothermal treatment of PET plastic wastes and glucose, respectively. Studies on temperature dependence of formation of organic acids showed thermal stability of acetic acid, whereas, formic acid decomposed readily under hydrothermal conditions. In general, results demonstrated that the presence of oxidants favored formation of organic acids with acetic acid being the major product. Keywords: hydrothermal treatment, organic acids, organic wastes, oxidant, supercritical water oxidation

Hydrothermal synthesis of two photoluminescent nitrogen-doped graphene quantum dots emitted green and khaki luminescence

International Nuclear Information System (INIS)

Zhu, Xiaohua; Zuo, Xiaoxi; Hu, Ruiping; Xiao, Xin; Liang, Yong; Nan, Junmin

2014-01-01

A simple and effective chemical synthesis of the photoluminescent nitrogen-doped graphene quantum dots (N-GQDs) biomaterial is reported. Using the hydrothermal treatment of graphene oxide (GO) in the presence of hydrogen peroxide (H 2 O 2 ) and ammonia, the N-GQDs are synthesized through H 2 O 2 exfoliating the GO into nanocrystals with lateral dimensions and ammonia passivating the generated active surface. Then, after a dialytic separation, two water-soluble N-GQDs with average size of about 2.1 nm/6.2 nm, which emit green/khaki luminescence and exhibit excitation dependent/independent photoluminescence (PL) behaviors, are obtained. In addition, it is also demonstrated that these two N-GQDs are stable over a broad pH range and have the upconversion PL property, showing this approach provides a simple and effective method to synthesize the functional N-GQDs. - Highlights: • Nitrogen-doped graphene quantum dots (N-GQDs) are prepared by hydrothermal routine. • Two N-GQDs with different size distribution emit green/khaki photoluminescence. • Two N-GQDs exhibit excitation-dependent/independent photoluminescence behaviors

Microwave assisted facile hydrothermal synthesis and characterization of zinc oxide flower grown on graphene oxide sheets for enhanced photodegradation of dyes

International Nuclear Information System (INIS)

Kashinath, L.; Namratha, K.; Byrappa, K.

2015-01-01

Graphical abstract: - Highlights: • Synthesis of hybrid ZnO–GO nanocomposite via microwave assisted facile hydrothermal method. • The in situ flower like ZnO nano particles are densely decorated and anchored on the surfaces of graphene oxide sheets. • They exhibited high adsorption measurement, increase in surface area and meso/micro porous in nature. • The structure and morphology plays a vital role in enhancing the photo response activities of degradation of dyes. - Abstract: Microwave assisted hydrothermal process of synthesis of ZnO–GO nanocomposite by using ZnCl 2 and NaOH as precursors is being reported first time. In this investigation, a novel route to study on synthesis, interaction, kinetics and mechanism of hybrid zinc oxide–graphene oxide (ZnO–GO) nanocomposite using microwave assisted facile hydrothermal method has been reported. The results shows that the ZnO–GO nanocomposite exhibits an enhancement and acts as stable photo-response degradation performance of Brilliant Yellow under the UV light radiation better than pure GO and ZnO nanoparticles. The microwave exposure played a vital role in the synthesis process, it facilitates with well define crystalline structure, porosity and fine morphology of ZnO/GO nanocomposite. Different molar concentrations of ZnO precursors doped to GO sheets were been synthesized, characterized and their photodegradation performances were investigated. The optical studies by UV–vis and Photo Luminescence shows an increase in band gap of nanocomposite, which added an advantage in photodegradation performance. The in situ flower like ZnO nano particles are were densely decorated and anchored on the surfaces of graphene oxide sheets which aids in the enhancement of the surface area, adsorption, mass transfer of dyes and evolution of oxygen species. The nanocomposite having high surface area and micro/mesoporous in nature. This structure and morphology supports significantly in increasing photo catalytic

Hydrothermal synthesis of size-controllable Yttrium Orthovanadate (YVO4) nanoparticles and its application in photocatalytic degradation of direct blue dye

International Nuclear Information System (INIS)

Mohamed, R.M.; Harraz, F.A.; Mkhalid, I.A.

2012-01-01

Graphical abstract: XRD patterns of YVO 4 nanopowders prepared at different hydrothermal times; where Y 1 = 4 h, Y 2 = 8 h, Y 3 = 12 h and Y 4 = 24 h. Highlights: ► Size control of Yttrium Orthovanadate. ► Hydrothermal synthesis. ► Removal of direct blue dye. - Abstract: Sized-controlled YVO 4 nanoparticles have been synthesized by a simple hydrothermal method by changing hydrothermal time from 4 to 24 h. The products were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), specific surface area (Brunauer–Emmett–Teller (BET)), and ultraviolet–visible spectroscopy (UV–vis) measurements. The results showed that the size of as-synthesized YVO 4 nanoparticles was in the range of 11–40 nm and was extremely dependent on the hydrothermal time. Photocatalytic measurement showed that the YVO 4 nanoparticles with particle size of about 11 nm (prepared by 4 h hydrothermal time) possess superior photocatalytic properties in the decolorization of direct blue dye. Due to simple preparation, high photocatalytic oxidation of direct blue dye and low cost, the YVO 4 photocatalyst is a potential candidate for pollutants removal and will find wide application in the coming future in photocatalytic oxidation processes. The overall kinetics of photodegradation of direct blue dye using YVO 4 nanopowders photocatalyst was found to be of first order. The photocatalyst could be easily removed from the reaction mixture and its recyclability with no loss of activity was possible for six times. The catalytic performance was found to decrease by 5% after run number six.

Hydrothermal synthesis of meso porous silica MCM-41 using commercial sodium silicate

International Nuclear Information System (INIS)

Melendez O, H. I.; Mercado S, A.; Garcia C, L. A.; Castruita, G.; Perera M, Y A.

2013-01-01

In this work, ordered meso porous silica MCM-41 was prepared by hydrothermal synthesis using industrial-grade sodium silicate (Na 2 SiO 3 ) as silica source, hexadecyltrimethyl-ammonium bromide (CTAB) as template agent and ethyl acetate as ph regulator. The influence of CTAB/SiO 2 molar ratio, reaction time, aging temperature, and co-surfactant type on the structural and morphological properties of the obtained silica was studied. The products were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy and nitrogen adsorption-desorption isotherms. Ordered meso porous MCM-41 silica was obtained at 80 C by using a range of CTAB/SiO 2 molar ratio from 0.35 to 0.71 and reaction times up to 72 h and isopropanol (i-Pr OH) as co-surfactant. (Author)

Ideas and perspectives: hydrothermally driven redistribution and sequestration of early Archaean biomass - the "hydrothermal pump hypothesis"

Science.gov (United States)

Duda, Jan-Peter; Thiel, Volker; Bauersachs, Thorsten; Mißbach, Helge; Reinhardt, Manuel; Schäfer, Nadine; Van Kranendonk, Martin J.; Reitner, Joachim

2018-03-01

Archaean hydrothermal chert veins commonly contain abundant organic carbon of uncertain origin (abiotic vs. biotic). In this study, we analysed kerogen contained in a hydrothermal chert vein from the ca. 3.5 Ga Dresser Formation (Pilbara Craton, Western Australia). Catalytic hydropyrolysis (HyPy) of this kerogen yielded n-alkanes up to n-C22, with a sharp decrease in abundance beyond n-C18. This distribution ( ≤ n-C18) is very similar to that observed in HyPy products of recent bacterial biomass, which was used as reference material, whereas it differs markedly from the unimodal distribution of abiotic compounds experimentally formed via Fischer-Tropsch-type synthesis. We therefore propose that the organic matter in the Archaean chert veins has a primarily microbial origin. The microbially derived organic matter accumulated in anoxic aquatic (surface and/or subsurface) environments and was then assimilated, redistributed and sequestered by the hydrothermal fluids (hydrothermal pump hypothesis).

One-step hydrothermal synthesis of three-dimensional porous graphene aerogels/sulfur nanocrystals for lithium–sulfur batteries

Energy Technology Data Exchange (ETDEWEB)

Jiang, Yong; Lu, Mengna; Ling, Xuetao; Jiao, Zheng; Chen, Lingli; Chen, Lu [School of Environmental and Chemical Engineering, Shanghai University, Shanghai 200444 (China); Hu, Pengfei [Instrumental Analysis and Research Center, Shanghai University, Shanghai 200444 (China); Zhao, Bing, E-mail: bzhao@shu.edu.cn [School of Environmental and Chemical Engineering, Shanghai University, Shanghai 200444 (China)

2015-10-05

Highlights: • 3D porous GA/S nanocrystals are prepared by a one-step hydrothermal method. • The structure is affected by hydrothermal temperature and liquid sulfur’s viscosity. • The hybrid delivers a capacity of 716.2 mA h g{sup −1} after 50 cycles at 100 mA g{sup −1}. • The nanosized S, strong adsorbability and intimate contact of GNS are main factors. - Abstract: Lithium–sulfur (Li–S) batteries are receiving significant attention as a new energy source because of its high theoretical capacity and specific energy. However, the low sulfur loading and large particles (usually in submicron dimension) in the cathode greatly offset its advantage in high energy density and lead to the instability of the cathode and rapid capacity decay. Herein, we introduce a one-step hydrothermal synthesis of three-dimensional porous graphene aerogels/sulfur nanocrystals to suppress the rapid fading of sulfur electrode. It is found that the hydrothermal temperature and viscosity of liquid sulfur have significant effects on particle size and loading mass of sulfur nanocrystals, graphitization degree of graphene and chemical bonding between sulfur and oxygen-containing groups of graphene. The hybrid could deliver a specific capacity of 716.2 mA h g{sup −1} after 50 cycles at a current density of 100 mA g{sup −1} and reversible capacity of 517.9 mA h g{sup −1} at 1 A g{sup −1}. The performance we demonstrate herein suggests that Li–S battery may provide an opportunity for development of rechargeable battery systems.

Synthesis of ZrO2 nanoparticles by hydrothermal treatment

International Nuclear Information System (INIS)

Machmudah, Siti; Widiyastuti, W.; Prastuti, Okky Putri; Nurtono, Tantular; Winardi, Sugeng; Wahyudiono,; Kanda, Hideki; Goto, Motonobu

2014-01-01

Zirconium oxide (zirconia, ZrO 2 ) is the most common material used for electrolyte of solid oxide fuel cells (SOFCs). Zirconia has attracted attention for applications in optical coatings, buffer layers for growing superconductors, thermal-shield, corrosion resistant coatings, ionic conductors, and oxygen sensors, and for potential applications including transparent optical devices and electrochemical capacitor electrodes, fuel cells, catalysts, and advanced ceramics. In this work, zirconia particles were synthesized from ZrCl 4 precursor with hydrothermal treatment in a batch reactor. Hydrothermal treatment may allow obtaining nanoparticles and sintered materials with controlled chemical and structural characteristics. Hydrothermal treatment was carried out at temperatures of 150 – 200°C with precursor concentration of 0.1 – 0.5 M. Zirconia particles obtained from this treatment were analyzed by using SEM, PSD and XRD to characterize the morphology, particle size distribution, and crystallinity, respectively. Based on the analysis, the size of zirconia particles were around 200 nm and it became smaller with decreasing precursor concentration. The increasing temperature caused the particles formed having uniform size. Zirconia particles formed by hydrothermal treatment were monoclinic, tetragonal and cubic crystal

Supercritical water oxidation treatment of textile sludge.

Science.gov (United States)

Zhang, Jie; Wang, Shuzhong; Li, Yanhui; Lu, Jinling; Chen, Senlin; Luo, XingQi

2017-08-01

In this work, we studied the supercritical water oxidation (SCWO) of the textile sludge, the hydrothermal conversion of typical textile compounds and the corrosion properties of stainless steel 316. Moreover, the influence mechanisms of NaOH during these related processes were explored. The results show that decomposition efficiency for organic matter in liquid phase of the textile sludge was improved with the increment of reaction temperature or oxidation coefficient. However, the organic substance in solid phase can be oxidized completely in supercritical water. Serious coking occurred during the high pressure water at 250-450°C for the Reactive Orange 7, while at 300 and 350°C for the polyvinyl alcohol. The addition of NaOH not only accelerated the destruction of organic contaminants in the SCWO reactor, but effectively inhibited the dehydration conversion of textile compounds during the preheating process, which was favorable for the treatment system of textile sludge. The corrosion experiment results indicate that the stainless steel 316 could be competent for the body materials of the reactor and the heat exchangers. Furthermore, there was prominent enhancement of sodium hydroxide for the corrosion resistance of 316 in subcritical water. On the contrary the effect was almost none during SCWO.

Easy and fast preparation of TiO{sub 2} - based nanostructures using microwave assisted hydrothermal synthesis

Energy Technology Data Exchange (ETDEWEB)

Bregadiolli, Bruna Andressa, E-mail: brunabregadiolli@fc.unesp.br [Universidade Estadual Paulista Julio de Mesquita Filho (UNESP), Bauru, SP (Brazil); Fernandes, Silvia Leticia; Graeff, Carlos Frederico de Oliveira [Universidade Estadual Paulista de Mesquita Filho (UNESP), Araraquara, SP (Brazil)

2017-07-15

TiO{sub 2} derivatives with distinct morphologies have been successfully obtained by microwave assisted hydrothermal synthesis in acidic and alkaline medium using mild conditions. Titanium tetraisopropoxide (TTIP) was used as precursor in different environmental conditions under low temperatures, inferior to 150 °C, and short synthesis times, from 2 to 60 min. X ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and N{sub 2} adsorption at 77 K (BET) were used to characterize the microstructural properties of the oxides. In the acidic synthesis the reaction time and temperature are not accompanied by significant changes in the structure of the material. However, in the basic conditions, the concentration of Na{sup +} ions strongly influences the particle morphology and growth. The morphology of the nanoparticles shows irregular spheres in acidic conditions, while in alkaline medium, needle like structures are formed as well as aggregated nanotube-like structures synthesized in only 30 min. Besides the difference in the morphology and structure, in both systems, high surface area was obtained. (author)

Hydrothermal synthesis of magnetic reduced graphene oxide sheets

International Nuclear Information System (INIS)

Shen, Jianfeng; Shi, Min; Ma, Hongwei; Yan, Bo; Li, Na; Ye, Mingxin

2011-01-01

Graphical abstract: An environmental friendly and efficient route for preparation of magnetic reduced graphene oxide composite with a one-step hydrothermal method was demonstrated. The reducing process was accompanied by generation of magnetic nanoparticles. Highlights: → A one-step hydrothermal method for preparation of MN-CCG was demonstrated. → Glucose was used as the 'green' reducing agent. → The reducing process was accompanied by generation of magnetic nanoparticles. → The prepared MN-CCG is highly water suspendable and sensitive to magnetic field. -- Abstract: We demonstrated an environmental friendly and efficient route for preparation of magnetic reduced graphene oxide composite (MN-CCG). Glucose was used as the reducing agent in this one-step hydrothermal method. The reducing process was accompanied by generation of magnetic nanoparticles. The structure and composition of the nanocomposite was confirmed by Fourier transform infrared spectroscopy, Raman spectroscopy, X-ray diffraction, thermal gravimetric analysis, atomic force microscopy and transmission electron microscopy. It was found that the prepared MN-CCG is highly water suspendable and sensitive to magnetic field.

Solvation in supercritical water

International Nuclear Information System (INIS)

Cochran, H.D.; Cummings, P.T.; Karaborni, S.

1991-01-01

The aim of this work is to determine the solvation structure in supercritical water composed with that in ambient water and in simple supercritical solvents. Molecular dynamics studies have been undertaken of systems that model ionic sodium and chloride, atomic argon, and molecular methanol in supercritical aqueous solutions using the simple point charge model of Berendsen for water. Because of the strong interactions between water and ions, ionic solutes are strongly attractive in supercritical water, forming large clusters of water molecules around each ion. Methanol is found to be a weakly-attractive solute in supercritical water. The cluster of excess water molecules surrounding a dissolved ion or polar molecule in supercritical aqueous solutions is comparable to the solvent clusters surrounding attractive solutes in simple supercritical fluids. Likewise, the deficit of water molecules surrounding a dissolved argon atom in supercritical aqueous solutions is comparable to that surrounding repulsive solutes in simple supercritical fluids. The number of hydrogen bonds per water molecule in supercritical water was found to be about one third the number in ambient water. The number of hydrogen bonds per water molecule surrounding a central particle in supercritical water was only mildly affected by the identify of the central particle--atom, molecule, or ion. These results should be helpful in developing a qualitative understanding of important processes that occur in supercritical water. 29 refs., 6 figs

Hydrothermal synthesis of meso porous silica MCM-41 using commercial sodium silicate

Energy Technology Data Exchange (ETDEWEB)

Melendez O, H. I.; Mercado S, A.; Garcia C, L. A.; Castruita, G.; Perera M, Y A., E-mail: ivan_melendez380@hotmail.com [Centro de Investigacion en Quimica Aplicada, Bldv. Enrique Reyna Hermosillo No. 140, Saltillo 25294, Coahuila (Mexico)

2013-08-01

In this work, ordered meso porous silica MCM-41 was prepared by hydrothermal synthesis using industrial-grade sodium silicate (Na{sub 2}SiO{sub 3}) as silica source, hexadecyltrimethyl-ammonium bromide (CTAB) as template agent and ethyl acetate as ph regulator. The influence of CTAB/SiO{sub 2} molar ratio, reaction time, aging temperature, and co-surfactant type on the structural and morphological properties of the obtained silica was studied. The products were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy and nitrogen adsorption-desorption isotherms. Ordered meso porous MCM-41 silica was obtained at 80 C by using a range of CTAB/SiO{sub 2} molar ratio from 0.35 to 0.71 and reaction times up to 72 h and isopropanol (i-Pr OH) as co-surfactant. (Author)

An effective hydrothermal route for the synthesis of multiple PDDA-protected noble-metal nanostructures.

Science.gov (United States)

Chen, Hongjun; Wang, Yuling; Dong, Shaojun

2007-12-10

In this article, we demonstrate an effective hydrothermal route for the synthesis of multiple PDDA-protected (PDDA = poly(diallyl dimethylammonium) chloride) noble-metal (including silver, platinum, palladium, and gold) nanostructures in the absence of any seeds and surfactants, in which PDDA, an ordinary and water-soluble polyelectrolyte, acts as both a reducing and a stabilizing agent. Under optimal experimental conditions, Ag nanocubes, Pt and Pd nanopolyhedrons, and Au nanoplates can be obtained, which were characterized by transmission electron microscopy , scanning electron microscopy, energy-dispersive spectroscopy, and X-ray diffraction. More importantly, the nanostructures synthesized show potential applications in surface-enhanced Raman scattering and electrocatalysis, in which Ag nanocubes and Pt nanopolyhedrons were chosen as the examples, respectively.

Natural cotton as precursor for the refractory boron carbide—a hydrothermal synthesis and characterization

Science.gov (United States)

Saritha Devi, H. V.; Swapna, M. S.; Raj, Vimal; Ambadas, G.; Sankararaman, S.

2018-01-01

Boron carbide (B4C) is an excellent covalent carbide that finds applications in industries and nuclear power plants. The present synthesis methods of boron carbide are expensive and involve the use of toxic chemicals that adversely affect environment. In the present work, we report for the first time the use of the hydrothermal method for converting the cellulose from cotton as the carbon precursor for B4C. The carbon precursor is converted into functionalized porous carbonaceous material by hydrothermal treatment followed by sodium borohydride. It is further treated with boric acid to make it a B4C precursor. The precursor is characterized by UV-visible diffuse reflectance, Raman, Fourier transform infrared, photoluminescent and energy dispersive spectroscopy. The morphology and structure analysis is carried out using field emission scanning electron microscopy and x-ray diffraction techniques. The results of structural and optical characterization of the sample synthesized are compared with the commercial B4C. The thermal stability of the sample is studied by thermogravimetric analysis. The sample annealed at 700 °C is found to be B4C devoid of amorphous carbon with a yield of 44.7%. The analysis reveals the formation of boron carbide from the sample.

Hydrothermal Synthesis of VO2 Polymorphs: Advantages, Challenges and Prospects for the Application of Energy Efficient Smart Windows.

Science.gov (United States)

Li, Ming; Magdassi, Shlomo; Gao, Yanfeng; Long, Yi

2017-09-01

Vanadium dioxide (VO 2 ) is a widely studied inorganic phase change material, which has a reversible phase transition from semiconducting monoclinic to metallic rutile phase at a critical temperature of τ c ≈ 68 °C. The abrupt decrease of infrared transmittance in the metallic phase makes VO 2 a potential candidate for thermochromic energy efficient windows to cut down building energy consumption. However, there are three long-standing issues that hindered its application in energy efficient windows: high τ c , low luminous transmittance (T lum ), and undesirable solar modulation ability (ΔT sol ). Many approaches, including nano-thermochromism, porous films, biomimetic surface reconstruction, gridded structures, antireflective overcoatings, etc, have been proposed to tackle these issues. The first approach-nano-thermochromism-which is to integrate VO 2 nanoparticles in a transparent matrix, outperforms the rest; while the thermochromic performance is determined by particle size, stoichiometry, and crystallinity. A hydrothermal method is the most common method to fabricate high-quality VO 2 nanoparticles, and has its own advantages of large-scale synthesis and precise phase control of VO 2 . This Review focuses on hydrothermal synthesis, physical properties of VO 2 polymorphs, and their transformation to thermochromic VO 2 (M), and discusses the advantages, challenges, and prospects of VO 2 (M) in energy-efficient smart windows application. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Driving Forces Controlling Host-Guest Recognition in Supercritical Carbon Dioxide Solvent.

Science.gov (United States)

Ingrosso, Francesca; Altarsha, Muhannad; Dumarçay, Florence; Kevern, Gwendal; Barth, Danielle; Marsura, Alain; Ruiz-López, Manuel F

2016-02-24

The formation of supramolecular host-guest complexes is a very useful and widely employed tool in chemistry. However, supramolecular chemistry in non-conventional solvents such as supercritical carbon dioxide (scCO2 ), one of the most promising sustainable solvents, is still in its infancy. In this work, we explored a successful route to the development of green processes in supercritical CO2 by combining a theoretical approach with experiments. We were able to synthesize and characterize an inclusion complex between a polar aromatic molecule (benzoic acid) and peracetylated-β-cyclodextrin, which is soluble in the supercritical medium. This finding opens the way to wide, environmental friendly, applications of scCO2 in many areas of chemistry, including supramolecular synthesis, reactivity and catalysis, micro and nano-particle formation, molecular recognition, as well as enhanced extraction processes with increased selectivity. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Supercritical CO{sub 2} mediated synthesis and catalytic activity of graphene/Pd nanocomposites

Energy Technology Data Exchange (ETDEWEB)

Tang, Lulu [School of Chemical Engineering, Yeungnam University, Gyeongsan, Gyeoungbuk 712-749 (Korea, Republic of); Nguyen, Van Hoa [School of Chemical Engineering, Yeungnam University, Gyeongsan, Gyeoungbuk 712-749 (Korea, Republic of); Department of Chemistry, Nha Trang University, 2 Nguyen Dinh Chieu, Nha Trang (Viet Nam); Shim, Jae-Jin, E-mail: jjshim@yu.ac.kr [School of Chemical Engineering, Yeungnam University, Gyeongsan, Gyeoungbuk 712-749 (Korea, Republic of)

2015-11-15

Highlights: • RGO/Pd composite was efficiently prepared via a facile method in supercritical CO{sub 2}. • Graphene sheets were coated uniformly with Pd nanoparticles with a size of ∼8 nm. • Composites exhibited excellent catalytic activity in the Suzuki reaction even after 10 cycles. - Abstract: Graphene sheets were decorated with palladium nanoparticles using a facile and efficient method in supercritical CO{sub 2}. The nanoparticles were formed on the graphene sheets by the simple hydrogen reduction of palladium(II) hexafluoroacetylacetonate precursor in supercritical CO{sub 2}. The product was characterized by X-ray diffraction, Fourier transform infrared spectroscopy, scanning electron microscopy, transmission electron microscopy, and X-ray photoelectron spectroscopy. Highly dispersed nanoparticles with various sizes and shapes adhered well to the graphene sheets. The composites showed high catalytic activities for the Suzuki reaction under aqueous and aerobic conditions within 5 min. The effects of the different Pd precursor loadings on the catalytic activities of the composites were also examined.

Selective Synthesis of Manganese/Silicon Complexes in Supercritical Water

Directory of Open Access Journals (Sweden)

Jiancheng Wang

2014-01-01

Full Text Available A series of manganese salts (Mn(NO32, MnCl2, MnSO4, and Mn(Ac2 and silicon materials (silica sand, silica sol, and tetraethyl orthosilicate were used to synthesize Mn/Si complexes in supercritical water using a tube reactor. X-ray diffraction (XRD, X-ray photoelectron spectrometer (XPS, transmission electron microscopy (TEM, and scanning electron microscopy (SEM were employed to characterize the structure and morphology of the solid products. It was found that MnO2, Mn2O3, and Mn2SiO4 could be obtained in supercritical water at 673 K in 5 minutes. The roles of both anions of manganese salts and silicon species in the formation of manganese silicon complexes were discussed. The inorganic manganese salt with the oxyacid radical could be easily decomposed to produce MnO2/SiO2 and Mn2O3/SiO2. It is interesting to found that Mn(Ac2 can react with various types of silicon to produce Mn2SiO4. The hydroxyl groups of the SiO2 surface from different silicon sources enhance the reactivity of SiO2.

Ideas and perspectives: hydrothermally driven redistribution and sequestration of early Archaean biomass – the “hydrothermal pump hypothesis”

Directory of Open Access Journals (Sweden)

J.-P. Duda

2018-03-01

Full Text Available Archaean hydrothermal chert veins commonly contain abundant organic carbon of uncertain origin (abiotic vs. biotic. In this study, we analysed kerogen contained in a hydrothermal chert vein from the ca. 3.5 Ga Dresser Formation (Pilbara Craton, Western Australia. Catalytic hydropyrolysis (HyPy of this kerogen yielded n-alkanes up to n-C22, with a sharp decrease in abundance beyond n-C18. This distribution ( ≤  n-C18 is very similar to that observed in HyPy products of recent bacterial biomass, which was used as reference material, whereas it differs markedly from the unimodal distribution of abiotic compounds experimentally formed via Fischer–Tropsch-type synthesis. We therefore propose that the organic matter in the Archaean chert veins has a primarily microbial origin. The microbially derived organic matter accumulated in anoxic aquatic (surface and/or subsurface environments and was then assimilated, redistributed and sequestered by the hydrothermal fluids (hydrothermal pump hypothesis.

Hydrothermal synthesis, structure and characterization of new ...

Indian Academy of Sciences (India)

Unknown

Keywords. Hydrothermal; crystal structure; solid electrolyte; iron (III) pyrophosphate. 1. Introduction ... tion, structure and electrical conductivity and the higher values of ..... type cavity structure. Acknowledgements. The authors would like to express their thanks to DST,. New Delhi, for financial assistance under the projects.

Hydrothermal synthesis of size-controllable Yttrium Orthovanadate (YVO{sub 4}) nanoparticles and its application in photocatalytic degradation of direct blue dye

Energy Technology Data Exchange (ETDEWEB)

Mohamed, R.M., E-mail: redama123@yahoo.com [Chemistry Department, Faculty of Science, King Abdulaziz University, P.O. Box 80203, Jeddah 21589 (Saudi Arabia); Advanced Materials Department, Central Metallurgical R and D Institute, CMRDI, P.O. Box 87, Helwan, Cairo 11421 (Egypt); Harraz, F.A. [Advanced Materials Department, Central Metallurgical R and D Institute, CMRDI, P.O. Box 87, Helwan, Cairo 11421 (Egypt); Mkhalid, I.A. [Chemistry Department, Faculty of Science, King Abdulaziz University, P.O. Box 80203, Jeddah 21589 (Saudi Arabia)

2012-08-15

Graphical abstract: XRD patterns of YVO{sub 4} nanopowders prepared at different hydrothermal times; where Y{sub 1} = 4 h, Y{sub 2} = 8 h, Y{sub 3} = 12 h and Y{sub 4} = 24 h. Highlights: Black-Right-Pointing-Pointer Size control of Yttrium Orthovanadate. Black-Right-Pointing-Pointer Hydrothermal synthesis. Black-Right-Pointing-Pointer Removal of direct blue dye. - Abstract: Sized-controlled YVO{sub 4} nanoparticles have been synthesized by a simple hydrothermal method by changing hydrothermal time from 4 to 24 h. The products were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), specific surface area (Brunauer-Emmett-Teller (BET)), and ultraviolet-visible spectroscopy (UV-vis) measurements. The results showed that the size of as-synthesized YVO{sub 4} nanoparticles was in the range of 11-40 nm and was extremely dependent on the hydrothermal time. Photocatalytic measurement showed that the YVO{sub 4} nanoparticles with particle size of about 11 nm (prepared by 4 h hydrothermal time) possess superior photocatalytic properties in the decolorization of direct blue dye. Due to simple preparation, high photocatalytic oxidation of direct blue dye and low cost, the YVO{sub 4} photocatalyst is a potential candidate for pollutants removal and will find wide application in the coming future in photocatalytic oxidation processes. The overall kinetics of photodegradation of direct blue dye using YVO{sub 4} nanopowders photocatalyst was found to be of first order. The photocatalyst could be easily removed from the reaction mixture and its recyclability with no loss of activity was possible for six times. The catalytic performance was found to decrease by 5% after run number six.

Hydrothermal-synthesized NiO nanowall array for lithium ion batteries

International Nuclear Information System (INIS)

Yan, Xiaoyan; Tong, Xili; Wang, Jian; Gong, Changwei; Zhang, Mingang; Liang, Liping

2013-01-01

Graphical abstract: Freestanding NiO nanowall array is prepared via a hydrothermal synthesis method and shows noticeable Li battery performance with good cycle life and high capacity. Highlights: ► NiO nanowall array is prepared by a hydrothermal synthesis method. ► NiO nanowall array with high capacity as anode material for Li ion battery. ► Nanowall array structure is favorable for fast ion/electron transfer. -- Abstract: We report a self-supported NiO nanowall array prepared by a facile hydrothermal synthesis method. The microstructure and morphology of the sample are characterized by means of X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The hydrothermal-synthesized NiO nanowalls with thicknesses of ∼20 nm arrange vertically to the substrate forming a net-like nanowall array structure. As anode material for lithium ion batteries, the NiO nanowall array exhibits better electrochemical performances with higher coulombic efficiency and better cycling performance as compared to the dense NiO film. The NiO nanowall array shows an initial coulombic efficiency of 76%, as well as good cycling stability with a capacity of 567 mAh g −1 at 0.3 A g −1 after 50 cycles, higher than those of the dense polycrystalline NiO film (361 mAh g −1 ). The superior electrochemical performance is mainly due to the unique nanowall array structure with shorter diffusion length for mass and charge transport

Is high-pressure water the cradle of life?

International Nuclear Information System (INIS)

Bassez, Marie-Paule

2003-01-01

Several theories have been proposed for the synthesis of prebiotic molecules. This letter shows that the structure of supercritical water, or high-pressure water, could trigger prebiotic synthesis and the origin of life deep in the oceans, in hydrothermal vent systems. Dimer geometries of high-pressure water may have a point of symmetry and a zero dipole moment. Consequently, simple apolar molecules found in submarine hydrothermal vent systems will dissolve in the apolar environment provided by the apolar form of the water dimer. Apolar water could be the medium which helps precursor molecules to concentrate and react more efficiently. The formation of prebiotic molecules could thus be linked to the structure of the water inside chimney nanochannels and cavities where hydrothermal piezochemistry and shock wave chemistry could occur. (letter to the editor)

Hydrothermal liquefaction of Spirulina and Nannochloropsis Salina under subcritical and supercritical water conditions

DEFF Research Database (Denmark)

Toor, Saqib; Reddy, H.; Deng, S.

2013-01-01

residue, and recycling process water for algae cultivation. GC-MS, elemental analyzer, FT-IR, calorimeter and nutrient analysis were used to analyze bio-crude, lipid-extracted algae and water samples produced in the hydrothermal liquefaction process. The highest bio-crude yield of 46% was obtained...

Synthesis of ZrO{sub 2} nanoparticles by hydrothermal treatment

Energy Technology Data Exchange (ETDEWEB)

Machmudah, Siti, E-mail: machmudah@chem-eng.its.ac.id; Widiyastuti, W., E-mail: machmudah@chem-eng.its.ac.id; Prastuti, Okky Putri, E-mail: machmudah@chem-eng.its.ac.id; Nurtono, Tantular, E-mail: machmudah@chem-eng.its.ac.id; Winardi, Sugeng, E-mail: machmudah@chem-eng.its.ac.id [Chemical Engineering Department, Sepuluh Nopember Institute of Technology, Surabaya 60111 (Indonesia); Wahyudiono,; Kanda, Hideki; Goto, Motonobu [Department of Chemical Engineering, Nagoya University, Nagoya 464-8603 (Japan)

2014-02-24

Zirconium oxide (zirconia, ZrO{sub 2}) is the most common material used for electrolyte of solid oxide fuel cells (SOFCs). Zirconia has attracted attention for applications in optical coatings, buffer layers for growing superconductors, thermal-shield, corrosion resistant coatings, ionic conductors, and oxygen sensors, and for potential applications including transparent optical devices and electrochemical capacitor electrodes, fuel cells, catalysts, and advanced ceramics. In this work, zirconia particles were synthesized from ZrCl{sub 4} precursor with hydrothermal treatment in a batch reactor. Hydrothermal treatment may allow obtaining nanoparticles and sintered materials with controlled chemical and structural characteristics. Hydrothermal treatment was carried out at temperatures of 150 – 200°C with precursor concentration of 0.1 – 0.5 M. Zirconia particles obtained from this treatment were analyzed by using SEM, PSD and XRD to characterize the morphology, particle size distribution, and crystallinity, respectively. Based on the analysis, the size of zirconia particles were around 200 nm and it became smaller with decreasing precursor concentration. The increasing temperature caused the particles formed having uniform size. Zirconia particles formed by hydrothermal treatment were monoclinic, tetragonal and cubic crystal.

Hydrothermal synthesis of high surface area ZIF-8 with minimal use of TEA

Science.gov (United States)

Butova, V. V.; Budnyk, A. P.; Bulanova, E. A.; Lamberti, C.; Soldatov, A. V.

2017-07-01

In this paper we present, for the first time, a simple hydrothermal recipe for the synthesis of ZIF-8 Metal-Organic Framework (MOF) with a large specific surface area (1340 m2/g by BET). An important feature of the method is that the product forms in aqueous medium under standard hydrothermal conditions without DMF and great excess of linker with the use of TEA as structure directing agent. The ZIF-8 crystal phase of the product was confirmed by XRD; this technique has been also exploited to check the crystallinity and to follow the changes in the MOF structure induced by heating. TGA and temperature dependent XRD testify the high thermal stability of the material (470 °C in N2 and at 400 °C in air). The IR spectral profile of the material provides a complete picture of vibrations assigned to the linker and the metal center. The systematic investigation of the products obtained by increasing the TEA amount in the reacting medium from 0 to 25.5 mol equivalent Zn2+, allowed us to understand its role and to find 2.6 mol equivalent Zn2+ as the minimum amount needed to obtain a single phase ZIF-8 material with the high standard reported above. The stability of the material under severe basic conditions makes it a promising candidate in heterogeneous catalysis. The material has shown high capacity in I2 uptake, making it interesting also for selective molecular adsorption.

Abiotic condensation synthesis of glyceride lipids and wax esters under simulated hydrothermal conditions.

Science.gov (United States)

Rushdi, Ahmed I; Simoneit, Bernd R T

2006-04-01

Precursor compounds for abiotic proto cellular membranes are necessary for the origin of life. Amphipathic compounds such as fatty acids and acyl glycerols are important candidates for micelle/bilayer/vesicle formation. Two sets of experiments were conducted to study dehydration reactions of model lipid precursors in aqueous media to form acyl polyols and wax esters, and to evaluate the stability and reactions of the products at elevated temperatures. In the first set, mixtures of n-nonadecanoic acid and ethylene glycol in water, with and without oxalic acid, were heated at discrete temperatures from 150 ( composite function)C to 300 ( composite function)C for 72 h. The products were typically alkyl alkanoates, ethylene glycolyl alkanoates, ethylene glycolyl bis-alkanoates and alkanols. The condensation products had maximum yields between 150 ( composite function)C and 250 ( composite function)C, and were detectable and thus stable under hydrothermal conditions to temperatures acid and glycerol were heated using the same experimental conditions, with and without oxalic acid, between 100 ( composite function)C and 250 ( composite function)C. The main condensation products were two isomers each of monoacylglycerols and diacylglycerols at all temperatures, as well as minor amounts of the fatty acid anhydride and methyl ester. The yield of glyceryl monoheptanoates generally increased with increasing temperature and glyceryl diheptanoates decreased noticeably with increasing temperature. The results indicate that condensation reactions and abiotic synthesis of organic lipid compounds under hydrothermal conditions occur easily, provided precursor concentrations are sufficiently high.

Supercritical Production of Nanoparticles - Part I: The SSEC Process - Part II: Characterization of Nanopartic

DEFF Research Database (Denmark)

Jensen, Henrik

with the crystallite size. Therefore special interest is being devoted to investigating these changes by developing new synthesis and characterizing methods. Wet chemical and gas phase syntheses are among the number of synthesis techniques that have been developed for nanoparticle formation. The sol-gel technique...... is the most broadly applied wet chemical process and it can be used for the production of nanosized materials in the formof particles or coatings for a wide range of materials. However, conventional sol-gel techniques have a number of drawbacks. The process maintains long reaction times and requires post....... The work presented in this thesis addresses the problems related to the conventional sol-gel techniques by using supercritical CO2 as the reaction media. Supercritical fluids exhibit gas like mass transfer properties and liquid like densities which are both particularly attractive to the sol-gel process...

Hydrothermal synthesis of hexagonal magnesium hydroxide nanoflakes

International Nuclear Information System (INIS)

Wang, Qiang; Li, Chunhong; Guo, Ming; Sun, Lingna; Hu, Changwen

2014-01-01

Graphical abstract: Hexagonal Mg(OH) 2 nanoflakes were synthesized via hydrothermal method in the presence of PEG-20,000. Results show that PEG-20,000 plays an important role in the formation of this kind of nanostructure. The SAED patterns taken from the different positions on a single hexagonal Mg(OH) 2 nanoflake yielded different crystalline structures. The structure of the nanoflakes are polycrystalline and the probable formation mechanism of Mg(OH) 2 nanoflakes is discussed. - Highlights: • Hexagonal Mg(OH) 2 nanoflakes were synthesized via hydrothermal method. • PEG-20,000 plays an important role in the formation of hexagonal nanostructure. • Mg(OH) 2 nanoflakes show different crystalline structures at different positions. • The probable formation mechanism of hexagonal Mg(OH) 2 nanoflakes was reported. - Abstract: Hexagonal magnesium hydroxide (Mg(OH) 2 ) nanoflakes were successfully synthesized via hydrothermal method in the presence of the surfactant polyethylene glycol 20,000 (PEG-20,000). Results show that PEG-20,000 plays an important role in the formation of this kind of nanostructure. The composition, morphologies and structure of the Mg(OH) 2 nanoflakes were characterized by X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), high-resolution transmission electron microscopy (HRTEM), and selected area electron diffraction (SAED). The SAED patterns taken from the different positions on a single hexagonal Mg(OH) 2 nanoflake show different crystalline structures. The structure of the nanoflakes are polycrystalline and the probable formation mechanism of Mg(OH) 2 nanoflakes is discussed. Brunauer–Emmett–Teller (BET) analysis were performed to investigate the porous structure and surface area of the as-obtained nanoflakes

Hydrothermal assisted synthesis of iron oxide-based magnetic silica spheres and their performance in magnetophoretic water purification

Energy Technology Data Exchange (ETDEWEB)

Caparros, C., E-mail: ccaparros@fisica.uminho.pt [Centro de Fisica, Universidade do Minho, Campus de Gualtar, 4710-057 Braga (Portugal); Benelmekki, M.; Martins, P.M. [Centro de Fisica, Universidade do Minho, Campus de Gualtar, 4710-057 Braga (Portugal); Xuriguera, E. [Facultat de Quimica, Universitat de Barcelona, 08028 Barcelona (Spain); Silva, C.J.R. [Departamento de Quimica, Universidade do Minho, Campus de Gualtar, 4710-057 Braga (Portugal); Martinez, Ll.M. [Sepmag Technologies, Parc Tecnologic del Valles, 08290 Barcelona (Spain); Lanceros-Mendez, S. [Centro de Fisica, Universidade do Minho, Campus de Gualtar, 4710-057 Braga (Portugal)

2012-08-15

Porous Magnetic Silica (PMS) spheres of about 400 nm diameter were synthesised by one-pot process using the classical Stber method combined with hydrothermal treatment. Maghemite nanoparticles ({gamma}-Fe{sub 2}O{sub 3}) were used as fillers and cetyltrimethylammonium bromide (CTAB) was used as templating agent. The application of the hydrothermal process (120 Degree-Sign C during 48 h) before the calcination leads to the formation of homogeneous and narrow size distribution PMS spheres. X-ray diffraction patterns (XRD), Infrared measurements (FTIR) and Transmission Electron microscopy (TEM) methods were used to determine the composition and morphology of the obtained PMS spheres. The results show a homogeneous distribution of the {gamma}-Fe{sub 2}O{sub 3} nanoparticles in the silica matrix with a 'hollow-like' morphology. Magnetophoresis measurements at 60 T m{sup -1} show a total separation time of the PMS spheres suspension of about 16 min. By using this synthesis method, the limitation of the formation of silica spheres without incorporation of magnetic nanoparticles is overcome. These achievements make this procedure interesting for industrial up scaling. The obtained PMS spheres were evaluated as adsorbents for Ni{sup 2+} in aqueous solution. Their adsorption capacity was compared with the adsorption capacity of magnetic silica spheres obtained without hydrothermal treatment before calcination process. PMS spheres show an increase of the adsorption capacity of about 15% of the initial dissolution of Ni{sup 2+} without the need to functionalize the silica surface. Highlights: Black-Right-Pointing-Pointer Homogeneous and controlled size porous magnetic silica spheres were obtained. Black-Right-Pointing-Pointer Magnetophoretic removing of Ni{sup 2+} processes was successfully preformed at HLGMF. Black-Right-Pointing-Pointer PMS show higher Ni{sup 2+} removing capacity than spheres without hydrothermal treatment. Black-Right-Pointing-Pointer PMS can be

Hydrothermal synthesis of mesoporous metal oxide arrays with enhanced properties for electrochemical energy storage

International Nuclear Information System (INIS)

Xiao, Anguo; Zhou, Shibiao; Zuo, Chenggang; Zhuan, Yongbing; Ding, Xiang

2015-01-01

Highlights: • NiO mesoporous nanowall arrays are prepared via hydrothermal method. • Mesoporous nanowall arrays are favorable for fast ion/electron transfer. • NiO mesoporous nanowall arrays show good supercapacitor performance. - Abstract: Mesoporous nanowall NiO arrays are prepared by a facile hydrothermal synthesis method with a following annealing process. The NiO nanowall shows continuous mesopores ranging from 5 to 10 nm and grows vertically on the substrate forming a porous net-like structure with macropores of 20–300 nm. A plausible mechanism is proposed for the growth of mesoporous nanowall NiO arrays. As cathode material of pseudocapacitors, the as-prepared mesoporous nanowall NiO arrays show good pseudocapacitive performances with a high capacitance of 600 F g −1 at 2 A g −1 and impressive high-rate capability with a specific capacitance of 338 F g −1 at 40 A g −1 . In addition, the mesoporous nanowall NiO arrays possess good cycling stability. After 6000 cycles at 2 A g −1 , a high capacitance of 660 F g −1 is attained, and no obvious degradation is observed. The good electrochemical performance is attributed to its highly porous morphology, which provides large reaction surface and short ion diffusion paths, leading to enhanced electrochemical properties

Synthesis and characterization of silica mesoporous material produced by hydrothermal continues pH adjusting path way

Directory of Open Access Journals (Sweden)

A. Salemi Golezani

2016-08-01

Full Text Available Mesoporous silica molecular sieves MCM-41 were synthesized under hydrothermal conditions. For this purpose, a solution with a molar coefficient of water, cetyltri-methyl ammonium bromide surfactants as template and sodium silicate as the source of SiO2 are used. Phase formation, morphology and gas absorption properties were investigated by XRD and BET analysis, respectively. The results showed that silica mesoporous material has been successfully synthesized. A favorable special surface and porosity volume together with regular arrangement of nano metric-hexagonal porosities were obtained from this synthesis. Thickness of the wall and average diameter of the pores are 0.8 nm and 4 nm, respectively.

High-throughput continuous hydrothermal synthesis of an entire nanoceramic phase diagram.

Science.gov (United States)

Weng, Xiaole; Cockcroft, Jeremy K; Hyett, Geoffrey; Vickers, Martin; Boldrin, Paul; Tang, Chiu C; Thompson, Stephen P; Parker, Julia E; Knowles, Jonathan C; Rehman, Ihtesham; Parkin, Ivan; Evans, Julian R G; Darr, Jawwad A

2009-01-01

A novel High-Throughput Continuous Hydrothermal (HiTCH) flow synthesis reactor was used to make directly and rapidly a 66-sample nanoparticle library (entire phase diagram) of nanocrystalline Ce(x)Zr(y)Y(z)O(2-delta) in less than 12 h. High resolution PXRD data were obtained for the entire heat-treated library (at 1000 degrees C/1 h) in less than a day using the new robotic beamline I11, located at Diamond Light Source (DLS). This allowed Rietveld-quality powder X-ray diffraction (PXRD) data collection of the entire 66-sample library in <1 day. Consequently, the authors rapidly mapped out phase behavior and sintering behaviors for the entire library. Out of the entire 66-sample heat-treated library, the PXRD data suggests that 43 possess the fluorite structure, of which 30 (out of 36) are ternary compositions. The speed, quantity and quality of data obtained by our new approach, offers an exciting new development which will allow structure-property relationships to be accessed for nanoceramics in much shorter time periods.

The effects of synthesis parameters on the formation of PbI2 particles under DTAB-assisted hydrothermal process

International Nuclear Information System (INIS)

Zhu Gangqiang; Hojamberdiev, Mirabbos; Liu Peng; Peng Jianhong; Zhou Jianping; Bian Xiaobin; Huang Xijin

2011-01-01

Highlights: ► Submicron- and micron-sized PbI 2 particles were hydrothermally synthesized. ► Structural transformation form belt-like to rod- and microtube-like was observed. ► Phase-pure PbI 2 particles could be hydrothermally obtained at pH 2 particles. ► The optical band gap energy of PbI 2 was slightly affected by morphology. - Abstract: Submicron- and micron-sized lead iodide (PbI 2 ) particles with well-controlled morphologies were successfully fabricated via a low-temperature hydrothermal process assisted by dodecyltrimethylammonium bromide (DTAB) as cationic surfactant. The as-synthesized powders were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, and UV–vis spectroscopy. The effects of synthesis parameters (temperature, time, pH, and surfactant amount) were systematically investigated. The obtained results showed that the submicron structure was belt-like at 100–120 °C, transformed to rod-like by increasing temperature to 140 °C and it became a microtube-like at 160–200 °C. By changing the pH of the synthesizing solution, it was found that a pure PbI 2 phase could be obtained below 7. With the addition of increasing amount of surfactant, microparticles were converted to microrods → submicron belts → microtubes. The time-dependent experimental results revealed that the dissolution–recrystallization and dissolution–recrystallization–self-oriented-attachment were considered to be the possible mechanisms for the formation of the belt- and tube-like PbI 2 submicron- and micron-sized particles, respectively. The optical properties of the PbI 2 particles synthesized at 100–200 °C for 8 h under hydrothermal conditions were also studied.

Hydrothermal synthesis of nanocubes of sillenite type compounds for photovoltaic applications and solar energy conversion of carbon dioxide to fuels

Science.gov (United States)

Subramanian, Vaidyanathan; Murugesan, Sankaran

2014-04-29

The present invention relates to formation of nanocubes of sillenite type compounds, such as bismuth titanate, i.e., Bi.sub.12TiO.sub.20, nanocubes, via a hydrothermal synthesis process, with the resulting compound(s) having multifunctional properties such as being useful in solar energy conversion, environmental remediation, and/or energy storage, for example. In one embodiment, a hydrothermal method is disclosed that transforms nanoparticles of TiO.sub.2 to bismuth titanate, i.e., Bi.sub.12TiO.sub.20, nanocubes, optionally loaded with palladium nanoparticles. The method includes reacting titanium dioxide nanotubes with a bismuth salt in an acidic bath at a temperature sufficient and for a time sufficient to form bismuth titanate crystals, which are subsequently annealed to form bismuth titanate nanocubes. After annealing, the bismuth titanate nanocubes may be optionally loaded with nano-sized metal particles, e.g., nanosized palladium particles.

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

Science.gov (United States)

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

2013-08-01

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

A Review on the Effects of Supercritical Carbon Dioxide on Enzyme Activity

Czech Academy of Sciences Publication Activity Database

Wimmer, Zdeněk; Zarevúcka, Marie

2010-01-01

Roč. 11, č. 1 (2010), s. 233-253 E-ISSN 1422-0067 R&D Projects: GA MŠk 2B06024 Institutional research plan: CEZ:AV0Z50380511; CEZ:AV0Z40550506 Keywords : enzyme * supercritical carbon dioxide * synthesis Subject RIV: CC - Organic Chemistry Impact factor: 2.279, year: 2010

Flow analysis in a supercritical water oxidation reactor

International Nuclear Information System (INIS)

Oh, C.H.; Kochan, R.J.; Beller, J.M.

1996-01-01

Supercritical water oxidation (SCWO), also known as hydrothermal oxidation (HTO), involves the oxidation of hazardous waste at conditions of elevated temperature and pressure (e.g., 500 C--600 C and 234.4 bar) in the presence of approximately 90% of water and a 10% to 20% excess amount of oxidant over the stoichiometric requirement. Under these conditions, organic compounds are completely miscible with supercritical water, oxygen and nitrogen, and are rapidly oxidized to carbon dioxide and water. The essential part of the process is the reactor. Many reactor designs such as tubular, vertical vessel, and transpiring wall type have been proposed, patented, and tested at both bench and pilot scales. These designs and performances need to be scaled up to a waste throughput 10--100 times that currently being tested. Scaling of this magnitude will be done by creating a numerical thermal-hydraulic model of the smaller reactor for which test data is available, validating the model against the available data, and then using the validated model to investigate the larger reactor performance. This paper presents a flow analysis of the MODAR bench scale reactor (vertical vessel type). These results will help in the design of the reactor in an efficient manner because the flow mixing coupled with chemical kinetics eventually affects the process destruction efficiency

Synthesis of mesoporous cerium-zirconium mixed oxides by hydrothermal templating method

Institute of Scientific and Technical Information of China (English)

无

2008-01-01

Mesoporous cerium-zirconium mixed oxides were prepared by hydrothermal method using cetyl trimethyl ammonium bromide (CTAB) as template.The effects of amount of template,pH value of solution and hydrothermal temperature on mesostructure of samples were systematically investigated.The final products were characterized by XRD,TEM,FT-IR,and BET.The results indicate that all the cerium-zirconium mixed oxides present a meso-structure.At molar ratio of n(CTAB)/n((Ce)+(Zr))=0.15,pH value of 9,and hydrothermal temperature of 120 ℃,the samples obtained possess a specific surface area of 207.9 m2/g with pore diameter of 3.70 nm and pore volume of 0.19 cm3/g.

A comparison of product yields and inorganic content in process streams following thermal hydrolysis and hydrothermal processing of microalgae, manure and digestate.

Science.gov (United States)

Ekpo, U; Ross, A B; Camargo-Valero, M A; Williams, P T

2016-01-01

Thermal hydrolysis and hydrothermal processing show promise for converting biomass into higher energy density fuels. Both approaches facilitate the extraction of inorganics into the aqueous product. This study compares the behaviour of microalgae, digestate, swine and chicken manure by thermal hydrolysis and hydrothermal processing at increasing process severity. Thermal hydrolysis was performed at 170°C, hydrothermal carbonisation (HTC) was performed at 250°C, hydrothermal liquefaction (HTL) was performed at 350°C and supercritical water gasification (SCWG) was performed at 500°C. The level of nitrogen, phosphorus and potassium in the product streams was measured for each feedstock. Nitrogen is present in the aqueous phase as organic-N and NH3-N. The proportion of organic-N is higher at lower temperatures. Extraction of phosphorus is linked to the presence of inorganics such as Ca, Mg and Fe in the feedstock. Microalgae and chicken manure release phosphorus more easily than other feedstocks. Copyright © 2015. Published by Elsevier Ltd.

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

Synthesis and luminescence properties of (Zn,Cd)S:Ag nanocrystals by hydrothermal method

International Nuclear Information System (INIS)

Luo Xixian; Cao Wanghe; Zhou Lixin

2007-01-01

ZnS:Ag and (Zn,Cd)S:Ag nanoparticles with particle sizes of about 50 and 150 nm have been prepared by hydrothermal method. The effects of hydrothermal process on the physical and luminescence characteristics are investigated. The photoluminescence intensities of hydrothermal treatment ZnS:Ag samples are 10 times higher than that of non-treated samples after annealing at 800 deg. C

Caldera unrest driven by CO2-induced drying of the deep hydrothermal system.

Science.gov (United States)

Moretti, R; Troise, C; Sarno, F; De Natale, G

2018-05-29

Interpreting volcanic unrest is a highly challenging and non-unique problem at calderas, since large hydrothermal systems may either hide or amplify the dynamics of buried magma(s). Here we use the exceptional ground displacement and geochemical datasets from the actively degassing Campi Flegrei caldera (Southern Italy) to show that ambiguities disappear when the thermal evolution of the deep hydrothermal system is accurately tracked. By using temperatures from the CO 2 -CH 4 exchange of 13 C and thermodynamic analysis of gas ascending in the crust, we demonstrate that after the last 1982-84 crisis the deep hydrothermal system evolved through supercritical conditions under the continuous isenthalpic inflow of hot CO 2 -rich gases released from the deep (~8 km) magma reservoir of regional size. This resulted in the drying of the base of the hot hydrothermal system, no more buffered along the liquid-vapour equilibrium, and excludes any shallow arrival of new magma, whose abundant steam degassing due to decompression would have restored liquid-vapour equilibrium. The consequent CO 2 -infiltration and progressive heating of the surrounding deforming rock volume cause the build-up of pore pressure in aquifers, and generate the striking temporal symmetry that characterizes the ongoing uplift and the post-1984 subsidence, both originated by the same but reversed deformation mechanism.

Synthesis of metal-doped Mn-Zn ferrite from the leaching solutions of vanadium slag using hydrothermal method

Science.gov (United States)

Liu, Shiyuan; Wang, Lijun; Chou, Kuochih

2018-03-01

Using vanadium slag as raw material, Metal-doped Mn-Zn ferrites were synthesized by multi-step processes including chlorination of iron and manganese by NH4Cl, selective oxidation of Fe cation, and hydrothermal synthesis. The phase composition and magnetic properties of synthesized metal-doped Mn-Zn ferrite were characterized by X-ray powder diffraction, Raman spectroscopy, transmission electron microscopy (TEM), X-ray photon spectra (XPS) and physical property measurement. It was found that Mn/Zn mole ratio significantly affected the magnetic properties and ZnCl2 content significantly influenced the purity of the phase of ferrite. Synthesized metal-doped Mn-Zn ferrite, exhibiting a larger saturation magnetization (Ms = 60.01 emu/g) and lower coercivity (Hc = 8.9 Oe), was obtained when the hydrothermal temperature was controlled at 200 °C for 12 h with a Mn/Zn mole ratio of 4. The effect of ZnCl2 content, Mn/Zn mole ratio and temperature on magnetic properties of the synthesized metal-doped Mn-Zn ferrite were systemically investigated. This process provided a new insight to utilize resources in the aim of obtaining functional materials.

Hydrothermal synthesis and white light emission of cubic ZrO2:Eu3+ nanocrystals

International Nuclear Information System (INIS)

Meetei, Sanoujam Dhiren; Singh, Shougaijam Dorendrajit

2014-01-01

Highlights: • White light emitting cubic ZrO 2 :Eu 3+ nanocrystal is synthesized by hydrothermal technique. • Eu 3+ is used to stabilize crystalline phase and to get red counterpart of the white light. • Defect emission and Eu 3+ emission combined to give white light. • The white light emitted from this nanocrystal resembles vertical daylight of the Sun. • Lifetime corresponding to red counterpart of the sample is far longer than conventional white light emitters. -- Abstract: Production of white light has been a promising area of luminescence studies. In this work, white light emitting nanocrystals of cubic zirconia doped with Eu 3+ are synthesized by hydrothermal technique. The dopant Eu 3+ is used to stabilize crystalline phase to cubic and at the same time to get red counterpart of the white light. The synthesis procedure is simple and precursor required no further annealing for crystallization. X-ray diffraction patterns show the crystalline phase of ZrO 2 :Eu 3+ to be cubic and it is confirmed by Fourier Transform Infrared spectroscopy. From transmission electron microscopy images, size of the crystals is found to be ∼5 nm. Photoluminescence emission spectrum of the sample, on monitoring excitation at O 2− –Eu 3+ charge transfer state shows broad peak due to O 2− of the zirconia and that of Eu 3+ emission. Commission Internationale de l’éclairage co-ordinate of this nanocrystal (0.32, 0.34) is closed to that of the ideal white light (0.33, 0.33). Correlated color temperature of the white light (5894 K) is within the range of vertical daylight. Lifetime (1.32 ms) corresponding to 5 D 0 energy level of the Eu 3+ is found to be far longer than conventional red counterparts of white light emitters. It suggests that the ZrO 2 :Eu 3+ nanocrystals synthesized by hydrothermal technique may find applications in simulating the vertical daylight of the Sun

One-step hydrothermal synthesis and electrochemical performance of sodium-manganese-iron phosphate as cathode material for Li-ion batteries

Science.gov (United States)

Karegeya, Claude; Mahmoud, Abdelfattah; Vertruyen, Bénédicte; Hatert, Frédéric; Hermann, Raphaël P.; Cloots, Rudi; Boschini, Frédéric

2017-09-01

The sodium-manganese-iron phosphate Na2Mn1.5Fe1.5(PO4)3 (NMFP) with alluaudite structure was obtained by a one-step hydrothermal synthesis route. The physical properties and structure of this material were obtained through XRD and Mössbauer analyses. X-ray diffraction Rietveld refinements confirm a cationic distribution of Na+ and presence of vacancies in A(2)', Na+ and small amounts of Mn2+ in A(1), Mn2+ in M(1), 0.5 Mn2+ and Fe cations (Mn2+,Fe2+ and Fe3+) in M(2), leading to the structural formula Na2Mn(Mn0.5Fe1.5)(PO4)3. The particles morphology was investigated by SEM. Several reactions with different hydrothermal reaction times were attempted to design a suitable synthesis protocol of NMFP compound. The time of reaction was varied from 6 to 48 h at 220 °C. The pure phase of NMFP particles was firstly obtained when the hydrothermal reaction of NMFP precursors mixture was maintained at 220 °C for 6 h. When the reaction time was increased from 6 to 12, 24 and 48 h, the dandelion structure was destroyed in favor of NMFP micro-rods. The combination of NMFP (NMFP-6H, NMFP-12H, NMFP-24H and NMFP-48H) structure refinement and Mössbauer characterizations shows that the increase of the reaction time leads to the progressive increment of Fe(III) and the decrease of the crystal size. The electrochemical tests indicated that NMFP is a 3 V sodium intercalating cathode. The comparison of the discharge capacity evolution of studied NMFP electrode materials at C/5 current density shows different capacities of 48, 40, 34 and 34 mA h g-1 for NMFP-6H, NMFP-12H, NMFP-24H and NMFP-48H respectively. Interestingly, all samples show excellent capacity retention of about 99% during 50 cycles.

Hydrothermal synthesis for fabrication and reprocessing of MOX nuclear fuel

International Nuclear Information System (INIS)

Ohta, Suguru; Yamamura, Tomoo; Shirasaki, Kenji; Satoh, Isamu; Shikama, Tatsuo

2011-01-01

To improve the nuclear proliferation resistance and to minimize use of chemicals, a new reprocessing and fabrication process of 'mixed oxide' (MOX) fuel was proposed and studied by using simulated spent fuel solutions. The process is consisting of the two steps, i.e. the removal of fission product (FP) from dissolved spent fuel by using carbonate solutions (Step-1), and hydrothermal synthesis of uranium dioxides (Step-2). In Step-1, rare earth (the precipitation ratio: 90%) and alkaline earth (10-50% for Sr) as FP were removed based on their low solubility of hydroxides and carbonate salts, with uranium kept dissolved for the certain carbonate solutions of weak base (Type 2) or mixtures of relatively strong base and weak base (Type 3). In Step-2, the features of uranium dioxides UO 2+x particles, i.e. stoichiometry (x=0.05-0.2), size (0.2-3 μm) and shape (cubic, spherical, rectangular parallelpiped, etc.), were controlled, and the cesium was removed down to 40 ppm by an addition of organic additives. The decontamination factors (DF) for cesium exceeds 10 5 , whereas the total DF of all the simulated FP were as low as the order of 10 which requires future studies for removal of alkaline earth, Re and Tc etc. (author)

Hydrothermal synthesis and crystal structure of CsFe23(HPO4)2(PO4)(H2O)

International Nuclear Information System (INIS)

Anisimova, N.Yu.; Ilyukhin, A.B.; Chudinova, N.N.; Serafin, M.

2001-01-01

The double acid iron-cesium orthophosphate CsFe 2 3 (HPO 4 ) 2 (PO 4 )(H 2 O) was prepared by hydrothermal synthesis (from the Fe 2 O 3 , Cs 2 CO 3 and H 3 PO 4 mixture at 290 Deg C during 1 h following by cooling to 25 Deg C). Its crystal structure (a = 5.021(3), b = 15.80(1), c = 13.646(8), β 94.49(4) Deg, sp. gr. P2 1 /n, Z = 4) was analyzed by X-ray diffraction. The structure is formed by the orthophosphate tetrahedrons and the FeO 6 octahedrons, the water molecule is coordinated by the iron atom [ru

Hydrothermal Synthesis and Electrochemical Properties of Spherical α-MnO2 for Supercapacitors.

Science.gov (United States)

Chen, Ya; Qin, Wenqing; Fan, Ruijuan; Wang, Jiawei; Chen, Baizhen

2015-12-01

In the present work, spherical α-MnO2 with a high specific capacitance was synthesized by a two-step hydrothermal route. MnCO3 precursors were first prepared by a common hydrothermal method, and then converted to α-MnO2 via a hydrothermal reaction between the precursors and KMnO4 solutions. The effects of hydrothermal temperature on the morphology, crystal structure and specific area of the MnO2 were investigated by scanning electron microscopy (SEM), X-ray diffraction (XRD) and BET measurements. The electrochemical capacitive properties of the manganese dioxides with different morphologies and structures were evaluated by cyclic voltammetry and galvonostatic charge-discharge tests. The results showed that the temperature in the second hydrothermal step had prominent impact on the capacitive properties of a-MnO2. The MnO2 synthesized at 150 *C exhibited a highest specific capacitance of 328.4 Fx g(-1) at a charge-discharge current density of 100 mA x g(-1).

Solid catalyzed isoparaffin alkylation at supercritical fluid and near-supercritical fluid conditions

Science.gov (United States)

Ginosar, Daniel M.; Fox, Robert V.; Kong, Peter C.

2000-01-01

This invention relates to an improved method for the alkylation reaction of isoparaffins with olefins over solid catalysts including contacting a mixture of an isoparaffin, an olefin and a phase-modifying material with a solid acid catalyst member under alkylation conversion conditions at either supercritical fluid, or near-supercritical fluid conditions, at a temperature and a pressure relative to the critical temperature(T.sub.c) and the critical pressure(P.sub.c) of the reaction mixture. The phase-modifying phase-modifying material is employed to promote the reaction's achievement of either a supercritical fluid state or a near-supercritical state while simultaneously allowing for decreased reaction temperature and longer catalyst life.

Application of supercritical fluid extraction in analytical science

International Nuclear Information System (INIS)

Kumar, Pradeep

2015-01-01

In the recent years, supercritical fluid extraction (SFE) has emerged as a promising alternative to conventional solvent extraction process owing to its potential to minimize the generation of the liquid volume and simplification of the extraction process.This technology is some times referred to as 'green technology' and 'clean technology'. Supercritical fluid extraction process assumes significance as it exhibits practical advantages such as enhanced extraction rate due to rapid mass transfer in supercritical fluid medium and change of solvent properties such as density by tuning pressure/temperature conditions. Supercritical fluids (SCF) offer faster, cleaner and efficient extraction owing to low viscosity, high density, low surface tension and better diffusivity properties. Higher diffusivity than liquids facilitates rapid mass transfer and faster completion of reaction. Due to low viscosity and surface tension, SCF can penetrate deep inside the material, extracting the component of interest. Liquid like solvating characteristics of SCFs enable dissolution of compounds whereas gas like diffusion characteristics provide conditions for high degree of extraction in shorter time duration. CO 2 has been widely employed as supercritical fluid owing to its moderate critical constants (Pc= 72.9 atm, Tc =304.3 K, ñ c = 0.47 g mL -1 ) and attractive properties such as being easily available, recyclable, non-toxic, chemically inert, non inflammable and radio-chemically stable. SCF finds application in variety of fields. In nuclear industry for separation and purification of actinides from liquids and solid matrices. In food industry, Decaffeination of coffee is done by SCF. Pharmaceutical industry, organic compounds can be extracted from plants by SC CO 2 avoiding liquid solvent usage. SCF may also be utilised for the production of fine powders. In polymer and plastics industries, examples of applications include the impregnation of medical material

Piezoelectric Materials Synthesized by the Hydrothermal Method and Their Applications

Directory of Open Access Journals (Sweden)

Takeshi Morita

2010-12-01

Full Text Available Synthesis by the hydrothermal method has various advantages, including low reaction temperature, three-dimensional substrate availability, and automatic polarization alignment during the process. In this review, powder synthesis, the fabrication of piezoelectric thin films, and their applications are introduced. A polycrystalline lead zirconate titanate (PZT thin film was applied to a micro ultrasonic motor, and an epitaxial lead titanate (PbTiO3 thin film was estimated as a ferroelectric data storage medium. Ferroelectric and piezoelectric properties were successfully obtained for epitaxial PbTiO3 films. As lead-free piezoelectric powders, KNbO3 and NaNbO3 powders were synthesized by the hydrothermal method and sintered together to form (K,NaNbO3 ceramics, from which reasonable piezoelectric performance was achieved.

Obtaining zeolite Y synthesized by hydrothermal treatment assisted by microwave

International Nuclear Information System (INIS)

Simoes, A.N.; Simoes, V.N.; Neiva, L.S.; Rodrigues, M.G.F.; Gama, L.; Oliveira, J. B.L.

2011-01-01

n search of new catalysts several man-made structures have been developed. The use of zeolites in catalysis is applied due to its ability to associate activity, selectivity and stability, the main conditions to have an effective catalyst. Thus, studies have been done on the hydrothermal synthesis of zeolites by microwave assisted, since the use of microwave radiation offers several advantages over conventional heating. In this context, this work aims to synthesis and characterization of zeolite Y via hydrothermal treatment in a microwave oven. The sample obtained was characterized by XRD, BET and SEM. XRD results showed the formation of zeolite Y in just 60 minutes. The sample showed high value of surface area, the latter being of 476.2 m² / g. The particles are agglomerated, but with a narrow distribution of size. (author)

Hydrothermal synthesis of a photovoltaic material based on CuIn0.5Ga0.5Se2

Science.gov (United States)

Castellanos Báez, Y. T.; Fuquen Peña, D. A.; Gómez-Cuaspud, J. A.; Vera-López, E.; Pineda-Triana, Y.

2017-12-01

The present work report, the synthesis and characterization of the CuIn0.5Ga0.5Se2 system (abbreviated CIGS), by the implementation of a hydrothermal route, in order to obtain a solid with appropriate properties in terms of surface, morphological and texture properties for potential applications in the design of photovoltaic cells. The synthesis was carried out using the corresponding stoichiometric quantities (Cu:In:Ga:Se 1:0.5:0.5:2), which were mixed in a Teflon vessel under stirring conditions. The homogeneous solution was treated in a steel autoclave at 300°C for 72 hours at the end of which the resulting material was characterized by X-Ray Diffraction (XRD) and Rietveld refinement. The results of the structural characterization allowed to confirm the obtaining of a chalcopyrite type structure, with a I-42 d (122) structure and cell parameters a=0.570, b=0.570, c=1.140nm, α=90, β=90, γ=90° oriented along (1 0 4) facet, detecting the presence of a secondary phases, related with CuInSe and CuIn metallic selenides, derived from synthesis process. The structural refinement allowing to validate the obtaining of a nanometric crystalline material (10-20nm) for potential applications in field of photovoltaic technology.

Direct Energy Supply to the Reaction Mixture during Microwave-Assisted Hydrothermal and Combustion Synthesis of Inorganic Materials

Directory of Open Access Journals (Sweden)

Roberto Rosa

2014-05-01

Full Text Available The use of microwaves to perform inorganic synthesis allows the direct transfer of electromagnetic energy inside the reaction mixture, independently of the temperature manifested therein. The conversion of microwave (MW radiation into heat is useful in overcoming the activation energy barriers associated with chemical transformations, but the use of microwaves can be further extended to higher temperatures, thus creating unusual high-energy environments. In devising synthetic methodologies to engineered nanomaterials, hydrothermal synthesis and solution combustion synthesis can be used as reference systems to illustrate effects related to microwave irradiation. In the first case, energy is transferred to the entire reaction volume, causing a homogeneous temperature rise within a closed vessel in a few minutes, hence assuring uniform crystal growth at the nanometer scale. In the second case, strong exothermic combustion syntheses can benefit from the application of microwaves to convey energy to the reaction not only during the ignition step, but also while it is occurring and even after its completion. In both approaches, however, the direct interaction of microwaves with the reaction mixture can lead to practically gradient-less heating profiles, on the basis of which the main observed characteristics and properties of the aforementioned reactions and products can be explained.

Hydrothermal synthesis of hydroxyapatite nanoparticles decorated with silver nanoparticles for application in biomaterials

International Nuclear Information System (INIS)

Assis, Jordanna Fernandes; Arantes, Tatiane Moraes; Cristovan, F.H.; Tada, Dayane Batista

2016-01-01

Full text: The hydroxyapatite nanoparticles (HA) have research attention because are material that exhibit biocompatibility with bone mineral phase of human body is great interest in the scientific community. Synthetic hydroxyapatite nanoparticles have excellent biocompatibility and bioactivity, due biocompatibility and osteo inducibility [1-3]. The hydroxyapatite nanoparticles were synthesized by hydrothermal processing and were characterized by X-ray diffraction (XRD), Raman spectroscopy and transmission electron microscopy (TEM). The XRD and Raman spectra showed crystalline hydroxyapatite colloidal nanoparticles were obtained in the hexagonal phase. XRD measure showed silver diffraction peaks cubic phase confirmed the presence of the silver nanoparticles decorated hydroxyapatite surface. TEM images showed HA nanoparticles presented a well defined nanorod shapes and narrow size distributions with dimensions (width and length) around of 5 nm and 50 nm decorated with silver nanoparticles of spherical shape about 20 nm in diameter The results showed that crystalline hydroxyapatite colloidal nanoparticles with rod-like morphology and uniform decorated with silver spherical nanoparticles size were obtained by hydrothermal synthesis. These nanoparticles The cell viability of the HA and HA/Ag was analyzed by reduction of the tetrazolium salt (MTT test). Embryonic mouse fibroblast cells were grown in the presence of nanoparticles for a total period of 96 hours. Analyses were made in 24h, 48h, 72h and 96h. The suspensions at the end of each period were analyzed in spectrophotometer. The 24h experiments were the most conclusive, with the silver presence in the HA, there is an increased in cellular proliferation. The results demonstrated that the HA/Ag nanoparticles have potential use as biomaterials in medical/odontological applications. (author)

Hydrothermal synthesis of hydroxyapatite nanoparticles decorated with silver nanoparticles for application in biomaterials

Energy Technology Data Exchange (ETDEWEB)

Assis, Jordanna Fernandes; Arantes, Tatiane Moraes, E-mail: fernandes.jordanna9@gmail.com [Universidade Federal de Goias (UFG), Goiania (Brazil); Cristovan, F.H.; Tada, Dayane Batista [Universidade Federal de Sao Paulo (UNIFESP), Sao Jose dos Campos, SP (Brazil)

2016-07-01

Full text: The hydroxyapatite nanoparticles (HA) have research attention because are material that exhibit biocompatibility with bone mineral phase of human body is great interest in the scientific community. Synthetic hydroxyapatite nanoparticles have excellent biocompatibility and bioactivity, due biocompatibility and osteo inducibility [1-3]. The hydroxyapatite nanoparticles were synthesized by hydrothermal processing and were characterized by X-ray diffraction (XRD), Raman spectroscopy and transmission electron microscopy (TEM). The XRD and Raman spectra showed crystalline hydroxyapatite colloidal nanoparticles were obtained in the hexagonal phase. XRD measure showed silver diffraction peaks cubic phase confirmed the presence of the silver nanoparticles decorated hydroxyapatite surface. TEM images showed HA nanoparticles presented a well defined nanorod shapes and narrow size distributions with dimensions (width and length) around of 5 nm and 50 nm decorated with silver nanoparticles of spherical shape about 20 nm in diameter The results showed that crystalline hydroxyapatite colloidal nanoparticles with rod-like morphology and uniform decorated with silver spherical nanoparticles size were obtained by hydrothermal synthesis. These nanoparticles The cell viability of the HA and HA/Ag was analyzed by reduction of the tetrazolium salt (MTT test). Embryonic mouse fibroblast cells were grown in the presence of nanoparticles for a total period of 96 hours. Analyses were made in 24h, 48h, 72h and 96h. The suspensions at the end of each period were analyzed in spectrophotometer. The 24h experiments were the most conclusive, with the silver presence in the HA, there is an increased in cellular proliferation. The results demonstrated that the HA/Ag nanoparticles have potential use as biomaterials in medical/odontological applications. (author)

Hydrothermal synthesis for new multifunctional materials: A few examples of phosphates and phosphonate-based hybrid materials

Energy Technology Data Exchange (ETDEWEB)

Rueff, Jean-Michel, E-mail: jean-michel.rueff@ensicaen.fr [Laboratoire CRISMAT, CNRS UMR 6508, ENSICAEN, 6 bd du Maréchal Juin, F-14050 Caen Cedex (France); Poienar, Maria [National Institute for Research and Development in Electrochemistry and Condensed Matter, Plautius Andronescu Str Nr. 1, 300224 Timisoara (Romania); Guesdon, Anne; Martin, Christine; Maignan, Antoine [Laboratoire CRISMAT, CNRS UMR 6508, ENSICAEN, 6 bd du Maréchal Juin, F-14050 Caen Cedex (France); Jaffrès, Paul-Alain [Université de Brest, Université Européenne de Bretagne, CNRS UMR 6521, CEMCA, SFR 148 ScInBios, 6 Avenue Victor Le Gorgeu, 29238 Brest (France)

2016-04-15

Novel physical or chemical properties are expected in a great variety of materials, in connection with the dimensionality of their structures and/or with their nanostructures, hierarchical superstructures etc. In the search of new advanced materials, the hydrothermal technique plays a crucial role, mimicking the nature able to produce fractal, hyperbranched, urchin-like or snow flake structures. In this short review including new results, this will be illustrated by examples selected in two types of materials, phosphates and phosphonates, prepared by this method. The importance of the synthesis parameters will be highlighted for a magnetic iron based phosphates and for hybrids containing phosphonates organic building units crystallizing in different structural types. - Graphical abstract: Phosphate dendrite like and phosphonate platelet crystals.

Facile hydrothermal synthesis of CeO 2 nanopebbles

Indian Academy of Sciences (India)

Cerium oxide (CeO2) nanopebbles have been synthesized using a facile hydrothermal method. X-ray diffraction pattern (XRD) and transmission electron microscopy analyses confirm the presence of CeO2 nanopebbles. XRD shows the formation of cubic fluorite CeO2 and the average particle size estimated from the ...

Extraction with supercritical gases

Energy Technology Data Exchange (ETDEWEB)

Schneider, G M; Wilke, G; Stahl, E

1980-01-01

The contents of this book derives from a symposium on the 5th and 6th of June 1978 in the ''Haus der Technik'' in Essen. Contributions were made to separation with supercritical gases, fluid extraction of hops, spices and tobacco, physicochemical principles of extraction, phase equilibria and critical curves of binary ammonia-hydrocarbon mixtures, a quick method for the microanalytical evaluation of the dissolving power of supercritical gases, chromatography with supercritical fluids, the separation of nonvolatile substances by means of compressed gases in countercurrent processes, large-scale industrial plant for extraction with supercritical gases, development and design of plant for high-pressure extraction of natural products.

Hydrothermal synthesis of 1D TiO2 nanostructures for dye sensitized solar cells

International Nuclear Information System (INIS)

Tacchini, I.; Ansón-Casaos, A.; Yu, Youhai; Martínez, M.T.; Lira-Cantu, M.

2012-01-01

Highlights: ► Hydrothermal synthesis allows the preparation of different 1D TiO 2 nanostructures easily. ► Nanotubular morphology demonstrates the highest photovoltaic efficiencies in dye sensitized cells (DSCs). ► Morphology at the nanoscale level is as decisive for DSC efficiency as it is TiO 2 crystal structure and surface area. - Abstract: Mono-dimensional titanium oxide nanostructures (multi-walled nanotubes and nanorods) were synthesized by the hydrothermal method and applied to the construction of dye sensitized solar cells (DSCs). First, nanotubes (TiNTs) and nanotubes loaded with titanium oxide nanoparticles (TiNT/NPs) were synthesized with specific surface areas of 253 m 2 /g and 304 m 2 /g, respectively. After that, thermal treatment of the nanotubes at 500 °C resulted in their transformation into the corresponding anatase nanorods (TiNT-Δ and TiNT/NPs-Δ samples). X-ray diffraction and Raman spectroscopy data indicated that titanium oxide in the pristine TiNT and TiNT/NP samples was converted into anatase phase TiO 2 during the heating. Additionally, specific surface areas and water adsorption capacities decreased after the heat treatment due to the sample agglomeration and the collapse of the inner nanotube channels. DSCs were fabricated with the nanotube TiNT and TiNT/NP samples and with the anatase nanorod TiNT-Δ and TiNT/NPs-Δ samples as well. The highest power conversion efficiency of η = 3.12% was obtained for the TiNT sample, despite its lower specific surface compared with the corresponding nanoparticle-loaded sample (TiNT/NP).

One-pot hydrothermal synthesis and characterization of CoFe2O4 nanoparticles and its application as magnetically recoverable catalyst in oxidation of alcohols by periodic acid

International Nuclear Information System (INIS)

Paul, Bappi; Purkayastha, Debraj Dhar; Dhar, Siddhartha Sankar

2016-01-01

A novel and facile approach for one-pot synthesis of spinel cobalt ferrite (CoFe 2 O 4 ) nanoparticles (NPs) is presented here. The synthesis involves homogeneous chemical precipitation followed by hydrothermal heating, using tributylamine (TBA) as a hydroxylating agent. Polyethylene glycol (PEG) 4000 was used as surfactant. As-synthesized CoFe 2 O 4 NPs were characterized by powder X-ray diffraction (XRD), transmission electron microscopy (TEM), N 2 adsorption-desorption isotherm (BET) and vibrating sample magnetometry (VSM). TEM image showed formation of spherical particles of sizes 2–30 nm. These NPs were used as magnetically recoverable catalyst in oxidation of alcohols to their corresponding aldehydes by periodic acid. This oxidative procedure is found to be highly efficient affording products in very high yield and selectivity. The easy magnetic separation of the catalyst and efficient reusability are key features of this methodology. - Highlights: • Hydrothermal synthesis of CoFe 2 O 4 NPs with (C 4 H 9 ) 3 N as hydroxylating agent. • The TEM images showed the particles to be spherical in shape with sizes 2–30 nm. • CoFe 2 O 4 was used as recyclable catalyst for oxidation of alcohols by periodic acid.

Enhanced performance of LiFePO4 through hydrothermal synthesis coupled with carbon coating and cupric ion doping

International Nuclear Information System (INIS)

Pei Bo; Wang Qiang; Zhang Weixin; Yang Zeheng; Chen Min

2011-01-01

Highlights: → Hydrothermal reaction has been adopted to synthesize LiFePO 4 with a narrow size distribution. → LiFePO 4 was modified with carbon coating and cupric cation (Cu 2+ ) doping simultaneously. → Electrochemical properties of LiFePO 4 were improved by carbon coating and cupric cation doping. - Abstract: A hydrothermal reaction has been adopted to synthesize pure LiFePO 4 first, which was then modified with carbon coating and cupric ion (Cu 2+ ) doping simultaneously through a post-heat treatment. X-ray diffraction patterns, transmission electron microscopy and scanning electron microscopy images along with energy dispersive spectroscopy mappings have verified the homogeneous existence of coated carbon and doped Cu 2+ in LiFePO 4 particles with phospho-olivine structure and an average size of 400 nm. The electrochemical performances of the material have been studied by cyclic voltammetry, electrochemical impedance spectroscopy and galvanostatic charge-discharge measurements. The carbon-coated and Cu 2+ -doped LiFePO 4 sample (LFCu5/C) exhibited an enhanced electronic conductivity of 2.05 x 10 -3 S cm -1 , a specific discharge capacity of 158 mAh g -1 at 50 mA g -1 , a capacity retention of 96.4% after 50 cycles, a decreased charge transfer resistance of 79.4 Ω and superior electrode reaction reversibility. The present synthesis route is promising in making the hydrothermal method more practical for preparation of the LiFePO 4 material and enhancement of electrochemical properties.

Large Marks-decahedral Pd nanoparticles synthesized by a modified hydrothermal method using a homogeneous reactor

International Nuclear Information System (INIS)

Zhao, Haiqiang; Qi, Weihong; Ji, Wenhai; Wang, Tianran; Peng, Hongcheng; Wang, Qi; Jia, Yanlin; He, Jieting

2017-01-01

Fivefold symmetry appears only in small particles and quasicrystals because internal stress in the particles increases with the particle size. However, a typical Marks decahedron with five re-entrant grooves located at the ends of the twin boundaries can further reduce the strain energy. During hydrothermal synthesis, it is difficult to stir the reaction solution contained in a digestion high-pressure tank because of the relatively small size and high-temperature and high-pressure sealed environment. In this work, we optimized a hydrothermal reaction system by replacing the conventional drying oven with a homogeneous reactor to shift the original static reaction solution into a full mixing state. Large Marks-decahedral Pd nanoparticles (~90 nm) have been successfully synthesized in the optimized hydrothermal synthesis system. Additionally, in the products, round Marks-decahedral Pd particles were also found for the first time. While it remains a challenge to understand the growth mechanism of the fivefold twinned structure, we proposed a plausible growth-mediated mechanism for Marks-decahedral Pd nanoparticles based on observations of the synthesis process.

Large Marks-decahedral Pd nanoparticles synthesized by a modified hydrothermal method using a homogeneous reactor

Energy Technology Data Exchange (ETDEWEB)

Zhao, Haiqiang; Qi, Weihong, E-mail: qiwh216@csu.edu.cn; Ji, Wenhai; Wang, Tianran; Peng, Hongcheng; Wang, Qi; Jia, Yanlin; He, Jieting [Central South University, School of Materials Science and Engineering (China)

2017-05-15

Fivefold symmetry appears only in small particles and quasicrystals because internal stress in the particles increases with the particle size. However, a typical Marks decahedron with five re-entrant grooves located at the ends of the twin boundaries can further reduce the strain energy. During hydrothermal synthesis, it is difficult to stir the reaction solution contained in a digestion high-pressure tank because of the relatively small size and high-temperature and high-pressure sealed environment. In this work, we optimized a hydrothermal reaction system by replacing the conventional drying oven with a homogeneous reactor to shift the original static reaction solution into a full mixing state. Large Marks-decahedral Pd nanoparticles (~90 nm) have been successfully synthesized in the optimized hydrothermal synthesis system. Additionally, in the products, round Marks-decahedral Pd particles were also found for the first time. While it remains a challenge to understand the growth mechanism of the fivefold twinned structure, we proposed a plausible growth-mediated mechanism for Marks-decahedral Pd nanoparticles based on observations of the synthesis process.

Hydrothermal Synthesis of Hydroxyapatite Nanorods for Rapid Formation of Bone-Like Mineralization

Science.gov (United States)

Hoai, Tran Thanh; Nga, Nguyen Kim; Giang, Luu Truong; Huy, Tran Quang; Tuan, Phan Nguyen Minh; Binh, Bui Thi Thanh

2017-08-01

Hydroxyapatite (HAp) is an excellent biomaterial for bone repair and regeneration. The biological functions of HAp particles, such as biomineralization, cell adhesion, and cell proliferation, can be enhanced when their size is reduced to the nanoscale. In this work, HAp nanoparticles were synthesized by the hydrothermal technique with addition of cetyltrimethylammonium bromide (CTAB). These particles were also characterized, and their size controlled by modifying the CTAB concentration and hydrothermal duration. The results show that most HAp nanoparticles were rod-like in shape, exhibiting the most uniform and smallest size (mean diameter and length of 39 nm and 125 nm, respectively) at optimal conditions of 0.64 g CTAB and hydrothermal duration of 12 h. Moreover, good biomineralization capability of the HAp nanorods was confirmed through in vitro tests in simulated body fluid. A bone-like mineral layer of synthesized HAp nanorods formed rapidly after 7 days. This study shows that highly bioactive HAp nanorods can be easily prepared by the hydrothermal method, being a potential nanomaterial for bone regeneration.

Processing of high level waste: Spectroscopic characterization of redox reactions in supercritical water. 1998 annual progress report

International Nuclear Information System (INIS)

Arrington, C.A. Jr.

1998-01-01

'The author is engaged in a collaborative research effort with Los Alamos staff scientists Steven Buelow, Jeanne Robinson, and Bernie Foy all staff members in group CST-6. The work proposed by these LANL staff scientists is directed towards the destruction of complexants and oxidation of chromium and technetium by hydrothermal processing in near critical or supercritical aqueous solutions. The work addresses two areas of investigation related to ongoing efforts at LANL: (1) kinetic studies of oxidation-reduction reactions in supercritical water; (2) measurement of physical properties of ionic solutes in supercritical water. All of the work during this first year was carried out at Los Alamos National Lab. During the Summer program at LANL all equipment and supplies were provided through Dr. Buelow''s program at LANL. The author has now set up a Raman spectroscopy lab at Furman. Using departmental funds he purchased an optical bench, a laser, and a CCD detector, and a grant from the Dreyfus Foundation assisted in the purchase of a Raman spectrometer. He is now able to carry out experiments using the Raman system at Furman. The plan is to continue the Summer collaboration at LANL and carry out experiments at Furman during the academic year.'

Size-controlled synthesis of NiFe2O4 nanospheres via a PEG assisted hydrothermal route and their catalytic properties in oxidation of alcohols by periodic acid

International Nuclear Information System (INIS)

Paul, Bappi; Purkayastha, Debraj Dhar; Dhar, Siddhartha Sankar

2016-01-01

Graphical abstract: - Highlights: • Hydrothermal synthesis of NiFe 2 O 4 NPs with (C 4 H 9 ) 3 N as hydroxylating agent. • PEG 4000 was used as surfactant to control sizes of NPs. • The TEM images revealed the material to be spherical in shape with sizes 2–10 nm. • NiFe 2 O 4 was used as recyclable catalyst for oxidation of alcohols by periodic acid. - Abstract: A novel and facile approach for synthesis of spinel nickel ferrites (NiFe 2 O 4 ) nanoparticles (NPs) employing homogeneous chemical precipitation followed by hydrothermal heating is reported. The synthesis involves use of tributylamine (TBA) as a hydroxylating agent in synthesis of nickel ferrites. Polyethylene glycol (PEG) 4000 was used as surfactant. As-synthesized NiFe 2 O 4 NPs were characterized by powder X-ray diffraction (XRD), transmission electron microscopy (TEM), N 2 adsorption–desorption isotherm (BET) and vibrating sample magnetometry (VSM). The XRD pattern revealed formation of cubic face-centered NiFe 2 O 4 and TEM image showed spherical particles of sizes 2–10 nm. These NiFe 2 O 4 NPs were used as magnetically recoverable catalyst in oxidation of cyclic alcohols to their corresponding aldehydes by periodic acid. This eco-friendly procedure affords products in very high yield and selectivity. The reusability of the catalyst is proved to be noteworthy as the material exhibits no significant changes in its catalytic activity even after five cycles of reuse.

Hydrothermal synthesis of h-MoO3 microrods and their gas sensing properties to ethanol

International Nuclear Information System (INIS)

Liu, Yueli; Yang, Shuang; Lu, Yu; Podval’naya, Natal’ya V.; Chen, Wen; Zakharova, Galina S.

2015-01-01

Highlights: • A simple hydrothermal acid-free method for the synthesis of h-MoO 3 microrods with the hexagonal cross-section is reported. • The h-MoO 3 phase is transformed to α-MoO 3 at 439 °C. • The h-MoO 3 microrods were employed to fabricate gas sensors to detect ethanol. • Sensor showed highest response with a sensitivity of 8.24–500 ppm C 2 H 5 OH at operating temperature of 332 °C. - Abstract: Hexagonal molybdenum trioxide (h-MoO 3 ) microrods were successfully synthesized via a novel and facile hydrothermal route from peroxomolybdate solution with the presence of NH 4 Cl as the mineralizer. A variety of the techniques including X-ray diffraction (XRD), scanning electron microscopy (SEM), differential scanning calorimetry combined with the thermal gravimetric analysis (DSC–TG) were used to characterize the product. The gas sensing test indicates that h-MoO 3 microrods have a good response to 5–500 ppm ethanol in the range of 273–380 °C, and the optimum operating temperature is 332 °C with a high sensitivity of 8.24 to 500 ppm ethanol. Moreover, it also has a good selectivity toward ethanol gas if compared with other gases, such as ammonia, methanol and toluene. The sensing mechanism of h-MoO 3 microrods to ethanol was also discussed.

Hydrothermal Synthesis of Nanostructured Manganese Oxide as Cathodic Catalyst in a Microbial Fuel Cell Fed with Leachate

Science.gov (United States)

Haoran, Yuan; Lifang, Deng; Tao, Lu; Yong, Chen

2014-01-01

Much effort has been devoted to the synthesis of novel nanostructured MnO2 materials because of their unique properties and potential applications as cathode catalyst in Microbial fuel cell. Hybrid MnO2 nanostructures were fabricated by a simple hydrothermal method in this study. Their crystal structures, morphology, and electrochemical characters were carried out by FESEM, N2-adsorption-desorption, and CV, indicating that the hydrothermally synthesized MnO2 (HSM) was structured by nanorods of high aspect ratio and multivalve nanoflowers and more positive than the naturally synthesized MnO2 (NSM), accompanied by a noticeable increase in oxygen reduction peak current. When the HSM was employed as the cathode catalyst in air-cathode MFC which fed with leachate, a maximum power density of 119.07 mW/m2 was delivered, 64.68% higher than that with the NSM as cathode catalyst. Furthermore, the HSM via a 4-e pathway, but the NSM via a 2-e pathway in alkaline solution, and as 4-e pathway is a more efficient oxygen reduction reaction, the HSM was more positive than NSM. Our study provides useful information on facile preparation of cost-effective cathodic catalyst in air-cathode MFC for wastewater treatment. PMID:24723824

Synthesis pf dimethyl carbonate in supercritical carbon dioxide

Energy Technology Data Exchange (ETDEWEB)

Ballivet-Tkatchenko, D.; Plasseraud, L. [Universite de Bourgogne-UFR Sciences et Techniques, Dijon (France). Lab. de Synthese et Electrosynthese Organometalliques]. E-mail: ballivet@u-bourgogne.fr; Ligabue, R.A. [Pontificia Univ. Catolica do Rio Grande do Sul, Porto Alegre, RS (Brazil). Dept. de Quimica Pura

2006-01-15

The reactivity of carbon dioxide with methanol to form dimethyl carbonate was studied in the presence of the n-butylmethoxytin compounds n-Bu{sub 3}SnOCH{sub 3}, n-Bu{sub 2}Sn(OCH{sub 3}){sub 2}, and [n-Bu{sub 2}(CH{sub 3}O)Sn]{sub 2}O. The reaction occurred under solventless conditions at 423 K and was produced by an increase in CO{sub 2} pressure. This beneficial effect is primarily attributed to phase behavior. The mass transfer under liquid-vapor biphasic conditions was not limiting when the system reached the supercritical state for a CO{sub 2} pressure higher than 16 MPa. Under these conditions, CO{sub 2} acted as a reactant and a solvent. (author)

Morphology-control of VO2 (B) nanostructures in hydrothermal synthesis and their field emission properties

International Nuclear Information System (INIS)

Yin Haihong; Yu Ke; Zhang Zhengli; Zhu Ziqiang

2011-01-01

VO 2 (B) nanostructures were synthesized via a facile hydrothermal process using V 2 O 5 as source material and oxalic acid as reductant. Three nanostructures of nanorods, nanocarambolas and nanobundles were found existing in the products, and a continuous changing of morphology was found in the synthesis process, during which the proportion of these three types of nanostructures can be adjusted by altering the concentrations of oxalic acid. The microstructures were evaluated using X-ray diffraction and scanning and transmission electron microscopies, respectively. FE properties measurement of these three types of nanostructures showed that the nanobundles have the best field emission performance with a turn-on field of ∼1.4 V/μm and a threshold field of ∼5.38 V/μm. These characteristics make VO 2 (B) nanostructures a competitive cathode material in field emission devices.

Supercritical CO 2 -philic nanoparticles suitable for determining the viability of carbon sequestration in shale

KAUST Repository

Xu, Yisheng

2015-01-01

© The Royal Society of Chemistry. A fracture spacing less than a decimeter is probably required for the successful sequestration of CO2 in shale. Tracer experiments using inert nanoparticles could determine if a fracturing this intense has been achieved. Here we describe the synthesis of supercritical CO2-philic nanoparticles suitable for this application. The nanoparticles are ~50 nm in diameter and consist of iron oxide (Fe3O4) and silica (SiO2) cores functionalized with a fluorescent polymeric corona. The nanoparticles stably disperse in supercritical carbon dioxide (scCO2) and are detectable to concentrations of 10 ppm. This journal is

Biocrude production via supercritical hydrothermal co-liquefaction of spent mushroom compost and aspen wood sawdust

DEFF Research Database (Denmark)

Jasiunas, Lukas; Pedersen, Thomas Helmer; Toor, Saqib Sohail

2017-01-01

The work investigates a new potential feedstock source for hydrothermal liquefaction (HTL) driven biocrude production. Specifically, the focus is set on utilizing spent mushroom compost (SMC), the primary waste by-product from mushroom farming. It is considered as a feedstock for HTL conversion due...

Effect of hydrothermal process for inorganic alumina sol on crystal structure of alumina gel

Directory of Open Access Journals (Sweden)

K. Yamamura

2016-09-01

Full Text Available This paper reports the effect of a hydrothermal process for alumina sol on the crystal structure of alumina gel derived from hydrothermally treated alumina sol to help push forward the development of low temperature synthesis of α-Al2O3. White precipitate of aluminum hydroxide was prepared with a homogeneous precipitation method using aluminum nitrate and urea in aqueous solution. The obtained aluminum hydroxide precipitate was peptized by using acetic acid at room temperature, which resulted in the production of a transparent alumina sol. The alumina sol was treated with a hydrothermal process and transformed into an alumina gel film by drying at room temperature. Crystallization of the alumina gel to α-Al2O3 with 900 °C annealing was dominant for a hydrothermal temperature of 100 °C and a hydrothermal time of 60 min, as production of diaspore-like species was promoted with the hydrothermal temperature and time. Excess treatments with hydrothermal processes at higher hydrothermal temperature for longer hydrothermal time prevented the alumina gel from being crystallized to α-Al2O3 because the excess hydrothermal treatments promoted production of boehmite.

Supercritical carbon dioxide design strategies: from drug carriers to soft killers.

Science.gov (United States)

Aguiar-Ricardo, Ana; Bonifácio, Vasco D B; Casimiro, Teresa; Correia, Vanessa G

2015-12-28

The integrated use of supercritical carbon dioxide (scCO(2)) and micro- and nanotechnologies has enabled new sustainable strategies for the manufacturing of new medications. 'Green' scCO(2)-based methodologies are well suited to improve either the synthesis or materials processing leading to the assembly of three-dimensional multifunctional constructs. By using scCO(2) either as C1 feedstock or as solvent, simple, economic, efficient and clean routes can be designed to synthesize materials with unique properties such as polyurea dendrimers and oxazoline-based polymers/oligomers. These new biocompatible, biodegradable and water-soluble polymeric materials can be engineered into multifunctional constructs with antimicrobial activity, targeting moieties, labelling units and/or efficiently loaded with therapeutics. This mini-review highlights the particular features exhibited by these materials resulting directly from the followed supercritical routes. © 2015 The Author(s).

Hydrothermal route to VO2 (B) nanorods: controlled synthesis and characterization

Science.gov (United States)

Song, Shaokun; Huang, Qiwei; Zhu, Wanting

2017-10-01

One-dimensional vanadium dioxides have attracted intensive attention owing to their distinctive structure and novel applications in catalysis, high energy lithium-ion batteries, chemical sensors/actuators and electrochemical devices etc. In this paper, large-scale VO2 (B) nanorods have been successfully synthesized via a versatile and environment friendly hydrothermal strategy using V2O5 as vanadium source and carbohydrates/alcohols as reductant. The obtained samples are characterized by XRD, FT-IR, TEM, and XPS techniques to investigate the effects of chemical parameters such as reductants, temperature, and time of synthesis on the structure and morphology of products. Results show that pure B phase VO2 with homogeneous nanorod-like morphology can be prepared easily at 180 °C for 3 days with glycerol as reluctant. Typically, the nanorod-like products are 0.5-1 μm long and 50 nm width. Furthermore, it is also confirmed that the products are consisted of VO2, corresponding to the B phase. More importantly, this novel approach is efficient, free of any harmful solvents and surfactants. Therefore, this efficient, green, and cost-saving route will have great potential in the large-scale fabrication of 1D VO2 (B) nanorods from the economic and environmental point of view.

Controllable hydrothermal synthesis of Ni/H-BEA with a hierarchical core-shell structure and highly enhanced biomass hydrodeoxygenation performance.

Science.gov (United States)

Ma, Bing; Cui, Huimei; Wang, Darui; Wu, Peng; Zhao, Chen

2017-05-11

Ni based catalysts are wildly used in catalytic industrial processes due to their low costs and high activities. The design of highly hierarchical core-shell structured Ni/HBEA is achieved using a sustainable, simple, and easy-tunable hydrothermal synthesis approach using combined NH 4 Cl and NH 3 ·H 2 O as a co-precipitation agent at 120 °C. Starting from a single-crystalline hierarchical H + -exchanged beta polymorph zeolite (HBEA), the adjustment of the precipitate conditions shows that mixed NH 4 Cl and NH 3 ·H 2 O precipitates with proper concentrations are vital in the hydrothermal synthesis for preserving a good crystalline morphology of HBEA and generating abundant highly-dispersed Ni nanoparticles (loading: 41 wt%, 5.9 ± 0.7 nm) encapsulated onto/into the support. NH 4 Cl solution without an alkali is unable to generate abundant Ni nanoparticles from Ni salts under the hydrothermal conditions, whereas NH 3 ·H 2 O seriously damages the pore structure. After studying the in situ changes in infrared, X-ray diffractometry, temperature-programmed reduction, and scanning electron microscopy measurements, as well as variations in the filtrate pH, Si/Al ratios, and solid sample Ni loading, a two-step dissolution-recrystallization process is proposed. The process consists of Si dissolution and no change in elemental Al, and after the dissolved Si(iv) concentrations have promoted Ni phyllosilicate nanosheet solubility, further growth of multilayered Ni phyllosilicate nanosheets commences. The precursor Ni phyllosilicate is changeable between Ni 3 Si 2 O 5 (OH) 4 and Ni 3 Si 4 O 10 (OH) 2 , because of competition in kinetically-favored and thermodynamically-controlled species caused by different basic agents. The superior catalytic performance is demonstrated in the metal/acid catalyzed biomass derived bulky stearic acid hydrodeoxygenation with 90% octadecane selectivity and a promising rate of 54 g g -1 h -1 , which highly excels the reported rates catalyzed by

Hydrothermal synthesis spherical TiO2 and its photo-degradation property on salicylic acid

International Nuclear Information System (INIS)

Guo Wenlu; Liu Xiaolin; Huo Pengwei; Gao Xun; Wu Di; Lu Ziyang; Yan Yongsheng

2012-01-01

Anatase TiO 2 spheres have been prepared using hydrothermal synthesis. The prepared spheres were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM) and UV-vis diffuse reflectance spectra (UV-vis DRS). The TiO 2 consisted of well-defined spheres with size of 3-5 μm. The photocatalytic activity of spherical TiO 2 was determined by degradation of salicylic acid under visible light irradiation. It was revealed that the degradation rate of the spherical TiO 2 which was processed at 150 °C for 48 h could reach 81.758%. And the kinetics of photocatalytic degradation obeyed first-order kinetic, which the rate constant value was 0.01716 S -1 of the salicylic acid onto TiO 2 (temperature: 150, time: 48 h). The kinetics of adsorption followed the pseudo-second-order model and the rate constant was 1.2695 g mg -1 of the salicylic acid onto TiO 2 (temperature: 150, time: 48 h).

Hydrothermal Synthesis of Co-Ru Alloy Particle Catalysts for Hydrogen Generation from Sodium Borohydride

Directory of Open Access Journals (Sweden)

Marija Kurtinaitienė

2013-01-01

Full Text Available We report the synthesis of μm and sub-μm-sized Co, Ru, and Co-Ru alloy species by hydrothermal approach in the aqueous alkaline solutions (pH ≥ 13 containing CoCl2 and/or RuCl3, sodium citrate, and hydrazine hydrate and a study of their catalytic properties for hydrogen generation by hydrolysis of sodium borohydride solution. This way provides a simple platform for fabrication of the ball-shaped Co-Ru alloy catalysts containing up to 12 wt% Ru. Note that bimetallic Co-Ru alloy bowls containing even 7 at.% Ru have demonstrated catalytic properties that are comparable with the ones of pure Ru particles fabricated by the same method. This result is of great importance in view of the preparation of cost-efficient catalysts for hydrogen generation from borohydrides. The morphology and composition of fabricated catalyst particles have been characterized using scanning electron microscopy, energy dispersive X-ray diffraction, and inductively coupled plasma optical emission spectrometry.

A universal salt model based on under-ground precipitation of solid salts due to supercritical water `out-salting'

Science.gov (United States)

Rueslåtten, H.; Hovland, M. T.

2010-12-01

One of the common characteristics of planets Earth and Mars is that both host water (H2O) and large accumulations of salt. Whereas Earth’s surface-environment can be regarded as ‘water-friendly’ and ‘salt hostile’, the reverse can be said for the surface of Mars. This is because liquid water is stable on Earth, and the atmosphere transports humidity around the globe, whereas on planet Mars, liquid water is unstable, rendering the atmosphere dry and, therefore, ‘salt-friendly’. The riddle as to how the salt accumulated in various locations on those two planets, is one of long-lasting and great debate. The salt accumulations on Earth are traditionally termed ‘evaporites’, meaning that they formed as a consequence of the evaporation of large masses of seawater. How the accumulations on Mars formed is much harder to explain, as an ocean only existed briefly. Although water molecules and OH-groups may exist in abundance in bound form (crystal water, adsorbed water, etc.), the only place where free water is expected to be stable on Mars is within underground faults, fractures, and crevices. Here it likely occurs as brine or in the form of ice. Based on these conditions, a key to understanding the accumulation of large deposits of salt on both planets is linked to how brines behave in the subsurface when pressurized and heated beyond their supercritical point. At depths greater than about 3 km (P>300 bars) water will no longer boil in a steam phase. Rather, it becomes supercritical and will attain the phase of supercritical water vapor (SCRIW) with a specific gravity of typically 0.3 g/cm3. An important characteristic of SCRIW is its inability to dissolve the common sea salts. The salt dissolved in the brines will therefore precipitate as solid particles when brines (seawater on the Earth) move into the supercritical P&T-domain (T>400°C, P>300 bars). Numerical modeling of a hydrothermal system in the Atlantis II Deep of the Red Sea indicates that a

Hydrothermal Synthesis and Photocatalytic Property of β-Ga2O3 Nanorods

Science.gov (United States)

Reddy, L. Sivananda; Ko, Yeong Hwan; Yu, Jae Su

2015-09-01

Gallium oxide (Ga2O3) nanorods were facilely prepared by a simple hydrothermal synthesis, and their morphology and photocatalytic property were studied. The gallium oxide hydroxide (GaOOH) nanorods were formed in aqueous growth solution containing gallium nitrate and ammonium hydroxide at 95 °C of growth temperature. Through the calcination treatment at 500 and 1000 °C for 3 h, the GaOOH nanorods were converted into single crystalline α-Ga2O3 and β-Ga2O3 phases. From X-ray diffraction analysis, it could be confirmed that a high crystalline quality of β-Ga2O3 nanorods was achieved by calcinating at 1000 °C. The thermal behavior of the Ga2O3 nanorods was also investigated by differential thermal analysis, and their vibrational bands were identified by Fourier transform infrared spectroscopy. In order to examine the photocatalytic activity of samples, the photodegradation of Rhodamine B solution was observed under UV light irradiation. As a result, the α-Ga2O3 and β-Ga2O3 nanorods exhibited high photodegeneration efficiencies of 62 and 79 %, respectively, for 180 min of UV irradiation time.

Hydrothermal Synthesis and Photocatalytic Property of β-Ga2O3 Nanorods.

Science.gov (United States)

Reddy, L Sivananda; Ko, Yeong Hwan; Yu, Jae Su

2015-12-01

Gallium oxide (Ga2O3) nanorods were facilely prepared by a simple hydrothermal synthesis, and their morphology and photocatalytic property were studied. The gallium oxide hydroxide (GaOOH) nanorods were formed in aqueous growth solution containing gallium nitrate and ammonium hydroxide at 95 °C of growth temperature. Through the calcination treatment at 500 and 1000 °C for 3 h, the GaOOH nanorods were converted into single crystalline α-Ga2O3 and β-Ga2O3 phases. From X-ray diffraction analysis, it could be confirmed that a high crystalline quality of β-Ga2O3 nanorods was achieved by calcinating at 1000 °C. The thermal behavior of the Ga2O3 nanorods was also investigated by differential thermal analysis, and their vibrational bands were identified by Fourier transform infrared spectroscopy. In order to examine the photocatalytic activity of samples, the photodegradation of Rhodamine B solution was observed under UV light irradiation. As a result, the α-Ga2O3 and β-Ga2O3 nanorods exhibited high photodegeneration efficiencies of 62 and 79 %, respectively, for 180 min of UV irradiation time.

Hydrothermal synthesis of porous triphasic hydroxyapatite/(alpha and beta) tricalcium phosphate.

Science.gov (United States)

Vani, R; Girija, E K; Elayaraja, K; Prakash Parthiban, S; Kesavamoorthy, R; Narayana Kalkura, S

2009-12-01

A novel, porous triphasic calcium phosphate composed of nonresorbable hydroxyapatite (HAp) and resorbable tricalcium phosphate (alpha- and beta-TCP) has been synthesized hydrothermally at a relatively low temperature. The calcium phosphate precursor for hydrothermal treatment was prepared by gel method in the presence of ascorbic acid. XRD, FT-IR, Raman analyses confirmed the presence of HAp/TCP. The surface area and average pore size of the samples were found to be 28 m2/g and 20 nm, respectively. The samples were found to be bioactive in simulated body fluid (SBF).

Self-assembly of hollow MoS{sub 2} microflakes by one-pot hydrothermal synthesis for efficient electrocatalytic hydrogen evolution

Energy Technology Data Exchange (ETDEWEB)

Chen, Aishi; Cui, Renjie; He, Yanna; Wang, Qi [Key Laboratory for Organic Electronics and Information Displays & Institute of Advanced Materials (IAM), Jiangsu National Synergetic Innovation Center for Advanced Materials (SICAM), Nanjing University of Posts & Telecommunications, Nanjing 210023 (China); Zhang, Jian, E-mail: iamjzhang@njupt.edu.cn [Key Laboratory for Organic Electronics and Information Displays & Institute of Advanced Materials (IAM), Jiangsu National Synergetic Innovation Center for Advanced Materials (SICAM), Nanjing University of Posts & Telecommunications, Nanjing 210023 (China); Yang, Jianping [School of Science, Nanjing University of Posts and Telecommunications (NUPT), Nanjing 210023 (China); Li, Xing’ao, E-mail: lxahbmy@126.com [Key Laboratory for Organic Electronics and Information Displays & Institute of Advanced Materials (IAM), Jiangsu National Synergetic Innovation Center for Advanced Materials (SICAM), Nanjing University of Posts & Telecommunications, Nanjing 210023 (China); School of Science, Nanjing University of Posts and Telecommunications (NUPT), Nanjing 210023 (China)

2017-07-31

Highlights: • A new hollow MoS{sub 2} microflakes are prepared by hydrothermal synthesis firstly. • SEM and TEM study show the structural nature of hollow microflakes in depth. • The unique hollow structures have large surface area owing to the cavity. • The hollow microflakes show better HER performance than their solid counterparts. - Abstract: Molybdenum disulfide (MoS{sub 2}) has emerged as a promising non-precious metal catalyst for hydrogen evolution reaction (HER) in recent years. Some strategies including nanotechnology as well as atom doping have been employed in the preparing of electrocatalysts for high-activity and stability. To the best of our knowledge, hollow MoS{sub 2} microflakes assembled from ultrathin nanosheets have not been prepared previously. In this work, a simple, facile and environmentally friendly hydrothermal synthesis was utilized for the fabrication of hollow MoS{sub 2} microflakes for the first time. The unique hollow structures have fascinating properties, such as the large surface and low density. The morphology and structure of MoS{sub 2} microflakes were confirmed by XRD, SEM, TEM and Raman. The composition of these materials was identified by the X-ray photoelectron spectroscopy. Notably, the as-prepared hollow MoS{sub 2} microflakes showed better electrocatalytic activity than other samples. The hollow flake-like structure can not only increase the active edge sites owing to the large specific surface area, but also enhance the electron transport to improve the electrocatalytic activity. Benefiting from these factors, the hollow MoS{sub 2} microflakes exhibited electrocatalytic activity and excellent stability with a low overpotential about 85 mV and a Tafel slope of 59 mV per decade.

Synthesis of nickel oxide - zirconia composites by coprecipitation route followed by hydrothermal treatment

International Nuclear Information System (INIS)

Yoshito, Walter Kenji; Ussui, Valter; Lazar, Dolores Ribeiro Ricci; Paschoal, Jose Octavio Armani

2009-01-01

Nickel oxide-yttria stabilized zirconia (NiO-YSZ) for use as solid oxide fuel cell anode were synthesized by coprecipitation to obtain amorphous zirconia and crystallized β-nickel gels of the corresponding metal hydroxides. Hydrothermal treatment at 200°C and 220 psi from 2 up to 16 hours, under stirring, was performed to produce nanocrystalline powder. The as-synthesized powders were uniaxially pressed and sintered in air. Powders were characterized by X-ray diffraction, laser scattering, scanning and transmission electron microscopy (SEM/TEM), gas adsorption technique (BET) and TGDTA thermal analysis. Ceramic samples were characterized by dilatometric analysis and density measurements by Archimedes method. The characteristics of hydrothermally synthesized powders and compacts were compared to those produced without temperature and pressure application. Crystalline powders were obtained after hydrothermal process, excluding the calcination step from this route. The specific surface area of powders decreases with increasing time of hydrothermal treatment while the agglomerate mean size is not affected by this parameter. (author)

Hydrothermal synthesis and characterization of a two-dimensional piperazinium cobalt–zinc phosphate via a metastable one-dimensional phase

International Nuclear Information System (INIS)

Torre-Fernández, Laura; Khainakova, Olena A.; Espina, Aránzazu; Amghouz, Zakariae; Khainakov, Sergei A.; Alfonso, Belén F.; Blanco, Jesús A.; García, José R.; García-Granda, Santiago

2015-01-01

A two-dimensional piperazinium cobalt–zinc phosphate, formulated as (C 4 N 2 H 12 ) 1.5 (Co 0.6 Zn 0.4 ) 2 (HPO 4 ) 2 (PO 4 )·H 2 O (2D), was synthesized under hydrothermal conditions. The crystal structure was determined using single-crystal X-ray diffraction data (monoclinic P2 1 /c, a=8.1165(3) Å, b=26.2301(10) Å, c=8.3595(4) Å, and β=110.930(5)°) and the hydrogen atom positions were optimized by DFT calculations. A single-crystal corresponding to one-dimensional metastable phase, (C 4 N 2 H 12 )Co 0.3 Zn 0.7 (HPO 4 ) 2 ·H 2 O (1D), was also isolated and the crystal structure was determined (monoclinic P2 1 /c, a=8.9120(6) Å, b=14.0290(1) Å, c=12.2494(5) Å, and β=130.884(6)°). The bulk was characterized by chemical (C–H–N) analysis, powder X-ray diffraction (PXRD), powder X-ray thermodiffractometry (HT-XRD), transmission electron microscopy (STEM(DF)-EDX and EFTEM), and thermal analysis (TG/SDTA-MS), including activation energy data of its thermal decomposition. The magnetic susceptibility and magnetization measurements show no magnetic ordering down to 4 K. - Graphical abstract: Hydrothermal synthesis and structural characterization of a two-dimensional piperazinium cobalt–zinc phosphate, (C 4 N 2 H 12 ) 1.5 (Co 0.6 Zn 0.4 ) 2 (HPO 4 ) 2 (PO 4 )·H 2 O (2D), have been reported. The crystal structure of a one-dimensional piperazinium cobalt–zinc phosphate, (C 4 N 2 H 12 )Co 0.3 Zn 0.7 (HPO 4 ) 2 ·H 2 O (1D) a metastable phase during the hydrothermal synthesis, was also determined. The thermal behavior of 2D compound is strongly dependent on the selected heating rate and the magnetic susceptibility and magnetization measurements show no magnetic ordering down to 4 K. - Highlights: • A 2D piperazinium cobalt–zinc phosphate has been synthesized and characterized. • Crystal structure of 1D metastable phase was also determined. • Thermal behavior of 2D compound is strongly dependent on the selected heating rate. • Magnetic

Effects of buffer layer annealing temperature on the structural and optical properties of hydrothermal grown ZnO

Energy Technology Data Exchange (ETDEWEB)

Zhao, X.Q.; Kim, C.R.; Lee, J.Y.; Heo, J.H.; Shin, C.M. [Department of Nano Systems Engineering, Center for Nano Manufacturing, Inje University, Obang-dong, Gimhae, Gyeongnam 621-749 (Korea, Republic of); Ryu, H., E-mail: hhryu@inje.ac.kr [Department of Nano Systems Engineering, Center for Nano Manufacturing, Inje University, Obang-dong, Gimhae, Gyeongnam 621-749 (Korea, Republic of); Chang, J.H. [Major of Nano Semiconductor, Korea Maritime University, 1 Dongsam-dong, Yeongdo-Ku, Busan 606-791 (Korea, Republic of); Lee, H.C. [Department of Mechatronics Engineering, Korea Maritime University, 1 Dongsam-dong, Yeongdo-Ku, Busan 606-791 (Korea, Republic of); Son, C.S. [Department of Electronic Materials Engineering, Silla University, Gwaebeop-dong, Sasang-gu, Busan 617-736 (Korea, Republic of); Lee, W.J. [Department of Nano Engineering, Dong-Eui University, 995 Eomgwangno, Busanjin-gu, Busan 614-714 (Korea, Republic of); Jung, W.G. [School of Advanced Materials Engineering, Kookmin University, 861-1 Jeongneung-dong, Seongbuk-gu, Seoul 136-702 (Korea, Republic of); Tan, S.T. [Institute of Microelectronics, 11 Science Park Road, Science Park II, Singapore 117685 (Singapore); Zhao, J.L. [School of Electrical and Electronic Engineering, Nanyang Technological University, Nanyang Avenue, Singapore 639798 (Singapore); Sun, X.W. [Institute of Microelectronics, 11 Science Park Road, Science Park II, Singapore 117685 (Singapore); School of Electrical and Electronic Engineering, Nanyang Technological University, Nanyang Avenue, Singapore 639798 (Singapore)

2009-02-01

ZnO was deposited on bare Si(1 0 0), as-deposited, and annealed ZnO/Si(1 0 0) substrates by hydrothermal synthesis. The effects of a ZnO buffer layer and its thermal annealing on the properties of the ZnO deposited by hydrothermal synthesis were studied. The grain size and root mean square (RMS) roughness values of the ZnO buffer layer increased after thermal annealing of the buffer layer. The effect of buffer layer annealing temperature on the structural and optical properties was investigated by photoluminescence, X-ray diffraction, atomic force microscopy, and scanning electron microscopy. Hydrothermal grown ZnO deposited on ZnO/Si(1 0 0) annealed at 750 deg. C with the concentration of 0.3 M exhibits the best structural and optical properties.

Hydrothermal synthesis of cathode materials

Science.gov (United States)

Chen, Jiajun; Wang, Shijun; Whittingham, M. Stanley

A number of cathodes are being considered for the next generation of lithium ion batteries to replace the expensive LiCoO 2 presently used. Besides the layered oxides, such as LiNi yMn yCo 1-2 yO 2, a leading candidate is lithium iron phosphate with the olivine structure. Although this material is inherently low cost, a manufacturing process that produces electrochemically active LiFePO 4 at a low cost is also required. Hydrothermal reactions are one such possibility. A number of pure phosphates have been prepared using this technique, including LiFePO 4, LiMnPO 4 and LiCoPO 4; this method has also successfully produced mixed metal phosphates, such as LiFe 0.33Mn 0.33Co 0.33PO 4. Ascorbic acid was found to be better than hydrazine or sugar at preventing the formation of ferric ions in aqueous media. When conductive carbons are added to the reaction medium excellent electrochemical behavior is observed.

Supercritical Water Reactors

International Nuclear Information System (INIS)

Bouchter, J.C.; Dufour, P.; Guidez, J.; Latge, C.; Renault, C.; Rimpault, G.

2014-01-01

The supercritical water reactor (SCWR) is one of the 6 concepts selected for the 4. generation of nuclear reactors. SCWR is a new concept, it is an attempt to optimize boiling water reactors by using the main advantages of supercritical water: only liquid phase and a high calorific capacity. The SCWR requires very high temperatures (over 375 C degrees) and very high pressures (over 22.1 MPa) to operate which allows a high conversion yield (44% instead of 33% for a PWR). Low volumes of coolant are necessary which makes the neutron spectrum shift towards higher energies and it is then possible to consider fast reactors operating with supercritical water. The main drawbacks of supercritical water is the necessity to use very high pressures which has important constraints on the reactor design, its physical properties (density, calorific capacity) that vary strongly with temperatures and pressures and its very high corrosiveness. The feasibility of the concept is not yet assured in terms of adequate materials that resist to corrosion, reactor stability, reactor safety, and reactor behaviour in accidental situations. (A.C.)

A facile hydrothermal synthesis, characterization and magnetic properties of mesoporous CoFe{sub 2}O{sub 4} nanospheres

Energy Technology Data Exchange (ETDEWEB)

Reddy, M. Penchal, E-mail: reddy@nimte.ac.cn [Center for Advanced Materials, Qatar University, Doha 2713 (Qatar); Mohamed, A.M.A. [Center for Advanced Materials, Qatar University, Doha 2713 (Qatar); Department of Metallurgical and Materials Engineering, Faculty of Petroleum and Mining Engineering, Suez University, Suez 4372 (Egypt); Zhou, X.B.; Du, S.; Huang, Q. [Ningbo Institute of Materials Technology and Engineering (NIMTE), Chinese Academy of Sciences (CAS), Ningbo 315201, Zhejiang, RP China (China)

2015-08-15

Mesoporous CoFe{sub 2}O{sub 4} nanospheres with an average size of 180 nm were fabricated via a facile hydrothermal process using ethylene glycol as solvent and sodium acetate (NaAc) as electrostatic stabilizer. In this method, ethylene glycol plays a vital role in the formation of cobalt nanoospheres as a solvent and reducing agent. The structure and morphology of the prepared materials were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high-resolution TEM (HRTEM), Fourier transform infrared spectroscopy (FTIR) and X-ray photoelectron spectroscopy (XPS). The nanospheres exhibited ferromagnetic properties with high saturation magnetization value of about 60.19 emu/g at room temperature. The BET surface area of the nanospheres was determined using the nitrogen absorption method. The porous CoFe{sub 2}O{sub 4} nanospheres displayed good magnetic properties, which may provide a very promising candidate for their applications in target drug delivery. - Highlights: • CoFe{sub 2}O{sub 4} nanospheres were prepared by hydrothermal synthesis for the first time. • Average grain size was found to be 180 nm. • Its structural, morphological, magnetic behavior was studied. • TEM observations confirmed the spherical morphology of the mesoporous ferrites.

Destruction of nitrates, organics, and ferrocyanides by hydrothermal processing

International Nuclear Information System (INIS)

Robinson, J.M.; Foy, B.R.; Dell'Orco, P.C.; Anderson, G.; Archuleta, F.; Atencio, J.; Breshears, D.; Brewer, R.; Eaton, H.; McFarland, R.; McInroy, R.; Reynolds, T.; Sedillo, M.; Wilmanns, E.; Buelow, S.J.

1993-01-01

This work targets the remediation of the aqueous mixed wastes stored in the underground tanks at the Department of Energy site in Hanford, Washington via hydrothermal processing. The feasibility of destroying the nitrate, organic, and ferrocyanide components of the wastes under supercritical and near critical conditions (623 degree K to 873 degree K, 22.1 MPa to 103.4 MPa) is addressed. A novel method was developed for determining the solubility of nitrate salts in supercritical water solutions at pressures ranging from 24.8 MPa to 30.3 MPa (3600 psi to 4400 psi) and temperatures from 723 degree K to 798 degree K. Sodium nitrate solubilities ranged from 293 mg/kg at 24.8 MPa and 798 degree K to 1963 mg/kg at 30.3 MPa and 723 degree K. Solubility was found to vary directly with pressure, and inversely with temperature. An empirical relationship was developed for the estimation of sodium nitrate solubility at water densities between 0.08 and 0.16 kg/L and temperatures between 723 degree K and 798 degree K. A small volume batch reactor equipped with optical diagnostics was used to monitor the phase behavior of a diluted variant of a tank 101-SY simulant. Preliminary results suggest that a single phase is formed at 83 MPa at 773 degree K

Hydrothermal processes above the Yellowstone magma chamber: Large hydrothermal systems and large hydrothermal explosions

Science.gov (United States)

Morgan, L.A.; Shanks, W.C. Pat; Pierce, K.L.

2009-01-01

Hydrothermal explosions are violent and dramatic events resulting in the rapid ejection of boiling water, steam, mud, and rock fragments from source craters that range from a few meters up to more than 2 km in diameter; associated breccia can be emplaced as much as 3 to 4 km from the largest craters. Hydrothermal explosions occur where shallow interconnected reservoirs of steam- and liquid-saturated fluids with temperatures at or near the boiling curve underlie thermal fields. Sudden reduction in confi ning pressure causes fluids to fl ash to steam, resulting in signifi cant expansion, rock fragmentation, and debris ejection. In Yellowstone, hydrothermal explosions are a potentially signifi cant hazard for visitors and facilities and can damage or even destroy thermal features. The breccia deposits and associated craters formed from hydrothermal explosions are mapped as mostly Holocene (the Mary Bay deposit is older) units throughout Yellowstone National Park (YNP) and are spatially related to within the 0.64-Ma Yellowstone caldera and along the active Norris-Mammoth tectonic corridor. In Yellowstone, at least 20 large (>100 m in diameter) hydrothermal explosion craters have been identifi ed; the scale of the individual associated events dwarfs similar features in geothermal areas elsewhere in the world. Large hydrothermal explosions in Yellowstone have occurred over the past 16 ka averaging ??1 every 700 yr; similar events are likely in the future. Our studies of large hydrothermal explosion events indicate: (1) none are directly associated with eruptive volcanic or shallow intrusive events; (2) several historical explosions have been triggered by seismic events; (3) lithic clasts and comingled matrix material that form hydrothermal explosion deposits are extensively altered, indicating that explosions occur in areas subjected to intense hydrothermal processes; (4) many lithic clasts contained in explosion breccia deposits preserve evidence of repeated fracturing

One-pot hydrothermal synthesis and characterization of CoFe{sub 2}O{sub 4} nanoparticles and its application as magnetically recoverable catalyst in oxidation of alcohols by periodic acid

Energy Technology Data Exchange (ETDEWEB)

Paul, Bappi; Purkayastha, Debraj Dhar; Dhar, Siddhartha Sankar, E-mail: ssd_iitg@hotmail.com

2016-09-15

A novel and facile approach for one-pot synthesis of spinel cobalt ferrite (CoFe{sub 2}O{sub 4}) nanoparticles (NPs) is presented here. The synthesis involves homogeneous chemical precipitation followed by hydrothermal heating, using tributylamine (TBA) as a hydroxylating agent. Polyethylene glycol (PEG) 4000 was used as surfactant. As-synthesized CoFe{sub 2}O{sub 4} NPs were characterized by powder X-ray diffraction (XRD), transmission electron microscopy (TEM), N{sub 2} adsorption-desorption isotherm (BET) and vibrating sample magnetometry (VSM). TEM image showed formation of spherical particles of sizes 2–30 nm. These NPs were used as magnetically recoverable catalyst in oxidation of alcohols to their corresponding aldehydes by periodic acid. This oxidative procedure is found to be highly efficient affording products in very high yield and selectivity. The easy magnetic separation of the catalyst and efficient reusability are key features of this methodology. - Highlights: • Hydrothermal synthesis of CoFe{sub 2}O{sub 4} NPs with (C{sub 4}H{sub 9}){sub 3}N as hydroxylating agent. • The TEM images showed the particles to be spherical in shape with sizes 2–30 nm. • CoFe{sub 2}O{sub 4} was used as recyclable catalyst for oxidation of alcohols by periodic acid.

Controllable synthesis of α- and β-MnO2: cationic effect on hydrothermal crystallization

International Nuclear Information System (INIS)

Huang Xingkang; Lv Dongping; Yue Hongjun; Attia, Adel; Yang Yong

2008-01-01

α- and β-MnO 2 were controllably synthesized by hydrothermally treating amorphous MnO 2 obtained via a reaction between Mn 2+ and MnO 4 - , and cationic effects on the hydrothermal crystallization of MnO 2 were investigated systematically. The crystallization is believed to proceed by a dissolution-recrystallization mechanism; i.e. amorphous MnO 2 dissolves first under hydrothermal conditions, then condenses to recrystallize, and the polymorphs formed are significantly affected by added cations such as K + , NH 4 + and H + in the hydrothermal systems. The experimental results showed that K + /NH 4 + were in competition with H + to form polymorphs of α- and β-MnO 2 , i.e., higher relative K + /NH 4 + concentration favoured α-MnO 2 , while higher relative H + concentration favoured β-MnO 2

Two-Step Hydrothermal Synthesis of Bifunctional Hematite-Silver Heterodimer Nanoparticles for Potential Antibacterial and Anticancer Applications

Science.gov (United States)

Trang, Vu Thi; Tam, Le Thi; Phan, Vu Ngoc; Van Quy, Nguyen; Huy, Tran Quang; Le, Anh-Tuan

2017-06-01

In recent years, the development of composite nanostructures containing noble metal and magnetic nanocrystals has attracted much interest because they offer a promising avenue for multifunctional applications in nanomedicine and pharmacotherapy. In this work, we present a facile two-step hydrothermal approach for the synthesis of bifunctional heterodimer nanoparticles (HDNPs) composed of hematite nanocubes (α-Fe2O3 NCs) and silver nanoparticles (Ag-NPs). The formation and magnetic property of α-Fe2O3-Ag HDNPs was analyzed by transmission electron microscopy, x-ray diffraction and vibrating sample magnetometer. Interestingly, the hydrothermal-synthesized α-Fe2O3-Ag HDNPs were found to display significant antibacterial activity against three types of infectious bacteria. The cytotoxicity of α-Fe2O3-Ag nanocomposite against lung cancer A549 cell line was investigated and compared with that of pure α-Fe2O3 NCs and Ag-NPs. The obtained results reveal that the α-Fe2O3-Ag nanocomposite exhibited higher anticancer performance than that of pure Ag-NPs, whereas pure α-Fe2O3 NCs were not cytotoxic to the tested cells. The inhibitory concentration (IC50) of the α-Fe2O3-Ag nanocomposite was found at 20.94 μg/mL. With the aforementioned properties, α-Fe2O3-Ag HDNPs showed a high potential as a multifunctional material for advanced biomedicine and nanotherapy applications.

Low Temperature Synthesis of Metal Oxides by a Supercritical Seed Enhanced Crystallization (SSEC) Process

DEFF Research Database (Denmark)

Jensen, Henrik; Brummerstedt Iversen, Steen; Joensen, Karsten Dan

2006-01-01

A novel method for producing crystalline nanosized metal oxides by a Supercritical Seed Enhanced Crystallization (SSEC) Process has been developed. The process is a modified sol-gel process taking place at temperatures as low as 95 ºC with supercritical CO2 as solvent and polypropylene as seeding...... material. The nanocrystalline product is obtained without having to resort to costly post-reaction processing and the product is obtained directly after the SSEC process. TiO2 powders produced by the SSEC process were shown to have a crystallinity of 60 % and a crystal size of 7.3 ± 2.6 nm....... The crystallinity can be controlled by changing the heating rate of the initial formation of the nanoparticles and the morphology can be altered by changing the process time....

Template-assisted hydrothermally synthesized iron-titanium binary oxides and their application as catalysts for ethyl acetate oxidation

Czech Academy of Sciences Publication Activity Database

Tsoncheva, T.; Ivanova, R.; Dimitrov, M.; Paneva, D.; Kovacheva, D.; Henych, Jiří; Vomáčka, Petr; Kormunda, M.; Velinov, N.; Mitov, I.; Štengl, Václav

2016-01-01

Roč. 528, NOV (2016), s. 24-35 ISSN 0926-860X R&D Projects: GA MŠk(CZ) LM2015073 Institutional support: RVO:61388980 Keywords : Effect of Fe/Ti ratio and temperature of hydrothermal treatment * Hydrothermal synthesis * Iron-titanium binary oxides Subject RIV: CA - Inorganic Chemistry Impact factor: 4.339, year: 2016

Supercritical fluids processing: emerging opportunities

International Nuclear Information System (INIS)

Kovaly, K.A.

1985-01-01

This publication on the emerging opportunities of supercritical fluids processing reveals the latest research findings and development trends in this field. These findings and development trends are highlighted, and the results of applications of technology to the business of supercritical fluids are reported. Applications of supercritical fluids to chemical intermediates, environmental applications, chemical reactions, food and biochemistry processing, and fuels processing are discussed in some detail

Synthesis of inorganic materials in a supercritical carbon dioxide medium. Application to ceramic cross-flow filtration membranes preparation

International Nuclear Information System (INIS)

Papet, Sebastien

2000-01-01

Membrane separations, using cross-flow mineral ceramic membranes, allows fractionation of aqueous solutions due to the molecular sieve effect and electrostatic charges. To obtain a high selectivity, preparation of new selective ceramic membranes is necessary. We propose in this document two different routes to prepare such cross-flow tubular mineral membranes. In the first exposed method, a ceramic material is used, titanium dioxide, synthesized in supercritical carbon dioxide by the hydrolysis of an organometallic precursor of the oxide. The influence of operating parameters is similar to what is observed during a liquid-phase synthesis (sol-gel process), and leads us to control the size and texture of the prepared particles. This material is then used to prepare mineral membrane with a compressed layer process. The particles are mixed with organic components to form a liquid suspension. A layer is then deposited on the internal surface of a tubular porous support by slip-casting. The layer is then dried and compressed on the support before sintering. The obtained membranes arc in the ultrafiltration range. A second process has been developed in this work. It consists on the hydrolysis, in a supercritical CO 2 medium, of a precursor of titanium dioxide infiltrated into the support. The obtained material is then both deposited on the support but also infiltrated into the porosity. This new method leads to obtain ultrafiltration membranes that retain molecules which molecular weight is round 4000 g.mol -1 . Furthermore, we studied mass transfer mechanisms in cross-flow filtration of aqueous solutions. An electrostatic model, based on generalized Nernst-Planck equation that takes into account electrostatic interactions between solutes and the ceramic material, lead us to obtain a good correlation between experimental results and the numerical simulation. (author) [fr

High-yield production of biodiesel by non-catalytic supercritical methanol transesterification of crude castor oil (Ricinus communis)

International Nuclear Information System (INIS)

Román-Figueroa, Celián; Olivares-Carrillo, Pilar; Paneque, Manuel; Palacios-Nereo, Francisco Javier; Quesada-Medina, Joaquín

2016-01-01

The synthesis of biodiesel from crude castor oil in a catalyst-free process using supercritical methanol in a batch reactor was investigated, studying the evolution of intermediate products as well as the conversion of triglycerides and the yield of FAMEs (fatty acid methyl esters) (biodiesel). Experiments were carried out in a temperature range of 250–350 °C (10–43 MPa) at reaction times of 15–90 min for a methanol-to-oil molar ratio of 43:1. Maintaining thermal stability of biodiesel is one of the most important concerns in high-yield supercritical biodiesel production. Hence, thermal decomposition degree of FAMEs was also investigated in different reaction conditions. The maximum yield of FAMEs (96.5%) was obtained at 300 °C (21 MPa) and 90 min. Under these conditions, the conversion of triglycerides was complete, the yield of intermediate products was low (3.29 and 1.41% for monoglycerides and diglycerides, respectively), and thermal decomposition of FAMEs did not occur. The maximum degree of thermal decomposition (80.9%) was produced at 350 °C (43 MPa) and 90 min. Methyl ricinoleate, whose fatty acid chain was the most abundant (88.09 mol%) in castor oil, was very unstable above 300 °C and 60 min, leading to low yields of FAMEs under these conditions. - Highlights: • Supercritical synthesis of biodiesel from crude castor oil was investigated. • Supercritical methanolysis of crude castor oil reached a high yield of FAMEs. • Ricinoleic acid methyl ester was very unstable above 300 °C and 60 min reaction.

Hydrothermal synthesis, characterization, and magneticproperties of cobalt chromite nanoparticles

Czech Academy of Sciences Publication Activity Database

Zákutná, Dominika; Repko, A.; Matulková, I.; Nižňanský, Daniel; Ardu, A.; Cannas, C.; Mantlíková, Alice; Vejpravová, Jana

2014-01-01

Roč. 16, č. 2 (2014), 1-14 ISSN 1388-0764 R&D Projects: GA ČR GAP108/10/1250 Institutional support: RVO:68378271 ; RVO:61388980 Keywords : cobalt chromite * hydrothermal method * nanoparticles * size effect * multiferroic materials Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 2.184, year: 2014

Controlled synthesis of MoO3 microcrystals by subsequent calcination of hydrothermally grown pyrazine–MoO3 nanorod hybrids and their photodecomposition properties

International Nuclear Information System (INIS)

Rajagopal, S.; Nataraj, D.; Khyzhun, O.Y.; Djaoued, Yahia; Robichaud, Jacques; Kim, Chang-Koo

2013-01-01

We present our results on successful synthesis of pyrazine–MoO 3 nanorod hybrids by using pyrazine and MoO 3 nanorods. On the first stage, MoO 3 nanorods were grown hydrothermally and, on the second stage, their mixture with pyrazine was again involved in a hydrothermal reaction to produce organic–inorganic hybrids. To understand the growth mechanism of the hybrids we varied time and temperature of the hydrothermal process. Intercalation of pyrazine was confirmed through X-ray diffraction analysis, X-ray photoelectron spectroscopy, X-ray emission spectroscopy, scanning electron microscopy methods. Upon calcinations, pyrazine was deintercalated, i.e. removed from the MoO 3 hybrid system, and the MoO 3 nanorods were found to bind together resulting in formation of MoO 3 microslabs with increased surface area. Photodecomposition performance of the MoO 3 nanorods, pyrazine–MoO 3 hybrids and MoO 3 microcrystals was studied against Procion Red MX-5B textile dye. A high photodecomposition performance was found to decrease when going from MoO 3 nanorods to MoO 3 microcrystal and, further, to pyrazine–MoO 3 hybrids. - Graphical abstract: Display Omitted - Highlights: • High aspect ratio MoO 3 nanorods were prepared through a new hydrothermal method. • Hybrids of pyrazine–MoO 3 were formed by intercalating pyrazine into MoO 3 nanorods. • Intercalation of pyrazine was confirmed in X-ray spectroscopic analysis. • After calcinations, MoO 3 crystal was retained by binding MoO 3 nanorods together. • High photodegradation performance was noticed from MoO 3 nanorods

Bio-oil production from hydrothermal liquefaction of Pteris vittata L.: Effects of operating temperatures and energy recovery.

Science.gov (United States)

Chen, Jinbo

2018-06-14

Hyper-accumulator biomass, Pteris vittata L., was hydrothermally converted into bio-oils via hydrothermal liquefaction (HTL) in sub-supercritical water. The distributions and characterizations of various products as well as energy recovery under different temperatures (250-390 °C) were investigated. The highest bio-oil yield of 16.88% was obtained at 350 °C with the hydrothermal conversion of 61.79%, where the bio-oil was dominated by alcohols, esters, phenols, ketones and acidic compounds. The higher heating values of bio-oil were in the range of 19.93-35.45 MJ/kg with a H/C ratio of 1.26-1.46, illustrating its high energy density and potential for use as an ideal liquid fuel. The main gaseous products were CO 2 , H 2 , CO, and CH 4 with the H 2 yield peaking at 22.94%. The total energy recovery from bio-oils and solid residues fell within the range of 37.72-45.10%, highlighting the potential of HTL to convert hyper-accumulator biomass into valuable fuels with high conversion efficiency. Copyright © 2018 Elsevier Ltd. All rights reserved.

Preparation of ultrasmall porous carbon nanospheres by reverse microemulsion-hydrothermal method

Science.gov (United States)

Wang, Jiasheng; Zhao, Yahong; Wang, Wan-Hui; Bao, Ming

Porous carbon nanospheres (CNSs) have wide applications. A big challenge in materials science is synthesis of discrete ultrasmall porous carbon nanospheres. Herein, we report a facile reverse microemulsion-hydrothermal method to prepare discrete porous CNSs. The obtained CNSs possess an average diameter of 20nm and pores of 0.7nm and 3.4nm. Our work has provided a convenient method for the controllable synthesis of ultrasmall porous CNSs with potential applications.

Synthesis of biodiesel fuel additives from glycerol using green chemistry and supercritical fluids

Science.gov (United States)

For every 3 moles of fatty acid esters produced, 1 mole of glycerol remains, ~11% of the biodiesel volume. One new method of glycerol use could be as a biodiesel fuel additive/extender using eco-friendly heterogeneous catalysts and supercritical fluids (SFs). SFs have advantages such as greater diff...

Selective synthesis of vitamin K3 over mesoporous NbSBA-15 catalysts synthesized by an efficient hydrothermal method.

Science.gov (United States)

Selvaraj, M; Park, D-W; Kim, I; Kawi, S; Ha, C S

2012-08-28

Well hexagonally ordered NbSBA-15 catalysts synthesized by an efficient hydrothermal method were used, for the first time, for the selective synthesis of vitamin K(3) by liquid-phase oxidation of 2-methyl-1-naphthol (2MN1-OH) under various reaction conditions. The recyclable NbSBA-15 catalysts were also reused to find their catalytic activities. To investigate the leaching of non-framework niobium species on the surface of silica networks, the results of original and recyclable NbSBA-15 catalysts were correlated and compared. To find an optimum condition for the selective synthesis of vitamin K(3), the washed NbSBA-15(2.2pH) was extensively used in this reaction with various reaction parameters such as temperature, time and ratios of reactant (2M1N-OH to H(2)O(2)), and the obtained results were also demonstrated. Additionally, the liquid-phase oxidation of 2M1N-OH was carried out with different solvents to find the best solvent with a good catalytic activity. Based on the all catalytic studies, the vitamin K(3) selectivity (97.3%) is higher in NbSBA-15(2.2pH) than that of other NbSBA-15 catalysts, and the NbSBA-15(2.2pH) is found to be a highly active and eco-friendly heterogeneous catalyst for the selective synthesis of vitamin K(3).

Improved seedless hydrothermal synthesis of dense and ultralong ZnO nanowires

International Nuclear Information System (INIS)

Tian Jinghua; Hu Jie; Li Sisi; Zhang Fan; Liu Jun; Shi Jian; Li Xin; Chen Yong; Tian Zhongqun

2011-01-01

Seedless hydrothermal synthesis has been improved by introducing an adequate content of ammonia into the nutrient solution, allowing the fabrication of dense and ultralong ZnO nanowire arrays over large areas on a substrate. The presence of ammonia in the nutrient solution facilitates the high density nucleation of ZnO on the substrate which is critical for the nanowire growth. In order to achieve an optimal growth, the growth conditions have been studied systematically as a function of ammonia content, growth temperature and incubation time. The effect of polyethyleneimine (PEI) has also been studied but shown to be of no benefit to the nucleation of ZnO. Ultradense and ultralong ZnO nanowires could be obtained under optimal growth conditions, showing no fused structure at the foot of the nanowire arrays. Due to different reaction kinetics, four growth regimes could be attributed, including the first fast growth, equilibrium phase, second fast growth and final erosion. Combining this simple method with optical lithography, ZnO nanowires could be grown selectively on patterned areas. In addition, the as-grown ZnO nanowires could be used for the fabrication of a piezoelectric nanogenerator. Compared to the device of ZnO nanowires made by other methods, a more than twice voltage output has been obtained, thereby proving an improved performance of our growth method.

Controlled synthesis of graphene sheets with tunable sizes by hydrothermal cutting

International Nuclear Information System (INIS)

Ma Chen; Chen Zhongxin; Fang Ming; Lu Hongbin

2012-01-01

We report a hydrothermal method that directly reduces graphene oxide (GO) into graphene nanosheets (GNs) with different sizes. In the presence of NaOH and hydrazine, the hydrothermal reaction at 80 °C resulted in the formation of GNs with a lateral size of ∼1 μm but the size of GNs decreased to ∼300 and ∼100 nm upon increasing the reaction temperature to 150 and 200 °C, respectively. The morphology of the resulting GNs was observed by atomic force microscopy and transmission electron microscopy. The thickness of GNs is basically <3 nm, indicates the GNs stack together in a few-layer manner. XRD, XPS, FTIR, and Raman spectroscopy were used to characterize the structural changes before and after reduction. The results suggested that the defect stability in GO and reduced GNs could be responsible for the temperature dependence of the size of reduced GNs.Graphical AbstractA hydrothermal method is proposed to simultaneously reduce and cut graphene oxide into graphene sheets with different sizes in a controlled manner, in which the reaction temperature as a critical parameter is used to control the size of resulting graphene sheets.

Immobilization of LiCl-Li 2 O pyroprocessing salt wastes in chlorosodalite using glass-bonded hydrothermal and salt-occlusion methods

Energy Technology Data Exchange (ETDEWEB)

Riley, Brian J.; Peterson, Jacob A.; Kroll, Jared O.; Frank, Steven M.

2018-04-01

In this study, salt occlusion and hydrothermal processes were used to make chlorosodalite through reaction with a high-LiCl salt simulating a waste stream following pyrochemical treatment of oxide-based used nuclear fuel. Some products were reacted with glass binders to increase chlorosodalite yield through alkali ion exchange and aide in densification. Hydrothermal processes included reaction of the salt simulant in an acid digestion vessel with either zeolite 4A or sodium aluminate and colloidal silica. Chlorosodalite yields in the crystalline products were nearly complete in the glass-bonded materials at values of 100 mass% for the salt-occlusion method, up to 99.0 mass% for the hydrothermal synthesis with zeolite 4A, and up to 96 mass% for the hydrothermal synthesis with sodium aluminate and colloidal silica. These results show promise for using chemically stable chlorosodalite to immobilize oxide reduction salt wastes.

Immobilization of LiCl-Li2O pyroprocessing salt wastes in chlorosodalite using glass-bonded hydrothermal and salt-occlusion methods

Science.gov (United States)

Riley, Brian J.; Peterson, Jacob A.; Kroll, Jared O.; Frank, Steven M.

2018-04-01

In this study, hydrothermal and salt-occlusion processes were used to make chlorosodalite through reactions with a high-LiCl salt simulating a waste stream generated from pyrochemical treatment of oxide-based used nuclear fuel. Some products were reacted with glass binders to increase chlorosodalite yield through alkali ion exchange and to aid in densification. Hydrothermal processes included reaction of the salt simulant in an autoclave with either zeolite 4A or sodium aluminate and colloidal silica. Chlorosodalite yields in the crystalline products were nearly complete in the glass-bonded materials at values of 100 mass% for the salt-occlusion method, up to 99.0 mass% for the hydrothermal synthesis with zeolite 4A, and up to 96 mass% for the hydrothermal synthesis with sodium aluminate and colloidal silica. These results show promise for using chemically stable chlorosodalite to immobilize oxide reduction salt wastes.

Size effect in barium titanate powders synthesized by different hydrothermal methods

International Nuclear Information System (INIS)

Sun Weian

2006-01-01

The size effect in barium titanate (BaTiO 3 ) was investigated both experimentally and theoretically. Tetragonal BaTiO 3 powders with average sizes from 80 to 420 nm were directly prepared by different hydrothermal methods. The tetragonality of the hydrothermal BaTiO 3 decreased with decreasing particle size, which exhibited a dependence on the synthesis method. A phenomenological model for the size effect was proposed to interpret the experimental observations. The influence of the defects, mainly the lattice hydroxyl, on the size effect was investigated to understand the correlation between the size effect and synthesis condition. The permittivities of BaTiO 3 powder at different particle sizes were calculated, which predicted a maximum permittivity of over 16 000 around the room-temperature critical size of ∼70 nm. The prediction was in good accordance with the experimental data reported recently

Hydrothermal simulation experiments as a tool for studies of the origin of life on Earth and other terrestrial planets: a review.

Science.gov (United States)

Holm, Nils G; Andersson, Eva

2005-08-01

The potential of life's origin in submarine hydrothermal systems has been evaluated by a number of investigators by conducting high temperature-high pressure experiments involving organic compounds. In the majority of these experiments little attention has been paid to the importance of constraining important parameters, such as the pH and the redox state of the system. This is particularly revealed in the apparent difficulties in interpreting experimental data from hydrothermal organic synthesis and stability studies. However, in those cases where common mineral assemblages have been used in an attempt to buffer the pH and redox conditions to geologically and geochemically realistic values, theoretical and experimental data seem to converge. The use of mineral buffer assemblages provides a convenient way by which to constrain the experimental conditions. Studies at high temperatures and pressure in the laboratory have revealed a number of reactions that proceed rapidly in hydrothermal fluids, including the Strecker synthesis of amino acids. In other cases, the verification of postulated abiotic reaction mechanisms has not been possible, at least for large molecules such as large fatty acids and hydrocarbons. This includes the Fischer-Tropsch synthesis reaction. High temperature-high pressure experimental methods have been developed and used successfully for a long time in, for example, mineral solubility studies under hydrothermal conditions. By taking advantage of this experimental experience new and, at times, unexpected directions can be taken in bioorganic geochemistry, one being, for instance, primitive two-dimensional information coding. This article critically reviews some of the organic synthesis and stability experiments that have been conducted under simulated submarine hydrothermal conditions. We also discuss some of the theoretical and practical considerations that apply to hydrothermal laboratory studies of organic molecules related to the origin of

Electrochemistry in supercritical fluids

Science.gov (United States)

Branch, Jack A.; Bartlett, Philip N.

2015-01-01

A wide range of supercritical fluids (SCFs) have been studied as solvents for electrochemistry with carbon dioxide and hydrofluorocarbons (HFCs) being the most extensively studied. Recent advances have shown that it is possible to get well-resolved voltammetry in SCFs by suitable choice of the conditions and the electrolyte. In this review, we discuss the voltammetry obtained in these systems, studies of the double-layer capacitance, work on the electrodeposition of metals into high aspect ratio nanopores and the use of metallocenes as redox probes and standards in both supercritical carbon dioxide–acetonitrile and supercritical HFCs. PMID:26574527

Polyvinylpyrrolidone (PVP)-assisted hydrothermal synthesis of luminescent YVO4:Eu3+ microspheres

International Nuclear Information System (INIS)

Wang Juan; Xu Yunhua; Hojamberdiev, Mirabbos; Wang Mingqiong; Zhu Gangqiang

2010-01-01

Spherical YVO 4 :Eu 3+ microstructures were hydrothermally synthesized by the reaction of NH 4 VO 3 , Y 2 O 3 , and Eu 2 O 3 at 180 deg. C for 24 h with the assistance of polyvinylpyrrolidone (PVP) as a surfactant. The resulting products were characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), and photoluminescence (PL) spectroscopy. The experimental results showed that ball-like YVO 4 :Eu 3+ microspheres with a diameter of about 4-5 μm, corresponding to the SEM observations, formed at 180 deg. C for 24 h using 0.2 g PVP with the molecular weight of 20,000 g mol -1 . The amount of PVP and the reaction time of hydrothermal processing were found to play a key role in the formation of YVO 4 :Eu 3+ microspheres. It has been observed that the relative luminescence intensities of the as-synthesized samples increased with increasing hydrothermal reaction times due mainly to the increase of crystallinity.

Supercritical synthesis and in situ deposition of PbS nanocrystals with oleic acid passivation for quantum dot solar cells

Energy Technology Data Exchange (ETDEWEB)

Tavakoli, M.M. [Department of Materials Science and Engineering, Sharif University of Technology, 14588 Tehran (Iran, Islamic Republic of); Simchi, A., E-mail: simchi@sharif.edu [Department of Materials Science and Engineering, Sharif University of Technology, 14588 Tehran (Iran, Islamic Republic of); Institute for Nanoscience and Nanotechnology, Sharif University of Technology, 14588 Tehran (Iran, Islamic Republic of); Aashuri, H. [Department of Materials Science and Engineering, Sharif University of Technology, 14588 Tehran (Iran, Islamic Republic of)

2015-04-15

Colloidal quantum dot solar cells have recently attracted significant attention due to their low-processing cost and surging photovoltaic performance. In this paper, a novel, reproducible, and simple solution-based process based on supercritical fluid toluene is presented for in situ growth and deposition PbS nanocrystals with oleic-acid passivation. A lead precursor containing sulfur was mixed with oleic acid in toluene and processed in a supercritical fluid condition at different temperatures of 140, 270 and 330 °C for 20 min. The quantum dots were deposited on a fluorine-doped tin oxide glass substrate inside the supercritical reactor. Transmission electron microscopy, X-ray diffraction, absorption and dynamic light scattering showed that the nanocrystals processed at the supercritical condition (330 °C) are fully crystalline with a narrow size distribution of ∼3 nm with an absorption wavelength of 915 nm (bandgap of 1.3 eV). Fourier transform infrared spectroscopy indicated that the PbS quantum dots are passivated by oleic acid molecules during the growth. Photovoltaic characteristics of Schottky junction solar cells showed an improvement over devices prepared by spin-coating. - Highlights: • Supercritical fluid processing and in situ deposition of PbS QDs are presented. • The prepared nanocrystals are mono-dispersed with an optical bandgap of 1.3 eV. • Photovoltaic performance of the in situ deposited nanocrystals is reported. • An improved PV performance compared to spin coated Schottky solar cells is shown.

Geochemical constraints on chemolithoautotrophic reactions in hydrothermal systems

Science.gov (United States)

Shock, Everett L.; McCollom, Thomas; Schulte, Mitchell D.

1995-06-01

Thermodynamic calculations provide the means to quantify the chemical disequilibrium inherent in the mixing of redeuced hydrothermal fluids with seawater. The chemical energy available for metabolic processes in these environments can be evaluated by taking into account the pressure and temperature dependence of the apparent standard Gibbs free energies of reactions in the S-H2-H2O system together with geochemical constraints on pH, activities of aqueous sulfur species and fugacities of H2 and/or O2. Using present-day mixing of hydrothermal fluids and seawater as a starting point, it is shown that each mole of H2S entering seawater from hydrothermal fluids represents about 200,000 calories of chemical energy for metabolic systems able to catalyze H2S oxidation. Extrapolating to the early Earth, which was likely to have had an atmosphere more reduced than at present, shows that this chemical energy may have been a factor of two or so less. Nevertheless, mixing of hydrothermal fluids with seawater would have been an abundant source of chemical energy, and an inevitable consequence of the presence of an ocean on an initially hot Earth. The amount of energy available was more than enough for organic synthesis from CO2 or CO, and/or polymer formation, indicating that the vicinity of hydrothermal systems at the sea floor was an ideal location for the emergence of the first chemolithoautotrophic metabolic systems.

Gasification of fruit wastes and agro-food residues in supercritical water

International Nuclear Information System (INIS)

Nanda, Sonil; Isen, Jamie; Dalai, Ajay K.; Kozinski, Janusz A.

2016-01-01

Highlights: • Supercritical water gasification of various fruit wastes and agro-food residues. • Coconut shell had superior carbon content and calorific value due to high lignin. • Maximum H_2 yields at 600 °C with 1:10 biomass-to-water ratio, 45 min and 23–25 MPa. • High H_2 yields from coconut shell, bagasse and aloe vera rind with 2 wt% K_2CO_3. • High CH_4 yields from coconut shell with 2 wt% NaOH due to methanation reaction. - Abstract: Considerable amounts of fruit wastes and agro-food residues are generated worldwide as a result of food processing. Converting the bioactive components (e.g., carbohydrates, lipids, fats, cellulose, hemicellulose and lignin) in food wastes to biofuels is a potential remediation approach. This study highlights the characterization and hydrothermal conversion of several fruit wastes and agro-food residues such as aloe vera rind, banana peel, coconut shell, lemon peel, orange peel, pineapple peel and sugarcane bagasse to hydrogen-rich syngas through supercritical water gasification. The agro-food wastes were gasified in supercritical water to study the impacts of temperature (400–600 °C), biomass-to-water ratio (1:5 and 1:10) and reaction time (15–45 min) at a pressure range of 23–25 MPa. The catalytic effects of NaOH and K_2CO_3 were also investigated to maximize the hydrogen yields and selectivity. The elevated temperature (600 °C), longer reaction time (45 min) and lower feed concentration (1:10 biomass-to-water ratio) were optimal for higher hydrogen yield (0.91 mmol/g) and total gas yield (5.5 mmol/g) from orange peel. However, coconut shell with 2 wt% K_2CO_3 at 600 °C and 1:10 biomass-to-water ratio for 45 min revealed superior hydrogen yield (4.8 mmol/g), hydrogen selectivity (45.8%) and total gas yield (15 mmol/g) with enhanced lower heating value of the gas product (1595 kJ/Nm"3). The overall findings suggest that supercritical water gasification of fruit wastes and agro-food residues could serve as

Hydrothermal synthesis of PEDOT/rGO composite for supercapacitor applications

Science.gov (United States)

Ahmed, Sultan; Rafat, M.

2018-01-01

In this study, PEDOT/rGO composite has been successfully synthesized using hydrothermal method. Precursor solution of EDOT monomer was mixed with a predetermined solution of graphene oxide (GO). The resultant mixture was then hydrothermally treated. Surface morphology, crystal structure vibrational response and thermal stability have been studied using standard characterization techniques: field-emission scanning electron microscopy, X-ray diffraction, Raman spectroscopy and thermo-gravimetric analysis. The observed results confirm that the required composite of PEDOT/rGO has indeed been synthesized. Electrochemical properties of the synthesized product were studied in 6 M KOH aqueous solution, using characterization techniques such as: cyclic voltammetry, electrochemical impedance spectroscopy and galvanostatic charge-discharge measurements. The results show a high value of specific capacitance (102.8 F g-1) at 10 mV s-1, indicating that the composite can be profitably used for energy storage devices.

Supercritical Water Gasification of Biomass in a Ceramic Reactor: Long-Time Batch Experiments

Directory of Open Access Journals (Sweden)

Daniele Castello

2017-10-01

Full Text Available Supercritical water gasification (SCWG is an emerging technology for the valorization of (wet biomass into a valuable fuel gas composed of hydrogen and/or methane. The harsh temperature and pressure conditions involved in SCWG (T > 375 °C, p > 22 MPa are definitely a challenge for the manufacturing of the reactors. Metal surfaces are indeed subject to corrosion under hydrothermal conditions, and expensive special alloys are needed to overcome such drawbacks. A ceramic reactor could be a potential solution to this issue. Finding a suitable material is, however, complex because the catalytic effect of the material can influence the gas yield and composition. In this work, a research reactor featuring an internal alumina inlay was utilized to conduct long-time (16 h batch tests with real biomasses and model compounds. The same experiments were also conducted in batch reactors made of stainless steel and Inconel 625. The results show that the three devices have similar performance patterns in terms of gas production, although in the ceramic reactor higher yields of C2+ hydrocarbons were obtained. The SEM observation of the reacted alumina surface revealed a good resistance of such material to supercritical conditions, even though some intergranular corrosion was observed.

Supercritical fluid extraction of bi & multi-layer graphene sheets from graphite by using exfoliation technique

Science.gov (United States)

Xavier, Gauravi; Dave, Bhoomi; Khanna, Sakshum

2018-05-01

In recent times, researchers have turned to explore the possibility of using Supercritical Fluid (SCFs) system to penetrate into the inert-gaping of graphite and exfoliate it into a number of layer graphene sheets. The supercritical fluid holds excellent wetting surfaces with low interfacial tension and high diffusion coefficients. Although SCFs exfoliation approach looks promising to developed large scale & low-cost graphene sheet but has not received much attention. To arouse interest and reflection on this approach, this review is organized to summarize the recent progress in graphene production by SCF technology. Here we present the simplest route to obtained layers of graphene sheets by intercalating and exfoliating graphite using supercritical CO2 processing. The layers graphene nano-sheets were collected in dichloromethane (DCM) solution which prevents the restocking of sheets. The obtained graphene sheets show the desired characteristics and thus can be used in physical, chemical and biological sciences. Thus this method provides an effortless and eco-friendly approach for the synthesis of layers of graphene sheets.

Review on plasmas in extraordinary media: plasmas in cryogenic conditions and plasmas in supercritical fluids

Science.gov (United States)

Stauss, Sven; Muneoka, Hitoshi; Terashima, Kazuo

2018-02-01

Plasma science and technology has enabled advances in very diverse fields: micro- and nanotechnology, chemical synthesis, materials fabrication and, more recently, biotechnology and medicine. While many of the currently employed plasma tools and technologies are very advanced, the types of plasmas used in micro- and nanofabrication pose certain limits, for example, in treating heat-sensitive materials in plasma biotechnology and plasma medicine. Moreover, many physical properties of plasmas encountered in nature, and especially outer space, i.e. very-low-temperature plasmas or plasmas that occur in high-density media, are not very well understood. The present review gives a short account of laboratory plasmas generated under ’extreme’ conditions: at cryogenic temperatures and in supercritical fluids. The fundamental characteristics of these cryogenic plasmas and cryoplasmas, and plasmas in supercritical fluids, especially supercritical fluid plasmas, are presented with their main applications. The research on such exotic plasmas is expected to lead to further understanding of plasma physics and, at the same time, enable new applications in various technological fields.

Synthesis and characterization of hexagonal nano-sized nickel selenide by simple hydrothermal method assisted by CTAB

Energy Technology Data Exchange (ETDEWEB)

Sobhani, Azam [Department of Inorganic Chemistry, Faculty of Chemistry, University of Kashan, Kashan, P.O. Box 87317-51167 (Iran, Islamic Republic of); Davar, Fatemeh [Institute of Nano Science and Nano Technology, University of Kashan, Kashan, P.O. Box 87317-51167 (Iran, Islamic Republic of); Salavati-Niasari, Masoud, E-mail: salavati@kashanu.ac.ir [Department of Inorganic Chemistry, Faculty of Chemistry, University of Kashan, Kashan, P.O. Box 87317-51167 (Iran, Islamic Republic of); Institute of Nano Science and Nano Technology, University of Kashan, Kashan, P.O. Box 87317-51167 (Iran, Islamic Republic of)

2011-07-01

Nano-sized nickel selenide powders have been successfully synthesized via an improved hydrothermal route based on the reaction between NiCl{sub 2}.6H{sub 2}O, SeCl{sub 4} and hydrazine (N{sub 2}H{sub 4}.H{sub 2}O) in water, in present of cetyltrimethyl ammonium bromide (CTAB) as surfactant, at various conditions. The products were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy and X-ray energy dispersive spectroscopy analysis. Effects of temperature, reaction time and reductant agent on the morphology, the particle sizes and the phase of the final products have been investigated. It was found that the phase and morphology of the products could be greatly influenced by these parameters. The synthesis procedure is simple and uses less toxic reagents than the previously reported methods. Photoluminescence (PL) was used to study the optical properties of NiSe samples.

Synthesis of indium oxide cubic crystals by modified hydrothermal route for application in room temperature flexible ethanol sensors

International Nuclear Information System (INIS)

Seetha, M.; Meena, P.; Mangalaraj, D.; Masuda, Yoshitake; Senthil, K.

2012-01-01

Highlights: ► For the first time HMT is used in the preparation of indium oxide. ► HMT itself acts as base for the precursor and results in cubic indium hydroxide. ► Modified hydrothermal route used for the preparation of cubic indium oxide crystals. ► As a new approach a composite film synthesized with prepared indium oxide. ► Film showed good response to ethanol vapours with quick response and recovery times. - Abstract: Indium oxide cubic crystals were prepared by using hexamethylenetetramine and indium chloride without the addition of any structure directing agents. The chemical route followed in the present work was a modified hydrothermal synthesis. The average crystallite size of the prepared cubes was found to be 40 nm. A blue emission at 418 nm was observed at room temperature when the sample was excited with a 380 nm Xenon lamp. This emission due to oxygen vacancies made the material suitable for gas sensing applications. The synthesized material was made as a composite film with polyvinyl alcohol which was more flexible than the films prepared on glass substrates. This flexible film was used as a sensing element and tested with ethanol vapours at room temperature. The film showed fast response as well as recovery to ethanol vapours with a sensor response of about 1.4 for 100 ppm of the gas.

Size-controlled synthesis of NiFe{sub 2}O{sub 4} nanospheres via a PEG assisted hydrothermal route and their catalytic properties in oxidation of alcohols by periodic acid

Energy Technology Data Exchange (ETDEWEB)

Paul, Bappi; Purkayastha, Debraj Dhar; Dhar, Siddhartha Sankar, E-mail: ssd_iitg@hotmail.com

2016-05-01

Graphical abstract: - Highlights: • Hydrothermal synthesis of NiFe{sub 2}O{sub 4} NPs with (C{sub 4}H{sub 9}){sub 3}N as hydroxylating agent. • PEG 4000 was used as surfactant to control sizes of NPs. • The TEM images revealed the material to be spherical in shape with sizes 2–10 nm. • NiFe{sub 2}O{sub 4} was used as recyclable catalyst for oxidation of alcohols by periodic acid. - Abstract: A novel and facile approach for synthesis of spinel nickel ferrites (NiFe{sub 2}O{sub 4}) nanoparticles (NPs) employing homogeneous chemical precipitation followed by hydrothermal heating is reported. The synthesis involves use of tributylamine (TBA) as a hydroxylating agent in synthesis of nickel ferrites. Polyethylene glycol (PEG) 4000 was used as surfactant. As-synthesized NiFe{sub 2}O{sub 4} NPs were characterized by powder X-ray diffraction (XRD), transmission electron microscopy (TEM), N{sub 2} adsorption–desorption isotherm (BET) and vibrating sample magnetometry (VSM). The XRD pattern revealed formation of cubic face-centered NiFe{sub 2}O{sub 4} and TEM image showed spherical particles of sizes 2–10 nm. These NiFe{sub 2}O{sub 4} NPs were used as magnetically recoverable catalyst in oxidation of cyclic alcohols to their corresponding aldehydes by periodic acid. This eco-friendly procedure affords products in very high yield and selectivity. The reusability of the catalyst is proved to be noteworthy as the material exhibits no significant changes in its catalytic activity even after five cycles of reuse.

Hydrothermal synthesis and characterization of a two-dimensional piperazinium cobalt–zinc phosphate via a metastable one-dimensional phase

Energy Technology Data Exchange (ETDEWEB)

Torre-Fernández, Laura; Khainakova, Olena A. [Departamentos de Química Física y Analítica y Química Orgánica e Inorgánica, Universidad de Oviedo-CINN, 33006 Oviedo (Spain); Espina, Aránzazu [Servicios Científico Técnicos, Universidad de Oviedo, 33006 Oviedo (Spain); Amghouz, Zakariae, E-mail: amghouz.uo@uniovi.es [Servicios Científico Técnicos, Universidad de Oviedo, 33006 Oviedo (Spain); Khainakov, Sergei A. [Servicios Científico Técnicos, Universidad de Oviedo, 33006 Oviedo (Spain); Alfonso, Belén F.; Blanco, Jesús A. [Departamento de Física, Universidad de Oviedo, 33007 Oviedo (Spain); García, José R.; García-Granda, Santiago [Departamentos de Química Física y Analítica y Química Orgánica e Inorgánica, Universidad de Oviedo-CINN, 33006 Oviedo (Spain)

2015-05-15

A two-dimensional piperazinium cobalt–zinc phosphate, formulated as (C{sub 4}N{sub 2}H{sub 12}){sub 1.5}(Co{sub 0.6}Zn{sub 0.4}){sub 2}(HPO{sub 4}){sub 2}(PO{sub 4})·H{sub 2}O (2D), was synthesized under hydrothermal conditions. The crystal structure was determined using single-crystal X-ray diffraction data (monoclinic P2{sub 1}/c, a=8.1165(3) Å, b=26.2301(10) Å, c=8.3595(4) Å, and β=110.930(5)°) and the hydrogen atom positions were optimized by DFT calculations. A single-crystal corresponding to one-dimensional metastable phase, (C{sub 4}N{sub 2}H{sub 12})Co{sub 0.3}Zn{sub 0.7}(HPO{sub 4}){sub 2}·H{sub 2}O (1D), was also isolated and the crystal structure was determined (monoclinic P2{sub 1}/c, a=8.9120(6) Å, b=14.0290(1) Å, c=12.2494(5) Å, and β=130.884(6)°). The bulk was characterized by chemical (C–H–N) analysis, powder X-ray diffraction (PXRD), powder X-ray thermodiffractometry (HT-XRD), transmission electron microscopy (STEM(DF)-EDX and EFTEM), and thermal analysis (TG/SDTA-MS), including activation energy data of its thermal decomposition. The magnetic susceptibility and magnetization measurements show no magnetic ordering down to 4 K. - Graphical abstract: Hydrothermal synthesis and structural characterization of a two-dimensional piperazinium cobalt–zinc phosphate, (C{sub 4}N{sub 2}H{sub 12}){sub 1.5}(Co{sub 0.6}Zn{sub 0.4}){sub 2}(HPO{sub 4}){sub 2}(PO{sub 4})·H{sub 2}O (2D), have been reported. The crystal structure of a one-dimensional piperazinium cobalt–zinc phosphate, (C{sub 4}N{sub 2}H{sub 12})Co{sub 0.3}Zn{sub 0.7}(HPO{sub 4}){sub 2}·H{sub 2}O (1D) a metastable phase during the hydrothermal synthesis, was also determined. The thermal behavior of 2D compound is strongly dependent on the selected heating rate and the magnetic susceptibility and magnetization measurements show no magnetic ordering down to 4 K. - Highlights: • A 2D piperazinium cobalt–zinc phosphate has been synthesized and characterized. • Crystal

Hydrothermal synthesis of CdWO 4 nanorods and their ...

African Journals Online (AJOL)

CdWO4 nanorods with wolframite structure were synthesized in the presence of the surfactant SDBS by a hydrothermal method, and characterized by a variety of techniques. The obtained products are CdWO4 nanorods with length of 0.8–2.5 μm and width of 50–250 nm. The surfactant SDBS plays a key role in the ...

Crystalline hydroxyapatite coatings synthesized under hydrothermal conditions on modified titanium substrates

International Nuclear Information System (INIS)

Suchanek, Katarzyna; Bartkowiak, Amanda; Gdowik, Agnieszka; Perzanowski, Marcin; Kąc, Sławomir; Szaraniec, Barbara; Suchanek, Mateusz; Marszałek, Marta

2015-01-01

Hydroxyapatite coatings were successfully produced on modified titanium substrates via hydrothermal synthesis in a Ca(EDTA) 2− and (NH 4 ) 2 HPO 4 solution. The morphology of modified titanium substrates as well as hydroxyapatite coatings was studied using scanning electron microcopy and phase identification by X-ray diffraction, and Raman and FTIR spectroscopy. The results show that the nucleation and growth of hydroxyapatite needle-like crystals with hexagonal symmetry occurred only on titanium substrates both chemically and thermally treated. No hydroxyapatite phase was detected on only acid etched Ti metal. This finding demonstrates that only a particular titanium surface treatment can effectively induce the apatite nucleation under hydrothermal conditions. - Highlights: • Bioactivation of titanium substrate by chemical and heat treatments • Precipitation of hydroxyapatite on modified titanium plates • Hydrothermal crystallization of hydroxyapatite by chelate decomposition method

Crystalline hydroxyapatite coatings synthesized under hydrothermal conditions on modified titanium substrates

Energy Technology Data Exchange (ETDEWEB)

Suchanek, Katarzyna, E-mail: Katarzyna.Suchanek@ifj.edu.pl [The Henryk Niewodniczański Institute of Nuclear Physics, Polish Academy of Sciences, Radzikowskiego Street 152, 31-342 Krakow (Poland); Bartkowiak, Amanda [The Henryk Niewodniczański Institute of Nuclear Physics, Polish Academy of Sciences, Radzikowskiego Street 152, 31-342 Krakow (Poland); Gdowik, Agnieszka [Faculty of Physics and Applied Computer Science, AGH University of Science and Technology, Mickiewicza 30, 30-059 Krakow (Poland); Perzanowski, Marcin [The Henryk Niewodniczański Institute of Nuclear Physics, Polish Academy of Sciences, Radzikowskiego Street 152, 31-342 Krakow (Poland); Kąc, Sławomir [Faculty of Metals Engineering and Industrial Computer Science, AGH University of Science and Technology, Mickiewica 30, 30-059 Krakow (Poland); Szaraniec, Barbara [Department of Biomaterials, AGH University of Science and Technology, Mickiewicza 30, 30-059 Krakow (Poland); Suchanek, Mateusz [Department of Chemistry and Physics, University of Agriculture in Krakow, Mickiewicza 21, 31-120 Krakow (Poland); Marszałek, Marta [The Henryk Niewodniczański Institute of Nuclear Physics, Polish Academy of Sciences, Radzikowskiego Street 152, 31-342 Krakow (Poland)

2015-06-01

Hydroxyapatite coatings were successfully produced on modified titanium substrates via hydrothermal synthesis in a Ca(EDTA){sup 2−} and (NH{sub 4}){sub 2}HPO{sub 4} solution. The morphology of modified titanium substrates as well as hydroxyapatite coatings was studied using scanning electron microcopy and phase identification by X-ray diffraction, and Raman and FTIR spectroscopy. The results show that the nucleation and growth of hydroxyapatite needle-like crystals with hexagonal symmetry occurred only on titanium substrates both chemically and thermally treated. No hydroxyapatite phase was detected on only acid etched Ti metal. This finding demonstrates that only a particular titanium surface treatment can effectively induce the apatite nucleation under hydrothermal conditions. - Highlights: • Bioactivation of titanium substrate by chemical and heat treatments • Precipitation of hydroxyapatite on modified titanium plates • Hydrothermal crystallization of hydroxyapatite by chelate decomposition method.

Advanced Thermal Storage for Central Receivers with Supercritical Coolants

Energy Technology Data Exchange (ETDEWEB)

Kelly, Bruce D.

2010-06-15

The principal objective of the study is to determine if supercritical heat transport fluids in a central receiver power plant, in combination with ceramic thermocline storage systems, offer a reduction in levelized energy cost over a baseline nitrate salt concept. The baseline concept uses a nitrate salt receiver, two-tank (hot and cold) nitrate salt thermal storage, and a subcritical Rankine cycle. A total of 6 plant designs were analyzed, as follows: Plant Designation Receiver Fluid Thermal Storage Rankine Cycle Subcritical nitrate salt Nitrate salt Two tank nitrate salt Subcritical Supercritical nitrate salt Nitrate salt Two tank nitrate salt Supercritical Low temperature H2O Supercritical H2O Two tank nitrate salt Supercritical High temperature H2O Supercritical H2O Packed bed thermocline Supercritical Low temperature CO2 Supercritical CO2 Two tank nitrate salt Supercritical High temperature CO2 Supercritical CO2 Packed bed thermocline Supercritical Several conclusions have been drawn from the results of the study, as follows: 1) The use of supercritical H2O as the heat transport fluid in a packed bed thermocline is likely not a practical approach. The specific heat of the fluid is a strong function of the temperatures at values near 400 °C, and the temperature profile in the bed during a charging cycle is markedly different than the profile during a discharging cycle. 2) The use of supercritical CO2 as the heat transport fluid in a packed bed thermocline is judged to be technically feasible. Nonetheless, the high operating pressures for the supercritical fluid require the use of pressure vessels to contain the storage inventory. The unit cost of the two-tank nitrate salt system is approximately $24/kWht, while the unit cost of the high pressure thermocline system is nominally 10 times as high. 3) For the supercritical fluids, the outer crown temperatures of the receiver tubes are in the range of 700 to 800 °C. At temperatures of 700 °C and above

Technology with Supercritical Fluid. Part 2. Applications

International Nuclear Information System (INIS)

Marongiu, B.; De Giorgi, M. R.; Porcedda, S.; Cadoni, E.

1998-01-01

The present article is based on a bibliographical analysis of the main applications of the supercritical fluid in various fields, as: extraction from solid matrices, division of liquid charges, chromatography HPLC with supercritical eluent, chemical and biochemical reactions in supercritical solvents etc [it

Supercritical transitiometry of polymers.

Science.gov (United States)

Randzio, S L; Grolier, J P

1998-06-01

Employing supercritical fluids (SCFs) during polymers processing allows the unusual properties of SCFs to be exploited for making polymer products that cannot be obtained by other means. A new supercritical transitiometer has been constructed to permit study of the interactions of SCFs with polymers during processing under well-defined conditions of temperature and pressure. The supercritical transitiometer allows pressure to be exerted by either a supercritical fluid or a neutral medium and enables simultaneous determination of four basic parameters of a transition, i.e., p, T, Δ(tr)H and Δ(tr)V. This permits determination of the SCF effect on modification of the polymer structure at a given pressure and temperature and defines conditions to allow reproducible preparation of new polymer structures. Study of a semicrystalline polyethylene by this method has defined conditions for preparation of new microfoamed phases with good mechanical properties. The low densities and microporous structures of the new materials may make them useful for applications in medicine, pharmacy, or the food industry, for example.

Effect of process parameters on hydrothermal liquefaction of oil palm biomass for bio-oil production and its life cycle assessment

International Nuclear Information System (INIS)

Chan, Yi Herng; Yusup, Suzana; Quitain, Armando T.; Tan, Raymond R.; Sasaki, Mitsuru; Lam, Hon Loong; Uemura, Yoshimitsu

2015-01-01

Highlights: • Water is used as a clean solvent to liquefy palm biomass to bio-oil. • The optimum liquefaction condition of oil palm biomass is 390 °C and 25 MPa. • Optimum reaction time for liquefaction of empty fruit bunch and palm mesocarp fiber is 120 min. • Optimum reaction time for liquefaction of palm kernel shell is 240 min. • From the life cycle assessment, a net 2.29 kg CO 2 equivalent is generated per kg of bio-oil produced. - Abstract: This paper presents the studies on the effect of three process parameters; temperature, pressure and reaction time on the subcritical and supercritical hydrothermal liquefaction of oil palm empty fruit bunch, palm mesocarp fiber and palm kernel shell. The effect of temperature (330–390 °C), pressure (25–35 MPa) and reaction time (30–240 min) on bio-oil yields were investigated using a Inconel batch reactor. The optimum liquefaction condition for empty fruit bunch, palm mesocarp fiber and palm kernel shell was at supercritical condition of water; 390 °C and 25 MPa. For the effect of reaction time, bio-oil from empty fruit bunch and palm mesocarp fiber attained maximum yields at 120 min, whereas bio-oil yield from palm kernel shell continued to increase at reaction time of 240 min. Lastly, a life cycle assessment based on a conceptual biomass hydrothermal liquefaction process for bio-oil production was constructed and presented

Pressure drop and friction factor correlations of supercritical flow

International Nuclear Information System (INIS)

Fang Xiande; Xu Yu; Su Xianghui; Shi Rongrong

2012-01-01

Highlights: ► Survey and evaluation of friction factor models for supercritical flow. ► Survey of experimental study of supercritical flow. ► New correlation of friction factor for supercritical flow. - Abstract: The determination of the in-tube friction pressure drop under supercritical conditions is important to the design, analysis and simulation of transcritical cycles of air conditioning and heat pump systems, nuclear reactor cooling systems and some other systems. A number of correlations for supercritical friction factors have been proposed. Their accuracy and applicability should be examined. This paper provides a comprehensive survey of experimental investigations into the pressure drop of supercritical flow in the past decade and a comparative study of supercritical friction factor correlations. Our analysis shows that none of the existing correlations is completely satisfactory, that there are contradictions between the existing experimental results and thus more elaborate experiments are needed, and that the tube roughness should be considered. A new friction factor correlation for supercritical tube flow is proposed based on 390 experimental data from the available literature, including 263 data of supercritical R410A cooling, 45 data of supercritical R404A cooling, 64 data of supercritical carbon dioxide (CO 2 ) cooling and 18 data of supercritical R22 heating. Compared with the best existing model, the new correlation increases the accuracy by more than 10%.

Degradation Characteristics of Wood Using Supercritical Alcohols

Directory of Open Access Journals (Sweden)

Jeeban Poudel

2012-11-01

Full Text Available In this work, the characteristics of wood degradation using supercritical alcohols have been studied. Supercritical ethanol and supercritical methanol were used as solvents. The kinetics of wood degradation were analyzed using the nonisothermal weight loss technique with heating rates of 3.1, 9.8, and 14.5 °C/min for ethanol and 5.2, 11.3, and 16.3 °C/min for methanol. Three different kinetic analysis methods were implemented to obtain the apparent activation energy and the overall reaction order for wood degradation using supercritical alcohols. These were used to compare with previous data for supercritical methanol. From this work, the activation energies of wood degradation in supercritical ethanol were obtained as 78.0–86.0, 40.1–48.1, and 114 kJ/mol for the different kinetic analysis methods used in this work. The activation energies of wood degradation in supercritical ethanol were obtained as 78.0–86.0, 40.1–48.1, and 114 kJ/mol. This paper also includes the analysis of the liquid products obtained from this work. The characteristic analysis of liquid products on increasing reaction temperature and time has been performed by GC-MS. The liquid products were categorized according to carbon numbers and aromatic/aliphatic components. It was found that higher conversion in supercritical ethanol occurs at a lower temperature than that of supercritical methanol. The product analysis shows that the majority of products fall in the 2 to 15 carbon number range.

Influence of Hydrothermal Treatment on Physicochemical Properties and Drug Release of Anti-Inflammatory Drugs of Intercalated Layered Double Hydroxide Nanoparticles

Directory of Open Access Journals (Sweden)

Zi Gu

2014-05-01

Full Text Available The synthesis method of layered double hydroxides (LDHs determines nanoparticles’ performance in biomedical applications. In this study, hydrothermal treatment as an important synthesis technique has been examined for its influence on the physicochemical properties and the drug release rate from drug-containing LDHs. We synthesised MgAl–LDHs intercalated with non-steroidal anti-inflammatory drugs (i.e., naproxen, diclofenac and ibuprofen using a co-precipitation method with or without hydrothermal treatment (150 °C, 4 h. After being hydrothermally treated, LDH–drug crystallites increased in particle size and crystallinity, but did not change in the interlayer anion orientation, gallery height and chemical composition. The drug release patterns of all studied LDH–drug hybrids were biphasic and sustained. LDHs loaded with diclofenac had a quicker drug release rate compared with those with naproxen and ibuprofen, and the drug release from the hydrothermally-treated LDH–drug was slower than the freshly precipitated LDH–drug. These results suggest that the drug release of LDH–drugs is influenced by the crystallite size of LDHs, which can be controlled by hydrothermal treatment, as well as by the drug molecular physicochemical properties.

Preparation of meta-stable phases of barium titanate by Sol-hydrothermal method

Directory of Open Access Journals (Sweden)

Mahalakshmi Selvaraj

2015-11-01

Full Text Available Two low-cost chemical methods of sol–gel and the hydrothermal process have been strategically combined to fabricate barium titanate (BaTiO3 nanopowders. This method was tested for various synthesis temperatures (100 °C to 250 °C employing barium dichloride (BaCl2 and titanium tetrachloride (TiCl4 as precursors and sodium hydroxide (NaOH as mineralizer for synthesis of BaTiO3 nanopowders. The as-prepared BaTiO3 powders were investigated for structural characteristics using x-ray diffraction (XRD, scanning electron microscopy (SEM and transmission electron microscopy (TEM. The overall analysis indicates that the hydrothermal conditions create a gentle environment to promote the formation of crystalline phase directly from amorphous phase at the very low processing temperatures investigated. XRD analysis showed phase transitions from cubic - tetragonal - orthorhombic - rhombohedral with increasing synthesis temperature and calculated grain sizes were 34 – 38 nm (using the Scherrer formula. SEM and TEM analysis verified that the BaTiO3 nanopowders synthesized by this method were spherical in shape and about 114 - 170 nm in size. The particle distribution in both SEM and TEM shows that as the reaction temperature increases from 100 °C to 250 °C, the particles agglomerate. Selective area electron diffraction (SAED shows that the particles are crystalline in nature. The study shows that choosing suitable precursor and optimizing pressure and temperature; different meta-stable (ferroelectric phases of undoped BaTiO3 nanopowders can be stabilized by the sol-hydrothermal method.

One-step, simple, and green synthesis of tin dioxide/graphene nanocomposites and their application to lithium-ion battery anodes

International Nuclear Information System (INIS)

Jiang, Zaixing; Zhang, Dongjie; Li, Yue; Cheng, Hao; Wang, Mingqiang; Wang, Xueqin; Bai, Yongping; Lv, Haibao; Yao, Yongtao; Shao, Lu; Huang, Yudong

2014-01-01

Highlights: • A one-step, simple and green approach to synthesis SnO 2 /graphene nanocomposites was proposed using a supercritical CO 2 method. • The SnO 2 /graphene nanocomposites was used as an anode, which exhibit extreme high lithium storage capacity and well cycling performance. - Abstract: Graphene with extraordinary thermal, mechanical and electrical properties offers possibilities in a variety of applications. Recent advances in the synthesis of graphene composites using supercritical fluids are highlighted. Supercritical fluids exhibit unique features for the synthesis of composites due to its low viscosity, high diffusivity, near-zero surface tension, and tunability. Here, we report the preparation of tin dioxide (SnO 2 )/graphene nanocomposite through supercritical CO 2 method. It demonstrates that the SnO 2 nanoparticles are homogeneously dispersed on the surface of graphene sheets with a particle size of 2.3–2.6 nm. The SnO 2 /graphene nanocomposites exhibit higher lithium storage capacity and better cycling performance compared to that of the similar CNT nanocomposites. The reported synthetic procedure is straightforward, green and inexpensive. And it may be readily adopted to produce large quantities of graphene based nanocomposites

Urea controlled hydrothermal synthesis of ammonium aluminum carbonate hydroxide rods

Science.gov (United States)

Wang, Fang; Zhu, Jianfeng; Liu, Hui

2018-03-01

In this study, ammonium aluminum carbonate hydroxide (AACH) rods were controllably prepared using the hydrothermal method by manipulating the amount of urea in the reaction system. The experimental results showed that AACH in rod shape was able to be gradually transformed from γ-AlOOH in cluster shape during the molar ratios of urea to Al in the reactants were ranged from 8 to 10, and the yield of AACH has increased accordingly. When the molar ratio of urea to Al reaches 11, pure AACH rods with a diameter of 500 nm and a length of 10 μm approximately was able to be produced. Due to the slow decomposition of urea during the hydrothermal reaction, the nucleation and growth of AACH crystal proceed step by step. Therefore, the crystal can fully grow on each crystal plane and eventually produce a highly crystalline rod-shaped product. The role of urea in controlling the morphology and yield of AACH was also discussed in this paper systematically.

Supercritical fluids in ionic liquids

NARCIS (Netherlands)

Kroon, M.C.; Peters, C.J.; Plechkova, N.V.; Seddon, K.R.

2014-01-01

Ionic liquids and supercritical fluids are both alternative environmentally benign solvents, but their properties are very different. Ionic liquids are non-volatile but often considered highly polar compounds, whereas supercritical fluids are non-polar but highly volatile compounds. The combination

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.

Hydrothermal Liquefaction of Biomass

Energy Technology Data Exchange (ETDEWEB)

Elliott, Douglas C.

2010-12-10

Hydrothermal liquefaction technology is describes in its relationship to fast pyrolysis of biomass. The scope of work at PNNL is discussed and some intial results are presented. HydroThermal Liquefaction (HTL), called high-pressure liquefaction in earlier years, is an alternative process for conversion of biomass into liquid products. Some experts consider it to be pyrolysis in solvent phase. It is typically performed at about 350 C and 200 atm pressure such that the water carrier for biomass slurry is maintained in a liquid phase, i.e. below super-critical conditions. In some applications catalysts and/or reducing gases have been added to the system with the expectation of producing higher yields of higher quality products. Slurry agents ('carriers') evaluated have included water, various hydrocarbon oils and recycled bio-oil. High-pressure pumping of biomass slurry has been a major limitation in the process development. Process research in this field faded away in the 1990s except for the HydroThermal Upgrading (HTU) effort in the Netherlands, but has new resurgence with other renewable fuels in light of the increased oil prices and climate change concerns. Research restarted at Pacific Northwest National Laboratory (PNNL) in 2007 with a project, 'HydroThermal Liquefaction of Agricultural and Biorefinery Residues' with partners Archer-Daniels-Midland Company and ConocoPhillips. Through bench-scale experimentation in a continuous-flow system this project investigated the bio-oil yield and quality that could be achieved from a range of biomass feedstocks and derivatives. The project was completed earlier this year with the issuance of the final report. HydroThermal Liquefaction research continues within the National Advanced Biofuels Consortium with the effort focused at PNNL. The bench-scale reactor is being used for conversion of lignocellulosic biomass including pine forest residue and corn stover. A complementary project is an international

Hydrothermal synthesis of tungsten doped tin dioxide nanocrystals

Science.gov (United States)

Zhou, Cailong; Li, Yufeng; Chen, Yiwen; Lin, Jing

2018-01-01

Tungsten doped tin dioxide (WTO) nanocrystals were synthesized through a one-step hydrothermal method. The structure, composition and morphology of WTO nanocrystals were characterized by x-ray diffraction, x-ray photoelectron spectroscopy, energy dispersive x-ray spectroscopy, UV-vis diffuse reflectance spectra, zeta potential analysis and high-resolution transmission electron microscopy. Results show that the as-prepared WTO nanocrystals were rutile-type structure with the size near 13 nm. Compared with the undoped tin dioxide nanocrystals, the WTO nanocrystals possessed better dispersity in ethanol phase and formed transparent sol.

Controlled synthesis of La1−xSrxCrO3 nanoparticles by hydrothermal method with nonionic surfactant and their ORR activity in alkaline medium

International Nuclear Information System (INIS)

Choi, Bo Hyun; Park, Shin-Ae; Park, Bong Kyu; Chun, Ho Hwan; Kim, Yong-Tae

2013-01-01

Graphical abstract: We demonstrate that Sr-doped LaCrO 3 nanoparticles were successfully prepared by the hydrothermal synthesis method using the nonionic surfactant Triton X-100 and the applicability of La 1−x Sr x CrO 3 to oxygen reduction reaction (ORR) electrocatalysis in an alkaline medium. Compared with the nanoparticles synthesized by the coprecipitation method, they showed enhanced ORR activity. - Highlights: • Sr-doped LaCrO 3 nanoparticles were successfully prepared by the hydrothermal method using the nonionic surfactant. • Homogeneously shaped and sized Sr-doped LaCrO 3 nanoparticles were readily obtained. • Compared with the nanoparticles synthesized by the coprecipitation method, they showed an enhanced ORR activity. • The main origin was revealed to be the decreased particle size due to the nonionic surfactant. - Abstract: Sr-doped LaCrO 3 nanoparticles were prepared by the hydrothermal method with the nonionic surfactant Triton X-100 followed by heat treatment at 1000 °C for 10 h. The obtained perovskite nanoparticles had smaller particle size (about 100 nm) and more uniform size distribution than those synthesized by the conventional coprecipitation method. On the other hand, it was identified with the material simulation that the electronic structure change by Sr doping was negligible, because the initially unfilled e g -band was not affected by the p-type doping. Finally, the perovskite nanoparticles synthesized by hydrothermal method showed much higher ORR activity by over 200% at 0.8 V vs. RHE than those by coprecipitation method

Supercritical fluid chromatography

Science.gov (United States)

Vigdergauz, M. S.; Lobachev, A. L.; Lobacheva, I. V.; Platonov, I. A.

1992-03-01

The characteristic features of supercritical fluid chromatography (SCFC) are examined and there is a brief historical note concerning the development of the method. Information concerning the use of supercritical fluid chromatography in the analysis of objects of different nature is presented in the form of a table. The roles of the mobile and stationary phases in the separation process and the characteristic features of the apparatus and of the use of the method in physicochemical research are discussed. The bibliography includes 364 references.

Correlation of supercritical-fluid extraction recoveries with supercritical-fluid chromatographic retention data: A fundamental study

NARCIS (Netherlands)

Lou, X.W.; Janssen, J.G.M.; Cramers, C.A.M.G.

1995-01-01

The possibility of using supercritical-fluid chromatographic retention data for examining the effects of operational parameters, such as pressure and flow rate, on the extraction characteristics in supercritical-fluid extraction (SFE) was investigated. A model was derived for calculating the

Hydrothermal synthesis spherical TiO{sub 2} and its photo-degradation property on salicylic acid

Energy Technology Data Exchange (ETDEWEB)

Guo Wenlu, E-mail: liu287856624@163.com [School of Biology and Chemical Engineering, Jiangsu University of Science and Technology, Mengxi Road 2, Zhenjiang 212003 (China); Liu Xiaolin [School of Biology and Chemical Engineering, Jiangsu University of Science and Technology, Mengxi Road 2, Zhenjiang 212003 (China); Huo Pengwei; Gao Xun; Wu Di; Lu Ziyang; Yan Yongsheng [School of Chemistry and Chemical Engineering, Jiangsu University, Zhenjiang 212013 (China)

2012-07-01

Anatase TiO{sub 2} spheres have been prepared using hydrothermal synthesis. The prepared spheres were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM) and UV-vis diffuse reflectance spectra (UV-vis DRS). The TiO{sub 2} consisted of well-defined spheres with size of 3-5 {mu}m. The photocatalytic activity of spherical TiO{sub 2} was determined by degradation of salicylic acid under visible light irradiation. It was revealed that the degradation rate of the spherical TiO{sub 2} which was processed at 150 Degree-Sign C for 48 h could reach 81.758%. And the kinetics of photocatalytic degradation obeyed first-order kinetic, which the rate constant value was 0.01716 S{sup -1} of the salicylic acid onto TiO{sub 2} (temperature: 150, time: 48 h). The kinetics of adsorption followed the pseudo-second-order model and the rate constant was 1.2695 g mg{sup -1} of the salicylic acid onto TiO{sub 2} (temperature: 150, time: 48 h).

Hydrothermal synthesis, crystal structures, and enantioselective adsorption property of bis(L-histidinato)nickel(II) monohydrate

Science.gov (United States)

Ramos, Christian Paul L.; Conato, Marlon T.

2018-05-01

Despite the numerous researches in metal-organic frameworks (MOFs), there are only few reports on biologically important amino acids, histidine in particular, on its use as bridging ligand in the construction of open-framework architectures. In this work, hydrothermal synthesis was used to prepare a compound based on Ni2+ and histidine. The coordination assembly of imidazole side chain of histidine with divalent nickel ions in aqueous condition yielded purple prismatic solids. Single crystal X-ray diffraction (XRD) analysis of the product revealed structure for Ni(C6H8N3O2)2 • H2O that has a monoclinic (C2) structure with lattice parameters, a = 29.41, b = 8.27, c = 6.31 Å, β = 90.01 ˚. Circular dichroism - optical rotatory dispersion (CD-ORD), Powder X-ray diffraction (PXRD) and Fourier transform - infrared spectroscopy (FT-IR) analyses are conducted to further characterize the crystals. Enantioselective adsorption analysis using racemic mixture of 2-butanol confirmed bis(L-histidinato)nickel(II) monohydrate MOF crystal's enantioselective property preferentially favoring the adsorption of (S)-2-butanol isomer.

MZnFe{sub 2}O{sub 4} (M = Ni, Mn) cubic superparamagnetic nanoparticles obtained by hydrothermal synthesis

Energy Technology Data Exchange (ETDEWEB)

Freire, R. M. [Universidade Federal do Ceara-UFC, Grupo de Quimica de Materiais Avancados (GQMAT)- Departamento de Quimica Analitica e Fisico-Quimica (Brazil); Ribeiro, T. S.; Vasconcelos, I. F. [Universidade Federal do Ceara, Departamento de Engenharia Metalurgica e de Materiais (Brazil); Denardin, J. C. [Universidad de Santiago de Chile, USACH, Departamento de Fisica (Chile); Barros, E. B. [Universidade Federal do Ceara-UFC, Departamento de Fisica (Brazil); Mele, Giuseppe [Universita del Salento, Dipartimento di Ingegneria dell' Innovazione (Italy); Carbone, L. [IPCF-CNR, UOS Pisa (Italy); Mazzetto, S. E.; Fechine, P. B. A., E-mail: fechine@ufc.br [Universidade Federal do Ceara-UFC, Grupo de Quimica de Materiais Avancados (GQMAT)- Departamento de Quimica Analitica e Fisico-Quimica (Brazil)

2013-05-15

MZnFe{sub 2}O{sub 4} (M = Ni or Mn) cubic nanoparticles have been prepared by hydrothermal synthesis in mild conditions and short time without any procedure of calcinations. The structural and magnetic properties of the mixed ferrites were investigated by X-ray diffraction, Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, Moessbauer spectroscopy, vibrating sample magnetometer, and Transmission electron microscopy (TEM). X-ray analysis showed peaks characteristics of the spinel phase. The average diameter of the nanoparticles observed by TEM measurements was approximately between 4 and 10 nm. Spectroscopy study of the spinel structure was performed based on Group Theory. The predicted bands were observed in FTIR and Raman spectrum. The magnetic parameters and Moessbauer spectroscopy were measured at room temperature and superparamagnetic behavior was observed for mixed ferrites. This kind of nanoparticles can be used as precursor in drug delivery systems, magnetic hyperthermia, ferrofluids, or magnetic imaging contrast agents.

Hydrothermal synthesis and characteristic photoluminescence of Er-doped SnO{sub 2} nanoparticles

Energy Technology Data Exchange (ETDEWEB)

Tuan, Pham Van; Hieu, Le Trung; Nga, La Quynh [International Training Institute for Materials Science, Hanoi University of Science and Technology, No.1, Dai Co Viet, Hanoi (Viet Nam); Dung, Nguyen Duc [Advanced Institute of Science and Technology, Hanoi University of Science and Technology, No.1, Dai Co Viet, Hanoi (Viet Nam); Ha, Ngo Ngoc [International Training Institute for Materials Science, Hanoi University of Science and Technology, No.1, Dai Co Viet, Hanoi (Viet Nam); Khiem, Tran Ngoc, E-mail: khiem@itims.edu.vn [International Training Institute for Materials Science, Hanoi University of Science and Technology, No.1, Dai Co Viet, Hanoi (Viet Nam)

2016-11-15

We report the characteristic photoluminescence (PL) spectra of erbium ion (Er{sup 3+})-doped tin dioxide (SnO{sub 2})nanoparticles. The materials were prepared via hydrothermal method at 180 °C with in 20 h by using various Er{sup 3+} ion concentrations ranging from 0.0 to 1.0 at%. After the synthesis, the materials were characterized through X-ray diffraction and high-resolution transmission electron microscopy. Crystallite SnO{sub 2} and its average particle diameter of approximately 5 nm did not change with Er{sup 3+} ion dopant concentration. Photoluminescence spectra showed the characteristic light emission from the Er{sup 3+} ions. The PL excitation spectra referred to an efficient energy transfer to Er{sup 3+} ions in the presence of SnO{sub 2}nanoparticles. The most intense Er-related emission of SnO{sub 2}:Er{sup 3+} nanoparticles in near infrared region was found in samples containing an Er{sup 3+} ion concentration of 0.25 at%. Although the absorption bandgaps of the materials were identified at approximately 3.8 eV, we found that efficient excitation comes with low excitation energy band edge. Excitation is possibly involved in shallow defects in SnO{sub 2} nanoparticles.

Hydrothermal synthesis of zeolite T from kaolin using two different structure-directing agents

Science.gov (United States)

Arshad, Sazmal E.; Lutfor Rahman, M.; Sarkar, Shaheen M.; Yusslee, Eddy F.; Patuwan, Siti Z.

2018-01-01

Zeolite T was synthesized from the molar chemical composition of 1SiO2:0.04Al2O3:0.26Na2O:0.09K2O:14H2O in the form of a homogenous milky solution in the presence of the two different structure-directing agents TMAOH and TEAOH respectively. Modification of the composition of silica was undertaken using metakaolin from calcined kaolin at 750 °C for 4 h, while the molar composition of each different SDA was variated from 0.05, 0.10, 0.15, 0.20 and 0.25. The homogenous mixture was left at room temperature for 24 h before undergoing hydrothermal synthesis at 100 °C for 168 h. The synthesized samples were filtered and aged at 120 °C for 2 h and each sample was calcined at high temperatures (545 °C for TMAOH and 520 °C for TEAOH) for template removal before characterization using XRD and SEM. Crystallization of the zeolite T in its major form only took place at a molar ratio of 0.10 of TMAOH, while TEAOH showed the species evolution of zeolite T into zeolite L and W for other molar ratios.

Synthesis of indium oxide cubic crystals by modified hydrothermal route for application in room temperature flexible ethanol sensors

Energy Technology Data Exchange (ETDEWEB)

Seetha, M., E-mail: seetha.phy@gmail.com [Department of Physics, SRM University, Kattankulathur, Kancheepuram Dt 603 203 (India); Meena, P. [Department of Physics, PSGR Krishnammal College for Women, Coimbatore 641 046 (India); Mangalaraj, D., E-mail: dmraj800@yahoo.com [DRDO-BU Centre for Life Sciences, Bharathiar University Campus, Coimbatore (India); Department of Nanoscience and Technology, Bharathiar University, Coimbatore 641 014 (India); Masuda, Yoshitake [National Institute of Advanced Industrial Science and Technology (AIST), Nagoya 463-8560 (Japan); Senthil, K. [School of Advanced Materials Science and Engineering, Sungkyunkwan University (Suwon Campus), Cheoncheon-dong 300, Jangan-gu, Suwon 440-746 (Korea, Republic of)

2012-03-15

Highlights: Black-Right-Pointing-Pointer For the first time HMT is used in the preparation of indium oxide. Black-Right-Pointing-Pointer HMT itself acts as base for the precursor and results in cubic indium hydroxide. Black-Right-Pointing-Pointer Modified hydrothermal route used for the preparation of cubic indium oxide crystals. Black-Right-Pointing-Pointer As a new approach a composite film synthesized with prepared indium oxide. Black-Right-Pointing-Pointer Film showed good response to ethanol vapours with quick response and recovery times. - Abstract: Indium oxide cubic crystals were prepared by using hexamethylenetetramine and indium chloride without the addition of any structure directing agents. The chemical route followed in the present work was a modified hydrothermal synthesis. The average crystallite size of the prepared cubes was found to be 40 nm. A blue emission at 418 nm was observed at room temperature when the sample was excited with a 380 nm Xenon lamp. This emission due to oxygen vacancies made the material suitable for gas sensing applications. The synthesized material was made as a composite film with polyvinyl alcohol which was more flexible than the films prepared on glass substrates. This flexible film was used as a sensing element and tested with ethanol vapours at room temperature. The film showed fast response as well as recovery to ethanol vapours with a sensor response of about 1.4 for 100 ppm of the gas.

Nonionic emulsion-mediated synthesis of zeolite beta

Indian Academy of Sciences (India)

Zeolite beta synthesis was first carried out in a newly developed emulsion system containing nonionic polyoxyethylated alkylphenol surfactant, which showed interesting non-conventional features. Compared to the conventional hydrothermal synthesis of zeolite beta, the reported nonionic emulsion system showed a faster ...

Hydrothermal formation and characterization of magnesium oxysulfate whiskers

International Nuclear Information System (INIS)

Xiang, L.; Liu, F.; Li, J.; Jin, Y.

2004-01-01

Magnesium oxysulfate (5Mg(OH) 2 ·MgSO 4 ·3H 2 O) whiskers with a diameter of 0.2-1.0 μm and a length of 20-50 μm were synthesized via the hydrothermal treatment of the slurry formed by mixing the MgSO 4 and NaOH solutions at room temperature. The composition, morphology, structure and thermal behavior of the hydrothermal products were examined with X-ray powder diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), thermo-gravimetric analysis (TGA) and chemical analysis. The experimental results indicated that the process parameters, such as the concentration of the reactant, the dispersion of the Mg(OH) 2 slurry and the temperature in hydrothermal treatment should be controlled carefully to synthesis 5Mg(OH) 2 ·MgSO 4 ·3H 2 O whiskers and to avoid the formation of the sectorial or granular impurities. 5Mg(OH) 2 ·MgSO 4 ·3H 2 O whiskers were decomposed gradually and converted finally to MgO particles after being heated in air at temperature up to 1050 deg. C. Granular products formed if the heating temperature was above 320 deg. C

Hydrothermal Liquefaction of Dried Distillers Grains with solubles: A reaction temperature study

DEFF Research Database (Denmark)

Mørup, Anders; Christensen, Per Runge; Aarup, David Friis

2012-01-01

provides rapid heating of biomass feeds and the option of performing multiple sequential repetitions. This bypasses long, uncontrollable temperature gradients and unintended changes in the reaction chemistry. The product, a crude bio-oil, was characterized in terms of yield, elemental composition......The effect of the reaction temperature on hydrothermal liquefaction of dried distillers grains with solubles (DDGS) was investigated using a novel stop-flow reactor system at varying temperatures (300–400 °C), fixed pressure (250 bar), and fixed reaction time (15 min). The stop-flow reactor......, and chemical composition. Higher reaction temperatures resulted in improved bio-oil yields, less char formation, and higher heating values of the bio-oil. A supercritical reaction temperature of 400 °C was found to produce bio-oil in the highest yields and of the best quality....

Drying of supercritical carbon dioxide with membrane processes

NARCIS (Netherlands)

Lohaus, Theresa; Scholz, Marco; Koziara, Beata; Benes, Nieck Edwin; Wessling, Matthias

2015-01-01

In supercritical extraction processes regenerating the supercritical fluid represents the main cost constraint. Membrane technology has potential for cost efficient regeneration of water-loaded supercritical carbon dioxide. In this study we have designed membrane-based processes to dehydrate

Supercritical water natural circulation flow stability experiment research

Energy Technology Data Exchange (ETDEWEB)

Ma, Dongliang; Zhou, Tao; Li, Bing [North China Electric Power Univ., Beijing (China). School of Nuclear Science and Engineering; North China Electric Power Univ., Beijing (China). Inst. of Nuclear Thermalhydraulic Safety and Standardization; North China Electric Power Univ., Beijing (China). Beijing Key Lab. of Passive Safety Technology for Nuclear Energy; Huang, Yanping [Nuclear Power Institute of China, Chengdu (China). Science and Technology on Reactor System Design Technology Lab.

2017-12-15

The Thermal hydraulic characteristics of supercritical water natural circulation plays an important role in the safety of the Generation-IV supercritical water-cooled reactors. Hence it is crucial to conduct the natural circulation heat transfer experiment of supercritical water. The heat transfer characteristics have been studied under different system pressures in the natural circulation systems. Results show that the fluctuations in the subcritical flow rate (for natural circulation) is relatively small, as compared to the supercritical flow rate. By increasing the heating power, it is observed that the amplitude (and time period) of the fluctuation tends to become larger for the natural circulation of supercritical water. This tends to show the presence of flow instability in the supercritical water. It is possible to observe the flow instability phenomenon when the system pressure is suddenly reduced from the supercritical pressure state to the subcritical state. At the test outlet section, the temperature is prone to increase suddenly, whereas the blocking effect may be observed in the inlet section of the experiment.

Hydrothermal synthesis of ZnSe:Cu quantum dots and their luminescent mechanism study by first-principles

Energy Technology Data Exchange (ETDEWEB)

Liang, Qingshuang; Bai, Yijia; Han, Lin; Deng, Xiaolong [State Key Laboratory of Rare Earth Resources Utilization, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, Changchun 130022 (China); Graduate School, Chinese Academy of Sciences, Beijing 10049 (China); Wu, Xiaojie [State Key Laboratory of Rare Earth Resources Utilization, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, Changchun 130022 (China); Wang, Zhongchang [WPI Research Center, Advanced Institute for Materials Research, Tohoku University, 2-1-1 Katahira, Aoba-ku, Sendai 980-8577 (Japan); Liu, Xiaojuan, E-mail: lxjuan@ciac.jl.cn [State Key Laboratory of Rare Earth Resources Utilization, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, Changchun 130022 (China); Meng, Jian, E-mail: jmeng@ciac.jl.cn [State Key Laboratory of Rare Earth Resources Utilization, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, Changchun 130022 (China)

2013-11-15

An one-pot synthesis of aqueous ZnSe:Cu nanocrystals (NCs) is realized in aqueous solution by a facile yet efficient hydrothermal technique. The dopant emission spectrum of the NCs is tunable, spanning a wide range from 438 to 543 nm. Room-temperature quantum yield for the NCs prepared at the optimal conditions reaches as high as 20% without any post-treatment. The ZnSe:Cu NCs prepared in a neutral aqueous solution (pH=8) are remarkably stable and exhibit comparatively high photoluminescent quantum yield (PL QY) as high as 17%. First-principles pseudopotential calculations using plane-wave basis functions have been performed. The formation energies of copper ions occupied in the interstitial octahedron and substitutional tetrahedral Zn{sup 2+} sites have been calculated. The occupation of copper ions in the interstitial octahedral site is found to be more thermodynamics-facilitated by −0.98 eV. The density of state analysis indicates that the Cu-related emission is primary dominated by the substitutional tetrahedral Cu ions, and the large dopant related emission width of ZnSe:Cu NCs originated from the corresponding Cu 3d impurity band. Highlights: • One-pot synthesis of aqueous ZnSe:Cu nanocrystals with tunable emission and high QY%. • ZnSe:Cu NCs exhibit high QY% at neutral pH suitable for biological application. • The microscopic mechanism underlying Cu-related emission has been provided.

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.

n-Type Conductivity of Cu2O Thin Film Prepared in Basic Aqueous Solution Under Hydrothermal Conditions

Science.gov (United States)

Ursu, Daniel; Miclau, Nicolae; Miclau, Marinela

2018-03-01

We report for the first time in situ hydrothermal synthesis of n-type Cu2O thin film using strong alkaline solution. The use of copper foil as substrate and precursor material, low synthesis temperature and short reaction time represent the arguments of a new, simple, inexpensive and high field synthesis method for the preparation of n-type Cu2O thin film. The donor concentration of n-type Cu2O thin film obtained at 2 h of reaction time has increased two orders of magnitude than previous reported values. We have demonstrated n-type conduction in Cu2O thin film prepared in strong alkaline solution, in the contradiction with the previous works. Based on experimental results, the synthesis mechanism and the origin of n-type photo-responsive behavior of Cu2O thin film were discussed. We have proposed that the unexpected n-type character could be explained by H doping of Cu2O thin film in during of the hydrothermal synthesis that caused the p-to-n conductivity-type conversion. Also, this work raises new questions about the origin of n-type conduction in Cu2O thin film, the influence of the synthesis method on the nature of the intrinsic defects and the electrical conduction behavior.

Argentine hydrothermal panorama

Energy Technology Data Exchange (ETDEWEB)

1976-12-01

An attempt is made to give a realistic review of Argentine thermal waters. The topics discussed are the characteristics of the hydrothermal resources, classification according to their mineral content, hydrothermal flora and fauna, uses of hydrothermal resources, hydrothermal regions of Argentina, and meteorology and climate. A tabulation is presented of the principal thermal waters. (JSR)

Sol-gel/hydrothermal synthesis of mixed metal oxide of Titanium and ...

African Journals Online (AJOL)

Mixed metal oxides of titanium and zinc nanocomposites were prepared through sol-gel method under hydrothermal condition using titanium oxy-(1, 2 - pentadione) and zinc acetate without hazardous additives. The resulting composites were characterized by X-Ray Diffractometer (XRD), Scanning Electron Microscope ...

Effects of Supercritical Environment on Hydrocarbon-fuel Injection

Institute of Scientific and Technical Information of China (English)

Bongchul Shin; Dohun Kim; Min Son; Jaye Koo

2017-01-01

In this study,the effects of environment conditions on decane were investigated.Decane was injected in subcritical and supercritical ambient conditions.The visualization chamber was pressurized to 1.68 MPa by using nitrogen gas at a temperature of 653 K for subcritical ambient conditions.For supercritical ambient conditions,the visualization chamber was pressurized to 2.52 MPa by using helium at a temperature of 653 K.The decane injection in the pressurized chamber was visualized via a shadowgraph technique and gradient images were obtained by a post processing method.A large variation in density gradient was observed at jet interface in the case of subcritical injection in subcritical ambient conditions.Conversely,for supercritical injection in supercritical ambient conditions,a small density gradient was observed at the jet interface.In a manner similar to that observed in other cases,supercritical injection in subcritical ambient conditions differed from supercritical ambient conditions such as sphere shape liquid.Additionally,there were changes in the interface,and the supercritical injection core width was thicker than that in the subcritical injection.Furthermore,in cases with the same injection conditions,the change in the supercritical ambient normalized core width was smaller than the change in the subcritical ambient normalized core width owing to high specific heat at the supercritical injection and small phase change at the interface.Therefore,the interface was affected by the changing ambient condition.Given that the effect of changing the thermodynamic properties of propellants could be essential for a variable thrust rocket engine,the effects of the ambient conditions were investigated experimentally.

Effects of supercritical environment on hydrocarbon-fuel injection

Science.gov (United States)

Shin, Bongchul; Kim, Dohun; Son, Min; Koo, Jaye

2017-04-01

In this study, the effects of environment conditions on decane were investigated. Decane was injected in subcritical and supercritical ambient conditions. The visualization chamber was pressurized to 1.68 MPa by using nitrogen gas at a temperature of 653 K for subcritical ambient conditions. For supercritical ambient conditions, the visualization chamber was pressurized to 2.52 MPa by using helium at a temperature of 653 K. The decane injection in the pressurized chamber was visualized via a shadowgraph technique and gradient images were obtained by a post processing method. A large variation in density gradient was observed at jet interface in the case of subcritical injection in subcritical ambient conditions. Conversely, for supercritical injection in supercritical ambient conditions, a small density gradient was observed at the jet interface. In a manner similar to that observed in other cases, supercritical injection in subcritical ambient conditions differed from supercritical ambient conditions such as sphere shape liquid. Additionally, there were changes in the interface, and the supercritical injection core width was thicker than that in the subcritical injection. Furthermore, in cases with the same injection conditions, the change in the supercritical ambient normalized core width was smaller than the change in the subcritical ambient normalized core width owing to high specific heat at the supercritical injection and small phase change at the interface. Therefore, the interface was affected by the changing ambient condition. Given that the effect of changing the thermodynamic properties of propellants could be essential for a variable thrust rocket engine, the effects of the ambient conditions were investigated experimentally.

Hydrothermal synthesis of MnO2/CNT nanocomposite with a CNT core/porous MnO2 sheath hierarchy architecture for supercapacitors

Science.gov (United States)

Xia, Hui; Wang, Yu; Lin, Jianyi; Lu, Li

2012-01-01

MnO2/carbon nanotube [CNT] nanocomposites with a CNT core/porous MnO2 sheath hierarchy architecture are synthesized by a simple hydrothermal treatment. X-ray diffraction and Raman spectroscopy analyses reveal that birnessite-type MnO2 is produced through the hydrothermal synthesis. Morphological characterization reveals that three-dimensional hierarchy architecture is built with a highly porous layer consisting of interconnected MnO2 nanoflakes uniformly coated on the CNT surface. The nanocomposite with a composition of 72 wt.% (K0.2MnO2·0.33 H2O)/28 wt.% CNT has a large specific surface area of 237.8 m2/g. Electrochemical properties of the CNT, the pure MnO2, and the MnO2/CNT nanocomposite electrodes are investigated by cyclic voltammetry and electrochemical impedance spectroscopy measurements. The MnO2/CNT nanocomposite electrode exhibits much larger specific capacitance compared with both the CNT electrode and the pure MnO2 electrode and significantly improves rate capability compared to the pure MnO2 electrode. The superior supercapacitive performance of the MnO2/CNT nancomposite electrode is due to its high specific surface area and unique hierarchy architecture which facilitate fast electron and ion transport.

Mechano-hydrothermal preparation of Li-Al-OH layered double hydroxides

Science.gov (United States)

Zhang, Fengrong; Hou, Wanguo

2018-05-01

A mechano-hydrothermal (MHT) method was used to synthesize Li-Al-OH layered double hydroxides (LDHs) from LiOH·H2O, Al(OH)3 and H2O as starting materials. A two-step synthesis was conducted, that is, Al(OH)3 was milled for 1 h, followed by hydrothermal treatment with LiOH·H2O solution. Effects of the LiOH/Al(OH)3 molar ratio (RLi/Al) and hydrothermal temperature (Tht) on the crystallinity, morphology, and composition of the product were examined. The resulting LDHs were characterized by X-ray diffraction, transmission electron microscopy, scanning electron microscopy, Fourier transform infrared, and elemental analyses. The results showed that pre-milling plays a key role in the LDH formation during subsequent hydrothermal treatment. The Li/Al molar ratio of the obtained LDHs keeps constant at 0.5, independent from theRLi/Al (0.5-5.0) in the starting materials. An increase in the Tht (20-80 °C) can enhance the crystallinity and morphology regularity of the products. The so-obtained Li-Al-OH LDHs exhibit high crystallinity and well-dispersity, which may have wider applications than the aggregate ones obtained using conventional mechanochemical and Li+-imbibition methods.

Hydrothermal synthesis and magnetic properties of Mn doped ZnS nanoparticles

Science.gov (United States)

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

2010-01-01

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

Hydrothermal synthesis and magnetic properties of Mn doped ZnS nanoparticles

International Nuclear Information System (INIS)

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

2010-01-01

Nanocrystallite Mn doped Zn 1-X S (X = 0 to 0.4) powders have been synthesized through a hydrothermal route. The effect of the hydrothermal temperature and Mn 2+ ions substitution on the crystal structure, crystallite size, microstructure and magnetic properties were investigated using (XRD), (SEM) and (VSM). The results revealed that wurtzite zinc sulfide phase was formed using thiourea as a sulfur source at temperature 150- 200 o C for 24 h. The crystallite size was (7.9-15.1 nm) was obtained at the same conditions. The doping of Mn 2+ ions decreased the crystallite size of the formed ZnS wurtzite phase was in the range between 7.9 and 3.8 nm. SEM micrographs showed that the produced ZnS and Mn doped ZnS particles were appeared as spherical shape. The magnetic properties were improved by substitution of Mn 2+ ions up to 0.2.

Spherical V-Fe-MCM-48: The Synthesis, Characterization and Hydrothermal Stability.

Science.gov (United States)

Qian, Wang; Wang, Haiqing; Chen, Jin; Kong, Yan

2015-04-14

Spherical MCM-48 mesoporous sieve co-doped with vanadium and iron was successfully synthesized via one-step hydrothermal method. The material was characterized by X-ray diffraction (XRD), nitrogen adsorption-desorption isotherms, inductively coupled plasma (ICP), scanning electron microscopy (SEM), transmission electron microscopy (TEM), diffuse reflectance UV-vis spectra, and X-ray photoelectron spectra (XPS) techniques. Results indicated that the V-Fe-MCM-48 showed an ordered 3D cubic mesostructure with spherical morphology, narrow pore size distribution and high specific surface area. Most of vanadium and iron atoms existing as tetrahedral V 4+ and Fe 3+ species were co-doped into the silicate framework. The particle sizes of V-Fe-MCM-48 were smaller and the specific area was much higher than those of of V-MCM-48. Additionally, the synthesized V-Fe-MCM-48 exhibited improved hydrothermal stability compared with the pure MCM-48.

Sulfur metabolizing microbes dominate microbial communities in Andesite-hosted shallow-sea hydrothermal systems.

Directory of Open Access Journals (Sweden)

Yao Zhang

Full Text Available To determine microbial community composition, community spatial structure and possible key microbial processes in the shallow-sea hydrothermal vent systems off NE Taiwan's coast, we examined the bacterial and archaeal communities of four samples collected from the water column extending over a redoxocline gradient of a yellow and four from a white hydrothermal vent. Ribosomal tag pyrosequencing based on DNA and RNA showed statistically significant differences between the bacterial and archaeal communities of the different hydrothermal plumes. The bacterial and archaeal communities from the white hydrothermal plume were dominated by sulfur-reducing Nautilia and Thermococcus, whereas the yellow hydrothermal plume and the surface water were dominated by sulfide-oxidizing Thiomicrospira and Euryarchaeota Marine Group II, respectively. Canonical correspondence analyses indicate that methane (CH(4 concentration was the only statistically significant variable that explains all community cluster patterns. However, the results of pyrosequencing showed an essential absence of methanogens and methanotrophs at the two vent fields, suggesting that CH(4 was less tied to microbial processes in this shallow-sea hydrothermal system. We speculated that mixing between hydrothermal fluids and the sea or meteoric water leads to distinctly different CH(4 concentrations and redox niches between the yellow and white vents, consequently influencing the distribution patterns of the free-living Bacteria and Archaea. We concluded that sulfur-reducing and sulfide-oxidizing chemolithoautotrophs accounted for most of the primary biomass synthesis and that microbial sulfur metabolism fueled microbial energy flow and element cycling in the shallow hydrothermal systems off the coast of NE Taiwan.

Sulfur metabolizing microbes dominate microbial communities in Andesite-hosted shallow-sea hydrothermal systems.

Science.gov (United States)

Zhang, Yao; Zhao, Zihao; Chen, Chen-Tung Arthur; Tang, Kai; Su, Jianqiang; Jiao, Nianzhi

2012-01-01

To determine microbial community composition, community spatial structure and possible key microbial processes in the shallow-sea hydrothermal vent systems off NE Taiwan's coast, we examined the bacterial and archaeal communities of four samples collected from the water column extending over a redoxocline gradient of a yellow and four from a white hydrothermal vent. Ribosomal tag pyrosequencing based on DNA and RNA showed statistically significant differences between the bacterial and archaeal communities of the different hydrothermal plumes. The bacterial and archaeal communities from the white hydrothermal plume were dominated by sulfur-reducing Nautilia and Thermococcus, whereas the yellow hydrothermal plume and the surface water were dominated by sulfide-oxidizing Thiomicrospira and Euryarchaeota Marine Group II, respectively. Canonical correspondence analyses indicate that methane (CH(4)) concentration was the only statistically significant variable that explains all community cluster patterns. However, the results of pyrosequencing showed an essential absence of methanogens and methanotrophs at the two vent fields, suggesting that CH(4) was less tied to microbial processes in this shallow-sea hydrothermal system. We speculated that mixing between hydrothermal fluids and the sea or meteoric water leads to distinctly different CH(4) concentrations and redox niches between the yellow and white vents, consequently influencing the distribution patterns of the free-living Bacteria and Archaea. We concluded that sulfur-reducing and sulfide-oxidizing chemolithoautotrophs accounted for most of the primary biomass synthesis and that microbial sulfur metabolism fueled microbial energy flow and element cycling in the shallow hydrothermal systems off the coast of NE Taiwan.

Hydrogen production from high-moisture content biomass in supercritical water

Energy Technology Data Exchange (ETDEWEB)

Antal, M.J. Jr.; Adschiri, T.; Ekbom, T. [Univ. of Hawaii, Honolulu, HI (United States)] [and others

1996-10-01

Most hydrogen is produced by steam reforming methane at elevated pressures. The goal of this research is to develop commercial processes for the catalytic steam reforming of biomass and other organic wastes at high pressures. This approach avoids the high cost of gas compression and takes advantage of the unique properties of water at high pressures. Prior to this year the authors reported the ability of carbon to catalyze the decomposition of biomass and related model compounds in supercritical water. The product gas consists of hydrogen, carbon dioxide, carbon monoxide, methane, and traces of higher hydrocarbons. During the past year the authors have: (a) developed a method to extend the catalyst life, (b) begun studies of the role of the shift reaction, (c) completed studies of carbon dioxide absorption from the product effluent by high pressure water, (d) measured the rate of carbon catalyst gasification in supercritical water, (e) discovered the pumpability of oil-biomass slurries, and (f) completed the design and begun fabrication of a flow reactor that will steam reform whole biomass feedstocks (i.e. sewage sludge) and produce a hydrogen rich synthesis gas at very high pressure (>22 MPa).

Study on optimizing ultrasonic irradiation period for thick polycrystalline PZT film by hydrothermal method.

Science.gov (United States)

Ohta, Kanako; Isobe, Gaku; Bornmann, Peter; Hemsel, Tobias; Morita, Takeshi

2013-04-01

The hydrothermal method utilizes a solution-based chemical reaction to synthesize piezoelectric thin films and powders. This method has a number of advantages, such as low-temperature synthesis, and high purity and high quality of the product. In order to promote hydrothermal reactions, we developed an ultrasonic assisted hydrothermal method and confirmed that it produces dense and thick lead-zirconate-titanate (PZT) films. In the hydrothermal method, a crystal growth process follows the nucleation process. In this study, we verified that ultrasonic irradiation is effective for the nucleation process, and there is an optimum irradiation period to obtain thicker PZT films. With this optimization, a 9.2-μm-thick PZT polycrystalline film was obtained in a single deposition process. For this film, ultrasonic irradiation was carried out from the beginning of the reaction for 18 h, followed by a 6 h deposition without ultrasonic irradiation. These results indicate that the ultrasonic irradiation mainly promotes the nucleation process. Copyright © 2012 Elsevier B.V. All rights reserved.

Geothermal energy production with supercritical fluids

Science.gov (United States)

Brown, Donald W.

2003-12-30

There has been invented a method for producing geothermal energy using supercritical fluids for creation of the underground reservoir, production of the geothermal energy, and for heat transport. Underground reservoirs are created by pumping a supercritical fluid such as carbon dioxide into a formation to fracture the rock. Once the reservoir is formed, the same supercritical fluid is allowed to heat up and expand, then is pumped out of the reservoir to transfer the heat to a surface power generating plant or other application.

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.

Crystalline hydroxyapatite coatings synthesized under hydrothermal conditions on modified titanium substrates.

Science.gov (United States)

Suchanek, Katarzyna; Bartkowiak, Amanda; Gdowik, Agnieszka; Perzanowski, Marcin; Kąc, Sławomir; Szaraniec, Barbara; Suchanek, Mateusz; Marszałek, Marta

2015-06-01

Hydroxyapatite coatings were successfully produced on modified titanium substrates via hydrothermal synthesis in a Ca(EDTA)(2-) and (NH4)2HPO4 solution. The morphology of modified titanium substrates as well as hydroxyapatite coatings was studied using scanning electron microcopy and phase identification by X-ray diffraction, and Raman and FTIR spectroscopy. The results show that the nucleation and growth of hydroxyapatite needle-like crystals with hexagonal symmetry occurred only on titanium substrates both chemically and thermally treated. No hydroxyapatite phase was detected on only acid etched Ti metal. This finding demonstrates that only a particular titanium surface treatment can effectively induce the apatite nucleation under hydrothermal conditions. Copyright © 2015 Elsevier B.V. All rights reserved.

Influence of bases on hydrothermal synthesis of titanate nanostructures

CSIR Research Space (South Africa)

Sikhwivhilu, LM

2009-03-01

Full Text Available a hydrothermal process. 14 In this study we report on the effect of base concentration, temperature and base type on the formation of nanotubes which form bundles. New information about the mechanism of the formation of the tubes is provided.... It appeared as though longer tubes were initially formed and then broke into shorter pieces with different sizes. The tube fracture is believed to be due to tube instability in base concentration. This clearly shows that depending on the experimental...

Bio-oil production from biomass via supercritical fluid extraction

Energy Technology Data Exchange (ETDEWEB)

Durak, Halil, E-mail: halildurak@yyu.edu.tr [Yuzuncu Yıl University, Vocational School of Health Services, 65080, Van (Turkey)

2016-04-18

Supercritical fluid extraction is used for producing bio-fuel from biomass. Supercritical fluid extraction process under supercritical conditions is the thermally disruption process of the lignocellulose or other organic materials at 250-400 °C temperature range under high pressure (4-5 MPa). Supercritical fluid extraction trials were performed in a cylindrical reactor (75 mL) in organic solvents (acetone, ethanol) under supercritical conditions with (calcium hydroxide, sodium carbonate) and without catalyst at the temperatures of 250, 275 and 300 °C. The produced liquids at 300 °C in supercritical liquefaction were analyzed and characterized by elemental, GC-MS and FT-IR. 36 and 37 different types of compounds were identified by GC-MS obtained in acetone and ethanol respectively.

Bio-oil production from biomass via supercritical fluid extraction

International Nuclear Information System (INIS)

Durak, Halil

2016-01-01

Supercritical fluid extraction is used for producing bio-fuel from biomass. Supercritical fluid extraction process under supercritical conditions is the thermally disruption process of the lignocellulose or other organic materials at 250-400 °C temperature range under high pressure (4-5 MPa). Supercritical fluid extraction trials were performed in a cylindrical reactor (75 mL) in organic solvents (acetone, ethanol) under supercritical conditions with (calcium hydroxide, sodium carbonate) and without catalyst at the temperatures of 250, 275 and 300 °C. The produced liquids at 300 °C in supercritical liquefaction were analyzed and characterized by elemental, GC-MS and FT-IR. 36 and 37 different types of compounds were identified by GC-MS obtained in acetone and ethanol respectively.

Enhancing power cycle efficiency for a supercritical Brayton cycle power system using tunable supercritical gas mixtures

Science.gov (United States)

Wright, Steven A.; Pickard, Paul S.; Vernon, Milton E.; Radel, Ross F.

2017-08-29

Various technologies pertaining to tuning composition of a fluid mixture in a supercritical Brayton cycle power generation system are described herein. Compounds, such as Alkanes, are selectively added or removed from an operating fluid of the supercritical Brayton cycle power generation system to cause the critical temperature of the fluid to move up or down, depending upon environmental conditions. As efficiency of the supercritical Brayton cycle power generation system is substantially optimized when heat is rejected near the critical temperature of the fluid, dynamically modifying the critical temperature of the fluid based upon sensed environmental conditions improves efficiency of such a system.

Effects of preparation conditions on the ionic conductivity of hydrothermally synthesized Li1+xAlxTi2-x(PO4)3 solid electrolytes

International Nuclear Information System (INIS)

Kim, Kwang Man; Shin, Dong Ok; Lee, Young-Gi

2015-01-01

Li 1+x Al x Ti 2-x (PO 4 ) 3 (LATP) solid electrolytes are prepared by hydrothermal reaction as an effective method to yield moderate ionic conductivity adoptable in actual lithium-ion batteries. Particularly examined in this study are the effects of the synthesis conditions, such as Al dopant concentration (x), hydrothermal reaction time, and calcination and sintering temperatures, on the ionic conductivity of the synthesized LATP. Through repeated synthesis and characterizations of the LATPs by variation of the values of condition variables, the optimum condition for the best LATP with adequate ionic conductivity applicable to actual lithium batteries are determined to be x = 0.3 or 0.4, a hydrothermal reaction time of 12 h, and calcination and sintering temperatures of 600 °C and 900 °C, respectively

Acid-base behavior in hydrothermal processing of wastes. 1998 annual progress report

International Nuclear Information System (INIS)

Johnson, K.P.; Rossky, P.J.

1998-01-01

'A new technology, hydrothermal oxidation (also called supercritical water oxidation), is being developed to treat high level nuclear wastes. Nitrates are reduced to nitrogen; furthermore, phosphates, alumina sludge, and chromium are solubilized, and the sludge is reconstituted as fine oxide particles. A major obstacle to development of this technology has been a lack of scientific knowledge of chemistry in hydrothermal solution above 350 C, particularly acid-base behavior, and transport phenomena, which is needed to understand corrosion, metal-ion complexation, and salt precipitation and recovery. The objective is to provide this knowledge with in-situ UV-vis spectroscopic measurements and fully molecular computer simulation. A major objective of the experimental studies has been to determine the equilibria for Cr(VI) up to 420 C as this is a key species to be removed from nuclear wastes. A wide range of concentrations of KOH and perchloric acid were utilized to manipulate the acid-base equilibria and to understand the effects of ion solvation and ion pairing. The second system is the equilibria between nitric acid, nitrous acid, nitrogen dioxide, nitrite and nitrate ions and oxygen. For both of these systems, chemical equilibria has not been measured previously in hydrothermal solution at these temperatures. On the theoretical side, the authors have focused on the study of the transport properties of aqueous ions in supercritical water. The motivation for these studies is two fold. First, although transport coefficients are fundamental to solution chemistry reaction rates, the behavior of such transport properties over wide ranges of density and temperature are not well established experimentally, particularly at the densities typically of interest (< 0.5 g/cc). Second, due to practical challenges, ionic association equilibria in SCW is typically accessed via measurements of conductivity followed by analysis through a theoretical model that incorporates ion

Hydrothermal synthesis and magnetic properties of Mn doped ZnS nanoparticles

Energy Technology Data Exchange (ETDEWEB)

Rashad, M M; Rayan, D A; El-Barawy, K [Central Metallurgical Research and Development Institute PO Box: 87 Helwan, Cairo (Egypt)

2010-01-01

Nanocrystallite Mn doped Zn{sub 1-X}S (X = 0 to 0.4) powders have been synthesized through a hydrothermal route. The effect of the hydrothermal temperature and Mn{sup 2+} ions substitution on the crystal structure, crystallite size, microstructure and magnetic properties were investigated using (XRD), (SEM) and (VSM). The results revealed that wurtzite zinc sulfide phase was formed using thiourea as a sulfur source at temperature 150- 200{sup o}C for 24 h. The crystallite size was (7.9-15.1 nm) was obtained at the same conditions. The doping of Mn{sup 2+} ions decreased the crystallite size of the formed ZnS wurtzite phase was in the range between 7.9 and 3.8 nm. SEM micrographs showed that the produced ZnS and Mn doped ZnS particles were appeared as spherical shape. The magnetic properties were improved by substitution of Mn{sup 2+} ions up to 0.2.

Synthesis of zinc oxide by microwave hydrothermal method for application to transesterification of soybean oil (biodiesel)

International Nuclear Information System (INIS)

Quirino, Max Rocha; Oliveira, Mateus José C.; Keyson, Davy; Lucena, Guilherme Leocárdio; Oliveira, João Bosco L.; Gama, Lucianna

2017-01-01

ZnO nanostructures were synthesized by microwave hydrothermal treatment using two different mineralization agents (NaOH and NH 4 OH), and were evaluated as catalysts for biodiesel synthesis. The materials were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and Brunauer-Emmett-Teller (BET) surface area analysis. The XRD patterns indicated the formation of the hexagonal wurtzite phase in both samples. SEM analysis showed completely different morphologies based on the mineralization agent employed. The ZnO nanostructures synthesized with NaOH (ZONa5 and ZONa5P) presented plate-like agglomerates, resulting in a quasi-spherical morphology, whereas the materials synthesized with NH 4 OH (ZONH5 and ZONH5P) presented a flower-like morphology. The ZONa5P sample showed an activity of 77.82% for the catalytic conversion of soybean oil into biodiesel by transesterification using methanol. - Highlights: • ZnO was synthesized by MH method in only 5 min. • The powders morphology is completely influenced by mineralization agent. • ZONa5P showed activity of 77.82% for the conversion of soybean oil into biodiesel.

In-Situ Synchrotron Radiation Study of Formation and Growth of Crystalline CexZr1-xO2 Nanoparticles Synthesized in Supercritical Water

DEFF Research Database (Denmark)

Tyrsted, Christoffer; Becker-Christensen, Jacob; Hald, Peter

2010-01-01

-zirconia system, the growth of ceria and zirconia nanoparticles is fundamentally different under supercritical water conditions. For comparison, ex situ synthesis has also been performed using an in-house supercritical flow reactor. The resulting samples were analyzed using PXRD, small-angle X-ray scattering......In situ synchrotron powder X-ray diffraction (PXRD) measurements have been conducted to follow the nucleation and growth of crystalline CexZr1-xO2 nanoparticles synthesized in supercritical water with a full substitution variation (x = 0, 0.2, 0.5, 0.8, and 1.0). Direction-dependent growth curves...... are determined and described using reaction kinetic models. A distinct change in growth kinetics is observed with increasing cerium content. For x = 0.8 and 1.0 (high cerium content), the growth is initially limited by the surface reaction kinetics; however, at a size of ∼6 nm, the growth changes and becomes...

Supercritical Fluids Processing of Biomass to Chemicals and Fuels

Energy Technology Data Exchange (ETDEWEB)

Olson, Norman K. [Iowa State Univ., Ames, IA (United States)

2011-09-28

The main objective of this project is to develop and/or enhance cost-effective methodologies for converting biomass into a wide variety of chemicals, fuels, and products using supercritical fluids. Supercritical fluids will be used both to perform reactions of biomass to chemicals and products as well as to perform extractions/separations of bio-based chemicals from non-homogeneous mixtures. This work supports the Biomass Program’s Thermochemical Platform Goals. Supercritical fluids are a thermochemical approach to processing biomass that, while aligned with the Biomass Program’s interests in gasification and pyrolysis, offer the potential for more precise and controllable reactions. Indeed, the literature with respect to the use of water as a supercritical fluid frequently refers to “supercritical water gasification” or “supercritical water pyrolysis.”

Two planets: Earth and Mars - One salt model: The Hydrothermal SCRIW-Model

Science.gov (United States)

Hovland, M. T.; Rueslaatten, H.; Johnsen, H. K.; Indreiten, T.

2011-12-01

One of the common characteristics of planets Earth and Mars is that both host water (H2O) and large accumulations of salt. Whereas Earth's surface-environment can be regarded as 'water-friendly' and 'salt hostile', the reverse can be said for the surface of Mars. This is because liquid water is stable on Earth, and the atmosphere transports humidity around the globe, whereas on planet Mars, liquid water is unstable, rendering the atmosphere dry and, therefore, 'salt-friendly'. The riddle as to how the salt accumulated in various locations on those two planets is one of long-lasting and great debate. The salt accumulations on Earth are traditionally termed 'evaporites', meaning that they formed by the evaporation of large masses of seawater. How the accumulations on Mars formed is much harder to explain, with a similar model, as surface water, representing a large ocean only existed briefly. Although water molecules and OH-groups may exist in abundance in bound form (crystal water, adsorbed water, etc.), the only place where free water is expected to be stable on Mars is within underground faults, fractures, and crevices. Here it likely occurs as brine or in the form of ice. Based on these conditions, a key to understanding the accumulation of large deposits of salt on both planets is linked to how brines behave in the subsurface when pressurized and heated beyond their supercritical point. At depths greater than about 3 km (i.e., a pressure, P>300 bars) water will no longer boil in a steam phase. Rather, it becomes supercritical and will form a supercritical water 'vapor' (SCRIW) with a specific gravity of typically 0.3 g/cm3. An important characteristic of SCRIW is its inability to dissolve the common sea salts. The salt dissolved in the brines will therefore precipitate as solid particles when brines (seawater on the Earth) move into the supercritical P&T-domain (above 400 C and 300 bars). Numerical modeling of a hydrothermal system in the Atlantis II Deep of the

Transport properties of supercritical carbon dioxide

NARCIS (Netherlands)

Lavanchy, F.; Fourcade, E.; de Koeijer, E.A.; Wijers, J.G.; Meyer, T.; Keurentjes, J.T.F.; Kemmere, M.F.; Meyer, T.

2005-01-01

Recently, supercritical fluids have emerged as more sustainable alternatives for the organic solvents often used in polymer processes. This is the first book emphasizing the potential of supercritical carbon dioxide for polymer processes from an engineering point of view. It develops a

A facile single injection Hydrothermal method for the synthesis of thiol capped CdTe Quantum dots as light harvesters

Energy Technology Data Exchange (ETDEWEB)

Jai Kumar, B.; Sumanth Kumar, D.; Mahesh, H.M., E-mail: hm_mahesh@rediffmail.com

2016-10-15

A facile, Single Injection Hydrothermal (SIH) method has been developed to synthesize high quality 3-Mercaptopropionic Acid (MPA) stabilized aqueous CdTe QDs, entirely in ambient environment. The synthesis protocol eliminates the use of inert atmosphere for reducing elemental Tellurium powder to Te precursor avoiding the oxidation of Te powder. The XRD result revealed that the synthesized QDs are in cubic zincblende type crystalline structure, without signature of Te oxidation. FTIR spectra have confirmed the attachment of short chained organic compound MPA to the surface of QDs by covalent bond. The Quantum confinement effect was clearly evident by shift in Longitudinal Optic (LO) peak of Raman spectra and absorption peak wavelength with respect to bulk CdTe materials. The optical direct band gap energy of CdTe QDs is between 3.63 eV to 1.96 eV and QDs size below 6 nm, confirm the QDs are well under strong Quantum confinement regime. Also, photoluminescence spectra depict a stable and high luminescence emission from green to dark red color. All these results corroborate that the synthesis of CdTe QDs procedure is very advantageous and present a simple, economical and easily up scalable method for large scale production.

Synthesis of Co3O4 nanocubes by hydrothermal route and their ...

Indian Academy of Sciences (India)

2018-02-02

Feb 2, 2018 ... Monodispersed Co3O4 nanocubes were prepared by a simple hydrothermal route with ... X-ray spectrometry, scanning electron microscopy and transmission electron ... spectrometry (EDS) of the product were obtained using.

A Novel Dual-Stage Hydrothermal Flow Reactor

DEFF Research Database (Denmark)

Hellstern, Henrik Christian; Becker, Jacob; Hald, Peter

2015-01-01

The dual-stage reactor is a novel continuous flow reactor with two reactors connected in series. It is designed for hydrothermal flow synthesis of nanocomposites, in which a single particle consists of multiple materials. The secondary material may protect the core nanoparticle from oxidation....... The dual-stage reactor combines the ability to produce advanced materials with an upscaled capacity in excess of 10 g/hour (dry mass). TiO2 was synthesized in the primary reactor and reproduced previous results. The dual-stage capability was succesfully demonstrated with a series of nanocomposites incl. Ti...

Synthesis of Titanium Dioxide nanoparticles via sucrose ester micelle-mediated hydrothermal processing route

International Nuclear Information System (INIS)

Anwar, N.S.; Kassim, A.; Lim, H.N.; Zakarya, S.A.; Huang, N.M.

2010-01-01

Titanium dioxide nanoparticles were synthesized via low-temperature sucrose ester micelle-mediated hydrothermal processing route using titanium isopropoxide as the precursor. X-ray diffractometer revealed that the samples possessed a mixed crystalline phases consisting of anatase and brookite in which anatase was the main phase. Upon increasing the hydrothermal reaction temperature, the degree of crystallinity of the nanoparticles improved and their morphology transformed from bundles of needles to rods and to spheres. Photo catalytic behaviour of the as-synthesized nanoparticles was investigated by photodegradation of methylene blue solution in an ultraviolet A irradiating photo reactor. The as-synthesized nanoparticles exhibited higher photo catalytic performance as compared to the commercial counterpart. (author)

Synthesis of nano-crystalline NiFe2O4 powders in subcritical and supercritical ethanol

Czech Academy of Sciences Publication Activity Database

Ćosović, A.; Žák, Tomáš; Glisić, S.; Sokić, M.; Lazarević, S.; Ćosović, V.; Orlović, A.

2016-01-01

Roč. 113, JUL (2016), s. 96-105 ISSN 0896-8446 R&D Projects: GA MŠk(CZ) ED1.1.00/02.0068 Institutional support: RVO:68081723 Keywords : supercritical * subcritical * nano-crystalline powders * nickel ferrite * metal oxide * magnetic properties Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 2.991, year: 2016

Hydrothermal synthesis, characterization, and thermal properties of alumino silicate azide sodalite, Na8[AlSiO4]6(N3)2

Science.gov (United States)

Borhade, A. V.; Wakchaure, S. G.; Dholi, A. G.; Kshirsagar, T. A.

2017-07-01

First time we report the synthesis, structural characterization and thermal behavior of an unusual N3 - containing alumino-silicate sodalite mineral. Azide sodalite, Na8[AlSiO4]6(N3)2 has been synthesized under hydrothermal conditions at 433 K in steel lined Teflon autoclave. The structural and microstructural properties of azide sodalite mineral was characterized by various methods including FT-IR, XRD, SEM, TGA, and MAS NMR. Crystal structure have been refined by Rietveld method in P\\bar 43n space group, indicating that the N3 - sodalite has cubic in lattice. High temperature study was carried out to see the effect of thermal expansion on cell dimension ( a o) of azide sodalite. Thermal behavior of sodalite was also assessed by thermogravimetric method.

The origin of methanethiol in midocean ridge hydrothermal fluids.

Science.gov (United States)

Reeves, Eoghan P; McDermott, Jill M; Seewald, Jeffrey S

2014-04-15

Simple alkyl thiols such as methanethiol (CH3SH) are widely speculated to form in seafloor hot spring fluids. Putative CH3SH synthesis by abiotic (nonbiological) reduction of inorganic carbon (CO2 or CO) has been invoked as an initiation reaction for the emergence of protometabolism and microbial life in primordial hydrothermal settings. Thiols are also presumptive ligands for hydrothermal trace metals and potential fuels for associated microbial communities. In an effort to constrain sources and sinks of CH3SH in seafloor hydrothermal systems, we determined for the first time its abundance in diverse hydrothermal fluids emanating from ultramafic, mafic, and sediment-covered midocean ridge settings. Our data demonstrate that the distribution of CH3SH is inconsistent with metastable equilibrium with inorganic carbon, indicating that production by abiotic carbon reduction is more limited than previously proposed. CH3SH concentrations are uniformly low (∼10(-8) M) in high-temperature fluids (>200 °C) from all unsedimented systems and, in many cases, suggestive of metastable equilibrium with CH4 instead. Associated low-temperature fluids (<200 °C) formed by admixing of seawater, however, are invariably enriched in CH3SH (up to ∼10(-6) M) along with NH4(+) and low-molecular-weight hydrocarbons relative to high-temperature source fluids, resembling our observations from a sediment-hosted system. This strongly implicates thermogenic interactions between upwelling fluids and microbial biomass or associated dissolved organic matter during subsurface mixing in crustal aquifers. Widespread thermal degradation of subsurface organic matter may be an important source of organic production in unsedimented hydrothermal systems and may influence microbial metabolic strategies in cooler near-seafloor and plume habitats.

Supercritical boiler material selection using fuzzy analytic network process

Directory of Open Access Journals (Sweden)

Saikat Ranjan Maity

2012-08-01

Full Text Available The recent development of world is being adversely affected by the scarcity of power and energy. To survive in the next generation, it is thus necessary to explore the non-conventional energy sources and efficiently consume the available sources. For efficient exploitation of the existing energy sources, a great scope lies in the use of Rankin cycle-based thermal power plants. Today, the gross efficiency of Rankin cycle-based thermal power plants is less than 28% which has been increased up to 40% with reheating and regenerative cycles. But, it can be further improved up to 47% by using supercritical power plant technology. Supercritical power plants use supercritical boilers which are able to withstand a very high temperature (650-720˚C and pressure (22.1 MPa while producing superheated steam. The thermal efficiency of a supercritical boiler greatly depends on the material of its different components. The supercritical boiler material should possess high creep rupture strength, high thermal conductivity, low thermal expansion, high specific heat and very high temperature withstandability. This paper considers a list of seven supercritical boiler materials whose performance is evaluated based on seven pivotal criteria. Given the intricacy and difficulty of this supercritical boiler material selection problem having interactions and interdependencies between different criteria, this paper applies fuzzy analytic network process to select the most appropriate material for a supercritical boiler. Rene 41 is the best supercritical boiler material, whereas, Haynes 230 is the worst preferred choice.

Thermodynamic Optimization of Supercritical CO{sub 2} Brayton Cycles

Energy Technology Data Exchange (ETDEWEB)

Rhim, Dong-Ryul; Park, Sung-Ho; Kim, Su-Hyun; Yeom, Choong-Sub [Institute for Advanced Engineering, Yongin (Korea, Republic of)

2015-05-15

The supercritical CO{sub 2} Brayton cycle has been studied for nuclear applications, mainly for one of the alternative power conversion systems of the sodium cooled fast reactor, since 1960's. Although the supercritical CO{sub 2} Brayton cycle has not been expected to show higher efficiency at lower turbine inlet temperature over the conventional steam Rankine cycle, the higher density of supercritical CO{sub 2} like a liquid in the supercritical region could reduce turbo-machinery sizes, and the potential problem of sodium-water reaction with the sodium cooled fast reactor might be solved with the use of CO{sub 2} instead of water. The supercritical CO{sub 2} recompression Brayton cycle was proposed for the better thermodynamic efficiency than for the simple supercritical CO{sub 2} Brayton cycle. Thus this paper presents the efficiencies of the supercritical CO{sub 2} recompression Brayton cycle along with several decision variables for the thermodynamic optimization of the supercritical CO{sub 2} recompression Brayton cycle. The analytic results in this study show that the system efficiency reaches its maximum value at a compressor outlet pressure of 200 bars and a recycle fraction of 30 %, and the lower minimum temperature approach at the two heat exchangers shows higher system efficiency as expected.

Hydrothermally synthesized PZT film grown in highly concentrated KOH solution with large electromechanical coupling coefficient for resonator

Science.gov (United States)

Feng, Guo-Hua; Lee, Kuan-Yi

2017-12-01

This paper presents a study of lead zirconate titanate (PZT) films hydrothermally grown on a dome-shaped titanium diaphragm. Few articles in the literature address the implementation of hydrothermal PZT films on curved-diaphragm substrates for resonators. In this study, a 50-μm-thick titanium sheet is embossed using balls of designed dimensions to shape a dome-shaped cavity array. Through single-process hydrothermal synthesis, PZT films are grown on both sides of the processed titanium diaphragm with good adhesion and uniformity. The hydrothermal synthesis process involves a high concentration of potassium hydroxide solution and excess amounts of lead acetate and zirconium oxychloride octahydrate. Varied deposition times and temperatures of PZT films are investigated. The grown films are characterized by X-ray diffraction and scanning electron microscopy. The 10-μm-thick PZT dome-shaped resonators with 60- and 20-μm-thick supporting layers are implemented and further tested. Results for both resonators indicate that large electromechanical coupling coefficients and a series resonance of 95 MHz from 14 MHz can be attained. The device is connected to a complementary metal-oxide-semiconductor integrated circuit for analysis of oscillator applications. The oscillator reaches a Q value of 6300 in air. The resonator exhibits a better sensing stability when loaded with water when compared with air.

Partial oxidation of n-hexadecane through decomposition of hydrogen peroxide in supercritical water

KAUST Repository

Alshammari, Y.M.

2015-01-01

© 2014 The Institution of Chemical Engineers. This work reports the experimental analysis of partial oxidation of n-hexadecane under supercritical water conditions. A novel reactor flow system was developed which allows for total decomposition of hydrogen peroxide in a separate reactor followed partial oxidation of n-hexadecane in a gasification reactor instead of having both reactions in one reactor. The kinetics of hydrothermal decomposition of hydrogen peroxide was studied in order to confirm its full conversion into water and oxygen under the desired partial oxidation conditions, and the kinetic data were found in a good agreement with previously reported literature. The gas yield and gasification efficiency were investigated under different operating parameters. Furthermore, the profile of C-C/C=C ratio was studied which showed the favourable conditions for maximising yields of n-alkanes via hydrogenation of their corresponding 1-alkenes. Enhanced hydrogenation of 1-alkenes was observed at higher O/C ratios and higher residence times, shown by the increase in the C-C/C=C ratio to more than unity, while increasing the temperature has shown much less effect on the C-C/C=C ratio at the current experimental conditions. In addition, GC-MS analysis of liquid samples revealed the formation of heavy oxygenated compounds which may suggest a new addition reaction to account for their formation under the current experimental conditions. Results show new promising routes for hydrogen production with in situ hydrogenation of heavy hydrocarbons in a supercritical water reactor.

Properties of ceria doped with gadolinia via microwave-assisted hydrothermal synthesis; Propriedades de ceria dopada com gadolinia via sintese hidrotermal assistida por micro-ondas

Energy Technology Data Exchange (ETDEWEB)

Carregosa, J.D.C.; Oliveira, R.M.P.B. [Universidade Federal de Sergipe (UFS), Sao Cristovao, SE (Brazil); Macedo, D.A. [Universidade Federal da Paraiba (UFPB), Joao Pessoa, PB (Brazil); Nascimento, R.M., E-mail: jdcovello@hotmail.com [Universidade Federal do Rio Grande do Norte (UFRN), Natal, RN (Brazil)

2016-07-01

The solid solution of CeO{sub 2} doped with Gd{sup 3+} (CGO) is a promising candidate for electrolyte in Solid Oxide Full Cells (SOFCs) operating in intermediate and low temperatures. The reduction of the working temperature of these energy conversion devices is the great technological challenge to its marketing. In this work, nanocrystalline powders of Ce{sub 1-x}Gd{sub x}O{sub 2-x/2} with x=0, x=0.1 e x=0.2 were obtained via microwave-hydrothermal synthesis at low temperature and times of synthesis (10 and 20 min at 120° C). The powders were analyzed by TG-DTA, DRX and dilatometry. The results showed characteristic peaks of the cubic fluorite-type structure, referring to the cerium oxide (CeO{sub 2}), without the presence of secondary peaks. It was also observed that the samples processed at levels of 10 and 20 minutes showed distinct behaviors in contrast to the concentrations of Gd{sup 3+}. (author)

Supercritical Fluid Chromatographic Separation of Dimethylpolysiloxane Polymer

Energy Technology Data Exchange (ETDEWEB)

Pyo, Dong Jin; Lim, Chang Hyun [Kangwon National University, Chuncheon (Korea, Republic of)

2005-02-15

Water was used as a polar modifier and a μ-porasil column as a saturator column. The μ-porasil column was inserted between the pump outlet and the injection valve. During the passage of the supercritical fluid mobile phase through the silica column, a polar modifier (water) can be dissolved in the pressurized supercritical fluid. Dimethylpolysiloxane polymer has been known as more polar polymer than polystyrene polymer. Dimethylpolysiloxane polymer has never been separated using water modified mobile phase. In this paper, using a μ-porasil column as a saturator column, excellent supercritical fluid chromatograms of dimethylpolysiloxane oligomers were obtained. The use of compressed (dense) gases and supercritical fluids as chromatographic mobile phases in conjunction with liquid chromatographic (LC)-type packed columns was first reported by Klesper et al. in 1962. During its relatively short history, supercritical fluid chromatography (SFC) has become an attractive alternative to GC and LC in certain industrially important applications. SFC gives the advantage of high efficiency and allows the analysis of nonvolatile or thermally labile mixtures.

Supercritical Fluid Chromatographic Separation of Dimethylpolysiloxane Polymer

International Nuclear Information System (INIS)

Pyo, Dong Jin; Lim, Chang Hyun

2005-01-01

Water was used as a polar modifier and a μ-porasil column as a saturator column. The μ-porasil column was inserted between the pump outlet and the injection valve. During the passage of the supercritical fluid mobile phase through the silica column, a polar modifier (water) can be dissolved in the pressurized supercritical fluid. Dimethylpolysiloxane polymer has been known as more polar polymer than polystyrene polymer. Dimethylpolysiloxane polymer has never been separated using water modified mobile phase. In this paper, using a μ-porasil column as a saturator column, excellent supercritical fluid chromatograms of dimethylpolysiloxane oligomers were obtained. The use of compressed (dense) gases and supercritical fluids as chromatographic mobile phases in conjunction with liquid chromatographic (LC)-type packed columns was first reported by Klesper et al. in 1962. During its relatively short history, supercritical fluid chromatography (SFC) has become an attractive alternative to GC and LC in certain industrially important applications. SFC gives the advantage of high efficiency and allows the analysis of nonvolatile or thermally labile mixtures

Factors influencing formation of highly dispersed BaTiO3 nanospheres with uniform sizes in static hydrothermal synthesis

International Nuclear Information System (INIS)

Gao, Jiabing; Shi, Haiyue; Dong, Huina; Zhang, Rui; Chen, Deliang

2015-01-01

Highly dispersed BaTiO 3 nanospheres with uniform sizes have important applications in micro/nanoscale functional devices. To achieve well-dispersed spherical BaTiO 3 nanocrystals, we carried out as reported in this paper the systematic investigation on the factors that influence the formation of BaTiO 3 nanospheres by the static hydrothermal process, including the NaOH concentrations [NaOH], molar Ba/Ti ratios (R Ba/Ti ), hydrothermal temperatures, and durations, with an emphasis on understanding the related mechanisms. Barium nitrate and TiO 2 sols derived from tetrabutyl titanate were used as the starting materials. The as-synthesized BaTiO 3 samples were characterized by X-ray diffraction, scanning electron microscopy, energy-dispersive X-ray analysis, thermogravimetry, differential thermal analysis, and FT-IR spectra. The highly dispersed BaTiO 3 nanospheres (76 ± 13 nm) were achieved under the optimum hydrothermal conditions at 200 °C for 10 h: [NaOH] = 2.0 mol L −1 and R Ba/Ti  = 1.5. Higher NaOH concentrations, higher Ba/Ti ratios, higher hydrothermal temperatures, and longer hydrothermal durations are favorable in forming BaTiO 3 nanospheres with larger fractions of tetragonal phase and higher yields; but too long hydrothermal durations resulted in abnormal growth and reduced the uniformity in particle sizes. The possible formation mechanisms for BaTiO 3 nanocrystals under the static hydrothermal conditions were investigated

Introduction to supercritical fluids a spreadsheet-based approach

CERN Document Server

Smith, Richard; Peters, Cor

2013-01-01

This text provides an introduction to supercritical fluids with easy-to-use Excel spreadsheets suitable for both specialized-discipline (chemistry or chemical engineering student) and mixed-discipline (engineering/economic student) classes. Each chapter contains worked examples, tip boxes and end-of-the-chapter problems and projects. Part I covers web-based chemical information resources, applications and simplified theory presented in a way that allows students of all disciplines to delve into the properties of supercritical fluids and to design energy, extraction and materials formation systems for real-world processes that use supercritical water or supercritical carbon dioxide. Part II takes a practical approach and addresses the thermodynamic framework, equations of state, fluid phase equilibria, heat and mass transfer, chemical equilibria and reaction kinetics of supercritical fluids. Spreadsheets are arranged as Visual Basic for Applications (VBA) functions and macros that are completely (source code) ...

Direct hydrothermal growth of GDC nanorods for low temperature solid oxide fuel cells

Science.gov (United States)

Hong, Soonwook; Lee, Dohaeng; Yang, Hwichul; Kim, Young-Beom

2018-06-01

We report a novel synthesis technique of gadolinia-doped ceria (GDC) nano-rod (NRs) via direct hydrothermal process to enhance performance of low temperature solid oxide fuel cell by increasing active reaction area and ionic conductivity at interface between cathode and electrolyte. The cerium nitrate hexahydrate, gadolinium nitrate hexahydrate and urea were used to synthesis GDC NRs for growth on diverse substrate. The directly grown GDC NRs on substrate had a width from 819 to 490 nm and height about 2200 nm with a varied urea concentration. Under the optimized urea concentration of 40 mMol, we confirmed that GDC NRs able to fully cover the substrate by enlarging active reaction area. To maximize ionic conductivity of GDC NRs, we synthesis varied GDC NRs with different ratio of gadolinium and cerium precursor. Electrochemical analysis revealed a significant enhanced performance of fuel cells applying synthesized GDC NRs with a ratio of 2:8 gadolinium and cerium precursor by reducing polarization resistance, which was chiefly attributed to the enlarged active reaction area and enhanced ionic conductivity of GDC NRs. This method of direct hydrothermal growth of GDC NRs enhancing fuel cell performance was considered to apply other types of catalyzing application using nano-structure such as gas sensing and electrolysis fields.

Simulation of Thermal Hydraulic at Supercritical Pressures with APROS

Energy Technology Data Exchange (ETDEWEB)

Kurki, Joona [VTT Technical Research Centre of Finland, P.O. Box 1000, FI02044 VTT (Finland)

2008-07-01

The proposed concepts for the fourth generation of nuclear reactors include a reactor operating with water at thermodynamically supercritical state, the Supercritical Water Reactor (SCWR). For the design and safety demonstrations of such a reactor, the possibility to accurately simulate the thermal hydraulics of the supercritical coolant is an absolute prerequisite. For this purpose, the one-dimensional two-phase thermal hydraulics solution of APROS process simulation software was developed to function at the supercritical pressure region. Software modifications included the redefinition of some parameters that have physical significance only at the subcritical pressures, improvement of the steam tables, and addition of heat transfer and friction correlations suitable for the supercritical pressure region. (author)

Hydrothermal synthesis of nickel hydroxide nanostructures in mixed solvents of water and alcohol

International Nuclear Information System (INIS)

Yang Lixia; Zhu Yingjie; Tong Hua; Liang Zhenhua; Li Liang; Zhang Ling

2007-01-01

Nickel hydroxide nanosheets and flowers have been hydrothermally synthesized using Ni(CH 3 COO) 2 .4H 2 O in mixed solvents of ethylene glycol (EG) or ethanol and deionized water at 200 deg. C for different time. The phase and morphology of the obtained products can be controlled by adjusting the experimental parameters, including the hydrothermal time and the volume ratio of water to EG or ethanol. The possible reaction mechanism and growth of the nanosheets and nanoflowers are discussed based on the experimental results. Porous nickel oxide nanosheets are obtained by heating nickel hydroxide nanosheets in air at 400 deg. C. The products were characterized by using various methods including X-ray diffraction (XRD), fourier transform infrared (FTIR), transmission electron microscopy (TEM), selected-area electron diffraction (SAED), field emission scanning electron microscopy (FESEM). The electrochemical property of β-Ni(OH) 2 nanosheets was investigated through the cyclic voltammogram (CV) measurement. - Graphical abstract: Nickel hydroxide nanosheets and flowers have been hydrothermally synthesized using Ni(CH 3 COO) 2 .4H 2 O in mixed solvents of ethylene glycol (EG) or ethanol and deionized water at 200 deg. C for different reaction time. Porous nickel oxide nanosheets are obtained by heating nickel hydroxide nanosheets in air at 400 deg. C

Template-free hydrothermal synthesis and high photocatalytic activity of ZnWO4 nanorods

International Nuclear Information System (INIS)

Gao, Bin; Fan, Huiqing; Zhang, Xiaojun; Song, Lixun

2012-01-01

Highlights: ► ZnWO 4 nanorods with uniform diameter are successfully prepared through a template-free hydrothermal method. ► The crystallinity of the products is influenced by the pH value of initial precursor suspension. ► Photocatalytic activity of the ZnWO 4 nanorods for degradation of methylene blue is evaluated. ► The ZnWO 4 nanorods exhibit good stability of photocatalytic activity. - Abstract: ZnWO 4 nanorods are successfully synthesized by a template-free hydrothermal method, and are characterized in detail by X-ray diffractometer (XRD), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM) and selected area electron diffraction (SAED). The results show that the ZnWO 4 nanorods with wolframite structure are well-crystallized single crystallites. The crystallinity of the products is influenced by the pH value of initial precursor suspension. The width and length of the synthesized samples increase with hydrothermal reaction temperature. The photocatalytic efficiency of the ZnWO 4 nanorods for degradation of methylene blue (MB) in aqueous solution under UV light irradiation declines greatly with increasing crystallinity. The ZnWO 4 nanorods prepared at pH of 4 have the best activity in photo-degradation of MB. After six recycles, photocatalytic activity loss of the catalyst is not obvious.

Photocatalytic properties of TiO{sub 2} prepared by coprecipitation and by hydrothermal synthesis and study of the effect of doping Gd{sup 3+}; Fotokatalyticke vlastnosti TiO{sub 2} pripraveneho koprecipitaciou a hydrotermalnou syntezou a studium vplyvu dopovania Gd{sup 3+}

Energy Technology Data Exchange (ETDEWEB)

Sipos, M [Univerzita Komenskeho v Bratislave, Prirodovedecka fakulta, Katedra anorganickej chemie, 84215 Bratislava (Slovakia)

2012-04-25

In this paper we described a synthesis of TiO{sub 2} nanopowders by coprecipitation and by hydrothermal method. We examined the effect of sample preparation procedure, of annealing temperature and doping by Gd{sup 3+} ions on the photocatalytic properties of TiO{sub 2}. We did not observe a correlation between primary micro-crystallites largeness and their photocatalytic activity. Sulfation and samples doping by G{sup d}3{sup +} ions enhances their photodegradation properties. Effect of doping is significantly larger at hydrothermally prepared samples. (authors)

Controllable Hydrothermal Conversion from Ni-Co-Mn Carbonate Nanoparticles to Microspheres

Directory of Open Access Journals (Sweden)

Yanqing Tang

2016-11-01

Full Text Available Starting from Ni-Co-Mn carbonate nanoparticles prepared by microreaction technology, uniform spherical particles of Ni1/3Co1/3Mn1/3CO3 with a size of 3–4 μm were obtained by a controllable hydrothermal conversion with the addition of (NH42CO3. Based on characterizations on the evolution of morphology and composition with hydrothermal treatment time, we clarified the mechanism of this novel method as a dissolution-recrystallization process, as well as the effects of (NH42CO3 concentration on the morphology and composition of particles. By changing concentrations and the ratio of the starting materials for nano-precipitation preparation, we achieved monotonic regulation on the size of the spherical particles, and the synthesis of Ni0.4Co0.2Mn0.4CO3 and Ni0.5Co0.2Mn0.3CO3, respectively. In addition, the spherical particles with a core-shell structure were preliminarily verified to be available by introducing nano-precipitates with different compositions in the hydrothermal treatment in sequence.

Hydrothermal processing of fermentation residues in a continuous multistage rig – Operational challenges for liquefaction, salt separation, and catalytic gasification

International Nuclear Information System (INIS)

Zöhrer, H.; De Boni, E.; Vogel, F.

2014-01-01

Fermentation residues are a waste stream of biomethane production containing substantial amounts of organic matter, and thus representing a primary energy source which is mostly unused. For the first time this feedstock was tested for catalytic gasification in supercritical water (T ≥ 374 °C, p ≥ 22 MPa) for methane production. The processing steps include hydrothermal liquefaction, salt separation, as well as catalytic gasification over a ruthenium catalyst in supercritical water. In continuous experiments at a feed rate of 1 kg h −1 a partial liquefaction and carbonization of some of the solids was observed. Significant amounts of heavy tars were formed. Around 50% of the feed carbon remained in the rig. Furthermore, a homogeneous coke was formed, presumably originating from condensed tars. The mineralization of sulfur and its separation in the salt separator was insufficient, because most of the sulfur was still organically bound after liquefaction. Desalination was observed at a salt separator set point temperature of 450 °C and 28 MPa; however, some of the salts could not be withdrawn as a concentrated brine. At 430 °C no salt separation took place. Higher temperatures in the salt separator were found to promote tar and coke formation, resulting in conflicting process requirements for efficient biomass liquefaction and desalination. In the salt separator effluent, solid crystals identified as struvite (magnesium ammonium phosphate) were found. This is the first report of struvite formation from a supercritical water biomass conversion process and represents an important finding for producing a fertilizer from the separated salt brine. - Highlights: • Continuous processing of fermentation residues in sub- and supercritical water. • Continuous separation of salt brines at supercritical water conditions. • Struvite crystals (magnesium ammonium phosphate) were recovered from the effluent. • Separation of sulfur from the biomass could

Hydrothermal synthesis of 3D hierarchical flower-like MoSe{sub 2} microspheres and their adsorption performances for methyl orange

Energy Technology Data Exchange (ETDEWEB)

Tang, Hua, E-mail: tanghua@mail.ujs.edu.cn; Huang, Hong; Wang, Xiaoshuai; Wu, Kongqiang; Tang, Guogang; Li, Changsheng

2016-08-30

Highlights: • 3D hierarchical flower-like MoSe{sub 2} microspheres have been fabricated via a hydrothermal method. • A possible evolution process of 3D hierarchical flower-like MoSe{sub 2} microspheres was discussed. • Flower-like MoSe{sub 2} microspheres exhibit excellent adsorption properties for dye methyl orange removal from aqueous solution. - Abstract: In this paper, we report a facile and versatile modified hydrothermal method for synthesis of three-dimensional (3D) hierarchical flower-like MoSe{sub 2} microspheres using selenium powders and sodium molybdate as raw materials. The as-prepared MoSe{sub 2} was investigated for application as an adsorbent for the removal of dye contaminants from water. Power X-ray diffraction (XRD), energy dispersive spectroscopy (EDS), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscope (XPS) and N{sub 2} adsorption-desorption analysis were carried out to study the microstructure of the as-synthesized product. A possible growth mechanism of MoSe{sub 2} flower-like microspheres was preliminarily proposed on the basis of observation of a time-dependent morphology evolution process. Moreover, the MoSe{sub 2} sample exhibited good adsorption properties, with maximum adsorption capacity of 36.91 mg/g for methyl orange. The adsorption process of methyl orange on 3D hierarchical flower-like MoSe{sub 2} microspheres was systematically investigated, which was found to obey the pseudo-second-order rate equation and Langmuir adsorption model.

Vanadium dioxide nanobelts: Hydrothermal synthesis and magnetic properties

Energy Technology Data Exchange (ETDEWEB)

Zakharova, G.S., E-mail: volkov@ihim.uran.ru [Institute of Solid State Chemistry, Ural Division, Russian Academy of Sciences, Pervomaiskaya ul. 91, Yekaterinburg 620041 (Russian Federation); Hellmann, I. [Leibniz-Institut fuer Festkoerper- und Werkstoffforschung (IFW) Dresden, Helmholtzstr. 20, D-01069 Dresden (Germany); Volkov, V.L. [Institute of Solid State Chemistry, Ural Division, Russian Academy of Sciences, Pervomaiskaya ul. 91, Yekaterinburg 620041 (Russian Federation); Taeschner, Ch.; Bachmatiuk, A.; Leonhardt, A.; Klingeler, R.; Buechner, B. [Leibniz-Institut fuer Festkoerper- und Werkstoffforschung (IFW) Dresden, Helmholtzstr. 20, D-01069 Dresden (Germany)

2010-09-15

VO{sub 2} (B) nanobelts were prepared by a hydrothermal method at 180 {sup o}C using V{sub 2}O{sub 5}.nH{sub 2}O sol and H{sub 2}C{sub 2}O{sub 4}.2H{sub 2}O as starting agents. The obtained nanobelts have diameters ranging from 50 to 100 nm in width, 20-30 nm in thickness with lengths up to 1.5 {mu}m. Measurements of the static magnetic susceptibility provide evidence for two phase transitions at T{sub 1} = 225 K and T{sub 2} = 290 K, respectively. Below T{sub 1}, the data suggest the presence quasi-free as well as of strongly antiferromagnetic correlated spins associated to V{sup 4+}-ions.

Mild Hydrothermal Synthesis of Ni–Cu Nanoparticles

Directory of Open Access Journals (Sweden)

G. H. Mohamed Saeed

2010-01-01

Full Text Available Magnetic Ni-rich Ni–Cu nanoparticles with Ni : Cu mass ratio (S of 2.0 and 2.6 were prepared using a mixture of polyoxyethylene (10 isooctylphenyl ether (Triton X-100 and sodium dodecyl sulfate (SDS in a mild hydrothermal condition at 95ºC. X-ray diffractometry (XRD showed that the nanoparticles prepared at S=2.0 possessed Ni–Cu alloy characteristic whereas the characteristic was absent at S=2.6. The XRD data was enhanced by Fourier transform infrared spectroscopy (FTIR which exhibited metal-metal (Ni–Cu band at 455 cm−1. Based on transmission electron microscopy (TEM, the average particle sizes for the nanoparticles prepared at S=2.0 and 2.6 were in the range of 19–23 nm. The as-prepared nanoparticles exhibited paramagnetic behaviour measured using a vibrating sample magnetometer (VSM and the specific saturation magnetization decreased at the higher concentration of Ni.

Supercritical fluid technology: concepts and pharmaceutical applications.

Science.gov (United States)

Deshpande, Praful Balavant; Kumar, G Aravind; Kumar, Averineni Ranjith; Shavi, Gopal Venkatesh; Karthik, Arumugam; Reddy, Meka Sreenivasa; Udupa, Nayanabhirama

2011-01-01

In light of environmental apprehension, supercritical fluid technology (SFT) exhibits excellent opportunities to accomplish key objectives in the drug delivery sector. Supercritical fluid extraction using carbon dioxide (CO(2)) has been recognized as a green technology. It is a clean and versatile solvent with gas-like diffusivity and liquid-like density in the supercritical phase, which has provided an excellent alternative to the use of chemical solvents. The present commentary provides an overview of different techniques using supercritical fluids and their future opportunity for the drug delivery industry. Some of the emerging applications of SFT in pharmaceuticals, such as particle design, drug solubilization, inclusion complex, polymer impregnation, polymorphism, drug extraction process, and analysis, are also covered in this review. The data collection methods are based on the recent literature related to drug delivery systems using SFT platforms. SFT has become a much more versatile and environmentally attractive technology that can handle a variety of complicated problems in pharmaceuticals. This cutting-edge technology is growing predominantly to surrogate conventional unit operations in relevance to the pharmaceutical production process. Supercritical fluid technology has recently drawn attention in the field of pharmaceuticals. It is a distinct conception that utilizes the solvent properties of supercritical fluids above their critical temperature and pressure, where they exhibit both liquid-like and gas-like properties, which can enable many pharmaceutical applications. For example, the liquid-like properties provide benefits in extraction processes of organic solvents or impurities, drug solubilization, and polymer plasticization, and the gas-like features facilitate mass transfer processes. It has become a much more versatile and environmentally attractive technology that can handle a variety of complicated problems in pharmaceuticals. This review is

Synthesis and characterization on titanium dioxide prepared by precipitation and hydrothermal treatment

International Nuclear Information System (INIS)

Santos, Andre V.P. dos; Yoshito, Walter K.; Lazar, Dolores R.R.; Ussui, Valter

2012-01-01

Surface properties of titanium dioxide (titania) are outstanding among ceramic materials and enables uses as catalysts, photoelectrochemical devices, solar cells and others. In many of these applications, it is necessary to keep the anatase phase, that is stable only in low temperatures (<400 deg C). In the present work, the influence of hydrothermal treatment on physical characteristics and crystal structure of titania powders synthesized by precipitation was investigated. Characterizations of obtained powders were carried out by X-ray diffraction, surface area analysis by N2 gas sorption (BET) and microstructure of powders and ceramics were analyzed by scanning electron microscopy. As prepared powders were formed as cylindrical pellets by uniaxial pressing and sintered at 1500 deg C for 01 hour. Results showed that anatase phase without formation of rutile phase can be formed in hydrothermally treated samples . Rutile phase is predominant in calcined and/or sintered samples (author)

Synthesis of boehmite by hydrothermal treatment used as inorganic binder for alumina powder

International Nuclear Information System (INIS)

Lima, M.B.; Tercini, M.B.; Yoshimura, H.N.

2012-01-01

Presently, due to the concerns with the environment, it has been developed studies to replace the organic binder by an inorganic binder for forming of ceramic powders, in order to avoiding the generation of polluting gases during sintering (firing). A potential alternative is the use of boehmite, produced by hydrothermal treatment on the surfaces of the alumina powder, previously ground in a ball mill using zirconia milling media to produce hydrated phases on alumina powder which are converted to boehmite. In the treated alumina powders, it was observed the formation of boehmite phase by X-ray diffraction analysis and Fourier transformed infrared (FTIR) spectroscopy, demonstrating the efficiency of boehmite formation during the hydrothermal treatment at 150°C for 3 hours.(author)

Chemical speciation of inorganic compounds under hydrothermal conditions. 1998 annual progress report

International Nuclear Information System (INIS)

Darab, J.G.; Fulton, J.L.; Steidler, G.T.; Stern, E.A.

1998-01-01

'To obtain the chemistry of metallic solute ions under aqueous and hydrothermal conditions in order to obtain key insights pertinent to the removal of toxic wastes. Elements present in Hanford tank wastes will be investigated to get a better understanding of how the high temperatures involved in vitrification will affect the hydrolysis-polymerization reaction. In the following summary of the x-ray absorption fine structure (XAFS) measurements under aqueous and hydrothermal conditions, most measurements below the critical temperature (375 C) were taken at about 200 bar pressure, while at supercritical temperatures the pressure was about 600 bar. Chemistry of Na 2 WO 4 Under Aqueous and Hydrothermal Conditions Tungsten, molybdenum, vanadium and, to a lesser agree, chromium, niobium and tantalum form isopolymetallates, polymeric species of rather complicated structure and complex chemical equilibria, in aqueous solution upon acidification. Except Tantalum, all of these elements are present in the Hanford tank wastes and it is not well understood how the high temperatures involved in vitrification will affect the hydrolysis-polymerization reaction. In March 1998, the authors launched a series of XAFS experiments to resolve these questions. Measurements were obtained for 0.2 molal tungstate solutions as a function of temperature (to 200 C) and as a function of starting pH. The outcome of these measurements is providing key insights into this chemistry as follows: (1) A change from tetrahedral to octahedral coordination of the oxygen atoms around the tungsten center atom can be detected upon increasing extent of polymerization. (2) At least one new feature shows up in the Fourier Transform of the k-weighted Chi plot (closely related to a radial distribution function) which is unambiguously attributed to a tungsten-tungsten scattering path, only present in the polymeric species. (3) Perhaps most interestingly, the XAFS data indicate a higher extent of polymerization at

Hydrothermal gasification of glucose and starch in a batch and continuous reactor

Directory of Open Access Journals (Sweden)

Kazuhiro Kumabe

2017-11-01

Full Text Available A batch reactor was used for the gasification of glucose and starch as carbohydrate model compounds. The effects of H2O in various states (low-pressure hot compressed water (LP-HCW, 300 °C and 10 MPa, high-pressure hot compressed water (HP-HCW, 360 °C and 20 MPa, high-temperature steam (HTS, 400 °C and 10 MPa, and supercritical water (SCW, 400 °C and 25 MPa, as well as reaction time (10, 30, and 60 min, sample concentration (10, 20, and 30 wt%, and catalyst (mixture of Ca(OH2 and Na2CO3 on gas production were investigated in the hydrothermal gasification. In addition, using a continuous reactor, the hydrothermal gasification of glucose was examined with LP-HCW (200 °C and 5 MPa, HP-HCW (200 °C and 25 MPa, HTS (600 °C, 5 MPa, and SCW (600 °C, 25 MPa in order to study the productions of gases and tar, and the mass balance. The reaction temperature affected gasification considerably, but pressure had little effect. In the batch experiments, the characteristics of the produced gases were almost identical after a reaction time of 10 min, and addition of Ca(OH2 and Na2CO3 as catalysts in a molar ratio of 7:3 led to selective production of H2 in the SCW gasification of 10 wt% glucose for 30 min. In a continuous experiment under the SCW conditions, the conversion efficiency of glucose to gas was 26% and the composition of the produced gas was 29 vol% CO, 23 vol% H2, and 16 vol% CH4. Under the hydrothermal conditions, glucose was mainly converted to char and suspended components of high-molecular-weight compounds such as fat, whereas starch was mainly converted to gas and liquid.

In-situ hydrothermal synthesis of three-dimensional MnO2-CNT nanocomposites and their electrochemical properties

International Nuclear Information System (INIS)

Teng, Fei; Santhanagopalan, Sunand; Wang, Ying; Meng, Dennis Desheng

2010-01-01

Three-dimensional (3-D) MnO 2 -carbon nanotube (CNT) nanocomposites were prepared by a simple one-pot hydrothermal method. An electrode was then prepared with these nanocomposites. For comparative investigation, MnO 2 microspheres were also hydrothermally prepared without adding CNTs. The as-synthesized MnO 2 microspheres were then mechanically mixed with CNTs to prepare a subsequent electrode. The samples were characterized by electron microscopy, X-ray diffraction, and electrochemical methods. It has been revealed that a 3-D conductive network of CNTs was formed with microspheres of MnO 2 nanorods interwoven with and connected by CNTs. As a result, the hydrothermally mixed MnO 2 -CNT electrode showed a higher specific capacitance than the mechanically mixed electrode. It has therefore been concluded that the hydrothermal mixing method yields a more homogeneous product that is better suited to take full advantages of both the high capacitance of MnO 2 and the high electrical conductivity of CNTs. The 3-D MnO 2 -CNT nanocomposites reported herein have provided a promising electrode material for supercapacitors and other electrochemical energy storage/conversion devices.

Controlled synthesis of La{sub 1−x}Sr{sub x}CrO{sub 3} nanoparticles by hydrothermal method with nonionic surfactant and their ORR activity in alkaline medium

Energy Technology Data Exchange (ETDEWEB)

Choi, Bo Hyun; Park, Shin-Ae [Energy System Major, School of Mechanical Engineering, Pusan National University, Busan 609-735 (Korea, Republic of); Park, Bong Kyu [GIFT Center, Pusan National University, Busan, 609-735 (Korea, Republic of); Chun, Ho Hwan, E-mail: chunahh@pusan.ac.kr [Global Core Research Center for Ships and Offshore Plants(GCRC-SOP), Pusan National University, Busan, 609-735 (Korea, Republic of); Kim, Yong-Tae, E-mail: yongtae@pusan.ac.kr [Energy System Major, School of Mechanical Engineering, Pusan National University, Busan 609-735 (Korea, Republic of)

2013-10-15

Graphical abstract: We demonstrate that Sr-doped LaCrO{sub 3} nanoparticles were successfully prepared by the hydrothermal synthesis method using the nonionic surfactant Triton X-100 and the applicability of La{sub 1−x}Sr{sub x}CrO{sub 3} to oxygen reduction reaction (ORR) electrocatalysis in an alkaline medium. Compared with the nanoparticles synthesized by the coprecipitation method, they showed enhanced ORR activity. - Highlights: • Sr-doped LaCrO{sub 3} nanoparticles were successfully prepared by the hydrothermal method using the nonionic surfactant. • Homogeneously shaped and sized Sr-doped LaCrO{sub 3} nanoparticles were readily obtained. • Compared with the nanoparticles synthesized by the coprecipitation method, they showed an enhanced ORR activity. • The main origin was revealed to be the decreased particle size due to the nonionic surfactant. - Abstract: Sr-doped LaCrO{sub 3} nanoparticles were prepared by the hydrothermal method with the nonionic surfactant Triton X-100 followed by heat treatment at 1000 °C for 10 h. The obtained perovskite nanoparticles had smaller particle size (about 100 nm) and more uniform size distribution than those synthesized by the conventional coprecipitation method. On the other hand, it was identified with the material simulation that the electronic structure change by Sr doping was negligible, because the initially unfilled e{sub g}-band was not affected by the p-type doping. Finally, the perovskite nanoparticles synthesized by hydrothermal method showed much higher ORR activity by over 200% at 0.8 V vs. RHE than those by coprecipitation method.

Synthesis of zinc oxide by microwave hydrothermal method for application to transesterification of soybean oil (biodiesel)

Energy Technology Data Exchange (ETDEWEB)

Quirino, Max Rocha [LABQUIM/Universidade Federal da Paraíba, Campus III, 58200-000, Bananeiras, PB (Brazil); Oliveira, Mateus José C. [DEMA/Universidade Federal de Campina Grande, Campina Grande, Campus I, 58429-900, Campina Grande, PB (Brazil); Keyson, Davy [DME/Universidade Federal da Paraíba, Campus – I, 58051-900, João Pessoa, PB (Brazil); Lucena, Guilherme Leocárdio, E-mail: guilhermelucena@cchsa.ufpb.br [LABQUIM/Universidade Federal da Paraíba, Campus III, 58200-000, Bananeiras, PB (Brazil); Oliveira, João Bosco L. [Universidade Federal do Rio Grande do Norte, Campus I, 59078-970, Natal, RN (Brazil); Gama, Lucianna [DEMA/Universidade Federal de Campina Grande, Campina Grande, Campus I, 58429-900, Campina Grande, PB (Brazil)

2017-01-01

ZnO nanostructures were synthesized by microwave hydrothermal treatment using two different mineralization agents (NaOH and NH{sub 4}OH), and were evaluated as catalysts for biodiesel synthesis. The materials were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and Brunauer-Emmett-Teller (BET) surface area analysis. The XRD patterns indicated the formation of the hexagonal wurtzite phase in both samples. SEM analysis showed completely different morphologies based on the mineralization agent employed. The ZnO nanostructures synthesized with NaOH (ZONa5 and ZONa5P) presented plate-like agglomerates, resulting in a quasi-spherical morphology, whereas the materials synthesized with NH{sub 4}OH (ZONH5 and ZONH5P) presented a flower-like morphology. The ZONa5P sample showed an activity of 77.82% for the catalytic conversion of soybean oil into biodiesel by transesterification using methanol. - Highlights: • ZnO was synthesized by MH method in only 5 min. • The powders morphology is completely influenced by mineralization agent. • ZONa5P showed activity of 77.82% for the conversion of soybean oil into biodiesel.

Supercritical Airfoil Coordinates

Data.gov (United States)

National Aeronautics and Space Administration — Rectangular Supercritical Wing (Ricketts) - design and measured locations are provided in an Excel file RSW_airfoil_coordinates_ricketts.xls . One sheet is with Non...

Theoretical models for supercritical fluid extraction.

Science.gov (United States)

Huang, Zhen; Shi, Xiao-Han; Jiang, Wei-Juan

2012-08-10

For the proper design of supercritical fluid extraction processes, it is essential to have a sound knowledge of the mass transfer mechanism of the extraction process and the appropriate mathematical representation. In this paper, the advances and applications of kinetic models for describing supercritical fluid extraction from various solid matrices have been presented. The theoretical models overviewed here include the hot ball diffusion, broken and intact cell, shrinking core and some relatively simple models. Mathematical representations of these models have been in detail interpreted as well as their assumptions, parameter identifications and application examples. Extraction process of the analyte solute from the solid matrix by means of supercritical fluid includes the dissolution of the analyte from the solid, the analyte diffusion in the matrix and its transport to the bulk supercritical fluid. Mechanisms involved in a mass transfer model are discussed in terms of external mass transfer resistance, internal mass transfer resistance, solute-solid interactions and axial dispersion. The correlations of the external mass transfer coefficient and axial dispersion coefficient with certain dimensionless numbers are also discussed. Among these models, the broken and intact cell model seems to be the most relevant mathematical model as it is able to provide realistic description of the plant material structure for better understanding the mass-transfer kinetics and thus it has been widely employed for modeling supercritical fluid extraction of natural matters. Copyright © 2012 Elsevier B.V. All rights reserved.

Effect of hydrothermal treatment on catalytic activity of amorphous mesoporous Cr2O3–ZrO2 nanomaterials for ethanol oxidation

International Nuclear Information System (INIS)

Mahmoud, Hala R.

2015-01-01

Mesoporous 0.25Cr 2 O 3 –0.75ZrO 2 binary oxide catalysts (CZ-H) with high specific surface areas were successfully synthesized by hydrothermal treatment. The effect of synthesis conditions, such as hydrothermal temperature and time of CZ-H nanomaterials were investigated by X-ray diffraction (XRD), high-resolution transmission electron microscopy (HR-TEM), energy dispersive spectroscopic (EDS), UV–vis diffuse reflectance spectroscopy (DRS) and N 2 adsorption–desorption measurements (BET). The XRD analysis indicated the formation of amorphous materials of binary oxides. The results showed that hydrothermal temperature and time of CZ-H nanomaterials had great influence on the average particle diameter and surface area. Under the optimum synthesis conditions, the best CZ-H nanomaterial synthesized at 210 °C for 3 h (i.e., CZ-H213), presented spherical structure with smallest average particle diameter found to be 1.5 nm and possessed highest surface area of 526.6 m 2 /g. Optical studies by UV–vis spectroscopy for the different CZ-H nanomaterials exhibit slightly blue shift from 3.20 to 3.33 eV due to quantum confined exciton absorption. Moreover, hydrothermal synthesis leads to catalysts with higher surface area and with better acid–base properties than conventional co-precipitation method. Compared to the other nanomaterials, the CZ-H213 catalyst appears to be the best candidate for further application in acid–base catalysis and reusability. - Graphical abstract: Display Omitted - Highlights: • Mesoporous 25%Cr 2 O 3 –75%ZrO 2 catalysts (CZ-H) were prepared by hydrothermal method. • The hydrothermal temperature and time modified the properties of CZ-H nanomaterials. • The best CZ-H nanomaterial synthesized at 210 °C for 3 h (i.e., CZ-H213). • A CZ-H213 nanomaterial had the highest S BET and smallest average particle diameter. • A mesoporous CZ-H213 used as a reusable active catalyst in the ethanol conversion

Hydrothermal synthesis of Ni_2P nanoparticle and its hydrodesulfurization of dibenzothiophene

International Nuclear Information System (INIS)

Zhao, Qi; Han, Yang; Huang, Xiang; Dai, Jinhui; Tian, Jintao; Zhu, Zhibin; Yue, Li

2017-01-01

Nanosized nickel phosphide (Ni_2P) has been synthesized via hydrothermal reaction with environmental-friendly red phosphorus and nickel chloride. The reaction mechanism has been studied by measurement techniques of IC, XRD ,TEM, EDS, and XPS. The results showed that the particle sizes of as-prepared Ni_2P are in nanoscale ranging from 10 to 30 nm. In hydrothermal reaction, red phosphorus reacts with water to its oxyacids, especially its hypophosphorous acid (or hypophosphite) which can reduce nickel chloride to nickel, and then metallic nickel will penetrate into the rest of red phosphorus to generate nano-Ni_2P. Furthermore, the catalytic performance of as-synthesized Ni_2P for the hydrodesulfurization of dibenzothiophene has been tested. It has been shown that the HDS reaction process over Ni_2P catalyst agrees well with the pseudo-first order kinetic equation, and the HDS conversion can reach up to 43.83% in 5 h with a stable increasing catalytic activity during the whole examination process.

Surfactant-assisted hydrothermal synthesis of CdS nanotips: optical and magnetic properties

International Nuclear Information System (INIS)

Mondal, Biswajit; Saha, Shyamal Kumar

2012-01-01

CdS nanotips with size 5–8 nm are synthesized by hydrothermal process using polyacrylamide (PAM) as surfactant. The shape of nanocrystals (NCs) changes from particles to nanorods or nanotips depending upon the amount of PAM used. Optical properties of the CdS NCs vary with hydrothermal temperature (T H ) due to formation of “S” vacancies. The Rietveld refinement of XRD data shows that “S” site occupancy decreases with increase in T H and amount of PAM indicating the formation of “S” vacancies. Size-dependent magnetic properties in these NCs indicate that the micron-size rods are diamagnetic in nature while the microrods ended with sharp tips show ferromagnetism even at room temperature. The origin of this ferromagnetism in nanotips is explained by the variation in density of “S” defects at the nanotips as well as in the nanorods. These ferromagnetic nanotips grown in the rods as side growth have potential applications in magnetic force microscopes.

Corrosion behavior of porous chromium carbide in supercritical water

International Nuclear Information System (INIS)

Dong Ziqiang; Chen Weixing; Zheng Wenyue; Guzonas, Dave

2012-01-01

Highlights: ► Corrosion behavior of porous Cr 3 C 2 in various SCW conditions was investigated. ► Cr 3 C 2 is stable in SCW at temperature below 420–430 °C. ► Cracks and disintegration were observed at elevated testing temperatures. ► Degradation of Cr 3 C 2 is related to the intermediate product CrOOH. - Abstract: The corrosion behavior of highly porous chromium carbide (Cr 3 C 2 ) prepared by a reactive sintering process was characterized at temperatures ranging from 375 °C to 625 °C in a supercritical water environment with a pressure of 25–30 MPa. The test results show that porous chromium carbide is stable in SCW environments at temperatures under 425 °C, above which disintegration occurred. The porous carbide was also tested under hydrothermal conditions of pressures between 12 MPa and 50 MPa at constant temperatures of 400 °C and 415 °C, respectively. The pressure showed little effect on the stability of chromium carbide in the tests at those temperatures. The mechanism of disintegration of chromium carbide in SCW environments is discussed.

Thermal stability of biodiesel in supercritical methanol

Energy Technology Data Exchange (ETDEWEB)

Hiroaki Imahara; Eiji Minami; Shusaku Hari; Shiro Saka [Kyoto University, Kyoto (Japan). Department of Socio-Environmental Energy Science

2008-01-15

Non-catalytic biodiesel production technologies from oils/fats in plants and animals have been developed in our laboratory employing supercritical methanol. Due to conditions in high temperature and high pressure of the supercritical fluid, thermal stability of fatty acid methyl esters and actual biodiesel prepared from various plant oils was studied in supercritical methanol over a range of its condition between 270{sup o}C/17 MPa and 380{sup o}C/56 MPa. In addition, the effect of thermal degradation on cold flow properties was studied. As a result, it was found that all fatty acid methyl esters including poly-unsaturated ones were stable at 270{sup o}C/17 MPa, but at 350{sup o}C/43 MPa, they were partly decomposed to reduce the yield with isomerization from cis-type to trans-type. These behaviors were also observed for actual biodiesel prepared from linseed oil, safflower oil, which are high in poly-unsaturated fatty acids. Cold flow properties of actual biodiesel, however, remained almost unchanged after supercritical methanol exposure at 270{sup o}C/17 MPa and 350{sup o}C/43 MPa. For the latter condition, however, poly-unsaturated fatty acids were sacrificed to be decomposed and reduced in yield. From these results, it was clarified that reaction temperature in supercritical methanol process should be lower than 300{sup o}C, preferably 270{sup o}C with a supercritical pressure higher than 8.09 MPa, in terms of thermal stabilization for high-quality biodiesel production. 9 refs., 3 figs., 4 tabs.

Hydrothermal synthesis and characterization of a binuclear complex and a coordination

Directory of Open Access Journals (Sweden)

Reza Mohamadinasab

2010-06-01

Full Text Available Two new copper complexes [(bipy(pydcCu(μ-OCO-pydcCu(bipy(H2O].3.5H¬2O (1 and {[(μ2-C2O4(2,2'-bipyCu].2H2O}n (2 (pydcH2 = pyridine-2,6-dicarboxylilic acid, bipy = 2,2'-bipyridine have been hydrothermally synthesized. Both complexes were characterized by IR spectroscopy, elemental analysis and single crystal X-ray diffraction studies. Complex 1 consists of two independent neutral molecules. In every moiety, metal ion center is in a distorted octahedral geometry. Coordination polymer (2 has been prepared from the reaction of bis-(cyclohexanone-oxal-dihydrazone,2,2'-bipyridine and Cu(NO32 in basic solution and under hydrothermal condition. The results showed that the bis-(cyclohexanone-oxal-dihydrazone was converted to oxalate ion under heating and basic pH. Each metal ion center in 2 is in a distorted octahedral geometry and is coordinated by four oxygen atoms of two bridged oxalate ions and two nitrogen atoms of 2,2'-bipyridine molecules. In the crystal structure of 2, some H-bonds and π-π interaction cause formation of a 3D network.

Hydrothermal preparation of hydrophobic and hydrophilic nanoparticles of iron oxide and a modification with CM-dextran

Czech Academy of Sciences Publication Activity Database

Repko, A.; Nižňanský, D.; Matulková, Irena; Kalbáč, Martin; Vejpravová, Jana

2013-01-01

Roč. 15, č. 7 (2013), s. 1-9 ISSN 1388-0764 Institutional support: RVO:68378271 ; RVO:61388955 Keywords : superparamagnetism * magnetite * carboxymethyl dextran * hydrothermal synthesis * nanocrystals Subject RIV: BM - Solid Matter Physics ; Magnetism; CF - Physical ; Theoretical Chemistry (UFCH-W) Impact factor: 2.278, year: 2013

Supercritical fluid extraction of oregano (Origanum vulgare) essentials oils: anti-inflammatory properties based on cytokine response on THP-1 macrophages.

Science.gov (United States)

Ocaña-Fuentes, A; Arranz-Gutiérrez, E; Señorans, F J; Reglero, G

2010-06-01

Two fractions (S1 and S2) of an oregano (Origanum vulgare) extract obtained by supercritical fluid extraction have been used to test anti-inflammatory effects on activated human THP-1 cells. The main compounds present in the supercritical extract fractions of oregano were trans-sabinene hydrate, thymol and carvacrol. Fractions toxicity was assessed using the mitochondrial-respiration-dependent 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium (MTT) reduction method for several concentrations during 24 and 48 h of incubation. Concentrations higher than 30 microg/mL of both supercritical S1 and S2 oregano fractions caused a reduction in cell viability in a dose-dependent manner. Oxidized-LDLs (oxLDLs) activated THP-1 macrophages were used as cellular model of atherogenesis and the release/secretion of cytokines (TNT-alpha, IL-1beta, IL-6 and IL-10) and their respective mRNA expressions were quantified both in presence or absence of supercritical oregano extracts. The results showed a decrease in pro-inflammatory TNF-alpha, IL-1beta and IL-6 cytokines synthesis, as well as an increase in the production of anti-inflammatory cytokine IL-10. These results may suggest an anti-inflammatory effect of oregano extracts and their compounds in a cellular model of atherosclerosis. Copyright 2010 Elsevier Ltd. All rights reserved.

Hydrothermal synthesis and characterization of sea urchin-like nickel and cobalt selenides nanocrystals

Energy Technology Data Exchange (ETDEWEB)

Liu Xiaohe [Department of Inorganic Materials, Central South University, Changsha, Hunan 410083 (China) and School of Metallurgical Science and Engineering, Central South University, Changsha, Hunan 410083 (China)]. E-mail: liuxh@mail.csu.edu.cn; Zhang Ning [Department of Inorganic Materials, Central South University, Changsha, Hunan 410083 (China); Yi Ran [Department of Inorganic Materials, Central South University, Changsha, Hunan 410083 (China); Qiu Guanzhou [Department of Inorganic Materials, Central South University, Changsha, Hunan 410083 (China); Yan Aiguo [Department of Inorganic Materials, Central South University, Changsha, Hunan 410083 (China); Wu Hongyi [Department of Inorganic Materials, Central South University, Changsha, Hunan 410083 (China); Meng Dapeng [Department of Inorganic Materials, Central South University, Changsha, Hunan 410083 (China); Tang, Motang [School of Metallurgical Science and Engineering, Central South University, Changsha, Hunan 410083 (China)

2007-05-25

Sea urchin-like nanorod-based nickel and cobalt selenides nanocrystals have been selective synthesized via a hydrothermal reduction route in which hydrated nickel chloride and hydrated cobalt chloride were employed to supply Ni and Co source and aqueous hydrazine (N{sub 2}H{sub 4}.H{sub 2}O) was used as reducing agent. The composition, morphology, and structure of final products could be easily controlled by adjusting the molar ratios of reactants and process parameters such as hydrothermal time. The morphology and phase structure of the final products have been investigated by X-ray diffraction, transmission electron microscopy, and scanning electron microscopy. The probable formation mechanism of the sea urchin-like nanorod-based nickel and cobalt selenides nanocrystals was discussed on the basis of the experimental results.

Advanced Supercritical Carbon Dioxide Brayton Cycle Development

Energy Technology Data Exchange (ETDEWEB)

Anderson, Mark [Univ. of Wisconsin, Madison, WI (United States); Sienicki, James [Argonne National Lab. (ANL), Argonne, IL (United States); Moisseytsev, Anton [Argonne National Lab. (ANL), Argonne, IL (United States); Nellis, Gregory [Univ. of Wisconsin, Madison, WI (United States); Klein, Sanford [Univ. of Wisconsin, Madison, WI (United States)

2015-10-21

Fluids operating in the supercritical state have promising characteristics for future high efficiency power cycles. In order to develop power cycles using supercritical fluids, it is necessary to understand the flow characteristics of fluids under both supercritical and two-phase conditions. In this study, a Computational Fluid Dynamic (CFD) methodology was developed for supercritical fluids flowing through complex geometries. A real fluid property module was implemented to provide properties for different supercritical fluids. However, in each simulation case, there is only one species of fluid. As a result, the fluid property module provides properties for either supercritical CO₂ (S-CO₂) or supercritical water (SCW). The Homogeneous Equilibrium Model (HEM) was employed to model the two-phase flow. HEM assumes two phases have same velocity, pressure, and temperature, making it only applicable for the dilute dispersed two-phase flow situation. Three example geometries, including orifices, labyrinth seals, and valves, were used to validate this methodology with experimental data. For the first geometry, S-CO₂ and SCW flowing through orifices were simulated and compared with experimental data. The maximum difference between the mass flow rate predictions and experimental measurements is less than 5%. This is a significant improvement as previous works can only guarantee 10% error. In this research, several efforts were made to help this improvement. First, an accurate real fluid module was used to provide properties. Second, the upstream condition was determined by pressure and density, which determines supercritical states more precise than using pressure and temperature. For the second geometry, the flow through labyrinth seals was studied. After a successful validation, parametric studies were performed to study geometric effects on the leakage rate. Based on these parametric studies, an optimum design strategy for the see

Fast infrared spectroscopy in supercritical fluids

International Nuclear Information System (INIS)

Sun, X.

2000-05-01

Chapter 1: Introduction. A brief introduction to supercritical fluids is given, illustrating why supercritical fluids are unique solvents and why there is a wide application of supercritical fluids in industry and laboratories. Potential ways for solvation in supercritical fluids to affect reactivity are briefly reviewed. A general introduction to the photochemistry of organometallic complexes is also given. Chapter 2: Time resolved vibrational spectroscopy. Time resolved resonance Raman is introduced and compared with Time-resolved infrared spectroscopy (TRIR). The different approaches of TRIR, including microsecond, nanosecond, and ultrafast (picosecond and femtosecond) systems are discussed. The advantages and disadvantages of these systems are also compared. The TRIR apparatus using an IR diode laser used for work in this thesis are described in detail. Experimental procedures for supercritical fluid TRIR experiments are described with emphasis on handling the IR cell for supercritical fluids and preparation of supercritical fluid solutions. Chapter 3: Photochemistry of group VIB hexacarbonyl compounds in supercritical noble gases and CO 2 solutions. A systematic TRIR study of the photolysis of M(CO) 6 in supercritical Ar, Kr, Xe, and CO 2 and the observation of M(CO) 5 L (M = Cr, Mo, and W; L = Ar (W only), Kr, Xe, and CO 2 ) is described. The second-order rate constants for the reaction of M(CO) 5 L with CO have been evaluated and the reactivity for each metal is Kr > Xe ∼ CO 2 . For M(CO) 5 Kr, M(CO) 5 Xe, or M(CO) 5 (CO 2 ), the reactivity is Cr ∼ Mo > W. In supercritical Kr doped with either Xe or CO 2 , the M(CO) 5 moiety interacts with Xe or CO 2 in preference to Kr. The effect of solvent density on the rate of the reaction of W(CO) 5 (CO 2 ) with CO has been investigated. The reaction of W(CO) 5 (CO 2 ) with CO in scCO 2 is predominantly a dissociative process. The activation energies for the reaction of W(CO) 5 Xe and W(CO) 5 (CO 2 ) with CO and

Nonionic emulsion-mediated synthesis of zeolite beta

Indian Academy of Sciences (India)

Administrator

, 18 Fuxue ... alkylation, disproportionation and other organic synthesis processes at present (Camblor et al 1996). Usually, zeolite beta is synthesized by hydrothermal method at ... However, microemulsion has not yet been applied to syn-.

Hydrothermal synthesis and electrochemical properties of nano-sized Co-Sn alloy anodes for lithium ion batteries

International Nuclear Information System (INIS)

He Jianchao; Zhao Hailei; Wang Jing; Wang Jie; Chen Jingbo

2010-01-01

Research highlights: → Nano-sized Co-Sn alloys were synthesized by hydrothermal route. → Li 2 O and CoSn can buffer the large volume change associated with lithiation of Sn. → A two-step reaction mechanism of CoSn 2 alloy during cycling was confirmed. - Abstract: Nano-sized Co-Sn alloys with a certain amount of Sn oxides used as potential anode materials for lithium ion batteries were synthesized by hydrothermal route. The effects of hydrothermal conditions and post annealing on the phase compositions and the electrochemical properties of synthesized powders were characterized by means of X-ray diffraction (XRD), field-emission scanning electron microscopy (FESEM) with energy dispersive spectra (EDS) analysis and galvanostatic cycling tests. Prolonging the dwelling time at the same hydrothermal temperature can increase the content of Sn oxides, which will lead to a high initial irreversible capacity loss but a better cycling stability owing to the buffer effect of irreversible product Li 2 O. Heat-treatment can increase the crystallinity and cause the presence of a certain amount of inert CoSn component, which both have positive impact on the cycling stability of Co-Sn electrode. By comparison with the lithiation/delithiation processes of metal Sn, a two-step mechanism of CoSn 2 alloy during cycling was confirmed.

Development of a test facility for analyzing supercritical fluid blowdown

International Nuclear Information System (INIS)

Roberto, Thiago D.; Alvim, Antonio C.M.

2015-01-01

The generation IV nuclear reactors under development mostly use supercritical fluids as the working fluid because higher temperatures improve the thermal efficiency. Supercritical fluids are used by modern nuclear power plants to achieve thermal efficiencies of around 45%. With water as the supercritical working fluid, these plants operate at a high temperature and pressure. However, experiments on supercritical water are limited by technical and financial difficulties. These difficulties can be overcome by using model fluids, which have more feasible supercritical conditions and exhibit a lower critical pressure and temperature. Experimental research is normally used to determine the conditions under which model fluids represent supercritical fluids under steady-state conditions. A fluid-to-fluid scaling approach has been proposed to determine model fluids that can represent supercritical fluids in a transient state. This paper presents an application of fractional scale analysis to determine the simulation parameters for a depressurization test facility. Carbon dioxide (CO 2 ) and R134a gas were considered as the model fluids because their critical point conditions are more feasible than those of water. The similarities of water (prototype), CO 2 (model) and R134a (model) for depressurization in a pressure vessel were analyzed. (author)

FY 1998 'The New Sunshine Project' leading R and D. Report on the results of the leading R and D of supercritical fluid utilization technology; 1998 nendo 'New Sunshine Keikaku' sendo kenkyu kaihatsu. Chorinkai ryutai riyo gijutsu sendo kenkyu kaihatsu seika hokokusho

Energy Technology Data Exchange (ETDEWEB)

NONE

1999-03-01

The paper reported the FY 1998 achievement of the supercritical fluid utilization leading R and D which started in FY 1997 on a 3-year plan. In the R and D, solvolysis reaction, oxidation reaction and hydrogenation reaction were taken up in the chemical process using supercritical fluid. In the study of solvolysis reaction, the basic data were obtained on decomposition conditions of thermoplastic and thermosetting plastics in supercritical water. Further, concerning the synthesis of environmental friendly type carbonate using CO2, a conversion rate of almost 100% was obtained. About the oxidation reaction, conditions were found out for burning low grade coal in supercritical water without emitting acid gas. This is considered to lead to a possibility of the supercritical water power generation. Relating to the hydrogenation reaction, a study was made on lightening technology of heavy distillate using supercritical water, and the conditions for effective emission of methane and hydrogen were found out. As to the base technology, a study was made of metal materials with high corrosion resistance against supercritical water. (NEDO)

Synthesis of potassium sodium niobate nanostructures by hydrothermal combining with the sol-gel method

Energy Technology Data Exchange (ETDEWEB)

Meng, Xianghe; Wang, Wen, E-mail: wangwen@hit.edu.cn; Ke, Hua; Rao, Jiancun; Zhou, Yu

2016-10-15

Graphical abstract: We prepared novel metastable perovskite K{sub 0.52}Na{sub 0.48}NbO{sub 3} microstructures with a morphotropic phase boundary (MPB) between rhombohedral and tetragonal via hydrothermal method with SDS surfactant-assist. - Highlights: • KNbO{sub 3}-type orthorhombic K{sub 1−x}Na{sub x}NbO{sub 3} nanowires were prepared by hydrothermal method. • Metastable K{sub 0.52}Na{sub 0.48}NbO{sub 3} microfingers have a morphotropic phase boundary. • Sodium dodecyl sulfate could improve the crystallinity of K{sub 0.52}Na{sub 0.48}NbO{sub 3} powders. • The Curie temperature of rhombohedral-tetragonal KNN was 555 °C. - Abstract: In this paper the K{sub 1−x}Na{sub x}NbO{sub 3}(KNN) nanostructures were synthesized by hydrothermal method using KNN gel powders as precursors. KNbO{sub 3}-type orthorhombic KNN nanowires and perovskite KNN microfingers with a morphotropic phase boundary (MPB) between rhombohedral and tetragonal characterized by X-ray diffraction and Raman spectroscopy were obtained at 190 °C and 220 °C, respectively. KNbO{sub 3}-type orthorhombic KNN nanowires had rectangular shape and the growth direction of these nanowires was [0 0 1]. The rhombohedral-tetragonal KNN microfingers were metastable, and changed the rhombohedral-tetragonal phase into the orthorhombic phase via thermal treatment at 600 °C then cooled down to room temperature. Sodium dodecyl sulfate (SDS) as surfactant was added to the hydrothermal reaction. It was found that SDS could improve the crystallinity of the rhombohedral-tetragonal K{sub 0.52}Na{sub 0.48}NbO{sub 3} and reduce the impurity effectively. The tetragonal-cubic phase transition temperature (Tc) of the rhombohedral-tetragonal powders appeared at 555 °C.

27.12 MHz plasma generation in supercritical carbon dioxide

International Nuclear Information System (INIS)

Kawashima, Ayato; Toyota, Hiromichi; Nomura, Shinfuku; Takemori, Toshihiko; Mukasa, Shinobu; Maehara, Tsunehiro; Yamashita, Hiroshi

2007-01-01

An experiment was conducted for generating high-frequency plasma in supercritical carbon dioxide; it is expected to have the potential for applications in various types of practical processes. It was successfully generated at 6-20 MPa using electrodes mounted in a supercritical cell with a gap of 1 mm. Emission spectra were then measured to investigate the physical properties of supercritical carbon dioxide plasma. The results indicated that while the emission spectra for carbon dioxide and carbon monoxide could be mainly obtained at a low pressure, the emission spectra for atomic oxygen could be obtained in the supercritical state, which increased with the pressure. The temperature of the plasma in supercritical state was estimated to be approximately 6000-7000 K on the assumption of local thermodynamic equilibrium and the calculation results of thermal equilibrium composition in this state showed the increase of atomic oxygen by the decomposition of CO 2

Accelerated Removal of Fe-Antisite Defects while Nanosizing Hydrothermal LiFePO4 with Ca(2).

Science.gov (United States)

Paolella, Andrea; Turner, Stuart; Bertoni, Giovanni; Hovington, Pierre; Flacau, Roxana; Boyer, Chad; Feng, Zimin; Colombo, Massimo; Marras, Sergio; Prato, Mirko; Manna, Liberato; Guerfi, Abdelbast; Demopoulos, George P; Armand, Michel; Zaghib, Karim

2016-04-13

Based on neutron powder diffraction (NPD) and high angle annular dark field scanning transmission electron microscopy (HAADF-STEM), we show that calcium ions help eliminate the Fe-antisite defects by controlling the nucleation and evolution of the LiFePO4 particles during their hydrothermal synthesis. This Ca-regulated formation of LiFePO4 particles has an overwhelming impact on the removal of their iron antisite defects during the subsequent carbon-coating step since (i) almost all the Fe-antisite defects aggregate at the surface of the LiFePO4 crystal when the crystals are small enough and (ii) the concomitant increase of the surface area, which further exposes the Fe-antisite defects. Our results not only justify a low-cost, efficient and reliable hydrothermal synthesis method for LiFePO4 but also provide a promising alternative viewpoint on the mechanism controlling the nanosizing of LiFePO4, which leads to improved electrochemical performances.

Supercritical fields and bald black holes

Energy Technology Data Exchange (ETDEWEB)

Irvine, J M

1975-01-01

The instability of a many-fermion ground state against particle-hole excitations is reviewed and the existence of supercritical electromagnetic and strong interaction fields is briefly discussed. The nature of associated phase changes and in particular the change in conservation laws which accompanies the phase changes is outlined. Finally, the supercritical gravitational field is considered and weight given to the argument that ''black holes have no hair.''

Nonionic surfactant-assisted hydrothermal synthesis of YVO4:Eu3+ powders in a wide pH range and their luminescent properties

International Nuclear Information System (INIS)

Wang Juan; Hojamberdiev, Mirabbos; Xu Yunhua; Peng Jianhong

2011-01-01

YVO 4 :Eu 3+ powders with different morphologies were fabricated by a simple hydrothermal method at 180 deg. C for 24 h in a wide pH range with the assistance of polyvinylpyrrolidone (PVP) as a nonionic surfactant. The as-synthesized samples were characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and photoluminescence spectroscopy (PL). The obtained results showed that the pH value of synthesis solution played a key role in the formation of final products with different morphologies, such as, microspheres, irregular microspheres with grain-like nanoparticles, stone-like structures with regular short nanorods, and smooth rhombohedrons. The PL measurements revealed that the emission intensity of the samples was first decreased, and then increased with increasing the pH value due mainly to the increase in crystallinity and decrease in surface defects.

Synthesis and characterization of boehmites obtained from gibbsite in presence of different environments

Energy Technology Data Exchange (ETDEWEB)

Denigres Filho, Ricardo Wilson Nastari; Rocha, Gisele de Araujo; Vieira-Coelho, Antonio Carlos, E-mail: acvcoelh@usp.br [Universidade de Sao Paulo (LPSS/EP/USP), SP (Brazil). Departamento de Engenharia Metalurgica e de Materiais. Laboratorio de Materias-Primas Particuladas; Montes, Celia Regina [Centro de Energia Nuclear na Agricultura (NUPEGEL/CENA/USP), Piracicaba, SP (Brazil). Nucleo de Pesquisas Geoquimicas e Geofisicas da Listosfera

2016-05-15

In this study, results related to boehmite synthesis by hydrothermal processes starting from a Bayer commercial gibbsite are reported. The processes have been conducted from aqueous suspensions with initial acidic or alkaline pH, without or with acetate ion, at 160 deg C for 72h to 168h. The final materials were characterized by X-ray diffraction (XRD), thermal methods (DTA and TGA) and scanning electron microscopy (SEM). The influence of the synthesis conditions on the morphology of the boehmite crystals obtained from the gibbsite at different hydrothermal processes are discussed. (author)

Supercritical heat transfer phenomena in nuclear system

International Nuclear Information System (INIS)

Seo, Kyoung Woo; Kim, Moo Hwan; Anderson, Mark H.; Corradini, Michael L.

2005-01-01

A supercritical water (SCW) power cycle has been considered as one of the viable candidates for advanced fission reactor designs. However, the dramatic variation of thermo-physical properties with a modest change of temperature near the pseudo-critical point make existing heat transfer correlations such as the Dittus-Boelter correlation not suitably accurate to calculate the heat transfer in supercritical fluid. Several other correlations have also been suggested but none of them are able to predict the heat transfer over a parameter range, needed for reactor thermal-hydraulics simulation and design. This has prompted additional research to understand the characteristic of supercritical fluid heat transfer

Hydrothermal synthesis and characterizations of Ti substituted Mn-ferrites

Energy Technology Data Exchange (ETDEWEB)

Mostafa, Nasser Y., E-mail: nmost69@yahoo.com [Faculty of Science, Taif University, P.O. Box 888 Al-Haweiah, Taif (Saudi Arabia); Chemistry Department, Faculty of Science, Suez Canal University, Ismailia 41522 (Egypt); Hessien, M.M. [Faculty of Science, Taif University, P.O. Box 888 Al-Haweiah, Taif (Saudi Arabia); Advanced materials Division-Central metallurgical R and D Institute (CMRDI), P.O. Box 87 Helwan, Cairo (Egypt); Shaltout, Abdallah A. [Faculty of Science, Taif University, P.O. Box 888 Al-Haweiah, Taif (Saudi Arabia); Spectroscopy Department, Physics Division, National Research Center, El Behooth Str., 12622 Dokki, Cairo (Egypt)

2012-07-15

Highlights: Black-Right-Pointing-Pointer Hydrothermal synthesized of well-crystallized Ti-substituted MnFe{sub 2}O{sub 4} nanoparticles at 180 Degree-Sign C without any calcination step. The chemical composition was represented by Mn{sub 1-2x}Ti{sub x}Fe{sub 2}O{sub 4} with x having values 0.0, 0.1, 0.2, 0.3 and 0.4. Black-Right-Pointing-Pointer The change in lattice parameter and saturation magnetization with increasing Ti-substitution was investigated and explained. Black-Right-Pointing-Pointer The change in microstructure due to Ti{sup 4+} ions substitutions was investigated using TEM analysis. - Abstarct: A series of well-crystallized Mn{sub 1-2x}Ti{sub x}Fe{sub 2}O{sub 4} nanoparticles with x values of 0.0, 0.1, 0.2, 0.3 and 0.4 have been synthesized by hydrothermal route at 180 Degree-Sign C in the presence of NaOH as mineralizer. The obtained ferrite samples were characterized by X-ray diffraction (XRD), transmission electron microscope (TEM) and vibrating sample magnetometer (VSM). The XRD analysis showed that pure single phases of cubic ferrites were obtained with x up to 0.2. However, samples with x > 0.2 showed traces of unreacted anatase. The increase in Ti-substitution up to x = 0.2 leads to an increase in the lattice parameter of the prepared ferrites. On the other hand, the increase in Ti-substitution over x = 0.2 leads to a decrease in the lattice parameter. The average crystallite size was in the range of 39-57 nm, where it is increased by increasing the Ti-substitution up to x = 0.3, then decreased for x = 0.4. According to VSM results, the saturation magnetization increased with Ti ion substitution of x = 0.1 and decreased for x > 0.1.

Effect of supercritical fluid density on nanoencapsulated drug particle size using the supercritical antisolvent method.

Science.gov (United States)

Kalani, Mahshid; Yunus, Robiah

2012-01-01

The reported work demonstrates and discusses the effect of supercritical fluid density (pressure and temperature of supercritical fluid carbon dioxide) on particle size and distribution using the supercritical antisolvent (SAS) method in the purpose of drug encapsulation. In this study, paracetamol was encapsulated inside L-polylactic acid, a semicrystalline polymer, with different process parameters, including pressure and temperature, using the SAS process. The morphology and particle size of the prepared nanoparticles were determined by scanning electron microscopy and transmission electron microscopy. The results revealed that increasing temperature enhanced mean particle size due to the plasticizing effect. Furthermore, increasing pressure enhanced molecular interaction and solubility; thus, particle size was reduced. Transmission electron microscopy images defined the internal structure of nanoparticles. Thermal characteristics of nanoparticles were also investigated via differential scanning calorimetry. Furthermore, X-ray diffraction pattern revealed the changes in crystallinity structure during the SAS process. In vitro drug release analysis determined the sustained release of paracetamol in over 4 weeks.

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.

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

Science.gov (United States)

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

2018-03-01

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

Carotenoids Functionality, Sources, and Processing by Supercritical Technology: A Review

Directory of Open Access Journals (Sweden)

Natália Mezzomo

2016-01-01

Full Text Available Carotenoid is a group of pigments naturally present in vegetal raw materials that have biological properties. These pigments have been used mainly in food, pharmaceutical, and cosmetic industries. Currently, the industrial production is executed through chemical synthesis, but natural alternatives of carotenoid production/attainment are in development. The carotenoid extraction occurs generally with vegetal oil and organic solvents, but supercritical technology is an alternative technique to the recovery of these compounds, presenting many advantages when compared to conventional process. Brazil has an ample diversity of vegetal sources inadequately investigated and, then, a major development of optimization and validation of carotenoid production/attainment methods is necessary, so that the benefits of these pigments can be delivered to the consumer.

Nanotechnology and supercritical fluids | Hamidreza | Journal of ...

African Journals Online (AJOL)

Supercritical fluid (SCF) technology has become an important tool of materials processing in the last two decades. Supercritical CO2 and H2O are extensively being used in the preparation of a great variety of nanomaterials. The interest in the preparation and application of nanometer size materials is increasing since they ...

Supercritical fluid technology for energy and environmental applications

CERN Document Server

Anikeev, Vladimir

2014-01-01

Supercritical Fluid Technology for Energy and Environmental Applications covers the fundamental principles involved in the preparation and characterization of supercritical fluids (SCFs) used in the energy production and other environmental applications. Energy production from diversified resources - including renewable materials - using clean processes can be accomplished using technologies like SCFs. This book is focused on critical issues scientists and engineers face in applying SCFs to energy production and environmental protection, the innovative solutions they have found, and the challenges they need to overcome. The book also covers the basics of sub- and supercritical fluids, like the thermodynamics of phase and chemical equilibria, mathematical modeling, and process calculations. A supercritical fluid is any substance at a temperature and pressure above its critical point where distinct liquid and gas phases do not exist. At this state the compound demonstrates unique properties, which can be "fine...

In-situ hydrothermal synthesis of three-dimensional MnO{sub 2}-CNT nanocomposites and their electrochemical properties

Energy Technology Data Exchange (ETDEWEB)

Teng, Fei; Santhanagopalan, Sunand [Department of Mechanical Engineering-Engineering Mechanics, Michigan Technological University, Houghton, MI 49931 (United States); Wang, Ying [Department of Mechanical Engineering, Louisiana State University, Baton Rouge, LA 70803 (United States); Meng, Dennis Desheng, E-mail: dmeng@mtu.ed [Department of Mechanical Engineering-Engineering Mechanics, Michigan Technological University, Houghton, MI 49931 (United States)

2010-06-11

Three-dimensional (3-D) MnO{sub 2}-carbon nanotube (CNT) nanocomposites were prepared by a simple one-pot hydrothermal method. An electrode was then prepared with these nanocomposites. For comparative investigation, MnO{sub 2} microspheres were also hydrothermally prepared without adding CNTs. The as-synthesized MnO{sub 2} microspheres were then mechanically mixed with CNTs to prepare a subsequent electrode. The samples were characterized by electron microscopy, X-ray diffraction, and electrochemical methods. It has been revealed that a 3-D conductive network of CNTs was formed with microspheres of MnO{sub 2} nanorods interwoven with and connected by CNTs. As a result, the hydrothermally mixed MnO{sub 2}-CNT electrode showed a higher specific capacitance than the mechanically mixed electrode. It has therefore been concluded that the hydrothermal mixing method yields a more homogeneous product that is better suited to take full advantages of both the high capacitance of MnO{sub 2} and the high electrical conductivity of CNTs. The 3-D MnO{sub 2}-CNT nanocomposites reported herein have provided a promising electrode material for supercapacitors and other electrochemical energy storage/conversion devices.

Selective chelation and extraction of lanthanides and actinides with supercritical fluids

International Nuclear Information System (INIS)

Brauer, R.D.; Carleson, T.E.; Harrington, J.D.; Jean, F.; Jiang, H.; Lin, Y.; Wai, C.M.

1994-01-01

This report is made up of three independent papers: (1) Supercritical Fluid Extraction of Thorium and Uranium with Fluorinated Beta-Diketones and Tributyl Phosphate, (2) Supercritical Fluid Extraction of Lanthanides with Beta-Diketones and Mixed Ligands, and (3) A Group Contribution Method for Predicting the Solubility of Solid Organic Compounds in Supercritical Carbon Dioxide. Experimental data are presented demonstrating the successful extraction of thorium and uranium using fluorinated beta-diketones to form stable complexes that are extracted with supercritical carbon dioxide. The conditions for extracting the lanthanide ions from liquid and solid materials using supercritical carbon dioxide are presented. In addition, the Peng-Robison equation of state and thermodynamic equilibrium are used to predict the solubilities of organic solids in supercritical carbon dioxide from the sublimation pressure, critical properties, and a centric factor of the solid of interest

Effects of Gravity on Supercritical Water Oxidation (SCWO) Processes

Science.gov (United States)

Hegde, Uday; Hicks, Michael

2013-01-01

The effects of gravity on the fluid mechanics of supercritical water jets are being studied at NASA to develop a better understanding of flow behaviors for purposes of advancing supercritical water oxidation (SCWO) technologies for applications in reduced gravity environments. These studies provide guidance for the development of future SCWO experiments in new experimental platforms that will extend the current operational range of the DECLIC (Device for the Study of Critical Liquids and Crystallization) Facility on board the International Space Station (ISS). The hydrodynamics of supercritical fluid jets is one of the basic unit processes of a SCWO reactor. These hydrodynamics are often complicated by significant changes in the thermo-physical properties that govern flow behavior (e.g., viscosity, thermal conductivity, specific heat, compressibility, etc), particularly when fluids transition from sub-critical to supercritical conditions. Experiments were conducted in a 150 ml reactor cell under constant pressure with water injections at various flow rates. Flow configurations included supercritical jets injected into either sub-critical or supercritical water. Profound gravitational influences were observed, particularly in the transition to turbulence, for the flow conditions under study. These results will be presented and the parameters of the flow that control jet behavior will be examined and discussed.

Supercritical carbon dioxide for textile applications and recent developments

Science.gov (United States)

Eren, H. A.; Avinc, O.; Eren, S.

2017-10-01

In textile industry, supercritical carbon dioxide (scCO2), possessing liquid-like densities, mostly find an application on textile dyeing processes such as providing hydrophobic dyes an advantage on dissolving. Their gas-like low viscosities and diffusion properties can result in shorter dyeing periods in comparison with the conventional water dyeing process. Supercritical carbon dioxide dyeing is an anhydrous dyeing and this process comprises the usage of less energy and chemicals when compared to conventional water dyeing processes leading to a potential of up to 50% lower operation costs. The advantages of supercritical carbon dioxide dyeing method especially on synthetic fiber fabrics hearten leading textile companies to alter their dyeing method to this privileged waterless dyeing technology. Supercritical carbon dioxide (scCO2) waterless dyeing is widely known and applied green method for sustainable and eco-friendly textile industry. However, not only the dyeing but also scouring, desizing and different finishing applications take the advantage of supercritical carbon dioxide (scCO2). In this review, not only the principle, advantages and disadvantages of dyeing in supercritical carbon dioxide but also recent developments of scCO2 usage in different textile processing steps such as scouring, desizing and finishing are explained and commercial developments are stated and summed up.

Hydrothermal synthesis and electrochemical performance of NiO microspheres with different nanoscale building blocks

International Nuclear Information System (INIS)

Wang Ling; Hao Yanjing; Zhao Yan; Lai Qiongyu; Xu Xiaoyun

2010-01-01

NiO microspheres were successfully obtained by calcining the Ni(OH) 2 precursor, which were synthesized via the hydrothermal reaction of nickel chloride, glucose and ammonia. The products were characterized by TGA, XRD and SEM. The influences of glucose and reaction temperature on the morphologies of NiO samples were investigated. Moreover, the possible growth mechanism for the spherical morphology was proposed. The charge/discharge test showed that the as-prepared NiO microspheres composed of nanoparticles can serve as an ideal electrode material for supercapacitor due to the spherical hollow structure. -- Graphical Abstract: Fig. 5 is the SEM image of NiO that was prepared in the different hydrothermal reaction temperatures. It showed that reaction temperature played a crucial role for the morphology of products.

Industrial applications and current trends in supercritical fluid technologies

OpenAIRE

Gamse Thomas

2005-01-01

Supercritical fluids have a great potential for wide fields of processes Although CO2 is still one of the most used supercritical gases, for special purposes propane or even fluorinated-chlorinated fluids have also been tested. The specific characteristics of supercritical fluids behaviour were analyzed such as for example the solubilities of different components and the phase equilibria between the solute and solvent. The application at industrial scale (decaffeinating of tea and coffee, hop...

Hydrothermal Processes

Science.gov (United States)

German, C. R.; von Damm, K. L.

2003-12-01

What is Hydrothermal Circulation?Hydrothermal circulation occurs when seawater percolates downward through fractured ocean crust along the volcanic mid-ocean ridge (MOR) system. The seawater is first heated and then undergoes chemical modification through reaction with the host rock as it continues downward, reaching maximum temperatures that can exceed 400 °C. At these temperatures the fluids become extremely buoyant and rise rapidly back to the seafloor where they are expelled into the overlying water column. Seafloor hydrothermal circulation plays a significant role in the cycling of energy and mass between the solid earth and the oceans; the first identification of submarine hydrothermal venting and their accompanying chemosynthetically based communities in the late 1970s remains one of the most exciting discoveries in modern science. The existence of some form of hydrothermal circulation had been predicted almost as soon as the significance of ridges themselves was first recognized, with the emergence of plate tectonic theory. Magma wells up from the Earth's interior along "spreading centers" or "MORs" to produce fresh ocean crust at a rate of ˜20 km3 yr-1, forming new seafloor at a rate of ˜3.3 km2 yr-1 (Parsons, 1981; White et al., 1992). The young oceanic lithosphere formed in this way cools as it moves away from the ridge crest. Although much of this cooling occurs by upward conduction of heat through the lithosphere, early heat-flow studies quickly established that a significant proportion of the total heat flux must also occur via some additional convective process (Figure 1), i.e., through circulation of cold seawater within the upper ocean crust (Anderson and Silbeck, 1981). (2K)Figure 1. Oceanic heat flow versus age of ocean crust. Data from the Pacific, Atlantic, and Indian oceans, averaged over 2 Ma intervals (circles) depart from the theoretical cooling curve (solid line) indicating convective cooling of young ocean crust by circulating seawater

Supercritical fluid analytical methods

International Nuclear Information System (INIS)

Smith, R.D.; Kalinoski, H.T.; Wright, B.W.; Udseth, H.R.

1988-01-01

Supercritical fluids are providing the basis for new and improved methods across a range of analytical technologies. New methods are being developed to allow the detection and measurement of compounds that are incompatible with conventional analytical methodologies. Characterization of process and effluent streams for synfuel plants requires instruments capable of detecting and measuring high-molecular-weight compounds, polar compounds, or other materials that are generally difficult to analyze. The purpose of this program is to develop and apply new supercritical fluid techniques for extraction, separation, and analysis. These new technologies will be applied to previously intractable synfuel process materials and to complex mixtures resulting from their interaction with environmental and biological systems

Structural behavior of supercritical fluids under confinement

Science.gov (United States)

Ghosh, Kanka; Krishnamurthy, C. V.

2018-01-01

The existence of the Frenkel line in the supercritical regime of a Lennard-Jones (LJ) fluid shown through molecular dynamics (MD) simulations initially and later corroborated by experiments on argon opens up possibilities of understanding the structure and dynamics of supercritical fluids in general and of the Frenkel line in particular. The location of the Frenkel line, which demarcates two distinct physical states, liquidlike and gaslike within the supercritical regime, has been established through MD simulations of the velocity autocorrelation (VACF) and radial distribution function (RDF). We, in this article, explore the changes in the structural features of supercritical LJ fluid under partial confinement using atomistic walls. The study is carried out across the Frenkel line through a series of MD simulations considering a set of thermodynamics states in the supercritical regime (P =5000 bar, 240 K ≤T ≤1500 K ) of argon well above the critical point. Confinement is partial, with atomistic walls located normal to z and extending to "infinity" along the x and y directions. In the "liquidlike" regime of the supercritical phase, particles are found to be distributed in distinct layers along the z axis with layer spacing less than one atomic diameter and the lateral RDF showing amorphous-like structure for specific spacings (packing frustration) and non-amorphous-like structure for other spacings. Increasing the rigidity of the atomistic walls is found to lead to stronger layering and increased structural order. For confinement with reflective walls, layers are found to form with one atomic diameter spacing and the lateral RDF showing close-packed structure for the smaller confinements. Translational order parameter and excess entropy assessment confirms the ordering taking place for atomistic wall and reflective wall confinements. In the "gaslike" regime of the supercritical phase, particle distribution along the spacing and the lateral RDF exhibit features

Molecular simulation of CO chemisorption on Co(0001) in presence of supercritical fluid solvent: A potential of mean force study

Energy Technology Data Exchange (ETDEWEB)

Asiaee, Alireza; Benjamin, Kenneth M., E-mail: kenneth.benjamin@sdsmt.edu [Department of Chemical and Biological Engineering, South Dakota School of Mines and Technology, 501 E. Saint Joseph St., Rapid City, South Dakota 57701 (United States)

2016-08-28

For several decades, heterogeneous catalytic processes have been improved through utilizing supercritical fluids (SCFs) as solvents. While numerous experimental studies have been established across a range of chemistries, such as oxidation, pyrolysis, amination, and Fischer-Tropsch synthesis, still there is little fundamental, molecular-level information regarding the role of the SCF on elementary heterogeneous catalytic steps. In this study, the influence of hexane solvent on the adsorption of carbon monoxide on Co(0001), as the first step in the reaction mechanism of many processes involving syngas conversion, is probed. Simulations are performed at various bulk hexane densities, ranging from ideal gas conditions (no SCF hexane) to various near- and super-critical hexane densities. For this purpose, both density functional theory and molecular dynamics simulations are employed to determine the adsorption energy and free energy change during CO chemisorption. Potential of mean force calculations, utilizing umbrella sampling and the weighted histogram analysis method, provide the first commentary on SCF solvent effects on the energetic aspects of the chemisorption process. Simulation results indicate an enhanced stability of CO adsorption on the catalyst surface in the presence of supercritical hexane within the reduced pressure range of 1.0–1.5 at a constant temperature of 523 K. Furthermore, it is shown that the maximum stability of CO in the adsorbed state as a function of supercritical hexane density at 523 K nearly coincides with the maximum isothermal compressibility of bulk hexane at this temperature.

Synthesis of three-dimensional rare-earth ions doped CNTs-GO-Fe3O4 hybrid structures using one-pot hydrothermal method

International Nuclear Information System (INIS)

Gao, Guo; Zhang, Qiang; Cheng, Xin-Bing; Sun, Rongjin; Shapter, Joseph G.; Yin, Ting; Cui, Daxiang

2015-01-01

Rechargeable lithium ion batteries (LIBs) are currently the dominant power source for all sorts of electronic devices due to their low cost and high energy density. The cycling stability of LIBs is significantly compromised due to the broad satellite peak for many anode materials. Herein, we develop a facile hydrothermal process for preparing rare-earth (Er, Tm) ions doped three-dimensional (3D) transition metal oxides/carbon hybrid nanocomposites, namely CNTs-GO-Fe 3 O 4 , CNTs-GO-Fe 3 O 4 -Er and CNTs-GO-Fe 3 O 4 -Tm. The GO sheets and CNTs are interlinked by ultrafine Fe 3 O 4 nanoparticles forming three-dimensional (3D) architectures. When evaluated as anode materials for LIBs, the CNTs-GO-Fe 3 O 4 hybrid composites have a bigger broad satellite peak. As for the CNTs-GO-Fe 3 O 4 -Er and CNTs-GO-Fe 3 O 4 -Tm hybrid composites, the broad satellite peak can be completely eliminated. When the current density changes from 5 C back to 0.1 C, the capacity of CNTs-GO-Fe 3 O 4 -Tm hybrid composites can recover to 1023.9 mAhg −1 , indicating an acceptable rate capability. EIS tests show that the charge transfer resistance does not change significantly after 500 cycles, demonstrating that the cycling stability of CNTs-GO-Fe 3 O 4 -Tm hybrid composites are superior to CNTs-GO-Fe 3 O 4 and CNTs-GO-Fe 3 O 4 -Er hybrid structures. - Graphical abstract: One-pot hydrothermal method for synthesis of rare-earth ions doped CNTs-GO-Fe 3 O 4 hybrid structures as anode materials of LIBs have been reported. - Highlights: • We report the synthesis of rare-earth ions doped CNTs-GO-Fe 3 O 4 hybrid structures. • The hybrid structures can improve the cycling stability of lithium storage. • As for anode materials, the broad satellite peak can be completely eliminated. • When the rate return back to 0.1 C, the capacity can recover to 1023.9 mAhg −1 . • After 500 cycles, the hybrid structures still exhibited excellent cycling stability

Oxidation stability of biodiesel fuel as prepared by supercritical methanol

Energy Technology Data Exchange (ETDEWEB)

Jiayu Xin; Hiroaki Imahara; Shiro Saka [Kyoto University, Kyoto (Japan). Department of Socio-Environmental Energy Science, Graduate School of Energy Science

2008-08-15

A non-catalytic supercritical methanol method is an attractive process to convert various oils/fats efficiently into biodiesel. To evaluate oxidation stability of biodiesel, biodiesel produced by alkali-catalyzed method was exposed to supercritical methanol at several temperatures for 30 min. As a result, it was found that the tocopherol in biodiesel is not stable at a temperature higher than 300{sup o}C. After the supercritical methanol treatment, hydroperoxides were greatly reduced for biodiesel with initially high in peroxide value, while the tocopherol slightly decreased in its content. As a result, the biodiesel prepared by the supercritical methanol method was enhanced for oxidation stability when compared with that prepared by alkali-catalyzed method from waste oil. Therefore, supercritical methanol method is useful especially for oils/fats having higher peroxide values. 32 refs., 8 figs., 3 tabs.

A study of oleic acid-based hydrothermal preparation of CoFe.sub.2./sub.O.sub.4./sub. nanoparticles

Czech Academy of Sciences Publication Activity Database

Repko, A.; Nižňanský, D.; Poltierová Vejpravová, Jana

2011-01-01

Roč. 13, č. 10 (2011), s. 5021-5031 ISSN 1388-0764 Institutional research plan: CEZ:AV0Z10100520 Keywords : cobalt ferrite * hydrothermal synthesis * magnetic particles * sperparamagnetism Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 3.287, year: 2011

Hydrothermal synthesis of core–shell TiO_2 to enhance the photocatalytic hydrogen evolution

International Nuclear Information System (INIS)

Jiang, Jinghui; Zhou, Han; Zhang, Fan; Fan, Tongxiang; Zhang, Di

2016-01-01

Graphical abstract: Core–shell TiO_2 with interior cavity was synthesized by a hydrothermal approach to enhance the photocatalytic performance. - Highlights: • Core–shell TiO_2 with interior cavity can be synthesized by hydrothermal approach. • Multiple reflection of incident light in cavity can increase the absorption. • Rutile can optimize the bandgap and delay the charge recombination. - Abstract: A hydrothermal approach was designed to synthesize core–shell TiO_2 with interior cavity by making sodium dodecyl sulfonate (SDS) as the surfactant and the mixture of water and ethanol as the solvent. The control experiment of solvent reveals ethanol and water are responsible for the formation of sphere and interior cavity, respectively. Besides, SDS can assist the growth of core–shell structure, and the sizes of sphere and interior cavity can be tuned by regulating the reaction time or temperature. UV–vis absorption proves core–shell structure with interior cavity can increase the absorption of incident light to enhance the optical activity of final product. The calculated bandgap and photoluminescence (PL) analyses reveal the coexistence of rutile in final product can optimize the bandgap to 3.03 eV and delay the charge recombination. As a result, an effective photocatalytic hydrogen evolution under full spectrum irradiation can be harvested by the as-synthesized core–shell spheres to reach a quantum yield, approximately 9.57% at 340 nm wavelength.

Hydrothermal synthesis of Fe-doped TiO2 nanostructure photocatalyst

International Nuclear Information System (INIS)

Nguyen, Van Nghia; Nguyen, Ngoc Khoa Truong; Nguyen, Phi Hung

2011-01-01

Fe-doped TiO 2 catalyst was prepared by the hydrothermal method. The resulting nanopowders were characterized by x-ray diffraction, transmission electron microscopy and Raman and UV-visible spectroscopies. The photocatalytic activity of the Fe-doped TiO 2 was tested by decomposition of methylene orange with a concentration of 10 mg l −1 in aqueous solution. The obtained results showed that methylene orange was significantly degraded after irradiation for 90 min under a halogen lamp and sunlight. The doping effect on the photocatalytic activity of the iron-doped catalyst samples are discussed

Influence of bases on hydrothermal synthesis of titanate nanostructures

Science.gov (United States)

Sikhwivhilu, Lucky M.; Sinha Ray, Suprakas; Coville, Neil J.

2009-03-01

A hydrothermal treatment of titanium dioxide (TiO2) with various bases (i.e., LiOH, NaOH, KOH, and NH4OH) was used to prepare materials with unique morphologies, relatively small crystallite sizes, and large specific surface areas. The experimental results show that the formation of TiO2 is largely dependent on the type, strength and concentration of a base. The effect of the nature of the base used and the concentration of the base on the formation of nanostructures were investigated using X-ray diffraction, Raman spectroscopy, transmission and scanning electron microscopy, as well as surface area measurements. Sodium hydroxide (NaOH) and potassium hydroxide (KOH) were both used to transform the morphology of starting TiO2 material.

Operation and Performance of the Supercritical Fluids Reactor (SFR)

National Research Council Canada - National Science Library

Hanush, R

1996-01-01

The Supercritical Fluids Reactor (SFR) at Sandia National Laboratories, CA has been developed to examine and solve engineering, process, and fundamental chemistry issues regarding the development of supercritical water oxidation (SCWO...

FY 1998 'The New Sunshine Project' leading R and D. Report on the results of the leading R and D of supercritical fluid utilization technology; 1998 nendo 'New Sunshine Keikaku' sendo kenkyu kaihatsu. Chorinkai ryutai riyo gijutsu sendo kenkyu kaihatsu seika hokokusho

Energy Technology Data Exchange (ETDEWEB)

NONE

1999-03-01

The paper reported the FY 1998 achievement of the supercritical fluid utilization leading R and D which started in FY 1997 on a 3-year plan. In the R and D, solvolysis reaction, oxidation reaction and hydrogenation reaction were taken up in the chemical process using supercritical fluid. In the study of solvolysis reaction, the basic data were obtained on decomposition conditions of thermoplastic and thermosetting plastics in supercritical water. Further, concerning the synthesis of environmental friendly type carbonate using CO2, a conversion rate of almost 100% was obtained. About the oxidation reaction, conditions were found out for burning low grade coal in supercritical water without emitting acid gas. This is considered to lead to a possibility of the supercritical water power generation. Relating to the hydrogenation reaction, a study was made on lightening technology of heavy distillate using supercritical water, and the conditions for effective emission of methane and hydrogen were found out. As to the base technology, a study was made of metal materials with high corrosion resistance against supercritical water. (NEDO)

Hydrothermal synthesis and upconversion luminescent properties of YVO4:Yb3+,Er3+ nanoparticles

International Nuclear Information System (INIS)

Liang, Yanjie; Chui, Pengfei; Sun, Xiaoning; Zhao, Yan; Cheng, Fuming; Sun, Kangning

2013-01-01

Graphical abstract: YVO 4 :Yb 3+ ,Er 3+ nanoparticles have been successfully prepared via a facile hydrothermal technique in the presence of citric acid as a complexing agent followed by a subsequent heat treatment process. The PL intensity of the sample increases with the increase of annealing temperature and excitation power. Under the excitation of a 980 nm diode laser, the samples show bright green luminescence. Highlights: ► YVO 4 :Yb 3+ ,Er 3+ nanoparticles were prepared by a hydrothermal approach. ► Bright green luminescence is observed under the excitation of a 980 nm laser diode. ► The PL intensity increases with the increase of annealing temperature. ► Energy transfer properties between Yb 3+ ion and Er 3+ ion were analyzed. -- Abstract: In this paper, YVO 4 :Yb 3+ ,Er 3+ nanoparticles have been successfully prepared via a facile hydrothermal technique in the presence of citric acid as a complexing agent followed by a subsequent heat treatment process. The nanostructures, morphologies and upconversion luminescent properties of the as-prepared YVO 4 :Yb 3+ ,Er 3+ upconverting nanoparticles were investigated by X-ray diffraction (XRD), transmission electron microscopy (TEM) and photoluminescent (PL) spectra. XRD results indicate that all the diffraction peaks of samples can be well indexed to the tetragonal phase of YVO 4 . TEM images demonstrate that the samples synthesized hydrothermally consist of granular-like nanoparticles ranging in size from about 30 to 50 nm. After being calcined at 500–800 °C for 2 h, the grain sizes of nanoparticles increase slightly. Additionally, the as-prepared nanoparticles show bright green luminescence corresponding to the 2 H 11/2 → 4 I 15/2 and 4 S 3/2 → 4 I 15/2 transitions of Er 3+ ions under the excitation of a 980 nm diode laser, which might find potential applications in fields such as phosphor powders, infrared detection and display devices

Controllable synthesis of (NH4)Fe2(PO4)2(OH)·2H2O using two-step route: Ultrasonic-intensified impinging stream pre-treatment followed by hydrothermal treatment.

Science.gov (United States)

Dong, Bin; Li, Guang; Yang, Xiaogang; Chen, Luming; Chen, George Z

2018-04-01

(NH 4 )Fe 2 (PO 4 ) 2 (OH)·2H 2 O samples with different morphology are successfully synthesized via two-step synthesis route - ultrasonic-intensified impinging stream pre-treatment followed by hydrothermal treatment (UIHT) method. The effects of the adoption of ultrasonic-intensified impinging stream pre-treatment, reagent concentration (C), pH value of solution and hydrothermal reaction time (T) on the physical and chemical properties of the synthesised (NH 4 )Fe 2 (PO 4 ) 2 (OH)·2H 2 O composites and FePO 4 particles were systematically investigated. Nano-seeds were firstly synthesized using the ultrasonic-intensified T-mixer and these nano-seeds were then transferred into a hydrothermal reactor, heated at 170 °C for 4 h. The obtained samples were characterized by utilising XRD, BET, TG-DTA, SEM, TEM, Mastersizer 3000 and FTIR, respectively. The experimental results have indicated that the particle size and morphology of the obtained samples are remarkably affected by the use of ultrasonic-intensified impinging stream pre-treatment, hydrothermal reaction time, reagent concentration, and pH value of solution. When such (NH 4 )Fe 2 (PO 4 ) 2 (OH)·2H 2 O precursor samples were transformed to FePO 4 products after sintering at 650 °C for 10 h, the SEM images have clearly shown that both the precursor and the final product still retain their monodispersed spherical microstructures with similar particle size of about 3 μm when the samples are synthesised at the optimised condition. Copyright © 2017 Elsevier B.V. All rights reserved.

Facile one-step hydrothermal synthesis and luminescence properties of Eu{sup 3+}-doped NaGd(WO{sub 4}){sub 2} nanophosphors

Energy Technology Data Exchange (ETDEWEB)

Jiang, Zehan; Cai, Peiqing; Chen, Cuili; Pu, Xipeng; Kim, Sun Il, E-mail: sikim@pknu.ac.kr; Jin Seo, Hyo, E-mail: hjseo@pknu.ac.kr

2017-06-01

Eu{sup 3+}-doped NaGd(WO{sub 4}){sub 2} nanophosphors were synthesized via a facile one-step hydrothermal method without any surfactants or a further heat treatment. X-ray powder diffraction (XRD), scanning electron microscope (SEM), fourier transform infrared spectroscopy (FT-IR), the photoluminescence (PL) excitation and emission spectra, and decay curves were used to characterize NaGd(WO{sub 4}){sub 2}:Eu{sup 3+} phosphors. The results show that the Eu{sup 3+}-concentration has little influence on the structure and morphology of the as-synthesized samples. However, pH value plays a vital role on the structure and morphology of NaGd(WO{sub 4}){sub 2}. The well-crystallized sheet-like NaGd(WO{sub 4}){sub 2} phosphors can be obtained only at pH = 5–7. On the basis of the time-dependent synthesis, a possible growth mechanism of sheet-like architectures is proposed. The luminescence properties of NaGd{sub 1-x}Eu{sub x}(WO{sub 4}){sub 2} (0 ≤ x ≤ 1) are investigated. It is found that the charge transfer band of Eu{sup 3+} shifts to lower energy and broadens with increasing the Eu{sup 3+}-concentration. - Highlights: • NaGd(WO{sub 4}){sub 2}:Eu{sup 3+} nanosheets were synthesized by facile one-step hydrothermal method. • Luminescence properties of NaGd(WO{sub 4}){sub 2}:Eu{sup 3+} phosphor were firstly reported. • The CT band of Eu{sup 3+} depends strongly on Eu{sup 3+}-concentrations.

Determination of major aromatic constituents in vanilla using an on-line supercritical fluid extraction coupled with supercritical fluid chromatography.

Science.gov (United States)

Liang, Yanshan; Liu, Jiaqi; Zhong, Qisheng; Shen, Lingling; Yao, Jinting; Huang, Taohong; Zhou, Ting

2018-04-01

An on-line supercritical fluid extraction coupled with supercritical fluid chromatography method was developed for the determination of four major aromatic constituents in vanilla. The parameters of supercritical fluid extraction were systematically investigated using single factor optimization experiments and response surface methodology by a Box-Behnken design. The modifier ratio, split ratio, and the extraction temperature and pressure were the major parameters which have significant effects on the extraction. While the static extraction time, dynamic extraction time, and recycle time had little influence on the compounds with low polarity. Under the optimized conditions, the relative extraction efficiencies of all the constituents reached 89.0-95.1%. The limits of quantification were in the range of 1.123-4.747 μg. The limits of detection were in the range of 0.3368-1.424 μg. The recoveries of the four analytes were in the range of 76.1-88.9%. The relative standard deviations of intra- and interday precision ranged from 4.2 to 7.6%. Compared with other off-line methods, the present method obtained higher extraction yields for all four aromatic constituents. Finally, this method has been applied to the analysis of vanilla from different sources. On the basis of the results, the on-line supercritical fluid extraction-supercritical fluid chromatography method shows great promise in the analysis of aromatic constituents in natural products. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Coprecipitation-assisted hydrothermal synthesis of PLZT hollow nanospheres

International Nuclear Information System (INIS)

Zhu, Renqiang; Zhu, Kongjun; Qiu, Jinhao; Bai, Lin; Ji, Hongli

2010-01-01

Lanthanum-modified lead zirconate titanate Pb 1-x La x (Zr 1-y Ti y )O 3 (PLZT) hollow nanospheres have been successfully prepared via a template-free hydrothermal method using the well-mixed coprecipitated precursors and the KOH mineralizer. The structure, composition, and morphology of the PLZT hollow nanospheres were characterized by XRD (X-ray diffraction), ICP (inductive coupled plasma emission spectrometer), FTIR (Fourier transform infrared spectra), TG/DTA (thermogravimetric analysis and differential thermal analysis), TEM (transmission electron microscopy) and SEAD (selected area diffraction). The results show that the composition and the morphology control of the PLZT products are determined by the KOH concentration. The PLZT hollow nanospheres with uniform size of about 4 nm were synthesized in the presence of 5 M KOH. The crystalline nanoparticles can be prepared at dilute KOH, in contrast to the amorphous powders prepared at concentrated KOH. Formation mechanisms of the PLZT hollow nanospheres are also discussed.

Photoluminescence properties of PZT 52/48 synthesized by microwave hydrothermal method using PVA with template

Energy Technology Data Exchange (ETDEWEB)

Teixeira, G.F., E-mail: guilmina@hotmail.com [Instituto de Quimica, Universidade Estadual Paulista, Departamento de Bioquimica e Tecnologia Quimica, Rua Francisco Degni s/n, Quitandinha, 14800-900 Araraquara, SP (Brazil); Gasparotto, G. [Instituto de Quimica, Universidade Estadual Paulista, Departamento de Bioquimica e Tecnologia Quimica, Rua Francisco Degni s/n, Quitandinha, 14800-900 Araraquara, SP (Brazil); Paris, E.C. [Empresa Brasileira de Pesquisa Agropecuaria, Embrapa Instrumentacao, Rua XV de novembro, 1452, Centro, 13.569-970 Sao Carlos, SP (Brazil); Zaghete, M.A.; Longo, E.; Varela, J.A. [Instituto de Quimica, Universidade Estadual Paulista, Departamento de Bioquimica e Tecnologia Quimica, Rua Francisco Degni s/n, Quitandinha, 14800-900 Araraquara, SP (Brazil)

2012-01-15

Lead Titanate Zirconate (PZT) perovskite powders were synthesized by microwave hydrothermal method (M-H) at 180 {sup o}C for different time periods (2, 4, 8 and 12 h) with the presence of aqueous polyvinyl alcohol (PVA) solution 0.36 g L{sup -1}. The X-Ray diffraction (XRD), SE-FEG as well as the measurements of photoluminescence (PL) emission were used for monitoring the formation of a perovskite phase with random polycrystalline distortion in the structure. Emission spectra with fixed excitation wavelength of 350 nm showed higher value for the powder obtained after undergoing 8 h of treatment. A theoretical model derived from previous calculations allows us to discuss the origin of photoluminescence emission in the powders, which can be further related to the local disorder in the network of both ZrO{sub 6} and TiO{sub 6} octahedral, and dodecahedral PbO{sub 12}. The new morphology initially observed from the PZT perovskite crystal growth bearing the shape of fine plates is found to be directly related to photoluminescence emission with energy lower than that present in the PZT with cube-like morphology that emits in 560 nm. - Highlights: > This work details the efficiency of microwave hydrothermal synthesis in obtaining PZT powders. > PVA is used as a crystallization agent of PZT particles. > PZT particles presented photoluminescent (PL) behavior. > There aren't previous reports of photoluminescent PZT obtained by microwave hydrothermal synthesis. > Photoluminescence is one more interesting property for technological applications this material.

Heat Transfer Phenomena of Supercritical Fluids

Energy Technology Data Exchange (ETDEWEB)

Krau, Carmen Isabella; Kuhn, Dietmar; Schulenberg, Thomas [Forschungszentrum Karlsruhe, Institute for Nuclear and Energy Technologies, 76021 Karlsruhe (Germany)

2008-07-01

In concepts for supercritical water cooled reactors, the reactor core is cooled and moderated by water at supercritical pressures. The significant temperature dependence of the fluid properties of water requires an exact knowledge of the heat transfer mechanism to avoid fuel pin damages. Near the pseudo-critical point a deterioration of heat transfer might happen. Processes, that take place in this case, are not fully understood and are due to be examined systematically. In this paper a general overview on the properties of supercritical water is given, experimental observations of different authors will be reviewed in order to identify heat transfer phenomena and onset of occurrence. The conceptional design of a test rig to investigate heat transfer in the boundary layer will be discussed. Both, water and carbon dioxide, may serve as operating fluids. The loop, including instrumentation and safety devices, is shown and suitable measuring methods are described. (authors)

Upgrading of bitumen using supercritical water

Energy Technology Data Exchange (ETDEWEB)

Kayukawa, T. [JGC Corp., Ibaraki (Japan)

2009-07-01

This presentation outlined the technical and economic aspects of thermal cracking by supercritical water. Supercritical water (SCW) is a commonly used method for upgrading heavy oil to produce pipeline-transportable oil from high-viscous bitumen. The process uses water and does not require hydrogen nor catalysts. Pre-heated bitumen and water enter a vertical reactor with flows of counter current at the supercritical point of water. The upgraded synthetic crude oil (SCO) and pitch are obtained from the top of the reactor when the bitumen is thermally cracked. Bench-scale studies have shown that Canadian oil sands bitumen can be converted to 80 volume per cent of SCO and 20 volume per cent of pitch. The SCO has satisfied Canadian pipeline specifications in terms of API gravity and kinetic viscosity. The kinetic viscosity of the pitch has also satisfied boiler fuel specifications. tabs., figs.

Hydrothermal synthesis and formation mechanism of hexagonal yttrium hydroxide fluoride nanobundles

International Nuclear Information System (INIS)

Tian, Li; Sun, QiLiang; Zhao, RuiNi; He, HuiLin; Xue, JianRong; Lin, Jun

2013-01-01

Graphical abstract: The formation of yttrium hydroxide fluorides nanobundles can be expressed as a precipitation transformation from cubic NaYF 4 to hexagonal NaYF 4 and to hexagonal Y(OH) 2.02 F 0.98 owing to ion exchange. - Highlights: • Novel Y(OH) 2.02 F 0.98 nanobundles have been successfully prepared by hydrothermal method. • The branched nanobundles composed of numerous oriented-attached nanoparticles has been studied. • The growth mechanism is proposed to be ion exchange and precipitation transformation. - Abstract: This article presents the fabrication of hexagonal yttrium hydroxide fluoride nanobundles via one-pot hydrothermal process, using yttrium nitrate, sodium hydroxide and ammonia fluoride as raw materials to react in propanetriol solvent. The X-ray diffraction pattern clearly reveals that the grown product is pure yttrium hydroxide fluoride, namely Y(OH) 2.02 F 0.98 . The morphology and microstructure of the synthesized product is testified to be nanobundles composed of numerous oriented-attached nanoparticles as observed from the field emission scanning electron microscopy (FESEM). The chemical composition was analyzed by the energy dispersive spectrum (EDS), confirming the phase transformation of the products which was clearly consistent with the result of XRD analysis. It is proposed that the growth of yttrium hydroxide fluoride nanobundles be attributed to ion exchange and precipitation transformation

Updated heat transfer correlations for supercritical water-cooled reactor applications

International Nuclear Information System (INIS)

Mokry, S.J.; Pioro, I.L.; Farah, A.; King, K.

2011-01-01

In support of the development of SuperCritical Water-cooled Reactors (SCWRs), research is currently being conducted for heat-transfer at supercritical conditions. Currently, there are no experimental datasets for heat transfer from power reactor fuel bundles to the fuel coolant (Water) available in open literature. Therefore, for preliminary calculations, heat-transfer correlations obtained with bare tube data can be used as a conservative approach. A large set of experimental data, for supercritical water was analyzed and an updated heat-transfer correlation for forced-convective heat-transfer, in the normal heat transfer regime, was developed. This experimental dataset was obtained within conditions similar to those for proposed SCWR concepts. Thus, this new correlation can be used for preliminary heat-transfer calculations in SCWR fuel channels. It has demonstrated a good fit for the analyzed dataset. Experiments with SuperCritical Water (SCW) are very expensive. Therefore, a number of experiments are performed in modeling fluids, such as carbon dioxide and refrigerants. However, there is no common opinion if SC modeling fluids' correlations can be applied to SCW and vice versa. Therefore, a correlation for supercritical carbon dioxide heat transfer was developed as a less expensive alternative to using supercritical water. The conducted analysis also meets the objective of improving our fundamental knowledge of the transport processes and handling of supercritical fluids. These correlations can be used for supercritical water heat exchangers linked to indirect-cycle concepts and the cogeneration of hydrogen, for future comparisons with other independent datasets, with bundle data, for the verification of computer codes for SCWR core thermalhydraulics and for the verification of scaling parameters between water and modeling fluids. (author)

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

Science.gov (United States)

Saji, Viswanathan S; Song, Hyun-Kon

2015-01-01

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

Potential of sub- and supercritical CO_2 reaction media for sol-gel deposition of silica-based molecular sieve membranes

International Nuclear Information System (INIS)

Durand, Veronique; Duchateau, Maxime; Drobek, Martin; Julbe, Anne; Hertz, Audrey; Ruiz, Jean-Christophe; Sarrade, Stephane

2014-01-01

A new eco-friendly method recently developed in our group has been further investigated for the preparation of gas selective silica-based molecular sieve membranes on/in macroporous tubular ceramic supports without any intermediate layer. The synthesis protocol under sub- and supercritical conditions was based on an 'On-Stream Supercritical Fluid Deposition method' (OS-SFD) applying supercritical carbon dioxide (scCO_2) as an attractive 'green' solvent with easily adjustable properties enabling a controlled solubilisation/reaction of precursors and their transport to the ceramic support. Parameters influencing the final membrane characteristics such as permeates flow rate, calcination treatment and deposition steps have been examined for a selected reaction mixture, transmembrane pressure and defined deposition temperatures. On-line monitoring of the membrane formation process (deposition signature curve) was used in this process. Membrane characteristics are discussed in correlation with their gas permeation properties. The optimized crack-free silica membranes prepared at 50 C have a compact microstructure but a thermal stability limited to 400 C. A second deposition run allowed a recovery of the molecular sieving behaviour with a thermally activated transport for He up to 350 C. These promising results demonstrate the potential of this novel method for the preparation of uniform molecular sieve membranes deposited directly on macroporous supports with virtually zero waste. (authors)

A finite-dimensional reduction method for slightly supercritical elliptic problems

Directory of Open Access Journals (Sweden)

Riccardo Molle

2004-01-01

Full Text Available We describe a finite-dimensional reduction method to find solutions for a class of slightly supercritical elliptic problems. A suitable truncation argument allows us to work in the usual Sobolev space even in the presence of supercritical nonlinearities: we modify the supercritical term in such a way to have subcritical approximating problems; for these problems, the finite-dimensional reduction can be obtained applying the methods already developed in the subcritical case; finally, we show that, if the truncation is realized at a sufficiently large level, then the solutions of the approximating problems, given by these methods, also solve the supercritical problems when the parameter is small enough.

Development of Nuclear Decontamination Technology Using Supercritical Fluid

Energy Technology Data Exchange (ETDEWEB)

Jung, Wonyoung; Park, Kwangheon; Park, Jihye; Lee, Donghee [Kyunghee Univ., Yongin (Korea, Republic of)

2014-05-15

Soil cleaning technologies that have been developed thus far increase treatment costs in contaminated soil recovery processes because they generate large amounts of secondary wastes. In this respect, this study is intended to develop soil decontamination methods using CO{sub 2}, which is a nontoxic, environmentally friendly substance, in order to fundamentally suppress the generation of secondary wastes from the decontamination process and to create high added values. In this study, to develop decontamination methods for uranium-contaminated soil using supercritical CO{sub 2}, a soil decontamination system using supercritical CO{sub 2} was constructed. In addition, the basic principle of supercritical CO{sub 2} decontamination using a TBP-HNO3 complex was explained. According to the results of the study, sea-sand samples having the same degree of contamination showed different results of decontamination according to the quantities of the TBP-HNO3 complex used as an extraction agent, which resulted in high extraction rates. Thus far, a most widely used method of extracting uranium has been the dissolving of uranium in acids. However, this method has the large adverse effect of generating strong acidic wastes that cannot be easily treated. On the other hand, supercritical CO{sub 2} requires critical conditions that are no more difficult to meet than those of other supercritical fluids, since its density can be changed from a very low state close to that of an ideal gas to a high state close to that of liquids. The critical gas conditions are a pressure of 71 bar and a temperature of 31 .deg. C, both of which are inexpensive to achieve. Moreover, CO{sub 2} is a solvent that is not harmful to the human body and few effects on environmental pollution. Therefore, nontoxic and environment friendly processes can be developed using supercritical CO{sub 2}. Supercritical CO{sub 2}'s advantages over prevailing methods suggest its potential for developing innovative

Development of Nuclear Decontamination Technology Using Supercritical Fluid

International Nuclear Information System (INIS)

Jung, Wonyoung; Park, Kwangheon; Park, Jihye; Lee, Donghee

2014-01-01

Soil cleaning technologies that have been developed thus far increase treatment costs in contaminated soil recovery processes because they generate large amounts of secondary wastes. In this respect, this study is intended to develop soil decontamination methods using CO 2 , which is a nontoxic, environmentally friendly substance, in order to fundamentally suppress the generation of secondary wastes from the decontamination process and to create high added values. In this study, to develop decontamination methods for uranium-contaminated soil using supercritical CO 2 , a soil decontamination system using supercritical CO 2 was constructed. In addition, the basic principle of supercritical CO 2 decontamination using a TBP-HNO3 complex was explained. According to the results of the study, sea-sand samples having the same degree of contamination showed different results of decontamination according to the quantities of the TBP-HNO3 complex used as an extraction agent, which resulted in high extraction rates. Thus far, a most widely used method of extracting uranium has been the dissolving of uranium in acids. However, this method has the large adverse effect of generating strong acidic wastes that cannot be easily treated. On the other hand, supercritical CO 2 requires critical conditions that are no more difficult to meet than those of other supercritical fluids, since its density can be changed from a very low state close to that of an ideal gas to a high state close to that of liquids. The critical gas conditions are a pressure of 71 bar and a temperature of 31 .deg. C, both of which are inexpensive to achieve. Moreover, CO 2 is a solvent that is not harmful to the human body and few effects on environmental pollution. Therefore, nontoxic and environment friendly processes can be developed using supercritical CO 2 . Supercritical CO 2 's advantages over prevailing methods suggest its potential for developing innovative decontamination methods, as demonstrated

Electrodeposition of germanium from supercritical fluids.

Science.gov (United States)

Ke, Jie; Bartlett, Philip N; Cook, David; Easun, Timothy L; George, Michael W; Levason, William; Reid, Gillian; Smith, David; Su, Wenta; Zhang, Wenjian

2012-01-28

Several Ge(II) and Ge(IV) compounds were investigated as possible reagents for the electrodeposition of Ge from liquid CH(3)CN and CH(2)F(2) and supercritical CO(2) containing as a co-solvent CH(3)CN (scCO(2)) and supercritical CH(2)F(2) (scCH(2)F(2)). For Ge(II) reagents the most promising results were obtained using [NBu(n)(4)][GeCl(3)]. However the reproducibility was poor and the reduction currents were significantly less than the estimated mass transport limited values. Deposition of Ge containing films was possible at high cathodic potential from [NBu(n)(4)][GeCl(3)] in liquid CH(3)CN and supercritical CO(2) containing CH(3)CN but in all cases they were heavily contaminated by C, O, F and Cl. Much more promising results were obtained using GeCl(4) in liquid CH(2)F(2) and supercritical CH(2)F(2). In this case the reduction currents were consistent with mass transport limited reduction and bulk electrodeposition produced amorphous films of Ge. Characterisation by XPS showed the presence of low levels of O, F and C, XPS confirmed the presence of Ge together with germanium oxides, and Raman spectroscopy showed that the as deposited amorphous Ge could be crystallised by the laser used in obtaining the Raman measurements.

Chemical deposition methods using supercritical fluid solutions

Science.gov (United States)

Sievers, Robert E.; Hansen, Brian N.

1990-01-01

A method for depositing a film of a desired material on a substrate comprises dissolving at least one reagent in a supercritical fluid comprising at least one solvent. Either the reagent is capable of reacting with or is a precursor of a compound capable of reacting with the solvent to form the desired product, or at least one additional reagent is included in the supercritical solution and is capable of reacting with or is a precursor of a compound capable of reacting with the first reagent or with a compound derived from the first reagent to form the desired material. The supercritical solution is expanded to produce a vapor or aerosol and a chemical reaction is induced in the vapor or aerosol so that a film of the desired material resulting from the chemical reaction is deposited on the substrate surface. In an alternate embodiment, the supercritical solution containing at least one reagent is expanded to produce a vapor or aerosol which is then mixed with a gas containing at least one additional reagent. A chemical reaction is induced in the resulting mixture so that a film of the desired material is deposited.

Optical wave microphone measurements of laser ablation of copper in supercritical carbon dioxide

Energy Technology Data Exchange (ETDEWEB)

Mitsugi, Fumiaki, E-mail: mitsugi@cs.kumamoto-u.ac.jp [Graduate School of Science and Technology, Kumamoto University, 2-39-1 Kurokami, Kumamoto 860-8555 (Japan); Ikegami, Tomoaki [Graduate School of Science and Technology, Kumamoto University, 2-39-1 Kurokami, Kumamoto 860-8555 (Japan); Nakamiya, Toshiyuki; Sonoda, Yoshito [Graduate School of Industrial Engineering, Tokai University, 9-1-1 Toroku, Kumamoto 862-8652 (Japan)

2013-11-29

Laser ablation plasma in a supercritical fluid has attracted much attention recently due to its usefulness in forming nanoparticles. Observation of the dynamic behavior of the supercritical fluid after laser irradiation of a solid is necessary for real-time monitoring and control of laser ablation. In this study, we utilized an optical wave microphone to monitor pulsed laser irradiation of a solid in a supercritical fluid. The optical wave microphone works based on Fraunhofer diffraction of phase modulation of light by changes in refractive index. We hereby report on our measurements for pulsed laser irradiation of a Cu target in supercritical carbon dioxide using an optical wave microphone. Photothermal acoustic waves which generated after single pulsed laser irradiation of a Cu target were detectable in supercritical carbon dioxide. The speed of sound around the critical point of supercritical carbon dioxide was clearly slower than that in gas. The optical wave microphone detected a signal during laser ablation of Cu in supercritical carbon dioxide that was caused by shockwave degeneration. - Highlights: • Photothermal acoustic wave in supercritical fluid was observed. • Sound speed around the critical point was slower than that in gas. • Optical wave microphone detected degeneration of a shockwave. • Ablation threshold of a solid in supercritical fluid can be estimated. • Generation of the second shockwave in supercritical phase was suggested.

Microwave assisted hydrothermal synthesis of Ag/AgCl/WO3 photocatalyst and its photocatalytic activity under simulated solar light

International Nuclear Information System (INIS)

Adhikari, Rajesh; Gyawali, Gobinda; Sekino, Tohru; Wohn Lee, Soo

2013-01-01

Simulated solar light responsive Ag/AgCl/WO 3 composite photocatalyst was synthesized by microwave assisted hydrothermal process. The synthesized powders were characterized by X-Ray Diffraction (XRD) spectroscopy, X-Ray Photoelectron Spectroscopy (XPS), Transmission Electron Microscopy (TEM), Diffuse Reflectance Spectroscopy (UV–Vis DRS), and BET surface area analyzer to investigate the crystal structure, morphology, chemical composition, optical properties and surface area of the composite photocatalyst. This photocatalyst exhibited higher photocatalytic activity for the degradation of rhodamine B under simulated solar light irradiation. Dye degradation efficiency of composite photocatalyst was found to be increased significantly as compared to that of the commercial WO 3 nanopowder. Increase in photocatalytic activity of the photocatalyst was explained on the basis of surface plasmon resonance (SPR) effect caused by the silver nanoparticles present in the composite photocatalyst. Highlights: ► Successful synthesis of Ag/AgCl/WO 3 nanocomposite. ► Photocatalytic experiment was performed under simulated solar light. ► Nanocomposite photocatalyst was very active as compared to WO 3 commercial powder. ► SPR effect due to Ag nanoparticles enhanced the photocatalytic activity.

A microporous potassium vanadyl phosphate analogue of mahnertite. Hydrothermal synthesis and crystal structure

International Nuclear Information System (INIS)

Yakubovich, Olga V.; Russian Academy of Science, Moscow; Steele, Ian M.; Kiriukhina, Galina V.; Dimitrova, Olga V.

2015-01-01

The novel phase K 2.5 Cu 5 Cl(PO 4 ) 4 (OH) 0.5 (VO 2 ).H 2 O was prepared by hydrothermal synthesis at 553 K. Its crystal structure was determined using low-temperature (100 K) single-crystal synchrotron diffraction data and refined against F 2 to R = 0.035. The compound crystallizes in the tetragonal space group I4/mmm, with unit-cell parameters a =9.8120(8), c = 19.954(1) Aa, V = 1921.1(2) Aa 3 , and Z = 4. Both symmetrically independent Cu 2+ sites show elongated square-pyramidal coordination. The V 5+ ions reside in strongly distorted five-vertex VO 5 polyhedra with 50% occupancy. The structure is based on a 3D anionic framework built from Cu- and V-centered five-vertex polyhedra and PO 4 tetrahedra. Channels in the [100] and [010] directions accommodate large K atoms and H 2 O molecules. The compound is a new structural representative of the topology shown by the lavendulan group of copper arsenate and phosphate minerals. Their tetragonal or pseudotetragonal crystal structures are characterized by two types of 2D slabs alternating along one axis of their unit cells. One slab, described by the formula [Cu 4 X(TO 4 ) 4 ] 8 (where X = Cl, O and T = As, P), is common to all phases, whereas the slab content of the other set differs among the group members. We suggest interpreting this family of compounds in terms of the modular concept and also consider the synthetic phase Ba(VO)Cu 4 (PO 4 ) 4 as a simplest member of this polysomatic series.

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.

The Iceland Deep Drilling Project 4.5 km deep well, IDDP-2, in the seawater-recharged Reykjanes geothermal field in SW Iceland has successfully reached its supercritical target

Science.gov (United States)

Friðleifsson, Guðmundur Ó.; Elders, Wilfred A.; Zierenberg, Robert A.; Stefánsson, Ari; Fowler, Andrew P. G.; Weisenberger, Tobias B.; Harðarson, Björn S.; Mesfin, Kiflom G.

2017-11-01

The Iceland Deep Drilling Project research well RN-15/IDDP-2 at Reykjanes, Iceland, reached its target of supercritical conditions at a depth of 4.5 km in January 2017. After only 6 days of heating, the measured bottom hole temperature was 426 °C, and the fluid pressure was 34 MPa. The southern tip of the Reykjanes peninsula is the landward extension of the Mid-Atlantic Ridge in Iceland. Reykjanes is unique among Icelandic geothermal systems in that it is recharged by seawater, which has a critical point of 406 °C at 29.8 MPa. The geologic setting and fluid characteristics at Reykjanes provide a geochemical analog that allows us to investigate the roots of a mid-ocean ridge submarine black smoker hydrothermal system. Drilling began with deepening an existing 2.5 km deep vertical production well (RN-15) to 3 km depth, followed by inclined drilling directed towards the main upflow zone of the system, for a total slant depth of 4659 m ( ˜ 4.5 km vertical depth). Total circulation losses of drilling fluid were encountered below 2.5 km, which could not be cured using lost circulation blocking materials or multiple cement jobs. Accordingly, drilling continued to the total depth without return of drill cuttings. Thirteen spot coring attempts were made below 3 km depth. Rocks in the cores are basalts and dolerites with alteration ranging from upper greenschist facies to amphibolite facies, suggesting that formation temperatures at depth exceed 450 °C. High-permeability circulation-fluid loss zones (feed points or feed zones) were detected at multiple depth levels below 3 km depth to bottom. The largest circulation losses (most permeable zones) occurred between the bottom of the casing and 3.4 km depth. Permeable zones encountered below 3.4 km accepted less than 5 % of the injected water. Currently, the project is attempting soft stimulation to increase deep permeability. While it is too early to speculate on the energy potential of this well and its economics, the IDDP

Niobium (V) doped bioceramics: evaluation of the hydrothermal route modified with citric acid and urea to obtain modified hydroxyapatite

International Nuclear Information System (INIS)

Simomukay, E.; Souza, E.C.F. de; Antunes, S.R.M.; Borges, C.P.F.; Michel, M.D.; Antunes, A.C.

2016-01-01

Synthetic hydroxyapatite (Ca 10 (PO 4 ) 6 (OH) 2 ; HA) has become a widely used ceramic material for bone reconstruction due to its biocompatibility with the bone tissue. This biocompatibility as well as other physical and chemical properties of the hydroxyapatite can be modified by the addition of different ions to its structure. Niobium (V) ion has not been commonly used in the hydroxyapatite synthesis. The objective of this study was to evaluate the use of hydrothermal route in the niobium (V) doped hydroxyapatite synthesis. The route used the niobium ammonium oxalate (NH 4 H 2 [NbO(C 2 O 4 ) 3 ].3H 2 O) complex as a niobium (V) ion precursor. The addition of citric acid and urea in the hydrothermal route is used for the control of synthesis pH and precipitation rate. Pure sample and sample added with 5.3 ppm of niobium (V) ion were prepared. The coexistence of other phases besides the hydroxyapatite was not observed in any of the samples through the use of X-ray diffraction and infrared spectroscopy (FTIR) techniques. The FTIR technique revealed the presence of hydroxyapatite characteristic functional groups. The scanning electron microscopy analysis showed the formation of agglomerates composed of round particles, confirmed by the transmission electron microscopy technique. The X-ray fluorescence spectroscopic analysis detected the presence of niobium in the doped sample. The results showed that niobium (V) doped hydroxyapatite can be synthesized by means of hydrothermal route, which may be considered as huge potential for future application in bioceramics. (author)

High Density Thermal Energy Storage with Supercritical Fluids

Science.gov (United States)

Ganapathi, Gani B.; Wirz, Richard

2012-01-01

A novel approach to storing thermal energy with supercritical fluids is being investigated, which if successful, promises to transform the way thermal energy is captured and utilized. The use of supercritical fluids allows cost-affordable high-density storage with a combination of latent heat and sensible heat in the two-phase as well as the supercritical state. This technology will enhance penetration of several thermal power generation applications and high temperature water for commercial use if the overall cost of the technology can be demonstrated to be lower than the current state-of-the-art molten salt using sodium nitrate and potassium nitrate eutectic mixtures.

Selective free radical reactions using supercritical carbon dioxide.

Science.gov (United States)

Cormier, Philip J; Clarke, Ryan M; McFadden, Ryan M L; Ghandi, Khashayar

2014-02-12

We report herein a means to modify the reactivity of alkenes, and particularly to modify their selectivity toward reactions with nonpolar reactants (e.g., nonpolar free radicals) in supercritical carbon dioxide near the critical point. Rate constants for free radical addition of the light hydrogen isotope muonium to ethylene, vinylidene fluoride, and vinylidene chloride in supercritical carbon dioxide are compared over a range of pressures and temperatures. Near carbon dioxide's critical point, the addition to ethylene exhibits critical speeding up, while the halogenated analogues display critical slowing. This suggests that supercritical carbon dioxide as a solvent may be used to tune alkene chemistry in near-critical conditions.

Dissolution-Induced Nanowire Synthesis on Hot-Dip Galvanized Surface in Supercritical Carbon Dioxide

Directory of Open Access Journals (Sweden)

Aaretti Kaleva

2017-07-01

Full Text Available In this study, we demonstrate a rapid treatment method for producing a needle-like nanowire structure on a hot-dip galvanized sheet at a temperature of 50 °C. The processing method involved only supercritical carbon dioxide and water to induce a reaction on the zinc surface, which resulted in growth of zinc hydroxycarbonate nanowires into flower-like shapes. This artificial patina nanostructure predicts high surface area and offers interesting opportunities for its use in industrial high-end applications. The nanowires can significantly improve paint adhesion and promote electrochemical stability for organic coatings, or be converted to ZnO nanostructures by calcining to be used in various semiconductor applications.

using Supercritical Fluid Extraction

African Journals Online (AJOL)

Methods: Supercritical CO2 extraction technology was adopted in this experiment to study the process of extraction of volatile oil from Polygonatum odoratum while gas chromatograph-mass spectrometer ..... Saponin rich fractions from.

Catalyst retention in continuous flow with supercritical carbon dioxide

NARCIS (Netherlands)

Stouten, S.C.; Noel, T.; Wang, Q.; Hessel, V.

2014-01-01

This review discusses the retention of organometallic catalysts in continuous flow processes utilizing supercritical carbon dioxide. Due to its innovative properties, supercritical carbon dioxide offers interesting possibilities for process intensification. As a result of safety and cost

A rapid hydrothermal synthesis of rutile SnO2 nanowires

International Nuclear Information System (INIS)

Lupan, O.; Chow, L.; Chai, G.; Schulte, A.; Park, S.; Heinrich, H.

2009-01-01

Tin oxide (SnO 2 ) nanowires with rutile structure have been synthesized by a facile hydrothermal method at 98 deg. C. The morphologies and structural properties of the as-grown nanowires/nanoneedles were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), selected area electron diffraction, X-ray diffraction and Raman spectroscopy. The SEM images reveal tetragonal nanowires of about 10-100 μm in length and 50-100 nm in radius. The Raman scattering peaks indicate a typical rutile phase of the SnO 2 . The effects of molar ratio of SnCl 4 to NH 4 OH on the growth mechanism are discussed

Dye-Sensitized Solar Cells with Anatase TiO2 Nanorods Prepared by Hydrothermal Method

Directory of Open Access Journals (Sweden)

Ming-Jer Jeng

2013-01-01

Full Text Available The hydrothermal method provides an effective reaction environment for the synthesis of nanocrystalline materials with high purity and well-controlled crystallinity. In this work, we started with various sizes of commercial TiO2 powders and used the hydrothermal method to prepare TiO2 thin films. We found that the synthesized TiO2 nanorods were thin and long when smaller TiO2 particles were used, while larger TiO2 particles produced thicker and shorter nanorods. We also found that TiO2 films prepared by TiO2 nanorods exhibited larger surface roughness than those prepared by the commercial TiO2 particles. It was found that a pure anatase phase of TiO2 nanorods can be obtained from the hydrothermal method. The dye-sensitized solar cells fabricated with TiO2 nanorods exhibited a higher solar efficiency than those fabricated with commercial TiO2 nanoparticles directly. Further, triple-layer structures of TiO2 thin films with different particle sizes were investigated to improve the solar efficiency.

Industrial applications and current trends in supercritical fluid technologies

Directory of Open Access Journals (Sweden)

Gamse Thomas

2005-01-01

Full Text Available Supercritical fluids have a great potential for wide fields of processes Although CO2 is still one of the most used supercritical gases, for special purposes propane or even fluorinated-chlorinated fluids have also been tested. The specific characteristics of supercritical fluids behaviour were analyzed such as for example the solubilities of different components and the phase equilibria between the solute and solvent. The application at industrial scale (decaffeinating of tea and coffee, hop extraction or removal of pesticides from rice, activity in supercritical extraction producing total extract from the raw material or different fractions by using the fractionated separation of beverages (rum, cognac, whisky, wine, beer cider, of citrus oils and of lipids (fish oils, tall oil were also discussed. The main interest is still for the extraction of natural raw materials producing food ingredients, nutraceuticals and phytopharmaceuticals but also cleaning purposes were tested such as the decontamination of soils the removal of residual solvents from pharmaceutical products, the extraction of flame retardants from electronic waste or precision degreasing and cleaning of mechanical and electronic parts. An increasing interest obviously exists for impregnation purposes based on supercritical fluids behaviour, as well as for the dying of fibres and textiles. The production of fine particles in the micron and submicron range, mainly for pharmaceutical products is another important application of supercritical fluids. Completely new products can be produced which is not possible under normal conditions. Supercritical fluid technology has always had to compete with the widespread opinion that these processes are very expensive due to very high investment costs in comparison with classical low-pressure equipment. Thus the opinion is that these processes should be restricted to high-added value products. A cost estimation for different plant sizes and

EDTA-assisted hydrothermal synthesis, characterization and photoluminescent properties of Mn{sup 2+}-doped ZnS

Energy Technology Data Exchange (ETDEWEB)

Viswanath, R. [Department of Studies and Research in Industrial Chemistry, School of Chemical Sciences, Kuvempu University, Shankaraghatta-577 451 (India); Bhojya Naik, H.S., E-mail: hsb_naik@rediffmail.com [Department of Studies and Research in Industrial Chemistry, School of Chemical Sciences, Kuvempu University, Shankaraghatta-577 451 (India); Yashavanth Kumar, G.S.; Prashanth Kumar, P.N.; Arun Kumar, G. [Department of Studies and Research in Industrial Chemistry, School of Chemical Sciences, Kuvempu University, Shankaraghatta-577 451 (India); Praveen, R. [Department of Technical Education, Automobile Technology Branch HMS Polytechnic (Government Aided), Tumkur-572102 (India)

2014-09-15

linked with suitable biomolecules. - Highlights: • Hydrothermal synthesis of EDTA-assisted ZnS:Mn{sup 2+} nanoparticles with 3–4 nm. • Well-defined quantum confinement effect Eg (NPs) = 4.59 eV > Eg (bulk) = 3.64 eV. • Investigation of fixed blue region with the red shift in yellow–orange region. • Origin of the additional luminescence observed.

Particle Formation by Supercritical Fluid Extraction and Expansion Process

Directory of Open Access Journals (Sweden)

Sujuan Pan

2013-01-01

Full Text Available Supercritical fluid extraction and expansion (SFEE patented technology combines the advantages of both supercritical fluid extraction (SFE and rapid expansion of supercritical solution (RESS with on-line coupling, which makes the nanoparticle formation feasible directly from matrix such as Chinese herbal medicine. Supercritical fluid extraction is a green separation technology, which has been developed for decades and widely applied in traditional Chinese medicines or natural active components. In this paper, a SFEE patented instrument was firstly built up and controlled by LABVIEW work stations. Stearic acid was used to verify the SFEE process at optimized condition; via adjusting the preexpansion pressure and temperature one can get different sizes of particles. Furthermore, stearic acid was purified during the SFEE process with HPLC-ELSD detecting device; purity of stearic acid increased by 19%, and the device can purify stearic acid.

Destruction of polyphasic systems in supercritical water reaction media

International Nuclear Information System (INIS)

Leybros, A.

2009-12-01

Spent ion exchange resins (IER) are, hence, radioactive process wastes for which there is no satisfactory industrial treatment. Supercritical water oxidation offers a viable alternative treatment to destroy the organic structure of resins by using supercritical water properties. The reactor used in Supercritical Fluids and Membranes Laboratory is a double shell stirred reactor. Total Organic Carbon reduction rates higher than 99% were obtained thanks to POSCEA2 experimental set-up when using a co-fuel, isopropyl alcohol. Influence of operating parameters was studied. A detailed reactional mechanism for cationic and anionic resins is created. For the solubilization of the particles in supercritical water, a mechanism has been created with the identified rate determining species and implemented into Fluent software through the EDC approach. Experimental temperature profiles are well represented by EDC model. Reaction rates are hence controlled by the chemical species mixing. (author)

Supercritical Water Reactor Cycle for Medium Power Applications

International Nuclear Information System (INIS)

BD Middleton; J Buongiorno

2007-01-01

Scoping studies for a power conversion system based on a direct-cycle supercritical water reactor have been conducted. The electric power range of interest is 5-30 MWe with a design point of 20 MWe. The overall design objective is to develop a system that has minimized physical size and performs satisfactorily over a broad range of operating conditions. The design constraints are as follows: Net cycle thermal efficiency (ge)20%; Steam turbine outlet quality (ge)90%; and Pumping power (le)2500 kW (at nominal conditions). Three basic cycle configurations were analyzed. Listed in order of increased plant complexity, they are: (1) Simple supercritical Rankine cycle; (2) All-supercritical Brayton cycle; and (3) Supercritical Rankine cycle with feedwater preheating. The sensitivity of these three configurations to various parameters, such as reactor exit temperature, reactor pressure, condenser pressure, etc., was assessed. The Thermoflex software package was used for this task. The results are as follows: (a) The simple supercritical Rankine cycle offers the greatest hardware simplification, but its high reactor temperature rise and reactor outlet temperature may pose serious problems from the viewpoint of thermal stresses, stability and materials in the core. (b) The all-supercritical Brayton cycle is not a contender, due to its poor thermal efficiency. (c) The supercritical Rankine cycle with feedwater preheating affords acceptable thermal efficiency with lower reactor temperature rise and outlet temperature. (d) The use of a moisture separator improves the performance of the supercritical Rankine cycle with feedwater preheating and allows for a further reduction of the reactor outlet temperature, thus it was selected for the next step. Preliminary engineering design of the supercritical Rankine cycle with feedwater preheating and moisture separation was performed. All major components including the turbine, feedwater heater, feedwater pump, condenser, condenser pump

Lanthanide phosphonates: Synthesis, thermal stability and magnetic characterization

Energy Technology Data Exchange (ETDEWEB)

Amghouz, Z., E-mail: amghouz.uo@uniovi.es [Departamentos de Quimica Fisica y Analitica y Quimica Organica e Inorganica, Universidad de Oviedo - CINN, 33006 Oviedo (Spain); Garcia, J.R.; Garcia-Granda, S. [Departamentos de Quimica Fisica y Analitica y Quimica Organica e Inorganica, Universidad de Oviedo - CINN, 33006 Oviedo (Spain); Clearfield, A. [Department of Chemistry, Texas A and M University, College Station, TX 77842-3012 (United States); Rodriguez Fernandez, J.; Pedro, I. de [CITIMAC, Facultad de Ciencias, Universidad de Cantabria, 39005 Santander (Spain); Blanco, J.A. [Departamento de Fisica, Universidad de Oviedo, 33007 Oviedo (Spain)

2012-09-25

Highlights: Black-Right-Pointing-Pointer Report of the complete series of lanthanide 1,4-phenylbis(phosphonate). Black-Right-Pointing-Pointer Synthesis under conventional hydrothermal synthesis or microwave-assisted hydrothermal synthesis. Black-Right-Pointing-Pointer Cation size is the key factor for the structural and particles size variations. Black-Right-Pointing-Pointer Thermal behaviour is characterized by unusual very high thermal stability. - Abstract: Series of novel organic-inorganic hybrids materials based on trivalent lanthanides (Ln = Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu) and 1,4-phenylbis(phosphonate) obtained under hydrothermal conditions either by oven heat or microwave irradiation. The anhydrous compounds containing La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, and Ho, are isostructural. However, the compounds based on Y, Er, Tm, Yb, and Lu are hydrated and their structures have not yet been solved. The series of compounds are characterized by PXRD, TEM, SEM-EDX and thermal analyses (TG-MS and DSC). TEM study show a variable particles size with a minimum mean-particle size of ca. 30 nm. These compounds exhibit unusual very high thermal stability. The size of particles and the thermal stability are depending on lanthanide(III) cation features. All the investigated materials show paramagnetic behaviour. The magnetic susceptibility data follow a Curie-Weiss laws with paramagnetic effective moments in good agreement with those expected for Ln{sup 3+} free ions.

Sodium-dodecyl-sulphate-assisted synthesis of Ni nanoparticles ...

Indian Academy of Sciences (India)

2017-11-20

Nov 20, 2017 ... the SDS concentration, while at high concentration (mole ratio of SDS:Ni(acac)2 = 4:1), the small ... Over the last decades, synthesis of magnetic metallic ... pared nickel nanoparticles (3.7 nm) via hydrothermal method.

Hydrothermally processed 1D hydroxyapatite: Mechanism of formation and biocompatibility studies

Energy Technology Data Exchange (ETDEWEB)

Stojanović, Zoran S.; Ignjatović, Nenad [Centre for Fine Particles Processing and Nanotechnologies, Institute of Technical Sciences of the Serbian Academy of Sciences and Arts, Knez Mihailova 35/4, 11000 Belgrade (Serbia); Wu, Victoria [Advanced Materials and Nanobiotechnology Laboratory, Department of Bioengineering, University of Illinois, 851 South Morgan Street, Chicago, IL 60607-7052 (United States); Žunič, Vojka [Advanced Materials Department, Jožef Stefan Institute, Jamova cesta 39, 1000 Ljubljana (Slovenia); Veselinović, Ljiljana [Centre for Fine Particles Processing and Nanotechnologies, Institute of Technical Sciences of the Serbian Academy of Sciences and Arts, Knez Mihailova 35/4, 11000 Belgrade (Serbia); Škapin, Srečo [Advanced Materials Department, Jožef Stefan Institute, Jamova cesta 39, 1000 Ljubljana (Slovenia); Miljković, Miroslav [Laboratory for Electron Microscopy, Faculty of Medicine University of Niš, Dr. Zoran Đinđić Boulevard 81, 18 000 Niš (Serbia); Uskoković, Vuk [Advanced Materials and Nanobiotechnology Laboratory, Department of Bioengineering, University of Illinois, 851 South Morgan Street, Chicago, IL 60607-7052 (United States); Department of Biomedical and Pharmaceutical Sciences, School of Pharmacy, Chapman University, 9401 Jeronimo Road, Irvine, CA 92618-1908 (United States); and others

2016-11-01

Recent developments in bone tissue engineering have led to an increased interest in one-dimensional (1D) hydroxyapatite (HA) nano- and micro-structures such as wires, ribbons and tubes. They have been proposed for use as cell substrates, reinforcing phases in composites and carriers for biologically active substances. Here we demonstrate the synthesis of 1D HA structures using an optimized, urea-assisted, high-yield hydrothermal batch process. The one-pot process, yielding HA structures composed of bundles of ribbons and wires, was typified by the simultaneous occurrence of a multitude of intermediate reactions, failing to meet the uniformity criteria over particle morphology and size. To overcome these issues, the preparation procedure was divided to two stages: dicalcium phosphate platelets synthesized in the first step were used as a precursor for the synthesis of 1D HA in the second stage. Despite the elongated particle morphologies, both the precursor and the final product exhibited excellent biocompatibility and caused no reduction of viability when tested against osteoblastic MC3T3-E1 cells in 2D culture up to the concentration of 2.6 mg/cm{sup 2}. X-ray powder diffraction combined with a range of electron microscopies and laser diffraction analyses was used to elucidate the formation mechanism and the microstructure of the final particles. The two-step synthesis involved a more direct transformation of DCP to 1D HA with the average diameter of 37 nm and the aspect ratio exceeding 100:1. The comparison of crystalline domain sizes along different crystallographic directions showed no signs of significant anisotropy, while indicating that individual nanowires are ordered in bundles in the b crystallographic direction of the P6{sub 3/m} space group of HA. Intermediate processes, e.g., dehydration of dicalcium phosphate, are critical for the formation of 1D HA alongside other key aspects of this phase transformation, it must be investigated in more detail in the

Hydrothermal synthesis of CdS nanoparticle/functionalized graphene sheet nanocomposites for visible-light photocatalytic degradation of methyl orange

International Nuclear Information System (INIS)

Yan, Shancheng; Wang, Bojun; Shi, Yi; Yang, Fan; Hu, Dong; Xu, Xin; Wu, Jiansheng

2013-01-01

CdS nanoparticle/functionalized graphene sheet (CdS NP/FGS) nanocomposites were successfully prepared in a one-step hydrothermal synthesis route. The samples were characterized by field emission scanning electron microscopy, transmission electron microscopy, X-ray diffraction, X-ray photoelectron spectroscopy, Fourier transform infrared spectroscopy, photoluminescence spectroscopy, and Raman spectroscopy. In addition, the photocatalytic performance of CdS NP/FGS composites and pure CdS in the degradation of methyl orange (MO) was examined using visible light. Results show that the addition of FGS can enhance the photocatalytic performance of CdS NP/FGS composites with a maximum degradation efficiency of 98.1% under visible light irradiation as compared with pure CdS (60.1%). This finding can be attributed to three reasons. First is the strong redox ability of CdS in the nanocomposite with smaller crystal size. Second is the increase in specific surface area for more adsorbed MO. Third is the reduction in electron–hole pair recombination with the introduction of FGS. Based on their high photocatalytic activity, the CdS NP/FGS composites can be expected to be a practical visible light photocatalyst.

Hydrothermal synthesis of CdS nanoparticle/functionalized graphene sheet nanocomposites for visible-light photocatalytic degradation of methyl orange

Energy Technology Data Exchange (ETDEWEB)

Yan, Shancheng, E-mail: yansc@njupt.edu.cn [School of Geography and Biological Information, Nanjing University of Posts and Telecommunications, Nanjing 210046 (China); National Laboratory of Solid State Microstructures, School of Electronic Science and Engineering, Nanjing University, Nanjing 210093 (China); Wang, Bojun [School of Geography and Biological Information, Nanjing University of Posts and Telecommunications, Nanjing 210046 (China); Shi, Yi [National Laboratory of Solid State Microstructures, School of Electronic Science and Engineering, Nanjing University, Nanjing 210093 (China); Yang, Fan; Hu, Dong; Xu, Xin; Wu, Jiansheng [School of Geography and Biological Information, Nanjing University of Posts and Telecommunications, Nanjing 210046 (China)

2013-11-15

CdS nanoparticle/functionalized graphene sheet (CdS NP/FGS) nanocomposites were successfully prepared in a one-step hydrothermal synthesis route. The samples were characterized by field emission scanning electron microscopy, transmission electron microscopy, X-ray diffraction, X-ray photoelectron spectroscopy, Fourier transform infrared spectroscopy, photoluminescence spectroscopy, and Raman spectroscopy. In addition, the photocatalytic performance of CdS NP/FGS composites and pure CdS in the degradation of methyl orange (MO) was examined using visible light. Results show that the addition of FGS can enhance the photocatalytic performance of CdS NP/FGS composites with a maximum degradation efficiency of 98.1% under visible light irradiation as compared with pure CdS (60.1%). This finding can be attributed to three reasons. First is the strong redox ability of CdS in the nanocomposite with smaller crystal size. Second is the increase in specific surface area for more adsorbed MO. Third is the reduction in electron–hole pair recombination with the introduction of FGS. Based on their high photocatalytic activity, the CdS NP/FGS composites can be expected to be a practical visible light photocatalyst.

Thermodynamic Aspects of Supercritical Fluids Processing: Applications of Polymers and Wastes Treatment Aspects thermodynamiques des procédés mettant en oeuvre des fluides supercritiques : applications aux traitements des polymères et des déchets

Directory of Open Access Journals (Sweden)

Beslin P.

2006-11-01

Full Text Available Supercritical fluid processes are of increasing interest for many fields : in supercritical fluid separation (petroleum-chemistry separation and purification, food industry and supercritical fluid chromatography (analytical and preparative separation, determination of physicochemical properties; as reaction media with continuously adjustable properties from gas to liquid (low-density polyethylene, waste destruction, polymer recycling; in geology and mineralogy (volcanoes, geothermal energy, hydrothermal synthesis; in particle, fibber and substrate formations (pharmaceuticals, explosives, coatings; in drying materials (gels. This paper presents the unusual physicochemical properties of supercritical fluids in relation to their engineering applications. After a short report of fundamental concepts of critical behavior in pure fluids, we develop in more details the tunable physicochemical properties of fluid in the supercritical domain. The second part of this paper describes the engineering applications of supercritical fluids relevant of chemical reactions and polymer processing. Each application presentation is divided in two parts : the first one recalls the basic concepts including general background, physicochemical properties and the second one develops the engineering applications relevant of the advocated domain. La mise en Suvre des fluides supercritiques est d'un intérêt croissant dans de nombreux domaines : pour la séparation (séparation et purification en pétrochimie, industrie alimentaire et la chromatographie par fluides supercritiques (séparation analytique et préparatoire, détermination des propriétés physicochimiques, comme milieux réactifs aux propriétés continûment ajustables allant du gaz au liquide (polyéthylène de faible densité, élimination des déchets, recyclage des polymères, en géologie et en minéralogie (volcanologie, énergie géothermique, synthèse hydrothermique, dans la formation des particules

Hydrothermal synthesis of silico-manganese nanohybrid for Cu(II) adsorption from aqueous solution

Energy Technology Data Exchange (ETDEWEB)

Zhu, Qiufeng, E-mail: zhuqiufeng@th.btbu.edu.cn; Wang, Liting; An, Zehuan; Ye, Hong; Feng, Xudong

2016-05-15

Highlights: • A novel silico-manganese nanohybrid adsorbent (SMNA) was synthesized by a hydrothermal method. • The adsorption capacities of the SMNA for Cu(II) are lower pH dependency. • As-adsorbents are very efficient at low metal concentration and substantial amounts of Cu(II) can be removed from aqueous solution. - Abstract: A novel silico-manganese nanohybrid adsorbent (SMNA) was synthesized by a facile hydrothermal method, and characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), nitrogen adsorption-desorption, Fourier transform infrared spectroscopy (FT-IR) and zeta potential measurement. The adsorption of Cu(II) ions from aqueous solution on the SMNA was investigated with variations in contact time, pH and initial Cu(II) concentration. The results showed that hydrothermal method would generate nanowire/nanorod incomplete crystallite (δ-MnO{sub 2}) adsorbent. The adsorption of Cu(II) onto SMNA increased sharply within 25 min and reached equilibrium gradually. The maximum adsorption capacities of SMNA for Cu(II) were ∼40–88 mg g{sup −1}, which was lower than δ-MnO{sub 2} (92.42 mg g{sup −1}) but had a lower pH dependency. As compared with δ-MnO{sub 2}, higher adsorption capacities of SMNA (7.5–15 wt% of silica doping amount) for Cu(II) could be observed when pH of the aqueous solution was low (<4). The pseudo-second-order model was the best choice to describe the adsorption behavior of Cu(II) onto SMNA, suggesting that the removal of Cu(II) by the as-prepared adsorbents was dominated by migration of Cu(II). The possibility of Cu(II) recovery was also investigated and it revealed that SMNA was a promising recyclable adsorbent for removal of heavy metal ions in water and wastewater treatment.

Can supercritical oxidation of sewage sludge be an alternative for supercritical gasification?; Kan superkritische oxidatie van zuiveringsslib een alternatief zijn voor superkritische vergassing?

Energy Technology Data Exchange (ETDEWEB)

Rulkens, W. [Wageningen UR, Wageningen (Netherlands); Wentink, J. [Horizon Solutions, Leiden (Netherlands)

2013-05-15

In the context of the development of The Energy Factory a number of technologies has been identified that may be interesting to develop further. Two of these techniques relate to the conversion of sludge in supercritical water: supercritical gasification of sludge and supercritical oxidation of sludge [Dutch] In het kader van de ontwikkeling van De Energiefabriek is een aantal technologieen geidentificeerd die mogelijk interessant zijn om verder te ontwikkelen. Twee van deze technieken hebben betrekking op de conversie van slib in superkritisch water: superkritische slibvergassing en superkritische sliboxidatie.

Destruction of energetic materials by supercritical water oxidation

International Nuclear Information System (INIS)

Beulow, S.J.; Dyer, R.B.; Harradine, D.M.; Robinson, J.M.; Oldenborg, R.C.; Funk, K.A.; McInroy, R.E.; Sanchez, J.A.; Spontarelli, T.

1993-01-01

Supercritical water oxidation is a relatively low-temperature process that can give high destruction efficiencies for a variety of hazardous chemical wastes. Results are presented examining the destruction of high explosives and propellants in supercritical water and the use of low temperature, low pressure hydrolysis as a pretreatment process. Reactions of cyclotrimethylene trinitramine (RDX), cyclotetramethylene tetranitramine (HMX), nitroguanidine (NQ), pentaerythritol tetranitrate (PETN), and 2,4,6-trinitrotoluene (TNT) are examined in a flow reactor operated at temperatures between 400 degrees C and 650 degrees C. Explosives are introduced into the reactor at concentrations below the solubility limits. For each of the compounds, over 99.9% is destroyed in less than 30 seconds at temperatures above 600 degrees C. The reactions produce primarily N 2 , N 2 O,CO 2 , and some nitrate and nitrite ions. The distribution of reaction products depends on reactor pressure, temperature, and oxidizer concentration. Kinetics studies of the reactions of nitrate and nitrite ions with various reducing reagents in supercritical water show that they can be rapidly and completely destroyed at temperatures above 525 degrees C. The use of slurries and hydrolysis to introduce high concentrations of explosives into a supercritical water reactor is examined. For some compounds the rate of reaction depends on particle size. The hydrolysis of explosives at low temperatures (<100 degrees C) and low pressures (<1 atm) under basic conditions produces water soluble, non-explosive products which are easily destroyed by supercritical water oxidation. Large pieces of explosives (13 cm diameter) have been successfully hydrolyzed. The rate, extent, and products of the hydrolysis depend on the type and concentration of base. Results from the base hydrolysis of triple base propellant M31A1E1 and the subsequent supercritical water oxidation of the hydrolysis products are presented

Hydrothermal synthesis of Ni{sub 2}P nanoparticle and its hydrodesulfurization of dibenzothiophene

Energy Technology Data Exchange (ETDEWEB)

Zhao, Qi; Han, Yang; Huang, Xiang, E-mail: materials@ouc.edu.cn; Dai, Jinhui; Tian, Jintao; Zhu, Zhibin; Yue, Li [Ocean University of China, Institute of Materials Science and Engineering (China)

2017-04-15

Nanosized nickel phosphide (Ni{sub 2}P) has been synthesized via hydrothermal reaction with environmental-friendly red phosphorus and nickel chloride. The reaction mechanism has been studied by measurement techniques of IC, XRD ,TEM, EDS, and XPS. The results showed that the particle sizes of as-prepared Ni{sub 2}P are in nanoscale ranging from 10 to 30 nm. In hydrothermal reaction, red phosphorus reacts with water to its oxyacids, especially its hypophosphorous acid (or hypophosphite) which can reduce nickel chloride to nickel, and then metallic nickel will penetrate into the rest of red phosphorus to generate nano-Ni{sub 2}P. Furthermore, the catalytic performance of as-synthesized Ni{sub 2}P for the hydrodesulfurization of dibenzothiophene has been tested. It has been shown that the HDS reaction process over Ni{sub 2}P catalyst agrees well with the pseudo-first order kinetic equation, and the HDS conversion can reach up to 43.83% in 5 h with a stable increasing catalytic activity during the whole examination process.

Kinetic models for supercritical CO2 extraction of oilseeds - a review

Directory of Open Access Journals (Sweden)

B. Nagy

2011-01-01

Full Text Available The supercritical fluid extraction of oilseeds is gaining increasing interest in commercial application for the last few decades, most particularly thanks to technical and environmental advantages of supercritical fluid extraction technology compared to current extraction methods with organic solvents. Furthermore, CO2 as a solvent is generally recognized as safe (GRAS. At present moment, supercritical fluid extractions on a commercial scale are limited to decaffeination, production of soluble hops extracts, sesame seed oil production and extraction of certain petroleum products. When considering industrial application, it is essential to test the applicability of the appropriate model for supercritical fluid extraction of oilseeds used for scale up of laboratory data to industrial design purposes. The aim of this paper is to review the most significant kinetic models reported in the literature for supercritical fluid extraction.

Supercritical fluid chromatography for lipid analysis in foodstuffs.

Science.gov (United States)

Donato, Paola; Inferrera, Veronica; Sciarrone, Danilo; Mondello, Luigi

2017-01-01

The task of lipid analysis has always challenged separation scientists, and new techniques in chromatography were often developed for the separation of lipids; however, no single technique or methodology is yet capable of affording a comprehensive screening of all lipid species and classes. This review acquaints the role of supercritical fluid chromatography within the field of lipid analysis, from the early developed capillary separations based on pure CO 2 , to the most recent techniques employing packed columns under subcritical conditions, including the niche multidimensional techniques using supercritical fluids in at least one of the separation dimensions. A short history of supercritical fluid chromatography will be introduced first, from its early popularity in the late 1980s, to the sudden fall and oblivion until the last decade, experiencing a regain of interest within the chromatographic community. Afterwards, the subject of lipid nomenclature and classification will be briefly dealt with, before discussing the main applications of supercritical fluid chromatography for food analysis, according to the specific class of lipids. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Hydrothermal Synthesis and Biocompatibility Study of Highly Crystalline Carbonated Hydroxyapatite Nanorods

Science.gov (United States)

Xue, Caibao; Chen, Yingzhi; Huang, Yongzhuo; Zhu, Peizhi

2015-08-01