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Thermal Treatment (thermal + treatment)
Kinds of Thermal Treatment Selected AbstractsOrganic Electronics: High Tg Cyclic Olefin Copolymer Gate Dielectrics for N,N,-Ditridecyl Perylene Diimide Based Field-Effect Transistors: Improving Performance and Stability with Thermal Treatment (Adv. Funct.ADVANCED FUNCTIONAL MATERIALS, Issue 16 2010Mater. Abstract A novel application of ethylene-norbornene cyclic olefin copolymers (COC) as gate dielectric layers in organic field-effect transistors (OFETs) that require thermal annealing as a strategy for improving the OFET performance and stability is reported. The thermally-treated N,N, -ditridecyl perylene diimide (PTCDI-C13)-based n-type FETs using a COC/SiO2 gate dielectric show remarkably enhanced atmospheric performance and stability. The COC gate dielectric layer displays a hydrophobic surface (water contact angle = 95° ± 1°) and high thermal stability (glass transition temperature = 181 °C) without producing crosslinking. After thermal annealing, the crystallinity improves and the grain size of PTCDI-C13 domains grown on the COC/SiO2 gate dielectric increases significantly. The resulting n-type FETs exhibit high atmospheric field-effect mobilities, up to 0.90 cm2 V,1 s,1 in the 20 V saturation regime and long-term stability with respect to H2O/O2 degradation, hysteresis, or sweep-stress over 110 days. By integrating the n-type FETs with p-type pentacene-based FETs in a single device, high performance organic complementary inverters that exhibit high gain (exceeding 45 in ambient air) are realized. [source] High Tg Cyclic Olefin Copolymer Gate Dielectrics for N,N,-Ditridecyl Perylene Diimide Based Field-Effect Transistors: Improving Performance and Stability with Thermal TreatmentADVANCED FUNCTIONAL MATERIALS, Issue 16 2010Jaeyoung Jang Abstract A novel application of ethylene-norbornene cyclic olefin copolymers (COC) as gate dielectric layers in organic field-effect transistors (OFETs) that require thermal annealing as a strategy for improving the OFET performance and stability is reported. The thermally-treated N,N, -ditridecyl perylene diimide (PTCDI-C13)-based n-type FETs using a COC/SiO2 gate dielectric show remarkably enhanced atmospheric performance and stability. The COC gate dielectric layer displays a hydrophobic surface (water contact angle = 95° ± 1°) and high thermal stability (glass transition temperature = 181 °C) without producing crosslinking. After thermal annealing, the crystallinity improves and the grain size of PTCDI-C13 domains grown on the COC/SiO2 gate dielectric increases significantly. The resulting n-type FETs exhibit high atmospheric field-effect mobilities, up to 0.90 cm2 V,1 s,1 in the 20 V saturation regime and long-term stability with respect to H2O/O2 degradation, hysteresis, or sweep-stress over 110 days. By integrating the n-type FETs with p-type pentacene-based FETs in a single device, high performance organic complementary inverters that exhibit high gain (exceeding 45 in ambient air) are realized. [source] The Effect of Thermal Treatment on the Morphology and Charge Carrier Dynamics in a Polythiophene,Fullerene Bulk Heterojunction,ADVANCED FUNCTIONAL MATERIALS, Issue 8 2005J. Savenije Abstract The influence of various thermal treatment steps on the morphology and the photoconductive properties of a non-contacted, 50,nm thick blend (50:50,wt.-%) of [6,6]-phenyl C61 -butyric acid methyl ester (PCBM) and poly(3-hexyl thiophene) (P3HT) spin-coated from chloroform has been studied using transmission electron microscopy (TEM) and the electrodeless time-resolved microwave conductivity technique. After annealing the film for 5,min at 80,°C, TEM images show the formation of crystalline fibrils of P3HT due to a more ordered packing of the polymer chains. The thermal treatment results in a large increase of the photoconductivity, due to an enhancement of the hole mobility in these crystalline P3HT domains from 0.0056,cm2,V,1,s,,1 for the non-annealed sample to 0.044,cm2,V,1,s,,1 for the sample annealed at 80,°C. In contrast, the temporal shape of the photoconductivity, with typical decay half-times, ,1/2, of 1,,s for the lowest excitation intensities, is unaffected by the temperature treatment. Further annealing of the sample at 130,°C results in the formation of three different substructures within the heterojunction: a PCBM:P3HT blend with PCBM-rich clusters, a region depleted of PCBM, and large PCBM single crystals. Only a minor increase in the amplitude, but a tenfold rise of the decay time of the photoconductivity, is observed. This is explained by the formation of PCBM-rich clusters and large PCBM single crystals, resulting in an increased diffusional escape probability for mobile charge carriers and hence reduced recombination. [source] Impact of Thermal Treatment on Color and Pigment Pattern of Red Beet (Beta vulgaris L.) PreparationsJOURNAL OF FOOD SCIENCE, Issue 6 2004K.M. Herbach ABSTRACT: The impact of heating at 85°C during 8 h on overall color and betalain pattern of red beet (Beta vulgaris L. ssp. vulgaris) juice was investigated. Although the hue angle of 358° in fresh juice was indicative of the typical red-purple appearance, heating for 8 h induced an unexpected shift to 62° resulting in a yellow-orange solution. To monitor the underlying structural alterations of betalains, a new high-performance liquid chromatography separation compatible with mass spectrometry was developed. Applying this method, 2 novel yellow neobetanin structures and 2 orange-red betanin degradation products were preliminarily identified, and neobetanin formation resulting from heat exposure was proven for the 1st time. These 5 compounds were held responsible for the orange shift of red beet juice during thermal treatment. The relevance of these findings for industrial beet processing was demonstrated by comparison of pigment patterns of heated red beet juice samples and a commercial concentrate. On the basis of these results, a scheme for the thermal degradation of betanin is proposed. [source] High-Throughput Screening of the Influence of Thermal Treatment on the Mechanical Properties of Semicrystalline Polymers: A Case Study for iPPMACROMOLECULAR RAPID COMMUNICATIONS, Issue 1 2004Konrad Schneider Abstract Summary: High-throughput screening is a convenient tool to determine the influence of parameters, such as composition or processing conditions on certain materials' properties. In the present study, iPP was used to construct a combinatorial library made from a processing temperature gradient requiring only a minimised amount of material. Clear changes in the crystalline modification and crystal morphology of the iPP, and their impact on mechanical properties have been identified. The construction of a combinatorial library to study the effect of thermal history upon the properties of polymers. [source] ChemInform Abstract: Effect of Thermal Treatment on the Electronic Conductivity Properties of Cobalt Spinel Phases Synthesized by Electro-Oxidation in Ternary Alkaline Electrolyte (KOH, LiOH, NaOH).CHEMINFORM, Issue 6 2009Myriam Douin Abstract ChemInform is a weekly Abstracting Service, delivering concise information at a glance that was extracted from about 200 leading journals. To access a ChemInform Abstract of an article which was published elsewhere, please select a "Full Text" option. The original article is trackable via the "References" option. [source] Effect of Equivalent Thermal Treatments on the Color and the Antioxidant Activity of Tomato PureeJOURNAL OF FOOD SCIENCE, Issue 9 2002M. Anese ABSTRACT: The influence of different heat treatments on color and antioxidant properties of tomato purees was investigated. The treatments were designed to produce the same total thermal effect against spoilage microorganisms. Although the development of nonenzymatic browning reactions occurred by increasing process temperature, no changes in redness were observed in the heated samples, due to the "masking" effect of lycopene. Also, the heat treatments had equivalent effect on the chain-breaking activity of the aqueous and lycopene tomato fractions. However the redox potential values increased as the heating temperature increased. All data together showed that the thermal resistance constant z values for color and chain-breaking activity were close to 10°C, but lower than 10°C for reducing properties. [source] 1-D-Tin(II) Phenylchalcogenolato Complexes ,1[Sn(EPh)2] (E = S, Se, Te) , Synthesis, Structures, Quantum Chemical Studies and Thermal BehaviourEUROPEAN JOURNAL OF INORGANIC CHEMISTRY, Issue 3 2010Andreas Eichhöfer Abstract A series of three 1-D-tin(II) phenylchalcogenolato complexes ,1[Sn(EPh)2] (E = S, Se, Te) were synthesized in yields > 80,% by reaction of SnCl2 with two equivalents of PhESiMe3 in organic solvents. In the crystal the molecules form two different types of one-dimensional chains. In ,1[Sn(SPh)2] the tin atoms are distorted trigonal pyramidal coordinated by sulfur atoms (two bonds within a monomer and one longer bond between neighbored monomers), while in ,1[Sn(EPh)2] (E = Se, Te) the tin atoms show contacts to two neighbored monomers leading to a fourfold coordination of the tin atoms by either selenium or tellurium atoms. The bond situation is discussed on the basis of density functional calculations. Thermal treatment mostly leads to the formation of the corresponding phase pure tin(II) chalcogenides however sublimation plays an increasing role ongoing from the tellurolato to the thiolato complex especially for the use of vacuum conditions. The investigation of the volatile cleavage products reveals the occurence of more complex reactions in the gas phase than the formal stoichiometric cleavage of EPh2 (E = S, Se, Te) with formation of SnE. [source] Formation of Metastable Na2CrO4 -Type LiNiPO4 from a Phosphate,Formate PrecursorEUROPEAN JOURNAL OF INORGANIC CHEMISTRY, Issue 1 2010Violeta Koleva Abstract High-pressure modification of LiNiPO4 with a Na2CrO4 -type structure was obtained at ambient pressure and low temperature from a mixed LiNi,phosphate,formate precursor, LiNiPO4Hx(HCOO)x·yH2O (where x , 1.2 and y , 2.5). The structural and thermal characterization of the precursor and the LiNiPO4 compositions were carried out by powder XRD analysis, IR spectroscopy, and DSC analysis. Thermal treatment of LiNiPO4Hx(HCOO)x·yH2O precursors between 450 and 650 °C yields a mixture of the two structural modifications of LiNiPO4: the Na2CrO4 type and the olivine type. It was established that the obtained Na2CrO4 -type LiNiPO4 is a metastable phase, which completely transforms at 700 °C into the olivine-type phase. The enthalpy of the phase transition is ,H = ,43.40 kJ,mol,1. The mechanism of formation of the two forms of LiNiPO4 from the LiNi,phosphate,formate precursor is discussed. [source] Synthesis and Structure of [nPr3N(CH2)6NnPr3][CuFe3Br3(SePh)6], [Cu5Fe(SePh)7(PPh3)4] and [Cu4Fe3(SePh)10(PPh3)4],EUROPEAN JOURNAL OF INORGANIC CHEMISTRY, Issue 1 2007Andreas Eichhöfer Abstract CuBr and Fe(OOCCH3)2 react with PhSeSiMe3 in acetonitrile in the presence of the diammonium salt [nPr3N(CH2)6NnPr3]Br2 to yield ionic [nPr3N(CH2)6NnPr3][CuFe3Br3(SePh)6]. The neutral complexes [Cu5Fe(SePh)7(PPh3)4] and [Cu4Fe3(SePh)10(PPh3)4] were obtained by similar reactions of different stoichiometric mixtures of CuOOCCH3 and FeCl2 with PPh3 and PhSeSiMe3. The crystal structures of the compounds were determined by single-crystal X-ray analysis to give new structural types of molecular cluster compounds formed by copper, iron and selenium. Thermal treatment of [Cu5Fe(SePh)7(PPh3)4] and [Cu4Fe3(SePh)10(PPh3)4] resultsin the formation of mixtures of binary Cu2Se and ternaryCuFeSe2.(© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2007) [source] Syntheses and Fluxional Processes of Diphenyl(2-thienyl)phosphane Derivatives of Triosmium ClustersEUROPEAN JOURNAL OF INORGANIC CHEMISTRY, Issue 10 2006Nitsa K. Kiriakidou Kazemifar Abstract Thermal treatment of [Os3(CO)12] with diphenyl(2-thienyl)phosphane, Ph2P(C4H3S), results in the formation of [Os3(CO)12,x{Ph2P(C4H3S)}x] (x = 1,3, 1,3), but no C,H bond activation was observed. Reaction of [H2Os3(CO)10] with diphenyl(2-thienyl)phosphane at ambient temperature affords [HOs3(,-H)(CO)10{Ph2P(C4H3S)}] (4), but when the samereaction is repeated at elevated temperatures, the cyclometallated species [(,-H)Os3(CO)9{,3 -Ph2P(C4H2S)}] (5) and[(,-H)Os3(CO)8{,3 -Ph2P(C4H2S)}{Ph2P(C4H3S)}] (6) are formed. In addition, two more products, tentatively assigned as [(,-H)Os3(CO)6{,3 -Ph2P(C4H2S)}{,-Ph2P(C4H3S)}{Ph2P(C4H3S)}] (7) and [(,-H)Os3(CO)7{,-Ph2P(C4H2S)}{,-Ph2P(C4H3S)}{Ph2P(C4H3S)}] (8) are obtained. The dynamic behaviours of 2, 5 and 6 have been studied by variable-temperature (VT) 1H and 31P{1H} NMR spectroscopy. The VT 31P{1H} NMR spectra of [Os3(CO)10{Ph2P(C4H3S)}2] (2) demonstrate that a mixture of two isomers, which are in rapid exchange at room temperature, is present and that the less common cis - trans isomer, whose structure has been determined by X-ray crystallography, is favoured for this cluster. The VT 1H NMR spectra of 5 indicate the presence of two isomers which are proposed to arise from an oscillation of the ,,,2 -vinyl group of the thienyl moiety between two metal atoms. A similar fluxional process is proposed to occur in 6 and the assignment of the room-temperature structure(s) of this cluster was confirmed by 1H- 187Os 2D HMQC spectroscopy. In addition to 2, the solid-state structures of 3, 5 and 6 have been determined by X-ray crystallography. (© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2006) [source] Layered [BaM(C3H2O4)2(H2O)4] (M = Fe or Co) Complexes , Spectroscopic, Magnetic and Thermal StudyEUROPEAN JOURNAL OF INORGANIC CHEMISTRY, Issue 16 2003Izaskun Gil de Muro Abstract Complexes with formula [BaM(C3H2O4)2(H2O)4], where M = Fe or Co, were synthesised and characterised. These two types of complexes are isostructural and crystallise in the Pccn space group. Their structure consists of two-dimensional networks of octahedral MO6 polyhedra in which the transition metal ions are coordinated by bridging malonate ligands, through the O-C-O atoms. These M-malonate units are extended along the crystallographic [101] plane. Spectroscopic data are consistent with the cations being in a high-spin octahedral symmetry. The two types of compounds exhibit 2D antiferromagnetic interactions as well as weak ferromagnetism below the Néel temperature, as a result of an intralayer misalignment of the spins. Thermal treatment of the metallo-organic precursors gave rise to BaMO3,y oxides at lower temperatures and reaction times than those found in the literature using the ceramic method. (© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2003). [source] Assembly of Pure Silver-Tungsten-Oxide Frameworks from Nanostructured Solution Processable Clusters and Their Evolution into Materials with a Metallic ComponentADVANCED MATERIALS, Issue 38 2010Thomas McGlone Silver-Tungsten-Oxide Frameworks: Isomerically pure forms of the unique isopolyoxotungstate system are incorporated into highly connected framework materials using Ag(I) as a linking unit. Thermal treatment of the materials leads to the formation of silver microparticles embedded in a tungsten oxide matrix. This novel synthetic approach promises to create a new class of nanostructured tungsten-silver-oxides with exciting physical properties, as well as exemplifies the potential for new frameworks based upon solution processable POM clusters. [source] Synthesis of dihydrothieno[2,3- b]pyridines based on titanium(IV) chloride-mediated michael reactions of 2-amino-4,5-dihydro-3-thiophenecarbonitriles with ,,,-unsaturated ketonesJOURNAL OF HETEROCYCLIC CHEMISTRY, Issue 4 2004Hiroshi Maruoka 2-Arnino-4,5-dihydro-3-thiophenecarbonitriles 1a-c reacted with ,,,-unsaturated ketones (e.g. methyl vinyl ketone 2 and benzalacetone 3) in the presence of titanium(IV) chloride to give the corresponding Michael adducts 4a-c and 5a-c. Thermal treatment of compounds 4a-c and 5a-c with titanium(IV) chloride caused intramolecular cyclocondensation to yield the corresponding tetrahydrothieno[2,3- b]pyridines 6a-c and 7a-c. Aromatization of 6a-c and 7a-c with potassium tert -butoxide in refluxing tert -butyl alcohol pro ceeded smoothly to afford the corresponding dihydrothieno[2,3- b]pyridines 8a-c and 9a-c. [source] New Route for the Extraction of Crude Zirconia from ZirconJOURNAL OF THE AMERICAN CERAMIC SOCIETY, Issue 9 2002Nicholas J. Welham A commercial grade of zircon (ZrSiO4) concentrate was mechanically milled with MgO for up to 100 h in a laboratory-scale mill. The resultant powders were subjected to thermal processing, chemical leaching, and X-ray diffraction (XRD). There was no direct evidence of reaction during the milling step, with no new phases evident from XRD. Leaching of the powder showed that a reaction had occurred, and increased solubility with milling time was attributed to the formation of a nanostructured Mg-Zr-Si oxide, which dissolved congruently. Heating the powders resulted in a number of thermal events, including the formation/crystallization of ZrO2 and Mg2SiO4. Thermal treatment of the milled powders allowed selective chemical leaching of the magnesium and silicon, leaving a powder containing ,90% ZrO2. [source] Synthesis of Titanate Derivatives Using Ion-Exchange ReactionJOURNAL OF THE AMERICAN CERAMIC SOCIETY, Issue 5 2000Chul-Tae Lee Two types of titanate derivatives, layered hydrous titanium dioxide (H2Ti4O9·nH2O) and potassium octatitanate (K2Ti8O17) with a tunnellike structure, were synthesized using an ion-exchange reaction. Fibrous potassium tetratitanate (K2Ti4O9·nH2O) was prepared by calcination of a mixture of K2CO3 and TiO2 with a molar ratio of 2.8 at 1050°C for 3 h, followed by boiling-water treatment of the calcined products for 10 h. The material then was transformed to layered H2Ti4O9·nH2O through an exchange of K+ ions with H+ ions using HCl. K2Ti8O17 was formed by a thermal treatment of KHTi4O9·nH2O. Pure KHTi4O9·nH2O phase was effectively produced by a treatment of K2Ti4O9 with 0.005M HCl solution for 30 min. Thermal treatment at 250°,500°C for 3 h resulted in formation of only K2Ti8O17. [source] Onion Cells After High Pressure and Thermal Processing: Comparison of Membrane Integrity Changes Using Different Analytical Methods and Impact on Tissue TextureJOURNAL OF FOOD SCIENCE, Issue 7 2010Maria E. Gonzalez Abstract:, Two different analytical methods were evaluated for their capacity to provide quantitative information on onion cell membrane permeability and integrity after high pressure and thermal processing and to study the impact of these processing treatments on cell compartmentalization and texture quality. To determine changes in cell membrane permeability and/or integrity the methodologies utilized were: (1) measurement of a biochemical product, pyruvate, formed as a result of membrane permeabilization followed by enzymatic activity and (2) leakage of electrolytes into solution. These results were compared to previously determined methods that quantified cell viability and 1H-NMR T2 of onions. These methods allowed for the monitoring of changes in the plasma and tonoplast membranes after high pressure or thermal processing. High pressure treatments consisted of 5 min holding times at 50, 100, 200, 300, or 600 MPa. Thermal treatments consisted of 30 min water bath exposure to 40, 50, 60, 70, or 90 °C. There was strong agreement between the methods in the determination of the ranges of high pressure and temperature that induce changes in the integrity of the plasma and tonoplast membranes. Membrane rupture could clearly be identified at 300 MPa and above in high pressure treatments and at 60 °C and above in the thermal treatments. Membrane destabilization effects could already be visualized following the 200 MPa and 50 °C treatments. The texture of onions was influenced by the state of the membranes and was abruptly modified once membrane integrity was lost. Practical Application:, In this study, we used chemical, biochemical, and histological techniques to obtain information on cell membrane permeability and onion tissue integrity after high pressure and thermal processing. Because there was strong agreement between the various methods used, it is possible to implement something relatively simple, such as ion leakage, into routine quality assurance measurements to determine the severity of preservation methods and the shelf life of processed vegetables. [source] Ultrastructural and Changes in Pectin Composition of Sweet Cherry from the Application of Prefreezing TreatmentsJOURNAL OF FOOD SCIENCE, Issue 9 2005Jesus Alonso ABSTRACT: Thermal and calcium pretreatments applied to preserve the sweet cherry texture by the freezing/thawing process produced biochemical changes in the pectic substances and ultrastructural alterations to the cells and tissues, which were visible under scanning electron microscopy. Partial dehydration of the epidermic tissue caused by calcium (100 mM CaCl2) and thermal (50 °C/10 min) pretreatment attenuated the surface damage produced by freezing. However, pretreatment at 70 °C/2 min caused partial destruction of the epidermic tissue and plasmolysis of the parenchymatic cells. After freezing, the cell walls in the parenchymatic tissue of the fruits pretreated with 100 mM CaCl2 exhibited swelling as a result of gelling of the cell-wall pectic material. Thermal pretreatments increased the ethylenediaminetetraacetic acid (EDTA)-soluble pectin fraction and reduced the degree of pectin esterification. Thermal treatments at 70 °C, without immersion in calcium, reduced the water- and pectinase-soluble pectin fractions, whereas immersion in calcium prevented depolymerization of these fractions. Immersion in 100 mM CaCl2 increased the water-soluble pectin fraction. [source] Optical absorption, paramagnetic resonance and depolarisation currents in MgAl2O4 spinelPHYSICA STATUS SOLIDI (C) - CURRENT TOPICS IN SOLID STATE PHYSICS, Issue 3 2007Roberto Paiva Abstract Optical Absorption (OA), Electron Paramagnetic Resonance (EPR) and Thermally Stimulated Depolarisation Currents (TSDC) techniques were applied to study the effects of irradiation and thermal treatments in the formation, aggregation and destruction processes of dipole defects in MgAl2O4 spinel. Irradiated MgAl2O4 crystals present two OA bands centred at 3.4 eV and 5.1 eV. The 3.4 eV band increases with the irradiation-dose, stabilizes its maximum height for doses near 10 kGy and is completely destroyed for thermal treatments above 500 K. This same band decays when the sample is maintained at room temperature reaching a constant value after a few weeks. The EPR spectrum is composed by two superimposed bands at g = 2.011. The gamma dose dependence, the thermal treatments between 370 K and 500 K and the thermal decay of the two bands at room temperature, show that each band behaves in a different way thus indicating that they are associated with two different defects. Gamma dose of 10 kGy produces a TSDC band at 245 K. When the sample is maintained at room temperature, after the gamma irradiation, for several weeks, a displacement in the peak position to 290 K, is observed. Thermal treatments above 500 K destroy the 290 K band. This band is associated to at least two V-type centres. (© 2007 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] Synthesis and characterization of compounds LixMn1+xFe2,2xO4 with spinel structure in the quasiternary system "LiO0,5 , MnOx , FeOx"CRYSTAL RESEARCH AND TECHNOLOGY, Issue 1 2006C. Wende Abstract The thermal decomposition of freeze-dried Li-Mn(II)-Fe(III)-formate precursors was investigated by means of DTA, TG and mass spectroscopy. By the thermal treatment of the prefired precursors between 400 and 1000°C, single phase solid solutions LixMn1+xFe2,2xO4 (0 , x , 1) with cubic spinel structure were obtained. To get single phase spinels, special conditions concerning the temperature T and the oxygen partial pressure p(O2) during the synthesis are required. Because of the high reactivity of the freeze-dried precursors, in comparison with the conventional solid state reaction, the reaction temperature can be lowered by 200°C. The cation distribution and the properties of the Li-Mn-ferrites were studied by chemical analysis, X-ray powder diffraction and magnetization measurements. It was found that for high substitution rates, almost all lithium occupies the tetrahedral coordinated A-sites of the spinel lattice AB2O4, while at small x-values, lithium ions are distributed over the tetrahedral and octahedral sites. (© 2005 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] Formation of diffusion-hindering interlayers in metals in contact by dedicated thermal treatmentCRYSTAL RESEARCH AND TECHNOLOGY, Issue 1-2 2005D. C. Meyer Abstract Thermal evolution of the structure of Fe/Al multilayers (MLs) with nominal composition 5*(5 nm Al / 5 nm Fe) prepared by crossed-beam pulsed laser deposition is studied by wide-angle X-ray scattering and X-ray reflectometry after different temperature-time procedures of thermal treatments under high-vacuum conditions. In comparison to direct thermal annealing at temperatures of 250 °C and 275 °C, respectively, which results in nearly complete mixing of the MLs and formation of the FeAl intermetallic compound, quite different behaviour was found after dedicated thermal pretreatment. Annealing at successive growing temperatures before final annealing at temperatures mentioned, resulted in conservation of pronounced multilayer structure. From the results it is generalised, that also in the case of ML systems, the tendency of mixing a dedicated tuning of interface characteristics by thermal treatment allows for formation of diffusion-hindering interlayers. (© 2005 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] Void formation in the Cu layer during thermal treatment of SiNx/Cu/Ta73Si27/SiO2/Si systemsCRYSTAL RESEARCH AND TECHNOLOGY, Issue 1-2 2005R. Hübner Abstract The thermal stability of a SiNx passivation layer and its influence on the annealing behavior of an amorphous Ta73Si27 diffusion barrier deposited between copper and SiO2 were analyzed by X-ray diffraction, glow discharge optical emission spectroscopy, Auger electron spectroscopy, scanning electron microscopy, and transmission electron microscopy. During heat treatment at a temperature Tan = 500 °C, diffusion of Cu atoms out of the Cu metallization into the SiNx passivation occurs. The Cu diffusion intensifies with increasing annealing temperature and annealing time and seems to be a necessary precondition for a defect formation process observed within the Cu metallization. Depending on the chemical composition of the SiNx/Cu interface, voids in the ,m-range can be formed within the Cu film. Compared to an unpassivated sample, heat treatment leads to a reduced diffusion of Ta atoms from the barrier through the copper into the SiNx/Cu interface. The barrier crystallization process into Ta5Si3 occurring during annealing at Tan = 600 °C is principally not affected by the presence of a SiNx passivation. (© 2005 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] Nano vanadyl-phthalocyanine crystals fabricated on KBr substrateELECTRICAL ENGINEERING IN JAPAN, Issue 2 2008Suguru Mototani Abstract Vanadyl-phthalocyanine (VOPc) thin films deposited on a KBr substrate by molecular beam epitaxy (MBE) consist of nano-VOPc crystals epitaxially grown. The nano-VOPc crystals acquire a square shape as a result of annealing at 150°C. The size of the nano-crystals is controllable by changing the conditions of MBE deposition and thermal treatment. The growth processes of nano-crystals on the KBr substrate are elucidated experimentally and are shown to be closely related to strong interaction between the VOPc molecules and the KBr substrate. Their mechanisms can be explained in terms of surface diffusion of the VOPc molecules on the KBr substrate. © 2008 Wiley Periodicals, Inc. Electr Eng Jpn, 163(2): 41,48, 2008; Published online in Wiley InterScience (www.interscience.wiley.com). DOI 10.1002/eej.20645 [source] Characterization of "Cd10S4(SPh)12", the Thermal Decomposition Product of (NMe4)4[Cd10S4(SPh)16]: Synthesis of a Neutral Cd54 Sulfide Cluster and of a Polymeric Chain of Thiolate-Bridged Cd17 Sulfide ClustersEUROPEAN JOURNAL OF INORGANIC CHEMISTRY, Issue 21 2010Maria Bendova Abstract Contrary to claims in the literature that a cluster of the composition of "Cd10S4(SPh)12" was formed by thermal treatment of (NMe4)4[Cd10S4(SPh)16], experimental evidence was gathered that the core structure of the cluster is not exclusively retained and other CdS species are also formed. When "Cd10S4(SPh)12" was treated with PhSH/NEt3 only a part of the material was converted into (NHEt3)4[Cd10S4(SPh)16]. From solutions of "Cd10S4(SPh)12" in strongly coordinating solvents the new neutral CdS clusters Cd54S28(SPh)52Lx (L = pyridine, DMSO or DMF) and [Cd17S4(SPh)26py], were crystallized. The latter forms polymeric chains of phenylthiolate-bridged Cd17 units. [source] Application of New Organic Fuels in the Direct MgAl2O4 Combustion SynthesisEUROPEAN JOURNAL OF INORGANIC CHEMISTRY, Issue 6 2008Robert Iano Abstract The paper presents a new version of MgAl2O4 solution-combustion synthesis, based on the individual reactivity of Mg(NO3)2 and Al(NO3)3 with respect to various fuels. Beside the traditionally used fuels (urea, glycine, ,-alanine), new organic reducing agents [monoethanolamine, triethanolamine, tris(hydroxymethyl)aminomethane and triethylenetetramine] have also been used. The study of the individual reactivities of Mg(NO3)2 and Al(NO3)3 with respect to each of the previously mentioned fuels suggested that there is a predilection of the two metal nitrates for certain fuels: urea is the optimum fuel for Al(NO3)3, whereas monoethanolamine represents the most suitable fuel for Mg(NO3)2. It has been shown by X-ray diffraction and thermal analysis that the use of a single fuel in the MgAl2O4 low-temperature combustion synthesis leads to the formation of an amorphous powder. In this case, the formation of pure crystalline MgAl2O4 requires a subsequent thermal treatment at 900 °C with 1 h soaking time. On the other hand, the use of fuel mixtures containing urea and monoethanolamine or urea and ,-alanine proved to be the rational solution for the direct formation of MgAl2O4. It has been shown that, by using the above-mentioned fuel mixtures, one can obtain pure nanocrystalline MgAl2O4 straight from the combustion reaction, no additional calcination being necessary. (© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2008) [source] Triacylglycerol migration and bloom in filled chocolates: Effects of low-temperature storageEUROPEAN JOURNAL OF LIPID SCIENCE AND TECHNOLOGY, Issue 3 2009Frédéric Depypere Abstract This study investigated the effect of storage temperature on triacylglycerol (TAG) migration, visual fat bloom and taste of industrially produced milk chocolates with a hazelnut-based filling. The chocolates were stored for up to 10,months at 18,°C, either directly after production or with the inclusion of a variable time at ,20 or 4,°C immediately after production and prior to further storage at 18,°C. TAG migration from the filling through the chocolate shell was quantified by HPLC analysis of chocolate sampled from the chocolates' surface. Both [OOO/SOS] and [LOO/SOS] were used as markers for oil migration. Compared to storage at 18,°C only, chilling or freezing of the chocolates for part of the storage time was found to reduce the amount of TAG migration. Effects on diffusion, capillary transport and TAG immobilization during the thermal treatment can be raised as possible reasons for this decrease. Furthermore, storage at ,20,°C decreased oil migration during subsequent storage at 18,°C. This suggests a crystallization effect during the storage at ,20,°C, leading to permanent (micro)structural changes. Although a thermal treatment at 4,°C compared to ,20,°C was less effective in retarding TAG migration, storage at low positive temperatures immediately after production appears already beneficial in the prevention of visual fat bloom. Adverse effects of the thermal treatments on the chocolates' taste were not observed. [source] Ultra-Fast Atomic Transport in Severely Deformed Materials,A Pathway to Applications?,ADVANCED ENGINEERING MATERIALS, Issue 8 2010Sergiy Divinski Abstract Severe plastic deformation of pure Cu and Cu-rich alloys was found to create a hierarchical combination of fast and ultra-fast diffusion paths ranging from non-equilibrium grain boundaries to non-equilibrium triple junctions, vacancy clusters, nano- and micro-pores, and finally to general high-angle grain boundaries. Under certain conditions, a percolating network of porosity can be introduced in the ultra-fine grained materials by a proper mechanical and thermal treatment. This network may offer promising opportunities for creating materials with tailor-made properties, including combinations of improved mechanical performance with a possibility of self repair using "vascular structures" for atom transport. Applications in such areas as drug eluting bioimplants and lead or polymer eluting materials for reduction of friction based on impregnation of porosity networks with these agents are also envisaged. [source] The Fate of Lead in MSWI-Fly Ash During Heat Treatment: An X-Ray Absorption Spectroscopy Study,ADVANCED ENGINEERING MATERIALS, Issue 6 2009Rudolf Paul Wilhelm Jozef Struis The study focuses on the potential of removing toxifying Pb from a certified, multi-element fly ash (BCR176) by thermal treatment between 300 and 950,°C under different carrier gas compositions (Ar or Ar,+,O2). The treatment was studied by in situ monitoring the evaporation rate of Pb, C, S, Na, and K during heating and by synchrotron X-ray absorption spectroscopy of selected samples collected during vaporization at the Pb L3 -edge. [source] The Coupling Effect of Small Nanocrystals and Free Volume on the Ductility of Cu46Zr47Al7 Bulk Metallic Glass Alloy,ADVANCED ENGINEERING MATERIALS, Issue 5 2009Feng Jiang Cu46Zr47Al7 bulk metallic glass (BMG) and its composite containing small in situ precipitated nanocrystals were prepared through copper mold casting. Different free volume states of these Cu46Zr47Al7 alloys were obtained through thermal treatment such as annealing and quenching. Three-point bending tests for these alloys were undertaken to evaluate their plastic deformation ability. Free volume changes were measured indirectly but quantitatively with differential scanning calorimetry (DSC) method. The results show that, the ductility of Cu46Zr47Al7 alloys is closely related with the free volume states and the ductility of thermally embrittled Cu46Zr47Al7 alloys samples can be partially recovered by restoring free volume through quenching process. The presence of small nanocrystals is more efficient than free volume to enhance the ductility. However, only with the concurrence of the small nanocrystals and the free volume, the Cu46Zr47Al7 BMG alloys will present excellent ductility. [source] In search of stable soil organic carbon fractions: a comparison of methods applied to soils labelled with 14C for 40 days or 40 yearsEUROPEAN JOURNAL OF SOIL SCIENCE, Issue 2 2008S. Bruun Summary A reliable method for the isolation of a stable fraction of soil organic carbon (SOC) would be very helpful for improving our understanding of the mechanisms responsible for stabilization of SOC and the dynamics of SOC turnover. We tested acid hydrolysis, physical fractionation (particle density/size), photo-oxidation, treatment with chemical oxidants (NaOCl and NaS2O8) and thermal treatment on two soils incubated with 14C-labelled barley straw for either 40 days or 40 years. Different intensities of the treatments were included. Acid hydrolysis, photo-oxidation and treatment with a chemical oxidant consistently removed more 40-year-old C than 40-day-old C, which suggests that the isolated fractions contained a large proportion of material with a relatively rapid turnover. The clay + silt associated SOC fraction contained a small proportion of 40-day-old C and a large proportion of 40-year-old C. This is consistent with a SOC fraction with medium turnover. The thermal treatment removed more 40-year-old C than 40-day-old C. At 400°C there was still a small proportion of the 40-year-old C remaining, whereas almost all the 40-day-old C was removed. This is consistent with a stable SOC fraction. However, because only 2,3% of the C remained after this treatment, the isolated SOC fraction may be of little quantitative importance. Furthermore, the thermally resistant fraction is likely to be heavily altered by the treatment, and therefore unsuitable for further studies of the chemical nature of stable SOC. 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