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1
Keceli, Ezgi. "Ruthenium(iii) Acetylacetonate." Master's thesis, METU, 2006. http://etd.lib.metu.edu.tr/upload/3/12607230/index.pdf.
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Ruthenium(III) acetylacetonate was employed for the first time as homogeneous catalyst in the hydrolysis of sodium borohydride. Ruthenium(III) acetylacetonate was not reduced by sodium borohydride under the experimental conditions and remains unchanged after the catalysis, as shown by FT-IR and UV-Vis spectroscopic characterization. Poisoning experiments with mercury, carbon disulfide or trimethylphosphite provide compelling evidence that ruthenium(III) acetylacetonate is indeed a homogenous catalyst in the hydrolysis of sodium borohydride.
Kinetics of the ruthenium(III) acetylacetonate catalyzed hydrolysis of sodium borohydride was studied depending on the catalyst concentration, substrate concentration and temperature. The hydrogen generation was found to be first order with respect to both the substrate concentration and catalyst concentration. The activation parameters of this reaction were also determined from the evaluation of the kinetic data: activation energyEa = 25.6 &
#61617
&
#61472
1.3 kJ.mol-1, the enthalpy of activation
&
#8710
H# = 24.6 ±
1.2 kJ.mol-1 and the entropy of activation &
#8710
S# = -170 ±
5 J&
#61655
mol-1&
#61655
K-1. Ruthenium(III) acetylacetonate provides the lowest activation energy ever found for the hydrolysis of sodium borohydride. Ruthenium(III) acetylacetonate was found to be highly active catalyst providing 1183 total turnovers in the hydrolysis of sodium borohydride over 180 min before they are deactivated. The recorded turnover frequency (TOF) is 6.55 min-1.
2
Khosla, Chetna Templeton J. L. "Intermediate oxidation state tungsten acetylacetonate complexes." Chapel Hill, N.C. : University of North Carolina at Chapel Hill, 2009. http://dc.lib.unc.edu/u?/etd,2296.
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Thesis (Ph. D.)--University of North Carolina at Chapel Hill, 2009.Title from electronic title page (viewed Jun. 26, 2009). "... in partial fulfillment of the requirements for the degree of Doctor of Philosophy in the Department of Chemistry." Discipline: Chemistry; Department/School: Chemistry.
3
Cross, Peggi Sue 1960. "The synthesis of aluminum hydrous oxide from aluminum acetylacetonate." Thesis, The University of Arizona, 1990. http://hdl.handle.net/10150/277276.
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A method for the preparation of submicron, monodispersed, spherical particles of aluminum hydrous oxide has been developed. The method consists of the hydrolysis of aluminum acetylacetonate in alcoholic solution by the direct addition of a base at room temperature. The effects of the process parameters including temperature, solvent, type and concentration of base, aluminum acetylacetonate concentration, and stirring time are examined as well as the process reproducibility, particle composition and particle stability. Results obtained have shown that monodispersed particles can be formed with a mean particle diameter of eighty five to two hundred and fifteen nanometers and the mean size is reproducible to within ten percent of the mean diameter. Particles that are redispersed in fresh solvent are stable for at least thirty days. A model is proposed which explains the kinetics of particle growth and the influence of experimental parameters such as temperature, pH, concentration and the solvent on the formation of particles.
4
Lozada-Garcia, Rolando. "Dynamics and Photodynamics of Acetylacetone in para-Hydrogen matrices." Phd thesis, Université Paris Sud - Paris XI, 2012. http://tel.archives-ouvertes.fr/tel-00780495.
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Acetylacetone (AcAc) exists as a mixture of enol and keto tautomers. Besides providing a good example for the study of tautomerization, it is a model system for investigating intramolecular hydrogen bonds in its enol form. Trapping AcAc in the soft para-Hydrogen (pH2 ) environment brings out new opportunities to investigate its properties. Infrared spectra of the samples give a good characterization of the two stable enol and keto tautomers. The keto/enol ratio in solid pH2 is found to be higher than in other matrices. While vibrational bands of keto are narrow, those of enol are broad, reflecting the intrinsic properties of the enol which exhibits three entangled large amplitude motions (two methyl torsions and the intramolecular hydrogen transfer). Surprisingly, narrowing of some of these bands is observed in a slow time evolution. This effect is interpreted as a consequence of nuclear spin conversion in the hydrogen atoms of the methyl groups, giving access to AcAc species differing by their nuclear spin symmetry. This offers new pertinent investigations on the large amplitude motions, especially on the intramolecular hydrogen transfer. AcAc/pH2 samples have been irradiated by UV laser beams. Irradiation at 266 nm induces isomerization from the stable chelated enol form to non chelated conformers, similarly to the case of other matrices. A clear IR signature of the conformers is obtained thanks to the pH2 host. Irradiation at 248 nm induces the enol/keto tautomerization. The kinetics of this interconversion highlights a non-direct process. Fragmentation is clearly observed under irradiation at 193 nm, followed by chemical reaction with the hydrogen host.
5
Unel, Ebru. "Ruthenium(iii) Acetylacetonate As Catalyst Precursor In The Dehydrogenation Of Dimethylamine-borane." Master's thesis, METU, 2011. http://etd.lib.metu.edu.tr/upload/12612980/index.pdf.
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Amine boranes have recently been considered as solid hydrogen storage materials with high capability of hydrogen storage. Dimethylamine borane is one of the promising amine boranes with high theoretical gravimetric capacity of 16.9 wt%. Dimethylamine borane can undergo dehydrogenation only in the presence of a suitable catalyst at moderate temperature.
In this project, throughout the dehydrogenation of dimethylamine borane (DMAB), the catalytic activity of ruthenium(III) acetylacetonate was examined for the first time. During the catalytic reaction, formation of a new in-situ ruthenium(II) species, [Ru{N2Me4}3(acac)H], is observed. Mercury poisoning experiment indicates that the in-situ ruthenium(II) species is a homogeneous catalyst in the dehydrogenation of dimethylamine borane. Kinetics of catalytic dehydrogenation of dimethylamine borane starting with ruthenium(III) acetylacetonate was investigated depending on catalyst concentration, substrate concentration and temperature. As a result, the hydrogen generation rate was found to be first-order with respect to catalyst concentration and zero-order regarding the substrate concentration. Besides, evaluation of the kinetic data yielded that the activation parameters for dehydrogenation reaction: the activation energy, Ea = 85 ±2 kJ&bull
mol-1
the enthalpy of activation, DH# = 82 ±
2 kJ&bull
mol-1 and the entropy of activation
DS# = -85 ±
5 J&bull
mol-1&bull
K-1. Additionally, before deactivation, [Ru{N2Me4}3(acac)H] provides 1700 turnovers over 100 hours in hydrogen evolution from the dehydrogenation of dimethlyamine borane. [Ru{N2Me4}3(acac)H] complex formed during the dehydrogenation of dimethylamine borane was isolated and characterized by UV-Visible, FTIR, 1H NMR, and Mass Spectroscopy. The isolated ruthenium(II) species was also tested as homogeneous catalyst in the dehydrogenation of dimethylamine borane.
6
Nerbel, Jörg. "Darstellung, Charakterisierung und Umsetzung von Alkoxiden und Acetylacetonaten des Aluminiums." [S.l. : s.n.], 2001. http://deposit.ddb.de/cgi-bin/dokserv?idn=967485274.
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7
De, Dea Silvia. "Nano-scale magnetic film formation by decompression of supercritical CO₂/ferric acetylacetonate solutions." Diss., Connect to a 24 p. preview or request complete full text in PDF format. Access restricted to UC campuses, 2008. http://wwwlib.umi.com/cr/ucsd/fullcit?p3296800.
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Thesis (Ph. D.)--University of California, San Diego, 2008.Title from first page of PDF file (viewed March 24, 2008). Available via ProQuest Digital Dissertations. Vita. Includes bibliographical references.
8
Sobal, Neli. "Kolloidale Nanosysteme aus magnetischen und metallischen Materialien : Synthese und Charakterisierung." Phd thesis, [S.l. : s.n.], 2003. http://deposit.ddb.de/cgi-bin/dokserv?idn=971615004.
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9
Waechtler, Thomas, Steffen Oswald, Nina Roth, Heinrich Lang, Stefan E. Schulz, and Thomas Gessner. "ALD of Copper and Copper Oxide Thin Films For Applications in Metallization Systems of ULSI Devices." Universitätsbibliothek Chemnitz, 2008. http://nbn-resolving.de/urn:nbn:de:bsz:ch1-200800914.
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As a possible alternative for growing seed layers required for electrochemical Cu deposition of metallization systems in ULSI circuits, the atomic layer deposition (ALD) of Cu is under consideration. To avoid drawbacks related to plasma-enhanced ALD (PEALD), thermal growth of Cu has been proposed by two-step processes forming copper oxide films by ALD which are subsequently reduced.
This talk, given at the 8th International Conference on Atomic Layer Deposition (ALD 2008), held in Bruges, Belgium from 29 June to 2 July 2008, summarizes the results of thermal ALD experiments from [(nBu3P)2Cu(acac)] precursor and wet O2. The precursor is of particular interest as it is a liquid at room temperature and thus easier to handle than frequently utilized solids such as Cu(acac)2, Cu(hfac)2 or Cu(thd)2. Furthermore the substance is non-fluorinated, which helps avoiding a major source of adhesion issues repeatedly observed in Cu CVD.
As result of the ALD experiments, we obtained composites of metallic and oxidized Cu on Ta and TaN, which was determined by angle-resolved XPS analyses. While smooth, adherent films were grown on TaN in an ALD window up to about 130°C, cluster-formation due to self-decomposition of the precursor was observed on Ta. We also recognized a considerable dependency of the growth on the degree of nitridation of the TaN. In contrast, smooth films could be grown up to 130°C on SiO2 and Ru, although in the latter case the ALD window only extends to about 120°C. To apply the ALD films as seed layers in subsequent electroplating processes, several reduction processes are under investigation. Thermal and plasma-assisted hydrogen treatments are studied, as well as thermal treatments in vapors of isopropanol, formic acid, and aldehydes. So far these attempts were most promising using formic acid at temperatures between 100 and 120°C, also offering the benefit of avoiding agglomeration of the very thin ALD films on Ta and TaN. In this respect, the process sequence shows potential for depositing ultra-thin, smooth Cu films at temperatures below 150°C.
10
O'Connor, Helen. "The use of acetylacetonate-based paramagnetic metalloligands in the construction of supramolecular magnetic coordination capsules." Thesis, University of Edinburgh, 2018. http://hdl.handle.net/1842/29547.
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In molecular magnetism, rational design and serendipity have played complementary roles in the synthesis of complexes which display a breadth of interesting physical characteristics. These range from the basic understanding of magneto‐structural correlations, to more complicated phenomena such as slow relaxation of the magnetisation, spin frustration effects, and tuning magnetic interactions with a view to spintronics. The inherent physical properties of these complexes has already afforded molecules which can behave as single‐molecule magnets, singlechain magnets, single‐ion magnets, magnetic metal‐organic frameworks, magnetic refrigerants, and molecular qubits. Even when the building blocks are well known, the rational design of magnetic clusters can be extremely difficult, with the shape and nuclearity often dominated by several internal and external factors. Metallosupramolecular processes proffer an attractive strategy to the rational design of these clusters by making use of structurally‐rigid precursors which, when combined in the correct stoichiometric ratio, can be used to construct various predefined discrete two‐ and three‐dimensional polygons and polyhedra. In particular, the use of metalloligands as structurally‐rigid precursors is appealing, not only because of their often‐straightforward synthesis, but because of their ability to be easily modified in order to create comparable building blocks with different chemical and physical properties. It is therefore surprising that there are limited examples of magnetic architectures built through this approach. Each chapter of this thesis aims to exploit the use of acetylacetonate‐based paramagnetic metalloligands for the synthesis of structurally analogous magnetic coordination capsules, with inherently different magnetic properties. Chapter 2 describes the structural and magnetic studies of fourteen tetradecanuclear coordination cubes, synthesised using the paramagnetic metalloligand [MIIIL3] (MIII = Cr, Fe; HL = 1‐(4‐pyridyl)butane‐1,3‐dione). The heterometallic [MIII8MII6L24]n+ (MII = Co, Ni, Cu, and Pd; n = 0‐ 12) cubes formed from the reaction of [MIIIL3] and a “naked” MII salt are all topologically similar, with the MIII ions occupying the corners of the cubes and the MII ions occupying the faces. Excluding the PdII‐based cube, all of the complexes display magnetic exchange interactions at low temperatures. Due to the enormous size of these clusters and their resulting matrices, the magnetic fitting was done using the process of statistical spectroscopy. Chapter 3 describes the structural and magnetic studies of five [MIII2MII3L6]n+ (MIII = Cr, Fe, and Al; MII = Co, Zn, and Pd; HL = 1‐(4‐pyridyl)butane‐1,3‐dione; n = 0‐6) trigonal bipyramids, built using the diamagnetic and paramagnetic metalloligands [MIIIL3]. [FeIII2CoII3L6Cl6] represents the first magnetic trigonal bipyramid synthesised through the pyridyl‐based metalloligand approach. SQUID magnetometry studies show a weak antiferromagnetic exchange interactions between the FeIII and CoII ions, while EPR spectroscopy measurements demonstrate a small increase in the zero‐field splitting parameter of the FeIII ion upon coordination of [FeIIIL3] to a MII ion. Complete active space self‐consistent field (CASSCF) calculations show the axial zero‐field splitting parameter of CoII to be ≈‐14 cm‐1, which is consistent with the magnetothermal and spectroscopic data. Chapter 4 describes the synthesis and characterisation of six magnetic trigonal bipyramids, synthesised through dynamic covalent reactions of the metalloligand [FeIIILNH23] (HLNH2 = 1‐(4‐ aminophenyl)butane‐1,3‐dione) with either a dialdehyde or diacyl dichloride. The three [FeIII2MII3Lim3]n+ (MII = Co, Ni; n = 0‐6) imine‐based cages are formed from the reaction of the metalloligand with 2,6‐pyridinedicarboxaldehyde in the presence of a templating MII salt and a catalytic amount of acid, whereas the three [FeIII2Lam3] amide‐based cages are formed from the reaction of the metalloligand with isophthaloyl chloride in the presence of a base. The [FeIII2NiII3Lim3]n+ trigonal bipyramid displays weak antiferromagnetic interactions between FeIII and NiII ions, with JFe‐Ni = ‐0.12 cm‐1 and DNi = 8.93 cm‐1, while the [FeIII2Lam3] amide‐based cages display interesting configurational features dominated by the enthalpic gain from a series of intermolecular interactions.
11
Saraidaridis, James D. "Analysis and performance of symmetric nonaqueous redox flow batteries." Thesis, University of Oxford, 2017. http://ora.ox.ac.uk/objects/uuid:2e3533c8-7540-4c14-858f-782292343ae3.
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Symmetric nonaqueous redox flow batteries (RFBs) use negative and positive battery solutions of the same solution composition to operate at high cell voltages. This research effort targets these systems since they offer performance improvements derived from using nonaqueous systems and symmetric active species. Nonaqueous solutions permit significantly higher cell voltages than state-of-the-art aqueous RFBs and symmetric active species chemistries reduce the required complexity of cell reactors. Both performance advantages correspond to significant cost improvements beyond already commercially competitive aqueous RFB chemistries. This document focuses on two classes of symmetric nonaqueous RFB chemistries: coordination complexes such as vanadium acetylacetonate [V(acac)3] or chromium acetylacetonate [Cr(acac)3], and organic active species such as 9,10-diphenylanthracene (DPA). V(acac)3 delivers reversible electrochemistry that supports a 2.2 V equilibrium cell potential, but there are some gaps in the understanding of its degradation mechanisms. Cr(acac)3 supports redox reactions that suggest cell potentials above 4 V, but shows signs of irreversibility in voltammetry experiments and is not yet well understood. Finally, the DPA system could be interesting because it does not use metal active species, and its voltammetry promises cell potentials above 3 V. Yet DPA suffers from low solubility in nonaqueous solvents that limit its practicality. These three systems show promise for symmetric nonaqueous RFBs and offer avenues for further improvement. Voltammetry and spectroelectrochemical electrolysis experiments on the metal coordination complexes clarify the mechanisms behind the voltammetry on these symmetric chemistries. Ligand dissociation causes the irreversible behavior observed in voltammetry on Cr(acac)3. The same experiments reaffirm the expected cyclability of V(acac)3. Chemical functionalization of the DPA center is performed to investigate the solubility and reactivity of various derivatives. Functionalizing DPA with ethylene glycol chains to form 'DdPA' significantly increases solubility limits from 0.6 mM and 44 mM for DPA in acetonitrile and 1,2-dimethoxyethane, respectively, to 12 mM and 0.21 M for DdPA in the same solvents. At the same time, DdPA retains redox activity that promises 3 V cell potentials. Ultimately, a custom, nonaqueous-compatible redox flow reactor was designed and used to test the performance of V(acac)3, DPA, and DdPA under various operating conditions. Contradicting previous reports, V(acac)3 delivers stable cycling over the 21- cycle experimental protocol. Exploration over a range of flow rates and current densities give energy and power densities up to 1.09 WhL-1 and 0.16 Wcm-2, respectively, for the battery solution compositions examined. These experiments further predict values up to 28 WhL-1 and at least 0.22 Wcm-2 for optimized V(acac)3 battery solutions. DPA and DdPA deliver the highest operating potential observed from organic nonaqueous RFBs, discharging at 3 V and 2.9 V, but require further work to understand degradation in the systems.
12
Nyamwihura, Rogers. "Synthesis of Gold Complexes From Diphosphine Ligands and Screening Reactions of Heterocyclic Acetylacetonato (ACAC) Ligands with Transitional Metal Complexes." Thesis, University of North Texas, 2015. https://digital.library.unt.edu/ark:/67531/metadc804890/.
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Syntheses of diphosphine gold (I) complexes from gold THT and two ligands, 4, 5-bis (diphenylphosphino)-4-cyclopenten-1, 3-dione (BPCD) and 2,3-bis(diphenylphosphino)-N-phenylmaleimide (BPPM), were done separately. The reactions happened under ice conditions followed by room temperature conditions and produced two diphosphine gold (I) complexes in moderated yield. Spectroscopic results including nuclear magnetic resonance (NMR) and X-ray crystallography were used to study and determine the structures of the products formed. Moreover, X-rays of all newly synthesized diphosphine gold (I) complexes were compared with the known X-ray structures of other phosphine and diphosphine gold (I) complexes. There were direct resemblances in terms of bond length and angle between these new diphosphine gold (I) complex structures and those already published. For instance, the bond lengths and angles from the newly prepared diphosphine gold (I) complexes were similar to those already published. Where there were some deviations in bond angles and length between the newly synthesized structures and those already published, appropriate explanation was given to explain the deviation. Heterocyclic ligands bearing acetylacetonate (ACAC) side arm(s) were prepared from ethyl malonyl chloride and the heterocyclic compounds 8-hydroxylquinoline, Syn-2-peridoxyaldoxime, quinoxalinol and 2, 6-dipyridinylmethanol. The products (heterocyclic ACAC ligands) from these reactions were screened with transition metal carbonyl compounds in thermolytic reactions. The complexes formed were studied and investigated using NMR and X-ray crystallography. Furthermore, the X-ray structures of the heterocyclic ACAC ligand or ligand A and that of rhenium complex 1 were compared with similar published X-ray structures. The comparison showed there were some similarities in terms of bond length and bond angles.
13
Winter, Silke. "Koordinationspolymere auf der Basis neuer oligofunktioneller Pyridinliganden." Doctoral thesis, Technische Universitaet Bergakademie Freiberg Universitaetsbibliothek "Georgius Agricola", 2009. http://nbn-resolving.de/urn:nbn:de:swb:105-6346328.
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Gegenstand der vorliegenden Arbeit ist der Entwurf und die Realisierung kristalliner organisch-anorganischer Festkörper mit wohldefinierten Hohlraumstrukturen auf der Grundlage von Metallkoordinationen. Basierend auf generellen Prinzipien des Crystal Engineering wurden anhand von drei Typen oligofunktioneller Liganden und ausgewählter koordinationschemischer Synthesemethoden neue polymere Komplexverbindungen hergestellt, die im Hinblick auf Koordinationsgeometrie und Liganddimensionalität strukturspezifische Unterschiede aufweisen. Diese sind durch Anwendung von strukturanalytischen Methoden belegt. Untersuchungsergebnisse der polymeren Komplexe als Rezeptoren für leichtflüchtige Lösungsmittel lassen erkennen, dass sich die erzeugten Koordinationspolymere potentiell als Beschichtungen in massensensitiven Sensoren eignen. Weiterhin konnte durch strukturgeometrische Untersuchungen an Modellkomplexen eine strukturelle Grundlage für den zukünftigen Entwurf von Koordinationspolymeren geschaffen werden.
14
Nielsen, Guilherme Fernandes [UNESP]. "Filmes orgânicos contendo óxido de alumínio depositados a plasma." Universidade Estadual Paulista (UNESP), 2011. http://hdl.handle.net/11449/99661.
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Filmes finos de alumina vêm sendo amplamente estudados em função de suas propriedades físicas e químicas. Em aplicações industriais, filmes de alumina são utilizados, por exemplo, em ferramentas de corte e em circuitos microeletrônicos. Neste trabalho empregou-se o processo de PECVD (do inglês, Plasma Enhanced Chemical Vapor Deposition) para sintetizar fimes contendo óxido de alumínio. Os filmes foram depositados a partir de plasmas excitados por radiofrequencia (13,56 MHz) em misturas de acetilacetonato de alumínio e argônio. Uma configuração experimental inédita foi empregada para permitir a incorporação de alumínio nos filmes: o pó do organometálico foi colocado diretamente no eletrodo por onde um plasma de argônio foi excitado. A pulverização catódica aliada a sublimação do organometálico faz com que haja, em determinadas condições, a deposição de filmes contendo alumina. Foram avaliados os efeitos da pressão do plasma e da potência do sinal de excitação nas propriedades dos filmes resultantes. A técnica de perfilometria foi utilizada para determinar a espessura da camada depositada. Difração de raios X (DRX), com a incidência de ângulos rasantes, foi empregada para investigar a estrutura do material. As técnicas de espectroscopia de absorção no infravermelho por transformada de Fourier (FTIR) e espectroscopia de energia dispersiva (EDS) foram respectivamente utilizadas para analisar a estrutura e a composição química dos filmes. A morfologia das amostras preparadas sobre aço-inoxidável foi analisada por microscopia eletrônica de varredura (MEV) enquanto a dureza foi avaliada por nanoindentação. Foram obtidos filmes amorfos com espessuras de até 7 μm que contêm carbono, alumínio, oxigênio e hidrogênio. Observou-se que as proporções de alumínio e carbono são altamente dependentes da energia cinética dos íons presentes no plasma...
Recently aluminium oxide thin films have been widely studied due to their important physical and chemical properties. Depositions in cutting tools and in microelectronic circuits are examples of industrial applications of industrial applications of aluminum oxide films. In this work, alumina-containing films were prepared by PECVD (Plasma Enhanced Chemical Vapor Deposition) using a new configuration of the plasma system; the metalorganic powder was placed directly on the powered electrode while the substrates were mounted on the grounded topmost electrode. The plasma was excited by applying radiofrequency (13.56 MHz) power to the lower electrode in an argon atmosphere. The sputtering combined with the sublimation of organometallic compound enabled the growth of an alumina-containing organic layer. The effect of the plasma excitation parameters on the properties of the resulting films was studied. Film thickness was measured using profilometry. Grazing angle incidence X-ray diffractometry (GAXRD) was used to determine the structure of the films. Fourier trasnform Infrared Spectroscopy (FTIR) and energy dispersive spectroscopy (EDS) techniques were used to analyze chemical structure and coposition, respectively. The surface morphology was analyzed by scanning electron microscopy (SEM) while film hardness was evaluated by nanoindentation Amorphous organic films were deposited with thicknesses of up to 7 μm. The films were composed of aluminum, carbon, oxygen and hydrogen, the proportions of carbon and aluminum being strongly dependent on the kinetic energy of the ions. The film surface was uniform but presented particulares and, in some cases, wrinkles. The proportion of such defects depends on the plasma excitation parameters
15
Demiralp, Tulin. "Testing The Ruthenium(iii) Acetylacetonate And 1,2-bis(diphenylphosphino)ethane System As Homogeneous Catalyst In The Hydrolysis Of Sodium Borohydride." Master's thesis, METU, 2008. http://etd.lib.metu.edu.tr/upload/3/12609539/index.pdf.
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Recent studies have shown that ruthenium(III) acetylacetonate is acting as homogeneous catalyst in the hydrolysis of sodium borohydride. Although trimethlyphosphite is found to be a poison for the catalytic hydrolysis of sodium borohydride, a longer observation of the reaction in the presence of ruthenium(III) acetylacetonate and 2 equivalent trimethylphosphite shows an unexpected enhancement in the catalytic activity after an induction period. The same rate enhancement is observed when 2 equivalent triphenylphosphine is added into the reaction solution. Addition of 1 equivalent 1,2-bis(diphenylphosphino)ethane, dppe, into the solution shows similarly a rate enhancement in the hydrolysis of sodium borohydride catalyzed by ruthenium(III) acetylacetonate. The effect of 1,2-bis(diphenylphosphino)ethane on the catalytic activity of ruthenium(III) acetylacetonate in the hydrolysis of sodium borohydride was studied by varying mole ratio of dppe / Ru(acac)3, ruthenium concentration, substrate concentration and temperature. The highest enhancement in the rate of hydrolysis was obtained when 1 equivalent dppe was used and therefore, this mole ratio of dppe / Ru(acac)3 was used in the further studies. The rate of the reaction was found to be first order in catalyst concentration and zero order in substrate concentration. From the evaluation of rate constant versus temperature data, the activation parameters for the hydrolysis of sodium borohydride catalyzed by ruthenium(III) acetylacetonate plus 1 equivalent dppe were found to be Ea= 59 ±2 kJ/mol, &
#8710
H&
#8800
= 60 ±
1 kJ.mol-1 and &
#8710
S&
#8800
= -50 ±
3 J.(mol.K)-1. A series of control experiments were performed to characterize the active catalyst. However, the only useful information could be obtained by comparison of the UV-vis electronic absorption spectra taken from the solution during the catalytic reaction, is that, ruthenium(III) is reduced to ruthenium(II) in the course of reaction. It was concluded that a ruthenium(II) species is formed as a transient and may be the active catalyst in the reaction. After the reaction, the only ruthenium species isolated from the solution was the ruthenium(III) acetylacetonate.
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Oluz, Zehra. "Additives For Photodegradable Polyethylene." Master's thesis, METU, 2012. http://etd.lib.metu.edu.tr/upload/12614537/index.pdf.
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Polyethylene (PE) is one of the most popular polymers used in daily life. However, saturated hydrocarbons cannot absorb the energy of light reaching to earth, so degradation process is rather slow which in return cause disposal problems. On the other hand, it was observed that in presence of oxygen and impurities in the polymer matrix, degradation can be rendered to shorter time intervals. This study covers investigation of effect of three different additives in UV induced oxidative degradation of polyethylene.
In this work vanadium (III) acetylacetonate, serpentine and Cloisite 30B were used as additives both together and alone to follow photodegradation of polyethylene. Amount of vanadium (III) acetylacetonate was kept constant at 0.2 wt%, while serpentine and Cloisite 30B were used between 1 and 4 wt%.
All compositions were prepared by using Brabender Torque Rheometer, and shaped as thin films by compression molding. Samples were irradiated by UV light up to 500 hours. Mechanical and spectroscopic measurements were carried out in certain time intervals to monitor the degradation.
It can be concluded that all combinations of three additives showed the fastest degradation behavior compared to pure PE. In the absence of vanadium (III) acetylacetonate the degradation was slowed and fluctuations were observed in the residual percentage strain at break values. There was not a significant change in tensile strength of all samples. Carbonyl index values followed by FTIR were always in increasing manner. Thermal properties were also investigated by DSC Thermograms and they did not change significantly.
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Waechtler, Thomas, Steffen Oswald, Nina Roth, Alexander Jakob, Heinrich Lang, Ramona Ecke, Stefan E. Schulz, et al. "Copper Oxide Films Grown by Atomic Layer Deposition from Bis(tri-n-butylphosphane)copper(I)acetylacetonate on Ta, TaN, Ru, and SiO2." Universitätsbibliothek Chemnitz, 2009. http://nbn-resolving.de/urn:nbn:de:bsz:ch1-200900734.
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The thermal atomic layer deposition (ALD) of copper oxide films from the non-fluorinated yet liquid precursor bis(tri-n-butylphosphane)copper(I)acetylacetonate, [(nBu3P)2Cu(acac)], and wet O2 on Ta, TaN, Ru and SiO2 substrates at temperatures of < 160°C is reported. Typical temperature-independent growth was observed at least up to 125°C with a growth-per-cycle of ~ 0.1 Å for the metallic substrates and an ALD window extending down to 100°C for Ru. On SiO2 and TaN the ALD window was observed between 110 and 125°C, with saturated growth shown on TaN still at 135°C. Precursor self-decomposition in a chemical vapor deposition mode led to bi-modal growth on Ta, resulting in the parallel formation of continuous films and isolated clusters. This effect was not observed on TaN up to about 130°C and neither on Ru or SiO2 for any processing temperature. The degree of nitridation of the tantalum nitride underlayers considerably influenced the film growth. With excellent adhesion of the ALD films on all substrates studied, the results are a promising basis for Cu seed layer ALD applicable to electrochemical Cu metallization in interconnects of ultralarge-scale integrated circuits. © 2009 The Electrochemical Society. All rights reserved. Es wird die thermische Atomlagenabscheidung (ALD) von Kupferoxidschichten, ausgehend von der unfluorierten, flüssigen Vorstufenverbindung Bis(tri-n-butylphosphan)kupfer(I)acetylacetonat, [(nBu3P)2Cu(acac)], sowie feuchtem Sauerstoff, auf Ta-, TaN-, Ru- und SiO2-Substraten bei Temperaturen < 160°C berichtet. Typisches temperaturunabhängiges Wachstum wurde zumindest bis 125°C beobachtet. Damit verbunden wurde für die metallischen Substrate ein Zyklenwachstum von ca. 0.1 Å erzielt sowie ein ALD-Fenster, das für Ru bis zu einer Temperatur von 100°C reicht. Auf SiO2 und TaN wurde das ALD-Fenster zwischen 110 und 125°C beobachtet, wobei auch bei 135°C noch gesättigtes Wachstum auf TaN gezeigt werden konnte. Die selbständige Zersetzung des Precursors ähnlich der chemischen Gasphasenabscheidung führte zu einem bimodalen Schichtwachstum auf Ta, wodurch gleichzeitig geschlossene Schichten und voneinander isolierte Cluster gebildet wurden. Dieser Effekt wurde auf TaN bis zu einer Temperatur von 130°C nicht beobachtet. Ebensowenig trat er im untersuchten Temperaturbereich auf Ru oder SiO2 auf. Der Nitrierungsgrad der TaN-Schichten beeinflusste hierbei das Schichtwachstum stark. Mit einer sehr guten Haftung der ALD-Schichten auf allen untersuchten Substratmaterialien erscheinen die Ergebnisse vielversprechend für die ALD von Kupferstartschichten, die für die elektrochemische Kupfermetallisierung in Leitbahnsystemen ultrahochintegrierter Schaltkreise anwendbar sind
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Jain, Himani Gaur [Verfasser], Volker [Akademischer Betreuer] Buck, and Christian [Akademischer Betreuer] Pflitsch. "Synthesis and characterization of carbon nanowalls by ICP-CVD using Aluminium-Acetylacetonate precursor / Himani Gaur Jain. Gutachter: Christian Pflitsch. Betreuer: Volker Buck." Duisburg, 2012. http://d-nb.info/1026846668/34.
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Masjedi, Mehdi. "Homogeneous Catalysts For The Hydrolysis Of Sodium Borohydride: Synthesis, Characterization And Catalytic Use." Phd thesis, METU, 2010. http://etd.lib.metu.edu.tr/upload/12612290/index.pdf.
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Recent study has shown that ruthenium(III) acetylacetonate acts as a homogeneous catalyst in the hydrolysis of sodium borohydride. When two equivalents of trimethylphosphite per ruthenium is added to the reaction solution containing sodium borohydride and ruthenium(III) acetylacetonate in the mixture of water and tetrahydrofuran, the rate of hydrogen generation is practically stopped (or reduced to the level of self hydrolysis). However, the catalytic hydrogen evolution of sodium borohydride restarts at an unexpectedly high rate in a certain period of time (induction time) after addition of trimethylphosphite. Consequently, trimethylphosphite known to be a poison in the hydrolysis, is involved in the formation of a new active catalyst (ruthenium species containing trimethylphosphite ligands) which has much higher catalytic activity in comparison with sole ruthenium(III) acetylacetonate. The same rate enhancement is observed by addition of two equivalents of triphenylphosphite per ruthenium into the medium. Varying the phosphorus compound affects not only the life time of catalyst but also the kinetic and activation parameters of the hydrolysis of sodium borohydride. However, varying the mole ratio of phosphorus compound to ruthenium does not affect the rate of hydrolysis or in other words, the rate of hydrogen generation is independent of phosphite concentration.
Trans- and cis-[Ru(acac)2{P(OMe)3}2] complexes do not show significant catalytic activity in hydrogen generation of sodium borohydride. However, catalytic activity of cis-isomer is highly increased in the presence of two equivalents of trimethylphosphite, showing that the active catalyst formed during hydrolysis of sodium borohydride starting with Ru(acac)3 or cis-[Ru(acac)2{P(OMe)3}2], has more than two phosphine ligands. For the first time, a ruthenium(I) complex was isolated from aqueous solution after finishing the catalytic hydrolysis of sodium borohydride starting with ruthenium(III) acetylacetonate and trimethylphosphite. Hydridotetrakis(trimethylphosphite)ruthenium(I), [Ru{P(OMe)3}4H] was isolated and characterized by single crystal X-ray diffraction, Mass, UV-visible, FTIR, 1H, 13C and 31PNMR spectroscopy. Following the catalytic reaction by UV-Visible spectroscopy shows in-situ formation of a Ru(II) species which is mostly converted back to ruthenium(III) acetylacetonate after hydrolysis reaction along with formation of [Ru{P(OMe)3}4H] complex as a minor product. Although Ru(II) species could not be isolated, adding 1 equivalent of 2,2'-bipyridine yielded [Ru(acac)(bipy){P(OMe)3}H] complex which could be isolated and characterized by Mass, UV-Visible, FTIR, 1H, 13C and 31PNMR spectroscopy. In-situ generated Ru(II) species has much higher catalytic activity in comparison with its stabilized form [Ru(acac)(bipy){P(OMe)3}H] or [Ru{P(OMe)3}4H] complex. Conclusively, the fac-[Ru(acac){P(OMe)3}3H] complex is believed to be the in-situ generated Ru(II) species and the active catalyst in the hydrolysis of sodium borohydride.
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Nielsen, Guilherme Fernandes. "Filmes orgânicos contendo óxido de alumínio depositados a plasma /." Bauru : [s.n.], 2011. http://hdl.handle.net/11449/99661.
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Orientador: Elidiane Cipriano RangelBanca: Rogerio Valentim Gelamo
Banca: Sandro Doninini Mancini
O programa de Pós graduação em Ciência e Tecnologia de Materiais, PosMat, tem carater institucional e integra as atividades de pesquisa em materiais de diversos campi da UNESP
Resumo: Filmes finos de alumina vêm sendo amplamente estudados em função de suas propriedades físicas e químicas. Em aplicações industriais, filmes de alumina são utilizados, por exemplo, em ferramentas de corte e em circuitos microeletrônicos. Neste trabalho empregou-se o processo de PECVD (do inglês, Plasma Enhanced Chemical Vapor Deposition) para sintetizar fimes contendo óxido de alumínio. Os filmes foram depositados a partir de plasmas excitados por radiofrequencia (13,56 MHz) em misturas de acetilacetonato de alumínio e argônio. Uma configuração experimental inédita foi empregada para permitir a incorporação de alumínio nos filmes: o pó do organometálico foi colocado diretamente no eletrodo por onde um plasma de argônio foi excitado. A pulverização catódica aliada a sublimação do organometálico faz com que haja, em determinadas condições, a deposição de filmes contendo alumina. Foram avaliados os efeitos da pressão do plasma e da potência do sinal de excitação nas propriedades dos filmes resultantes. A técnica de perfilometria foi utilizada para determinar a espessura da camada depositada. Difração de raios X (DRX), com a incidência de ângulos rasantes, foi empregada para investigar a estrutura do material. As técnicas de espectroscopia de absorção no infravermelho por transformada de Fourier (FTIR) e espectroscopia de energia dispersiva (EDS) foram respectivamente utilizadas para analisar a estrutura e a composição química dos filmes. A morfologia das amostras preparadas sobre aço-inoxidável foi analisada por microscopia eletrônica de varredura (MEV) enquanto a dureza foi avaliada por nanoindentação. Foram obtidos filmes amorfos com espessuras de até 7 μm que contêm carbono, alumínio, oxigênio e hidrogênio. Observou-se que as proporções de alumínio e carbono são altamente dependentes da energia cinética dos íons presentes no plasma... (Resumo completo, clicar acesso eletrônico abaixo)
Abstract: Recently aluminium oxide thin films have been widely studied due to their important physical and chemical properties. Depositions in cutting tools and in microelectronic circuits are examples of industrial applications of industrial applications of aluminum oxide films. In this work, alumina-containing films were prepared by PECVD (Plasma Enhanced Chemical Vapor Deposition) using a new configuration of the plasma system; the metalorganic powder was placed directly on the powered electrode while the substrates were mounted on the grounded topmost electrode. The plasma was excited by applying radiofrequency (13.56 MHz) power to the lower electrode in an argon atmosphere. The sputtering combined with the sublimation of organometallic compound enabled the growth of an alumina-containing organic layer. The effect of the plasma excitation parameters on the properties of the resulting films was studied. Film thickness was measured using profilometry. Grazing angle incidence X-ray diffractometry (GAXRD) was used to determine the structure of the films. Fourier trasnform Infrared Spectroscopy (FTIR) and energy dispersive spectroscopy (EDS) techniques were used to analyze chemical structure and coposition, respectively. The surface morphology was analyzed by scanning electron microscopy (SEM) while film hardness was evaluated by nanoindentation Amorphous organic films were deposited with thicknesses of up to 7 μm. The films were composed of aluminum, carbon, oxygen and hydrogen, the proportions of carbon and aluminum being strongly dependent on the kinetic energy of the ions. The film surface was uniform but presented particulares and, in some cases, wrinkles. The proportion of such defects depends on the plasma excitation parameters
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Schreck, Heinrich [Verfasser]. "Ueber die Chelatbildung und Extraktion des dreiwertigen Actiniums, Americiums, Curiums und Californiums mit Acetylaceton und einigen seiner Derivate / Heinrich Schreck." Karlsruhe : KIT-Bibliothek, 2008. http://d-nb.info/1186086467/34.
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Erbe, Manuela, Jens Hänisch, Thomas Freudenberg, Anke Kirchner, Stefan Kaskel, Ingolf Mönch, Ludwig Schultz, and Bernhard Holzapfel. "Improved REBa₂Cu₃O₇₋ₓ (RE ═ Y, Gd) structure and superconducting properties by addition of acetylacetone in TFA-MOD precursor solutions." Royal Society of Chemistry, 2014. https://tud.qucosa.de/id/qucosa%3A36162.
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For developing commercially utilized high-performance high-temperature superconductors, the fabrication of biaxially textured (RE)Ba₂Cu₃O₇₋ₓ (REBCO, RE ═ Y, Gd) coated conductors via metal–organic decomposition of trifluoroacetate precursors (TFA-MOD) has become an interesting strategy for industrial scale-up due to low costs and simple operation. However, the hygroscopic nature of commonly used precursor solutions makes them very sensitive to water pollution through air humidity. This can lead to a degradation of the final microstructure, which in return deteriorates critical current densities. Here, we present a new method to overcome that problem by using a moderator of 2,4-pentanedione (acac) in a pre-existing REBCO precursor solution. Our results show that even initially low-performance solutions can be enhanced to such an extent that they finally outperform standard high-performance solutions and the temperature window for their optimal growth widens significantly. Scanning electron microscopy gives evidence of considerable microstructural improvements, e.g. avoidance of pore formation and grooves, reduction of buckling and surface granularity. X-ray investigations indicate texture improvements, and electrical measurements reveal that transport critical current densities (Jc) increase in self-field and applied magnetic fields. For YBCO, a molar ratio of acac/RE ═ 0.64 is most effective and leads to an increase of the maximum pinning force density Fmaxp from 1.0 to 2.4 GN mˉ³ at 77 K. For GdBCO, a broad window of annealing temperatures (790–840°C) is possible for films with Jc values above 2.9 MA cmˉ² and Fmaxp above 3 GN mˉ³ at 77 K.
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FILOTTI, LIVIU. "Composites cerine - alumine. Preparation et caracterisation des precurseurs acetylacetonates de cerium. Reduction de la cerine en conditions douces. Essais de metallisation selective." Paris 7, 1998. http://www.theses.fr/1998PA077054.
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Des echantillons de cerine hautement dispersee sur l'alumine sont prepares soit par impregnation de ce(no#3)#3. 6h#2o soit par greffage du chelate ce(acac)#4 (acac = pentane-2,4-dionato-o,o). Plusieurs ameliorations sont d'abord apportees aux procedures de synthese et a la caracterisation de ce chelate de cerium(iv). Pour le complexe de cerium(iii) avec le meme ligand, ce(acac)#3. (h#2o)#2. H#2o, une structure est proposee a partir du diagramme de drx et de donnees spectrales (ir, uv-visible, proche ir). Les especes intermediaires resultant de l'impregnation ou du greffage sont ensuite analysees par reflexion diffuse (uv-visible, pir) et analyse gravimetrique. Les nanoparticules de cerine supportee obtenues par l'oxydation de ces especes ont une taille moyenne plus faible dans le cas du greffage (2,5 a 4 nm) que dans celui de l'impregnation (6 a 8 nm). La largeur de bande interdite de la cerine supportee augmente pour des tailles de particules inferieures a 5 nm (effet quantique). Des bandes sont egalement observees au-dela du seuil d'absorption ( < 350 nm) ; elles sont attribuees a des transitions localisees de transfert de charge ce#4#+ o#2# impliquant des ions superficiels a coordinence incomplete. La reduction superficielle de la cerine (massique ou supportee) par l'hydrazine en conditions douces conduit a l'apparition de nouveaux etats electroniques dans la bande interdite. L'etude spectroscopique, principalement par uv-vis et rpe, permet d'associer ces etats a des cations ce#3#+ et a des lacunes anioniques (centres de couleur de type f). Les essais de metallisation selective de la cerine des composites ceo#2/al#2o#3 sont realises selon deux methodes originales, la deposition electroless et la photoreduction a l'interface semi-conducteur/solution. Le but recherche a ete approche dans le cas du palladium, mais pour le platine la deposition selective a echoue, en raison des cinetiques de reduction defavorables. Cependant, les resultats obtenus suggerent une procedure combinee (en deux etapes : irradiation + reduction), qui semble prometteuse pour la fixation selective du platine.
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Winter, Silke. "Koordinationspolymere auf der Basis neuer oligofunktioneller Pyridinliganden - Synthese, Charakterisierung und Anwendungspotenzial." Doctoral thesis, Freiberg : TU Bergakademie Freiberg, Fakultät Chemie und Physik, 2003. https://fridolin.tu-freiberg.de/archiv/html/ChemieWinterSilke634632.html.
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Riazanova, Anastasia. "Direct Nanoprototyping of Functional Materials via Focused Electron Beam." Doctoral thesis, KTH, Teknisk materialfysik, 2013. http://urn.kb.se/resolve?urn=urn:nbn:se:kth:diva-132365.
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During recent years the demand for nanoscale materials with tailor-made functional properties as bulk species, is continuously and progressively rising for such fields as e.g. micro- and nano-electronics, plasmonics, spintronics, bio-technology, bio-sensing and life sciences. Preserving and / or improving properties of functional materials with their simultaneous size reduction and high-resolution site-specific positioning is indeed very challenging, for both conductors and insulators. One of the advanced nanoprototyping methods that can be utilized for this purpose is the Electron-Beam-Induced Deposition, or shortly EBID. This process is based on a local decomposition by a focused electron beam of a precursor gas molecules adsorbed on the sample’s surface. The beauty of this method is that it gives a unique possibility of rapid creation of site-specific nanoscale 3D structures of precise shape in a single operation. It’s an additive process that can be easily combined with other patterns. However, besides all the benefits, EBID has some constraints, in particular low purity of the deposited materials, due to the organometallic nature of the used precursors. Chemical composition of EBID patterns is strongly dependent on the chosen gas chemistry, the substrate, many deposition parameters and post-treatment processes applied to the deposited structures. In our research we focused on deposition of Co, Au, SiO2, C, W and Pt, their purification and shape control. And this thesis presents an overview of our accomplishments in this field. Depending on the gas chemistry of interest, three major purification approaches of EBID-grown materials were tested out: - Post-deposition annealing: in air and in the controlled atmosphere, - Deposition onto a preheated substrate, - Deposition in the presence of reactive gases. As a result, a dramatic purity improvement was observed and a significant advancement was achieved in creation of high-purity gold, cobalt and silicon dioxide nanoscale structures. In particular: 1) For the Me2Au(acac) precursor, we developed a nanofabrication routine combining application of wetting buffer layers, fine tuning of EBID parameters and subsequent post-annealing step, which led to formation of high-purity planar and high aspect ratio periodic Au nanopatterns. We also describe the adopted and gently adjusted wet etching method of undesirable buffer layer removal, required in some cases for the further device application. 2) For the Co2(CO)8 precursor, in-situ seeded growth in conjunction with EBID at the elevated substrate temperature resulted in a deposition of pure nanocrystalline Co with magnetic and transport properties close to the bulk material. 3) For the tetraethyl orthosilicate precursor, or shortly TEOS, assisting of the deposition process with the additional oxygen supply led to the EBID of carbon-free amorphous insulating Si-oxide, with the absorption and refraction properties comparable to those for fused silica. Several applications of EBID nanopatterns are also discussed.QC 20131028
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Goma, Joseph. "Préparation et caractérisation de catalyseurs de type ziegler utilises en synthèse fischer-tropsch en phase liquide." Poitiers, 1988. http://www.theses.fr/1988POIT2328.
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Etude de la reaction dans le benzene et dans le melange benzene-hexane du triethylaluminium avec les acetylacetonates de cobalt (co(acac)::(2) et co(acac)::(3)). La nature des synthons depend du rapport co/al. Comparaison avec le diethylzinc
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Battaglin, Felipe Augusto Darriba [UNESP]. "Abordagem inovadora com plasma de baixa temperatura para a deposição de filmes a partir do acetilacetonato de alumínio." Universidade Estadual Paulista (UNESP), 2016. http://hdl.handle.net/11449/143092.
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Filmes de alumina foram depositados a partir de uma nova metodologia de deposição a plasma, utilizando o pó de acetilacetonato de alumínio (AAA) como precursor. Em trabalho prévio do grupo, foi demonstrada a viabilidade do sputtering do AAA em plasmas de argônio para deposição de filmes finos. Os bons resultados obtidos estimularam o desenvolvimento do presente trabalho, visando o aperfeiçoamento da metodologia de deposição. Para isso, primeiramente foram investigados os efeitos da alteração da composição química da atmosfera do plasma, por meio da incorporação de diferentes proporções de oxigênio (O2%) ao argônio, tornando o processo um sputtering reativo. As deposições foram realizadas espalhando-se o pó do AAA no eletrodo inferior de um sistema de plasma acoplado capacitivamente. Argônio, oxigênio ou a mistura de ambos foram admitidos até a pressão de 11,0 Pa. O plasma foi gerado pela aplicação de sinal de radiofrequência (13,56 MHz, 150 W) ao eletrodo contendo o pó, mantendo-se o eletrodo superior, também utilizado como porta-amostras, aterrado. O tempo de deposição foi de 90 minutos. Investigou-se o efeito da O2%, variada de 0 a 100%, nas propriedades dos filmes. Na etapa subsequente, filmes foram depositados por sputtering reativo utilizando-se a condição considerada ótima na última etapa do trabalho (O2% = 25%) e mantendo-se as condições de pressão, potência e tempo de tratamento constantes. Todavia, ao invés de aterrar o porta-amostras, pulsos retangulares negativos (600 V, 2 kHz, 1-100% de ciclo de trabalho) foram aplicados, promovendo bombardeamento iônico durante a deposição por sputtering reativo. O efeito do ciclo de trabalho dos pulsos nas propriedades dos filmes foi avaliado. Na última etapa do trabalho, filmes foram depositados pelo sputtering reativo a partir de atmosferas contendo 25% de O2 e 75% de Ar e em condições mais energéticas que as utilizadas nos ciclos anteriores. Para tal um primeiro conjunto de amostras foi preparado mediante aquecimento resistivo do porta-amostras (410ºC) em plasma de menor pressão (4,0 Pa) que a anteriormente utilizada. O tempo de deposição foi de 28 minutos. Um segundo conjunto de amostras foi preparado associando-se bombardeamento iônico de mais alta energia, pela aplicação de pulsos de 1200 V (20% ciclo de trabalho) ao porta-amostras e também reduzindo a pressão da atmosfera de deposição para 4,0 Pa. Nesta condição, o tempo de deposição foi de 60 minutos. Comparou-se os resultados obtidos nestes experimentos aos equivalentes obtidos anteriormente. A espessura da camada foi obtida por meio de um perfilômetro e a taxa de deposição pela razão entre espessura e tempo de deposição. A composição elementar e a estrutura molecular dos filmes foram investigadas através das técnicas de espectroscopia de retroespalhamento Rutherford e de absorção no infravermelho, respectivamente. Difração de raios X foi utilizada para investigar a microestrutura dos filmes. Inspeções na morfologia e composição química das superfícies foram conduzidas associando microscopia eletrônica de varredura e espectroscopia de energia dispersiva. A rugosidade foi derivada de perfis topográficos adquiridos por perfilometria e microscopia de força atômica, enquanto a molhabilidade da superfície foi determinada através da técnica de gota séssil. De forma geral, os filmes depositados apresentaram contribuições de grupos orgânicos e de inorgânicos relacionados à alumina amorfa. O aumento da O2% afetou a cinética do plasma, proporcionando alterações na taxa de deposição (1 a 25 nm/min), rugosidade (1 a 13 nm) e redução na concentração de carbono proveniente do precursor, de 43% (O2% = 0%) para 6% (O2% = 100%). Com o aumento na O2% também foram encontradas variações na densidade dos filmes, dentro da faixa de 0,7 a 1,9 g/cm³, e tendência de queda no ângulo de contato de 53 para 17°. Por sua vez, quando o bombardeamento iônico é associado ao processo de deposição, altera-se a taxa de crescimento dos filmes (3 a 29 nm/min) e a morfologia da superfície, por meio do alívio de tensões internas e aumento da estabilidade física da estrutura resultante. A composição química não sofreu alterações, devido as condições do sputtering reativo permanecerem inalteradas nas deposições. Já a rugosidade e a molhabilidade da superfície apresentaram comportamentos condizentes com os resultados da morfologia e topografia. Quando condições mais energéticas de deposição foram empregadas, filmes óxidos com contaminações orgânicas foram obtidos para a deposição que empregou aquecimento resistivo do porta-amostras. Nesta condição, devido a redução na pressão total, mesmo com o aquecimento resistivo a taxa de deposição foi maior (~ 6 vezes) que aquela obtida sem aquecimento. Para a situação em que bombardeamento iônico de alta energia foi utilizado, estrutura e composição química similares ao do composto precursor foram obtidas. Os resultados são interpretados em termos dos processos predominantes em cada uma das metodologias empregadas.
Alumina films were deposited by a new plasma deposition method using aluminum acetylacetonate (AAA) powder as precursor. In a previous study by our group, the feasibility of AAA sputtering in argon plasmas for thin films deposition was demonstrated. The good results obtained stimulated the development of this work, aiming at the improvement of the deposition methodology. For this, the effects of modifications in the chemical composition of the plasma atmosphere were first investigated, through the use of different oxygen to argon proportions (O2%), making the process a reactive sputtering. The depositions were performed by spreading the AAA powder on the lower electrode of a capacitively coupled plasma system. Argon, oxygen or a mixture of both were admitted up to a pressure of 11.0 Pa. Application of radiofrequency power (13.56 MHz, 150 W) to the powder covered electrode generated the plasma, keeping the upper electrode, also used as a sample holder, grounded. Deposition times of 90 minutes were used. The effects of varying the oxygen proportion from 0 to 100%, on the film properties were studied. In the subsequent stage, films were deposited by reactive sputtering using the condition considered best in the last stage of the work (O2% = 25%) and keeping the pressures, power and treatment time constant. Instead of grounding the sample holder, however, negative rectangular pulses (600 V, 2 kHz, 1-100% duty cycle) were applied, promoting ion bombardment during the deposition by reactive sputtering. The influence of the pulse duty cycle on the properties of the films was evaluated. In the last study stage, films were deposited by reactive sputtering from atmospheres containing 25% O2 and 75% Ar and with more energetic conditions than those used in previous cycles. For such, a first samples set was prepared by resistive heating of the sample holder (410ºC) in a lower plasma pressure (4.0 Pa) than that previously used. The deposition time was 28 minutes. A second samples set was carried out associating ion bombardment of the highest energy, by the application of the 1200 V pulses (20% duty cycle) to the sample holder and also reducing the pressure of the deposition atmosphere to 4.0 Pa. In this condition, the deposition time was 60 minutes. The results obtained in these experiments were compared to the equivalent obtained previously. Film thickness was obtained by profilometry and the deposition rate calculated as the ratio between the thickness and deposition time. Elemental composition and molecular structure of the films were investigated using Rutherford backscattering and infrared absorption spectroscopy, respectively. X-ray diffraction was used to investigate the microstructure of the films. Surface morphology and chemical composition were studied using scanning electron microscopy and energy dispersive spectroscopy. Roughness was derived from topographic profiles acquired by profilometry and atomic force microscopy, whereas the surface wettability was determined using the sessile drop technique. In general, the deposited films showed contributions from organic and inorganic groups related to amorphous alumina. Increasing in O2% affected the plasma kinetics, providing changes in deposition rate (1 to 25 nm/min), roughness (1 to 13 nm) and reduction in the carbon concentration coming from the precursor, 43% (O2% = 0%) to 6% (O2% = 100%). With the increase in O2% it was also found variations in the films density, within the range from 0.7 to 1.9 g/cm³, and a downward trend in the contact angle of 53 to 17°. In turn, when the ion bombardment is associated with the deposition process, changes are found in the deposition rate (3 to 29 nm/min) and the surface morphology, through the internal strains relief and increased in the physical stability of resulting structure. The chemical composition did not suffer changes because the conditions of the reactive sputtering remain unchanged in the depositions. The roughness and surface wettability showed behavior consistent with the morphology and topography results. When more energetic conditions were employed, oxide films with organic contaminations were obtained for the deposition which applied the sample holder resistive heating. In this condition, due to the reduction in the total pressure, even with the resistive heating the deposition rate was higher (~ 6 times) than that obtained without heating. For the situation which high-energy ion bombardment was used, the structure and chemical composition similar to the precursor were obtained. The results are interpreted in terms of the prevailing processes in each of the methodologies applied.
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Graciun, Steliana. "Transfert de proton par effet tunnel dans des cristaux à liaison hydrogène : étude par spectroscopie optique des dimères d'acide benzoïque et de la molécule d'acétylacétone." Université Joseph Fourier (Grenoble), 1999. http://www.theses.fr/1999GRE10259.
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L'introduction d'une molecule dopante (le friedlander-thioindigo) en site de substitution dans un cristal d'acide benzoique permet de sonder dans son voisinage la dynamique des protons acides. Le transfert concerte de protons, par effet tunnel, le long des liaisons hydrogene intermoleculaires au sein des dimeres d'acide benzoique est caracterise a partir des spectres optiques du dopant. L'element de matrice d'effet tunnel est mesure par la technique de brulage de trous spectraux. Cette donnee experimentale permet de tester la validite des modeles theoriques concernant le transfert de proton. Les mesures optiques (absorption, emission) sont aussi utilisees pour analyser l'influence de la nature et de la taille du dopant sur la dynamique des protons. L'etude par spectroscopie raman de l'acetylacetone dans sa forme enolique apporte des informations sur la localisation ou la delocalisation du proton le long de la liaison hydrogene intramoleculaire, en fonction de la temperature. Quelques resultats preliminaires de diffusion de neutron ont ete obtenus sur ce cristal. Dans la perspective d'une etude plus approfondie, des molecules d'acetylacetone selectivement deuterees ont ete preparees, puis caracterisees par resonance magnetique nucleaire.
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Khayar, Mohammed. "Étude de l'adsorption des tensio-actifs sur les minéraux peu conducteurs : caractérisation diélectrique : application a la flottation des pulpes minérales." Nancy 1, 1993. http://www.theses.fr/1993NAN10057.
Full textAbstract:
Les techniques diélectriques haute fréquence (0,4-120 mhz) permettent de préciser in situ la nature des interactions adsorbat/adsorbant lors des processus de flottation, grâce à la détermination de la permittivité complexe. L'adsorption de l'oléate de sodium (collecteur complexant) sur les minéraux de type sel (fluorine, barytine et calcite) et celle de la salicylaldoxime et de l'acetylacetone (collecteurs chelatants) sur la malachite entrainent une augmentation sensible de la permittivité diélectrique indépendamment de la fréquence. L'interaction adsorbat/adsorbant serait donc de type chimique. Les collecteurs agissant par effet électrostatique tels que le dodecylsulfate et la dodecylamine (collecteurs ioniques) ont peu d'effet sur les caractéristiques diélectriques des pulpes minérales. La grande sensibilité de la technique permet d'analyser les phénomènes d'adsorption au cours de la formation de la monocouche. Elle s'est révélée particulièrement efficace pour l'étude du pouvoir déprimant des composés tels que le quebracho ou le silicate de sodium et des phénomènes de coadsorption collecteur-déprimant
30
Travnikova, Oksana. "Structure and Dynamics of Core-Excited Species." Doctoral thesis, Uppsala : Acta Universitatis Upsaliensis, 2008. http://urn.kb.se/resolve?urn=urn:nbn:se:uu:diva-8904.
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Ndwandwe, Silindile Nomathemba. "Synthesis and characterization of carbon nanomaterials using BIS(acetylacetonato)oxovanadium(IV), Manganese(III) Acetylacetonate, Co-Zn and CoAI as catalyst precursors." Thesis, 2011. http://hdl.handle.net/10352/120.
Full textAbstract:
Thesis. (M.Tech. (Chemistry)) -- Vaal University of Technology, 2011.Bis(acetylacetonato)oxovanadium(IV), Manganese(III) acetylacetonate, Co-Zn and Co-Al were prepared as catalyst precursors for the synthesis of carbon materials in a catalytic chemical vapor deposition (CCVD) reactor. The carbon materials produced were characterized with Raman spectroscopy, Scanning electron microscope (SEM), Energy dispersive spectroscopy (EDS), X-ray diffraction (XRD), High resolution transmission electron microscopy (TEM) and Thermogravimetric analysis, (TGA). Carbon material prepared from bis(acetylacetonato)oxovanadium(IV) catalyst precursor showed the presence of carbon spheres with average diameter of 104μm together with small traces of carbon nanotubes or amorphous carbon. Synthesis of bis(acetylacetonato)oxovanadium(IV) catalyst precursor yielded approximately 92% of carbon material. Carbon material prepared from Manganese(III) acetylacetonate catalyst precursor showed the presence of carbon spheres with diameter of 87.5μm. Synthesis of Manganese(III) acetylacetonate catalyst precursor yielded approximately 97% of carbon material. Carbon material produced from Co-Zn and Co-Al catalyst precursors showed the presence of carbon nanotubes with small amounts of amorphous carbon. The use of Co-Zn catalyst precursor yielded approximately 80% of carbon nanotubes, whereas Co-Al catalyst precursor yielded approximately 98% of carbon nanotubes.
Vaal University of Technology; NRF; SASOL
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Chen, May Lin, and 陳美玲. "Structural studies of bis(acetylacetonato)titanium(IV) complexes." Thesis, 1994. http://ndltd.ncl.edu.tw/handle/24577207228666485863.
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Chen, Yu-Ting, and 陳郁婷. "The NMR Investigation on the Keto‒Enol Tautomerization of Acetylacetone." Thesis, 2018. http://ndltd.ncl.edu.tw/handle/838tv8.
Full textAbstract:
碩士中原大學
化學研究所
106
The fascinating tautomerization process involving hydrogen migration of acetylacetone (denoted as Acac) has drawing much research attention over the past years. This microscopic molecular level tautomerization process will result in the macroscopic ensemble Keto‒to‒Enol equilibrium. In order to have a global understanding of the Acac tautomerization, the nuclear magnetic resonance (NMR) technology was used on both the microscopic electron cloud investigation (such as chemical shift observation) and the macroscopic ensemble average phenomenon of spectra themself. Thermodynamically, the Keto‒to‒Enol interstructural conversion of Acac is essentially an enthalpy-controlled mechanism. Besides the relatively fixed bond energy and conjugated resonance energy, the intramolecular hydrogen bonding of Acac plays a key role in the Acac’s Enol/Keto ratio. A series of multinuclear 1H, 2D, 13C, 17O and diffusion experiments in different solvents, temperatures, and concentrations were performed. Experimental results show that the Keto to Enol ratio of pure Acac is roughly 1 : 4. The main factor that affects Acac’s Enol/Keto ratio is the intramolecular hydrogen bond strength of the Enol structure. A higher temperature is thus more favorable to the Keto form structure. A lower dielectric constant solvent has less effect on the intramolecular hydrogen bond strength and therefore favors the Enol tautomer. Protic solvents, such as water, will quickly and completely destroy the intramolecular hydrogen bonding and cause the Acac to have more Keto molecules than its Enol molecules.
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Mariba, Epiphania Rumbidzai Memoraine. "Gas phase extraction of metals from oxides using the ligand acetylacetone." Thesis, 2010. http://hdl.handle.net/10539/8748.
Full textAbstract:
Gas phase extraction using organic ligands has been gaining interest because it
eliminates many of the problems encountered in conventional mineral processing
methods. This process was successfully used to extract iron using the ligand
acetylacetone from Fe2O3 in a fluidized bed reactor, with above 80% extraction being
achieved after four hours for some experimental conditions. The extraction was
shown to be dependent on temperature, ligand flow rate and the surface area available
for reaction, with extraction increasing as each of the variables was increased.
Chrome could not be extracted successfully, with only a maximum of 12% extraction
being achieved after four hours. It was shown that the process could be used to
successfully separate mixtures containing both iron and chrome oxides by extracting
iron and leaving chrome in the solid phase. Classic shrinking core reaction models
were tested on data obtained to evaluate their fit of experimental data with theoretical
predictions. The chemical reaction limiting shrinking core model was suggested to be
the one that predominantly described the experimental data. There is need however to
develop a model which takes into account the influence of all the variables identified
as affecting the extraction. There is also need to identify ligands which will react
selectively with other metal oxides and not iron in order to the see if the other metals
can also be successfully extracted. Further work should be done on this promising
technology.
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Dikio, Charity Wokwu. "Synthesis, characterization and anti-bacterial studies or Hydrazide Schiff bases of Acetylacetonate metal complexes." Thesis, 2014. http://hdl.handle.net/10352/303.
Full textAbstract:
M. Tech. (Chemistry, Department of Chemistry), Vaal University of TechnologyInfectious diseases, a group of illnesses caused by specific pathogens or its toxins is a leading cause of death globally. Treatment with antibiotics is a key intervention in the control and management of many infectious disease. However, the increasing incidence of antibiotics failure, due to the emergence of drug resistant pathogens, is rendering the use of antibiotics chemotherapy ineffective. A possible solution is to synthesize new compounds with broad spectrum characteristics and superior drug performances as alternative to conventional antibiotics. Schiff Bases are biologically active ligands. They form metal complexes with superior biological activities. This research aims to synthesize some Schiff Base metal complexes and investigate their biological effects on Staphylococcus aureus and Enterococcus faecalis. Metal acetylacetonates of Vanadium, Copper, Cobalt, Zinc, Magnesium, Manganese, Cadmium, Nickel and Iron were synthesized and characterized by Fourier transform infrared spectroscopy. Four Schiff bases, LI, L2, L3 and L4 were also synthesized by the condensation of 4- (diethylamino)-2-hydroxybenzaldehyde with 4-nitrobenzohydrazide and 4-methoxybenzohydrazide to form L1 and L2. 4-(dimethylamino) benzaldehyde was reacted with 4-nitrobenzohydrazide and 4-methoxybenzohydrazide to form L3 and L4 respectively. The Schiff base ligands were then reacted with synthesized Vanadium, manganese, cobalt and magnesium acetylacetonates to form Schiff base complexes (SBC 1A to 4D). Schiff bases ligands and complexes were characterized by FT-IR, 1H-NMR, 13C-NMR, TGA and DTA. Fourier Transform infrared spectroscopy (FTIR) of the acetylacetonates showed the formation of metal acetylacetonates as characterized by the absence of the carbonyl stretching n(C=O) vibration in metal acetylacetonate spectra as compared to pure acetylacetone. Metal acetylacetonates also showed the presence of metal oxygen vibration frequency, n(M-O-C), in the spectra obtained. Thermogravimetric analysis (TGA) and Derivative or Differential Thermogravimetric analysis (DTA) of the Schiff base ligands showed the presence of a single decomposition product in L1, L2, L3 and L4 indicating the formation of a single reaction product while those of Schiff base complexes showed the formation of several decomposition products. Proton and carbon thirteen Nuclear Magnetic Resonance (1H- and 13C-NMR) spectroscopy of the Schiff base ligands indicated the presence of hydrogen and carbon-13 in different environments. The chemical shifts of the hydrogens and carbon-13 provided evidence that Schiff base ligands were formed. The strongest evidence is the presence of the azomethine hydrogen and carbon in the spectra of the Schiff base ligands. The presence of aromatic hydrogens and carbon at chemical shift environments found in literature also confirmed the formation of Schiff base ligand. The NMR spectra of Schiff base complexes showed the presence of azomethine (HC=N) and aromatic hydrogens at expected chemical shifts. The synthesized Schiff bases and their corresponding metal complexes were screened for their invitro antibacterial activities against two Gram-positive (Staphylococcus aureues and Enterococcus feacalis) bacterial strains by the Agar-well diffusion methods.The ligands and complexes were tested against confirmed S. aureus and E. faecalis strains and only 4 exhibited antimicrobial activities. The ligands and complexes were effective against the S. aureusand E. faecalis isolates.
VUT
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Kao, Hsiao-Wen, and 高筱雯. "Preparation and Characterization of Titanium Dioxide Nanoparticles Using different Acetylacetonate Titanium Precursors by Hydrothermal Method." Thesis, 2007. http://ndltd.ncl.edu.tw/handle/776arg.
Full textAbstract:
碩士國立臺北科技大學
有機高分子研究所
95
The semiconductor photochemical catalysis is the new technology for organic pollution that is paid much attention to at present. Many scholars carry on a large amount of research work in the photochemical catalysis organic waste water and atmospheric organic pollutant aspect , discovered titanium dioxide has suitable potentiality to the remaining organic matter regarding in the waste water toxic material as well as the air.The photocatalytic application of TiO2 nanoparticles shows strong correlation with its particle size and crystal property. Therefore, the systematic investigation on the TiO2 synthesis as well as the crystal phase evolution of the TiO2 product becomes very important. In general, TiO2 synthesis used precursors for the titanium alkoxide or titanium metal salt which are hydrolyzed and thermal treatment to obtain TiO2 crystals. Some reports indicated that adding chealting agent in the process of TiO2 synthesis effects the particle size, homogeneity, and crystallize of the final products. In this work, we have designed the new type of TiO2 precursors: Titanium isopropoxide (1) and titanium bis(acetylacetonate) diisopropoxide (2) as initial compound for TiO2 synthesis that used hydrothermal method and high temperature calcination. prepared for TiO2 crystals . Hydrothermal method can avoid the titanium dioxide surface OH dehydration causes the titanium dioxide particle size increase and surface area decrease at high temperature in the calcine process, influence its photochemical catalysis result. Such prepared TiO2 samples were characterized by X-ray diffraction (XRD) for the crystal structure, by transmission electron microscopy (TEM) for dimensions and distribution, by electron spectroscopy for chemical analysis (ESCA) for chemical state and by nitrogen gas adsorption/desorption isotherm for surface area measurement. By tailing the reaction condition, such as the content of acetylacetonate in the precursor molecule, the reaction time, and the calcinations temperature, the growth of TiO2 particles can be well controlled. The preliminary results show that using both precursors, anatase TiO2 was successfully obtained at hydrothermal temperature as low as 150 ºC. TiO2 was obtained at calcinations temperature as high as 800 ºC, phase transformation from anatase to rutile. Further study for the optimized condition in preparing the TiO2 is currently under the investigation.
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Wang, Chu-Chan, and 王柱讚. "Organic Intermediates Prepared From Derivatives of Acetylacetone in the Presence of Base." Thesis, 2009. http://ndltd.ncl.edu.tw/handle/61829464657470366629.
Full textAbstract:
碩士中原大學
化學研究所
97
Abstract By Michael addition or nuclepohilic substitution, a series of acetylacetone derivatives can be prepared. These compounds, dissolved in sodium hydroxide underwent acyl cleavage. The acyl cleavage of acetylaceton derivatives 3 give 5-ketohexanenitrile , 4-phenylbutan-2-one , 3-benzyl-4-phenylbutan-2-one , hex-5-en-2-one , 3-methylcyclohexen-2-one , 3ethyl-2-cyclohexen-1-one , 1-hydroxybicyclo[3.3.1]nonan-3-one , 7-methyl-4,4a-5,6-tetrahydro-2(3H)naphthalenone , 7-ethyl-1-methyl-4,4a,5,6-tetrahydronaphthalen-2(3H)-one can also be prepaered by this method. 7-methyl-4,4a-5,6-tetrahydro-2(3H)naphthalenone can be used for augmenting or enhancing the aroma or taste of consumable material. This synthesis of 7-methyl-4,4a-5,6-tetrahydro-2(3H)naphthalenone method takes fewer steps and give good yield compand to reations method.
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Mpana, Nakedi Reneilwe. "The extraction of aluminium from fly ash using acetylacetone in gaseous phase." Thesis, 2012. http://hdl.handle.net/10539/11700.
Full textAbstract:
Fly ash is a coal waste produced as a result of coal combustion in coal fired power plants and
it is considered as a potential source of aluminium because it contains 14.8-31 wt%
aluminium(III) oxide in amorphous and mullite phases depending on the coal type. Mullite is
a crystalline structure formed by aluminium(III) oxide and silicate. The extraction of
aluminium from a mixture of 31 wt% aluminium(III) oxide and silica as well as from fly ash
collected from Eskom, Kendal Power Station using acetylacetone has been studied. A
mixture of 31 wt% aluminium(III) oxide and silica was prepared based on the aluminium(III)
oxide weight percentage in the fly ash. The extraction temperature, reaction time,
acetylacetone flow rate, fly ash particle size distribution and bed weight were varied. The
extraction was shown to be dependent on the reaction time, temperature, bed weight and
acetylacetone flow rate. The extraction increased with increasing temperature from 90 0C to
250 0C, 250 0C was chosen as maximum temperature to avoid the decomposition of
aluminium(III) acetylacetonate. The extraction increased with increasing acetylacetone flow
rate from 2 to 6 mL/min and stabilized at 6 mL/min and the extraction percentage increased
with decreasing bed weight. A maximum of 64% of available aluminium was extracted from
a 31 wt% aluminium(III) oxide and silica mixture after 600 minutes at 250 0C using 6
mL/min acetylacetone flow rate. The extraction from the fly ash stabilized at about 18% after
360 minutes at 250 0C, 6 mL/min acetylacetone flow rate. The result showed that extraction
is dependent on the mineralogy of the feed material. The result also showed that the particle
size distribution and the introduction of nitrogen, a carrier gas, have no significant influence
on the extraction of aluminium from the fly ash. A kinetic model was developed and used to
model the extraction results. The model fits the data obtained from the extraction of
aluminium from a 31wt% aluminium(III) oxide and silica mixture at 250 0C and 6 mL/min
acetylacetone flow rate well. When used to model extraction data of a fly ash sample at
similar reaction conditions, the model fits the experimental results only up to 240 minutes
extraction time. The activation energy of the reaction was found to be 11.5 kJ/mol. There is
need however to develop a model which takes into account the influence of temperature and
acetylacetone flow rate.
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Chen, I.-Hsieh, and 謝逸傑. "Preparation and study of tetra-acetylacetonate titanium of a precursor for Titanium Dioxide by Hydrothermal Method." Thesis, 2006. http://ndltd.ncl.edu.tw/handle/4474gq.
Full textAbstract:
碩士國立臺北科技大學
有機高分子研究所
94
Titanium dioxide (TiO2) is one of the most important semiconductors for photocatalytic application due to its strong oxidizing power of its holes, high photostability and redox selectivity. The photocatalytic activity of TiO2 shows strong correlation with its particle size and crystal property. The investigation of various preparation-conditions effecting on the TiO2 synthesis as well as the crystal phase evolution and surface area of the TiO2 products thus becomes very important. The most commonly used precursors for TiO2 synthesis is the titanium alkoxides or titanium metal salt which are hydrolyzed followed by thermal treatment to obtain TiO2 crystal. In this work, we applied chelated type of precursors: Tetra-acetylacetonate titanium,(Ti-tetreaACAC). We just prove that we can successfully synthesize TiO2 nanoparticle using the Ti-chelating precursors and study some of the correlation between the as-prepared TiO2 with the synthesis condition, mainly in the temperature effect. The same way to prepared Titanium butyl phosphate that compared with Tetra-acetylacetonate titanium. The crystal structure of the product was examined by X-ray diffraction (XRD) and the particle dimension and morphology were examined by transmission electron microscopy (TEM). For 4AcAc-Ti, the preliminary results show that the anatase TiO2 was successfully obtained at hydrothermal temperature as low as 150 ºC but the best one is use chelate 4AcAc-Ti. The anatase TiO2 particles was irregular but near oval in shape with average size of 13 nm and well dispersed as observed by TEM. Upon calcination, a phase transformation from anatase to rutile and brookite was aroused at temperatures above 600 ºC. The TiO2 particles became aggregated with undefined shape after high temperature calcination. Compare result was obtained for BAP but with less intensity of XRD peaks indicating the incomplete crystallization of TiO2. Further study for the optimized condition in preparing the TiO2 is currently under the investigation.
40
Nerbel, Jörg [Verfasser]. "Darstellung, Charakterisierung und Umsetzung von Alkoxiden und Acetylacetonaten des Aluminiums / vorgelegt von Jörg Nerbel." 2001. http://d-nb.info/967485274/34.
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Liu, Shuo-Chih, and 劉碩祈. "Determination of Beryllium in Olive Leaves by GFAAS using Acetylacetone as a Chelating Agent." Thesis, 2007. http://ndltd.ncl.edu.tw/handle/43751980306168952673.
Full textAbstract:
碩士東海大學
環境科學與工程學系
95
The levels of beryllium (Be) in olive leaves may be very low and have not been reported neither in certified reference materials (e.g. BCR CRM No.62) nor in the literature until present. The purpose of this study is trying to develop a method for the determination of Be in olive leaves using microwave digestion, chelating with acetylacetone(acac) and then measured by GFAAS. In this thesis, an amount (20 mg) of dried olive leaves sample (BCR CRM No. 62) was placed in a 7-mL teflon microvessel. A two-stage microwave digestion procedure using conc. HNO3 and H2O2 , respectively, was employed in order to completely decompose the sample matrix and allow the Be2+ dissolved in the acidic solution. The pH of the digested mixture was adjusted to 5.0 - 6.0 by NH3(aq). After adding ammonium acetate buffer and acac to the solution, the mixture was allowed to react at room temperature for about 1 h to form a chelate of Be(acac)2. The chelate was preconcentrated on two home-made Oasis cartridges in series, and each cartridge was eluted with methanol and adjusted to 1.00 mL. A portion (20 µL ) was introduced into a graphite cuvette and then measured by GFAAS. The content of Be in 20 mg olive leaves was found as 0.23 ng by using the standard addition method. Good recoveries(100 – 103 %)were obtained with a relative standard deviation (RSD,n=3) < 4.0%. The method detection limit (MDL,3σ) for Be was found to be 0.013 ng [or 0.65(ng/g)]; the calibration graph was linear up to 0.53 ng [or 26.5 (ng/g)].
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WANG, PEI-LIAN, and 王佩蓮. "NMR relaxation analysis on the formation of outer-sphere-complexes between chloroform and tris (acetylacetonato) chromium (III) in solutions." Thesis, 1988. http://ndltd.ncl.edu.tw/handle/15625471373911055551.
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Peng, Hui-Mei, and 彭惠美. "Preparation and Characterization of Ethoxy Iso-Propoxy Titanium Acetylacetonate Catalyst of a precursor for Titanium Dioxide by Hydrothermal Method." Thesis, 2006. http://ndltd.ncl.edu.tw/handle/2emc65.
Full textAbstract:
碩士國立臺北科技大學
有機高分子研究所
94
Titanium dioxide is one of the most potential materials for semi-light fibre, polyene and engineering plastic , etc. application. Every year continue being up to 5~10% of the rate of increase. In addition, the photocatalytic application of the fibre. The photocatalytic application of TiO2 shows strong correlation with its particle size and crystal property. Therefore, the investigation of preparation on the TiO2 synthesis as well as the crystal phase evolution of the TiO2 product becomes very important. In general, TiO2 synthesis used precursors for the titanium alkoxide or titanium metal salt which are hydrolyzed and thermal treatment to obtain TiO2 crystals. Some report indicated that adding catalytic agent can control the particle size, homogeneity and crystallize for TiO2. To study, we applied new type of a precursor : ethoxy iso-propoxy titanium acetylacetonate, as initial compound for TiO2 synthesis that used hydrothermal method and high temperature calcination. prepared for TiO2 crystals . The crystal structure of the product was by X-ray diffraction(XRD) and the particle dimension. For ethoxy iso-propoxy titanium acetylacetonate, the preliminary results show that the anatase TiO2 was successfully obtained at hydrothermal temperature as low as 150 ºC. TiO2 was obtained at hydrothermal temperature as high as 700 ºC of anatase phase change from rutile phase. The TiO2 particles became aggregated by transmission electron microscopy (TEM). Further study for the optimized condition in preparing the TiO2 is currently under the investigation. In the photocatalytic experimental,the degradation of methylene blue was selected as a test-reaction to confer the photocatalytic activity.
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Lin, Jing-Kuen, and 林靖焜. "Determination of Beryllium in Coal by Graphite-Furnace Atomic Absorption Spectrophotometry Using Acetylacetone(acac) as a Chelating Agent." Thesis, 2003. http://ndltd.ncl.edu.tw/handle/85621680535754572031.
Full textAbstract:
碩士東海大學
環境科學系
91
In this thesis, 10 mg of coal sample was weighed accurately and placed in each of four 7-mL teflon vessels. Appropriate amounts of Be(II) (prepared in methanol) were added to the vessels by the standard addition method. On the next day, conc. HNO3 (500 L) and H2O2 (50 L) were added to each vessel. The mixture was microwave digested at 80℃ for 10 min. After digestion, the pH of the acidic coal mixture was adjusted to 5.0-6.0 by NH3(aq) (1.0 M) and then filtered to remove the coal residue. Appropriate amounts of ammonium acetate buffer (25 mmol, pH=6.0) and acetylacetone (acac, 50 L) were added to the filtrate to form a Be(acac)2 chelate. After preconcentration on a home-made C18 cartridge, the Be(acac)2 chelate was eluted with methanol (2.00 mL). A portion (20 L) was introduced into a graphite cuvette and the content of Be was measured by GFAAS. The observed values [0.987±0.029 (g/g), n=6] of Be in a coal certified reference material (SRM 1632c) were in agreement with the certified value [1.0 (g/g)].The method detection limits（3 σ） were in the range 0.29-0.74 ng [or 29-74 (ng/g)] of Be by testing five coal samples. The calibration graph was linear up to 25.0 ng [or 2.5 (g/g)] of Be by using the proposed method. Concentrations of Be in another coal reference material (SRM 1635, but uncertified for Be) and three real samples (No.1, No.2, and No.3) were measured as 0.540±0.003 (g/g), 0.097±0.003 (g/g), 1.099±0.030 (g/g), and 0.722±0.019 (g/g), respectively. Recoveries of 95.5-103.9% were obtained by spiking Be(II) (about 0.5 to 2.5 times) to each coal sample with %RSD≦5.5% (n=5).
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Rajendra, Kumar G. "Triarylborane Functionalized Dicyanovinyl and Acetylacetone Based Molecular Platforms : Building Blocks for Multiple Anion Sensors and Efficient Phosphorescence Emitters." Thesis, 2016. http://hdl.handle.net/2005/3149.
Full textAbstract:
Triarylborane Functionalized Dicyanovinyl and Acetylacetone Based Molecular Platforms:
Building Blocks for Multiple Anion Sensors and Efficient Phosphorescence Emitters
The main objective of this thesis is to design a simple strategy for triarylborane based multiple anion sensors and development of triarylborane incorporated phosphorescent metal complexes. The thesis consists of eight chapters and the contents of each chapter are given below.
Chapter 1
This chapter gives a general introduction to recent advances relevant to the theme of the thesis. A review of the fundamental characteristics of triarylboranes and their applications in various fields such as chemical sensors and optoelectronics is presented. Advances in boron chemistry in the areas such as anion sensors, solid state emissive and phosphorescence materials are discussed in detail. The scope of the thesis is outlined at the end of the chapter.
Chapter 2
The second chapter deals with the general experimental techniques and synthetic procedures followed in this thesis.
Chapter 3
This chapter deals with a rational design strategy for differential identification of fluoride and cyanide ions using TAB based sensors. In general, most of the triarylboranes give similar optical responses towards fluoride and cyanide ions as they follow similar sensing mechanism. In order to circumvent this problem, two TAB-DCV conjugates (1 and 2) are designed and synthesised. The DCV unit is highly specific for cyanide ion owing to the presence of electrophilic carbon center. Probes 1 and 2 differ in steric crowding around the boron center. The less crowded boron center in 1 binds with fluoride as well as with cyanide ions giving similar optical response (luminescence is quenched in presence of F¯
and CN¯). In the case of 2, selectivity of boron center towards fluoride is tuned by increasing the steric crowding around the boron unit.
The dicyanovinyl unit acts as selective sensing site for cyanide ions. As a result,
2 gives different fluorogenic response towards the anions F¯ and CN¯ which were considered as interfering anions in TAB based sensor chemistry. Thus, a modular design principle is developed for differential identification of fluoride and cyanide ions using TAB.
Chapter 4
In this chapter, detailed photophysical studies of TAB-amine-DCV conjugates and colorimetric discrimination of fluoride and cyanide ions are discussed. Presence of amine based donor between the two electron deficient sites enhances the electronic conjugation in 3−5. Since there are two different acceptor sites with a common donor, two distinct charge transfer
transition bands are observed in the visible region of electromagnetic spectrum. The absorption and emission spectra of these compounds show pronounced sensitivity to solvent polarity, signifying large excited state dipolmonents. Anion binding studies confirms that these compounds are highly selective towards fluoride and cyanide ions. Fluoride ions selectively interact with boron center and block the corresponding charge transfer transition thereby leading to a distinct colour change which is observable by naked eye. On the other hand, cyanide interacts with boron as well as DCV unit and blocks both the charge transfer transitions which results in disappearance of colour. Hence, compounds 4 and 5 exhibit different colorimetric signals for fluoride and cyanide ions. Since the absorption bands of 3 do not fall in the visible region, it does not show any colorimetric response towards the aforementioned anions. The anion sensing mechanisms are established by 1H, and 19F NMR studies.
Chapter 5
This chapter presents a systematic study of the effect of length of π-electronic conjugation on the optical properties and anion sensing abilities of a series of TAB-oligothiophene-DCV conjugates (6−8). Their absorption as well as emission bands undergo redshift upon increasing the number of thiophene units between TAB and DCV units as the π-electronic
conjugation in 6−8 is greatly dependent on the number of thiophene units. Their fluorescence emission is highly sensitive to solvent polarity. In the case of 6, the emission band undergoes a redshift with reduced intensity. In the case of 7 the emission band undergoes a redshift but the intensity is not affected by solvent polarity. In the case of 8, the emission band undergoes redshift with enhanced intensity in polar solvents. Interestingly, 7 and
8 show solvent viscosity dependent fluorescence. Structural reorganisation is restricted in viscous medium and results in enhanced emission for 7 and 8. Further, these compounds exhibit selective response towards the fluoride and cyanide ions with different colorimetric responses. Test strips made up of probes 7 and 8 have potential application in identifying fluoride and cyanide ions in aqueous medium.
Chapter 6
This chapter describes synthesis and optical characterisation of triarylborane incorporated
acetylacetone (acacH) ligands (9, 10) and their borondifluoride complexes (11, 12). AcacH ligands and BF2 complexes show solvent dependent emission phenomena due to the involvement of charge transfer transition. Their optical properties are highly dependent on molecular conformations. Complex with duryl spacer
(12) exhibits more red shifted emission in polar solvents due to the enhanced charge transfer transition facilitated by twisted rigid geometry. In presence of fluoride and cyanide ions, the borondifluoride complexes are not stable. The anions concomitantly interact with tricoordinate boron as well as acac-BF2 unit to give rise to complex
pattern of photoluminescence spectral changes during the titration experiment. The binding pathway and the possible species involved are established with the help of 1H, 19F and 11B NMR spectral studies in presence of the anions. Complexes 11 and 12 act as selective chemodosimetric sensors for fluoride and cyanide ions.
Chapter 7
In this chapter, the synthesis and optical
characterisations of triarylborane
conjugated cyclometalated platinum complexes are discussed. A series of square planar platinum complexes are synthesised with different cyclometalating ligands. Complexes (13−18) exhibit a range of luminescence from green to red in solution as well as in the solid state. Their emission intensities are highly sensitive towards atmospheric oxygen suggesting that they originate from a triplet excited state. A maximum of 85% quantum yield is observed for complex 15 in solution state while complex 14 showed a maximum of 58% quantum yield in solid state. Complexes with rigid molecular conformation (14, 16 and 18) showed higher luminescence quantum yield than those having phenyl spacer (13, 15 and 17). The sterically encumbered boryl (-BMes2) group significantly reduces π-π stacking between the square planar entities. Thus, complexes 13−18 show bright luminescence in solid state compared to model complexes without boryl group. The effect of Lewis acidic boron center on luminescence behaviour is explored by fluoride binding studies.
Chapter 8
This chapter is divided into two parts. Part-I describes the synthesis and optical characterisation of triarylborane conjugated cyclometalated iridium complexes (19−24). They are brightly luminescent in solution state with high sensitivity towards atmospheric oxygen. Complex 20 shows a highest quantum yield of 91%. Interestingly, under ambient atmospheric conditions, they exhibit a rare type of dual emission. Life time data suggest that the lower energy emission band originates from cyclometalated iridium based triplet excited state while higher energy emission band originates from boryl ased singlet excited state. Fluoride binding at the boron site results in luminescence quenching; evidently, tri-coordinate boron has a major contribution to the luminescence features of these iridium complexes. Part-II deals with synthesis of triarylborane conjugated pyrazole ligand (25) and its binuclear iridium complexes (26−28) in which two iridium centers are bridged by hydroxo as well as pyrazolato ligands. These binuclear iridium complexes exhibit higher luminescence quantum yield than TAB-acac-Iridium complexes (mononuclear complexes; part I). Binding of fluoride ions at the boron center has a minor impact on their luminescence nature. High sensitivity of their luminescence towards atmospheric oxygen indicates the involvement of triplet excited state in their emission process.
46
weng, chung-heh, and 翁崇賀. "A study on the Determination of Beryllium in Rice by Graphite-Furnace Atomic Absorption Spectrophotometry using Acetylacetone(acac) as a Chelating Agent." Thesis, 2006. http://ndltd.ncl.edu.tw/handle/34544296306346782584.
Full textAbstract:
碩士東海大學
環境科學與工程學系
94
Abstract In this thesis, an amount (10 mg) of dried rice sample (GBW 08508) was placed in a 7-mL teflon microvessel. Two-stage microwave digestion procedure using conc. HNO3 (500 µL) and H2O2 (75 µL), respectively, was employed at 85℃ for 7 min, in order to completely decompose the sample matrix and allow the Be2+ dissolved in the acidic solution. The pH of the digested mixture was adjusted to 5.0 - 6.0 by NH3(aq). After adding ammonium acetate buffer (7.5 mmol, pH＝6) and acetylacetone (50 µL) to the solution, the mixture was allowed to react at room temperature for about 1 h to form a chelate of Be(acac)2. The chelate was preconcentrated on two home-made Oasis cartridges in series, and each cartridge was eluted with methanol and adjusted to 1.00 mL. A portion (20 µL ) was introduced into a graphite cuvette and then measured by GFAAS. Since no certified reference materials (CRM) for Be in rice are available at present, the content of Be in 10 mg rice was found as 0.24 ng by using the standard addition method. Good recoveries (99 – 102％) were obtained with a relative standard deviation (RSD, n＝3)≦6.0％. The method detection limit (MDL, 3σ) for Be was found to be 0.014 ng [or 1.4 (ng/g)]；the calibration graph was linear up to 1.44 ng [or 144 (ng/g)].
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Liu, Pei-Yi, and 劉佩宜. "Measurement of Trace Amounts of Beryllium in Livers of Poultry and Live-stock by Graphite-Furnace Atomic Absorption Spectrophotometry Using Acetylacetone as a Chelating Agent." Thesis, 2009. http://ndltd.ncl.edu.tw/handle/33910308397460625186.
Full textAbstract:
碩士東海大學
環境科學與工程學系
97
Abstract The amounts of beryllium in livers of poultry and live-stock maybe very small. The objective of this thesis is to develop a method for the determination of trace amounts of beryllium in livers of poultry and live-stock using microwave digestion, chelating with acetylacetone (acac) and then measured by graphite-furnace atomic absorption spectrophotometry (GFAAS). An amount (20 mg) of dried liver sample (including BCR CRM - 185R bovine liver with an uncertified value for Be, and three samples collected in Kaohsiung, Taiwan, R. O. C.) was placed in a 7-mL teflon vessel. Conc. HNO3 and H2O2 were added to each sample and the mixture was microwave digested at 85 ℃ for 10 min. The pH of the digested solution was adjusted to 5.0 - 6.0 by NH3 (aq). Appropriate amounts of NH4OAc buffer and acac were added to the solution to form a chelate of Be(acac)2. The chelate was pre-concentrated on two home-made Oasis cartridges in series. Each cartridge was prewashed with 2.0 mL of water (discarded), eluted with methanol, and adjusted to 1.00 mL. A portion (20 μL) was introduced into a graphite tube and the amount of Be was measured by GFAAS. The Be contents measured in four liver samples (BCR - 185R bovine liver, and three samples collected in Kaohsiung, Taiwan, R. O. C.) were between 2.3 and 4.7 ng/g. Good spiked recoveries (97.8 – 100.7%) were obtained for these four samples with a relative standard deviation (RSD, n = 3) ≤ 2.8%. The method detection limit (MDL, 3) for Be was found to be 0.17 ng/g; the calibration graph was linear up to 27 ng/g. The proposed method could be applied to measurements of Be in livers of poultry and live-stock.
48
Ya-Yun, Tsai, and 蔡亞耘. "Measurement of Trace Amounts of Beryllium in Muscles of Poultry and Live-stock by Graphite-Furnace Atomic Absorption Spectrophotometry using Acetylacetone (acac) as a Chelating Agent." Thesis, 2009. http://ndltd.ncl.edu.tw/handle/89057772945903319395.
Full textAbstract:
碩士東海大學
環境科學與工程學系
97
The levels of beryllium ( Be ) in muscles of poultry and live-stock maybe very low and have not been reported in muscles of poultry and live-stock certified reference materials ( e.g. BCR CRM-384 ). The purpose of this thesis is to develop a method for the determination of Be in muscles of poultry and live-stock using microwave digestion, chelating with acetylacetone（acac）, pre-concentrating by solid-phase extraction, eluting with methanol and then measured by GFAAS. Trace amounts of Be (0.004 - 0.56 ng) in a dried pork muscle sample (20 mg) could be accurately determined by graphite-furnace atomic absorption spectrophtometry (GFAAS) after treating with microwave digestion (HNO3/H2O2) at 85C for 10 min and using acetylacetone as a chelating agent in the presence of an acetate buffer (pH 6.0). The method detection limit (MDL, 3) for Be was found to be 0.19 ng/g; the calibration graph was linear up to 28 ng/g. The Be contents measured in four muscle samples (BCR CRM - 384 pork muscle, and three samples collected in Kaohsiung, Taiwan, R. O. C.) were between 2.5 and 3.0 ng/g. Good spiked recoveries (95.7 – 103.2%) were obtained for these four samples with a relative standard deviation (RSD, n = 3) ≤ 2.1%. The proposed method could be applied to measurements of Be in muscles of poultry and live-stock.
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Mateshov, Dauren. "Experimental Study of In Situ Combustion with Decalin and Metallic Catalyst." 2010. http://hdl.handle.net/1969.1/ETD-TAMU-2010-12-8722.
Full textAbstract:
Using a hydrogen donor and a catalyst for upgrading and increasing oil recovery during in situ combustion is a known and proven technique. Based on research conducted on this process, it is clear that widespread practice in industry is the usage of tetralin as a hydrogen donor. The objective of the study is to find a cheaper hydrogen donor with better or the same upgrading performance. Decalin (C10H18) is used in this research as a hydrogen donor. The experiments have been carried out using field oil and water saturations, field porosity and crushed core for porous medium.
Four in situ combustion runs were performed with Gulf of Mexico heavy oil, and three of them were successful. The first run was a control run without any additives to create a base for comparison. The next two runs were made with premixed decalin (5 percent by oil weight) and organometallic catalyst (750 ppm). The following conditions were kept constant during all experimental runs: air injection rate at 3.1 L/min and combustion tube outlet pressure at 300 psig. Analysis of the performance of decalin as a hydrogen donor in in-situ combustion included comparison of results with an experiment where tetralin was used. Data from experiments of Palmer (Palmer-Ikuku, 2009) was used for this purpose, where the same oil, catalyst and conditions were used.
Results of experiments using decalin showed better quality of produced oil, higher recovery factor, faster combustion front movement and higher temperatures of oxidation. API gravity of oil in a run with decalin is higher by 4 points compared to a base run and increased 5 points compared to original oil. Oil production increased by 7 percent of OOIP in comparison with base run and was 2 percent higher than the experiment with tetralin. The time required for the combustion front to reach bottom flange decreased 1.6 times compared to the base run. The experiments showed that decalin and organometallic catalysts perform successfully in in situ combustion, and decalin is a worthy replacement for tetralin.
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Степанова, В. В., and V. V. Stepanova. "Бесферментный электрохимический сенсор на основе органического комплекса никеля (II), полиэтиленимина и углеродных нанотрубок для определения глюкозы : магистерская диссертация." Master's thesis, 2019. http://hdl.handle.net/10995/78546.
Full textAbstract:
Объектом исследования являлась глюкоза. Актуальность работы заключается в практическом применении бесферментных электрохимических сенсоров для контроля уровня глюкозы в крови при сахарном диабете. Цель работы: разработка бесферментного электрохимического сенсора для определения глюкозы с использованием органических комплексов никеля (II), в качестве чувствительных элементов, и самоорганизующихся слоев полимера с молекулярными отпечатками на основе полиэтиленимина, в качестве селективного элемента. Комплекс ацетилацетонат никеля (II) проявляет электрокаталитические свойства. С помощью полученного сенсора были проведены измерения глюкозы в модельных растворах, имитирующих сыворотку крови. Было выявлено отсутствие влияния посторонних соединений. Полученные ПМО обладают селективностью. Страниц 59, рисунков 47, таблиц 3, библиографических наименований 61.The object of the study was glucose. The relevance of the work lies in the practical application of enzyme-free electrochemical sensors to control blood glucose levels in diabetes mellitus. Objective: to develop an enzyme-free electrochemical sensor for glucose determination using organic nickel (II) complexes, as sensitive elements, and self-assembled polymer layers with molecular prints based on polyethyleneimine, as a selective element. The nickel (II) acetylacetonate complex exhibits electrocatalytic properties. Using the obtained sensor, glucose was measured in model solutions simulating blood serum. It was revealed the absence of the influence of extraneous compounds. The resulting MIPs have selectivity.