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  Partner: UNT Libraries
 Decade: 2000-2009
 Year: 2004
 Degree Discipline: Chemistry
 Collection: UNT Theses and Dissertations
Baeyer-Villiger Oxidation of 1,7- & 1,9-dibromopentacyclo[5.4.0.02,6.03,10.05,9]undecane-8,11-dione

Baeyer-Villiger Oxidation of 1,7- & 1,9-dibromopentacyclo[5.4.0.02,6.03,10.05,9]undecane-8,11-dione

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Date: May 2004
Creator: Akinola, Adeniyi O.
Description: Baeyer-Villiger oxidation of 1,9-dibromopentacyclo[5.4.0.02,6.03,10.05,9]undecane-8,11-dione (1,9-dibromo-PCU-8,11-dione) was performed by using an excess amount of m-chloroperbenzoic acid (3 equivalents) and resulted in the formation of the corresponding monolactone. The reaction would not proceed to the dilactone stage. The structure of the reaction product was established unequivocally via single crystal X-ray diffraction. Baeyer-Villiger oxidation of 1,9-dibromo-PCU-8,11-dione using ceric ammonium nitrate (CAN) was also performed and afforded a mixture of lactones. Only one of these lactones, which also contained an alkene functionality, could be isolated and characterized. 1,7-dibromo-PCU-8,11-dione was also reacted with CAN, yielding the mono-lactone, which has also been characterized.
Contributing Partner: UNT Libraries
Improvement of Homogeneity and Adhesion of Diamond-Like Carbon Films on Copper Substrates

Improvement of Homogeneity and Adhesion of Diamond-Like Carbon Films on Copper Substrates

Date: August 2004
Creator: Vavilala, Suma
Description: Electrodeposition method is used to deposit diamond-like carbon (DLC) films on copper substrates via anodic oxidation at low temperature. These films are characterized using Raman spectroscopy, Fourier transform infrared spectroscopy and scanning electron microscopy. Homogeneity of these films is studied using Raman spectroscopy and scanning electron microscopy. Scotch tape peel tests indicate adherent film on copper substrate. Carbon phase transformation is studied using thermal annealing experiments in conjunction with Raman spectroscopy and scanning electron microscopy. A cathodic electrochemical method is also studied to deposit diamond-like carbon films on copper substrates. However, films deposited by the cathodic route have poor adhesion and quality compared to anodically deposited films. It is also possible to grow diamond phase on copper substrates using acetylene in liquid ammonia via electrodeposition route. An electrochemical method is proposed for boron doping into DLC films.
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Investigation of Structure and Properties of Low Temperature Deposited Diamond-Like Carbon Films

Investigation of Structure and Properties of Low Temperature Deposited Diamond-Like Carbon Films

Date: August 2004
Creator: Pingsuthiwong, Charoendee
Description: Electrodeposition is a novel method for fabrication of diamond-like carbon (DLC) films on metal substrates. In this work, DLC was electrochemically deposited on different substrates based on an anodic oxidation cyclization of acetylene in liquid ammonia. Successfully anodic deposition was carried out for DLC onto nickel substrate at temperatures below -40°C. Comparative studies were performed on a series of different carbon sources (acetylene, sodium acetylide, and a mixture of acetylene and sodium acetylide). The films were characterized using a variety of methods including Raman spectroscopy, Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), XPS valence band spectra, and/or scanning electron microscopy (SEM). Raman spectroscopy is used as a bench mark technique to verify the presence of deposited DLC films, to access the films homogeneities, and to provide the ratio of the different carbon phases, mainly disordered graphite (D) and graphite (G) phases in the films. A combination of the Raman with FTIR and valence band spectra analysis allowed the distinction between hydrogenated DLC and unhydrogenated DLC films. Three different kinds of DLC [(1) hydrogenated DLC (a-C:H); (2) tetrahedral hydrogenated DLC (ta-C:H); and (3) graphitic-like DLC] were deposited depending upon the deposition conditions and substrates. Temperature and current density are ...
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Preparation and characterization of praseodymium oxide films and powders.

Preparation and characterization of praseodymium oxide films and powders.

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Date: May 2004
Creator: Shang, Yajuan
Description: Nanocrystalline praseodymium oxide films have been successfully generated on stainless steel substrates. The electrochemical deposition was performed in the cathode compartment of a divided electrochemical cell with a regular three-electrode configuration. The green films obtained by electrodeposition were then annealed at high temperatures for 1-3 hours. X-ray diffraction revealed the fluorite structure of Pr6O11 and the crystallite size was calculated. X-ray photoelectron spectroscopy was employed to study the composition of the oxide films and also the oxidation state of Pr. Scanning electron microscopy was utilized to study the surface texture and microstructure of deposits. Fourier transform infrared spectrometery was used to investigate the composition of the films. The effects of different conditions on the green films were also studied such as different pH values of the electrolyte solution, different deposition modes, different supporting electrolytes and different applied current densities. Sintering experiments were conducted to investigate the properties of the green films. Praseodymium oxide powders were also successfully prepared by combining electrochemical methods with sintering processes. The praseodymium oxide powders were characterized by X-ray diffraction and Fourier transform infrared spectroscopy. The crystallite sizes of the powders were evaluated.
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Studies in regiospecific oxidation reactions of 1-methyl-pentacyclo[5.4.0.02,6.03,10.05,9]undecane-8,11-dione.

Studies in regiospecific oxidation reactions of 1-methyl-pentacyclo[5.4.0.02,6.03,10.05,9]undecane-8,11-dione.

Date: May 2004
Creator: Vappala, Indu
Description: Baeyer-Villiger oxidation of 1-methylpentacyclo[5.4.0.02,6.03,10.05,9] undecane-8,11-dione, performed by using m-chloroperbenzoic acid in 1:1 molar ratio, resulted in the formation of monolactone. The corresponding dilactone, was synthesized by reacting 1-methyl-PCU-8,11-dione with m-chloroperbenzoic acid in 1:2 molar ratio. 6-Methyl-1,4,4a,8a-tetrahydro-1,4-methanonaphthalene-5,8-dione was converted into the corresponding exo-6,7-monoepoxide via treatment with 30% aqueous hydrogen peroxide. Epoxidation of this monoepoxide by using m-chloroperbenzoic acid afforded the corresponding bis-epoxide. Ceric ammonium nitrate (CAN) promoted oxidation of 1-methyl-PCU-8,11-dione afforded "methylated lactones" and a "methylated alkene."
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Thermodynamics of Mobile Order Theory: Solubility and Partition Aspects

Thermodynamics of Mobile Order Theory: Solubility and Partition Aspects

Date: August 2004
Creator: De Fina, Karina M.
Description: The purpose of this thesis is to analyze the thermochemical properties of solutes in nonelectrolyte pure solvents and to develop mathematical expressions with the ability to describe and predict solution behavior using mobile order theory. Solubilities of pesticides (monuron, diuron, and hexachlorobenzene), polycyclic aromatic hydrocarbons (biphenyl, acenaphthene, and phenanthrene), and the organometallic ferrocene were studied in a wide array of solvents. Mobile order theory predictive equations were derived and percent average absolute deviations between experimental and calculated mole fraction solubilities for each solute were as follows: monuron in 21 non-alcoholic solvents (48.4%), diuron in 28 non-alcoholic solvents (60.1%), hexachlorobenzene (210%), biphenyl (13.0%), acenaphthene (37.8%), phenanthrene (41.3%), and ferrocene (107.8%). Solute descriptors using the Abraham solvation model were also calculated for monuron and diuron. Coefficients in the general solvation equation were known for all the solvents and solute descriptors calculated using multilinear regression techniques.
Contributing Partner: UNT Libraries