Inorganic Chemistry Commons^™

Novel Microwave Assisted Synthesis Of Zns Nanomaterials, Suresh Pillai, Michael Seery, Damian Synnott, John Colreavy, Stephen Hinder

Articles

A novel ambient pressure microwave-assisted technique is developed in which silver and indium modified ZnS is synthesised. The as prepared ZnS is characterised by X-ray diffraction, UV-Vis spectroscopy, X-ray photoelectron spectroscopy and luminescence spectroscopy. This procedure produced crystalline materials with particle sizes below 10 nm. The synthesis technique leads to defects in the crystal which induce mid energy levels in the band gap and lead to indoor light photocatalytic activity. Increasing the amount of silver causes a phase transition from cubic blende to hexagonal phase ZnS. In a comparative study, when the ZnS cubic blende is heated in a conventional …

A Highly Efficient Tio2-Xcx Nano-Heterojunction Photocatalyst For Visible-Light Induced Antibacterial Applications, Vinodkumar Etacheri, Michael Seery, Stephen Hinder, Georg Michlits, Suresh Pillai

Articles

Visible-light-induced antibacterial activity of carbon-doped anatase-brookite titania nano-heterojunction photocatalysts are reported for the first time. These heterostructures were prepared using a novel low temperature (100 °C) non-hydrothermal low power microwave (300 W) assisted method. Formation of interband C 2p states was found to be responsible for the band gap narrowing of the carbon doped heterojunctions. The most active photocatalyst obtained after 60 minutes of microwave irradiation exhibits a 2-fold higher visible-light induced photocatalytic activity in contrast to the standard commercial photocatalyst Evonik-Degussa P-25. Staphylococcus aureus inactivation rate constant for carbon-doped nano-heterojunctions and the standard photocatalyst was 0.0023 and -0.0081 min …

Preparation Of Phosphonoterephthalic Acids Via Palladium-Catalyzed Coupling Of Aromatic Iodoesters, Nathaniel Ivan, Vladimir Benin, Alexander Morgan

Chemistry Faculty Publications

The current article reports in detail the preparation of two phosphonoterephthalic acids: 2-phosphonoterephthalic acid (1) and 2,5-diphosphonoterephthalic acid (2). Efficient, scalable syntheses have been developed for both compounds based on Pd-catalyzed coupling reactions of iodinated terephthalate esters. Phosphonoterephthalic acids are potentially useful as flame-retardant additives or as monomers for the construction of acid-pendant polymer chains.

Reaction Between Polyol-Esters And Phosphate Esters In The Presence Of Metal Carbides, David W. Johnson, Carolyn Iacullo, John E. Hils

Chemistry Faculty Publications

The reaction of metal carbides with polyol esters found in aerospace lubricants and phosphate esters commonly used as additives was investigated. Carbides were of particular interest since modern materials under consideration at high temperature bearings have surfaces that are primarily metal carbides. Vanadium and chromium carbide were found to react with the ester and phosphate ester by a transesterification reaction, producing an alkyl phosphate which is less stable than the aromatic phosphate esters. In the process, the metal carbide is converted to the metal phosphate and metal polyphosphate, evidenced by the infrared and Raman spectra of the solid residue and …

Preparation, Characterization And Applications Of Functionalized Carbon Nano-Onions, Mahendra K. Sreeramoju

Theses and Dissertations--Chemistry

Carbon nano-onions (CNOs) discovered by Ugarte in 1992 are multi-layered fullerenes that are spherical analogs of multi-walled carbon nanotubes with diameters varying from 6 nm to 30 nm. Among the various methods of synthesis, CNOs prepared by graphitization of nanodiamonds (N-CNOs) and underwater electric arc of graphite rods (A-CNOs) are the subject of our research. N-CNOs are considered as more reactive than A-CNOs due to their smaller size, high curvature and surface defects.

This dissertation focuses on structural analysis and surface functionalization of N- CNOs with diameters ranging from 6—10 nm. Synthetic approaches such as oleum- assisted oxidation, Freidel-Crafts acylation …

Physicochemical Modifications And Applications Of Carbon Nano-Onions For Electrochemical Energy Storage, Rituraj Borgohain

Theses and Dissertations--Chemistry

Carbon nano-onions (CNOs), concentrically multilayered fullerenes, are prepared by several different methods. We are studying the properties of two specific CNOs: A-CNOs and N-CNOs. A-CNOs are synthesized by underwater arc discharge, and N-CNOs are synthesized by high-temperature graphitization of commercial nanodiamond. In this study the synthesis of A-CNOs are optimized by designing an arc discharge aparatus to control the arc plasma. Moreover other synthesis parameters such as arc power, duty cycles, temperature, graphitic and metal impurities are controlled for optimum production of A-CNOs. Also, a very efficient purification method is developed to screen out A-CNOs from carboneseous and metal impurities. …

Synthesis Of Palladium-Based Electrocatalysis—From Pure Metal To Bimetallic Nanoparticles, Haijun Gao

Masters Theses

This thesis focuses on synthesis and characterization of palladium-based nanoparticles. Background information of the research in this thesis is provided in Chapter 1. Preparation and characterization of pure palladium nanoparticles are presented in Chapter 2. A fast and convenient method to prepare ultra small Pd nanoparticles via Pluronic P123 reduction is discussed in detail. Impregnation method and poly method are also studied in this chapter. Chapter 3 reports the studies of these methods to prepare ultra small bimetallic (bimetallic means a mixture of two metals) palladium-based nanoparticles. Oleylamine-mediated method used Pd nanoparticles prepared via P123 reduction as precursor. Ultra small …

Studies On Molecular Sieve Crystallization And Heteroatomic Substitution, Adam R. Macintosh

Electronic Thesis and Dissertation Repository

Molecular sieves have been scientifically and industrially important materials since their inception. These porous, crystalline networks of tetrahedrally coordinated atoms bridged by oxygen are known for their extremely high surface area and low density, making them excellent systems for catalysis. The framework of the AlPO₄ family of molecular sieves is itself non-catalytic, but through heteroatomic substitution these materials can diversify into the catalytically active silicoaluminophosphate (SAPO) and metalloaluminophosphate (MAPO) families of heterogeneous acid and redox catalysts. Research into the methods by which these substitutions occur, and the effects therein on the crystallization of the sieves, is of great importance, …

Ionothermal Synthesis Of High Silica Zeolites In Deep Eutectic Solvents (Des), Zheng Sonia Lin

Electronic Thesis and Dissertation Repository

Phase-pure high silica zeolites have been synthesized using different deep eutectic solvents for the first time. ZSM-5 was made in tetrapropylammonium bromide/pentaerythritol. The reaction is affected by the amounts of seeding, water content, and organic structure-directing agent (SDA). Sodalite and ZSM-39 were prepared in tetramethylammonium chloride (TMACl)/1, 6-hexanediol by using the mineralizing agents NaOH and NH₄F, respectively. In urea/choline chloride, ZSM-5, Beta, ZSM-39, and ZSM-11 were made by using different organic SDAs in the presence of fluoride. The reaction temperature and the choice of organic SDA affect the type of structures being produced.

The crystallization of ZSM-39 in …

Surface Functionalized Water-Dispersible Magnetite Nanoparticles: Preparation, Characterization And The Studies Of Their Bioapplications, Haiou Qu

University of New Orleans Theses and Dissertations

Iron oxide magnetic nanoparticle synthesis and their surface functionalization hold a crucial position in the design and fabrication of functional materials for a variety of biomedical applications. Non-uniform nanoparticles with poor crystallinity, prepared by conventional methods, have only limited value in biological areas. Large scale synthesis methods that are able to produce high quality, mono-dispersed iron oxide nanoparticles using low cost and environment friendly chemicals are highly desirable. Following synthesis, appropriate surface functionalization is necessary to direct the dispersibility of nanoparticles in aqueous solution in order to provide them with acceptable colloidal stability against the ion strength and many biomolecules …

The Synthesis And Characterization Of Novel Group 13 Nanostructured Building Block Heterogeneous Silicate Catalysts, Joshua G. Abbott

Doctoral Dissertations

A building block approach and sequential addition methodology were utilized to prepare heterogeneous silicate catalysts containing atomically dispersed group 13 metal (B, Al, Ga) centers. The octa(trimethyltin) silsequioxane, Si8[sub]O12[sub](OSnMe3[sub])8[sub], was used as the building block for the synthesis of these materials. Reaction of the building block with a variety of group 13 metal chlorides led to the formation of cross-linked matrices. All prepared materials were characterized by gravimetric analysis, gas absorption, IR, and NMR. In addition, aluminum and boron samples where characterized by 27[sup]Al and 11[sup]B solid state NMR, and gallium samples were studied using x-ray absorption techniques.

Studies found …

Reactions Of Methyl Perfluoroalkyl Ethers With Isopropyl Alcohol: Experimental And Theoretical Studies, Howard Knachel, Vladimir Benin, Chadwick Barklay, Janine C. Birkbeck, Billy D. Faubion, William E. Moddeman

Chemistry Faculty Publications

The reaction of an isomeric mixture of the methyl perfluoroalkyl ether, C4F9OCH3 (Novec-7100), in the presence of isopropyl alcohol (IPA) and/or water has been studied by measuring the rate of product formation using an ion-selective electrode (ISE) for fluoride ion, Karl Fisher coulometric titrations for water, and 1H and 19F NMR spectroscopy for product identification and rate studies. The results showed the methyl perfluoroalkyl ether to be very stable with products forming at the rate of ∼1 ppm per year at a laboratory temperature of 20 °C. Measurements over the temperature range of 6° to 100 °C were made on …

Investigating The Electron Transport And Light Scattering Enhancement In Radial Core-Shell Metal-Metal Oxide Novel 3d Nanoarchitectures For Dye Sensitized Solar Cells, Gayatri Sahu

University of New Orleans Theses and Dissertations

Dye-sensitized solar cells (DSSCs) have attained considerable attention during the last decade because of the potential of becoming a low cost alternative to silicon based solar cells. Electron transport is one of the prominent processes in the cell and it is further a complex process because the transport medium is a mesoporous film. The gaps in the pores are completely filled by an electrolyte with high ionic strength, resulting in electron-ion interactions. Therefore, the electron transport in these so called state-of-the-art systems has a practical limit because of the low electron diffusion coefficient (D_n) in this mesoporous film …

The Synthesis And Characterization Of Novel Titanosilicates For Next Generation Hydrogen Storage, James R. Humble

Chancellor’s Honors Program Projects

No abstract provided.

Solid-State Nuclear Magnetic Resonance Spectroscopy Of Unreceptive Quadrupolar Nuclei In Inorganic Materials, Andre Sutrisno

Electronic Thesis and Dissertation Repository

Preparation and characterization of inorganic materials is a crucial practice because understanding the relationship between structure and property is important for improving current performance and developing novel materials. Many metal centers in technologically and industrially important materials are unreceptive low-γ quadrupolar nuclei (i.e., possessing low natural abundance, low NMR frequencies and large quadrupole moments) and they usually give rise to very broad NMR resonances and low signal-to-noise ratios, making it difficult to acquire their solid-state NMR spectra. This thesis focuses on the characterization of inorganic materials using solid-state NMR (SSNMR) spectroscopy at very high magnetic field of …

Optical And Electrochemical Sensors For The Detection Of Metal Ions And Nerve Gas Mimics Via Fluorescein And Coumarin Derivatives, Fasil Adefris Abebe

Dissertations

Trace element detection of metals, for example, iron, Copper and zinc, are important in biological systems and in the environment. Many of us are aware that our cells contain metal ions that are “tied” up in proteins. However, chelatable or “free” trace elements can also be found in small quantities, and can have a negative impact on our bodies. Despite the increasing surge in developing sensors for metals and nerve gas agents, efficient detection still remains a challenge. Among the various sensors developed so far, fluorescence sensors play an important role due to their simplicity. I design fluorescein-based chemosensors for …

Optical And Electrochemical Properties Of Monolayer Protected Gold Clusters Modified With Fluorophores, Mary Sajini Devadas

Dissertations

My research focused on the synthesis, characterization and the investigation of the optical and electrochemical properties of monolayer-protected quantum-sized gold clusters. Significant research attention was focused on the solution phase optical and electrochemical properties of these clusters. Highly monodisperse Au clusters with different types of ligands were successfully synthesized with sizes varying from 1 nm to 13 nm. These preformed gold clusters were modified with fluorophores and pseudo-rotaxanes for developing better nonlinear optical materials for sensing and biological imaging purposes. We have tried to focus on the interaction of the outer ligand shell, made up of –S-Au-S-Au-S- bonds, with the …

Synthesis And Flame Retardant Testing Of New Boronated And Phosphonated Aromatic Compounds, Vladimir Benin, Sravanthi Durganala, Alexander Morgan

Chemistry Faculty Publications

The present report describes the preparation and use of some dimethyl terephthalate derivatives in transition metal-catalyzed coupling reactions to produce new reactive flame retardants. Dimethyl iodoterephthalate and dimethyl 2,5-diiodoterephthalate were successfully employed in the preparation of phosphonic and boronic esters and acids. The latter were tested for heat release with a microcombustion calorimeter (ASTM D7309) to determine the potential for heat release reduction of these flame retardant molecules. The results showed that the addition of boronic or phosphonic acids greatly lowered the heat release, due to a condensed phase (char formation) mechanism. Adding ester groups to the boronic acids or …

Transition Metal Complexes With Reactive Trimethylsilylchalcogenolate Ligands: Precursors For The Preparation Of Ternary Nanoclusters, Chhatra Bahadur Khadka

Electronic Thesis and Dissertation Repository

The Co²⁺ and Mn²⁺ complexes (N,N´-tmeda)Co(ESiMe₃)₂ (E = S, 1a; E = Se, 1b), (3,5-Me₂C₅H₃N)₂Co(ESiMe₃)₂ (E = S, 2a; E = Se, 2b), [Li(N,N´-tmeda)]₂[(N,N´-tmeda)Mn₅(μ-ESiMe₃)₂(ESiMe₃)₄(μ₄-E)(μ₃-E)₂] (E = S, 3a; E = Se, 3b), [Li(N,N´-tmeda)]₂[Mn(SSiMe₃)₄] (4), [Li(N,N´-tmeda)]4[Mn₄(SeSiMe₃)₄(μ_{3 …}

Synthesis Of An Antimicrobial Textile Coating, William M. Morris

Chemistry and Biochemistry

A titania nanosol was synthesized and coated onto nylon/cotton blended textile substrates. The substrates were characterized via SEM for adhesion and nanoparticle formation, then subjected to antimicrobial efficacy tests. The titania nanosol was successfully coated on to textiles samples. Particles were observed to be around 2 by 3 micrometers and formed between the interstitial space of textile fibers. Although larger than typical nanoparticles, the coatings exhibited what seemed to be antimicrobial activity. Titania nanosol coated textile samples were subjected to Kirby Bauer Assay in the presence of S. aureus. The coated textile sample exhibited an inhibition of growth around its …

The Tetrafluoroborate Salt Of 4-Methoxybenzyl N-2-(Dimethylamino)Ethyl-N-Nitrosocarbamate: Synthesis, Crystal Structure And Dft Calculations, Helene Hedian, Vladimir Benin

Chemistry Faculty Publications

The tetrafluoroborate salt of 4-methoxybenzyl N-2-(dimethylamino)ethyl-N-nitrosocarbamate was prepared in two steps, via the corresponding carbamate. Its crystal structure is monoclinic, space group P21/c. The unit cell dimensions are: a = 19.499(8) Å, b = 5.877(3) Å, c = 15.757(7) Å, α = 90°, β = 110.019(7)°, γ = 90°, V = 1696.5(12) Å3, Z = 4. The structure exhibits an unexpected, pseudo-gauche conformation with respect to the C2–C3 bond, due to a stabilizing hydrogen bond between the carbonyl oxygen (O1) and the hydrogen atom at the trialkylammonium center (H3n), with a distance between them of …

Electrochemistry Of Pani/Metal Composites In Basic Solutions, Tamthinhan Quy

UNLV Theses, Dissertations, Professional Papers, and Capstones

Polyaniline (PANI) has been extensively investigated due to its unique conductivity, which is primarily dependent on the oxidation state of the material and the solution pH. PANI is an insulator when it is oxidized, and the solution pH exceeds four. Numerous attempts to extend PANI's conductivity to neutral and alkaline environments have been unsuccessful. However, our previous study has demonstrated that PANI/Pd composite is conductive and catalytically active in a basic solution, pH ∼ 12. Therefore, the conductivity and the electrochemical properties of PANI composites including PANI/Au, PANI/Pd and PANI/Pt were evaluated in basic solutions. The fundamental studies of PANI/metal …

Vapor Liquid Solid Growths Of Germanium And Gallium Antimonide Nanowires, Ralph Alvarez, Esmeralda Arreola, Michael Oye, Meyya Meyyappan

STAR Program Research Presentations

Determining the optimal growth parameters for germanium (Ge) and gallium antimonide (GaSb) nanowires is the focus of this research. Given the fact that nano materials behave differently from their bulk counterparts we are researching some variables that influence nanowire diameter and length such as temperature, ramp rate, gas flow rate, and catalyst particle size. Based on the nano material size which is typically a few 10s of nanometers wide, these nano materials can be engineered to take advantage of their optical properties. Specifically the infrared (IR) response of Ge and GaSb nanowires are directly controllable based on their geometry. Fine …

Application Of Raman Spectroscopy To Lubricants, Lubricated Surfaces And Lubrication Phenomena, David W. Johnson

Chemistry Faculty Publications

Recent advances in lasers and detector technologies and the development of low-cost instruments and fiber-optic probes have brought about an explosion in the lubrication systems being studied by Raman spectroscopy. This article provides examples of the use of Raman spectroscopy in the study of lubrication phenomena, including the characterization of liquid lubricants, lubricant additives, and solid lubricants; the study of vapor-phase lubrication; and the use of coated nanoparticles as lubricants.

Resorbable Polymer-Hydroxyapatite Composites For Bone Trauma Treatment: Synthesis And Properties, Troy E. Wiegand

Department of Chemistry: Dissertations, Theses, and Student Research

Contemporary therapies for hard tissue replacement involve allographs, where the donor and recipient are of the same species, or the use of xenogenic transplants. Intraspecies materials are often in short supply and interspecies materials are subject to immunological barriers such as disease and tissue rejection. Synthetic composites are unencumbered by these limitations. Poly lactic acid (PLLA) and its copolymers have been used in medicine due to their ability to be resorbed by the body without adverse effects. PLLA’s are currently most commonly used in resorbable sutures and gauzes, but there is increasing interest in using them in conjunction with hydroxyapatite …

A Sodium Salt Of The Dimer Of Boronoterephthalic Acid Anhydride, Scott Simmons, Albert Fratini, Vladimir Benin

Chemistry Faculty Publications

The title compound, sodium bis­(6-carb­oxy-1-hy­droxy-3-oxo-1,3-dihydro-2,1-benzoxaborol-1-yl)oxidanium, Na+·C16H15B2O13-, was prepared in two steps from 2-bromo-p-xylene. Its crystal structure was determined at 140 K and has triclinic (P) symmetry. The compound presents a unique structural motif, including two units of the cyclic anhydride of boronoterephthalic acid, joined by a protonated, and thereby trivalent, oxonium center. Association in the crystal is realized by complementary hydrogen bonding of the carboxyl groups, as well as by coordination of the sodium cations to the oxygen centers on the five-membered rings.

Theoretical Investigation Of A Reported Antibiotic From The 'Miracle Tree' Moringa Oleifera, Michael Horwath, Vladimir Benin

Chemistry Faculty Publications

Moringa oleifera, sometimes called the “Miracle Tree,” has received international attention for its potential to improve health in impoverished tropical areas. In addition to high vitamin content in the leaves and pods, the tree contains compounds with antioxidant and antibacterial properties. This study focused on the theoretical investigation of the suggested structure of one antibacterial compound, “pterygospermin,” whose existence was proposed after some studies of the roots of M. oleifera. The structure of pterygospermin was first proposed by a research group working in the 1950s, but later studies have not found evidence of this compound and have instead …

Low Temperature Growth Of High Purity, Low Resistivity Copper Films By Atomic Layer Deposition, Thomas J. Knisley

Thomas J Knisley

No abstract provided.

Volatility And High Thermal Stability In Mid To Late First Row Transition Metal Diazadienyl Complexes, Thomas J. Knisley

Thomas J Knisley

No abstract provided.

Fabrication And Catalytic Property Of Cerium Oxide Nanomaterials, Keren Jiang

Department of Chemistry: Dissertations, Theses, and Student Research

Cerium oxide, or ceria (CeO_x: x = 1.5 to 2), has been widely used as a heterogeneous catalyst. Ceria has several properties make it high catalytic active: the fluctuating valence of cerium, the high oxygen storage capacity and high oxygen mobility in the nonstoichiometric ceria. With the high abundance of cerium on earth crust, ceria is a highly effective alternative of the noble metal catalysts. Research has been focused on designing nanostructured ceria and ceria related materials in recent years. The catalytic activity of ceria can be enhanced by the nanoscale effect which can be applied for various …