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Preparation And Instability Of Nanocrystalline Cuprous Nitride, Malinda D. Reichert, Miles A. White, Michelle J. Thompson, Gordon J. Miller, Javier Vela 2016 Iowa State University

Preparation And Instability Of Nanocrystalline Cuprous Nitride, Malinda D. Reichert, Miles A. White, Michelle J. Thompson, Gordon J. Miller, Javier Vela

Javier Vela-Becerra

Low-dimensional cuprous nitride (Cu3N) was synthesized by nitridation (ammonolysis) of cuprous oxide (Cu2O) nanocrystals using either ammonia (NH3) or urea (H2NCONH2) as the nitrogen source. The resulting nanocrystalline Cu3N spontaneously decomposes to nanocrystalline CuO in the presence of both water and oxygen from air at room temperature. Ammonia was produced in 60% chemical yield during Cu3N decomposition, as measured using the colorimetric indophenol method. Because Cu3N decomposition requires H2O and produces substoichiometric amounts of NH3>, we conclude that this reaction proceeds through a ...


Selenium-Modified Tio2 And Its Impact On Photocatalysis, Erin M. Rockafellow, Jessica M. Haywood, Travis Witte, Robert S. Houk, William S. Jenks 2016 Iowa State University

Selenium-Modified Tio2 And Its Impact On Photocatalysis, Erin M. Rockafellow, Jessica M. Haywood, Travis Witte, Robert S. Houk, William S. Jenks

Robert S. Houk

This work describes the preparation of a selenium-modified TiO2 photocatalyst and a preliminary evaluation of its photocatalytic activity. Se-TiO2 displayed greater visible absorption than undoped TiO2 and was still capable of degrading quinoline at a slightly faster rate than undoped TiO2 under UV light. Se-TiO2 was also able to degrade organic molecules under purely visible light by a single electron transfer pathway. Irradiation with >435 nm light showed no evidence of efficient production of HO•-like species. Se-TiO2 was also examined under hypoxic conditions, where the Se atoms were capable of trapping photogenerated electrons as evidenced by XPS.


Electron Counting Rules And Electronic Structure In Tetrameric Transition-Metal (T)-Centered Rare-Earth (R) Cluster Complex Halides (X), Simon Steinberg, Thomas Bell, Gerd Meyer 2016 Universität zu Köln

Electron Counting Rules And Electronic Structure In Tetrameric Transition-Metal (T)-Centered Rare-Earth (R) Cluster Complex Halides (X), Simon Steinberg, Thomas Bell, Gerd Meyer

Gerd Meyer

Electron partition schemes are a beneficial means to systematize bonding networks and to identify structure-bonding relationships in polar intermetallics. One prolific class of polymetal networks with simple counterions is the broad family of transition-metal (T)-centered rare-earth metal (R) cluster halides (X), which can be isolated or condensed to oligomers and chains. While the electronic structures of R cluster monomers and chains encapsulating T atoms have been studied systematically, the band structures of oligomers, in particular, the most frequent Friauf-type {T4R16} tetramers, have been investigated to a lesser extent. Therefore, the band structures of prototypical compounds with {T4R16}-type tetramers ...


Preparation And Instability Of Nanocrystalline Cuprous Nitride, Malinda D. Reichert, Miles A. White, Michelle J. Thompson, Gordon J. Miller, Javier Vela 2016 Iowa State University

Preparation And Instability Of Nanocrystalline Cuprous Nitride, Malinda D. Reichert, Miles A. White, Michelle J. Thompson, Gordon J. Miller, Javier Vela

Gordon Miller

Low-dimensional cuprous nitride (Cu3N) was synthesized by nitridation (ammonolysis) of cuprous oxide (Cu2O) nanocrystals using either ammonia (NH3) or urea (H2NCONH2) as the nitrogen source. The resulting nanocrystalline Cu3N spontaneously decomposes to nanocrystalline CuO in the presence of both water and oxygen from air at room temperature. Ammonia was produced in 60% chemical yield during Cu3N decomposition, as measured using the colorimetric indophenol method. Because Cu3N decomposition requires H2O and produces substoichiometric amounts of NH3>, we conclude that this reaction proceeds through a ...


Ultrafast Spectroscopy And Energy Transfer In An Organic/Inorganic Composite Of Zinc Oxide And Graphite Oxide, Jeff A. Secor 2016 Graduate Center, City University of New York

Ultrafast Spectroscopy And Energy Transfer In An Organic/Inorganic Composite Of Zinc Oxide And Graphite Oxide, Jeff A. Secor

All Graduate Works by Year: Dissertations, Theses, and Capstone Projects

The energy transfers and nature of defect levels of an organic/inorganic composite of Zinc Oxide and Graphite are studied with multidimensional spectroscopy. The edge and surface states of each composite are uncovered using excitation emission experiments showing which defect states are mediating the energy transfer from the metal oxide to the graphite oxide. Multidimensional time resolved spectroscopy further describes the effect of the carbon phase on the energy transfer pathways in the material.


Preparation, Characterization, Electrochemistry, And Infrared Spectroelectrochemistry Of Ruthenium Nitrosyl Porphyrins Containing Η1-O Bonded Axial Carboxylates, Dennis Awasabisah, Nan Xu, Krishna P. Sharmah-Gautam, Douglas R. Powell, Michael J. Shaw, George B. Richter-Addo 2016 University of Oklahoma Norman Campus

Preparation, Characterization, Electrochemistry, And Infrared Spectroelectrochemistry Of Ruthenium Nitrosyl Porphyrins Containing Η1-O Bonded Axial Carboxylates, Dennis Awasabisah, Nan Xu, Krishna P. Sharmah-Gautam, Douglas R. Powell, Michael J. Shaw, George B. Richter-Addo

SIUE Faculty Research, Scholarship, and Creative Activity

The synthesis, characterization and redox behavior of eight low-spin nitrosyl carboxylate compounds (por)Ru(NO)(η1-OC(=O)R) (por = T(p-OMe)PP: R = Me (1), i-Pr (2), t-Bu (3), p-C6H4NO2 (4), Fc (5), CF3 (8); por = TTP: R = Fc (6)) and (T(p-OMe)PP)Ru(NO)(OC6HF4) (7) are reported. The compounds are moderately stable in air as solids. Their IR (KBr) spectral data show ʋNO's in the 1839-1861 range cm-1. The X-ray crystal structures of compounds 1, 2, 5-7, and 8 have been determined, and reveal ...


Derivation And Implementation Of The Gradient Of The R–7 Dispersion Interaction In The Effective Fragment Potential Method, Emilie B. Guidez, Peng Xu, Mark S. Gordon 2016 Iowa State University

Derivation And Implementation Of The Gradient Of The R–7 Dispersion Interaction In The Effective Fragment Potential Method, Emilie B. Guidez, Peng Xu, Mark S. Gordon

Chemistry Publications

The dispersion interaction energy may be expressed as a sum over Rn terms, with n ≥ 6. Most implementations of the dispersion interaction in model potentials are terminated at n = 6. Those implementations that do include higher order contributions commonly only include even power terms, despite the fact that odd power terms can be important. Because the effective fragment potential (EFP) method contains no empirically fitted parameters, the EFP method provides a useful vehicle for examining the importance of the leading R–7 odd power term in the dispersion expansion. To fully evaluate the importance of the R–7 contribution ...


Procesy Cieplne I Aparaty (Lab), Wojciech M. Budzianowski 2016 Wroclaw University of Technology

Procesy Cieplne I Aparaty (Lab), Wojciech M. Budzianowski

Wojciech Budzianowski

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Design Of First-Row Transition Metal Bis(Alkoxide) Complexes And Their Reactivity Toward Nitrene And Carbene Transfer, James Bellow 2016 Wayne State University

Design Of First-Row Transition Metal Bis(Alkoxide) Complexes And Their Reactivity Toward Nitrene And Carbene Transfer, James Bellow

Wayne State University Dissertations

The novel alkoxide ligand [OCtBu2Ph], or [OR], was synthesized in a single step as a lithium salt. It was then reacted with a series of first-row transition metal(II) halides, with widely varying results. Upon reaction with chromium, manganese, iron, or cobalt(II) chloride, dimeric complexes of the form M2(OR)4Li2Cl2 were formed, which displayed rare seesaw geometry at the metal. This unusual geometry was confirmed by various spectroscopic and computational studies. Computational studies also indicate that the steric bulk of the ligand, as well as the inclusion of lithium atoms in the molecules, are what lead to the ...


Europium(Ii)-Containing Complexes For Responsive Magnetic Resonance Imaging, Levi Alexander Ekanger 2016 Wayne State University

Europium(Ii)-Containing Complexes For Responsive Magnetic Resonance Imaging, Levi Alexander Ekanger

Wayne State University Dissertations

The research projects described in this dissertation are focused on studying the oxidation of EuII-containing complexes within the context of responsive MRI. Prior to this research, EuII had not been explored within the context of oxidation-responsive MRI nor had the use of this ion been reported in vivo. The results of these studies enable predictions about the oxidation-responsive behavior of EuII-containing complexes in vitro and in vivo.

The EuII-containing cryptate 1.33 was used to evaluate EuII-based positive contrast enhancement after intravenous, intraperitoneal, and subcutaneous injections. The transitory behavior of the positive contrast enhancement correlated with reported levels of oxygenation ...


Synthesis And Heteroallene Reactivity Of Bis(Aldimino)Pyridine Nickel Complexes In Four Different Oxidation States, Blake Reed 2016 Wayne State University

Synthesis And Heteroallene Reactivity Of Bis(Aldimino)Pyridine Nickel Complexes In Four Different Oxidation States, Blake Reed

Wayne State University Dissertations

A series of redox non-innocent bis(aldimino)pyridine ligands were synthesized. These were then reacted with nickel(II) salts to form Ni[NNN]X2 complexes. Cyclic voltammograms of these nickel(II) complexes suggest that more reduced states can be achieved. Reduction of these nickel(II) complexes lead to distorted square planar complexes with the halide bent ~20° out of the plane. EPR suggests that spin density is located on the metal as g-values of >2.01 were obtained. This differs from previously reported analogous bis(ketimino)pyridine complexes, which show a ligand-based radical and nickel(II). DFT confirms that as ...


New Approaches To Chalcogenide Materials For Thermoelectrics: Lead Telluride-Based Nanostructures And Facile Synthesis Of Tetrahedrite And Doped Derivatives, Derak Justin James 2016 Wayne State University

New Approaches To Chalcogenide Materials For Thermoelectrics: Lead Telluride-Based Nanostructures And Facile Synthesis Of Tetrahedrite And Doped Derivatives, Derak Justin James

Wayne State University Dissertations

The overall purpose of this work is to address several of the roadblocks to use of thermoelectric materials for generation of electricity, namely inefficient processing of materials and low performance, commonly rated by the figure of merit, ZT=T2/tot. The ZT includes  as the Seebeck coefficient,  as electrical resistivity, T as the average temperature, and tot as total thermal conductivity. tot is the sum of electronic charge carrier (C) and lattice (L) contributions to thermal conductivity. Attempts to increase ZT in the literature to values >1 have focused on decreasing the thermal conductivity via nanostructuring or optimizing the ...


Tuning Complexity By Lithiation: A Family Of Intergrowth Structures Using Condensed Hypho-Icosahedra In The Li-Doped Ca–Zn System, Qisheng Lin, Ran Zhu, Gordon J. Miller 2016 The Ames Laboratory

Tuning Complexity By Lithiation: A Family Of Intergrowth Structures Using Condensed Hypho-Icosahedra In The Li-Doped Ca–Zn System, Qisheng Lin, Ran Zhu, Gordon J. Miller

Chemistry Publications

Cluster chemistry of intermetallics with valence electron counts (VECs) in the range of 2.0–3.0 is intriguing. Lithiation of polar intermetallics in this VEC region is found to be an effective chemical route to produce new complex structures with different stability mechanisms. In this work, two new complex intermetallic structures have been discovered in the Ca–Li–Zn system: Ca12LixZn59–xand Ca15LixZn75–x. Ca12LixZn59–x, x ≈ 5.65(3)–14.95(3), forms in the trigonal space group Rm, with a = 9.074(1)–9.1699(2) Å, c ...


Investigating The Influence Of Gold Nanoparticles On The Photocatalytic And Catalytic Reactivity Of Porous Tungsten Oxide Microparticles, Daniel P. DePuccio 2016 University of Vermont

Investigating The Influence Of Gold Nanoparticles On The Photocatalytic And Catalytic Reactivity Of Porous Tungsten Oxide Microparticles, Daniel P. Depuccio

Graduate College Dissertations and Theses

Tungsten oxide (WO3) is a semiconducting transition metal oxide with interesting electronic, structural, and chemical properties that have been exploited in applications including catalysis, gas sensing, electrochromic displays, and solar energy conversion. Nanocrystalline WO3 can absorb visible light to catalyze heterogeneous photooxidation reactions. Also, the acidity of the WO3 surface makes this oxide a good thermal catalyst in the dehydration of alcohols to various industrially relevant chemicals. This dissertation explores the photocatalytic and thermal catalytic reactivity of nanocrystalline porous WO3 microparticles. Furthermore, investigations into the changes in WO3 reactivity are carried out after modifying the porous WO3 particles with gold ...


Exploring Conditions For The Enhancement Of Acene Semiconductors Through The Use Of The Diels-Alder Reaction, Brittni Qualizza Qualizza 2016 Loyola University Chicago

Exploring Conditions For The Enhancement Of Acene Semiconductors Through The Use Of The Diels-Alder Reaction, Brittni Qualizza Qualizza

Dissertations

This dissertation demonstrates the application of SAMs to the surface of acene crystals, specifically of tetracene and rubrene, using the Diels-Alder reaction. The second chapter details preliminary reaction results and two analytical methods which were employed to confirm adsorption of the dienophile on the surface of single crystals, tetracene and rubrene. These were mass spectrometry and X-ray photoelectron spectroscopy (XPS). Mass spectrometry experiments distinguish the chemical identity of adduct on the crystals and also it discerned chemi- and physisorbed molecules from one another. XPS was used to prove face selectivity of the reaction by the detection of dichloromaleic anhydride. From ...


Surface Analysis Of Model Systems: From A Metal-Graphite Interface To An Intermetallic Catalyst, Emma J. Kwolek 2016 Iowa State University

Surface Analysis Of Model Systems: From A Metal-Graphite Interface To An Intermetallic Catalyst, Emma J. Kwolek

Graduate Theses and Dissertations

This thesis summarizes research completed on two different model systems. In the first system, we investigate the deposition of the elemental metal dysprosium on highly-oriented pyrolytic graphite (HOPG) and its resulting nucleation and growth. The goal of this research is to better understand the metal-carbon interactions that occur on HOPG and to apply those to an array of other carbon surfaces. This insight may prove beneficial to developing and using new materials for electronic applications, magnetic applications and catalysis.

In the second system, we investigate the intermetallic single crystal NaAu2. We conducted a characterization of the clean (111) surface along ...


Iridium Porphyrin Synthesis, Reactivity And Catalysis, And The Nanogold-Catalyzed Synthesis Of Lactams, Taiwo Olawale Dairo 2016 Iowa State University

Iridium Porphyrin Synthesis, Reactivity And Catalysis, And The Nanogold-Catalyzed Synthesis Of Lactams, Taiwo Olawale Dairo

Graduate Theses and Dissertations

The work presented in this report focuses on the synthesis and characterization of new iridium(III) porphyrin complexes, the iridium porphyrin-catalyzed insertion of diazo esters into the S-H bond of thiols (S-H insertion), and the efficient nanogold-catalyzed oxidation of amines into lactams, in the presence of atmospheric oxygen. Preliminary results of the nanogold-catalyzed synthesis of N,N'-disubstituted ureas from the room temperature reaction between primary amines, carbon monoxide and oxygen, are presented as well.

Upon treatment of (carbonyl)chloro(meso-tetra-p-tolylporphyrinato)iridium(III), (TTP)Ir(CO)Cl, with excess primary amines (amine = RNH2 = benzylamine, n-butylamine, isopropylamine, and tert-butylamine), at 23 ...


Magnetic Doping Of Semiconductor Molecular Models And Colloidal Nanocrystals, Swamy Pittala 2016 University of Massachusetts Amherst

Magnetic Doping Of Semiconductor Molecular Models And Colloidal Nanocrystals, Swamy Pittala

Doctoral Dissertations

Spin-based electronics use the spins of electrons in addition to their charges and have potential applications to create a next generation of quantum computers, capable of storing vast amounts of data in an energy-efficient way. Diluted magnetic semiconductor quantum dots (DMS-QDs) have shown great promise as ideal materials for application in spin-based electronics. However, doping impurities into quantum confined colloidal nanocrystals (NCs) has been a great challenge due to the lack of control over the dopant reactivity during the specific stages of nucleation and growth. The mechanism of dopant incorporation into nanocrystals is complex and well-defined and atomically precise molecular ...


Lanthanide Alkyl And Silyl Compounds: Synthesis, Reactivity And Catalysts For Green Chemistry, Aradhana Pindwal 2016 Iowa State University

Lanthanide Alkyl And Silyl Compounds: Synthesis, Reactivity And Catalysts For Green Chemistry, Aradhana Pindwal

Graduate Theses and Dissertations

The last few decades have witnessed enormous research in the field of organometallic lanthanide chemistry. Our research group has developed a few rare earth alkyl compounds containing tris(dimethylsilyl)methyl ligand and explored their reactivity. This thesis focusses on extending the study of lanthanide alkyl and silyl compounds to develop strategies for their synthesis and explore their reactivity and role as catalysts in processes such as hydrosilylation and cross-dehydrocoupling.

Two novel ligands, alkyl, –C(SiHMe2)3 and silyl, –Si(SiHMe2)3 have been used to synthesize homoleptic organometallic lanthanide complexes. The silyl anion, KSi(SiHMe2)3, is prepared from the ...


Organic Molecular Cages As Templates For The Synthesis Of Metallic Nanoparticles: From Stabilization To Application And Assembly, Ryan McCaffrey 2016 University of Colorado at Boulder

Organic Molecular Cages As Templates For The Synthesis Of Metallic Nanoparticles: From Stabilization To Application And Assembly, Ryan Mccaffrey

Chemistry & Biochemistry Graduate Theses & Dissertations

Shape-persistent 3-D covalent organic polyhedrons (COPs) with well-defined intrinsic cavities have been well studied in materials chemistry due to their applications in host-guest chemistry, chemical sensing and gas adsorption and separation. However, the use of 3-D COPs as endo-templates for the synthesis of metallic nanoparticles has not been intensely explored. The purpose of the work described within this thesis is to answer the following questions: Can discrete, purely organic hollow molecular structures be designed in such a way as to facilitate the size-controlled synthesis of metallic nanoparticles? What are the applications of such organic-inorganic hybrid structures? Is it feasible for ...


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