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Surface Chemical Deposition of Advanced Electronic Materials

Description: The focus of this work was to examine the direct plating of Cu on Ru diffusion barriers for use in interconnect technology and the substrate mediated growth of graphene on boron nitride for use in advanced electronic applications. The electrodeposition of Cu on Ru(0001) and polycrystalline substrates (with and without pretreatment in an iodine containing solution) has been studied by cyclic voltammetry (CV), current-time transient measurements (CTT), in situ electrochemical atomic force microscopy (EC-AFM), and X-ray photoelectron spectroscopy (XPS). The EC-AFM data show that at potentials near the OPD/UPD threshold, Cu crystallites exhibit pronounced growth anisotropy, with lateral dimensions greatly exceeding vertical dimensions. XPS measurements confirmed the presence and stability of adsorbed I on the Ru surface following pre-treatment in a KI/H2SO4 solution and following polarization to at least −200 mV vs. Ag/AgCl. CV data of samples pre-reduced in I-containing electrolyte exhibited a narrow Cu deposition peak in the overpotential region and a UPD peak. The kinetics of the electrodeposited Cu films was investigated by CTT measurements and applied to theoretical models of nucleation. The data indicated that a protective I adlayer may be deposited on an air-exposed Ru electrode as the oxide surface is electrochemically reduced, and that this layer will inhibit reformation of an oxide during the Cu electroplating process. A novel method for epitaxial graphene growth directly on a dielectric substrate of systematically variable thickness was studied. Mono/multilayers of BN(111) were grown on Ru(0001) by atomic layer deposition (ALD), exhibiting a flat (non-nanomesh) R30(3x3) structure. BN(111) was used as a template for growth of graphene by chemical vapor deposition (CVD) of C2H4 at 1000 K. Characterization by LEED, Auger, STM/STS and Raman indicate the graphene is in registry with the BN substrate, and exhibits a HOPG-like 0 eV bandgap density-of-states (DOS).
Date: December 2010
Creator: Bjelkevig, Cameron
Partner: UNT Libraries

Investigation of Novel Electrochemical Synthesis of Bioapatites and Use in Elemental Bone Analysis

Description: In this research, electrochemical methods are used to synthesize the inorganic fraction of bone, hydroxyapatite, for application in biological implants and as a calibration material for elemental analysis in human bone. Optimal conditions of electrochemically deposited uniform apatite coatings on stainless steel were investigated. Apatite is a ceramic with many different phases and compositions that have beneficial characteristics for biomedical applications. Of those phases hydroxyapatite (HA) is the most biocompatible and is the primary constituent of the inorganic material in bones. HA coatings on metals and metal alloys have the ability to bridge the growth between human tissues and implant interface, where the metal provides the strength and HA provides the needed bioactivity. The calcium apatites were electrochemically deposited using a modified simulated body fluid adjusted to pH 4-10, for 1-3 hours at varying temperature of 25-65°C while maintaining cathodic potentials of -1.0 to -1.5V. It was observed that the composition and morphology of HA coatings change during deposition by the concentration of counter ions in solution, pH, temperature, applied potential, and post-sintering. The coatings were characterized by powder x-ray diffraction, Fourier transform infrared spectroscopy, and scanning electron microscopy. The precipitated powders from the experiment were also characterized, with results showing similarities to biological apatite. There is a need for quantitative elemental analysis of calcified biological matrices such as bone and teeth; however there are no suitable calibration materials commercially available for quantitative analysis. Matrix-matched standards are electrochemically synthesized for LA-ICP-MS analysis of human bone. The synthetic bioapatite is produced via a hydrothermal electrochemical process using a simulated body fluid solution to form hydroxyapatite. Additional bioapatite standards are synthesized containing trace amounts of metals. The x-ray diffraction of the synthesized standards shows an increase in cell volume for the crystal structure from 0.534 to 0.542 nm3 with the substitution of ...
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Date: December 2012
Creator: DeLeon, Vallerie H.
Partner: UNT Libraries

Ion Replacement Program Annual Report: 1993

Description: Annual report of the Ion Replacement Electrorefining Program at Aronne National Laboratory describing their research and activities. There are three key accomplishments highlighted for the year: (1) identification of a suitable sodium(beta){double_prime}-alumina/molten salt electrolyte system that functions reproducibly at 723 K, (2) actual separation of dysprosium and lanthanum in experiments, and (3) the identification of a metal alloy, Li{sub x}Sb, as an alternative ion replacement electrode.
Date: July 1993
Creator: Tomczuk, Z.
Partner: UNT Libraries Government Documents Department

An Experimental Study of the Electrodeposition of Lead

Description: This thesis aimed to study some of the general principles underlying electrodeposition together with experimental facts regarding the effects of changing constituents of the plating solutions, variations in hydrogen-ion concentrations, and variation in current density used in the electrodeposition of lead.
Date: June 1937
Creator: Roberts, Ira Clifford
Partner: UNT Libraries

LIGA-based microsystem manufacturing:the electrochemistry of through-mold depostion and material properties.

Description: The report presented below is to appear in ''Electrochemistry at the Nanoscale'', Patrik Schmuki, Ed. Springer-Verlag, (ca. 2005). The history of the LIGA process, used for fabricating dimensional precise structures for microsystem applications, is briefly reviewed, as are the basic elements of the technology. The principal focus however, is on the unique aspects of the electrochemistry of LIGA through-mask metal deposition and the generation of the fine and uniform microstructures necessary to ensure proper functionality of LIGA components. We draw from both previously published work by external researchers in the field as well as from published and unpublished studies from within Sandia.
Date: June 1, 2005
Creator: Kelly, James J. (Sandia National Laboratories, Livermore, CA) & Goods, Steven Howard (Sandia National Laboratories, Livermore, CA)
Partner: UNT Libraries Government Documents Department

Reversible Guest Exchange Mechanisms in Supramolecular Host-Guest Assemblies

Description: Synthetic chemists have provided a wide array of supramolecular assemblies able to encapsulate guest molecules. The scope of this tutorial review focuses on supramolecular host molecules capable of reversibly encapsulating polyatomic guests. Much work has been done to determine the mechanism of guest encapsulation and guest release. This review covers common methods of monitoring and characterizing guest exchange such as NMR, UV-VIS, mass spectroscopy, electrochemistry, and calorimetry and also presents representative examples of guest exchange mechanisms. The guest exchange mechanisms of hemicarcerands, cucurbiturils, hydrogen-bonded assemblies, and metal-ligand assemblies are discussed. Special attention is given to systems which exhibit constrictive binding, a motif common in supramolecular guest exchange systems.
Date: September 1, 2006
Creator: Pluth, Michael D. & Raymond, Kenneth N.
Partner: UNT Libraries Government Documents Department

Incorporating Electrochemistry and X-ray Diffraction Experiments Into an Undergraduate Instrumental Analysis Course

Description: Experiments were designed for an undergraduate instrumental analysis laboratory course, two in X-ray diffraction and two in electrochemistry. Those techniques were chosen due their underrepresentation in the Journal of Chemical Education. Paint samples (experiment 1) and pennies (experiment 2) were characterized using x-ray diffraction to teach students how to identify different metals and compounds in a sample. in the third experiment, copper from a penny was used to perform stripping analyses at different deposition times. As the deposition time increases, the current of the stripping peak also increases. the area under the stripping peak gives the number of coulombs passed, which allows students to calculate the mass of copper deposited on the electrode surface. the fourth experiment was on the effects of variable scan rates on a chemical system. This type of experiment gives valuable mechanistic information about the chemical system being studied.
Date: May 2012
Creator: Molina, Cathy
Partner: UNT Libraries

Calcium/metal Sulfide Battery Development Program. Progress Report, October 1979 - September 1980

Description: A Ca-Al-Si/FeS2 cell has been developed and has exhibited reasonably stable capacity through 3200 h of operation. This system is expected to be capable of meeting the ultimate performance goals (i.e., 160 W.h/kg) of this development program. Further tests of this cell system in the coming year will better define its ultimate performance capabilities.
Date: March 1981
Creator: Barney, Duane L.; Roche, M. F.; Preto, S. K.; Ross, L. E.; Otto, N. C. & Martino, F. J.
Partner: UNT Libraries Government Documents Department

Cu Electrodeposition on Ru with a Chemisorbed Iodine Surface Layer.

Description: An iodine surface layer has been prepared on Ru(poly) and Ru(0001) electrodes by exposure to iodine vapor in UHV and polarizing in a 0.1 M HClO4/0.005 M KI solution, respectively. A saturation coverage of I on a Ru(poly) electrode passivates the Ru surface against significant hydroxide, chemisorbed oxygen or oxide formation during exposure to water vapor over an electrochemical cell in a UHV-electrochemistry transfer system. Immersion of I-Ru(poly) results in greater hydroxide and chemisorbed oxygen formation than water vapor exposure, but an inhibition of surface oxide formation relative that of the unmodified Ru(poly) surface is still observed. Studies with combined electrochemical and XPS techniques show that the iodine surface adlayer remained on top of the surface after cycles of overpotential electrodeposition/dissolution of copper on both Ru(poly) and Ru(0001) electrodes. These results indicate the potential bifunctionality of iodine layer to both passivate the Ru surface in the microelectronic processing and to act as a surfactant for copper electrodeposition. The electrodeposition of Cu on Ru(0001) or polycrystalline Ru was studied using XPS with combined ultrahigh vacuum/electrochemistry methodology (UHV-EC) in 0.1 M HClO4 with Cu(ClO4)2 concentrations ranging from 0.005 M to 0.0005 M, and on polycrystalline Ru in a 0.05M H2SO4/0.005 M CuSO4/0.001 M NaCl solution. The electrochemical data show well-defined cyclic voltammograms (CV) with a Cu underpotential deposition (UPD) peak and overpotential deposition (OPD) peak. XPS spectra of Ru electrodes emersed from perchloric acid solution at cathodic potentials indicate that ClO4- anions dissociate to yield specifically adsorbed Cl and ClOx species. Subsequent Cu deposition results in the formation of a thin, insoluble Cu(II) film with Cu(I) underneath. In contrast, similar deposition on polycrystalline Ru in the sulfuric acid/Cu sulfate solution with NaCl added yields only Cu(0), indicating that the formation of Cu(II) and Cu(I) involves both Cl and perchlorate interactions with the ...
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Date: August 2005
Creator: Lei, Jipu
Partner: UNT Libraries

Synthesis and Electrochemistry of Li3MnO4: Mn in the +5 OxidationState

Description: Computational and experimental work directed at exploringthe electrochemical properties of tetrahedrally coordinated Mn in the +5oxidation state is presented. Specific capacities of nearly 700 mAh/g arepredicted for the redox processes of LixMnO4 complexes based on twotwo-phase reactions. One is topotactic extractionof Li from Li3MnO4 toform LiMnO4 and the second is topotactic insertion of Li into Li3MnO4 toform Li5MnO4. In experiments, it is found that the redox behavior ofLi3MnO4 is complicated by disproportionation of Mn5+ in solution to formMn4+ and Mn7+ and byother irreversible processes; although an initialcapacity of about 275 mAh/g in lithiumcells was achieved. Strategiesbased on structural considerations to improve the electrochemicalproperties of MnO4n- complexes are given.
Date: June 19, 2007
Creator: Saint, Juliette.A.; Doeff, Marca M. & Reed, John
Partner: UNT Libraries Government Documents Department

Environment-assisted-cracking under measured and/or controlled ectrochemical potential

Description: Longer-term stress corrosion cracking (SCC) experiments, described in the activity plan E-20-56, are well underway at LLNL to evaluate the SCC susceptibility of candidate corrosion-resistant inner container materials in a 90°ºC acidic brine containing 5 weight percent (wt%) NaCl using fatigue-precracked wedge-loaded double-cantilever-beam (DCB) specimens. The results of a recent localized corrosion study have revealed that the propensity to pitting and crevice corrosion in susceptible alloys is characterized by "critical potentials" obtained from the cyclic potentiodynamic polarization (CPP) experiments described in the activity plan E-20-43/44. It is also well known that the tendency to SCC can be influenced by the electrochemical potential. But the role of electrochemistry in SCC has not been explored to a large extent. Therefore, the proposed activity is aimed at evaluating the SCC behavior of susceptible container materials under measured and/or controlled electrochemical potential in repository-relevant environments using DCB and slow-strain-rate (SSR) test specimens. The magnitude of the controlled potential will be selected based on the measured "critical potentials" obtained from the CPP experiment performed earlier in a similar environment. The resultant data will enable the mechanistic understanding of the cracking process in materials of interest under the synergistic influence of applied stress and corrosive medium, which will be utilized in developing and validating the SCC models for long-term performance assessment.
Date: November 7, 1997
Creator: Roy, A.
Partner: UNT Libraries Government Documents Department


Description: Nickel hydroxides have been used as the active material in the positive electrodes of several alkaline batteries for over a century. These materials continue to attract a lot of attention because of the commercial importance of nickel-cadmium and nickel-metal hydride batteries. This review gives a brief overview of the structure of nickel hydroxide battery electrodes and a more detailed review of the solid state chemistry and electrochemistry of the electrode materials. Emphasis is on work done since 1989.
Date: November 1997
Creator: McBreen, J.
Partner: UNT Libraries Government Documents Department

Fluorinated Dodecaphenylporphyrins: Synthetic and Electrochemical Studies Including the First Evidence of Intramolecular Electron Transfer Between an Fe(II) Porphyrin -Anion Radical and an Fe(I) Porphyrin

Description: Dodecaphenylporphyrins with varying degrees of fluorination of the peripheral phenyl rings (FXDPPS) were synthesized as model compounds for studying electronic effects in nonplan~ porphyrins, and detailed electrochemical studies of the chloroiron(HI) complexes of these compounds were undertaken. The series of porphyrins, represented as FeDPPCl and as FeFXDPPCl where x = 4, 8 (two isomers), 12, 20,28 or 36, could be reversibly oxidized by two electrons in dichloromethane to give n-cation radicals and n-dications. All of the compounds investigated could also be reduced by three electrons in benzonitrile or pyridine. In benzonitrile, three reversible reductions were observed for the unfluorinated compound FeDPPC1, whereas the FeFXDPPCl complexes generally exhibited irreversible first and second reductions which were coupled to chemical reactions. The chemical reaction associated with the first reduction involved a loss of the chloride ion after generation of Fe FXDPPC1. The second chemical reaction involved a novel intramolecular electron transfer between the initially generated Fe(H) porphyrin n-anion radical and the final Fe(I) porphyrin reduction product. In pyridine, three reversible one electron reductions were observed with the second reduction affording stable Fe(II) porphyrin o - anion radicals for ail of the complexes investigated.
Date: October 19, 1998
Creator: D'Souza, F.; Forsyth, T.P.; Fukuzumi, S.; Kadish, K.M.; Krattinger, B.; Lin, M. et al.
Partner: UNT Libraries Government Documents Department

Light scattering studies of an electrorheological fluid in oscillatory shear

Description: We have conducted a real time, two-dimensional light scattering study of the nonlinear dynamics of field-induced structures in an electrorheological fluid subjected to oscillatory shear. We have developed a kinetic chain model of the observed dynamics by considering the response of a fragmenting/aggregating particle chain to the prevailing hydrodynamic and electrostatic forces. This structural theory is then used to describe the nonlinear rheology of ER fluids.
Date: December 31, 1995
Creator: Martin, J.E. & Odinek, J.
Partner: UNT Libraries Government Documents Department

Investigation of Primary Li-Si/FeS2 Cells

Description: The factors that limit the performance of thermally activated Li-Si/FeS2 batteries were defined through the use of electrochemical characterization tests and post-test examinations. For the characterization tests, 82 individual cells were instrumented with multiple voltage sensors and discharged under isothermal and isobaric conditions. The voltage data for the sensors were recorded to determine the ohmic and electrochemical impedances of each cell component at different levels of discharge. The data analysis completed to date has demonstrated that this approach can successfully differentiate the influence of various operating parameters (e.g., temperature, current density), electrode structures (e.g., FeS2 particle size), and additives on cell capacity, specific energy, and power capability. Thirty cells selected from these tests and additional tests at SNL were examined using optical and scanning electron microscopy, energy dispersive spectroscopy, and X-ray diffraction. These analyses documented microstructural and compositional changes in the active materials and electrolyte. In general, the electrochemical impedance of the FeS2 electrode limited cell performance. Several methods (including use of fine FeS2 particle size, graphite additions, and higher operating temperatures) produced measurable reductions in this impedance and yielded significant improvements in specific energy and power. Additions of KCl to the negative electrode extended the low-temperature capacity of this electrode by counterbalancing gradients in electrolyte composition that develop during discharge.
Date: April 1987
Creator: Redey, L.; Smaga, J. A.; Battles, J. E. & Guidotti, Ronald
Partner: UNT Libraries Government Documents Department

Proceedings of the Symposium and Workshop on Advanced Battery Research and Design : March 22-24, 1976

Description: The idea for this meeting evolved from interest expressed by members of the Chicago Section of the Electrochemical Society in convening a symposium on the development of high-energy secondary batteries. The relevance of this subject is evidenced by the several research programs that have been initiated recently in the United States and Europe to develop advanced batteries for use as energy storage devices on electric utility networks and as power sources for electric automobiles.
Date: 1976?
Creator: Selman, J. Robert; Steunenberg, Robert K.; Barghusen, John J. & Howard, William G.
Partner: UNT Libraries Government Documents Department

Copper Electrodeposition on Iridium, Ruthenium and Its Conductive Oxide Substrate

Description: The aim of this thesis was to investigate the physical and electrochemical properties of sub monolayer and monolayer of copper deposition on the polycrystalline iridium, ruthenium and its conductive oxide. The electrochemical methods cyclic voltammetry (CV) and chronocoulometry were used to study the under potential deposition. The electrochemical methods to oxidize the ruthenium metal are presented, and the electrochemical properties of the oxide ruthenium are studied. The full range of CV is presented in this thesis, and the distances between the stripping bulk peak and stripping UPD peak in various concentration of CuSO4 on iridium, ruthenium and its conductive oxide are shown, which yields thermodynamic data on relative difference of bonding strength between Cu-Ru/Ir atoms and Cu-Cu atoms. The monolayer of UPD on ruthenium is about 0.5mL, and on oxidized ruthenium is around 0.9mL to 1.0mL. The conductive oxide ruthenium presents the similar properties of ruthenium metal. The pH effect of stripping bulk peak and stripping UPD peak of copper deposition on ruthenium and oxide ruthenium was investigated. The stripping UPD peak and stripping bulk peak disappeared after the pH ≥ 3 on oxidized ruthenium electrode, and a new peak appeared, which means the condition of pH is very important. The results show that the Cl- , SO42- , Br- will affect the position of stripping bulk peak and stripping UPD peak: the stripping bulk peak will shift and decrease if the concentration of halide ions is increasing, and the monolayer of UPD will increase at the same time.
Date: December 2003
Creator: Huang, Long
Partner: UNT Libraries