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Electrodeposition of Gold and Silver from Cyanide Solutions

Description: From Introduction: "This report on the electrodeposition of gold and silver from cyanide solutions represents work that has occupied my time at intervals during the past 20 years, The investigations has been carried on simultaneously with my duties as professor of mining and metallurgy of the University of California."
Date: 1919
Creator: Christy, S. B.
Partner: UNT Libraries Government Documents Department

Electrochemical Depostion of Bismuth on Ruthenium and Ruthenium Oxide Surfaces

Description: Cyclic voltammetry experiments were performed to compare the electrodeposition characteristics of bismuth on ruthenium. Two types of electrodes were used for comparison: a Ru shot electrode (polycrystalline) and a thin film of radio-frequency sputtered Ru on a Ti/Si(100) support. Experiments were performed in 1mM Bi(NO3)3/0.5M H2SO4 with switching potentials between -0.25 and 0.55V (vs. KCl sat. Ag/AgCl) and a 20mV/s scan rate. Grazing incidence x-ray diffraction (GIXRD) determined the freshly prepared thin film electrode was hexagonally close-packed. After thermally oxidizing at 600°C for 20 minutes, the thin film adopts the tetragonal structure consistent with RuO2. a hydrated oxide film (RuOx?(H2O)y) was made by holding 1.3V on the surface of the film in H2SO4 for 60 seconds and was determined to be amorphous. Underpotential deposition of Bi was observed on the metallic surfaces and the electrochemically oxidized surface; it was not observed on the thermal oxide.
Date: May 2012
Creator: Taylor, Daniel M.
Partner: UNT Libraries

Electrodeposit of Nickel

Description: The purpose of this study is to investigate the varying conditions in types of solutions, concentrations of solutions, hydrogen-ion concentration, current densities and potentials in the electro deposition of nickel.
Date: August 1937
Creator: Rohrer, Charles Stephen
Partner: UNT Libraries

Influence of Bath Composition at Acidic pH on Electrodeposition of Nickel-Layered Silicate Nanocomposites for Corrosion Protection

Description: This article describes how nickel-layered silicate nanocomposite films were electrochemically deposited using pulsed potentiostatic conditions from an acidic plating bath containing exfoliated layered silicate to enhance adhesion to the substrate, corrosion resistance, and mechanical properties.
Date: September 25, 2013
Creator: Tientong, Jeerapan; Thurber, Casey; D'Souza, Nandika; Mohamed, Adel M. A. & Golden, Teresa
Partner: UNT College of Arts and Sciences

The Preparation of Thin Films of Plutonium by Electrodeposition

Description: This report discusses methods for preparing thin films of plutonium on metallic disks, which are used for alpha energy analysis, fission counting, and preparation of geometry standards in ordinary counting. Various methods of preparation were tested and analyzed, but electrodeposition was the most effective method. Deposition was then tested, but the yields were "somewhat erratic".
Date: March 22, 1950
Creator: Miller, H. W. & Brouns, R. J.
Partner: UNT Libraries Government Documents Department

Understanding and Tailoring the Mechanical Properties of LIGA Fabricated Materials

Description: LIGA fabricated materials and components exhibit several processing issues affecting their metallurgical and mechanical properties, potentially limiting their usefulness for MEMS applications. For example, LIGA processing by metal electrodeposition is very sensitive to deposition conditions which causes significant processing lot variations of mechanical and metallurgical properties. Furthermore, the process produces a material with a highly textured lenticular rnicrostructural morphology suggesting an anisotropic material response. Understanding and controlling out-of-plane anisotropy is desirable for LIGA components designed for out-of-plane flexures. Previous work by the current authors focused on results from a miniature servo-hydraulic mechanical test frame constructed for characterizing LIGA materials. Those results demonstrated microstructural and mechanical properties dependencies with plating bath current density in LIGA fabricated nickel (LIGA Ni). This presentation builds on that work and fosters a methodology for controlling the properties of LIGA fabricated materials through processing. New results include measurement of mechanical properties of LIGA fabricated copper (LIGA Cu), out-of-plane and localized mechanical property measurements using compression testing and nanoindentation of LIGA Ni and LIGA Cu.
Date: January 25, 1999
Creator: Buchheit, T.E.; Christenson, T.R.; Lavan, D.A. & Schmale, D.T.
Partner: UNT Libraries Government Documents Department

The Revival of Electrochemistry: Electrochemical Deposition of Metals in Semiconductor Related Research

Description: Adherent Cu films were electrodeposited onto polycrystalline W foils from purged solutions of 0.05 M CuSO4 in H2SO4 supporting electrolyte and 0.025 M CuCO3∙Cu(OH)2 in 0.32 M H3BO3 and corresponding HBF4 supporting electrolyte, both at pH = 1. Films were deposited under constant potential conditions at voltages between -0.6 V and -0.2 V versus Ag/AgCl. All films produced by pulses of 10 s duration were visible to the eye, copper colored, and survived a crude test called "the Scotch tape test", which involves sticking the scotch tape on the sample, then peeling off the tape and observing if the copper film peels off or not. Characterization by scanning electron microscopy (SEM)/energy dispersive X-ray (EDX) and X-ray photon spectroscopy (XPS) confirmed the presence of metallic Cu, with apparent dendritic growth. No sulfur impurity was observable by XPS or EDX. Kinetics measurements indicated that the Cu nucleation process in the sulfuric bath is slower than in the borate bath. In both baths, nucleation kinetics does not correspond to either instantaneous or progressive nucleation. Films deposited from 0.05 M CuSO4/H2SO4 solution at pH > 1 at -0.2 V exhibited poor adhesion and decreased Cu reduction current. In both borate and sulfate baths, small Cu nuclei are observable by SEM upon deposition at higher negative overpotentials, while only large nuclei (~ 1 micron or larger) are observed upon deposition at less negative potentials. Osmium metal has been successfully electrodeposited directly onto p-Si (100) from both Os3+ and Os4+ in both sulfuric and perchloric baths. This electrochemical deposition of osmium metal can provide sufficient amount of osmium which overcome ion beam implantation limitations. The deposited metal can undergo further processing to form osmium silicides, such as Os2Si3, which can be used as optical active materials. The higher osmium concentration results in large deposition currents and ...
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Date: August 2005
Creator: Wang, Chen
Partner: UNT Libraries

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

Electrodeposited Ag-Stabilization Layer for High Temperature Superconducting Coated Conductors: Preprint

Description: We developed a non-aqueous based electrodepostion process of Ag-stabilization layer on YBCO superconductor tapes. The non-aqueous electroplating solution is non-reactive to the HTS layer thus does not detoriate the critical current capability of the superconductor layer when plated directly on the HTS tape. The superconducting current capabilities of these tapes were measured by non-contact magnetic measurements.
Date: November 1, 2010
Creator: Bhattacharya, R. N.; Mann, J.; Qiao, Y.; Zhang, Y. & Selvamanickam, V.
Partner: UNT Libraries Government Documents Department

Non-cyanide silver plating

Description: Lawrence Livermore National Laboratory (LLNL) and Technic, Inc. have entered into a CRADA (Cooperative Research and Development Agreement) with the goal of providing industry with an environmentally benign alternative to the presently used silver cyanide plating process. This project has been in place for about six months and results are quite promising. The main objective, that of deposition of deposits as thick as 125 um (5 mils), has been met. Property data such as stress and hardness have been obtained and the structure of the deposit has been analyzed via metallography and x-ray diffraction. These results will be presented in this paper, along with plans for future work.
Date: November 7, 1995
Creator: Dini, J.W.
Partner: UNT Libraries Government Documents Department

The use of fractally-designed waveforms in electroforming

Description: Pulsed electrodeposition offers the potential for superior control of deposit properties because of the additional control variables available. However, optimization of pulsed deposition processes is a challenge because of the complexity. E.g., the tendency of electroforms to acquire irregularities such as dendritic growths or other morphological instabilities, creates the need for methods to control these undesirable phenomena. One such method is periodic reverse pulses. Optimization of periodic reverse processes is not simple and can lead to local solutions that do not optimize all properties simultaneously. One method for global optimization that might, for example, control surface irregularities on several size scales, uses a periodic reverse design based on fractal time series. This incorporates deplating pulses of several lengths within one self- similar waveform. The properties of fractals permit control of highly complex designs with a small number of input variables. The creation of such waveforms, their properties, and their use in a lead- plating process are described. Speculation on the potential for further application of this method is offered. 26 figs, 11 refs.
Date: March 1, 1996
Creator: Bullock, J.S.; Lawson, R.L. & Kirkpatrick, J.R.
Partner: UNT Libraries Government Documents Department

Optimizing fabrication of electrodeposited 3D surface features

Description: Selective electrodeposition onto specially masked surfaces (producing blind holes with non-conductive side walls) has been investigated. The thick masks are low cost polymer sheet into which holes and other patterns are machined. Plating with this type of masking system is one method of fabricating medium aspect ratio metallic structures (structures whose width to length ratio is greater than 10/1). The experiment was conducted with deposits of OFC copper from an acid sulfate solution, but similar results are expected with other metals. Structure diameter varied from 0.25 mm to 3.8 mm (0.01`` to 0.150``). The effect of current density, electrolyte concentration, solution temperature, and agitation on deposition rate were investigated. Deposit quality, deposition rate, and optimal plating parameters were evaluated.
Date: July 1, 1998
Creator: Steffani, C., LLNL
Partner: UNT Libraries Government Documents Department

Modeling electrodeposition for LIGA microdevice fabrication

Description: To better understand and to help optimize the electroforming portion of the LIGA process, we have developed one and two-dimensional numerical models describing electrode-position of metal into high aspect-ratio molds. The one-dimensional model addresses dissociation, diffusion, electromigration, and deposition of multiple ion species. The two-dimensional model is limited to a single species, but includes transport induced by forced flow of electrolyte outside the mold and by buoyancy associated with metal ion depletion within the mold. To guide model development and to validate these models, we have also conducted a series of laboratory experiments using a sulfamate bath to deposit nickel in cylindrical molds having aspect ratios up to twenty-five. The experimental results indicate that current densities well in excess of the diffusion-limited currents may still yield metal deposits of acceptable morphology. However, the numerical models demonstrate that such large ion fluxes cannot be sustained by convection within the mold resulting from flow across the mold top. Instead, calculations suggest that the observed enhancement of transport probably results from natural convection within the molds, and that buoyancy-driven flows may be critical to metal ion transport even in micron-scale features having very large aspect ratios. Taking advantage of this enhanced ion transport may allow order-of-magnitude reductions in electroforming times for LIGA microdevice fabrication. 42 refs., 14 figs., 1 tab.
Date: February 1, 1998
Creator: Griffiths, S.K.; Nilson, R.H. & Bradshaw, R.W.
Partner: UNT Libraries Government Documents Department

Electrodeposition research progress report, March 1--31, 1948

Description: Plating of Postum out of Nitric Acid and Hydrofluoric Acid Solutions -- W. Abel and W. Raiff. Postum was plated out of 1.5 normal nitric acid and 1.0 normal hydrofluoric acid under similar conditions. The hydrofluoric acid plate was better appearing, and had a much higher curie density. However, neutron counts in these runs were quite similar. Neutron Counts -- W. Abel and W. Raiff. A study of the change of neutron counts over a period of time was started. Conversion of Active Hydrofluoric Acid Solutions to Hydrochloric Acid Solutions -- W. Raiff. A 99.99+ per cent conversion was effected. Conversion of Production Solutions to 1.0 Normal Hydrofluoric Add Solutions -- R. Bell. Good conversion has been achieved; however, further work needs to be done on complete change of postum from the production solution to 1.0 normal hydrofluoric acid solutions.
Date: December 31, 1948
Creator: Orban, E.
Partner: UNT Libraries Government Documents Department

Cu Electrodeposition on Ru-Ta and Corrosion of Plasma Treated Cu in Post Etch Cleaning Solution

Description: In this work, the possibility of Cu electrodeposition on Ru-Ta alloy thin films is explored. Ru and Ta were sputter deposited on Si substrate with different composition verified by RBS. Four point probe, XRD, TEM and AFM were used to study the properties of Ru-Ta thin films such as sheet resistance, crystallinity, grain size, etc. Cyclic voltammetry is used to study the Cu electrodeposition characteristics on Ru-Ta after various surface pretreatments. The results provide insights on the removal of Ta oxide such that it enables better Cu nucleation and adhesion. Bimetallic corrosion of Cu on modified Ru-Ta surface was studied in CMP related chemicals. In Cu interconnect fabrication process, the making of trenches and vias on low-k dielectric films involves the application of fluorocarbon plasma etch gases. Cu microdots deposited on Ru and Ta substrate were treated by fluorocarbon plasma etch gases such as CF4, CF4+O2, CH2F2, C4F8 and SF6 and investigated by using x-ray photoelectron spectroscopy, contact angle measurement and electrochemical techniques. Micropattern corrosion screening technique was used to measure the corrosion rate of plasma treated Cu. XPS results revealed different surface chemistry on Cu after treating with plasma etching. The fluorine/carbon ratio of the etching gases results in different extent of fluorocarbon polymer residues and affects the cleaning efficiency and Cu corrosion trends.
Date: August 2011
Creator: Sundararaju Meenakshiah Pillai, Karthikeyan
Partner: UNT Libraries

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

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.
Date: August 2004
Creator: Vavilala, Suma
Partner: UNT Libraries

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

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 the most important parameters to govern the quality of the deposited films, where adding of acetylide into the electrolyte led to films with a higher degree of graphitic phases. The proposed mechanism for acetylene anodic oxidation does not involve direct electron transfer but electrochemical cyclization of acetylene radical cations and hydrogen abstraction at the termination steps. Sodium acetylide, however, dissociates to an acetylenic ion, C2H-, in liquid ammonia. The electrochemistry heterogeneity also leads to island and two-dimensional (2D) nucleation growth of DLC films. Different bond formations of metal to carbon and different chemisorptions of acetylene on metal play important roles ...
Date: August 2004
Creator: Pingsuthiwong, Charoendee
Partner: UNT Libraries

Monsanto Chemical Company, Unit 3 progress report, January 16--31, 1948

Description: Solubilities -- Orban: The solubility of postum in various concentrations of nitric acid was determined at 25.4{degrees}C. Hydrofluoric and Trifluoroacetic Acids -- Abel and Raiff: Details of this work will be reported in the next Progress Report. Conversion of Nitric Acid Solutions to Hydrofluoric Acid Solutions -- Bell: Conversion of production solutions to hydrofluoric acid solutions was tried by precipitation with ammonium oxalate, aluminum hydroxide, ammonium hydroxide, and sodium carbonate. Silver and Teflon discs were used.
Date: December 31, 1948
Partner: UNT Libraries Government Documents Department

Electrodeposition of adherent copper film on unmodified tungsten.

Description: Adherent Cu films were electrodeposited onto polycrystalline W foils from purged solutions of 0.05 M CuSO4 in H2SO4 supporting electrolyte and 0.025 M CuCO3∙Cu(OH)2 in 0.32 M H3BO3 and corresponding HBF4 supporting electrolyte, both at pH = 1. Films were deposited under constant potential conditions at voltages between -0.6 V and -0.2 V vs Ag/AgCl. All films produced by pulses of 10 s duration were visible to the eye, copper colored, and survived a crude test called "the Scotch tape test", which stick the scotch tape on the sample, then peel off the tape and see if the copper film peels off or not. Characterization by scanning electron microscopy (SEM), energy dispersive X-ray (EDX) and X-ray photon spectroscopy (XPS) confirmed the presence of metallic Cu, with apparent dendritic growth. No sulfur impurity was observable by XPS or EDX. Kinetics measurements indicate that the Cu nucleation process in the sulfuric bath is slower than in the borate bath. In both baths, nucleation kinetics do not correspond to either instantaneous or progressive nucleation. Films deposited from 0.05 M CuSO4/H2SO4 solution at pH > 1 at -0.2 V exhibited poor adhesion and decreased Cu reduction current. In both borate and sulfate baths, small Cu nuclei are observable by SEM upon deposition at higher negative overpotentials, while only large nuclei (~ 1 micron or larger) are observed upon deposition at less negative potentials.
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Date: May 2004
Creator: Wang, Chen
Partner: UNT Libraries

Electrochemical Deposition of Nickel Nanocomposites in Acidic Solution for Increased Corrosion Resistance

Description: The optimal conditions for deposition of nickel coating and Ni-layered double hydroxide metal matrix composite coatings onto stainless steel discs in a modified all-sulfate solutions have been examined. Nickel films provide good general corrosion resistance and mechanical properties as a protective layer on many metallic substrates. In recent years, there has been interest in incorporation nano-dimensional ceramic materials, such as montemorillonite, into the metal matrices to improve upon the corrosion and mechanical properties. Layered double hydroxides have been used as corrosion enhancer in polymer coatings by increasing mechanical strength and lowering the corrosion rate but until now, have not been incorporated in a metal matrix by any means. Layered double hydroxides can be easily synthesized in a variety of elemental compositions and sizes but typically require the use of non-polar solvents to delaminate into nanodimensional colloidal suspensions. The synthesis of a Zn-Al LDH has been studied and characterized. The effects of the non-polar solvents dimethylformamide and n-butanol on the deposition and corrosion resistance of nickel coatings from a borate electrolyte bath have been studied, a nickel-LDH nanocomposite coating has been synthesized by electrochemical deposition and the corrosion resistance has been studied. Results indicate an improvement in corrosion resistance for the coatings with minimal change in the nickel matrix's internal strain and crystallite size.
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Date: August 2017
Creator: Daugherty, Ryan E.
Partner: UNT Libraries