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 Degree Discipline: Analytical Chemistry
 Collection: UNT Theses and Dissertations
Adherence/Diffusion Barrier Layers for Copper Metallization: Amorphous Carbon:Silicon Polymerized Films

Adherence/Diffusion Barrier Layers for Copper Metallization: Amorphous Carbon:Silicon Polymerized Films

Date: May 2004
Creator: Pritchett, Merry
Description: Semiconductor circuitry feature miniaturization continues in response to Moore 's Law pushing the limits of aluminum and forcing the transition to Cu due to its lower resistivity and electromigration. Copper diffuses into silicon dioxide under thermal and electrical stresses, requiring the use of barriers to inhibit diffusion, adding to the insulator thickness and delay time, or replacement of SiO2 with new insulator materials that can inhibit diffusion while enabling Cu wetting. This study proposes modified amorphous silicon carbon hydrogen (a-Si:C:H) films as possible diffusion barriers and replacements for SiO2 between metal levels, interlevel dielectric (ILD), or between metal lines (IMD), based upon the diffusion inhibition of previous a-Si:C:H species expected lower dielectric constants, acceptable thermal conductivity. Vinyltrimethylsilane (VTMS) precursor was condensed on a titanium substrate at 90 K and bombarded with electron beams to induce crosslinking and form polymerized a-Si:C:H films. Modifications of the films with hydroxyl and nitrogen was accomplished by dosing the condensed VTMS with water or ammonia before electron bombardment producing a-Si:C:H/OH and a-Si:C:H/N and a-Si:C:H/OH/N polymerized films in expectation of developing films that would inhibit copper diffusion and promote Cu adherence, wetting, on the film surface. X-ray Photoelectron Spectroscopy was used to characterize Cu metallization of ...
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Analysis of PAH and PCB Emissions from the Combustion of dRDF and the Nondestructive Analysis of Stamp Adhesives

Analysis of PAH and PCB Emissions from the Combustion of dRDF and the Nondestructive Analysis of Stamp Adhesives

Date: May 1989
Creator: Poslusny, Matthew
Description: This work includes two unrelated areas of research. The first portion of this work involved combusting densified refuse derived fuel (dRDF) with coal and studying the effect that Ca(0H)2 binder had on reducing polycyclic aromatic hydrocarbon (PAH) and polychlorinated biphenyl (PCB) emissions. The second area of work was directed at developing nondestructive infrared techniques in order to aid in the analysis of postage stamp adhesives. With Americans generating 150-200 million tons a year of Municipal Solid Waste (MSW) and disposing of nearly ninety percent of it in landfills, it is easy to understand why American landfills are approaching capacity. One alternative to landfilling is to process the MSW into RDF. There are technical and environmental problems associated with RDF. This work provides some answers concerning the amount of PAH and PCB emissions generated via the combustion of RDF with coal. It was found that the Ca(OH)2 binder greatly reduced both the PAH and the PCB emissions. In fact, PAH emissions at the ten-percent level were reduced more by using the binder than by the pollution control equipment. If the Ca(0H)2 binder can reduce not only PAH and PCB emissions, but also other noxious emissions, such as acid gases or dioxin, ...
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The Analysis of PCDD and PCDF Emissions from the Cofiring of Densified Refuse Derived Fuel and Coal

The Analysis of PCDD and PCDF Emissions from the Cofiring of Densified Refuse Derived Fuel and Coal

Date: August 1990
Creator: Moore, Paul, 1962-
Description: The United States leads the world in per capita production of Municipal Solid Waste (MSW), generating approximately 200 million tons per year. By 2000 A.D. the US EPA predicts a 20% rise in these numbers. Currently the major strategies of MSW disposal are (i) landfill and (ii) incineration. The amount of landfill space in the US is on a rapid decline. There are -10,000 landfill sites in the country, of which only 65-70% are still in use. The Office of Technology Assessment (OTA) predicts an 80% landfill closure rate in the next 20 years. The development of a viable energy resource from MSW, in the form of densified Refuse Derived Fuel (dRDF), provides solutions to the problems of MSW generation and fossil fuel depletions. Every 2 tons of MSW yields approximately 1 ton of dRDF. Each ton of dRDF has an energy equivalent of more than two barrels of oil. At current production rates the US is "throwing away" over 200,000,000 barrels of oil a year. In order to be considered a truly viable product dRDF must be extensively studied; in terms of it's cost of production, it's combustion properties, and it's potential for environmental pollution. In 1987 a research ...
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Calcium Silicates: Glass Content and Hydration Behavior

Calcium Silicates: Glass Content and Hydration Behavior

Date: August 1987
Creator: Zgambo, Thomas P. (Thomas Patrick)
Description: Pure, MgO doped and B2C3 doped monocalcium, dicalcium, and tricalcium silicates were prepared with different glass contents. Characterization of the anhydrous materials was carried out using optical microscopy, infrared absorption spectroscopy, and X-ray powder diffraction. The hydration of these compounds was studied as a function of the glass contents. The hydration studies were conducted at 25°C. Water/solid ratios of 0.5, 1, 10, and 16 were used for the various experiments. The hydration behavior was monitored through calorimetry, conductometry, pH measurements, morphological developments by scanning electron microscopy, phase development by X-ray powder diffraction, and percent combined water by thermogravimetry. A highly sensitive ten cell pseudo-adiabatic microcalorimeter was designed and constructed for early hydration studies. Conductometry was found to be of great utility in monitoring the hydration of monocalcium silicate and the borate doped dicalcium silicates.
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Chemistry, Detection, and Control of Metals during Silicon Processing

Chemistry, Detection, and Control of Metals during Silicon Processing

Date: May 2005
Creator: Hurd, Trace Q.
Description: This dissertation focuses on the chemistry, detection, and control of metals and metal contaminants during manufacturing of integrated circuits (ICs) on silicon wafers. Chapter 1 begins with an overview of IC manufacturing, including discussion of the common aqueous cleaning solutions, metallization processes, and analytical techniques that will be investigated in subsequent chapters. Chapter 2 covers initial investigations into the chemistry of the SC2 clean - a mixture of HCl, H2O2, and DI water - especially on the behavior of H2O2 in this solution and the impact of HCl concentration on metal removal from particle addition to silicon oxide surfaces. Chapter 3 includes a more generalized investigation of the chemistry of metal ions in solution and how they react with the silicon oxide surfaces they are brought into contact with, concluding with illumination of the fundamental chemical principles that govern their behavior. Chapter 4 shows how metal contaminants behave on silicon wafers when subjected to the high temperature (≥ 800 °C) thermal cycles that are encountered in IC manufacturing. It demonstrates that knowledge of some fundamental thermodynamic properties of the metals allow accurate prediction of what will happen to a metal during these processes. Chapter 5 covers a very different but ...
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Copper Electrodeposition on Iridium, Ruthenium and Its Conductive Oxide Substrate

Copper Electrodeposition on Iridium, Ruthenium and Its Conductive Oxide Substrate

Date: December 2003
Creator: Huang, Long
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. ...
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Cu Electrodeposition on Ru with a Chemisorbed Iodine Surface Layer.

Cu Electrodeposition on Ru with a Chemisorbed Iodine Surface Layer.

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Date: August 2005
Creator: Lei, Jipu
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 ...
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Determination of Solute Descriptors for Illicit Drugs Using Gas Chromatographic Retention Data and Abraham Solvation Model

Determination of Solute Descriptors for Illicit Drugs Using Gas Chromatographic Retention Data and Abraham Solvation Model

Date: August 2015
Creator: Mitheo, Yannick K.
Description: In this experiment, more than one hundred volatile organic compounds were analyzed with the gas chromatograph. Six capillary columns ZB wax plus, ZB 35, TR1MS, TR5, TG5MS and TG1301MS with different polarities have been used for separation of compounds and illicit drugs. The Abraham solvation model has five solute descriptors. The solute descriptors are E, S, A, B, L (or V). Based on the six stationary phases, six equations were constructed as a training set for each of the six columns. The six equations served to calculate the solute descriptors for a set of illicit drugs. Drugs studied are nicotine (S= 0.870, A= 0.000, B= 1.073), oxycodone(S= 2.564. A= 0.286, B= 1.706), methamphetamine (S= 0.297, A= 1.570, B= 1.009), heroin (S=2.224, A= 0.000, B= 2.136) and ketamine (S= 1.005, A= 0.000, B= 1.126). The solute property of Abraham solvation model is represented as a logarithm of retention time, thus the logarithm of experimental and calculated retention times is compared.
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Direct Inject Mass Spectrometry for Illicit Chemistry Detection and Characterization

Direct Inject Mass Spectrometry for Illicit Chemistry Detection and Characterization

Date: May 2016
Creator: Williams, Kristina
Description: The field of direct inject mass spectrometry includes a massive host of ambient ionization techniques that are especially useful for forensic analysts. Whether the sample is trace amounts of drugs or explosives or bulk amounts of synthetic drugs from a clandestine laboratory, the analysis of forensic evidence requires minimal sample preparation, evidence preservation, and high sensitivity. Direct inject mass spectrometry techniques can rarely provide all of these. Direct analyte-probed nanoextraction coupled to nanospray ionization mass spectrometry, however, is certainly capable of achieving these goals. As a multifaceted tool developed in the Verbeck laboratory, many forensic applications have since been investigated (trace drug and explosives analysis). Direct inject mass spectrometry can also be easily coupled to assays to obtain additional information about the analytes in question. By performing a parallel artificial membrane assay or a cell membrane stationary phase extraction prior to direct infusion of the sample, membrane permeability data and receptor activity data can be obtained in addition to the mass spectral data that was already being collected. This is particularly useful for characterizing illicit drugs and their analogues for a biologically relevant way to schedule new psychoactive substances.
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Electrochemical Synthesis and Characterization of Inorganic Materials from Aqueous Solutions

Electrochemical Synthesis and Characterization of Inorganic Materials from Aqueous Solutions

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Date: December 2006
Creator: Yuan, Qiuhua
Description: The dissertation consists of the following three sections: 1. Hydroxyapatite (HA) coatings. In this work, we deposited HA precursor films from weak basic electrolytic solution (pH= 8-9) via an electrochemical approach; the deposits were changed into crystallite coatings of hydroxyapatite by sintering at specific temperatures (600-800 ºC). The formed coatings were mainly characterized by powder X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), and scanning electron microscopy (SEM). XRD patterns show well-defined peaks of HA when sintered under vacuum conditions. FTIR measurements indicate the existence of hydroxyl groups, which were confirmed by the characteristic intensity of the stretching and bending bands at ~3575 and ~630 cm-1, respectively. The SEM shows an adhesive, crack free morphology for the double-layer coating surface of the samples sintered in a vacuum furnace. 2. Silver/polymer/clay nanocomposites. Silver nanoparticles were prepared in layered clay mineral (montmorillonite)/polymer (PVP: poly (vinyl pyrrolidone)) suspension by an electrochemical approach. The silver particles formed in the bulk suspension were stabilized by the PVP and partially exfoliated clay platelets, which acted as protective colloids to prevent coagulation of silver nanoparticles together. The synthesized silver nanoparticles/montmorillonite/PVP composite was characterized and identified by XRD, SEM, and TEM (transmission electron microscopy) measurements. 3. Ce-doped lead ...
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Electrodeposition of adherent copper film on unmodified tungsten.

Electrodeposition of adherent copper film on unmodified tungsten.

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Date: May 2004
Creator: Wang, Chen
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 ...
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Electrodeposition of Copper on Ruthenium Oxides and Bimetallic Corrosion of Copper/Ruthenium in Polyphenolic Antioxidants

Electrodeposition of Copper on Ruthenium Oxides and Bimetallic Corrosion of Copper/Ruthenium in Polyphenolic Antioxidants

Date: August 2007
Creator: Venkataraman, Shyam S.
Description: Copper (Cu) electrodeposition on ruthenium (Ru) oxides was studied due to important implications in semiconductor industry. Ruthenium, proposed as the copper diffusion barrier/liner material, has higher oxygen affinity to form different oxides. Three different oxides (the native oxide, reversible oxide, and irreversible oxide) were studied. Native oxide can be formed on exposing Ru in atmosphere. The reversible and irreversible oxides can be formed by applying electrochemical potential. Investigation of Cu under potential deposition on these oxides indicates the similarity between native and reversible oxides by its nature of inhibiting Cu deposition. Irreversible oxide formed on Ru surface is rather conductive and interfacial binding between Cu and Ru is greatly enhanced. After deposition, bimetallic corrosion of Cu/Ru in different polyphenols was studied. Polyphenols are widely used as antioxidants in post chemical mechanical planarization (CMP). For this purpose, different trihydroxyl substituted benzenes were used as antioxidants. Ru, with its noble nature enhances bimetallic corrosion of Cu. Gallic acid (3,4,5 - trihydroxybenzoic acid) was chosen as model compound. A mechanism has been proposed and validity of the mechanism was checked with other antioxidants. Results show that understanding the chemical structure of antioxidants is necessary during its course of reaction with Cu.
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Electrodeposition of Diamond-like Carbon Films

Electrodeposition of Diamond-like Carbon Films

Date: August 2002
Creator: Chen, Minhua
Description: Electrodeposition of diamond-like carbon (DLC) films was studied on different substrates using two different electrochemical methods. The first electrochemical method using a three-electrode system was studied to successfully deposit hydrogenated DLC films on Nickel, Copper and Brass substrates. The as-deposited films were characterized by scanning electron microscopy (SEM), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), fourier transform infrared spectroscopy (FTIR) and cyclic voltammetry (CV). A variety of experimental parameters were shown to affect the deposition process. The second electrochemical method was developed for the first time to deposit hydrogen free DLC films on Ni substrates through a two-electrode system. The as-deposited films were characterized by Raman spectroscopy and FTIR. According to Raman spectra, a high fraction of diamond nanocrystals were found to form in the films. Several possible mechanisms were discussed for each deposition method. An electrochemical method was proposed to deposit boron-doped diamond films for future work.
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Experimental Determination of L, Ostwald Solubility Solute Descriptor for Illegal Drugs By Gas Chromatography and Analysis By the Abraham Model

Experimental Determination of L, Ostwald Solubility Solute Descriptor for Illegal Drugs By Gas Chromatography and Analysis By the Abraham Model

Date: May 2012
Creator: Wang, Zhouxing
Description: The experiment successfully established the mathematical correlations between the logarithm of retention time of illegal drugs with GC system and the solute descriptor L from the Abraham model. the experiment used the method of Gas Chromatography to analyze the samples of illegal drugs and obtain the retention time of each one. Using the Abraham model to calculate and analyze the sorption coefficient of illegal drugs is an effective way to estimate the drugs. Comparison of the experimental data and calculated data shows that the Abraham linear free energy relationship (LFER) model predicts retention behavior reasonably well for most compounds. It can calculate the solute descriptors of illegal drugs from the retention time of GC system. However, the illegal drugs chosen for this experiment were not all ideal for GC analysis. HPLC is the optimal instrument and will be used for future work. HPLC analysis of the illegal drug compounds will allow for the determination of all the solute descriptors allowing one to predict the illegal drugs behavior in various Abraham biological and medical equations. the results can be applied to predict the properties in biological and medical research which the data is difficult to measure. the Abraham model will predict ...
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Fabrication and light scattering study of multi-responsive nanostructured hydrogels and water-soluble polymers.

Fabrication and light scattering study of multi-responsive nanostructured hydrogels and water-soluble polymers.

Date: December 2003
Creator: Xia, Xiaohu
Description: Monodispersed microgels composed of poly-acrylic acid (PAAc) and poly(N-isopropylacrylamide) (PNIPAM) interpenetrating networks were synthesized by 2-step method with first preparing PNIPAM microgel and then polymerizing acrylic acid that interpenetrates into the PNIPAM network. The semi-dilute aqueous solutions of the PNIPAM-PAAc IPN microgels exhibit an inverse thermo-reversible gelation. Furthermore, IPN microgels undergo the reversible volume phase transitions in response to both pH and temperature changes associated to PAAc and PNIPAM, respectively. Three applications based on this novel hydrogel system are presented: a rich phase diagram that opens a door for fundamental study of phase behavior of colloidal systems, a thermally induced viscosity change, and in situ hydrogel formation for controlled drug release. Clay-polymer hydrogel composites have been synthesized based on PNIPAM gels containing 0.25 to 4 wt% of the expandable smectic clay Na-montmorillonite layered silicates (Na-MLS). For Na-MLS concentrations ranging from 2.0 to 3.2 wt%, the composite gels have larger swelling ratio and stronger mechanical strength than those for a pure PNIPAM. The presence of Na-MLS does not affect the value of the lower critical solution temperature (LCST) of the PNIPAM. Surfactant-free hydroxypropyl cellulose (HPC) microgels have been synthesized in salt solution. In a narrow sodium chloride concentration range from 1.3 ...
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FTIR-ATR Characterization of Hydrogel, Polymer Films, Protein Immobilization and Benzotriazole Adsorption on Copper Surface

FTIR-ATR Characterization of Hydrogel, Polymer Films, Protein Immobilization and Benzotriazole Adsorption on Copper Surface

Date: December 2007
Creator: Pillai, Karthikeyan
Description: Plasma polymerization techniques were used to synthesize and deposit hydrogel on silicon (Si) substrate. Hydrogel is a network of polymer chains that are water-insoluble and has a high degree of flexibility. The various fields of applications of hydrogel include drug release, biosensors and tissue engineering etc. Hydrogel synthesized from different monomers possess a common property of moisture absorption. In this work two monomers were used namely 1-amino-2-propanol (1A2P) and 2(ethylamino)ethanol (2EAE) to produce polymer films deposited on Si ATR crystal. Their moisture uptake property was tested using FTIR-ATR technique. This was evident by the decrease in -OH band in increasing N2 purging time of the films. Secondly, two monomer compounds namely vinyl acetic acid and glycidyl methacrylate which have both amine and carboxylic groups are used as solid surface for the immobilization of bovine serum albumin (BSA). Pulsed plasma polymerization was used to polymerize these monomers with different duty cycles. Initial works in this field were all about protein surface adsorption. But more recently, the emphasis is on covalent bonding of protein on to the surface. This immobilization of protein on solid surface has a lot of applications in the field of biochemical studies. The polymerization of vinyl acetic acid ...
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Fundamental Studies of Copper Corrosion in Interconnect Fabrication Process and Spectroscopic Investigation of Low-k Structures

Fundamental Studies of Copper Corrosion in Interconnect Fabrication Process and Spectroscopic Investigation of Low-k Structures

Date: December 2015
Creator: Goswami, Arindom
Description: In the first part of this dissertation, copper bimetallic corrosion and its inhibition in cleaning processes involved in interconnect fabrication is explored. In microelectronics fabrication, post chemical mechanical polishing (CMP) cleaning is required to remove organic contaminants and particles left on copper interconnects after the CMP process. Use of cleaning solutions, however, causes serious reliability issues due to corrosion and recession of the interconnects. In this study, different azole compounds are explored and pyrazole is found out to be a potentially superior Cu corrosion inhibitor, compared to the most widely used benzotriazole (BTA), for tetramethyl ammonium hydroxide (TMAH)-based post CMP cleaning solutions at pH 14. Micropattern corrosion screening results and electrochemical impedance spectroscopy (EIS) revealed that 1 mM Pyrazole in 8 wt% TMAH solution inhibits Cu corrosion more effectively than 10 mM benzotriazole (BTA) under same conditions. Moreover, water contact angle measurement results also showed that Pyrazole-treated Cu surfaces are relatively hydrophilic compared to those treated with BTA/TMAH. X-ray photoelectron spectroscopy (XPS) analysis supports Cu-Pyrazole complex formation on the Cu surface. Overall Cu corrosion rate in TMAH-based highly alkaline post CMP cleaning solution is shown to be considerably reduced to less than 1Å/min by addition of 1 mM Pyrazole. In ...
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Hydrogen terminated silicon surfaces: Development of sensors to detect metallic contaminants and stability studies under different environments

Hydrogen terminated silicon surfaces: Development of sensors to detect metallic contaminants and stability studies under different environments

Date: August 2002
Creator: Ponnuswamy, Thomas Anand
Description: Hydrogen terminated silicon surfaces have been utilized to develop sensors for semiconductor and environmental applications. The interaction of these surfaces with different environments has also been studied in detail. The sensor assembly relevant to the semiconductor industry utilizes a silicon-based sensor to detect trace levels of metallic contaminants in hydrofluoric acid. The sensor performance with respect to two non-contaminating reference electrode systems was evaluated. In the first case, conductive diamond was used as a reference electrode. In the second case, a dual silicon electrode system was used with one of the silicon-based electrodes protected with an anion permeable membrane behaving as the quasi reference electrode. Though both systems could function well as a suitable reference system, the dual silicon electrode design showed greater compatibility for the on-line detection of metallic impurities in HF etching baths. The silicon-based sensor assembly was able to detect parts- per-trillion to parts-per-billion levels of metal ion impurities in HF. The sensor assembly developed for the environmental application makes use of a novel method for the detection of Ni2+using attenuated total reflection (ATR) technique. The nickel infrared sensor was prepared on a silicon ATR crystal uniformly coated by a 1.5 micron Nafion film embedded with dimethylglyoxime ...
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Interfacial Electrochemistry and Surface Characterization: Hydrogen Terminated Silicon, Electrolessly Deposited Palladium & Platinum on Pyrolyzed Photoresist Films and Electrodeposited Copper on Iridium

Interfacial Electrochemistry and Surface Characterization: Hydrogen Terminated Silicon, Electrolessly Deposited Palladium & Platinum on Pyrolyzed Photoresist Films and Electrodeposited Copper on Iridium

Date: December 2003
Creator: Chan, Raymond
Description: Hydrogen terminated silicon surfaces play an important role in the integrated circuit (IC) industry. Ultra-pure water is extensively used for the cleaning and surface preparation of silicon surfaces. This work studies the effects of ultra-pure water on hydrogen passivated silicon surfaces in a short time frame of 120 minutes using fourier transform infrared spectroscopy – attenuated total reflection techniques. Varying conditions of ultra-pure water are used. This includes dissolved oxygen poor media after nitrogen bubbling and equilibration under nitrogen atmosphere, as well as metal contaminated solutions. Both microscopically rough and ideal monohydride terminated surfaces are examined. Hydrogen terminated silicon is also used as the sensing electrode for a potentiometric sensor for ultra-trace amounts of metal contaminants. Previous studies show the use of this potentiometric electrode sensor in hydrofluoric acid solution. This work is able to shows sensor function in ultra-pure water media without the need for further addition of hydrofluoric acid. This is considered a boon for the sensor due to the hazardous nature of hydrofluoric acid. Thin carbon films can be formed by spin coating photoresist onto silicon substrates and pyrolyzing at 1000 degrees C under reducing conditions. This work also shows that the electroless deposition of palladium and ...
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Interfacial Electrochemistry of Metal Nanoparticles Formation on Diamond and Copper Electroplating on Ruthenium Surface

Interfacial Electrochemistry of Metal Nanoparticles Formation on Diamond and Copper Electroplating on Ruthenium Surface

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Date: May 2003
Creator: Arunagiri, Tiruchirapalli Natarajan
Description: An extremely facile and novel method called spontaneous deposition, to deposit noble metal nanoparticles on a most stable form of carbon (C) i.e. diamond is presented. Nanometer sized particles of such metals as platinum (Pt), palladium (Pd), gold (Au), copper (Cu) and silver (Ag) could be deposited on boron-doped (B-doped) polycrystalline diamond films grown on silicon (Si) substrates, by simply immersing the diamond/Si sample in hydrofluoric acid (HF) solution containing ions of the corresponding metal. The electrons for the reduction of metal ions came from the Si back substrate. The diamond/Si interfacial ohmic contact was of paramount importance to the observation of the spontaneous deposition process. The metal/diamond (M/C) surfaces were investigated using Raman spectroscopy, scanning electron microscopy (SEM), x-ray photoelectron spectroscopy (XPS) and x-ray diffractometry (XRD). The morphology (i.e. size and distribution) of metal nanoparticles deposits could be controlled by adjusting the metal ion concentration, HF concentration and deposition time. XRD data indicate the presence of textured and strained crystal lattices of Pd for different Pd/C morphologies, which seem to influence the electrocatalytic oxidation of formaldehyde (HCHO). The sensitivity of electrocatalytic reactions to surface crystal structure implies that M/C could be fabricated for specific electrocatalytic applications. The research also ...
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Interfacial Study of Copper Electrodeposition with the Electrochemical Quartz Crystal Microbalance (EQCM)

Interfacial Study of Copper Electrodeposition with the Electrochemical Quartz Crystal Microbalance (EQCM)

Date: May 2005
Creator: Ojeda Mota, Oscar Ulises
Description: The electrochemical quartz crystal microbalance (EQCM) has been proven an effective mean of monitoring up to nano-scale mass changes related to electrode potential variations at its surface. The principles of operation are based on the converse piezoelectric response of quartz crystals to mass variations on the crystal surface. In this work, principles and operations of the EQCM and piezo-electrodes are discussed. A conductive oxide, ruthenium oxide (RuO2) is a promising material to be used as a diffusion barrier for metal interconnects. Characterization of copper underpotential deposition (UPD) on ruthenium and RuO2 electrodes by means of electrochemical methods and other spectroscopic methods is presented. Copper electrodeposition in platinum and ruthenium substrates is investigated at pH values higher than zero. In pH=5 solutions, the rise in local pH caused by the reduction of oxygen leads to the formation of a precipitate, characterized as posnjakite or basic copper sulfate by means of X-ray electron spectroscopy and X-ray diffraction. The mechanism of formation is studied by means of the EQCM, presenting this technique as a powerful in-situ sensing device.
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Metal Oxide Reactions in Complex Environments: High Electric Fields and Pressures above Ultrahigh Vacuum

Metal Oxide Reactions in Complex Environments: High Electric Fields and Pressures above Ultrahigh Vacuum

Date: August 2005
Creator: Qin, Feili
Description: Metal oxide reactions at metal oxide surfaces or at metal-metal oxide interfaces are of exceptional significance in areas such as catalysis, micro- and nanoelectronics, chemical sensors, and catalysis. Such reactions are frequently complicated by the presence of high electric fields and/or H2O-containing environments. The focus of this research was to understand (1) the iron oxide growth mechanism on Fe(111) at 300 K and 500 K together with the effect of high electric fields on these iron oxide films, and (2) the growth of alumina films on two faces of Ni3Al single crystal and the interaction of the resulting films with water vapor under non-UHV conditions. These studies were conducted with AES, LEED, and STM. XPS was also employed in the second study. Oxidation of Fe(111) at 300 K resulted in the formation of Fe2O3 and Fe3O4. The substrate is uniformly covered with an oxide film with relatively small oxide islands, i.e. 5-15 nm in width. At 500 K, Fe3O4 is the predominant oxide phase formed, and the growth of oxide is not uniform, but occurs as large islands (100 - 300 nm in width) interspersed with patches of uncovered substrate. Under the stress of STM induced high electric fields, dielectric ...
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Methods Development for Simultaneous Determination of Anions and Cations by Ion Chromatography

Methods Development for Simultaneous Determination of Anions and Cations by Ion Chromatography

Date: May 1987
Creator: Jones, Vonda K. (Vonda Kaye)
Description: The problem with which this research is concerned is the determination of inorganic anions and cations with single injection ion chromatography. Direct detection of the separated analyte ions occurs after the analyte ions have passed through ion-exchange resins where they are separated according to their affinity for the ion-exchange resin active sites. The techniques involve the use of essentially a non-suppressed ion chromatographic system followed by a suppressed ion chromatographic system. With this system it is possible to accomplish both qualitative and quantitative determinations.
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Model Development for the Catalytic Calcination of Calcium Carbonate

Model Development for the Catalytic Calcination of Calcium Carbonate

Date: December 1987
Creator: Huang, Jin-Mo
Description: Lime is one of the largest manufactured chemicals in the United States. The conversion of calcium carbonate into calcium oxide is an endothermic reaction and requires approximately two to four times the theoretical quantity of energy predicted from thermodynamic analysis. With the skyrocketing costs of fossil fuels, how to decrease the energy consumption in the calcination process has become a very important problem in the lime industry. In the present study, many chemicals including lithium carbonate, sodium carbonate, potassium carbonate, lithium chloride, magnesium chloride, and calcium chloride have been proved to be the catalysts to enhance the calcination rate of calcium carbonate. By mixing these chemicals with pure calcium carbonate, these additives can increase the calcination rate of calcium carbonate at constant temperatures; also, they can complete the calcination of calcium carbonate at relatively low temperatures. As a result, the energy required for the calcination of calcium carbonate can be decreased. The present study has aimed at developing a physical model, which is called the extended shell model, to explain the results of the catalytic calcination. In this model, heat transfer and mass transfer are two main factors used to predict the calcination rate of calcium carbonate. By using the ...
Contributing Partner: UNT Libraries
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