Metallurgy Commons^™

Electrochemical Characterization Of Copper Deposited On Plasma And Thermally Modified Titanium Surfaces, K. S. Teng, J. L. Delplancke, Jiangfan Zhang, T. J. O'Keefe

Electrical and Computer Engineering Faculty Research & Creative Works

Thin oxide films were grown at temperatures from 373 to 1073 K in plasma and in air on commercially pure titanium substrates. It was determined that the color, thickness, composition, phase, and polarization behavior in a copper electrolyte varied with operating conditions: temperature, oxygen partial pressure, and plasma composition. High-temperature and high oxygen partial pressure plasma produced a thick oxide film. The surface film structure transformed from TiO2 (anatase) to TiO2 (rutile) at a temperature of 600 °C. A lower oxide of the form TinO2n-1, such as Ti2O3 (which may be porous) or possibly Ti3O5, was formed on a thermally …

Electrodeposition Of Copper On Thermally Oxidized 316 L Stainless Steel Substrates, Z. Zhou, Thomas J. O'Keefe

Materials Science and Engineering Faculty Research & Creative Works

The effect of thermal oxidation of 316 L stainless steel cathode blanks used in copper electrodeposition was studied. Current and potential step experiments were performed to evaluate electrochemical changes caused by the oxidation treatments. SEM and AES were used to characterize the stainless-steel substrates and the deposited copper films. Particular emphasis was given to the initial stages of copper nucleation and growth. The copper electro crystallization process was strongly influenced by the temperature employed in oxidizing the stainless steel. Dense, uniform and fine copper nuclei were obtained on the stainless-steel substrate oxidized in air at 200°C and 300°C for 3 …

Analysis Of The Value Of The Fe Examination For The Assessment Of Student Learning In Engineering And Science Topics, John L. Watson

Materials Science and Engineering Faculty Research & Creative Works

This paper presents the results of a project, which investigated the potential of fully using previously unreleased data from the nationally normed Fundamentals of Engineering (FE) examination to assess learning in key engineering and science topics. In the past, very limited information was released by the National Council of Examiners for Engineers and Surveyors (NCEES) for the eight hour FE examination, which is composed of 150-200 questions in ten morning and five afternoon topics. For the purposes of this project the NCEES agreed to release information to the University of Missouri-Rolla (UMR) to permit the value of the FE data …

Organically Deposited Metallic Films For Device Fabrication, Thomas J. O'Keefe, M. Stroder, Matthew O'Keefe

Materials Science and Engineering Faculty Research & Creative Works

Advances in integrated circuit density, speed and complexity are dependent on lower resistance, finer line width on-chip interconnections. Methods for incorporating copper interconnects into IC fabrication processes have been developed which accomplish this objective but most of these methods use some form of blanket metal deposition that requires mechanical and/or chemical removal of excess material. To date, investigations into the selective deposition of conductor materials for device fabrication have met with limited success. A new process for selectively depositing metallic conductors using inexpensive, organic-based chemical solutions could potentially force a paradigm shift in the deposition of metals for microelectronic applications. …

Maskless, Direct Deposition Of Copper Onto Aluminum Bond Pads For Flip Chip Applications, M. Fang, Thomas J. O'Keefe, M. Stroder, W. Shih, Matthew O'Keefe, R. Strawser, D. Via

Materials Science and Engineering Faculty Research & Creative Works

Flip chip interconnection of integrated circuits (IC) for packaging applications such as direct chip attachment use Pb-Sn solders as the connection between the die and the substrate. Under bump metallization is typically used to transition from the non-solderable Al bond pad on the IC to a solderable surface such as copper using traditional blanket metal deposition, photolithography and etching procedures. In this study, we report for the first time the use of a novel process for selectively depositing adherent copper directly onto aluminum thin films, eliminating the need for adhesion promoting transition layers and additional patterning steps. Utilizing copper bearing …

Strip Casting With Fluxing Agent Applied To Casting Roll, Robert S. Williams, Ronald J. O'Malley, Richard C. Sussman

Materials Science and Engineering Faculty Research & Creative Works

A strip caster (10) for producing a continuous strip (24) includes a tundish (12) for containing a melt (14), a pair of horizontally disposed water cooled casting rolls (22) and devices (29) for electrostatically coating the outer peripheral chill surfaces (44) of the casting rolls with a powder flux material (56). The casting rolls are juxtaposed relative to one another for forming a pouting basin (18) for receiving the melt through a teeming tube (16) thereby establishing a meniscus (20) between the rolls for forming the strip. The melt is protected from the outside air by a non-oxidizing gas passed …

The Effect Of Casting Shape And Size On Solidification Time: A New Approach, Murat Tiryakioǧlu, Ergin Tiryakioǧlu, Donald R. Askeland

Materials Science and Engineering Faculty Research & Creative Works

The limitations of Chvorinov's Rule for predicting the solidification time of a casting are discussed and previous studies intended to modify Chvorinov's Rule in order to express the effect of the size and shape of castings on solidification time are reviewed. A new model that introduces a shape factor is presented that predicts the solidification times of castings as well as or better than Chvorinov's Rule, particularly for more complex shapes. The validity of the new model is compared with the conventional Chvorinov's Rule by a statistical analysis of twelve sets of data obtained from the literature.

A Positron Annihilation Study Of Rotating Beam Fatigue Damage In The Superalloy Haynes 188, D. Hoeckelman, Hollis P. Leighly

Materials Science and Engineering Faculty Research & Creative Works

No abstract provided.

Effect Of Additives On Anomalous Deposition In Zinc-Cobalt Alloy Electrogalvanizing, H. M. Wang, Thomas J. O'Keefe

Materials Science and Engineering Faculty Research & Creative Works

Alloys of Zn-Co were deposited from sulphate electrolytes containing various additives to study their influence on the anomalous behavior of the reactions. The effects of antimony, germanium and arsenic on the Zn-Co alloy composition and structure were examined. The results showed that the composition and structure of Zn-Co alloys deposited could be dramatically changed by antimony, and to a lesser extent by germanium and arsenic. A concentration of Sb(III) as low as 5 mg dm-3 increased the cobalt content by a factor of approximately 3; however, the deposit morphology was very dendritic. Germanium additions nearly doubled the cobalt content and …

Solubility Of Red Phosphorous In Lead, Sean E. Walker

Opportunities for Undergraduate Research Experience Program (OURE)

The determination of the solubility of red phosphorus in lead can be used to produce a plot of the solubility with respect to temperature and pressure. The plot is produced with experimental data, activity determination from present thermodynamic data, and compilation of the two sets of data into the semi-regular solution format. A lead-phosphorus solubility diagram is necessary to determine the amount phosphorus that will be absorbed by lead and will remain unreacted in a given process.

Characterization Of Phase Transformation Behavior In Electrolytically Produced Indium-Thallium Shape Memory Alloy Films, Chong Ho Sonu, Thomas J. O'Keefe

Materials Science and Engineering Faculty Research & Creative Works

Indium-thallium alloys in the range 15-38 at. % Tl were electrodeposited from a sulfate electrolyte by using pulsed current. The relationship between composition and phase structure of the alloys deposited was investigated with regard to the shape memory effect. To date there have been no reported experimental studies describing the electrodeposition of InTl alloys capable of undergoing such transformations. Not only did the deposited alloys exhibit the shape memory effect, but the composition-phase relationship exhibited was shown to deviate from that reported for alloys in an equilibrium condition. The results show that the temperature and the temperature interval for the …

Positron Annihilation Determination Of Damage Caused By Fatigue Cycling In The Superalloy Haynes 188, D. Hoeckelman, Hollis P. Leighly

Materials Science and Engineering Faculty Research & Creative Works

No abstract provided.

Density Changes During Isothermal Annealing Of A Quenched Pb–7.45 At% Sn Alloy, Hollis P. Leighly, A. Belaidi

Materials Science and Engineering Faculty Research & Creative Works

The increase in density of a Pb–7.45 at% Sn alloy annealed at 150, 165, 180, and 195 °C and quenched at 20, 21.5, 23, 25, and 30 °C is measured isothermally. This increase in density accompanies the formation of the Sn‐rich phase precipitating as a function of time at the quenching temperature. The quenching is rapid enough to retain some vacancies at equilibrium at the annealing temperature. These vacancies accelerate the early stages of precipitation. The change in density versus time obeys the kinetic law allowing the determination of the reaction rate constant for several annealing and quenching conditions. Copyright …

A Study Of High Temperature Oxidation Resistance Of Plasma Treated Nb-Ti-Al Alloys, Roderick R. Rowland

Opportunities for Undergraduate Research Experience Program (OURE)

The effect of plasma treatment on the oxidation behavior of Ti-22Al-27Nb (atomic%) has been studied. The alloy, cast as an ingot by triple VAR and worked to a billet, was cut into smaller samples and oxidation plasma pre-treated. Oxidation plasma pre-treatments were conducted at four ambient temperatures: 25°C, 200°C, 400°C, and 500°C. Both the untreated and plasma pre-treated samples were oxidized at 700°C and 1000°C for one hour, in a muffle furnace. The oxidation behavior of the samples led us to do an extended oxidation of 100 hours at 700°C. The 200°C plasma pre-treated samples showed a definite leveling out …

Solidification Modeling Of Centrifugal Casting, Stephen M. Lane

Opportunities for Undergraduate Research Experience Program (OURE)

This paper describes the methodology used to estimate the solidification time of castings produced by processes in which normal thermal analysis cannot be used, such as centrifugal casting. This methodology utilizes the relationship between microstructure, in particular secondary dendrite arm spacing (SDAS), and freezing time. Using this method it is shown that position within the casting and casting geometry affect the SDAS and freezing time. However, the SDAS did not vary across the wall section due to differences in filling pattern compared to sand casting. Further research is necessary to determine filling pattern effects on microstructure.

Electrochemical Technique For Evaluating Surface Area Of A Treated Copper Foil, Gregory Lea

Opportunities for Undergraduate Research Experience Program (OURE)

In order to increase the strength of copper foil bonded to a polymeric substrate material, a dendritic layer is electrodeposited onto the foil. Treating the foil in this manner causes its surface to be rough and porous, thus providing for better penetration of the adhesive and a greater surface area for bonding. The process is particularly helpful in the manufacturing of printed circuit cards, due to the added bond strength which greatly enhances the durability of the printed circuit cards.

The Influence Of Matrix Microstructure, G. M. Vyletel, J. E. Allison, David C. Van Aken

Materials Science and Engineering Faculty Research & Creative Works

The low-cycle and high-cycle fatigue behavior and cyclic response of naturally aged and artificially aged 2219/TiC/15p and unreinforced 2219 Al were investigated utilizing plastic strain-controlled and stress-controlled testing. The cyclic response of both the reinforced and un-reinforced materials was similar for all plastic strain amplitudes tested except that the saturation stress level for the composite was always greater than that of the unreinforced material. The cyclic response of the naturally aged materials exhibited cyclic hardening and, in some cases, cyclic softening, while the cyclic response for the artificially aged materials showed no evidence of either cyclic hardening or softening. The …

A Study Of Fatigue Failure In Superalloys Using Positron Annihilation, D. Hoeckelman, Hollis P. Leighly

Materials Science and Engineering Faculty Research & Creative Works

This study shows there are significant changes occurring in the open volume defect concentration during fatigue cycling as measured by the S parameter. These changes are dependent upon the stress ratio, R = σmin/σmax, the maximum stress, σmax, and the number of fatigue cycles. The decline in the S parameter is due to the elimination of the residual vacancies. This decline is followed by an increase due to the generation of dislocations and the formation of small microcracks. This is followed by a decline in the S parameter due to growth of the microcracks ultimately leading to failure. Copyright © …

Galvanic Stripping Of Fe⁺³ And Pb⁺² Ions And Dissolution Of Metallic Fe, Zn, Pb And Cd Using Di(2-Ethylhexyl)Phosphoric Acid, Luis Miguel Chia Aquije

Doctoral Dissertations

"Two systems were evaluated using the principles of the galvanic stripping process. One of them, the removal of Pb⁺² ions from di-2(ethylhexyl) phosphoric acid (D2EHPA) was performed using metallic zinc. The other, the removal of Fe⁺³ ions from D2EHPA used metallic iron as reductant and was performed simultaneously with the organic phase using a slightly acidic aqueous solution of hydrochloric acid. In addition, the dissolution of metallic zinc, iron, lead, and cadmium in D2EHPA was studied in order to better understand the anodic step in the mechanism of the galvanic stripping process.

Increased temperature was found to dramatically …

Electrochemical Evaluation Of The Adherence Of Zinc To Aluminum Cathodes, Jang Sop Han, Thomas J. O'Keefe

Materials Science and Engineering Faculty Research & Creative Works

Excess fluoride ions in zinc electrolyte are known to cause problems with the removal of electrowon zinc from aluminum blanks. The mechanisms responsible for this undesirable adherence were studied. Acid zinc sulfate electrolyte similar to that employed in zinc electrowinning was used. Using electrolyte containing various fluoride ion concentrations, the initial nucleation and growth morphology of zinc and the aluminum electrode surface were examined using scanning electron microscopy. Electrochemical tests were also carried out in various solutions to obtain a better understanding of the polarization behavior of the system. © 1992.

The Effect Of Additives On The Nucleation And Growth Of Copper Onto Stainless Steel Cathodes, M. Sun, Thomas J. O'Keefe

Materials Science and Engineering Faculty Research & Creative Works

A potentiostatic technique has been used to study the effects of chloride ion, glue, and thiourea on the initial electrodeposition of copper. A stainless steel (AISI 304) rotating disc electrode (RDE) with an electrolyte containing 40 g/1 Cu²⁺ and 180 g/1 H₂SO₄ at 40 °C was employed. The current transients from the potential step measurements for the additive-free electrolyte could be fitted to a model that assumed progressive nucleation followed by growth of three-dimensional (3-D) centers under diffusion control. The growth mechanism and the type of nuclei were also confirmed by scanning electron microscopy (SEM) of …

The Degradation Of Aluminium Cathodes By Fluoride Ion During Zinc Electrowinning, J. S. Han, Thomas J. O'Keefe

Materials Science and Engineering Faculty Research & Creative Works

The influence of fluoride ions on aluminum cathode surface degradation during zinc electrowinning has been studied. Electrolyte with a composition similar to that employed in plant operations has been used. A direct correlation is shown between the electrolyte fluoride content and the number of deposition cycles possible before zinc removal becomes difficult. The role of initial nucleation and starting electrode morphology is discussed in terms of the degree of adherence observed. Electrochemical tests have also been made on the electrodes at various stages of the process in an attempt to gain a better fundamental understanding of the mechanisms responsible for …

Stimulation Of Amorphizing Reactions In Co-Si Multi-Layers, Jeanne K. Jackson

Opportunities for Undergraduate Research Experience Program (OURE)

Co-Si multi-layer specimens do not normally amorphize. To possibly stimulate amorphization, Ti was added by evaporation and the specimens were annealed at 300 and 400 degrees Celsius. The results showed that amorphization occurred at 400 degrees Celsius in the presence of Ti, but did not occur at 300 degrees Celsius. Further research would be necessary to conclude whether the amorphization was stimulated by the addition of Ti or the temperature increase.

Effect Of Ultrasound On Acidified Brine Leaching Of Double-Kiln Treated Eaf Dust, J. A. Barrera-Godinez, Thomas J. O'Keefe, Johh L. Watson

Materials Science and Engineering Faculty Research & Creative Works

The U.S. steel industry produces approximately 500,000 tons/year of electric arc furnace (EAF) dust, which is classified as a hazardous waste. Increasing disposal costs of these dusts have encouraged studies to investigate treatment processes to render the material non-hazardous, and to possibly recover metal values. This research project was designed to examine the hydrometallurgical recovery of zinc from EAF dusts that have been treated by a double kiln fuming process. The test work consisted essentially of acidified brine leaching of the pelletized calcine to determine the influence of traditional conditions, such as acid concentration, temperature and agitation, plus the application …

Sme Annual Meeting. Phoenix, Usa. February 22-27, 1992, Johh L. Watson

Materials Science and Engineering Faculty Research & Creative Works

No abstract provided.

Solvent Extraction Reagent Entrainment Effects On Zinc Electrowinning From Waste Oxide Leach Solutions, M. Neira, Thomas J. O'Keefe, Johh L. Watson

Materials Science and Engineering Faculty Research & Creative Works

A considerable quantity of metal-containing waste oxide is generated by the primary metal industry, and under increased environmental regulation, treatment of these wastes has become viable. Hydrometallurgical processing is often appropriate and one potential treatment process for zinc oxide wastes involves leaching the oxide with an acid, purifying by a solvent extraction operation, and recovering metallic zinc by electrowinning the purified leach solution. The purification stage is frequently critical and the introduction of a solvent extraction organic reagent into the flowsheet can be detrimental to downstream processes. The object of this study was to determine the effect of organics, entrained …

Measuring Hydrogen In Galvanized Steels, Timothy O'Hearn

Opportunities for Undergraduate Research Experience Program (OURE)

There has been much investigation in the past concerning ways to eliminate the embrittling effects of hydrogen in galvanized steel components. Such galvanized parts are used extensively in the automotive industry. One solution that is commonly used is to anneal the galvanized parts at approximately 200 degrees Celsius for 4 to 24 hours. This annealing process does restore the ductility. However, very few if any experiments have been done to measure the amount of hydrogen released and the temperature dependence of the hydrogen release. This investigation is part of an on going effort to measure the hydrogen released from galvanized …

Effects Of Sample Orientation On The Corrosion Of Zinc In Ammonium Sulfate And Sodium Hydroxide Solutions, D. Abayarathna, Edward Boyd Hale, Thomas J. O'Keefe, Y. M. Wang, D. Radovic

Physics Faculty Research & Creative Works

The corrosion and electrochemical properties of three zinc single crystal surfaces with different orientations have been investigated. In near-neutral 1 M (NH₄)₂SO₄, the corrosion rates on all three surfaces were found to be similar. However, the SEM morphologies of the corresponding corroded surfaces were markedly different from each other, but consistent with preferential attack of {1120} surfaces. In alkaline 0.5 N NaOH solution, the three sample orientations showed significantly different reactivities, with the (1120) surface exhibiting the highest reactivity and corrosion rate. Here, passivation ultimately occurred and the difference in the corrosion performance of …

Positron Study Of Defects And Diffusion Induced Grain Boundary Migration In A Pb-Sn System, A. Belaidi, Hollis P. Leighly, H. Aourag, B. Khelifa, M. Oubadi, A. Elias

Materials Science and Engineering Faculty Research & Creative Works

The Pb-Sn system discloses a remarkable effect at the intermediate α → α + β phase boundary. The observation of the sharp transient peak in the S-parameter curve which is analogous to those found in thermal capacity curves is, as far as the authors are aware, unique in such positron measurements. This effect is interpreted in terms of positron trapping in defects associated with the strains accompanying the initial stage of transformation. This short note offers a new approach to the underlying phenomenon published in J. Phys. F. Met. Phys., 12 (1982) 813 by A. Belaidi, H. P. Leighly Jr. …

Electrochemical Evaluation Of Copper Deposition With Gas Sparging, D. A. Uceda, Thomas J. O'Keefe

Materials Science and Engineering Faculty Research & Creative Works

The influence of gas sparging during copper electrolysis was studied using standard electrochemical techniques. The polarization behavior of acid copper electrolytes was determined in the presence and absence of gas sparging on vertical electrodes. Tracer ion techniques were employed to determine the effect of gas sparging and forced circulation of the electrolyte on the mass transfer characteristics of the system. In addition to the potentiodynamic scans, 3-h copper deposits were produced for morphology and orientation studies. The effect of current density and temperature on deposition were also studied. The polarization experiments have shown that a mass transfer component becomes evident …