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Ultrasonic attenuation in superconducting molybdenum-rhenium alloys.

Investigation of longitudinal sound attenuation in superconducting Mo-Re alloys as a function of temperature, magnetic field, and frequency. Evaporated thin film CdS transducers were used for the measurements at frequencies up to 3 GHz. The normal state attenuation coefficient was found to be proportional to the square of frequency over this frequency range. Measurements in zero magnetic field yielded a value of the energy gap parameter close to the threshold value of 3.56 kTc, appropriate to a weakly coupled dirty limit superconductor.

Ashkin, M.↗

Effect of Substrate Surface Finish on the Lubrication and Failure Mechanisms of Molybdenum Disulfide Films

An optical microscope was used to study the lubrication and failure mechanisms of rubbed (burnished) MoS2 films applied to three substrate surface finishes - polished, sanded, and sandblasted - as a function of sliding distance. The lubrication mechanism was the plastic flow of thin films of MoS2 between flat plateaus on the rider and on the metallic substrate. If the substrates were rough, flat plateaus were created during 'run in' and the MoS2 flowed across them. Wear life was extended by increasing surface roughness since valleys in the roughened substrate served as reservoirs for MoS2 and a deposit site for wear debris. In moist air, the failure mechanism was the transformation of metallic colored MoS2 films to a black, powdery material that was found by X ray diffraction to consist primarily of alpha iron and MoO3 powders. In dry argon, the failure mechanism was the gradual depletion of the MoS2 film from the contact region by transverse flow. Analysis of the wear debris on the wear track at failure showed it consisted mainly of alpha iron and some residual MoS2. No molybdenum oxides were found.

Fusaro, R. L.↗

Effect of substrate surface finish on the lubrication and failure mechanisms of molybdenum disulfide films

An optical microscope was used to study the lubrication and failure mechanisms of rubbed (burnished) MoS2 films applied to three substrate surface finishes - polished, sanded, and sandblasted - as a function of sliding distance. The lubrication mechanism was the plastic flow of thin films of MoS2 between flat plateaus on the rider and on the metallic substrate. If the substrate was rough, flat plateaus were created during 'run-in' and the MoS2 flowed across them. Wear life was extended by increasing surface roughness since valleys in the roughened substrate served as reservoirs for MoS2 and a deposit site for wear debris. In moist air, the failure mechanism was the transformation of metallic-colored MoS2 films to a black, powdery material that was found by X-ray diffraction to consist primarily of alpha-iron and MoO3 powders. In dry argon, the failure mechanism was the gradual depletion of the MoS2 film from the contact region by transverse flow. Analysis of the wear debris on the wear track at failure showed it consisted mainly of alpha-iron and some residual MoS2. No molybdenum oxides were found.

Fusaro, R. L.↗

Lubrication and failure mechanisms of molybdenum disulfide films. 2: Effect of substrate roughness

An optical microscope was used to study the lubrication and failure mechanisms of rubbed MoS2 films applied to three substrate surface finishes; polished, sanded, and sandblasted as a function of sliding distance. The lubrication mechanism was the plastic flow of thin films of MoS2 between flat plateaus on the rider and on the metallic substrate. If the substrate was rough, flat plateaus were created during run-in and the MoS2 flowed across them. Wear life was extended by increasing surface roughness since valleys in the roughened substrate served as reservoirs for MoS2 and as deposit sites for wear debris. In moist air the failure mechanism was the transformation of metallic colored MoS2 films to a black, powdery material that was found by X-ray diffraction to be alpha iron, MoO3, and possibly FeMoO3. In dry argon the failure mechanism was the gradual depletion of MoS2 from the contact region by transverse flow, and the wear debris on the track at failure was alpha iron, residual MoS2, and possibly FeS.

Fusaro, R. L.↗

Thin Film Solar Cells: Organic, Inorganic and Hybrid

Thin film solar cells are an important developing resource for hundreds of applications including space travel. In addition to being more cost effective than traditional single crystal silicon cells, thin film multi-crystaline cells are plastic and light weight. The plasticity of the cells allows for whole solar panels to be rolled out from reams. Organic layers are being investigated in order to increase the efficiency of the cells to create an organic / inorganic hybrid cell. The main focus of the group is a thin film inorganic cell made with the absorber CuInS2. So far the group has been successful in creating the layer from a single-source precursor. They also use a unique method of film deposition called chemical vapor deposition for this. The general makeup of the cell is a molybdenum back contact with the CuInS2 layer, then CdS, ZnO and aluminum top contacts. While working cells have been produced, the efficiency so far has been low. Along with quantum dot fabrication the side project of this that is currently being studied is adding a polymer layer to increase efficiency. The polymer that we are using is P3OT (Poly(3-octylthiopene-2,5-diyll), retroregular). Before (and if) it is added to the cell, it must be understood in itself. To do this simple diodes are being constructed to begin to look at its behavior. The P3OT is spin coated onto indium tin oxide and silver or aluminum contacts are added. This method is being studied in order to find the optimal thickness of the layer as well as other important considerations that may later affect the composition of the finished solar cell. Because the sun is the most abundant renewable, energy source that we have, it is important to learn how to harness that energy and begin to move away from our other depleted non-renewable energy sources. While traditional silicon cells currently create electricity at relatively high efficiencies, they have drawbacks such as weight and rigidness that make them unattractive especially for space applications. Thin film photovoltaics have the potential to alleviate these problems and create a cheap and efficient way to harness the power of the sun.

Dankovich, John↗

Lubricating properties of molybdenum disulfide. Part 3: Performance of molybdenum disulfide-containing oils in fluid lubrication

The lubricating properties of a straight mineral oil with and without MoS2 powder were studied. Bearing testers of thrust-collar type and of journal bearing type were used for thin- and fluid-film conditions, respectively. The effectiveness of the MoS2 powder in the oil differed depending on the conditions of the rubbing surfaces. For fluid film conditions, considerable effects of the MoS2 were observed, in contrast to the thin-film cases. The addition of MoS2 powder was effective only when the lubricant film was formed between surfaces thickly enough to allow the inflow of MoS2 particles.

Soda, Norimune↗

Auger spectroscopy analysis of lubrication with zinc dialkyldithiophosphate of several metal combinations in sliding contact

Sliding friction experiments were conducted with aluminum and other riders rubbing on disks of various elemental metals in the presence of a thin film of zinc dialkyldithiophosphate (ZDP). Auger emission spectroscopy was used to in situ monitor the changes in surface chemistry with rubbing under various loads. The metal disks examined included iron, titanium, rhodium, tungsten, molybdenum, and copper. For equivalent films of ZDP the film is a more effective lubricant for some metals than it is for others. The important active element in the compound varies with the metal lubricated and is a function of metal chemistry. The zinc in the ZDP is susceptible to electron beam induced desorption.

Buckley, D. H.↗

Bearing endurance tests in vacuum for sputtered molybdenum disulfide films

Angular-contact, 440C stainless steel, ball bearings with sputtered MoS2 films 0.0000006 x 10-7m (6000 A) thick were evaluated in a vacuum bearing chamber (1750 rpm, 137.9-N- (31-lbf-) thrust load) for endurance. Two types of sputtered films were evaluated: (1) MOS2 sputtered directly onto bearing components, and (2) a thin 0.0000001 x 10-7m (1000 A) underlayer of Cr3Si2 subsequently sputtered with MoS2. Bearing test evaluations in vacuum showed that endurance lives of more than 1000 hours (105,000,000 cycles) were obtained with bearings (cage, races, and balls) directly sputtered with MoS2. The same endurance lives were also obtained when only the races and cage were sputtered with an underlayer of Cr3Si2 and subsequently with MoS2.

Spalvins, T.↗

Alkali metal-refractory metal biphase electrode for AMTEC

An electrode having increased output with slower degradation is formed of a film applied to a beta-alumina solid electrolyte (BASE). The film comprises a refractory first metal M.sup.1 such as a platinum group metal, suitably platinum or rhodium, capable of forming a liquid or a strong surface adsorption phase with sodium at the operating temperature of an alkali metal thermoelectric converter (AMTEC) and a second refractory metal insoluble in sodium or the NaM.sup.1 liquid phase such as a Group IVB, VB or VIB metal, suitably tungsten, molybdenum, tantalum or niobium. The liquid phase or surface film provides fast transport through the electrode while the insoluble refractory metal provides a structural matrix for the electrode during operation. A trilayer structure that is stable and not subject to deadhesion comprises a first, thin layer of tungsten, an intermediate co-deposited layer of tungsten-platinum and a thin surface layer of platinum.

Williams, Roger M.↗

Lubrication and failure mechanisms of molybdenum disulfide films. 1: Effect of atmosphere

Friction, wear, and wear lives of rubbed molybdenum disulfide (MoS2 films applied to sanded 440C HT steel surfaces were evaluated in moist air, dry air, and dry argon. Optical microscope observations were made as a function of sliding distance to determine the effect of moisture and oxygen on the lubricating and failure mechanisms of MoS2 films. In general, the lubrication process consisted of the formation of a thin, metallic colored, coalesced film of MoS2 that flowed between the surfaces in relative motion. In air, failure was due to the transformation of the metallic colored, coalesced films to a black, powdery material. Water in the air appeared to accelerate the transformation rate. In argon, no transformation of MoS2 was observed with the microscope, but cracking and spalling of the coalesced film occurred and resulted in the gradual depletion of the film.

Fusaro, R. L.↗

A Comparison of the Lubricating Mechanisms of Graphite Fluoride and Molybdenum Disulfide Films

A microscopic study of 440C steel sliding surfaces lubricated by graphite fluoride or molybdenum disulfide solid lubricant rubbed films was conducted. The sliding surfaces, along with the friction, wear, and wear life were observed as a function of the number of sliding revolutions in three different atmospheres: moist air, dry air, or dry argon. In general, the lubricating mechanisms of the two solid lubricants were found to be relatively similar; that is, a dynamic, thin, layer-like film was formed between the two metallic surfaces. The mechanisms of failure were found to be somewhat different, however. Failure of MoS2 films was very dependent on atmospheric degradation, while that of graphite fluoride films was more dependent on flow of the lubricant film out of the contact zone.

Fusaro, R. L.↗

Holographic fabrication of gratings in metal substrates

A program for investigating the grain enlargement resulting from the laser recrystallization of a thin gallium arsenide film on a patterned substrate, a technique known as graphoepitaxy was evaluated. More specifically, the effects of recrystallizing an uncapped gallium arsenide film using a continuous wave neodymium YAG laser operating at 1.06 microns were studied. In an effort to minimize arsenic loss from the film, the specimens were held in an arsine atmosphere during recrystallization. Two methods for fabricating patterned substrates were developed, one using reactive ion etching of a molybdenum film on both sapphire and silicon substates and another by preferential wet etching of a silicon substrate onto which a film of molybdenum was subsequently deposited.

Fletcher, R. M.↗

A comparison of the lubricating mechanisms of graphite fluoride and molybdenum disulfide films

A microscopic study of 440 C steel sliding surfaces lubricated by graphite fluoride or molybdenum disulfide solid lubricant rubbed films was conducted. The sliding surfaces, along with the friction, wear, and wear life were observed as a function of the number of sliding revolutions in three different atmospheres: moist air (10,000 ppm H2O), dry air (less than 20 ppm H2O), or dry argon (less than 20 ppm H2O). In general, the lubricating mechanisms of the two solid lubricants were found to be relatively similar; that is, a dynamic, thin, layer-like film (which sheared on relative motion) was formed between the two metallic surfaces. The mechanisms of failure were found to be somewhat different, however. Failure of MoS2 films was very dependent on atmospheric degradation, while that of graphite fluoride films was more dependent on flow of the lubricant film out of the contact zone

Fusaro, R. L.↗

Stuffed MO layer as a diffusion barrier in metallizations for high temperature electronics

Auger electron spectroscopy was employed to characterize the diffusion barrier properties of molybdenum in the CrSi2/Mo/Au metallization system. The barrier action of Mo was demonstrated to persist even after 2000 hours annealing time at 300 C in a nitrogen ambient. At 340 C annealing temperature, however, rapid interdiffusion was observed to have occurred between the various metal layers after only 261 hours. The presence of controlled amounts of oxygen in the Mo layer is believed to be responsible for suppressing the short circuit interdiffusion between the thin film layers. Above 340 C, its is believed that the increase in the oxygen mobility led to deterioration of its stuffing action, resulting in the rapid interdiffusion of the thin film layers along grain boundaries.

Boah, J. K.↗

Advances in Solid State Joining of Haynes 230 High Temperature Alloy

The J-2X engine is being designed for NASA s new class of crew and launch vehicles, the Ares I and Ares V. The J-2X is a LOX/Hydrogen upper stage engine with 294,000 lbs of thrust and a minimum Isp of 448 seconds. As part of the design criteria to meet the performance requirements a large film-cooled nozzle extension is being designed to further expand the hot gases and increases the specific impulse. The nozzle extension is designed using Haynes 230, a nickel-chromium-tungsten-molybdenum superalloy. The alloy was selected for its high strength at elevated temperatures and resistance to hydrogen embrittlement. The nozzle extension is manufactured from Haynes 230 plate spun-forged to form the contour and chemically-milled pockets for weight reduction. Currently fusion welding is being evaluated for joining the panels which are then mechanically etched and thinned to required dimensions for the nozzle extension blank. This blank is then spun formed into the parabolic geometry required for the nozzle. After forming the nozzle extension, weight reduction pockets are chemically milled into the nozzle. Fusion welding of Haynes results in columnar grains which are prone to hot cracking during forming processes. This restricts the ability to use spin forging to produce the nozzle contour. Solid state joining processes are being pursued as an alternative process to produce a structure more amenable to spin forming. Solid state processes have been shown to produce a refined grain structure within the joint regions as illustrated in Figure 1. Solid state joining processes include friction stir welding (FSW) and a patented modification termed thermal stir welding (TSW). The configuration of TSWing utilizes an induction coil to preheat the material minimizing the burden on the weld tool extending its life. This provides the ability to precisely select and control the temperature. The work presented in this presentation investigates the feasibility of joining the Haynes 230 alloy using the solid state welding processes of FSW and TSW. Process descriptions and attributes of each weld process will be presented. Weld process set-up and welding techniques will be discussed leading to the challenges experienced in joining the superalloy. Mechanical property data will also be presented.

Ding, R. Jeffrey↗

X-Ray photoelectron spectroscopy study of radiofrequency-sputtered titanium, carbide, molybdenum carbide, and titanium boride coatings and their friction properties

Radiofrequency sputtered coatings of titanium carbide, molybdenum carbide and titanium boride were tested as wear resistant coatings on stainless steel in a pin on disk apparatus. X-ray photoelectron spectroscopy (XPS) was used to analyze the sputtered films with regard to both bulk and interface composition in order to obtain maximum film performance. Significant improvements in friction behavior were obtained when properly biased films were deposited on deliberately preoxidized substrates. XPS depth profile data showed thick graded interfaces for bias deposited films even when adherence was poor. The addition of 10 percent hydrogen to the sputtering gas produced coatings with thin poorly adherent interfaces. Results suggest that some of the common practices in the field of sputtering may be detrimental to achieving maximum adherence and optimum composition for these refractory compounds.

Brainard, W. A.↗

Lifetime studies of high power rhodium/tungsten and molybdenum electrodes for application to AMTEC (alkali metal thermal-to-electric converter)

A detailed and fundamental model for the electrochemical behavior of AMTEC electrodes is developed which can aid in interpreting the processes which occur during prolonged operation of these electrodes. Because the sintering and grain growth of metal particles is also a well-understood phenomenon, the changes in electrode performance which accompany its morphological evolution may be anticipated and modeled. The grain growth rate observed for porous Mo AMTEC electrodes is significantly higher than that predicted from surface diffusion data obtained at higher temperatures and incorporated into the grain growth model. The grain growth observed under AMTEC conditions is also somewhat higher than that measured for Mo films on BASE (beta-alumina solid electrolyte) substrates in vacuum or at similar temperatures. Results of modeling indicate that thin Mo electrodes may show significant performance degradation for extended operation (greater than 10,000 h) at higher operating temperatures (greater than 1150 K), whereas W/Rh and W/Pt electrodes are expected to show adequate performance at 1200 K for lifetimes greater than 10,000 h. It is pointed out that current collection grids and leads must consist of refractory metals such as Mo and W which do not accelerate sintering or metal migration.

Williams, R. M.↗

Analysis of Electrical Characteristics of Thin Film Photovoltaic Cells

Solar energy is the most abundant form of energy in many terrestrial and extraterrestrial environments. Often in extraterrestrial environments sunlight is the only readily available form of energy. Thus the ability to efficiently harness solar energy is one of the ultimate goals in the design of space power systems. The essential component that converts solar energy into electrical energy in a solar energy based power system is the photovoltaic cell. Traditionally, photovoltaic cells are based on a single crystal silicon absorber. While silicon is a well understood technology and yields high efficiency, there are inherent disadvantages to using single crystal materials. The requirements of weight, large planar surfaces, and high manufacturing costs make large silicon cells prohibitively expensive for use in certain applications. Because of silicon s disadvantages, there is considerable ongoing research into alternative photovoltaic technologies. In particular, thin film photovoltaic technologies exhibit a promising future in space power systems. While they are less mature than silicon, the better radiation hardness, reduced weight, ease of manufacturing, low material cost, and the ability to use virtually any exposed surface as a substrate makes thin film technologies very attractive for space applications. The research group lead by Dr. Hepp has spent several years researching copper indium disulfide as an absorber material for use in thin film photovoltaic cells. While the group has succeeded in developing a single source precursor for CuInS2 as well as a unique method of aerosol assisted chemical vapor deposition, the resulting cells have not achieved adequate efficiencies. While efficiencies of 11 % have been demonstrated with CuInS2 based cells, the cells produced by this group have shown efficiencies of approximately 1 %. Thus, current research efforts are turning towards the analysis of the individual layers of these cells, as well as the junctions between them, to determine the cause of the poor yields. As a student of electrical engineering with some material science background, my role in this research is to develop techniques for analyzing the electrical characteristics of the CuInS2 cells. My first task was to design a shadow mask to be used to place molybdenum contacts under a layer of CuInS;! in order to analyze the contact resistance between the materials. In addition, I have also analyzed evaporated aluminum top contacts and have tested various methods of increasing their thicknesses in order to decrease series resistance. More recently I have worked with other members of the research group in reviving a vertical cold-wall reactor for experimentation with CuInS2 quantum dots. As part of that project, I have improved the design for a variable frequency and pulse width square wave generator to be used in driving the precursor injection process. My task throughout the remainder of my tenure is to continue to analyze and develop tools for the analysis of electrical properties of the CuInS2 cells with the ultimate goal of discovering ways to improve the efficiency of our photovoltaic cells. Traditionally, photovoltaic cells are based on a single crystal silicon absorber. While The research group lead by Dr. Hepp has spent several years researching copper indium

Kasick, Michael P.↗