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Electrically Conductive, Corrosion-Resistant Coatings Through Defect Chemistry for Metallic Interconnects

Description: The principal objective of this work was to develop oxidation protective coatings for metallic interconnect based on a defect chemistry approach. It was reasoned that the effectiveness of a coating is dictated by oxygen permeation kinetics; the slower the permeation kinetics, the better the protection. All protective coating materials investigated to date are either perovskites or spinels containing metals exhibiting multiple valence states (Co, Fe, Mn, Cr, etc.). As a result, all of these oxides exhibit a reasonable level of electronic conductivity; typically at least about {approx}0.05 S/cm at 800 C. For a 5 micron coating, this equates to a maximum {approx}0.025 {Omega}cm{sup 2} area specific resistance due to the coating. This suggests that the coating should be based on oxygen ion conductivity (the lower the better) and not on electronic conductivity. Measurements of ionic conductivity of prospective coating materials were conducted using Hebb-Wagner method. It was demonstrated that special precautions need to be taken to measure oxygen ion conductivity in these materials with very low oxygen vacancy concentration. A model for oxidation under a protective coating is presented. Defect chemistry based approach was developed such that by suitably doping, oxygen vacancy concentration was suppressed, thus suppressing oxygen ion transport and increasing effectiveness of the coating. For the cathode side, the best coating material identified was LaMnO{sub 3} with Ti dopant on the Mn site (LTM). It was observed that LTM is more than 20 times as effective as Mn-containing spinels. On the anode side, LaCrO3 doped with Nb on the Cr site (LNC) was the material identified. Extensive oxidation kinetics studies were conducted on metallic alloy foils with coating {approx}1 micron in thickness. From these studies, it was projected that a 5 micron coating would be sufficient to ensure 40,000 h life.
Date: December 31, 2006
Creator: Virkar, Anil V.
Partner: UNT Libraries Government Documents Department

L- and M-shell x-ray production cross sections of Nd, Gd, Ho, Yb, Au, and Pb by 25-MeV carbon and 32-MeV oxygen ions

Description: Article discussing research on L- and M-shell x-ray production cross sections of Nd, Gd, Ho, Yb, Au, and Pb by 25-MeV carbon and 32-MeV oxygen ions.
Date: October 15, 1987
Creator: Andrews, M. C.; McDaniel, Floyd Del. (Floyd Delbert), 1942-; Duggan, Jerome L.; Miller, P. D.; Pepmiller, P. L.; Krause, H. F. et al.
Partner: UNT College of Arts and Sciences

Low-energy deposition of high-strength Al(0) alloys from an ECR plasma

Description: Low-energy deposition of Al(O) alloys from an electron cyclotron resonance (ECR) plasma offers a scaleable method for the synthesis of thick, high-strength Al layers. This work compares alloy layers formed by an ECR-0{sub 2} plasma in conjunction with Al evaporation to 0-implanted Al (ion energies 25-200 keV); and it examines the effects of volume fraction of A1{sub 2}0{sub 3} phase and deposition temperature on the yield stress of the material. TEM showed the Al(O) alloys contain a dense dispersion of small {gamma}-Al{sub 2}0{sub 3} precipitates ({approximately}l nm) in a fine-grain (10-100 nm) fcc Al matrix when deposited at a temperature of {approximately}100C, similar to the microstructure for gigapascal-strength 0-implanted Al. Nanoindentation gave hardnesses for ECR films from 1.1 to 3.2 GPa, and finite-element modeling gave yield stresses up to 1.3 {plus_minus} 0.2 GPa with an elastic modulus of 66 GPa {plus_minus} 6 GPa (similar to pure bulk Al). The yield stress of a polycrystalline pure Al layer was only 0.19 {plus_minus} 0.02 GPa, which was increased to 0.87 {plus_minus} 0.15 GPa by implantation with 5 at. % 0.
Date: December 31, 1995
Creator: Barbour, J.C.; Follstaedt, D.M.; Knapp, J.A.; Myers, S.M.; Marshall, D.A. & Lad, R.J.
Partner: UNT Libraries Government Documents Department

Carbon, nitrogen, and oxygen ion implantation of stainless steel

Description: Ion implantation experiments of C, N, and O into stainless steel have been performed, with beam-line and plasma source ion implantation methods. Acceleration voltages were varied between 27 and 50 kV, with pulsed ion current densities between 1 and 10 mA/cm{sup 2}. Implanted doses ranged from 0.5 to 3 {times} 10{sup 18}cm{sup -2}, while workpiece temperatures were maintained between 25 and 800 C. Implant concentration profiles, microstructure, and surface mechanical properties of the implanted materials are reported.
Date: December 31, 1995
Creator: Rej, D.J.; Gavrilov, N.V. & Emlin, D.
Partner: UNT Libraries Government Documents Department

Lithium insertion into hollandite-type TiO{sub 2}.

Description: Hollandite-type TiO{sub 2} compounds, isostructural with {alpha}-MnO{sub 2}, have been investigated as insertion electrodes for lithium batteries. Parent materials of K{sub x}Ti{sub 8}O{sub 16} (0 < x < 2) were treated with concentrated acid to yield TiO{sub 2} products that were essentially free of potassium. Lithium can be inserted into the (2 x 2) tunnels of the TiO{sub 2} structure chemically (with n-butyllithium) and electrochemically to an approximate composition Li{sub 0.5}TiO{sub 2}. The lithium ions can be easily removed from the lithiated structure by chemical reaction with bromine; cyclic voltammetry indicates that high voltages are required to remove the lithium by electrochemical methods. The poor electrochemical behavior of hollandite-TiO{sub 2} contrasts strongly with {alpha}-MnO{sub 2} electrodes. The superior properties of {alpha}-MnO{sub 2} electrodes are attributed to the presence of oxygen ions, either as H{sub 2}O or Li{sub 2}O, in the (2 x 2) channels; lithia-stabilized electrodes, 0.15Li{sub 2}O {center_dot} -MnO{sub 2}, show good cycling behavior and a rechargeable capacity of approximately 180 mAh/g.
Date: September 2, 1998
Creator: Noailles, L. D.
Partner: UNT Libraries Government Documents Department

MeV ion beam induced index of refraction changes in layered GaAs/AlGaAs waveguides

Description: Previously, we showed that localized optical modifications could be produced without subsequent post thermal annealing in selectively masked planar GaAs/Al{sub .4}Ga{sub .6}As waveguide structures using 10 MeV oxygen ions. In our present investigation, irradiation experiments were performed on masked GaAs/Al{sub .4}Ga{sub .6}As waveguide samples at 298 K using 10 MeV oxygen and 8 MeV carbon ions. The two ion incident energies were chosen to yield the maximum electronic stopping power near the interface separating the top cladding layer and the guiding layer. This localized modification process emphasizes the crucial role that the electronic energy transfer plays on the degree to which the refractive index of the guiding layer is altered. Propagation loss measurements on the fabricated channel waveguides were performed by end fire coupling a laser diode source at a wavelength of 1.3 {mu}m. Observation of the extracted propagation loss values reveal that further optimization of the ion beam parameters are required before practical applications can be achieved. The relative efficiency of the various ions to induce optically altered regions which serve as lateral confinement barriers of laser light shows that this fabrication process is sensitive to the ion beam current.
Date: December 31, 1995
Creator: Taylor, T.; Ila, D. & Zimmerman, R.L.
Partner: UNT Libraries Government Documents Department

Surface Modification of AISI-4620 Steel With Intense Pulsed Ion Beams

Description: A 300-keV, 30-kA, 1-{micro}s intense beam of carbon, oxygen, and hydrogen ions is used for the surface treatment of AISI-4620 steel coupons, a common material used in automotive gear applications. The beam is extracted from a magnetically-insulated vacuum diode and deposited into the top 1 {micro}m of the target surface. The beam-solid interaction causes a rapid melt and resolidification with heating and cooling rates of up to 10{sup 10} K/sec. Treated surfaces are smoothed over 1-{micro}m scale-lengths, but are accompanied by 1-{micro}m diameter craters and larger-scale roughening over >=10 {micro}m, depending on beam fluence and number of pulses. Treated surfaces are up to 1.8 x harder with no discernible change in modulus over depths of 1 {micro}m or more Qualitative improvements in the wear morphology of treated surfaces are reported.
Date: September 1, 1996
Creator: Rej, D.J.; Davis, H.A.; Nastasi, M.; Olson, J.C.; Peterson, E.J.; Reiswig, R.D. et al.
Partner: UNT Libraries Government Documents Department

Collisional Cooling of Negative Ion Beams

Description: Investigations have been conducted to determine the feasibility of using collisional cooling for reducing the energy spreads and, consequently, the emittances of negative-ion beams. We have designed a gas-filled RF-quadrupole ion cooler equipped with provisions for retarding energetic negative ion beams to energies below thresholds for electron detachment at injection and for re-acceleration to high energies after the cooling process. The device has been used to cool O{sup -} and F{sup -} ion beams with initial energy spreads, {Delta}E > 10 eV to final energy spreads, {Delta}E {approx} 2 eV FWHM. Overall transmission efficiencies of {approx}14% for F{sup -} beams have been obtained. Experimental results show that electron detachment is the major loss mechanism for negative ions.
Date: June 29, 2001
Creator: Liu, Y.
Partner: UNT Libraries Government Documents Department

Modification of the optical properties of glass by sequential ion implantation

Description: The linear and nonlinear optical properties of a series of samples formed by the sequential implantation of Ti, O and Au are examined. Energies of implantation for each ion were chosen using TRIM calculations to insure overlap of the ion distributions. The Ti was implanted with nominal doses of 1.2 and 2 {times} 10{sup 17} ions/cm{sup 2}. The samples were implanted with oxygen to the same nominal dose as the Ti. Au was then implanted with a nominal dose of 6 {times} 10{sup 16} ions/cm{sup 2}. The samples were subsequently annealed in oxygen at 900 C for two hours. The Ti and O are incorporated into the host network, while the Au forms nanosize colloids. The presence of the Ti in the substrate causes a shift in the surface plasmon resonance frequency of the Au metal colloids as well as an increase in the nonlinear response of the composites. The results are interpreted in terms of effective medium theory.
Date: December 1994
Creator: Magruder, R. H., III; Osborne, D. H., Jr. & Zuhr, R. A.
Partner: UNT Libraries Government Documents Department

Influence of Oxygen Ion Implantation on the Damage and Annealing Kinetics of Iron-Implanted Sapphire

Description: The effects of implanted oxygen on the damage accumulation in sapphire which was previously implanted with iron was studied for (0001) sapphire implanted with iron and then with oxygen. The energies were chosen to give similar projected ranges. One series was implanted with a 1:l ratio (4x10{sup 16} ions/cm{sup 2} each) and another with a ratio of 2:3 (4x10{sup 16} fe{sup +}/cm{sup 2}; 6x10{sup 16} O{sup +}/cm{sup 2}). Retained damage, X, in the Al-sublattice, was compared to that produced by implantation of iron alone. The observed disorder was less for the dual implantations suggesting that implantation of oxygen enhanced dynamic recovery during implantation. Samples were annealed for one hour at 800 and 1200 C in an oxidizing and in a reducing atmosphere. No difference was found in the kinetics of recovery in the Al-sublattice between the two dual implant conditions. However, the rate of recovery was different for each from samples implanted with iron alone.
Date: November 14, 1999
Creator: Hunn, J.D. & McHargue, C.J.
Partner: UNT Libraries Government Documents Department


Description: Resonant x-ray scattering is a powerful experimental technique for probing orbital and charge ordering. It involves tuning the incident photon energy to an absorption edge of the relevant ion and observing scattering at previously ''forbidden'' Bragg peaks, and it allows high-resolution, quantitative studies of orbital and charge order--even from small samples. Further, resonant x-ray scattering from orbitally ordered systems exhibits polarization- and azimuthal-dependent properties that provide additional information about the details of the orbital order that is difficult, or impossible, to obtain with any other technique. In the manganites, the sensitivity to charge and orbital ordering is enhanced when the incident photon energy is tuned near the Mn K absorption edge (6.539 keV), which is the lowest energy at which a 1s electron can be excited into an unoccupied state. In this process, the core electron is promoted to an intermediate excited state, which decays with the emission of a photon. The sensitivity to charge ordering is believed to be due to the small difference in K absorption edges of the Mn{sup 3+} and Mn{sup 4+} sites. For orbital ordering, the sensitivity arises from a splitting--or difference in the weight of the density of states [239]--of the orbitals occupied by the excited electron in the intermediate state. In the absence of such a splitting, there is no resonant enhancement of the scattering intensity. In principle, other absorption edges in which the intermediate state is anisotropic could be utilized, but the strong dipole transition to the Mn 4p levels--and their convenient energies for x-ray diffraction--make the K edge well-suited to studies of manganites. The Mn 4p levels are affected by the symmetry of the orbital ordering, which makes the technique sensitive to the orbital degree of freedom. Therefore resonant x-ray scattering can be used to obtain important quantitative information concerning the ...
Date: May 13, 2002
Creator: Nelson, C. S.; Hill, J. P. & Gibbs, D.
Partner: UNT Libraries Government Documents Department

Negative ion detachment cross sections. Interim progress report

Description: During past year, we have measured cross sections for associative and collisional detachment for several negative ions in collisions with atomic hydrogen. Additional experiments have been performed in which the formation of secondary negative ions and electrons by means of low energy ion impact on surfaces has been studied. Brief descriptions of these activities along with future plans for the project follow.
Date: December 1, 1991
Creator: Champion, R. L. & Doverspike, L. D.
Partner: UNT Libraries Government Documents Department

Low-energy continuum-electron emission at O{degrees} from O{sup q+} + He collisions

Description: Low-energy continuum-electron emission along the beam direction, i.e., at 0{degree}, has been investigated for 1.1--6.2 keV/u 0{sup 8+} and 2.6 keV/u o{sup q+} (q = 3, 6, and 8) colliding with He. Spectra were obtained for continuum electrons associated with bound-state capture and with no projectile charge change, respectively. As for previous measurements for 3.75 keV/u 0{sup 6+} + He, continuum electrons at 0{degree} were observed only when accompanied by bound-state capture. Cross sections for these continuum electrons are found to be increasing functions of both the projectile energy and the charge state over the ranges investigated.
Date: December 31, 1992
Creator: Tanis, J. A.; Haar, R. R.; Schneider, D.; Clark, M. W.; Prior, M. H.; Dubois, R. D. et al.
Partner: UNT Libraries Government Documents Department

Photo-oxidation of Ge Nanocrystals: Kinetic Measurements by InSitu Raman Spectroscopy

Description: Ge nanocrystals are formed in silica by ion beam synthesis and are subsequently exposed by selective HF etching of the silica. Under ambient conditions, the exposed nanocrystals are stable after formation of a protective native oxide shell of no more than a few monolayers. However, under visible laser illumination at room temperature and in the presence of O{sub 2}, the nanocrystals rapidly oxidize. The oxidation rate was monitored by measuring the Raman spectra of the Ge nanocrystals in-situ. The intensity ratio of the anti-Stokes to the Stokes line indicated that no significant laser-induced heating of illuminated nanocrystals occurs. Therefore, the oxidation reaction rate enhancement is due to a photo-chemical process. The oxidation rate varies nearly linearly with the logarithm of the laser intensity, and at constant laser intensity the rate increases with increasing photon energy. These kinetic measurements, along with the power dependencies, are described quantitatively by an electron active oxidation mechanism involving tunneling of optically excited electrons through the forming oxide skin and subsequent transport of oxygen ions to the Ge nanocrystal surface.
Date: November 22, 2006
Creator: Sharp, I.D.; Xu, Q.; Yuan, C.W.; Beeman, J.W.; Ager III, J.W.; Chrzan, D.C. et al.
Partner: UNT Libraries Government Documents Department

Hydrogen Production and Delivery Research

Description: In response to DOE's Solicitation for Grant Applications DE-PS36-03GO93007, 'Hydrogen Production and Delivery Research', SRI International (SRI) proposed to conduct work under Technical Topic Area 5, Advanced Electrolysis Systems; Sub-Topic 5B, High-Temperature Steam Electrolysis. We proposed to develop a prototype of a modular industrial system for low-cost generation of H{sub 2} (<$2/kg) by steam electrolysis with anodic depolarization by CO. Water will be decomposed electrochemically into H{sub 2} and O{sub 2} on the cathode side of a high-temperature electrolyzer. Oxygen ions will migrate through an oxygen-ion-conductive solid oxide electrolyte. Gas mixtures on the cathode side (H{sub 2} + H{sub 2}O) and on the anode side (CO + CO{sub 2}) will be reliably separated by the solid electrolyte. Depolarization of the anodic process will decrease the electrolysis voltage, and thus the electricity required for H{sub 2} generation and the cost of produced H{sub 2}. The process is expected to be at least 10 times more energy-efficient than low-temperature electrolysis and will generate H{sub 2} at a cost of approximately $1-$1.5/kg. The operating economics of the system can be made even more attractive by deploying it at locations where waste heat is available; using waste heat would reduce the electricity required for heating the system. Two critical targets must be achieved: an H{sub 2} production cost below $2/kg, and scalable design of the pilot H{sub 2} generation system. The project deliverables would be (1) a pilot electrolysis system for H{sub 2} generation, (2) an economic analysis, (3) a market analysis, and (4) recommendations and technical documentation for field deployment. DOE was able to provide only 200K out of 1.8M (or about 10% of awarded budget), so project was stopped abruptly.
Date: October 15, 2007
Creator: Balachov, Iouri
Partner: UNT Libraries Government Documents Department

Economic Analysis for Conceptual Design of Supercritical O2-Based PC Boiler

Description: This report determines the capital and operating costs of two different oxygen-based, pulverized coal-fired (PC) power plants and compares their economics to that of a comparable, air-based PC plant. Rather than combust their coal with air, the oxygen-based plants use oxygen to facilitate capture/removal of the plant CO{sub 2} for transport by pipeline to a sequestering site. To provide a consistent comparison of technologies, all three plants analyzed herein operate with the same coal (Illinois No 6), the same site conditions, and the same supercritical pressure steam turbine (459 MWe). In the first oxygen-based plant, the pulverized coal-fired boiler operates with oxygen supplied by a conventional, cryogenic air separation unit, whereas, in the second oxygen-based plant, the oxygen is supplied by an oxygen ion transport membrane. In both oxygen-based plants a portion of the boiler exhaust gas, which is primarily CO{sub 2}, is recirculated back to the boiler to control the combustion temperature, and the balance of the flue gas undergoes drying and compression to pipeline pressure; for consistency, both plants operate with similar combustion temperatures and utilize the same CO{sub 2} processing technologies. The capital and operating costs of the pulverized coal-fired boilers required by the three different plants were estimated by Foster Wheeler and the balance of plant costs were budget priced using published data together with vendor supplied quotations. The cost of electricity produced by each of the plants was determined and oxygen-based plant CO{sub 2} mitigation costs were calculated and compared to each other as well as to values published for some alternative CO{sub 2} capture technologies.
Date: September 1, 2006
Creator: Seltzer, Andrew & Robertson, Archie
Partner: UNT Libraries Government Documents Department

CRADA Final Report: Properties of Vacuum Deposited Thin Films of Lithium Phosphorous Oxynitride (Lipon) with an Expanded Composition Range

Description: Thin films of an amorphous, solid-state, lithium electrolyte, referred to as ''Lipon'', were first synthesized and characterized at ORNL in 1991. This material is typically prepared by magnetron sputtering in a nitrogen plasma, which allows nitrogen atoms to substitute for part of the oxygen ions of Li{sub 3}PO{sub 4}. Lipon is the key component in the successful fabrication of ORNL's rechargeable thin film microbatteries. Cymbet and several other US Companies have licensed this technology for commercialization. Optimizing the properties of the Lipon material, particularly the lithium ion conductivity, is extremely important, yet only a limited range of compositions had been explored prior to this program. The goal of this CRADA was to develop new methods to prepare Lipon over an extended composition range and to determine if the film properties might be significantly improved beyond those previously reported by incorporating a larger N component into the film. Cymbet and ORNL investigated different deposition processes for the Lipon thin films. Cymbet's advanced deposition process not only achieved a higher deposition rate, but also permitted independent control the O and N flux to the surface of the growing film. ORNL experimented with several modified sputtering techniques and found that by using sectored sputter targets, composed of Li{sub 3}PO{sub 4} and Li{sub 3}N ceramic disks, thin Lipon films could be produced over an expanded composition range. The resulting Lipon films were characterized by electrical impedance, infrared spectroscopy, and several complementary analytical techniques to determine the composition. When additional N plus Li are incorporated into the Lipon film, the lithium conductivity was generally degraded. However, the addition of N accompanied by a slight loss of Li gave an increase in the conductivity. Although the improvement in the conductivity was only very modest and was a disappointing conclusion of this study, forcing a higher N ...
Date: December 29, 2003
Creator: Dudney, N.J.
Partner: UNT Libraries Government Documents Department

Furnace and Heat Recovery Area Design and Analysis for Conceptual Design of Supercritical O2-Based PC Boiler

Description: The objective of the furnace and heat recovery area design and analysis task of the Conceptual Design of Supercritical Oxygen-Based PC Boiler study is to optimize the location and design of the furnace, burners, over-fire gas ports, and internal radiant surfaces. The furnace and heat recovery area were designed and analyzed using the FW-FIRE, Siemens, and HEATEX computer programs. The furnace is designed with opposed wall-firing burners and over-fire air ports. Water is circulated in the furnace by forced circulation to the waterwalls at the periphery and divisional wall panels within the furnace. Compared to the air-fired furnace, the oxygen-fired furnace requires only 65% of the surface area and 45% of the volume. Two oxygen-fired designs were simulated: (1) with cryogenic air separation unit (ASU) and (2) with oxygen ion transport membrane (OITM). The maximum wall heat flux in the oxygen-fired furnace is more than double that of the air-fired furnace due to the higher flame temperature and higher H{sub 2}O and CO{sub 2} concentrations. The coal burnout for the oxygen-fired case is 100% due to a 500 F higher furnace temperature and higher concentration of O{sub 2}. Because of the higher furnace wall temperature of the oxygen-fired case compared to the air-fired case, furnace water wall material was upgraded from T2 to T92. Compared to the air-fired heat recovery area (HRA), the oxygen-fired HRA total heat transfer surface is 35% less for the cryogenic design and 13% less for the OITM design due to more heat being absorbed in the oxygen-fired furnace and the greater molecular weight of the oxygen-fired flue gas. The HRA tube materials and wall thickness are nearly the same for the air-fired and oxygen-fired design since the flue gas and water/steam temperature profiles encountered by the heat transfer banks are similar.
Date: May 1, 2006
Creator: Seltzer, Andrew
Partner: UNT Libraries Government Documents Department

Modeling for CVD of Solid Oxide Electrolyte

Description: Because of its low thermal conductivity, high thermal expansion and high oxygen ion conductivity yttria-stabilized zirconia (YSZ) is the material of choice for high temperature electrolyte applications. Current coating fabrication methods have their drawbacks, however. Air plasma spray (APS) is a relatively low-cost process and is suitable for large and relatively complex shapes. it is difficult to produce uniform, relatively thin coatings with this process, however, and the coatings do not exhibit the columnar microstructure that is needed for reliable, long-term performance. The electron-beam physical vapor deposition (EB-PVD) process does produce the desirable microstructure, however, the capital cost of these systems is very high and the line-of-sight nature of the process limits coating uniformity and the ability to coat large and complex shapes. The chemical vapor deposition (CVD) process also produces the desirable columnar microstructure and--under proper conditions--can produce uniform coatings over complex shapes. CVD has been used for many materials but is relatively undeveloped for oxides, in general, and for zirconia, in particular. The overall goal of this project--a joint effort of the University of Louisville and Oak Ridge National Laboratory (ORNL)--is to develop the YSZ CVD process for high temperature electrolyte applications. This report describes the modeling effort at the University of Louisville, which supports the experimental work at ORNL. Early work on CVD of zirconia and yttria used metal chlorides, which react with water vapor to form solid oxide. Because of this rapid gas-phase reaction the water generally is formed in-situ using the reverse water-gas-shift reaction or a microwave plasma. Even with these arrangements gas-phase nucleation and powder formation are problems when using these precursors. Recent efforts on CVD of zirconia and YSZ have focused on use of metal-organic precursors (MOCVD). These are more stable in the gas-phase and can produce dense, crystalline films. With metal-organic CVD, ...
Date: September 18, 2002
Creator: Starr, T.L.
Partner: UNT Libraries Government Documents Department