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At least 487 records · Page 27

High-Temperature, Oxidation-Resistant Thermocouples

Aluminum substituted for rhodium, which is scarce and expensive. Electromotive force increases with aluminum content in Pt/Al leg of Pt(Pt/Al) thermocouple. Wires baked longer in aluminizing bed produce larger voltages. Thermocouples containing platinum/aluminum legs used instead of thermocouples of type R in furnaces, heat engines, and chemical reactors. Expecially suited to high-velocity oxidizing environments. Constructed as thin-film sensors on turbine blades and vanes, where pre-oxidation provides insulating film needed between thermocouple legs. Because aluminum content slowly depleted by oxidation, long-term use recommended only where maximum temperature is 1,200 degrees C or less.

Smialek, James L.↗

High Temperature - Thin Film Strain Gages Based on Alloys of Indium Tin Oxide

A stable, high temperature strain gage based on reactively sputtered indium tin oxide (ITO) was demonstrated at temperatures up to 1050 C. These strain sensors exhibited relatively large, negative gage factors at room temperature and their piezoresistive response was both linear and reproducible when strained up to 700 micro-in/in. When cycled between compression and tension, these sensors also showed very little hysteresis, indicating excellent mechanical stability. Thin film strain gages based on selected ITO alloys withstood more than 50,000 strain cycles of +/- 500 micro-in/in during 180 hours of testing in air at 1000 C, with minimal drift at temperature. Drift rates as low as 0.0009%/hr at 1000 C were observed for ITO films that were annealed in nitrogen at 700 C prior to strain testing. These results compare favorably with state of the art 10 micro-m thick PdCr films deposited by NASA, where drift rates of 0.047%/hr at 1050 C were observed. Nitrogen annealing not only produced the lowest drift rates to date, but also produce the largest dynamic gage factors (G = 23.5). These wide bandgap, semiconductor strain sensors also exhibited moderately low temperature coefficients of resistance (TCR) at temperatures up to 1100 C, when tested in a nitrogen ambient. A TCR of +230 ppm/C over the temperature range 200 C < T < 500 C and a TCR of -469 ppm/C over the temperature range 600 C < T < 1100 C was observed for the films tested in nitrogen. However, the resistivity behavior changed considerably when the same films were tested in oxygen ambients. A TCR of -1560 ppm/C was obtained over the temperature range of 200 C < T < 1100 C. When similar films were protected with an overcoat or when ITO films were prepared with higher oxygen contents in the plasma, two distinct TCR's were observed. At T < 800 C, a linear TCR of -210 ppm/C was observed and at T > 800 C, a linear TCR of -2170 DDm/C was observed. The combination of a moderately low TCR and a relatively large gage factor make these semiconducting oxide films promising candidates for the active strain elements in high temperature thin film strain gages, particularly in applications where static strain measurement is desired.

Gregory, Otto J.↗

Site-specific plan-view (S)TEM sample preparation from thin films using a dual-beam FIB-SEM

To fully evaluate the atomic structure, and associated properties of materials using transmission electron microscopy, examination of samples from three non-collinear orientations is needed. This is particularly challenging for thin films and nanoscale devices built on substrates due to limitations with plan-view sample preparation. In this work, a new method for preparation of high-quality, site-specific, plan-view TEM samples from thin-films grown on substrates, is presented and discussed. Here, it is based on using a dual-beam focused ion beam scanning electron microscope (FIB-SEM) system. To demonstrate the method, the samples were prepared from thin films of perovskite oxide BaSnO 3 grown on a SrTiO 3 substrate and metal oxide IrO 2 on a TiO 2 substrate, ranging from 20–80 nm in thicknesses using molecular beam epitaxy. While the method is optimized for the thin films, it can be extended to other site-specific plan-view samples and devices build on wafers. Aberration-corrected STEM was used to evaluate the quality of the samples and their applicability for atomic-resolution imaging and analysis.

BaSnO3↗

Nano-crystalline porous tin oxide film for carbon monoxide sensing

A tin oxide sol is deposited on platinum electrodes (12) of a sensor (10). The sol is calcined at a temperature of 500 to 800.degree. C. to produce a thin film of tin oxide with a thickness of about 150 nm to 2 .mu. and having a nano-crystalline structure with good stability. The sensor rapidly detects reducing gases, such as carbon monoxide, or hydrocarbons and organic vapors. Sensors using films calcined at around 700.degree. C. have high carbon monoxide selectivity with a response time of around 4 minutes and a recovery time of 1 minute, and therefore provide good detection systems for detection of trace amounts of pollutants such as toxic and flammable gases in homes, industrial settings, and hospitals.

Liu, Chung-Chiun↗

Size-Induced Ferroelectricity in Antiferroelectric Oxide Membranes (Adv. Mater. 17/2023)

Thin Films. In article number 2210562, Ruijuan Xu, Kevin J. Crust, Varun Harbola, and co-workers report intrinsic size-driven scaling in lead-free antiferroelectric thin films. They demonstrate an intriguing antiferroelectric-to-ferroelectric transition upon reducing the thickness of antiferroelectric NaNbO 3 membranes. Here, the image shows the coexistence of ferroelectric and antiferroelectric phases in freestanding NaNbO 3 membranes.

36 MATERIALS SCIENCE↗

Understanding non-stochiometric deposition of multi-principal elemental NiCoCr thin films

Multi-principal elemental NiCoCr thin films with compositional flexibility have potential applications as a thermal barrier, corrosion-resistant coatings, and functional energy materials. In this study, the non-stochiometric multi-principal element alloy thin film formation behavior from an equiatomic ablation target of NiCoCr using pulsed laser deposition has been reported. Here, the effect of varying laser fluence on compositions of constituent elements in the NiCoCr thin films is systematically investigated. The increase in laser fluence typically increases the likelihood of acquiring undesirable particulates in thin films. Therefore, to maintain the film quality the laser fluences are adjusted within the range of 1.3–3.3 J·cm -2 , while the film thicknesses are kept constant at ~30 nm. Results show that the constituent elements are well-distributed in the formed NiCoCr thin films, however, having average atomic percentages of Ni and Cr twice as high as Co irrespective of the equiatomic composition of individual elements in the ablation target. This stochiometric alteration in the as-deposited thin films is governed by the rate of ablation and subsequent evaporation of each element, which is facilitated by the optical properties and vapor pressure of individual constituent elements. Additionally, electron energy-loss spectroscopy and x-ray absorption spectroscopy analysis reveal that the thin films have partially oxidized, with the Cr oxidation contributing the most to the O-K edge in comparison to Ni and Co. Finally, this study presents a laser-assisted pathway for fabricating compositionally flexible NiCoCr thin films and develops an understanding of the non-equilibrium laser-material interactions and how the intrinsic properties of constituent elements affect the stoichiometric flow of materials from the target to the final film deposition.

36 MATERIALS SCIENCE↗

Quantifying Properties for a Mechanistic, Predictive Understanding of Aqueous Impact on Aging of Medium and Low Voltage AC and DC Cabling in Nuclear Power Plants

To address the gap in knowledge in understanding degradation in relevant service conditions, this project aimed to develop a mechanistic, predictive model of medium and low voltage cable failure based on the primary environmental degradation parameters of aqueous immersion time, temperature, and the oxidation extent. To do so, we took a two-fold approach toward evaluating degradation as related to the aqueous condition. First, we evaluated the chemical, mechanical, and electrical properties of polymers that comprise the cabling insulation under varied aqueous conditions at different temperatures. Secondly, we evaluated the performance of insulation materials under similar accelerated aging conditions in addition to the dielectric breakdown of the cabling under submersion conditions. Thermal oxidation and immersion of LDPE thin films were done using a Parr vessel and the extent of oxidation was monitored using the carbonyl index from ATR-FTIR spectrum, a ratio quantifying the carbonyl functionality produced on the LDPE film surface. Increasing the temperature, oxidation time, and oxygen pressure increased the water-vapor permeability and the carbonyl content. Thermogravimetric analysis of the films confirmed that there is indeed an initial weight loss of the smaller molecular weight molecules and volatiles. At higher temperatures, there is a secondary mass loss. Up to 70°C, the mass loss curves were similar until 80°C, when the aged films decreased at a much greater rate with respect to increasing temperature. This was seen in the 10, 50, 90% weight loss temperatures. The mechanical properties of sheet PP and HDPE as well as injection molded LDPE, HDPE, HDPP dog bones were plotted with respect to the time spent in the Parr vessel during thermal oxidation. For the sheet PP and HDPE, the UTS and the modulus of elasticity decreased while the elongation increased. The injection-molded LDPE, HDPE, and HDPP dog bones experienced a similar trend where the changes in the properties were within experimental uncertainty. This analysis of LDPE in dry and immersive oxygen-rich environments is an important baseline for future experiments looking at other degradation mechanisms. A predictive aging model for low-density polyethylene insulative cable housings was developed. This model revealed a combination of physical and chemical processes which lead to an increase in permeability and a decrease in strength of the insulator. In creating this predictive model, a gap of knowledge in the literature was revealed in two areas: understanding how the crystallinity of a polymer changes with time and visualizing the predicted pores formed through the insulator which leads to failure. Developing and using an adapted ATR-FTIR method, crystallinity was monitored and compared to bulk crystallinity found via DSC. Inhomogeneity in crystallinity changes were observed but the FTIR method but was found to be less reliable. Pore visualization was found utilizing electrical impedance spectroscopy saturated aged polyethylene films with synthesized citrate-capped gold nanoparticles, and chloroauric acid precursor. results indicate a decreasing impedance of the polyethylene films caused by the transport of ions through the film. SEM imaging was then performed for elemental analysis of the films and counter electrodes for the presence of ions. Chloride and gold ions were detected; however, no nanoparticles were found. This gives an estimated pore size of at least 0.3 nm through the aged film. Cyclic submergence of polyethylene and polypropylene in aqueous solutions of copper sulfate and Harrison’s solution were examined. It was discovered that aging in these mixed conditions and at 90°C did cause a small, yet significant increase to tensile strength for both unaged polyethylene and polypropylene. The PE and PP in cycled and submerged conditions did not have tensile strengths significantly different from dry-aged after 16 weeks. For both solutions, it was determined that capacitance increases with both water tree depth and cable temperature and is relatively independent of changing water tree AR. As for resistance, there is no apparent change between depth percentages of 10 and 80 for both solutions. This is because the water tree has not yet entered the conductor and thus there is no shorting current flowing through the tree yet. Between 80 and 100% water tree depth, it is observed that for both solutions there is a rapid decrease in resistance because the tree is now impacting the conductor shield and allowing shorting current to flow through it. The relationship between resistance and temperature was found to be inversed. As temperature increases, resistance decreases for both water tree solutions with distilled water having the most apparent difference across the range of temperatures simulated. With regards to water tree AR, resistance was found to be relatively independent at depth percentages of 10, 50, and 70, but there was some relationship at 100% depth for both solutions. At this depth, as water tree AR increased, resistance was found to also increase. Through the examination of voltage and electric field distribution plots, it was confirmed for EPR cables that increasing water tree depth leads to increasing distortion. The increase in shorting current at 100% depth for aqueous copper sulfate compared to distilled water was also visualized. Lastly, the relationship between shorting current and temperature for narrow water trees was visualized and validated using the distribution plots. This study has led to a better understanding of the effect of cable temperature, water tree solution, and geometry of the tree region on cable degradation. Furthermore, this study has documented simulation results of water tree degradation in EPR MV cables, which had been previously lacking in information. Future work in this area will add frequency into the mix and examine what effect it has on the rate of cable degradation as a result of water treeing. To compliment the work being carried by UMD on different polymer chemistries, harvested medium voltage (MV) cables were selected for accelerated aging study at ORNL. These medium voltage cables are representative of the vintages and materials that are currently in use at existing nuclear power plants (NPPs). These cables were immersed in water at 90°C and energized for a period of two years at elevated voltage. Partial discharge was measured during this period of time to track potential degradation. Unfortunately, due to the absence of failure, the extent of integration between the UMD techniques and the harvested MV insulation was limited. However, based on the findings and from the UMD research in the previous sections on polyethylene and polypropylene, follow-on characterization for harvested MV cable insulation should focus on sample preparation to take advantage of the UMD techniques to better understand mechanistic degradation in MV cable insulations. This would include: 1.) Utilization of solutions and impedance measurement insulation to track permeability in harvested and accelerated aging insulation samples, 2.) Adaptation of gold nanoparticle synthesis for electrical impedance spectroscopy with supporting SEM characterization to study pore formation in harvested and accelerated aged insulation samples, & 3.) ATR-FTIR crystallinity with multiple temperature dependent harvested MV cable insulation under different air and submerged accelerated aging. In addition, low voltage dielectric spectroscopy and high voltage dissipation factor, tan δ, could be implemented as a condition monitoring tool for harvested MV cable insulation in submerged environments.

24 POWER TRANSMISSION AND DISTRIBUTION↗

Expanding the Zinc Precursor Toolbox: A Comparative Study of Precursors for Thermal ALD of ZnO Thin Films

Atomic layer deposition (ALD) of zinc oxide (ZnO) has been widely researched using diethyl zinc (DEZ)-based methods. The significant importance of thin films of ZnO as transparent conductive oxides (TCO) in optoelectronic devices and photovoltaics warrants examining alternative Zn precursors for ZnO ALD as potential replacements for the pyrophoric DEZ. In this study, we investigated three alternative Zn precursors: Zn(EEKI)2, Zn(DMP)2, ZnEt(HMDS), in the process development for high-quality ZnO thin films and compared them to DEZ. The ALD processes were studied using in situ spectroscopic ellipsometry. The properties of the ALD ZnO films were characterized using ex situ X-ray photoelectron spectroscopy (XPS), Rutherford backscattering spectrometry and nuclear reaction analysis (RBS/NRA), X-ray diffraction (XRD), atomic force microscopy (AFM), transmission electron microscopy (TEM), and ultraviolet-visible (UV/Vis) spectrophotometry. These measurements confirmed the formation of pure, stoichiometric, and polycrystalline ZnO films using all four Zn precursors. Although the selected precursors are chemically diverse Zn compounds, they all yielded saturating ALD processes and high-quality ZnO thin films at 200 °C. This study highlights the potential benefits of alternative zinc precursors in designing ALD processes for ZnO thin films.

Obenlüneschloß, Jorit↗

Achieving Higher Activity of Acidic Oxygen Evolution Reaction Using an Atomically Thin Layer of IrO x over Co 3 O 4

The development of electrocatalysts with reduced iridium (Ir) loading for the oxygen evolution reaction (OER) is essential to produce low-cost green hydrogen from water electrolysis under acidic conditions. Herein, an atomically thin layer of iridium oxide (IrO x ) has been uniformly dispersed onto cobalt oxide (Co 3 O 4 ) nanocrystals to improve the efficient use of Ir for acidic OER. In situ characterization and theoretical calculations reveal that compared to the conventional IrOx cluster, the atomically thin layer of IrO x shows stronger interaction with the Co 3 O 4 and consequently higher OER activity due to the Ir-O-Co bond formation at the interface. Equally important, the facile synthetic method and the promising activity in the proton exchange membrane water electrolyzer, reaching 1 A cm -2 at 1.7 V with remarkable durability, enable potential scale-up applications. In conclusion, these findings provide a mechanistic understanding for designing active, stable and lower-cost electrocatalysts with well-defined structures for acidic OER.

58 GEOSCIENCES↗

Epitaxial thinning process

A method is described for thinning an epitaxial layer of a wafer that is to be used in producing diodes having a specified breakdown voltage and which also facilitates the thinning process. Current is passed through the epitaxial layer, by connecting a current source between the substrate of the wafer and an electrolyte in which the wafer is immersed. When the wafer is initially immersed, the voltage across the wafer initially drops and then rises at a steep rate. When light is applied to the wafer the voltage drops, and when the light is interrupted the voltage rises again. These changes in voltage, each indicate the breakdown voltage of a Schottky diode that could be prepared from the wafer at that time. The epitaxial layer is thinned by continuing to apply current through the wafer while it is immersed and light is applied, to form an oxide film and when the oxide film is thick the wafer can then be cleaned of oxide and the testing and thinning continued. Uninterrupted thinning can be achieved by first forming an oxide film, and then using an electrolyte that dissolves the oxide about as fast as it is being formed, to limit the thickness of the oxide layer.

Siegel, C. M.↗

Oxidation Temperature-Dependent Electrochemical Doping of WO 3 Deposited via Atomic Layer Deposition

Silicon-based photoelectrochemical devices show promise for the performance of light-driven CO 2 reduction but suffer from instability under photoelectrochemical conditions relevant to CO 2 reduction. Coating silicon electrodes with thin layers of metal oxides has shown promise to passivate unstable silicon surfaces, and many different metal oxides can be deposited on silicon using various techniques. In this study, we investigate the fundamental photoelectrochemical performance of WO 3 -coated silicon photoelectrodes, which were generated by oxidation of W-metal films deposited via atomic layer deposition on both degenerately doped (nSi + ) and low-doped (pSi) silicon. Two different oxidation temperatures were investigated (400 and 600 °C), and it was found that the monoclinic phase of WO 3 predominates at both temperatures but that more grain boundaries are present in the 600 °C film. From X-ray photoelectron spectroscopy, the stoichiometry of both films was found to be 1:3 W:O, and low electron energy loss experiments indicate band gaps of 3.0 and 3.1 eV for 400 and 600 °C films, respectively. Cyclic voltammetry experiments showed that the electron transfer kinetics increased after continued redox cycling, particularly for the material produced at 400 °C. X-ray photoelectron spectra suggest that the observed increase in electrode conductivity is due to the formation of oxygen vacancies in the film. Electrochemical impedance spectroscopy indicated that charge transport through the films was impacted by the grain boundaries that formed during oxidation of the film. Photoelectrochemical studies on pSi/WO 3 electrodes were highly variable, only producing a photocurrent and photovoltage with some samples. Our best sample, formed at 400 °C, produced a photovoltage of 180 mV, which is lower than what has previously been reported for WO 3 -coated silicon (500 mV). We hypothesize that the variability in photoelectrochemical experiments arose from a roughened WSiO x interface that is generated during film preparation. WO 3 shows promise as a metal oxide coating for silicon, but our results suggest that formation of a high-quality interface between Si and WO 3 is vital for best performance.

Charge transfer↗

Cobalt Oxide-Coated Single Crystalline Bismuth Vanadate Photoanodes for Efficient Photoelectrochemical Chlorine Generation

Bismuth vanadate (BiVO 4 ) is an outstanding photoanode material for photoelectrochemical water splitting. Here in this work, a series of single crystalline BiVO 4 photoanodes are synthesized by pulsed laser deposition (PLD). Once coated with a thin layer of cobalt oxide (CoO x ) cocatalyst, also by PLD, the photoanodes support efficient photoelectrochemical generation of chlorine (Cl 2 ) from brine under simulated solar light. The activity of the chlorine generation reaction (ClER) is optimized when the thickness of CoO x is about 3 nm, with the faradic efficiency of ClER exceeding 60%. Detailed studies show that the CoO x cocatalyst layer is amorphous, uniform in thickness, and chemically robust. As such, the cocatalyst also effectively protects the underlying BiVO 4 photoanodes against chlorine corrosion. This work provides insights into using artificial photosynthesis for byproducts that carry significant economic value while avoiding the energetically expensive oxygen evolution reactions.

36 MATERIALS SCIENCE↗

Exploring the First High-Entropy Thin Film Libraries: Composition Spread-Controlled Crystalline Structure

Thin films of two types of high-entropy oxides (HEOs) have been deposited on 76.2 mm Si wafers using combinatorial sputter deposition. In one type of the oxides, (MgZnMnCoNi)O x , all the metals have a stable divalent oxidation state and similar cationic radii. In the second type of oxides, (CrFeMnCoNi)O x , the metals are more diverse in the atomic radius and valence state, and have good solubility in their sub-binary and ternary oxide systems. Therefore, the resulting HEO thin films were characterized using several high-throughput analytical techniques. The microstructure, composition, and electrical conductivity obtained on defined grid maps were obtained for the first time across large compositional ranges. The crystalline structure of the films was observed as a function of the metallic elements in the composition spreads, that is, the Mn and Zn in (MgZnMnCoNi)O x and Mn and Ni in (CrFeMnCoNi)O x . The (MgZnMnCoNi)O x sample was observed to form two-phase structures, except single spinel structure was found in (MgZnMnCoNi)O x over a range of Mn > 12 at. % and Zn < 44 at. %, while (CrFeMnCoNi)O x was always observed to form two-phase structures. Composition-controlled crystalline structure is not only experimentally demonstrated but also supported by density function theory calculation.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

High-Temperature Tensile and Creep Test Results on Thin Wall Tube Specimens of ODS Alloys 14YWT and OFRAC

High-temperature tensile and strain rate jump (SRJ) creep tests were conducted on axial specimens fabricated from thin wall tubes of the oxide dispersion strengthened (ODS) alloys 14YWT and OFRAC. The dimensions of the 14YWT thin wall tube was 10.7 mm OD, 0.5 mm WT and 0.92 m and of the OFRAC thin wall tube was 8.5 mm OD + 0.5 mm WT and 1.78 m in length. The axial specimens fabricated from the thin wall tubes were based on a dual-gauge design with gauge dimensions of 4 mm long and 2 mm wide. The tensile tests were conducted in air at 800ºC, 900ºC and 1,000ºC and the SRJ creep tests were conducted in air at 800ºC. Two axial specimens were used in each tensile and SRJ creep tests. The results of the tensile tests showed much lower yield stress (YS) compared to ultimate tensile strength (UTS) indicative of large work hardening properties. The results showed the UTS of OFRAC was higher than that of 14YWT by ~35 MPa at 800ºC. At 900ºC, the UTS of OFRAC and 14YWT was similar at 900ºC and at 1000ºC, the UTS of 14YWT was higher than that of OFRAC by ~10 MPa. The ductility properties of OFRAC were greater than that of 14YWT with higher values of uniform elongation (UE) and total elongation (TE) at all tensile test temperatures. The creep properties of 14YWT and OFRAC were evaluated by the strain rate jump test method at 800ºC. The stress exponent (n) for creep was obtained from the SRJ test data by plotting the values of the log strain rate against the log stress, which is measured from the stress-strain curve generated during the SRJ test. The results showed the highest stress exponents of n = 19.8 and n = 35.0 were measured from the two SRJ tests on 14YWT. The stress exponent measured from one successful SRJ test on OFRAC was n = 13.3, which was lower than that of 14YWT. Nevertheless, these high values of stress exponent are consistent with ODS ferritic alloys such as 14YWT and OFRAC since they indicate dislocation-particle interactions are the dominant creep mechanism for specific ranges of temperature and stress. The results obtained from the tensile and SRJ creep tests conducted on axial specimens in this study indicate that 14YWT and OFRAC retain high strengths at temperatures up to 1,000ºC and good creep performance at 800ºC.

36 MATERIALS SCIENCE↗

Fission fragment assisted reactor concept for space propulsion: Foil reactor

The concept is to fabricate a reactor using thin films or foils of uranium, uranium oxide and then to coat them on substrates. These coatings would be made so thin as to allow the escaping fission fragments to directly heat a hydrogen propellant. The idea was studied of direct gas heating and direct gas pumping in a nuclear pumped laser program. Fission fragments were used to pump lasers. In this concept two substrates are placed opposite each other. The internal faces are coated with thin foil of uranium oxide. A few of the advantages of this technology are listed. In general, however, it is felt that if one look at all solid core nuclear thermal rockets or nuclear thermal propulsion methods, one is going to find that they all pretty much look the same. It is felt that this reactor has higher potential reliability. It has low structural operating temperatures, very short burn times, with graceful failure modes, and it has reduced potential for energetic accidents. Going to a design like this would take the NTP community part way to some of the very advanced engine designs, such as the gas core reactor, but with reduced risk because of the much lower temperatures.

Wright, Steven A.↗

Isotopic study of oxygen diffusion in oxide coatings

Diffusion of oxygen in thin films of silicon dioxide was studied using oxygen isotopically enriched in oxygen of atomic mass 18 (O-18). This subject is of interest because thin films of dielectrics such as SiO2 are proposed for use as a protective coatings for solar mirrors in low Earth orbit, which is a strongly oxidizing environment. Films of this material were prepared with a direct current magnetron using reactive sputtering techniques. To produce (O-18)- enriched SiO2, a standard 3.5-in.-diameter silicon wafer was reactively sputtered using (O-18)-enriched (95 percent) oxygen as the plasma feed gas. The films were characterized using Rutherford backscattering and Secondary Ion Mass Spectrometer (SIMS) to establish stoichiometry and purity. Subsequently, the films were exposed to an air-derived oxygen plasma in a standard laboratory plasma reactor for durations of up to 10 hr. The concentration ratio of O-16 as a function of depth was determined using SIMS profiling and compared to a baseline, nonplasma exposed sample. A value for the diffusivity of oxygen near the surface of these films was obtained and found to be about 10(-15)sq cm/sec.

Gulino, Daniel A.↗

Ellipsometric study of oxide films formed on LDEF metal samples

The optical constants of samples of six different metals (Al, Cu, Ni, Ta, W, and Zr) exposed to space on the Long Duration Exposure Facility (LDEF) were studied by variable angle spectroscopic ellipsometry. Measurements were also carried out on portions of each sample which were shielded from direct exposure by a metal bar. A least-squares fit of the data using an effective medium approximation was then carried out, with thickness and composition of surface films formed on the metal substrates as variable parameters. The analysis revealed that exposed portions of the Cu, Ni, Ta, and Zr samples are covered with porous oxide films ranging in thickness from 500 to 1000 A. The 410 A thick film of Al2O3 on the exposed Al sample is practically free of voids. Except for Cu, the shielded portions of these metals are covered by thin non-porous oxide films characteristic of exposure to air. The shielded part of the Cu sample has a much thicker porous coating of Cu2O. The tungsten data could not be analyzed.

Franzen, W.↗