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At least 235 records · Page 13

Determining Concentration of Nanoparticles from Ellipsometry

A method of using ellipsometry or polarization analysis of light in total internal reflection of a surface to determine the number density of gold nanoparticles on a smooth substrate has been developed. The method can be modified to enable determination of densities of sparse distributions of nanoparticles in general, and is expected to be especially useful for measuring gold-nanoparticle-labeled biomolecules on microarrays. The method is based on theoretical calculations of the ellipsometric responses of gold nanoparticles. Elements of the calculations include the following: For simplicity, the gold nanoparticles are assumed to be spherical and to have the same radius. The distribution of gold nanoparticles is assumed to be a sub-monolayer (that is, sparser than a monolayer). The optical response of the sub-monolayer is modeled by use of a thin-island-film theory, according to which the polarizabilities parallel and perpendicular to the substrate are functions of the wavelength of light, the dielectric functions (permittivities expressed as complex functions of frequency or wavelength) of the gold and the suspending medium (in this case, the suspending medium is air), the fraction of the substrate area covered by the nanoparticles, and the radius of the nanoparticles. For the purpose of the thin-island-film theory, the dielectric function of the gold nanoparticles is modeled as the known dielectric function of bulk gold plus a correction term that is necessitated by the fact that the mean free path length for electrons in gold decreases with decreasing radius, in such a manner as to cause the imaginary part of the dielectric function to increase with decreasing radius (see figure). The correction term is a function of the nanoparticle radius, the wavelength of light, the mean free path and the Fermi speed of electrons in bulk gold, the plasma frequency of gold, and the speed of light in a vacuum. These models are used to calculate ellipsometric responses for various concentrations of gold nanoparticles having an assumed radius. The modeled data indicates distinct spectral features for both the real and the imaginary part of the dielectric function. An ellipsometric measurement would determine this distinct feature and thus can be used to measure nanoparticle concentration. By "ellipsometric responses" is meant the intensities of light measured in various polarization states as functions of the angle of incidence and the polarization states of the incident light. These calculated ellipsometric responses are used as calibration curves: Data from subsequent ellipsometric measurements on real specimens are compared with the calibration curves. The concentration of the nanoparticles on a specimen is assumed to be that of the calibration curve that most closely matches the data pertaining to that specimen.

Venkatasubbarao, Srivatsa↗

Chemical colloids versus biological colloids: a comparative study for the elucidation of the mechanism of protein fiber formation

Fiber formation from murine serum amyloid A1 (SAA) was compared to the linear aggregation and fiber formation of colloidal gold particles. Here we report the similarities of these processes. Upon incubation with acetic acid, SAA misfolds and adopts a new conformation, which we termed saa. saa apparently is less soluble than SAA in aqueous solution; it aggregates and forms nucleation units and then fibers. The fibers appear as a string of the nucleation units. Additionally, an external electric field promotes saa fiber formation. These properties of saa are reminiscent of colloidal gold formation from gold ions and one-dimensional aggregation of the gold colloids. Colloidal gold particles were also found to be capable of aggregating one-dimensionally under an electric field or in the presence of polylysine. These gold fibers resembled in structure that of saa fibers. In summary, protein aggregation and formation of fibers appear to follow the generalized principles derived in colloidal science for the aggregation of atoms and molecules, including polymers such as polypeptides. The analysis of colloidal gold formation and of one-dimensional aggregation provides a simple model system for the elucidation of some aspects of protein fiber formation.

Colloids↗

Detecting Airborne Mercury by Use of Palladium Chloride

Palladium chloride films have been found to be useful as alternatives to the gold films heretofore used to detect airborne elemental mercury at concentrations of the order of parts per billion (ppb). Somewhat more specifically, when suitably prepared palladium chloride films are exposed to parts-per-billion or larger concentrations of airborne mercury, their electrical resistances change by amounts large enough to be easily measurable. Because airborne mercury adversely affects health, it is desirable to be able to detect it with high sensitivity, especially in enclosed environments in which there is a risk of leakage of mercury from lamps or other equipment. The detection of mercury by use of gold films involves the formation of gold/mercury amalgam. Gold films offer adequate sensitivity for detection of airborne mercury and could easily be integrated into an electronic-nose system designed to operate in the temperature range of 23 to 28 C. Unfortunately, in order to regenerate a gold-film mercury sensor, one must heat it to a temperature of 200 C for several minutes in clean flowing air. In preparation for an experiment to demonstrate the present sensor concept, palladium chloride was deposited from an aqueous solution onto sets of gold electrodes and sintered in air to form a film. Then while using the gold electrodes to measure the electrical resistance of the films, the films were exposed, at a temperature of 25 C, to humidified air containing mercury at various concentrations from 0 to 35 ppb (see figure). The results of this and other experiments have been interpreted as signifying that sensors of this type can detect mercury in room-temperature air at concentrations of at least 2.5 ppb and can readily be regenerated at temperatures <40 C.

Ryan, Margaret↗

Body of Knowledge (BOK) for Copper Wire Bonds

Copper wire bonds have replaced gold wire bonds in the majority of commercial semiconductor devices for the latest technology nodes. Although economics has been the driving mechanism to lower semiconductor packaging costs for a savings of about 20% by replacing gold wire bonds with copper, copper also has materials property advantages over gold. When compared to gold, copper has approximately: 25% lower electrical resistivity, 30% higher thermal conductivity, 75% higher tensile strength and 45% higher modulus of elasticity. Copper wire bonds on aluminum bond pads are also more mechanically robust over time and elevated temperature due to the slower intermetallic formation rate - approximately 1/100th that of the gold to aluminum intermetallic formation rate. However, there are significant tradeoffs with copper wire bonding - copper has twice the hardness of gold which results in a narrower bonding manufacturing process window and requires that the semiconductor companies design more mechanically rigid bonding pads to prevent cratering to both the bond pad and underlying chip structure. Furthermore, copper is significantly more prone to corrosion issues. The semiconductor packaging industry has responded to this corrosion concern by creating a palladium coated copper bonding wire, which is more corrosion resistant than pure copper bonding wire. Also, the selection of the device molding compound is critical because use of environmentally friendly green compounds can result in internal CTE (Coefficient of Thermal Expansion) mismatches with the copper wire bonds that can eventually lead to device failures during thermal cycling. Despite the difficult problems associated with the changeover to copper bonding wire, there are billions of copper wire bonded devices delivered annually to customers. It is noteworthy that Texas Instruments announced in October of 2014 that they are shipping microcircuits containing copper wire bonds for safety critical automotive applications. An evaluation of copper wire bond technology for applicability to spaceflight hardware may be warranted along with concurrently compiling a comprehensive understanding of the failure mechanisms involved with copper wire bonded semiconductor devices.

Body of Knowledge (BOK)↗

High reliability bond program using small diameter aluminum wire

The program was undertaken to characterize the performance of small diameter aluminum wire ultrasonically bonded to conductors commonly encountered in hybrid assemblies, and to recommend guidelines for improving this performance. Wire, 25.4, 38.1 and 50.8 um (1, 1.5 and 2 mil), was used with bonding metallization consisting of thick film gold, thin film gold and aluminum as well as conventional aluminum pads on semiconductor chips. The chief tool for evaluating the performance was the double bond pull test in conjunction with a 72 hour - 150 C heat soak and -65 C to +150 C thermal cycling. In practice the thermal cycling was found to have relatively little effect compared to the heat soak. Pull strength will decrease after heat soak as a result of annealing of the aluminum wire; when bonded to thick film gold, the pull strength decreased by about 50% (weakening of the bond interface was the major cause of the reduction). Bonds to thin film gold lost about 30 - 40% of their initial pull strenth; weakening of the wire itself at the bond heel was the predominant cause. Bonds to aluminum substrate metallization lost only about 22%. Bonds between thick and thin film gold substrate metallization and semiconductor chips substantiated the previous conclusions but also showed that in about 20 to 25% of the cases, bond interface failure occurred at the semiconductor chip.

Macha, M.↗

Containerless low gravity processing of glass forming and immiscible alloys

Under normal one-g conditions immiscible alloys segregate extensively during solidification due to sedimentation of the more dense of the immiscible liquid phases. Immiscible (hypermonotectic) gold-rhodium alloys were processed in the 100 meter drop tube under low gravity, containerless conditions to determine the feasibility of producing dispersed structures. Three alloy compositions were utilized. Alloys containing 10 percent by volume of the gold-rich hypermonotectic phase exhibited a tendency for the gold-rich liquid to wet the outer surface of the samples. This wetting tendency led to extensive segregation in several cases. Alloys containing 80 and 90 percent by volume of the gold-rich phase possessed completely different microstructures from the 10 percent samples when processed under low-g, containerless conditions. Several samples exhibited microstructures consisting of well dispersed 2 to 3 microns diameter rhodium-rich spheres in a gold-rich matrix.

Andrews, J. Barry↗

Contact formation in gallium arsenide solar cells

Gold and gold-based alloys, commonly used as solar cell contact materials, are known to react readily with gallium arsenide. Experiments were performed to identify the mechanisms involved in these GaAs-metal interactions. It is shown that the reaction of GaAs with gold takes place via a dissociative diffusion process. It is shown further that the GaAs-metal reaction rate is controlled to a very great extent by the condition of the free surface of the contact metal, an interesting example of which is the previously unexplained increase in the reaction rate that has been observed for samples annealed in a vacuum environment as compared to those annealed in a gaseous ambient. A number of other hard-to-explain observations, such as the low-temperature formation of voids in the gold lattice and crystallite growth on the gold surface, are explained by invoking this mechanism.

Weizer, Victor G.↗

Corrosion Prevention in Copper Combustion Chamber Liners of Liquid Oxygen/Methane Booster Engines

Prior research conducted by United Technologies Research Center and Rockwell International Rocketdyne Division encountered severe copper corrosion while flowing hydrocarbon fuels through copper cooling tubes. These experimental results have very important implications for the development of low-cost, regeneratively cooled, oxygen/hydrocarbon bipropellant booster engines. Aerojet TechSystems undertook a program sponsored by NASA/Lewis Research Center in 1986 with two objectives: (1) to define the corrosive interaction process that occurs between hydrocarbon fuels and copper combustion chamber liner materials, using both static and dynamic test methods, and (2) to identify and demonstrate protective measures against this corrosive process. The results of the first program task demonstrated that the most damaging corrosive process was caused by trace amounts of sulfur-containing impurities in the hydrocarbon fuel which react with the copper chamber liner material to form cuprous sulfide (Cu2S), as reported in Paper No. AlAA 88-3215. Experiments were conducted which demonstrated this corrosive process with Mil-Spec RP-1, propane, and methane fuels in contact with OFHC, NASA-Z, and ZrCu coppers. The preliminary results of the second program task demonstrated that electrodeposited gold and platinum coatings held promise of preventing corrosion of copper chamber liners by methane contaminated with sulfur-containing impurities, as reported in Paper No. AIAA 89-2738. Experiments were conducted which demonstrated greatly reduced corrosion of copper by hydrogen sulfide (H2S) and methyl mercaptan (CH3SH) as measured impurities in methane. This paper presents the concluding, confirmatory results from the second program task. The efficacy of a protective gold coating on NASA-Z copper cooling channel walls was conclusively demonstrated. Tests were conducted in the Aerojet Carbothermal Test Facility which provide realistic simulations of booster engine cooling channel conditions such as temperature, pressure, flow velocity, and heat flux. Dynamic test series were performed with methane containing 5 and 10 ppm (by volume) hydrogen sulfide. Gold-plated and unplated copper alloy specimens were evaluated. The tests demonstrated that gold coatings were effective in preventing corrosion of the copper. Posttest metallographic examinations of the unplated specimens showed severe corrosion as a result of reaction with the sulfur containing contaminant in the fuel. In contrast, posttest metallographic examination of the gold-coated specimens showed no corrosion under similar operating conditions. The findings from metallurgical and chemical analyses of the copper specimens, chemical analysis of the methane, and description of all test conditions are provided. Conclusions are reached as to the efficacy of the plating methods and the effectiveness of the metal coatings in the prevention of corrosion in hydrocarbon-fueled booster engine combustion chamber liners.

S D Rosenberg↗

Projectile compositions and modal frequencies on the chemistry of micrometeoroids LDEF experiment

The Chemistry of Micrometeoroids Experiment (LDEF instrument A0187-1) exposed witness plates of high-purity gold (greater than 99.99 percent Au) and commercial aluminum (greater than 99 percent Al) with the objective of analyzing the residues of cosmic-dust and orbital-debris particles associated with hypervelocity impact craters. The gold substrates were located approximately 8 deg off LDEF's trailing edge (Bay A03), while the aluminum surfaces resided in Bay A11, approximately 52 deg from LDEF's leading edge. SEM-EDX techniques were employed to analyze the residues associated with 199 impacts on the gold and 415 impacts on the aluminum surfaces. The residues that could be analyzed represent natural or man-made materials. The natural particles dominate at all particle sizes less than 5 micron. It is possible to subdivide both particle populations into subclasses. Chondritic compositions dominate the natural impactors (71 percent), followed by monomineralic, mafic-silicate compositions (26 percent), and by Fe-Ni rich sulfides (approximately 3 percent). Approximately 30 percent of all craters on the gold collectors were caused by man-made debris such as aluminum, paint flakes, and other disintegrated, structural and electronic components. Equations-of-state and associated calculations of shock stresses for typical LDEF impacts into the gold and aluminum substrates suggest that substantial vaporization may have occurred during many of the impacts and is the reason why approximately 50 percent of all craters did not contain sufficient residue to permit analysis by the SEM-EDX technique. After converting the crater diameters into projectile sizes using encounter speeds typical for the trailing-edge and forward-facing (Row 11) directions, and accounting for normalized exposure conditions of the CME collectors, we derived the absolute and relative fluxes of specific projectile classes. The natural impactors encounter all LDEF pointing directions with comparable, modal frequencies suggesting compositional (and dynamic) homogeneity of the interplanetary-dust environment in near-Earth orbit.

Bernhard, Ronald P.↗

Low resistance contacts for shallow junction semiconductors

A method of enhancing the specific contact resistivity in InP semiconductor devices and improved devices produced thereby are disclosed. Low resistivity values are obtained by using gold ohmic contacts that contain small amounts of gallium or indium and by depositing a thin gold phosphide interlayer between the surface of the InP device and the ohmic contact. When both the thin interlayer and the gold-gallium or gold-indium contact metallizations are used, ultra low specific contact resistivities are achieved. Thermal stability with good contact resistivity is achieved by depositing a layer of refractory metal over the gold phosphide interlayer.

Fatemi, Navid S.↗

Improved fuel-cell-type hydrogen sensor

Modified hydrogen sensor replaces oxygen cathode with a cathode consisting of a sealed paste of gold hydroxide and a pure gold current collector. The net reaction which occurs during cell operation is the reduction of the gold hydroxide to gold and water, with a half-cell potential of 1.4 volts.

Rudek, F. P.↗

Diffusion and structural changes in microcircuit interconnections

The interdiffusion of platimum and gold films, a couple utilized in beam lead microcircuits, has been studied for temperatures up to 550 C. Gold-on-platinum couples and separate platimum and gold films 80-450 nm thick, were deposited by electron beam evaporation onto oxidized (111) silicon substrates. Diffusion was monitored by means of spectral reflectance versus wavelength in the band 500-1000 nm. The separate metal films showed good adhesion and stable reflectances (after an initial change) for at least 6 h at diffusion temperatures, in contrast to the couples. Analysis of platinum diffusion through the gold films yielded an activation energy about 38 kcal/g-atom and a pre-exponential factor of the order 0.001 sq cm/sec, values close to those for volume diffusion. The pre-exponential factor especially is dependent upon film deposition conditions.

Nowak, W. B.↗

Chromium electrodes for REDOX cells

An improved electrode having a gold coating for use in the anode compartment of a REDOX cell is described. The anode fluid utilizes a chromic/chromous couple. A carbon felt is soaked in methanol, rinsed in water, dried and then heated in KOH after which it is again washed in deionized water and dried. The felt is then moistened with a methanol water solution containing chloroauric acid and is stored in a dark place while still in contact with the gold-containing solution. After all the gold-containing solution is absorbed in the felt, the latter is dried by heat and then heat treated at a substantially greater temperature. The felt is then suitable for use as an electrode and is wetted with water or up to two molar HCl prior to installation in a REDOX cell. The novelty of the invention lies in the use of KOH for cleaning the felt and the use of alcohol as a carrier for the gold together with the heat treating procedure.

Jalan, V.↗

Tribological properties of ceramic/Ti3Al-Nb sliding couples for use as candidate seal materials to 700 deg C

Tribological properties of Ti3Al-Nb intermetallic disks sliding against alumina-boria-silicate fabric were ascertained in air at temperatures from 25 to 700 C. These materials are candidates for sliding seal applications for the National AeroSpace Plane. The tests were done using a pin on disk tribometer. Sliding was unidirectional at 0.27 m/sec under a nominal contact stress of 340 kPa. Gold sputter or ion plating deposited films were used to reduce friction and wear. Rhodium and palladium films were used beneath the gold lubricating films to prevent diffusion of the substrate into the gold at high temperature. The friction and wear of the unlubricated specimens was unacceptable. Friction coefficients were generally greater than 1.0. The ion plated gold films, when used with a rhodium diffusion barrier reduced friction by almost a factor of 2. Wear was also substantially reduced. The sputter deposited films were not adherent unless the substrate was sputter cleaned immediately prior to film deposition. Palladium did not function as a diffusion barrier.

Dellacorte, Christopher↗

Rugged Low-Resistance Contacts To High-Tc Superconductors

Newly developed technique involving use of gold makes possible to fabricate low-resistance contacts with rugged connections to high-Tc superconductors. Gold diffused into specimen of superconducting material by melting gold beads onto surface of specimen, making strong mechanical contacts. Shear strength of gold bead contacts greater than epoxy or silver paste. Practical use in high-current-carrying applications of new high-Tc materials, including superconducting magnets, long-wavelength sensors, electrical ground planes at low temperatures, and efficient transmission of power.

Caton, Randall↗