The solubility of carbon in palladium and platinum.
Saturation solubility of carbon in solid Pd and Pt obtained by equilibrating excess graphite at various high temperatures
Mclellan, R. B.↗
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Effect of particle size on the chemisorption and decomposition of carbon monoxide by palladium and nickel clusters
The chemisorption of gases on well-defined, supported metal particles is a model for basic processes in heterogeneous catalysis. In this study, the chemisorption and decomposition of carbon monoxide on palladium and nickel particles was examined as a function of particle size. Particulate films with average particle sizes ranging from 1 to 10 nm were grown by vapor deposition on UHV-cleaved mica. Successive CO adsorption-desorption cycles resulted in the accumulation of carbon on the particles, which suppressed CO adsorption. The rate of carbon accumulation was strongly dependent on particle size and was higher for Ni than for Pd over the same size range. Carbon was removed from both metals by oxygen treatments at elevated temperatures. However, a mixture of CO and O2 was effective for monitoring the removal of carbon from palladium.
Doering, D. L.↗
Carbon Materials Embedded with Metal Nanoparticles as Anode in Lithium-Ion Batteries
Carbon materials containing metal nanoparticles that can form an alloy with lithium were tested for their capacity and cycle life to store and release lithium electrochemically. Metal nanoparticles may provide the additional lithium storage capacity as well as additional channels to conduct lithium in carbon. The cycle life of this carbon-metal composite can be long because the solid-electrolyte interface (SEI) on the carbon surface may protect both lithium and the metal particles in the carbon interior. In addition, the voids in the carbon interior may accommodate the nanoparticle's volume change, and such volume change may not cause much internal stress due to small sizes of the nanoparticles. This concept of improving carbon's performance to store and release lithium was demonstrated using experimental cells of C(Pd)/0.5M Lil-50/50 (vol.%) EC and DMC/Li, where C(Pd) was graphitized carbon fibers containing palladium nanoparticles, EC was ethylene carbonate, and DMC was dimethyl carbonate. However, such improvement was not observed if the Pd nanoparticles are replaced by aluminum, possibly because the aluminum nanoparticles were oxidized in air during storage, resulting in an inert oxide of aluminum. Further studies are needed to use this concept for practical applications.
Hung, Ching-cheh↗
Three-Dimensional Polybenzobisoxazoles and Polybenzobisthiazoles
Due to the poor compressive strength properties of high performance liquid crystalline polymers such as polybenzobisoxazoles (PBOs) and polybenzobisthiazoles (PBTs), we have prepared homopolymers and copolymers with PBO and PBT pendant groups on a central star-like unit, 2.7-diamino-9,9'-bis(4-aminophenyl)fluorene, in order to improve upon their compressive strength properties. The fluorene moiety was prepared by the reaction of 2,7-dinitro-9-fluorene with aniline and aniline hydrochloride, followed by reduction with palladium on carbon. The central star-like unit was characterized by FTIR, FTNMR, and elemental analysis. The PBO and PBT pendant groups were synthesized by the polycondensation of 4,6-diaminoresorcinol dihydrochloride with terephthaloyl chloride and 2,5-diamino-1,4-benzendithiol dihydrochloride with terephthaloyl chloride in poly(phosphoric acid), respectively. The resulting linear polymers containing the dicarboxylic end groups were attached to the central star-like unit by refluxing with 2,7-diamino-9,9'-bis(4-aminophenyl) fluorene to give the star-like polymers. The star-like PBO and PBT were soluble in methanesulfonic acid. Further characterization of the polymers is ongoing.
Bray, M.↗
Development of a solid electrolyte carbon dioxide and water reduction system for oxygen recovery
A 1/4-man solid electrolyte oxygen regeneration system, consisting of an electrolyzer, a carbon deposition reactor, and palladium membranes for separating hydrogen, was operated continuously in a 180-day test. Oxygen recovery from the carbon dioxide-water feed was 95%. One percent of the oxygen was lost to vacuum with the hydrogen off-gas. In a space cabin, the remaining 4% would have been recycled to the cabin and recovered. None of the electrolysis cells used in the 180-day test failed. Electrolysis power rose 20% during the test; the average power was 283.5 watts/man. Crew time was limited to 18 min/day of which 12 min/day was used for removing carbon. The success achieved in operating the system can be attributed to an extensive component development program, which is described. Stability of operation, ease of control, and flexibility in feed composition were demonstrated by the life test.
Elikan, L.↗
UHV studies of the interaction of CO with small supported metal particles, Pd/mica
The interaction of carbon monoxide with small palladium particles supported on UHV-cleaved and heat-treated single-crystal mica was studied. The Pd particles were characterized and tested using the techniques of flash thermal desorption, Auger electron spectroscopy, core electron energy loss spectroscopy, and transmission electron microscopy. Evidence is presented for CO decomposition on Pd particles during CO adsorption-desorption experiments. The rate of CO decomposition increased rapidly with diminishing particle size. Residual carbon from CO decomposition blocked CO adsorption and had a strong poisoning effect on the CO oxidation reaction.
Doering, D. L.↗
Black Carbon (Soot) Aerosol in the Lower Stratosphere and Upper Troposphere
We have used two approaches to measure BCA in the stratosphere. The first method consists of collecting aerosols by impaction on quartz rods, upon which are mounted strips of polystyrene filter material. Each 25 mm by 0.5 mm filter strip is alternately masked and exposed in 5 mm long sections. After sampling, the optical density of the exposed sections is measured and compared with the optical density of the masked (unexposed) sections. The filter strip is a Lambertian collector, the scattering property of which is not affected by the deposition of liquid sulfuric acid droplets which dominate the stratospheric aerosol. Hence, all attenuation greater in the exposed than in the non-exposed sections is due to absorption by BCA or rare opaque materials such as meteoritic iron. In a second approach we expose carbon-coated gold or palladium wires to air outside the aircraft boundary layer [Farlow et al., 1979; Pueschel et al., 1989]. With a field emission scanning electron microscope we are able to characterize BCA particles in addition to the dominant sulfuric acid droplets. Typically, soot is comprised of 20 nm diameter spheres linked together as branching chains or loosely packed aggregates (Figure 1a). The microscope has a lateral image resolution of 1.5 nm and can clearly resolve individual spheres making up BCA aggregates. Their morphology is uniquely different from that of the liquid sulfuric acid-water aerosol (Figure 1b). We approximate the size of each BCA particle by that of a sphere of equivalent volume and fit a lognormal size distribution to both the BCA and H2SO4/H2O aerosols. Both sampler types have been mounted on NASA's ER-2 high-altitude research aircraft (altitude ceiling of 70,000 feet), and on NASA's DC-8 (40,000 feet ceiling) aircraft to sample aerosols from a significant portion of the atmosphere.
Pueschel, R. F.↗
Conductometric Sensors for Detection of Elemental Mercury Vapor
Several organic and inorganic materials have been tested for possible incorporation into a sensing array in order to add elemental mercury vapor to the suite of chemical species detected. Materials have included gold films, treated gold films, polymer-carbon composite films, gold-polymer-carbon composite films and palladium chloride sintered films. The toxicity of mercury and its adverse effect on human and animal health has made environmental monitoring of mercury in gas and liquid phases important (1,2). As consumer products which contain elemental mercury, such as fluorescent lighting, become more widespread, the need to monitor environments for the presence of vapor phase elemental mercury will increase. Sensors in use today to detect mercury in gaseous streams are generally based on amalgam formation with gold or other metals, including noble metals and aluminum. Recently, NASA has recognized a need to detect elemental mercury vapor in the breathing atmosphere of the crew cabin in spacecraft and has requested that such a capability be incorporated into the JPL Electronic Nose (3). The detection concentration target for this application is 10 parts-per-billion (ppb), or 0.08 mg/m3. In order to respond to the request to incorporate mercury sensing into the JPL Electronic Nose (ENose) platform, it was necessary to consider only conductometric methods of sensing, as any other transduction method would have required redesign of the platform. Any mercury detection technique which could not be incorporated into the existing platform, such as an electrochemical technique, could not be considered.
mercury sensor↗
Surface and Interface Properties of PdCr/SiC Schottky Diode Gas Sensor Annealed at 425 C
The surface and interface properties of Pd(0.9)Cr(0.1)/SiC Schottky diode gas sensors both before and after annealing are investigated using Auger Electron Spectroscopy (AES), Scanning Electron Microscopy (SEM), and Energy Dispersive Spectroscopy (EDS). At room temperature the alloy reacted with SiC and formed Pd(x)Si only in a very narrow interfacial region. After annealing for 250 hours at 425 C, the surface of the Schottky contact area has much less silicon and carbon contamination than that found on the surface of an annealed Pd/SiC structure. Palladium silicides (Pd(x)Si) formed at a broadened interface after annealing, but a significant layer of alloy film is still free of silicon and carbon. The chromium concentration with respect to palladium is quite uniform down to the deep interface region. A stable catalytic surface and a clean layer of Pd(0.9)Cr(0.1) film are likely responsible for significantly improved device sensitivity.
Chen, Liang-Yu↗
Surface and Interface Properties of PdCr/SiC Schottky Diode Gas Sensor Annealed at 425 C
The surface and interface properties of Pd(0.9,)Cr(0.1)/SiC Schottky diode gas sensors both before and after annealing are investigated using Auger electron spectroscopy (AES), scanning electron microscopy (SEM), and energy dispersive spectroscopy (EDS). At room temperature the alloy reacted with SiC and formed Pd,Si only in a very narrow interfacial region. After annealing for 250 h ,It 425 C, the surface of the Schottky contact area his much less silicon and carbon contamination than that found on the surface of an annealed Pd/SiC structure. Palladium silicides (Pd(x)Si) formed at a broadened interface after annealing, but a significant layer of alloy film is still free of silicon and carbon. The chromium concentration with respect to palladium is quite uniform down to the deep interface region. A stable catalytic surface and a clean layer of Pd(0.9)Cr(0.1) film are likely responsible for significantly improved device sensitivity.
Chen, Liang-Yu↗
Surface and Interface Study of PdCr/SiC Schottky Diode Gas Sensor Annealed at 425 C
The surface and interface properties of Pd(sub 0.9)Cr(sub 0.1/SiC Schottky diode gas sensor both before and after annealing are investigated using Auger Electron Spectroscopy (AES), Scanning Electron Microscopy (SEM), and Energy Dispersive Spectroscopy (EDS). At room temperature the alloy reacted with SiC and formed Pd(sub x)Si only in a very narrow interfacial region. After annealing for 250 hours at 425 deg. C, the surface of the Schottky contact area has much less silicon and carbon contamination than that found on the surface of an annealed Pd/SiC structure. Pd(sub x)Si formed at a broadened interface after annealing, but a significant layer of alloy film is still free of silicon and carbon. The chromium concentration with respect to palladium is quite uniform down to the deep interface region. A stable catalytic surface and a clean layer of Pd(sub 0.9)Cr(sub 0.1) film are likely responsible for significantly improved device sensitivity.
Chen, Liang-Yu↗
Preparation of a Bimetal Using Mechanical Alloying for Environmental or Industrial Use
Following the 1976 Toxic Substances Control Act ban on their manufacture, PCBs remain an environmental threat. PCBs are known to bio-accumulate and concentrate in fatty tissues. Further complications arise from the potential for contamination of commercial mixtures with other more toxic chlorinated compounds such as polychlorinated dibenzodioxins (PCDDs) and polychlorinated dibenzofurans (PCDFs). Until recently, only one option was available for the treatment of PCB-contaminated materials: incineration. This may prove to be more detrimental to the environment than the PCBs themselves due to the potential for formation of PCDDs. Metals have been used for the past ten years for the remediation of halogenated solvents and other contaminants in the environment; however, zero-valent metals alone do not possess the activity required to dehalogenate PCBs. Palladium has been shown to act as an excellent catalyst for the dechlorination of PCBs with active metals. This invention is a method for the production of a palladium/magnesium bimetal capable of dechlorinating PCBs using mechanical milling/mechanical alloying. Other base metals and catalysts may also be alloyed together (e.g., nickel or zinc) to create a similarly functioning catalyst system. Several bimetal catalyst systems currently can be used for processes such as hydrogen peroxide synthesis, oxidation of ethane, selective oxidation, hydrogenation, and production of syngas for further conversion to clean fuels. The processes for making these bimetal catalysts often involve vapor deposition. This technology provides an alternative to vapor deposition that may provide equally active catalysts. A hydrogenation catalyst including a base material coated with a catalytic metal is made using mechanical milling techniques. The hydrogenation catalysts are used as an excellent catalyst for the dehalogenation of contaminated compounds and the remediation of other industrial compounds. The mechanical milling technique is simpler and cheaper than previously used methods for producing hydrogenation catalysts. Preferably, the hydrogenation catalyst is a bimetallic particle formed from a zero-valent iron or zero-valent magnesium particle coated with palladium that is impregnated onto a high-surface-area graphite support. The zero-valent metal particles should be microscale or nanoscale zero-valent magnesium or zero-valent iron particles. Other zero-valent metal particles and combinations may be used. Additionally, the base material may be selected from a variety of minerals including, but not limited to, alumina and zeolites. The catalytic metal is preferably selected from the group consisting of noble metals and transition metals, preferably palladium. The mechanical milling process includes milling the base material with a catalytic metal impregnated into a high-surface-area support to form the hydrogenation catalyst. In a preferred mechanical milling process, a zero-valent metal particle is provided as the base material, preferably having a particle size of less than about 10 microns, preferably 0.1 to 10 microns or smaller, prior to milling. The catalytic metal is supported on a conductive carbon support structure prior to milling. For example, palladium may be impregnated on a graphite support. Other support structures such as semiconductive metal oxides may also be used.
Quinn, Jacqueline↗
Conceptual design study of a six-man solid electrolyte system for oxygen reclamation
A six-man solid electrolyte oxygen regeneration system (SEORS) that will produce 12.5 lbs/day of oxygen has been designed. The SEORS will simultaneously electrolyze both carbon dioxide and water vapor and be suitable for coupling with a carbon dioxide concentration system of either molecular sieve, solid amine or hydrogen depolarized electrochemical type. The total system will occupy approximately 19 cu ft (34.5 in. x .26 in. x 36 in. high) and will weigh approximately 500 pounds. It is estimated that the total electrical power required will be 1783 watts. The system consists of three major components; electrolyzer, hydrogen diffuser, and carbon deposition reactor. There are 108 electrolysis stacks of 12 cells each in the electrolyzer. Only 2/3 of the 108 stacks will be operated at a time; the remainder will be held in reserve. The design calls for 96 palladium membranes for hydrogen removal to give 60 percent redundancy. Four carbon deposition reactors are employed. The iron catalyst tube in each reactor weighs 7.1 lb and 100 percent redundancy is allowed.
Morris, J. P.↗
Preparation and analysis of particulate metal deposits
Small particles and clusters of palladium were grown by deposition from the vapor phase under ultrahigh vacuum conditions. Amorphous and crystalline support films of Al2O3 and ultrathin amorphous carbon films were used as substrate materials. The growth of the metal deposit was monitored in situ by scanning transmission diffraction of energy-filtered 100 kV electrons and high resolution transmission electron microscopy (TEM) analysis was performed in a separate instrument. It was established by in situ TEM, however, that the transfer of specimens in this case did not unduly affect the size and distribution of deposit particles. It was found that the cleanness, stoichiometry, crystallinity and structural perfection of the support surface play an essential role in determining the crystalline perfection and structure of the particles. The smallest palladium clusters reproducibly prepared contained not more than six atoms but size determinations below 1 nm average particle diameter are very problematic with conventional TEM. Palladium particles grown on carbon supports feature an impurity-stabilized mosaic structure.
Poppa, H.↗
Preparation and evaluation of advanced catalysts for phosphoric acid fuel cells
The platinum electrocatalysts were characterized for their crystallite sizes and the degree of dispersion on the carbon supports. One application of these electrocatalysts was for anodic oxidation of hydrogen in hot phosphoric acid fuel cells, coupled with the influence of low concentrations of carbon monoxide in the fuel gas stream. In a similar way, these platinum on carbon electrocatalysts were evaluated for oxygen reduction in hot phosphoric acid. Binary noble metal alloys were prepared for anodic oxidation of hydrogen and noble metal-refractory metal mixtures were prepared for oxygen reduction. An exemplar alloy of platinum and palladium (50/50 atom %) was discovered for anodic oxidation of hydrogen in the presence of carbon monoxide, and patent disclosures were submitted. For the cathode, platinum-vanadium alloys were prepared showing improved performance over pure platinum. Preliminary experiments on electrocatalyst utilization in electrode structures showed low utilization of the noble metal when the electrocatalyst loading exceeded one weight percent on the carbon.
Stonehart, P.↗
Characterization of the LTC catalyst: Performance against common air pollutants
One of the important qualities of the Low-Temperature Catalyst (LTC) is the rapid oxidation of carbon monoxide to carbon dioxide under a wide variety of conditions. The catalytic material is a palladium-copper activated complex which reacts with various contaminant molecules through a continuous oxidation/reduction cycle. The alumina substrate enhances LTC activity with its favorable surface chemistry and very high surface area. About 10 percent surface water is necessary to facilitate the oxidation of CO. This reaction shows a log-log dependence on contact time, suggesting a Langmuir-Hinshelwood mechanism. In the tube tests, LTC removed 90 to 100 percent of contaminating carbon monoxide in the temperature region of 20 to 4000 C, and at ambient over a range of 25 to 65 percent relative humidity. In contrast, NO2 is chemisorbed by the LTC/alumina material--the amount strongly dependent on temperature increases but independent of humidity. The LTC catalyst has demonstrated excellent capability to remove an important variety of hazardous pollutant gases which are common factors to poor indoor air quality. The Instapure Air Filtration System incorporates the LTC catalyst in a 50:50 mixture with activated carbon to effectively remove particulate, odors, and hazardous gases at room temperature and humidities. The ability to remove hazardous gases is unique for the category of portable air filtration equipment. The wide variety of pollutant gases that LTC removes suggests that catalytic technology is adaptable to a considerable range of commercial and industrial applications.
Collins, Marcia F.↗
Investigation of low temperature carbon monoxide oxidation catalysts
Carbon monoxide generation rates related to the use of commerical equipment in Spacelab, added to the normal metabolic and subsystem loads, will produce carbon monoxide levels in excess of the maximum allowable concentration. In connection with the sensitivity of carbon monoxide oxidation catalysts to poisoning at room temperature, catalysts for an oxidation of carbon monoxide at low temperatures have been investigated. It was found that platinum and palladium are the only effective room temperature catalysts which are effective at 333 K. Hopcalite was ineffective at ambient temperatures, but converted CO with 100 percent efficiency at 333 K. Poisoning tests showed the noble metal catalysts to be very sensitive, and Hopcalite to be very resistant to poisoning.
Jagow, R. B.↗
Metal Decorated Multi-Walled Carbon Nanotube/Polyimide Composites with High Dielectric Constants and Low Loss Factors
The measurement of observable electromagnetic phenomena in materials and their derived intrinsic electric material properties are of prime importance in the discovery and development of material systems for electronic and aerospace applications. Nanocomposite materials comprised of metal decorated multi-walled carbon nanotubes (MWCNTs) were prepared by a facile method and characterized. Metal particles such as silver, platinum and palladium with diameters ranging from less than 5 to over 50 nanometers were distributed randomly on the MWCNTs. The metal-containing MWCNTs were then melt mixed into a polymer matrix and the mixture extruded as ribbons. These extruded ribbons exhibited a moderate to high degree of MWCNT alignment as determined by HRSEM. These ribbons were then fabricated into test specimens while maintaining MWCNT alignment and subsequently characterized for electromagnetic properties at 8-12 GHz. The present study is focused on silver decorated MWCNTs dispersed in an Ultem polyimide matrix. The results of the electromagnetic characterization showed that certain sample configurations exhibited a decoupling of the permittivity and loss factor (?? and ??) indicating that these properties could be tailored within certain limits. The decoupling and independent control of these fundamental electrical material parameters offer a new class of materials with potential applications in electronics, microwave engineering and optics.
Ghose, Sayata↗