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Fabrication of Pd-13 percent Cr alloy wires is described. Melting, casting, swaging and annealing processes are discussed. Drawing to reach two diameters (0.003 inch and 0.00176 inch) of wire is described. Representative micrographs of the Pd-Cr alloy at selected stages during wire fabrication are included. The resistance of the wire was somewhat lower, by about 15 to 20 percent, than comparable wire of other alloys used for strain gages.
A newly developed alloy, palladium-13 weight percent chromium (Pd13Cr), was identified by United Technologies Research Center under a NASA contract to be the best material for high temperature strain gage applications. An electrical resistance strain gage that can provide accurate static strain measurement to a temperature higher than that of a commercially available gage is urgently needed in aerospace and aeronautics research. A strain gage made of a 25.4 micron (1 mil) diameter Pd13Cr wire has been recently demonstrated to be usable for static strain measurements to 800 C. This compares to the 400 C temperature limit of the commercially available strain gages. The performance of the Pd-Cr gage, however, strongly depends on the quality of the Pd13Cr wire. Four batches of Pd-Cr wires purchased from three different manufacturers were therefore evaluated to determine the best source of the wire for strain gage applications. The three suppliers were Precious Metal Institute in China, Sigmund Cohn Co., and G & S Titanium, Inc. in the United States. Two batches of wires obtained from Previous Metal Institute in 1987 and 1992, respectively are referred to herein as China87 and China92 wires. The mechanical, chemical and electrical properties of these wires, both as-received and after high temperature exposures at 800 C for 50 hours were analyzed. The elastic modulus and the failure strength of the wires were evaluated using a tensile test machine equipped with a laser speckle strain measurement system. The chemical and microstructural properties of the wires were inspected using a plasma atomic emission spectrometer and a scanning electron microscope (SEM) equipped with an energy dispersive X-ray spectroscope (EDS). The electrical stability and repeatability of the wires were determined by measuring the electrical resistance of the wires during three thermal cycles to 1000 C and a ten-hour soak at 1000 C. As a result of this study, the wire which has the highest strength, the least impurities content, the best oxidation resistance and the best electrical stability will be selected for upcoming strain gage applications.
Active magnetic bearings are used to provide a long-life, low-loss suspension of a high-speed flywheel rotor. This paper describes a modeling effort used to understand the stability boundaries of the PD controller used to control the active magnetic bearings on a high speed test rig. Limits of stability are described in terms of allowable stiffness and damping values which result in stable levitation of the nonrotating rig. Small signal stability limits for the system is defined as a nongrowth in vibration amplitude of a small disturbance. A simple mass-force model was analyzed. The force resulting from the magnetic bearing was linearized to include negative displacement stiffness and a current stiffness. The current stiffness was then used in a PD controller. The phase lag of the control loop was modeled by a simple time delay. The stability limits and the associated vibration frequencies were measured and compared to the theoretical values. The results show a region on stiffness versus damping plot that have the same qualitative tendencies as experimental measurements. The resulting stability model was then extended to a flywheel system. The rotor dynamics of the flywheel was modeled using a rigid rotor supported on magnetic bearings. The equations of motion were written for the center of mass and a small angle linearization of the rotations about the center of mass. The stability limits and the associated vibration frequencies were found as a function of nondimensional magnetic bearing stiffness and damping and nondimensional parameters of flywheel speed and time delay.
Ti-Ag and Ti-Pd-Ag solar cell contacts structure and degradation dependence on high temperature and humidity environmental exposure
The elastic pd differential cross section at center-of-mass angles between 91 and 164 deg was determined for 316, 364, 470, and 590 MeV proton scattering in a backward hemisphere. For the three largest energies, the cross sections were within 10% of each other at any given angle larger than 130 deg. The extrapolated 180 deg differential cross section remained nearly constant from 316 to 590 MeV.
A UHV technique is presented for evaluating the adsorption-desorption properties of UHV vapor-deposited metal particles supported on insulating substrates. Desorption studies of CO from particulate and continuous Pd films supported on mica were performed. The desorption results indicate that: the CO desorption energies from the deposited metals are much lower than those from bulk single crystals; two desorption states exist for the vapor-deposited films; and the lower energy desorption peak of the vapor-deposited films is coverage dependent. Possible reasons for the difference between previously reported CO desorption studies on bulk substrates and the present results are discussed.
An exploratory study, dealing with the preparation of well-defined particulate metal deposits that can be used in model studies of catalytic reactions, was performed. Small metal particles of Fe and Pd were grown in situ in an electron microscope by vapor deposition onto different phase of electron transparent alumina substrates. The results show that characteristic properties of the deposits, such as particle density, size distribution, habit, and orientation, are strongly dependent on the cleanliness, phase, and crystallographic orientation of the alumina substrate; also, the deposition conditions can be chosen in such a way as to reproducibly manipulate the overall deposit structure.
Samples of Pd(40)Ni(40)P(20) glass, produced by cooling the melt at 1 or 800 K/s, are heated in a differential scanning calorimeter to determine the crystallization kinetics. Optical microscopy shows that eutectic crystallization proceeds both by growth from the surface of the samples and by the growth of spherical regions around preexisting nuclei in the interior. A modified Kissinger (1957) analysis is used to obtain the activation energy for crystal growth (3.49 eV). The steady state homogeneous nucleation frequency at 590 K is about 10 million/cu m per sec. This is estimated to be the maximum nucleation frequency: it is too low to account for the observed population of quenched-in nuclei, which are therefore presumed to be heterogeneous. The major practical obstacle to glass formation in this system is heterogeneous nucleation.
The dendritic microstructure and solute compression profiles for Pb-8 pct Au and Pb-3 pct Pd alloy samples are examined. Two groups of models, the minimum undercooled dendrite tip model of Burden and Hunt (1974) and Laxmanan (1974, 1984) and marginal stability at the dendrite tip models of Trivedi (1980) and Laxmanan (1974) are used to predict growth behavior of the alloy samples. The experimentally observed dendrite tip radius, primary arm spacing, and liquid composition at the dendrite tip are compared with theoretical predictions. It is observed that the modified minimum undercooling dendrite tip model and both of the marginal stability models accurately predict dendritic behavior. It is concluded that quantitative comparison of the primary arm spacing measurements can not form the basis for distinguishing among the various dendrite growth models in a positive temperature gradient.
An investigation of Pb-8 pct Au and Pb-3 pct Pd alloy specimens which have been partially directionally solidified and then quenched is performed in order to characterize their dendritic microstructural details and solute composition profiles. A controlled sectioning technique is employed to measure dendrite tip radii. It is found that most of the observed behavior is predicted quite well by a modification of the Burden and Hunt (1974) model proposed by Laxmanan (1984), in addition to the models based on the marginal stability approach. Results indicate that quantitative comparison of the primary arm spacing measurements can not form the basis of distinguishing among the various dendrite growth models in a positive temperature gradient.
Partitioning coefficients for metal/sulfide liquid, troilite/sulfide liquid, and schreibersite/sulfide liquid were determined for Ag, Au, Mo, Ni, Pd, and Tl (using EMPA and proton-induced X-ray microprobe and ion microprobe analyses) in order to understand the chronometer systems of iron meteorites. In general, the obtained schreibersite/metal and troilite/metal partition coefficients for 'compatible' elements were quite similar to those inferred from natural assemblages, reinforcing an earlier made conclusion that there is a class of elements for which experimental troilite/metal and schreibersite/metal partition coefficients approximate those inferred from natural samples. The consistency between experimental and natural assemblages, however, was not observed for Ag, Pb, and Tl, indicating that the abundances of these elements determined in 'metal' and 'troilite' separates from iron meteorites are influenced by trace minerals that concentrate incompatible elements.
A phase boundary for H-Pd(100) was calculated using the Metropolis (1953) algorithm and the embedded atom method (EAM) described by Daw and Foiles (1987). The calculated phase boundary agreed with an experimentally determined phase boundary in its curvature and the coverage at which maximum Tc appeared, but was about 125 K lower than the experimental phase boundary.
Atomistic modeling of the site substitution behavior of Pd in NiTi (J. Alloys and Comp. (2004), in press) has been extended to examine the behavior of several other alloying additions, namely, Fe, Pt, Au, Al, Cu, Zr and Hf in this important shape memory alloy. It was found that all elements, to a varying degree, displayed absolute preference for available sites in the deficient sublattice. How- ever, the energetics of the different substitutional schemes, coupled with large scale simulations indicate that the general trend in all cases is for the ternary addition to want to form stronger ordered structures with Ti.
A high resolution thermometer was developed using dilute aloy of Mn in Pd as the magnetic sensing element instead of the traditional paramagnetic salt.
One of the most elusive geochemical aspects of the early Earth has been explaining the near chondritic relative abundances of the highly siderophile elements (HSE; Au, Re and the platinum group elements) in Earth's primitive upper mantle (PUM). Perhaps they were delivered to the Earth after core formation, by late addition of carbonaceous chondrite material. However, the recognition that many moderately siderophile elements can be explained by high pressure and temperature (PT) metal-silicate equilibrium, leads to the question whether high PT equilibrium can also explain the HSE concentrations. Answers to this question have been slowed by experimental difficulties (nugget effect and very low solubilities). But two different perspectives have emerged from recent studies. One perspective is that D(M/S) for HSE at high PT are not low enough to explain terrestrial mantle depletions of these elements (for Pd and Pt). A second perspective is D(M/S) are reduced substantially at high PT and even low enough to explain terrestrial mantle depletions (for Au and Pt). Issues complicating interpretation of all experiments include use of MgO- and FeO-free silicate melts, and S-free and FeNi metal-free systems. In addition, conclusions for Pt rest on an interpretation that the tiny metallic nuggets plaguing many such experiments, were formed upon quench. There is not agreement on this issue, and the general question of HSE solubility at high PT remains unresolved
Since approximately 1990 high pressure and temperature (PT) experiments on metal-silicate systems have showed that partition coefficients (D) for siderophile (iron-loving) elements are much different than those measured at low PT conditions. The high PT data have been used to argue for a magma ocean during growth of the early Earth. Initial conclusions were based on experiments and calculations for a small number of elements such as Ni and Co. However, for many elements only a limited number of experimental data were available then, and they only hinted at values of metal-silicate D's at high PT conditions. In the ensuing decades there have been hundreds of new experiments carried out and published on a wide range of siderophile elements. At the same time several different models have been advanced to explain the siderophile elements in the earth's mantle: a) intermediate depth magma ocean; 25-30 GPa, b) deep magma ocean; up to 50 GPa, and c) early reduced and later oxidized magma ocean. Some studies have drawn conclusions based on a small subset of siderophile elements, or a set of elements that provides little leverage on the big picture (like slightly siderophile elements), and no single study has attempted to quantitatively explain more than 5 elements at a time. The purpose of this abstract is to update the predictive expressions outlined by Righter et al. (1997) with new experimental data from the last decade, test the predictive ability of these expressions against independent datasets (there are more data now to do this properly), and to apply the resulting expressions to the siderophile element patterns in Earth's upper mantle. The predictive expressions have the form: lnD = alnfO2 + b/T + cP/T + d(1Xs) + e(1Xc) + SigmafiXi + g These expressions are guided by the thermodynamics of simple metal-oxide equilibria that control each element, include terms that mimic the activity coefficients of each element in the metal and silicate, and quantify the effect of variable oxygen fugacity. Preliminary results confirm that D(Ni) and D(Co) converge at pressures near 25-30 GPa and approximately 2200 K, and show that D(Pd) and D(Cu) become too low at the PT conditions of the deepest models. Furthermore, models which force fit V and Cr mantle concentrations by metal-silicate equilibrium overlook the fact that at early Earth mantle fO2, these elements will be more compatible in Mg-perovskite and (Fe,Mg)O than in metal. Thus an intermediate depth magma ocean, at 25-30 GPa, 2200 K, and at IW-2, can explain more mantle siderophile element concentrations than other models.
The partition coefficients of Pt and other Pt Group Elements (PGE) between metal and silicate D(sub Metal-Silicate) and also between silicate minerals and silicate melts D(sub Metal-Silicate) are among the most challenging coefficients to obtain precisely. The PGE are highly siderophile elements (HSE) with D(sub Metal-Silicate) >10(exp 3) due to the fact that their concentrations in silicates are very low (ppb to ppt range). Therefore, the analytical difficulty is increased by the possible presence of HSE-rich-nuggets in reduced silicate melts during experiments). These tiny HSE nuggets complicate the interpretation of measured HSE concentrations. If the HSE micro-nuggets are just sample artifacts, then their contributions should be removed before calculations of the final concentration. On the other hand, if they are produced during the quench, then they should be included in the analysis. We still don't understand the mechanism of nugget formation well. Are they formed during the quench by precipitation from precursor species dissolved homogeneously in the melts, or are they precipitated in situ at high temperature due to oversaturation? As these elements are important tracers of early planetary processes such as core formation, it is important to take up this analytical and experimental challenge. In the case of the Earth for example, chondritic relative abundances of the HSE in some mantle xenoliths have led to the concept of the "late veneer" as a source of volatiles (such as water) and siderophiles in the silicate Earth. Silicate crystal/liquid fractionation is responsible for most, if not all, the HSE variation in the martian meteorite suites (SNC) and Pt is the element least affected by these fractionations. Therefore, in terms of reconstructing mantle HSE abundances for Mars, Pt becomes a very important player. In the present study, we have performed high temperature experiments under various redox conditions in order to determine the abundances of Pt, Au, Ru and Pd in minerals (olivine and diopside) and in silicate melts, but also to characterize the sizes, density and chemistry of HSE nuggets when present in the samples.
Earth's core contains approximately 10 percent light elements that are likely a combination of S, C, Si, and O, with Si possibly being the most abundant. Si dissolved into Fe liquids can have a large effect on the magnitude of the activity coefficient of siderophile elements (SE) in Fe liquids, and thus the partitioning behavior of those elements between core and mantle. The effect of Si can be small such as for Ni and Co, or large such as for Mo, Ge, Sb, As. The effect of Si on many siderophile elements is unknown yet could be an important, and as yet unquantified, influence on the core-mantle partitioning of SE. Here we report new experiments designed to quantify the effect of Si on the partitioning of P, Au, Pd, and many other SE between metal and silicate melt. The results will be applied to Earth, for which we have excellent constraints on the mantle siderophile element concentrations.