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All sourcesNASA NTRSDOE OSTI
NASA NTRS1991

Stability of Y-Ba-Cu-oxide phases in salt flux

The results of an investigation into the possibility of growing YBa2Cu3O7 (or Y123) single crystals from a NaCl-KCl flux (salt flux) are presented. They are compared with results for Y123 crystals grown from a Ba-Cu-oxide flux system. The chosen salt flux composition was 1:1 (NaCl:KCl). The preparation method of the solutes is presented, with particular attention given to the compounds surrounding the Y123 phase, such as Y2BaCuO6 (Y211). Optical microscopy was introduced to study the morphology of the sample; X-ray diffraction was used for phase identification; and a chemical analysis was effected. The Y123, Y211, and BaCuO2 phases were shown to be dissociated in the NaCl-KCl flux, and could not be recrystallized. A small amount of the flux could be added to create large-grain Y123 crystals, but single-crystal growth was not possible in a top-seeded NaCl-KCl solution. This is attributed to significant differences in solubility of the crystal elements, and phase separation caused by CuO crystal formation.

Tao, Y. K.↗
NASA NTRS1990

Magnetism and superconductivity of some Tl-Cu oxides

Many copper oxide based Thallium compounds have now been discovered. In comparison to the Bi-compounds, the Tl-system shows a richer diversity; viz., High Temperature Superconductors (HTSC) can be obtained with either one or two Tl-0 layers (m = 1,2); also, the triple-digit phases are easier to synthesize. The value of d, oxygen stoichiometry, is critical to achieving superconductivity. The Tl system is robust to oxygen loss; Tl may be lost or incorporated by diffusion. A diffusion coefficient equal to 10 ms at 900 C was determined. Both ortho-rhombic and tetragonal structures are evidenced, but HTSC behavior is indifferent to the crystal symmetry. This system has the highest T(sub c) confirmed. T(sub c) generally increases with p, the number of CuO layers, but tends to saturate at p = 3. Zero resistance as high as 125K has been observed. Most of these HTSC's are hole type, but the Ce-doped specimens may be electronic. The magnetic aspects were studied; because in addition to defining the perfectly diamagnetic ground state as in the conventional superconductors, magnetism of the copper oxides show a surprising variety. This is true of both the normal and the superconducting states. Also, due to the large phonon contribution to the specific heat at the high T(sub c) accurate thermal measurement of important parameters such as the sp. heat jump, electronic density of states, D(Ef) and coherence length are uncertain, and thus, are estimated from the magnetic results. Results from the Tl-system CuO, LaBaCuO, 120 and the Bi-CuO compounds are discussed. The emphasis is on the role of magnetism in the TlCuO HTSC, but technological aspects are also pointed out.

Datta, Timir↗
NASA NTRS1991

Magnetism and superconductivity of some Tl-Cu oxides

Many copper oxide based Thallium compounds are now known. In comparison to the Bi-compounds, the Tl-system shows a richer diversity; i.e., High Temperature Superconductors (HTSC) can be obtained with either one or two Tl-0 layers (m = 1,2); also, the triple-digit phases are easier to synthesize. The value of d, oxygen stoichiometry, is critical to achieving superconductivity. The Tl system is robust to oxygen loss; Tl may be lost or incorporated by diffusion. A diffusion coefficient equal to 10 ms at 900 C was determined. Both ortho-rhombic and tetragonal structures are found, but HTSC behavior is indifferent to the crystal symmetry. This system has the highest T(sub c) confirmed. T(sub c) generally increases with p, the number of CuO layers, but tends to saturate at p = 3. Zero resistance was observed at temperatures as great as 125 K. Most of these HTSC's are hole type, but the Ce-doped specimens may be electronic. The magnetic aspects were studied; because in addition to defining the perfectly diamagnetic ground state as in conventional superconductors, magnetism of the copper oxides show a surprising variety. This is true of both the normal and the superconducting states. Also, due to the large phonon contribution to the specific heat at the high T(sub c) jump, electronic density of states, D(Ef), and coherence length are uncertain, and thus, are estimated from the magnetic results. Results from the Tl-system CuO, LaBaCuO,120 and the Bi-CuO compounds are discussed. The emphasis is on the role of magnetism in the Tl-CuO HTSC, but technological aspects are also pointed out.

Datta, Timir↗
NASA NTRS2002

The General Isothermal Oxidation Behavior of Cu-8Cr-4Nb

Oxidation kinetics of Cu-8Cr-4Nb was investigated by TGA (thermogravimetric) exposures between 500 and 900-C (at 25-50 C intervals) and the oxide scale morphologies examined by microscopy and micro-analysis. Because Cu-8Cr-4Nb is comprised of fine Cr2Nb precipitates in a Cu matrix, the results were interpreted by comparison with the behavior of copper (OFHC) and 'NARloy-Z' (a rival candidate material for thrust cell liner applications in advanced rocket engines) under the same conditions. While NARloy-Z and Cu exhibited identical oxidation behavior, Cu-8Cr-4Nb differed markedly in several respects: below approx. 700 C its oxidation rates were significantly lower than those of Cu; At higher temperatures its oxidation rates fell into two categories: an initial rate exceeding that of Cu, and a terminal rate comparable to that of Cu. Differences in oxide morphologies paralleled the kinetic differences at higher temperature: While NARloy-Z and Cu produced a uniform oxide scale of Cu2O inner layer and CuO outer layer, the inner (Cu2O) layer on Cu-8Cr-4Nb was stratified, with a highly porous/spongy inner stratum (responsible for the fast initial kinetics) and a dense/blocky outer stratum (corresponding to the slow terminal kinetics). Single and spinel oxides of Nb and Cr were found at the interface between the oxide scale and Cu-8Cr-4Nb substrate and it appears that these oxides were responsible for its suppressed oxidation rates at the intermediate temperatures. No difference was found between Cu-8Cr-4Nb oxidation in air and in oxygen at 1.0 atm.

Thomas-Ogbuji, L. U.↗
NASA NTRS2008

Comparison of the Isothermal Oxidation Behavior of As-Cast Cu-17%Cr and Cu-17%Cr-5%Al: Oxidation Kinetics - Part 1

The isothermal oxidation kinetics of as-cast Cu-17%Cr and Cu-17%Cr-5%Al in air were studied between 773 and 1173 K under atmospheric pressure. These observations reveal that Cu- 17%Cr-5%Al oxidizes at significantly slower rates than Cu-17%Cr. The rate constants for the alloys were determined from generalized analyses of the data without an a priori assumption of the nature of the oxidation kinetics. Detailed analyses of the isothermal thermogravimetric weight change data revealed that Cu-17%Cr exhibited parabolic oxidation kinetics with an activation energy of 165.9 +/- 9.5 kJ/mol. In contrast, the oxidation kinetics for the Cu-17%Cr- 5%Al alloy exhibited a parabolic oxidation kinetics during the initial stages followed by a quartic relationship in the later stages of oxidation. Alternatively, the oxidation behavior of Cu-17%CR- 5%Al could be better represented by a logarithmic relationship. The parabolic rate constants and activation energy data for the two alloys are compared with literature data to gain insights on the nature of the oxidation mechanisms dominant in these alloys.

Raj. Sai V.↗
NASA NTRS2008

Comparison of the Isothermal Oxidation Behavior of As-Cast Cu-17%Cr and Cu-17%Cr-5%Al: Oxidation Kinetics - Part 1

The isothermal oxidation kinetics of as-cast Cu-17%Cr and Cu-17%Cr-5%Al in air were studied between 773 and 1173 K under atmospheric pressure. These observations reveal that Cu- 17%Cr-5%Al oxidizes at significantly slower rates than Cu-17%Cr. The rate constants for the alloys were determined from generalized analyses of the data without an a priori assumption of the nature of the oxidation kinetics. Detailed analyses of the isothermal thermogravimetric weight change data revealed that Cu-17%Cr exhibited parabolic oxidation kinetics with an activation energy of 165.9 9.5 kJ mol-1. In contrast, the oxidation kinetics for the Cu-17%Cr- 5%Al alloy exhibited a parabolic oxidation kinetics during the initial stages followed by a quartic relationship in the later stages of oxidation. Alternatively, the oxidation behavior of Cu-17%CR- 5%Al could be better represented by a logarithmic relationship. The parabolic rate constants and activation energy data for the two alloys are compared with literature data to gain insights on the nature of the oxidation mechanisms dominant in these alloys.

Raj. Sai V.↗
NASA NTRS1988

Transport critical current and magnetization measurements of melt-processed YBa2Cu3O(7-x)

This paper reports on the magnetic field dependence of the transport critical current and dc magnetic susceptibility measurements on YBa2Cu3O(7-x) superconductors formed by melt-solid reactions at 950 C between Ba-Cu-O (or Tb-Ba-cu-O) and solid nonstoichiometric Y-Ba-Cu oxide. Four-probe dc critical current measurements at 77, 64, and 4.2 K show strong depression of the critical current density with increasing magnetic field, in agreement with a model of weakly linked superconducting regions. Diamagnetic shielding and Meissner flux expulsion measurements in the temperature range 10-300 K show about one-third volume fraction of perfect superconductivity. Both shielding and flux expulsion were observed to be approximately temperature independent below 60 K, indicating strong coupling between the grains throughout the entire volume below this temperature.

Hermann, A. H.↗
NASA NTRS1990

Electronic structure Fermi liquid theory of high T(sub c) superconductors: Comparison with experiments

For years, there has been controversy on whether the normal state of the Cu-oxide superconductors is a Fermi liquid or some other exotic ground state. However, some experimentalists are clarifying the nature of the normal state of the high T(sub c) superconductors by surmounting the experimental difficulties in producing clean, well characterized surfaces so as to obtain meaningful high resolved photoemission data, which agrees with earlier positron-annihilation experiments. The experimental work on high resolution angle resolved photoemission by Campuzano et al. and positron-annihilation studies by Smedskjaer et al. has verified the calculated Fermi surfaces in YBa2Cu3O7 superconductors and has provided evidence for the validity of the energy band approach. Similar good agreement was found for Bi2Sr2CaCu2O8 by Olson et al. As a Fermi liquid (metallic) nature of the normal state of the high T(sub c) superconductors becomes evident, these experimental observations have served to confirm the predictions of the local density functional calculations and hence the energy band approach as a valid natural starting point for further studies of their superconductivity.

Freeman, A. J.↗
NASA NTRS1991

Processing Bi-Pb-Sr-Ca-Cu-O superconductors from amorphous state

The bismuth based high T sub c superconductors can be processed via an amorphous Bi-Pb-Sr-Ca-Cu oxide. The amorphous oxides were prepared by melting the constituent powders in an alumina crucible at 1200 C in air followed by pouring the liquid onto an aluminum plate, and rapidly pressing with a second plate. In the amorphous state, no crystalline phase was identified in the powder x ray diffraction pattern of the quenched materials. After heat treatment at high temperature the amorphous materials crystallized into a glass ceramic containing a large fraction of the Bi2Sr2Ca2Cu3O(x) phase T sub c = 110 K. The processing method, crystallization, and results of dc electrical resistivity and ac magnetic susceptibility measurements are discussed.

Chiang, C. K.↗
NASA NTRS1992

Interaction of atomic oxygen with thin film and bulk copper: An XPS, AES, XRD, and profilometer study

The University of Alabama in Huntsville (UAH) experiment A-0114 was designed primarily to study degradation of material surfaces due to low earth orbital (LEO) atmospheric oxygen. The experiment contained 128 one inch circular samples: metals, polymers, carbons, and semiconductors. Among metal samples, copper has shown some interesting new results. Two types of copper samples, a film sputter coated on fused silica and a bulk piece of OFHC copper, were characterized employing a variety of techniques such as X-ray and Auger electron spectroscopies, X-ray diffraction, and high resolution profilometry. Cu 2p core level spectra were used to characterize the presence of Cu2O and CuO in addition to Cu Auger LMM lines. These results are supported by our recent X-ray diffraction studies which clearly establish the presence of Cu oxides which we were unable to prove in our earlier work. Profilometry showed an increase in thickness of the film sample where exposed to 106.7 +/- 0.5 nm from an initial thickness of 74.2 +/- 1.1 nm. Further studies with SEM and ellipsometry are underway.

Raikar, Genesh N.↗
NASA NTRS1991

Crystal growth of YBa2Cu3O(7-x) and reaction of gold crucible with Ba-Cu-rich flux

YBa2Cu3O(7-x) crystals are grown in a gold crucible by a self-flux method. The flux moves along the gold surface due to surface wetting and leaves Y123 crystals behind. The obtained crystals are clean and have a size up to two millimeters and a Tc is greater than 90 K. In an effort to recycle the used crucibles, it is found that the used gold is contaminated by copper. A CuO thin film is easily formed on the surface of the crucible that is made of the used gold. This film provides good surface wetting and a buffer layer, which reduces the reaction between gold and the Y-Ba-Cu-oxide melt.

Tao, Y. K.↗
NASA NTRS2008

Comparison of the Isothermal Oxidation Behavior of As-Cast Cu-17 Percent Cr and Cu-17 Percent Cr-5 Percent Al: Oxidation Kinetics - Part 1

The isothermal oxidation kinetics of as-cast Cu-17%Cr and Cu-17%Cr-5%Al in air were studied between 773 and 1173 K under atmospheric pressure. These observations reveal that Cu-17%Cr-5%Al oxidizes at significantly slower rates than Cu-17%Cr. The rate constants for the alloys were determined from generalized analyses of the data without an a priori assumption of the nature of the oxidation kinetics. Detailed analyses of the isothermal thermogravimetric weight change data revealed that Cu-17%Cr exhibited parabolic oxidation kinetics with an activation energy of 165.9+/-9.5 kJ/mol. In contrast, the oxidation kinetics for the Cu-17%Cr-5%Al alloy exhibited a parabolic oxidation kinetics during the initial stages followed by a quartic relationship in the later stages of oxidation. Alternatively, the oxidation behavior of Cu-17%CR-5%Al could be better represented by a logarithmic relationship. The parabolic rate constants and activation energy data for the two alloys are compared with literature data to gain insights on the nature of the oxidation mechanisms dominant in these alloys.

Raj, S. V.↗
NASA NTRS1990

Ternary and quaternary oxides of Bi, Sr, and Cu

Before the discovery of superconductivity in an oxide of Bi, Sr, and Cu, the system Bi-Sr-Cu-O had not been studied, although several solid phases had been identified in the two-component regions of the ternary system Bi2O3-SrO-CuO. The oxides Sr2CuO3, SrCu2O2, SrCuO2, and Bi2CuO4 were then well known and characterized, and the phase diagram of the binary system Bi2O3 -SrO had been established in the temperature range 620 to 1000 C. Besides nine solutions of compositions Bi(2-2x) Sr(x) O(3-2x) and different symmetries, this diagram includes three definite compounds of stoichiometries Bi(2)SrO4, Bi2Sr2O5, and Bi2Sr3O6 (x = 0.50, 0.67 and 0.75 respectively), only the second of which with known unit-cell of orthorhombic symmetry, dimensions (A) a = 14.293(2), b = 7.651(2), c = 6.172(1), and z = 4. The first superconducting oxide in the system Bi-Sr-Cu-O was initially formulated as Bi2Sr2Cu2O(7+x), with an orthorhombic unit-cell of parameters (A) a = 5.32, b = 26.6, c = 48.8. In a preliminary study the same oxide was formulated with half the copper content, Bi(2)Sr(2)CuO(6+x), and indexed its reflections assuming an orthorhombic unit-cell of dimensions (A) a = 5.390(2), b = 26.973(8), c = 24.69(4). Subsequent studies by diffraction techniques have confirmed the composition 2:2:1. A new family of oxygen-deficient perovskites, was characterized, after identifying by x ray diffraction the phases present in the products of thermal treatments of about 150 mixtures of analytical grade Bi2O3, Sr(OH)2-8H2O and CuO at different molar ratios. X ray diffraction data are presented for some other oxides of Bi and Sr, as well as for various quaternary oxides, among them an oxide of Bi, Sr, and Cu.

Casais, M. T.↗
NASA NTRS1991

Ternary and quaternary oxides of Bi, Sr and Cu

Before the discovery of superconductivity in an oxide of Bi, Sr, and Cu, the system Bi-Sr-Cu-O had not been studied, although several solid phases had been identified in the two-component regions of the ternary system Bi2O3-Si-O-CuO. The oxides Sr2CuO3, SrCu2O2, SrCuO2, and Bi2CuO4 were then well known and characterized, and the phase diagram of the binary system Bi2O3-SrO had been established in the temperature range 620 to 1000 C. Besides nine solutions of compositions Bi(2-2x) Sr(x) O(3-2x) and different symmetries, this diagram includes three definite compounds of stoichiometries Bi(2)BrO4. Bi2Sr2O5, and Bi2Sr3O6 (x - 0.50, 0.67 and 0.75 respectively), only the second of which with known unit-cell of orthorhombic symmetry, dimensions (A) a = 14.293(2), b = 7.651(2), c = 6.172(1), and z = 4. The first superconducting oxide in the system Bi-Sr-Cu-O was initially formulated as Bi2Sr2Cu2O(7+x), with an orthorhombic unit-cell of parameters (A) a = 5.32, b = 26.6, c = 48.8. In a preliminary study the same oxide was formulated with half the copper content, Bi(2)Sr(2)CuO(6+x), and index its reflections assuming an orthorhombic unit-cell of dimensions (A) a = 5.390(2), b = 26.973(8), c = 24.69(4). Subsequent studies by diffraction techniques have confirmed the composition 2:2:1. A new family of oxygen-deficient perovskites, was characterized, after identifying by x ray diffraction the phases present in the products of thermal treatments of about 150 mixtures of analytical grade Bi2O3, Sr(OH)2-8H2O and CuO at different molar ratios. X ray diffraction data are presented for some other oxides of Bi and Sr, as well as for various quaternary oxides, among them an oxide of Bi, Sr, and Cu.

Casais, M. T.↗
NASA NTRS2000

Oxidation Behavior of GRCop-84 (Cu-8Cr-4Nb) at Intermediate and High Temperatures

The oxidation behavior of GRCop-84 (Cu-8 at %Cr-4 at %Nb) has been investigated in air and in oxygen, for durations of 0.5 to 50 hours and temperatures ranging from 500 to 900 C. For comparison, data was also obtained for the oxidation of Cu and NARloy-Z (Cu-3 wt% Ag-0.5 wt% Zr) under the same conditions. Arrhenius plots of those data showed that all three materials had similar oxidation rates at high temperatures (> 750 C). However, at intermediate temperatures (500 to 750 C) GRCop exhibited significantly higher oxidation resistance than Cu and NARloy-Z. The oxidation kinetics of GRCop-84 exhibited a sharp and discontinuous jump between the two regimes. Also, in the high temperature regime GRCop-84 oxidation rate was found to change from a high initial value to a significantly smaller terminal value at each temperature, with progress of oxidation; the two different oxidation rates were found to correlate with a porous intial oxide and a dense final oxide, respectively.

Thomas-Ogbuji, Linus U.↗
NASA NTRS1988

Effects of oxidation and roughness on Cu contact resistance from 4 to 290 K

Knowledge of the factors influencing contact resistance is important for optimizing system design in cryogenic applications. In space cryogenics, indirect cooling of infrared components is the primary concern. The presence of bolted joints results in contact resistances which can dominate all other contributions to the overall heat transfer rate. Here, thermal and electrical contact resistances measured between 4 K and 290 K for a series of bolted OFHC Cu contacts are reported. Surface roughness is found to have little effect on the overall contact resistance within the experimental limits, while oxidation can increase the contact resistance by as much as a factor of 100. Thermal and electrical contact resistances measured on the same contact show that the contact resistance temperature dependence does not follow the bulk dependence. For example, the residual resistance ratio (RRR) of the OFHC Cu is 110, but for contacts made from this material, the RRR is about two.

Nilles, M. J.↗
NASA NTRS2008

Comparison of the Isothermal Oxidation Behavior of As-Cast Cu-17 Percent Cr and Cu-17 Percent Cr-5 Percent Al: Scale Microstructures - Part 2

The isothermal oxidation kinetics of as-cast Cu-17%Cr and Cu-17%Cr-5%Al in air were studied between 773 and 1173 K under atmospheric pressure. Details of the oxidation kinetics of these alloys were discussed in Part I. This paper analyzes the microstructures of the scale and its composition in an attempt to elucidate the oxidation mechanisms in these alloys. The scales formed on Cu-17%Cr specimens oxidized between 773 and 973 K consisted of external CuO and subsurface Cu2O layers. The total thickness of these scales varied from about 10 m at 773 K to about 450 m at 973 K. In contrast, thin scales formed on Cu-17%Cr-5%Al alloys oxidized between 773 and 1173 K. The exact nature of these scales could not be determined by x-ray diffraction but energy dispersive spectroscopy analyses were used to construct a scale composition map. Phenomenological oxidation mechanisms are proposed for the two alloys.

Raj, S. V.↗