Microstructural stability and nanoindentation of an electrodeposited nanocrystalline Ni-1.5wt.%P alloy

Microstructural stability of nanocrystalline Ni-1.5wt.%P alloy with an initial grain size of 3 nm processed by pulsed electrodeposition was studied using differential scanning calorimetry (DSC) and annealing. Microstructural characterization suggests that the observed exothermic peak during heating in DSC is related to both concurrent grain growth and Ni3P formation. Nanoindentation on samples with grain sizes from 3 to 50 nm revealed a breakdown in Hall-Petch strengthening in nano Ni-P alloy at grain sizes <= 10 nm, consistent with some previous observations. It is concluded that there is a grain boundary weakening regime for grain sizes < 10 nm, based on analysis which show that the data cannot be rationalized in terms of microstrain relaxation, variation in elastic modulus, texture evolution and duplex structure formation.

Electron microscopy and diffraction of ordering in Ni---W alloys

Electron microscopy and diffraction studies of ordering in stoichiometric Ni-20%W and off-stoichiometric Ni-15%W alloys have been carried out. The specimens of Ni-20%W were first disordered at 1398 K for 4 h and then quenched rapidly into water. Short range order (SRO) spots were observed at {1 1/2 0}* positions. Two hitherto unknown metastable phases: D-2h(25)-Ni2W and DO22-Ni3W were observed in the diffraction patterns. Long range order (LRO) transformations were studied at 1103 and 1213 K. Kinetics and mechanism of transformations have been identified. Ni-15%W specimens were solution treated at 1523 K for 1 h followed by quenching in water. SRO spots similar to those found in Ni-20%W were observed in this alloy as well. The transition to LRO was studied at 1093 K. Distinct Ni4W precipitates could be observed after 5 h of annealing at this temperature. After 100 h of annealing precipitates were found to grow into faceted shape coherent with the disordered matrix. After prolonged annealing for over 150 h the Ni4W precipitates began to lose coherency by the generation of misfit dislocations. The microstructural observations have been compared for the stoichiometric and off-stoichiometric alloys.

Superconducting properties of Tl1?yPbyCaSr2Cu2O7: Role of Pb and oxygen stoichiometry

In the Tl1-yPbyCaSr2Cu2O7 system, monophasic superconducting compositions are formed in the range 0.25 < y < 0.60 and the minimum Pb content required to stabilize the tetragonal 1122 phase is about 25%. Maximum Tc is found when y = 0.5, at which composition the hole concentration is optimal. Metallic compositions of Tl1?yPbyCaSr2Cu2O7 (y = 0.25) and Tl0.75Pb0.25Y1?xCaxSr2Cu2O7 (0.80 less-than-or-equals, slant X less-than-or-equals, slant 1.0) become superconducting on decreasing the oxygen content by vacuum annealing.

Optical and electrical properties of hydrogen-passivated gallium antimonide

The effect of hydrogen-plasma passivation on the optical and electrical properties of gallium antimonide bulk single crystals is presented. Fundamental changes of the radiative recombination after hydrogenation in undoped, zinc-doped, tellurium-doped, and codoped (with Zn and Te) GaSb are reported. The results of optical measurements indicate that passivation of acceptors is more efficient than that of the donors and, in general, the passivation efficiency depends on the doping level. Passivation of deep nonradiative centers is reflected by the gain of photoluminescence intensity and decrease in deep-level transient spectroscopy peak height. Extended defects like grain boundaries and dislocations have also been found to be passivated. The thermal stability of the passivated deep level and extended defects is higher than that of the shallow level. The kinetics of thermally released hydrogen in the bulk has been studied by reverse-bias annealing experiments.

Rapid thermal processed thin films of niobium pentoxide (Nb2 O5) deposited by reactive magnetron sputtering

Niobium pentoxide thin films have been deposited on silicon and platinum-coated silicon substrates by reactive magnetron sputtering. The as-deposited films were amorphous and showed good electrical properties in terms of a dielectric permittivity of about 30, and leakage current density of 10(-6) A cm(-2) al a field of 120 kV cm(-1). A rapid thermal annealing process at 800 degrees C further increased the dielectric constant to 90 and increased the leakage current density to 5 x 10(-6) A cm(-2). The current-voltage characteristics observed at low and high fields suggested a combination of phenomena at different regimes of applied electric field. The capacitance-voltage characteristics performed in the metal-insulator-semiconductor configuration indicated good electronic interfaces with a nominal trap density of 4.5 x 10(12) cm(-2) eV(-1), which is consistent with the behavior observed with conventional dielectrics such as SiO2 on silicon surfaces.

Rapid thermal processed thin films of reactively sputtered Ta2O5

Rapid thermal processed thin films of reactively sputtered tantalum pentoxide Ta2O5 thin films have been deposited on silicon and platinum coated silicon substrates by reactive magnetron sputtering. The as-deposited films were amorphous and showed good electrical properties in terms of a dielectric permittivity of about 24 and leakage current density of 9 x 10(-8) A cm(-2). A rapid thermal annealing process at temperatures above 700 degrees C crystallized the films, increased the dielectric relative permittivity, and decreased the leakage current. The dielectric constant for a film rapidly annealed at 850 degrees C increased to 45 and its leakage current density lowered to 2 x 10(-8) A cm(-2). The dielectric measurements in the MIS configuration showed that Ta2O5 might be used as a dielectric material instead of SiO2 or Si3N4 for integrated devices. The current voltage characteristics observed at low and high fields suggested different conduction mechanisms.

Retarding effect of surface hydroxylation on titanium(IV) oxide photocatalyst in the degradation of phenol

Nanosized powders of TiO2 (anatase) were prepared by the hydrothermal method, acid-medium hydrolysis or by vacuum freeze-drying of sols, and annealing at temperatures <700-degrees-C. Photocatalytic activities of these powders in the mineralization of phenol, were evaluated in comparison to that of Degussa P25. Kinetic data indicated that surface hydroxylation had a retarding effect on the degradation of phenol. Formation of stable peroxotitanium species were observed on hydroxylated powders, whereas only V(Ti)-O- hole trap centres were detected by EPR on the heat treated samples. The data supports direct hole oxidation of the substrate preadsorbed on the photocatalyst, which is otherwise blocked by surface hydroxyls.

Structural and electrical transport properties of Al-Cu-Cr quasicrystals

Transport properties of quasicrystals in rapidly solidified as well as heat-treated Al65CU20Cr15 alloys were studied over a wide temperature range as a function of structure and microstructure. The characterization was done using x-ray diffraction, transmission electron microscopy and differential scanning calorimetry. Particular attention was paid to primitive to face-centered quasicrystalline transformation which occurs on annealing and the effect of microstructures on the transport behavior. The temperature dependence of resistivity is found to depend crucially on the microstructure of the alloy. Further, ordering enhances the negative temperature coefficient of resistivity. The low-temperature (T less than or equal to 25 K) resistivity of Al65Cu20Cr15 has been compared with that of Al63.5Cu24.5Fe12 alloy. In this region p(T) can be well described by a root T contribution arising from electron-electron interaction. We discuss our results in view of current theories.

Reactivation kinetics of boron acceptors in hydrogenated silicon during zero bias anneal

The reactivation kinetics of passivated boron accepters in hydrogenated silicon during zero bias annealing in the temperature range of 65-130 degrees C are reported, For large annealing times and high annealing temperatures, the reactivation process follows second-order kinetics and is rate limited by a thermally activated <(H)over tilde (2)> complex formation process, For short annealing times and low annealing temperatures, the reactivation rate is found to be larger than that due to <(H)over tilde (2)> complex formation alone. We conclude that the faster reactivation is caused by the diffusion of the liberated hydrogen atoms into the bulk as well as <(H)over tilde (2)> complex formation. The effective diffusion coefficient of hydrogen is measured and found to obey the Arrhenius relation with an activation energy (1.41 +/- 0.1) eV. (C) 1997 American Institute of Physics.

Studies on structural and electrical properties of barium strontium titanate thin films developed by metallo-organic decomposition

Thin films of barium strontium titanate (BST) including BaTiO3 and SrTiO3 end members were deposited using the metallo-organic decomposition (MOD) technique. Processing parameters such as nonstoichiometry, annealing temperature and time, film thickness and doping concentration were correlated with the structural and electrical properties of the films. A random polycrystalline structure was observed for all MOD films under the processing conditions in this study. The microstructures of the films showed multi-grains structure through the film thickness. A dielectric constant of 563 was observed for (Ba0.7Sr0.3)TiO3 films rapid thermal annealed at 750 degrees C for 60 s. The dielectric constant increased with annealing temperature and film thickness, while the dielectric constant could reach the bulk values for thicknesses as thin as similar to 0.3 mu m. Nonstoichiometry and doping in the films resulted in a lowering of the dielectric constant. For near-stoichiometric films, a small dielectric dispersion obeying the Curie-von Schweidler type dielectric response was observed. This behavior may be attributed to the presence of the high density of disordered grain boundaries. All MOD processed films showed trap-distributed space-charge limited conduction (SCLC) behavior with slope of similar to 7.5-10 regardless of the chemistry and processing parameter due to the presence of main boundaries through the film thickness. The grain boundaries masked the effect of donor-doping, so that all films showed distributed-trap SCLC behavior without discrete-traps. Donor-doping could significantly improve the time-dependent dielectric breakdown behavior of BST thin films, mostly likely due to the lower oxygen vacancy concentration resulted from donor-doping. From the results of charge storage density, leakage current and time-dependent dielectric breakdown behavior, BST thin films are found to be promising candidates for 64 and 256Mb ULSI DRAM applications. (C) 1997 Elsevier Science S.A.

Radiation induced modifications on microstructure and related properties of high temperature superconductor YBCO

Role of swift heavy ion irradiation on the modification of transport and structural properties of high temperature superconductors is studied. Good quality YBCO thin films prepared by high pressure oxygen sputtering and laser ablation were used in this investigation. Resistivity and atomic force microscopy (AFM) were mainly used to probe superconducting and microstructural modifications resulted from the irradiation of high energy and heavy ions like 100 MeV oxygen and 200 MeV silver. Radiation induced sputtering or erosion is likely to be a major disastrous component of such high energy irradiation that could be powerful in masking phase coherence effects, atleast in grain boundaries. The extent of damage/nature of defects other than columnar defects produced by swift heavy ions is discussed in the light of AFM measurements. The effect of high energy oxygen ion irradiation is anomalous. A clear annealing effect at higher doses is seen. (C) 1999 Elsevier Science B.V. All rights reserved.

Tensile flow behaviour of 2.25Cr-1Mo ferritic steel base metal and simulated heat affected zone structures of 2.25Cr-1Mo weld joint

Tensile tests in the temperature range 298 to 873 K have been performed on 2.25Cr-1Mo base metal and simulated heat affected zone (HAZ) structures of its weld joint, namely coarse grain bainite, fine grain bainite and intercritical structure. Tensile flow behaviour of all the microstructural conditions could be adequately described by the Hollomon equation (sigma = K-1 epsilon(n1)) at higher (> 623 K) temperatures. Deviation from the Hollomon equation was observed at low strains and lower (< 623 K) temperatures. The Ludwigson modification of Hollomon's equation, sigma = K-1 epsilon(n1) + exp (K-2 + n(2) epsilon), was found to describe the flow curve. In general, the flow parameters n(1), K-1, n(2) and K-2 were found to decrease with increase in temperature except in the intermediate temperature range (423 to 623 K). Peaks/plateaus were observed in their variation with temperature in the intermediate temperature range coinciding with the occurrence of serrated flow in the load-elongation curve. The n(1) Value increased and the K-1 value decreased with the type of microstructure in the order: coarse grain bainite, fine grain bainite, base metal and intercritical structure. The variation of nl with microstructure has been rationalized on the basis of mean free path (MFP) of dislocations which is directly related to the inter-particle spacing. Larger MFP of dislocations lead to higher strain hardening exponents n(1).

Insulator-metal transition and magnetoresistance of La0.5Ca0.5MnOy induced by tuning the oxygen content

The oxygen content of La0.5Ca0.5MnOy was tuned by annealing the samples at high temperatures in flowing nitrogen with graphite powder nearby. The reduction of oxygen content has dramatic effect on the electrical transport and magnetic properties. The samples with y=2.983, 2.83, and 2.803 show an insulator-metal transition, and an unusual temperature and magnetic-field dependence of the magnetoresistance. The paramagnetic-ferromagnetic transition also shifts to lower temperatures and the antiferromagnetic transition at lower temperature is suppressed. The results are discussed in terms of the effect of oxygen vacancies on the various properties of La0.5Ca0.5MnOy. (C) 2002 American Institute of Physics.

Magnetically tunable nonlinear current-voltage characteristics in oxygen deficient manganite perovskites

(La0.667Ca0.333Mn1-xMO3-delta)-O-x (M = Mg, Li or Re) exhibit insulating behaviour and nonlinear current-voltage (J-E) relationship with voltage-limiting characteristics at temperatures below the ferromagnetic transition (T-c). The high current region is set in at field strengths <60 V/cm. Nonlinearity exponent, alpha in the relation J = kE(alpha) increases inversely with temperature. In presence of an external magnetic field, the J-E curves show higher current density at lower field strengths. Microstructural studies indicate that there is no segregation of secondary phases in the grain boundary regions. There is remarkable changes in p(T) as well as J-E curves with the grain size. Annealing studies in lower p(O2) atmospheres indicate that there is significant out-diffusion of oxygen ions through the grain boundary layer (GBL) regions creating oxygen vacancies in the GBL regions. The concentration of Mn4+ ions is lowered at the GBL due to oxygen vacancies, reducing the probability of hopping and resulting in insulating behaviour. Therefore an insulating barrier is introduced between two conducting grains and the carrier motion between the grains is inhibited. Thus below T-c, where sufficient increase in resistivity is observed the conduction may be arising as a result of spin dependent tunneling across the barrier. External electric field lowers the barrier height and establishes carrier transport across the barrier. Above certain field strength, barrier height diminishes significantly and thereby allowing large number of carriers for conduction, giving rise to highly nonlinear conductivity. (C) 2002 Elsevier Science B.V. All rights reserved.

Phase transformation and semiconductor-metal transition in thin films of VO2 deposited by low-pressure metalorganic chemical vapor deposition

Thin films of the semiconducting, monoclinic vanadium dioxide, VO2(M) have been prepared on ordinary glass by two methods: directly by low-pressure metalorganic chemical vapor deposition (MOCVD), and by argon-annealing films of the VO2(B) phase deposited by MOCVD. The composition and microstructure of the films have been examined by x-ray diffraction, scanning electron microscopy, and transmission electron microscopy. Films made predominantly of either the B or the M phase, as deposited, can only be obtained over a narrow range of deposition temperatures. At the lower end of this temperature range, the as-deposited films are strongly oriented, although the substrate is glass. This can be understood from the drive to minimize surface energy. Films of the B phase have a platelet morphology, which leads to an unusual microstructure at the lower-deposition temperatures. Those grown at similar to370 degreesC convert to the metallic, rutile (R) phase when annealed at 550 degreesC, whereas those deposited at 420 degreesC transform to the R phase only at 580 degreesC. (When cooled to room temperature, the annealed films convert reversibly from the R phase to the M phase.) Electron microscopy shows that annealing leads to disintegration of the single crystalline VO2(B) platelets into small crystallites of VO2(R), although the platelet morphology is retained. When the annealing temperature is relatively low, these crystallites are nanometer sized. At a higher-annealing temperature, the transformation leads to well-connected and similarly oriented large grains of VO2(R), enveloped in the original platelet. The semiconductor-metal transition near 68 degreesC leads to a large jump in resistivity in all the VO2(M) films, nearly as large as in epitaxial films on single-crystal substrates. When the annealed films contain well-connected large grains, the transition is very sharp. Even when preferred orientation is present, the transition is not as sharp in as-deposited VO2(M), because the crystallites are not densely packed as in annealed VO2(B). However, the high degree of orientation in these films leads to a narrow temperature hysteresis. (C) 2002 American Institute of Physics.