Yttrium barium copper oxide thin films on yttria-stabilized zirconia: growth and properties

Y Ba Cu oxide thin films were grown epitaxially on single cryst. yttria-stabilized zirconia substrates by laser deposition. [on SciFinder(R)]

Very thin yttrium barium copper oxide films made by coevaporation

Superconducting YBa2Cu3O7 thin films with various thicknesses from 100 Å to 5000 Å were deposited on (100) SrTiO3 substrates with std. BaF2 coevaporation process. The films had crit. temps. of up to 93 K. The best crit. currents were 1 × 106 A/cm2 at 77 K and 3 × 107 A/cm2 at 4.2 K. The crit. current was generally higher for thinner films. Two different etching methods were used to pattern the films for jc measurements: Ar ion etching and EDTA wet etching. The wet etching was found to work well for thicker films (>1000 Å). For the thinner films, the ion etching process was preferred because of the reduced film surface degrdn. [on SciFinder(R)]

Melt textured Y123 bulk and thick film

YBa2Cu3O7-δ - 25mol%Y2BaCuO5 bars and thick films have been melt textured using a stationary furnace with a temperature gradient of 3 or 6°C/cm. Samples are heated above the peritectic reaction temperature and quenched to just above the solidification temperature and then slowly cooled below the solidification temperature. All bar shaped samples consist of 2-5 mm grains though the grain orientations strongly depend on the heat treatment conditions. The bar shows the maximum Jc of above 3,000 A/cm2, whereas the maximum Jc of 200 A/cm2 and Tczero of 88K are obtained for the thick film on (100) LaAlO3 single crystal.

The formation of YBa2Cu3O7-x in melt-texture heat treatments

A study of the bulk formation of YBa2Cu3O7-x from the Y2BaCuO5 plus liquid regime reveals that phase formation occurs at appreciable rates below 950°C in air. This result has been observed for phase-pure YBa2Cu3O7-x starting material given two types of heat treatment: held at 1100°C and slow-cooled from 1030°C at 6°C/h or heat-treated isothermally. Differential thermal analysis, with a cooling rate of 10°C/min indicates that the degree of undercooling for the peritectic formation of YBa2Cu3O7-x is greater than 100°C. © 1994.

The extrusion of continuous lengths of YBa2Cu3O7-x wire using hydroxypropyl methylcellulose

Wires of YBa2Cu3O7-x were fabricated by extrusion using a hydroxypropyl methylcellulose (HPMC) binder. As little as 2 wt.% binder was added to an oxide prepared by a novel co-precipitation process, to produce a plastic mass which readily gave continuous extrusion of long lengths of wire in a reproducible fashion. Critical temperatures of 92K were obtained for wires given optimum high-temperature heat treatments. Critical current densities greater than 1000 A cm-1 were measured at 77.3K using heat treatments at around 910°C for 10h. These transport critical current densities, measured on centimeter-long wires, were obtained with microstructures showing a relatively dense and uniform distribution of randomly oriented, small YBa2Cu3O7-x grains. © 1993.

YBCO thin films on Yttria stabilized Zirconia and LaAlO3-growth and properties

Laser deposition was used to deposit YBaCuO thin films on Yttria-stabilized Zirconia substrates, at substrate holder temperatures of 710-765 °C. We observed a transition from singlecrystalline to polycrystalline growth at a temperature of ∼750 °C. All films were highly c-axis oriented and had critical temperatures between 89.5 and 92 K. In the twinned singlecrystalline films, the lowest measured microwave surface resistance was 0.37 mΩ at 4.2 K and 21.5 GHz, and the highest critical current 5×106 A/cm2 at 77 K. The polycrystalline films had up to a factor of 50 higher surface resistance and a factor of 10 lower critical current. A meander line resonator made of a film on a LaAlO3 substrate, showed a microwave surface resistance of 5μΩ at 4.2 K and 2.5 GHz. © 1991.

Sintering and densification mechanisms of Y2BaCuO5 pellets

The sintering and densification of Y2BaCuO5 (Y-211) pellets made from powders with different characteristics have been investigated in the temperature range 1000-1140°C. A pellet made from powder containing Ba-rich secondary phases shows very early liquid-assisted sintering and densification and clear evidence of exaggerated grain growth. The melting of BaCuO2 and YBa2Cu3O7-δ (Y-123) secondary phases increases the rate of densification of Y-211 pellets made from other powders at temperatures above 1025-1030°C. All the liquid produced by the melting of the latter phases recrystallizes as intergranular layers of Y-123. These intergranular layers account for the darker appearance and for measurable electrical conductivities at room temperature of the pellets sintered at the higher temperatures. The development of exaggerated grain growth within a uniform fine-grained matrix opens the possibility of using controlled secondary recrystallization to obtain large single domains of Y-211, provided that the trapping of porosity can be avoided or minimized. © 1999 Elsevier Science S.A.

Observation of exsolution textures within Ba-Cu-O-rich solidified melts of Y-Ba-Cu-O materials and their relationship to Y123 nucleation and texturing

Layers (about 60-100 μm thick) of almost pure BaCuO2 (BC1), as determined using X-ray diffractometry (XRD) and scanning electron microscopy (SEM), coat the surfaces of YBa2Cu3O7-x (Y123) samples partial melt processed using a single-zone vertical furnace. The actual Cu/Ba ratio of the BC1 phase is 1.2-1.3 as determined using energy dispersive X-ray spectrometry (EDS). The nominally BC1 phase displays an exsolution of BC1.5 or BC2 in the form of thin plates (about 50-100 nm thick) along {100}-type cleavage planes or facets. The exsolved phase also fills cracks within the BC1 layer that require it to be in a molten state at some stage of processing. The samples were influenced by Pt contamination from the supporting wire, which may have stabilised the BC1.5 phase. Many of the Y123 grains have the same morphology as the exsolution domains, and run nearly parallel to the thin plates of the exsolved phases, strongly indicating that Y123 nucleation took place at the interface between the BC1 and the BC1.5 or BC2 exsolved phases. The network of nearly parallel exsolved 'channels' provides a matrix and a mechanism through which a high degree of local texture can be initiated in the material.

Study of in situ laser deposited YBCO thin films

YBCO thin films were fabricated by laser deposition, in situ on MgO substrates, using both O2 and N2O as process gas. Films with Tc above 90 K and jc of 106 A/cm2 at 77 K were grown in oxygen at a substrate temperature of 765 °C. Using N2O, the optimum substrate temperature was 745 °C, giving a Tc of 87 K. At lower temperatures, the films made in N2O had higher Tc (79 K) than the films made in oxygen (66 K). SEM and STM investigations of the film surfaces showed the films to consist of a comparatively smooth background surface and a distribution of larger particles. Both the particle size and the distribution density depended on the substrate temperature.

Phase composition of the rapidly quenched melt of YBa2Cu3O7-y+20 mol% Y2BaCuO5

Samples of YBa2Cu3O7-y+20 mol% Y2BaCuO5, with thicknesses ranging between 50-250 μm, have been melt processed and rapidly quenched from temperatures between 985 and 1100°C by immersing them in liquid nitrogen. The phase composition and microstructures of these samples have been characterised using a combination of X-ray diffractometry, optical microscopy and scanning electron microscopy with energy dispersive X-ray spectroscopy. The quenched melt of samples quenched from temperatures greater than 985°C appears relatively homogeneous but consists of Ba2Cu3Ox (BC1.5) and BaCu2O2 (BC2) regions. At about 985°C, BaCuO2 (BC1) crystallises from the melt and most of the BC1.5 decomposes into BC1 and CuO or into BC1 and BC2. The crystallisation of BC1 induces segregation of elements in the melt and this is very significant for the melt texturing of YBCO.

Effects of PtO2 and CeO2 additives on the microstructures of the quenched melts of Y-Ba-Cu-O materials

The microstructures of the quenched melts of samples of Y123 and Y123+15-20 mol% Y211 with PtO2 and CeO2 additives have been examined with optical microscopy, Scanning Electron Microscopy (SEM), Energy Dispersive X-ray Spectrometry (EDS) and X-ray Diffractometry (XRD). Significantly higher temperatures are required for the formation of dendritic or lamellar eutectic patterns throughout the samples with PtO2 and CeO2 additives as compared to samples without additives. The BaCuO2 (BCl) phase appears first in solid form and, instead of rapidly melting, is slowly dissolving or decomposing in the oxygen depleted melt. PtO2 and CeO2 additives slow down or shift to higher temperatures the dissolution or decomposition process of BCl. A larger fraction of BCl in solid form explains why samples with additives have higher viscosities and hence lower diffusivities than samples without additives. There is also a reduction in the Y solubility to about half the value in samples without additives. The mechanism that limits the Ostwald ripening of the Y211 particles is correlated to the morphology of the quenched partial melt. It is diffusion controlled for a finely mixed morphology and interface-controlled when the melt quenches into dendritic or lamellar eutectic patterns. The change in the morphology of the Y211 particles from blocky to acicular is related to an equivalent undercooling of the Y-Ba-Cu-O partial melt, particularly through the crystallization of BCl.

Interfacial microstructure in Y1Ba2Cu3O7-δ high Tc superconductors

The microstructures of YBa2Cu3O7-δ ceramics prepared from freeze dried powders and containing an excess of CuO have been studied by analytical electron microscopy. Special attention has been paid to the interfacial microstructure. It was found that a liquid phase formed during sintering between 890°C and 920°C and this promoted grain growth and densification. Both clean grain boundaries and boundaries containing an amorphous intergranular film, which was rich in Cu, have been observed. Both CuO and BaCuO2 were present as secondary phases.

Microstructure of an artificial grain boundary weak link in an YBa2Cu3O(7-δ) thin film grown on a (100)(110), [001]-tilt Y-ZrO2 bicrystal

The microstructure of an artificial grain boundary in an YBa2Cu3O7-δ (YBCO) thin film grown on a (100)(110), [001]-tilt yttria-stabilized-zirconia (YSZ) bicrystal substrate has been studied using transmission electron microscopy (TEM). The orientation relationship between the YBCO film and the YSZ substrate was [001]YBCO∥[001]YSZ and [110]YBCO∥[100]YSZ for each half of the bicrystal film. However, the exact boundary geometry of the bicrystal substrate was not transferred to the film. The substrate boundary was straight while the film boundary was wavy. In several cases there was bending of the lattice confined within a distance of a few basal-plane lattice spacings from the boundary plane and microfaceting. No intergranular secondary phase was observed but about 25% of the boundary was covered by c-axis-tilted YBCO grains and a-axis-oriented grains, both of which were typically adjacent to CuO grains or surrounded by a thin Cu-rich amorphous layer.

Binder effect on microstructure and properties of YBa2Cu3O7-x extruded wires

YBa2Cu3O7-x wires have been extruded with 2 and 5 wt.% of hydroxy propyl methylcellulose (HPMC) as binder. Both sets of wires sintered below 930°C have equiaxed grains while the wires sintered above this temperature have elongated grains. In the temperature range which gives equiaxed grains, the wires extruded with 5 wt.% HPMC have higher grain size and density. Cracks along the grain boundaries are often observed in the wires having elongated grains. Critical current density, Jc, increases initially, reaches a peak and then decreases with the sintering temperature. The sintering temperature giving a peak in Jc strongly depends on the heat treatment scheme for the wires extruded with 5 wt.% HPMC. TEM studies show that defective layers are formed along grain boundaries for the wires extruded with 5 wt.% HPMC after 5 h oxygenation. After 55 h oxygenation, the defective layers become more localised and grain boundaries adopt an overall cleaner appearance. Densification with equiaxed grains and clean grain boundaries produces the highest Jc's for polycrystalline YBa2Cu3O7 wires.

Microstructural characterization of quenched melt-textured YBa2Cu3O7-δ materials

The microstructure of YBa2Cu3O7-δ (YBCO) materials, melt-textured in air and quenched from the temperature range 900-990°C, has been characterized using a combination of x-ray diffractometry, optical microscopy, scanning electron microscopy, transmission electron microscopy, and energy dispersive x-ray spectrometry. BaCu2O2 and BaCuO2 were found to coexist in samples quenched from the temperature range 920-960°C. The formation of BaCu2O2 preceded the formation of YBCO. Once the YBCO had formed, BaCu2O2 was present at the solidification front filling the space between nearly parallel platelets of YBCO. Large Y2BaCuO5 particles at the solidification front appeared divided into smaller ones as a result of their dissolution in the liquid that quenched as BaCu2O2.