Structural characterisation of kaolinite : NaCl intercalate and its derivatives

Kaolinite:NaCl intercalates with basal layer dimensions of 0.95 and 1.25 nm have been prepared by direct reaction of saturated aqueous NaCl solution with well-crystallized source clay KGa-1. The intercalates and their thermal decomposition products have been studied by XRD, solid-state 23Na, 27Al, and 29Si MAS NMR, and FTIR. Intercalate yield is enhanced by dry grinding of kaolinite with NaCl prior to intercalation. The layered structure survives dehydroxylation of the kaolinite at 500°–600°C and persists to above 800°C with a resultant tetrahedral aluminosilicate framework. Excess NaCl can be readily removed by rinsing with water, producing an XRD ‘amorphous’ material. Upon heating at 900°C this material converts to a well-crystallized framework aluminosilicate closely related to low-camegieite, NaAlSiO4, some 350°C below its stability field. Reaction mechanisms are discussed and structural models proposed for each of these novel materials.

Re-melting of Bi-2212/Ag laminated tapes by partial melting process

Bi-2212 tapes are prepared by a combination of dip-coating and partial melt processing. We investigate the effect of re-melting of those tapes by partial melting followed by slow cooling on the structure and superconducting properties. Microstructural studies of re-melted samples show that they have the same overall composition as partially melted tapes. However, the fractional volumes of the secondary phases differ and the amounts and distribution of the secondary phases have a significant effect on the critical current. Critical current of Bi-2212/Ag tapes strongly depends on the maximum processing temperature. Initial J(c)'s of the tapes, which are partially melted, then slowly solidified at optimum conditions and finally post-annealed in an inert atmosphere, are up to 10.4 x 10(3) A/cm(2). It is found that the maximum processing temperature at initial partial melting has an influence on the optimum re-heat treatment conditions for the tapes. Re-melted tapes processed at optimum conditions recover superconducting properties after post-annealing in an inert atmosphere: the J(c) values of the tapes are about 80-110% of initial J(c)'s of those tapes.

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.

Bi-2212/Ag laminated tapes: Bending and joining effects

Superconducting composite Bi-2212/Ag tapes and their joints are fabricated by a combination of dip-coating and partial melt processing. The heat treated tapes have a critical current (Ic) between 8 and 26A, depending on tape thickness and the number of Bi-2212 layers. Current transmissions between 80% and 100% have been achieved through the joints of tapes. Different types of HTS joints of Bi-2212/Ag laminated tapes are made and their transport properties during winding operations are investigated. Irreversible strain values (ε irrev) for laminated tapes and their joints are determined and it is found that the degradation of Ic during tape bending depends on the type of joint.

Superconducting joints of Bi-2212/Ag tapes and laminates

Different types of HTS joints of Bi-2212/Ag tapes and laminates, which are fabricated by dip-coating and partial-melt processes, have been investigated. All joints are prepared using green single and laminated tapes and according to the scheme: coating-joining-processing. The heat treated tapes have critical current (Ic) between 7 and 27 A, depending on tape thickness and the number of Bi-2212 ceramic layers in laminated tapes. It is found that the current transport properties of joints depend on the type of laminate, joint configuration and joint treatment, Ic losses in joints of Bi-2212 tapes and laminates are attributed to defects in their structure, such as pores, secondary phases and misalignment of Bi-2212 grains near the Ag edges. By optimizing joint configuration, current transmission up to 100% is achieved for both single tapes and laminated tapes.

Bi-2212/Ag tapes and laminates : effects of bending

Superconducting Bi-2212 tapes and laminates are fabricated by a combination of dip-coating and partial melt processing. The heat treated tapes have critical current densities (Jc) up to 11 kAcm -2. We investigate the degradation of critical current (Ic) during bending experiments for both single tapes and tapes with laminate structure. Although degradation of Ic is observed in both forms, the characteristics of the degradation differ. It is determined that laminated tapes perform better than single tapes when critical current is measured against bending radius, and laminated tapes tolerate a higher strain for a given reduction in critical current. It is found that increasing the number of Bi-2212 layers increases the total Ic of the laminated tape, but degradation of critical current is more pronounced during bending because of the increased total thickness of the laminate structure. It is also found that addition of silver to the Bi-2212 layers reduces critical current degradation during bending for both tapes and laminates.

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.

Synthesis and characterisation of nanoscale magnesium oxide powders and their application in thick films of Bi2Sr2CaCu2O8

Nanoscale MgO powder was synthesized from magnesite ore by a wet chemical method. Acid dissolution was used to obtain a solution from which magnesium containing complexes were precipitated by either oxalic acid or ammonium hydroxide, The transformation of precipitates to the oxide was monitored by thermal analysis and XRD and the transformed powders were studied by electron microscopy. The MgO powders were added as dopants to Bi2SrCa2CuO8 powders and high temperature superconductor thick films were deposited on silver. Addition of suitable MgO powder resulted in increase of critical current density, J(c), from 8,900 Acm(-2) to 13,900 Acm(-2) measured at 77 K and 0 T. The effect of MgO addition was evaluated by XRD, electron microscopy and critical current density measurements. (C) 1998 Elsevier Science B.V.

Melt-textured YBa2Cu3O7-x wires having plate-like grains

YBCO wires which consist of well oriented plate-like fine grains are fabricated using a moving furnace to achieve higher mechanical strength. Melt-texturing experiments have been undertaken on YBCO wires with two different compositions: YBa1.5Cu2.9O7-x, and YBa1.8Cu3.0O7-x. Wires are extruded from a mixture of precursor powders (formed by a coprecipitation process) then textured by firing in a moving furnace. Size of secondary phases such as barium cuprate and copper oxide, and overall composition of the sample affect the orientation of the fine grains. At zero magnetic field, the YBa1.5Cu2.9O7-x wire shows the highest critical current density of 1,450 Acm-2 and 8,770 Acm-2 at 77K and 4.2K, respectively. At 1 T, critical current densities of 30 Acm-2 and 200 Acm-2, respectively, are obtained at 77K and 4.2K. Magnetisation curves are also obtained for one sample to evaluate critical current density using the Bean model. Analysis of the microstructure indicates that the starting composition of the green body significantly affects the achievement of grain alignment via melt-texturing processes.

Partial melt processing and electrical properties of Bi-Sr-Ca-Cu-o superconducting thick films on (100) MgO substrates

Superconducting thick films of Bi2Sr2CaCu2Oy (Bi-2212) on single-crystalline (100) MgO substrates have been prepared using a doctor-blade technique and a partial-melt process. It is found that the phase composition and the amount of Ag addition to the paste affect the structure and superconducting properties of the partially melted thick films. The optimum heat treatment schedule for obtaining high Jc has been determined for each paste. The heat treatment ensures attainment of high purity for the crystalline Bi-2212 phase and high orientation of Bi-2212 crystals, in which the c-axis is perpendicular to the substrate. The highest Tc, obtained by resistivity measurement, is 92.2 K. The best value for Jct (transport) of these thick films, measured at 77 K in self-field, is 8 × 10 3 Acm -2.

Microstructural investigation of Bi-Sr-Ca-Cu-oxide thick films on alumina substrates

The microstructure of Bi-Sr-Ca-Cu-oxide (BSCCO) thick films on alumina substrates has been characterized using a combination of X-ray diffractometry, scanning electron microscopy, transmission electron microscopy of sections across the film/substrate interface and energy-dispersive X-ray spectrometry. A reaction layer formed between the BSCCO films and the alumina substrates. This chemical interaction is largely responsible for off-stoichiometry of the films and is more significant after partial melting of the films. A new phase with fee structure, lattice parameter a = 2.45 nm and approximate composition Al3Sr2CaBi2CuOx has been identified as reaction product between BSCCO and Al2O3.

FT Raman spectroscopic characterization of oxalate precursors to YBCO superconductors

FT Raman spectroscopy has been used to characterise the composition of the oxalate precursor to YBCO superconductors. By comparison to spectra of barium, copper and yttrium oxalate it is concluded that the co-precipitate incorporates not only the individual oxalate species but also a species ascribed to a mixed oxalate system. Significantly, Raman spectroscopy demonstrated that the precursor was not amorphous as previously deduced from XRD studies. In contrast, it is hypothesised that the sample consists of very small crystalline particles.

Manufacture of specific BSCCO powder compositions by co-precipitation

A co-precipitation process for large-scale manufacture of bismuth-based HTSC powders has been demonstrated. Powders manufactured by this process have a high phase purity and precisely reproducible stoichiometry. Controlled time and temperature variations are used to convert precursors to HTSC compounds and to obtain specific particle-size distributions. The process has been demonstrated for a variety of compositions in the BSCCO system. Electron microscopy X-ray diffraction, inductively coupled plasma spectroscopy and magnetic-susceptibility measurements are used to characterize the powders.

Bulk manufacture of YBCO powders by coprecipitation

This work presents an assessment of the coprecipitation technique for the reliable production of high-temperature superconducting (HTS) copper-oxide powders in quantities scaled up to 1 kg. This process affords precise control of cation stoichiometry (< 4% relative), occurs rapidly (almost instantaneously) and can be suitably developed for large-scale (e.g. tonne) manufacture of HTS materials. The process is based upon a simple control of the chemistry of the cation solution and precipitation with oxalic acid. This coprecipitation method is applicable to all copper-oxides and has been demonstrated in this work using over thirty separate experiments for the following compositions: YBa2Cu3O7-δ, Y2BaCuO5 and YBa2Cu4O8. The precursor powders formed via this coprecipitation process are fine-grained (∼ 5-10 nm), chemically homogeneous at the nanometer scale and reactive, Conversion to phase-pure HTS powders can therefore occur in minutes at appropriate firing temperatures. © 1995.

Shape-formed ceramic superconductors by slip-casting

In order to rigorously test emerging applications using prototypes and pilot designs, high temperature superconductor (HTS) materials must be fabricated into a variety of shapes in an economical manner. We have developed a simple, economical, ceramic slip-casting approach to form complex shaped monolithic HTS articles for which high bulk density has been achieved. The sintered articles exhibit good Meissner signal and consist of phase-pure HTSC phase. A low transport critical current density is observed and is explained on the basis of densification and grain growth. © 1995 The Metallurgical of Society of AIME.