Continuous Deposition of YBCO Films for Coated Conductor Using PLD Method

A reel-to-reel PLD system was set up for studying YBCO coated conductor. YBCO films could be continuously grown on the CeO₂/YSZ/Y₂O₃ buffered Ni-5W tape. Some deposition parameters were investigated. XRD θ–2θ scans were employed to characterize the c-axis orientation and in-plane texture of YBCO films deposited with different laser repetition rates and tape moving speeds. We investigated the dependence of critical current I _c on laser repetition rates and tape moving speeds for YBCO films. It had been found that a-axis oriented grains appeared as YBCO layer thickness increased, which prevented the values of I _c improved.     

Spray Pyrolysis of MgO Templates on 321-Austenitic Stainless Steel Substrates for YBa2Cu3O7 Deposition by PLD

Spray pyrolysis was used to deposit MgO films on polycrystalline 321-austentic stainless steel substrates using magnesium nitrates and magnesium acetates as precursors. The MgO films deposited from the nitrate precursors were amorphous; however, MgO (200) oriented films were obtained when the acetates precursors were used. The texture of the films was improved with increasing the concentration and the deposition temperature. To evaluate the performance of the MgO buffers, PLD was used to deposit YBCO on MgO-buffered 321 substrates. Only the smoothest MgO films were found as good buffers for the deposition of c-axis oriented YBCO films. The superconducting transition temperature was broad and the T _C onset was 83.6 K. Austenitic 321 steel is an alternative for C276 as a substrate for thin film deposition.     

Microstructural study of YBa2Cu3O7/SrTiO3/YBa2Cu3O7 heteroepitaxial trilayer films grown on (100) SrTiO3 substrates

Detailed transmission electron microscopic study has been carried out on heteroepitaxial YBa₂Cu₃O₇/SrTiO₃/YBa₂Cu₃O₇ trilayer thin films grown on (100)SrTiO₃ substrates prepared by DC and RF magnetron sputtering. The microstructural results showed the existence of somea-axis-oriented YBCO grains 20–90 nm wide in thec-axis-oriented YBCO matrix. Some of thea-axis grains in the lower YBCO thin film layer have protruded into the above SrTiO₃ layer, which may cause short circuit between the two YBCO superconducting layers. This is unsuitable for the application of trilayer thin films for microelectronic devices. The defects on the surface of the substrates would also influence the growth quality of the YBCO thin films.     

Microstructures ofa-axis oriented YBa2Cu3O7-δ thin films prepared by low temperature and template processes

Highly a-axis oriented epitaxial thin films of YBa₂Cu₃O_7– have been prepared by both a low temperature process and also a self-template technique. Films deposited at low temperature showed good crystallinity whereas films grown on a template exhibited a high transition temperature into the superconducting state. Detailed transmission electron microscopic investigations have been performed on these two kinds ofa-axis oriented films. Significant differences have been found in the microstructures of these films. The dominant defects formed in these films are misoriented grains which mainly show ac-axis orientation. The origin of the nucleation of misoriented grains is attributed to surface defects of the substrate. No boundary between the template layer and upper layer could be distinguished for films made by the self-template process. A thinc-axis intermediate layer with a thickness of 2–5 unit cells was observed at the interface between thea-axis film and the SrTiO₃ substrate for both kinds of films. The formation and influence of such an intermediate layer needs further study.     

Nanostructural characterization of YBCO films on metal tape with textured buffer layer fabricated by pulsed-laser deposition

Thick YBa₂Cu₃O_7-x (YBCO) films with high critical current density (J_c) values were deposited by pulsed-laser deposition (PLD) on Hastelloy with a textured CeO₂/Gd₂Zr₂O₇ buffer layer. Both cross-sectional and plan-view TEM specimens of the YBCO films were prepared, and then the nanostructural characterization of the films was performed by transmission electron microscopy (TEM). The YBCO films less than 1 μm thick were predominantly composed of c-axis-oriented grains, however, many a-axis-oriented grains, which grew larger with the increase of the thickness of the YBCO film, were formed beyond about 1 μm from the CeO₂ interface. We found Y₂O₃ and copper oxides between a- and c-axes-oriented grains. In particular, Y₂O₃ grains were formed between the {001} plane of an a-axis-oriented grain and the {100} or {010} plane of a c-axis-oriented grain. The orientation relationships between Y₂O₃ and YBCO are found to be; (001)YBCO//(001)Y₂O₃ and (100)YBCO//(110)Y₂O₃. In addition, we also found gaps between YBCO grains. Since a-axis-oriented grain growth and the formation of Y₂O₃, copper oxides and the gaps are considered to reduce the J_c values of the YBCO film, it is important to determine the optimum process conditions to suppress the nucleation of a-axis-oriented grains, impurity oxides and gaps.     

Growth and Characterization of YBCO Thin Films by Sequential Deposition and Annealing

A novel thin film growth procedure, sequential deposition and annealing (SDA), which contains the advantages of both in situ and ex situ procedures, was proposed. Y₁Ba₂Cu₃O_{7 – x} (YBCO) high temperature superconducting thin films were grown and characterized by the SDA procedure. Purely c-axis-oriented YBCO thin films with no foreign phases and other oriented grains were successfully prepared. The superconducting transition properties of SDA-grown YBCO thin films were measured by measurement of inductance and resistance. The inductance measurements gave a T _c ^onset of 85 K and a T _c of 5 K. The resistance measurements gave a T _c ^onset of 90 K and a T _c of 5 K. Atomic force microscopy studies showed that SDA-grown YBCO thin films had micrometer-size grains surrounded by many nanometer-size grains. The nanometer-size grains in SDA-grown YBCO thin films are responsible for degradation of superconducting transition properties.     

Fabrication and microstructure of the d.c.-magnetron-sputtered YBa2Cu3O7 − x superconducting thin films

Systematic investigations were conducted to determine the effect of deposition conditions on the microstructure and superconducting properties of YBa₂Cu₃O_{7 – x} thin films produced by d.c. magnetron sputtering on (001) MgO substrate. The films were c-axis preferentially oriented with respect to the (001) MgO surface at substrate temperatures of 680–700 C. X-ray diffraction patterns clearly indicated the existence of the c-axis alignment normal to the substrate surface and some second phases. The second phases, including a Cu-rich phase and Y₂O₃, were identified by energy dispersive X-ray spectrometer and the microstructures were analysed by electron and atomic force microscopes.     

Microstructures of YBa2Cu3O7/La0.7Ca0.3MnO3 and La0.7Ca0.3MnO3/YBa2Cu3O7 bi-layers grown on (001)LaAlO3

Epitaxial YBa₂Cu₃O₇/La_0.7Ca_0.3MnO₃ (YBCO/LCMO) bi-layers and La_0.7Ca_0.3MnO₃/YBa₂Cu₃O₇ (LCMO/YBCO) bi-layers were grown on (001)LaAlO₃ by pulsed laser deposition, and their microstructures were compared by transmission electron microscopy investigation. In the YBCO(100 nm)/LCMO(150 nm) bi-layers, the LCMO layer consists of columnar grains of ~ 17 nm in diameter and contains mixed orientation domains of [100]_c, [010]_c and [001]_c. The YBCO layer is totally c-axis oriented and the YBCO lattices are tilted − 2.5° to + 2.5° as they grew on the rough surfaces of LCMO columnar grains. For the LCMO(140 nm)/YBCO(140 nm) bi-layers, the LCMO/YBCO interface is sharp and flat. The initial 12-nm thickness of the YBCO layer is composed of c-axis oriented domains, and the upper part of YBCO layer is [100] oriented. The LCMO layer was predominantly [001]_c oriented while [100]_c-oriented domains were occasionally observed.     

Characterization of Superconductor Coplanar Resonators Deposited on Different Substrates by Thermal Coevaporation

This study is based on two commercially available YBCO thin films deposited by the thermal coevaporation method on different substrates (MgO and LaAlO₃). Those films should be optimized for microwave applications. The structure and microstructure of the film deposited on LaAlO₃ have been investigated, respectively by XRD and SEM. These characterizations showed the high quality of the films concerning the c-axis orientation and the smooth and homogenous morphology. The films have then been etched into two different coplanar line resonators by ionic method (YBCO/LaAlO₃) and chemical one (YBCO/MgO) and their microwave properties have been characterized in two different cryogenic experimental set-ups. Despite the differences between these coplanar resonators, we have obtained the same intrinsic parameters (λ₀ = 190 nm, T _c=87 K with γ = 3) corresponding to the data provided by THEVA and a very low surface resistance (R _s=0.4 m Ω at 31 K and 10 GHz).     

Anisotropy of optical constants of YBCO

Otto configuration attenuated total reflection (ATR) measurements of the excitation of surface plasmons in the infrared have been carried out on YBCO films deposited on MgO (100) substrates. The dielectric constants for YBCO at 3.392m are determined to be –10+15i forc-axis material. The anisotropic nature of the cuprate is seen from films with other orientations: nearlya-axis material has constants of 4.0+7.0i. It is thus not metallic in its optical response along thec-axis which lies parallel to the substrate plane. Ellipsometric measurements in the visible onc-axis material point to a maximum surface plasmon energy of 1 eV.     

Pure and fully texturized Sr2FeMoO6 thin films prepared by pulsed laser deposition from target made with citrate-gel method

Sr₂FeMoO₆ (SFMO) thin films were grown on SrTiO₃ and MgO single crystal substrates by pulsed laser deposition. The SFMO target with nanometer sized grains for the film preparation was made from powder prepared by citrate-gel method. The parameters for ablation were optimized and the importance of the substrate temperature is observed. Film quality was verified with various X-ray diffraction methods and magnetometric measurements. The films are pure, without impurities such as metallic iron, Fe₂O₃, SrMoO₃ or SrMoO₄ and they are completely c-axis oriented. The Curie temperature for the films is higher than room temperature.     

Surface Morphology and Profile Analysis for Five-Layer YBa<Subscript>2</Subscript>Cu<Subscript>3</Subscript>O<Subscript>7−<Emphasis Type="Italic">δ</Emphasis></Subscript> Thick Films Prepared by Low-Fluorine Metallorganic Deposition

Thick YBa₂Cu₃O_7?δ (YBCO) films grown by metallorganic deposition (MOD) are very significant for high-performance superconducting wires. In the present work, the modified MOD method with reduced fluorine content in precursor solution (namely LF-MOD in the following) is applied to prepare the YBCO films with the purpose of reducing the processing time as well as increasing thickness. Five-layer YBCO films with a thickness of more than 2.5 μm are achieved after the effect of high-temperature annealing time (t _a) on the morphology and texture of YBCO films is systematically investigated. It is suggested that an annealing time as long as 6 h appears necessary to achieve a good performance for such a thick YBCO film. To understand the evolution of texture with thickness, plasma etching is employed to characterize the profile morphology at different depths inside the films, revealing the a-axis grains together with the impurity phases arising from the incomplete reaction mostly present at the top surface only.     

Preparation and characterization of highly <Emphasis Type="Italic">c</Emphasis>-axis textured MgO buffer layer grown on Si(100) substrate by RF magnetron sputtering for use as growth template of ferroelectric thin film

Highly c-axis textured MgO thin films were grown directly on Si(100) substrates without any buffer layer by RF magnetron sputtering for use as growth template of ferroelectric film. We fixed the target-to-substrate spacing of 40 mm and then changed the substrate temperature, deposition pressure, and RF power to study the effect of deposition parameters on the growth of c-axis textured MgO thin films. The as-grown films were post-annealed by the rapid thermal annealing (RTA) and furnace annealing to improve the film quality. The experimental results show that the optimum deposition parameters are substrate temperature of 350 °C, oxygen pressure of 15 mTorr and RF power of 75 W. The full width at half maximum intensity (FWHM) of MgO(200) peak obtained from the XRD measurement was 0.8°, and it was further reduced to 0.5° and 0.27° after annealing by RTA and furnace, respectively. Highly c-axis textured PZT and BaTiO₃ films could be obtained on this template. Hysteresis loops of the BaTiO₃ films deposited on MgO(100) single crystalline substrate and MgO(200)/Si(100) template were measured for comparison. The results show that MgO/Si templates thus obtained are suitable for the synthesis of perovskite ferroelectric thin films.     

Effect of Melt Processing Programme on Microstructure and Properties of YBCO Thick Films

The screen printing technique was used in the fabrication of YBa₂Cu₃O_7−σ (YBCO) superconducting thick films on yttria stabilised zirconia (YSZ) substrates. Different slow cooling rates were used in the preparation of YBCO thick films after fast cooling from the melt processing temperature. The effects of the melt processing programme on texturing, microstructure and superconducting properties of the melt processed YBCO films were studied. Slow cooling rates between 1005 and 990 °C were effective in increasing the interaction of viscous molten with reduced film/substrate, and hence a relatively large grain size has been obtained. Moreover, different c-axis texturing ratios and grain morphologies were observed.     

Critical current density and microstructure of YBa2Cu3O7 thin films post-annealed at a low oxygen partial pressure

Post-annealing of thin films of YBa₂Cu₃O₇ (YBCO) has been performed at 29 Pa and 750°C. For films 0.6 m thick, a critical current density >1 MA cm^–2 is obtained at 77 K, with a sharp eddy current response at 25 MHz. Microstructural investigation of these films by crosssectional and planar transmission electron microscopy reveals that the YBCO film has thec-axis normal to the plane of the substrate in a continuous sheet of varying thickness, frequently covering the entire thickness of the film. Mutually perpendicular rods with thec-axis in the plane of the LaAlO₃ substrate are also seen. The microstructure and critical current density of these films are compared with those of previously reported films post-annealed in atmosphericpressure oxygen.     

Superconducting thin films of Bi-Pb-Sr-Ca-Cu-O synthesized by the spray-inductively coupled plasma technique

Superconducting thin films of Bi-Pb-Sr-Ca-Cu-O were synthesized on polycrystalline MgO substrates by injecting atomized aqueous solutions of appropriate nitrates into an inductively coupled r.f. plasma (ICP) under atmospheric pressure (the spray-ICP technique). 1–2 m thick films composed ofc-axis oriented phases (c=2.4 and 3.0 nm) could be synthesized in runs of 15–20 min. The phase compositions of the films were varied fromc=2.4 nm phase toc=3.0 nm phase through their mixed phases by increasing the distance of the substrates from the ICP. In some cases the mixed phases contained a small amount ofc=3.7 nm phase. Annealing in air (850 °C for 10 min and then 800 °C for 5 h) convertedc=2.4 nm phase toc=3.0 nm phase. The best as-deposited film showedT _c (resistance = 0) at 55 K, and after annealing its resistance began to drop around 110 K and reached zero at 75 K.     

Effect of Sputtering Parameters on Superconducting Properties of GdBaCuO Epitaxial Thin Film Deposited by ICP Method

Thin films of GdBaCuO (GBCO) have been deposited in situ onto LaAlO₃ single crystal substrates by inverted cylindrical sputtering pattern (ICP). The superconductive properties of the thin films' dependence on the substrate temperature and sputtering pressure have been systematically investigated. By optimization of the deposition parameter, high-quality c-axis epitaxial GBCO thin films of T _c0>92 K were reproducibly grown. The T _c of the best sample is as high as 93.2 K. Upon changing the target composition to GdBa₂Cu₄O _y (Gd₁₂₄), it was observed that the samples always show some a-axis oriented films, implying that excess copper would favor a-axis growth in thin films. The superconductivity of the thin films under higher substrate temperature (T _s>800°C) was clearly improved by the procedure of special post-oxygenization at 400°C with an ozone atmosphere. This is very useful for preparing large-area thin films of GBCO.     

Study of Josephson effects in microbridges of Bi-Sr-Ca-Cu-O films made by spray pyrolysis

Superconducting Bi-Sr-Ca-Cu-O (2212) films were prepared by spraying stoichiometric aqueous solutions of nitrates of bismuth, strontium, calcium and copper on heated MgO (100) substrates and subsequent annealing in air. TheR-T curves of the films show metallic behaviour above the superconducting transition temperature.T _c (R=0) is observed between 80 and 85 K. Annealing temperature has a profound effect onT _c (R=0) and on the orientation of the film. Annealing in air in near-melting region yields highly oriented films withc-axis perpendicular to the substrate. These films show a sharp superconducting transition with zero resistance at 85 K. Microbridges of the dimensions of 50 μm × 50 μm have been patterned photolithographically followed with chemical etching. The 1 V characteristics of the microbridges show Josephson effects due to the presence of grain boundary weaklinks. The temperature dependence of the critical current for these microbridges suggest formation of superconductor-normal-superconductor type weaklinks.     

High-pressure dc sputtering of High-Tc BPSCCO thin films withTc(0) above 100 K

High-T _c Bi(Pb)-Sr-Ca-Cu-O thin films have been made on single-crystal MgO substrates using high-pressure dc sputtering technique. X-ray studies confirm the crystallinity and highly oriented structure withc-axis perpendicular to the substrate. By optimizing the annealing schedule the formation of the high-T _c phase is stabilized. The best film exhibited superconducting transition temperature with zero-resistance temperature,T _c(0), as high as 101 K. Temperature dependence ofJ _c indicates the presence of Josephson-type weak links.     

Mixed State Hall Resistivity in YBCO c-Axis-Oriented Thin Films

Hall voltage measurements on YBCO c-axis-oriented thin films in the mixed state were carried out. The films were grown on MgO substrates utilising evaporation technique followed by relatively low heating temperature. Hall voltage was measured in low magnetic fields perpendicular to the film surface, in which sign reversal near T _c was observed. Relatively large transverse voltage was found to be insensitive to the magnetic field inversion (even Hall effect). This effect is discussed in terms of the vortices guided motion model which is argued to give a reasonable explanation for the even Hall effect in type II superconductors.