Special features in the synthesis and properties of thin Y-Ba-Cu-O high-temperature superconductor films free of secondary phases

Data on the structure and transport properties of thin Y-Ba-Cu-O (YBCO) high-temperature superconductor films obtained by magnetron sputtering of a stoichiometric target in a system with a 90° off-axis geometry are reported. It is shown that the films prepared under these conditions are free of copper-rich secondary phases and are characterized by the surface roughness height below 10 nm. The films possess a perfect structure and exhibit high superconducting properties: c-axis misorientation in microblocks FWHM(005)YBCO=0.4–0.5°; zero-resistance temperature T _co=89 K; critical (pinning) current density j _p=1.5–2 MA/cm² (77 K).     

Effect of Firing Temperature on the Structure and Superconducting Properties of YBa<Subscript>2</Subscript>Cu<Subscript>3</Subscript>O<Subscript>7−<Emphasis Type="Italic">x</Emphasis></Subscript> Films

YBa₂Cu₃O_7−x (YBCO) films were prepared on LaAlO₃ single crystal substrate under various firing temperatures (750–800 °C) in the crystallization process by metalorganic deposition (MOD) method. The coating solution was made by mixing the fluorine-free precursor solution containing Y and Cu with Ba–fluorine precursor solution (Ba-TFA). The effect of firing temperature on the structure and superconducting properties of YBCO films was systematically investigated. The results indicated that YBCO-films were smooth, crack-free, exhibited good textures and retain high oxygen content according to the XRD and SEM images. Sample of YBCO-film fired at 780 °C showed highest superconducting properties including high critical transition temperature T _c=89 K, sharp transition temperature ΔT _c<1 K, and critical current density J _c=2.8 MA cm⁻², which are attributable to excellent in-plane textures and dense microstructures with good connectivity between the grains.     

Growth parameter effect in superconducting YBa2Cu4O8 thin films by d.c. magnetron sputtering

High- T _c YBa₂Cu₄O₈ (124) thin films have been made by d.c. magnetron sputtering deposition on (100) MgO substrates. The effect of several processing variables, including the ratio of oxygen to argon, total pressure, and substrate temperature, on the superconducting properties of the thin films, were systematically investigated. The as-prepared films annealed in flowing oxygen at 800°C for 4 h under ambient pressure obtained nearly phase-pure 124 and exhibited superconducting onset transition at 75 K.     

Physicochemical and structural characteristics of TiC and VC thin films deposited by DC reactive magnetron sputtering

Vanadium carbide and titanium carbide films were deposited on Si substrates by direct current reactive magnetron sputtering, varying the substrate temperature during deposition and the reactive gas (CH₄) pressure. The physicochemical and structural properties of the films were characterized for stoichiometric films (V/C = 1 and Ti/C = 1), which display good performance concerning wear, friction, and corrosion. The techniques used to characterize the films were Rutherford backscattering spectrometry in channeling geometry, ¹²C(α,α)¹²C nuclear resonant scattering, glancing angle X-ray diffraction, X-ray reflectometry, and X-ray photoelectron spectroscopy. The results revealed that the ideal conditions for deposition of these films are a CH₄ partial pressure of 0.5 × 10⁻³ mbar and a substrate temperature of 400 °C. In such conditions, the deposition rates are 7 nm s⁻¹ for TiC and 8.5 nm s⁻¹ for VC at a target power density of 5.5 W cm⁻². The density of the films, as determined here by X-ray reflectometry, are slightly higher than those for the bulk materials.     

Re−Ni2B2C superconducting borocarbides: “In situ” growth of thin films, transport and point contact spectroscopy

High quality c-axis oriented films of the intriguing intermetallic superconducting compound YNi₂B₂C have been obtained “in situ” by magnetron sputtering on MgO substrates held at about 800°C. The films showed maximum T_c=15.3 K, †T_c≈0.1 K, room temperature resistivity ρ≈50μΩ·cm, critical current J_c≈10⁵ A/cm² and B_c2≈6 T. Superconducting films were also obtained on Al₂O₃ and LaAlO₃ single-crystal substrates. From the ρ(T) dependence a value of the Debye temperature Θ _D =330±20 K can be deduced. At low temperatures the resistivity follows a quadratic power law possibly indicative of a high value of the electron-phonon interaction parameter λ. In order to clarify the role of λ in these compounds, point contact spectroscopy measurements have been performed on YNi₂B₂C and HoNi₂B₂C bulk samples prepared by inductive melting using a Low Temperature Scanning Tunneling Microscope (LTSTM). In the point contact regime clear evidence of a superconducting gap have been found in both compounds, corresponding to a moderate strong coupling behaviour (2†/KT_c≈3.8).     

In situ grown superconducting YBCO films on buffered silicon substrates for device applications

Thin films of YBa₂Cu₃O_7– (YBCO) have been grownin situ on silicon single-crystal (100) substrate by using SrTiO₃ as a buffer layer. The deposition has been carried out by on-axis rf magnetron sputtering method. The deposition condition have been optimized by studying the plasma characteristics and correlating them with the superconducting performance of the film. Films deposited at substrate temperature in the range of 680–700°C from stoichiometric YBCO targets in an argon + oxygen mixture (31) are superconducting and showc-axis epitaxy. Compositional confirmation has been carried out using Rutherford backscattering. Scanning tunneling microscopy of the films reveal formation of well-defined layered structure with some defects in the initial stages ofin situ growth of the films. Films grown on SrTiO₃ substrates have excellent crystalline quality (XRD), transition temperatureT _c0=81 K and the critical current densityJ _c >2×10⁵ A/cm² for unpatterned films at 77 K. On silicon substrates using buffer layers thein situ deposited YBCO films shows a higher transition width andT _c0 is also slightly less (71 K).     

Copper nitride films deposited by dc reactive magnetron sputtering

Copper nitride (Cu₃N) films were deposited on glass substrates by sputtering of copper target under various substrate temperatures in the range 303–523 K using dc reactive magnetron sputtering. The substrate temperature highly influenced the structural, mechanical, electrical and optical properties of the deposited films. The X-ray diffraction measurements showed that the films were of polycrystalline nature and exhibit preferred orientation of (111) phase of Cu₃N. The microhardness of the films increased from 2.7 to 4.4 GPa with the increase of substrate temperature from 303 to 473 K thereafter decreased to 4.1 GPa at higher temperature of 523 K. The electrical resistivity of the films decreased from 8.7 × 10⁻¹ to 1.1 × 10⁻³ Ωcm and the optical band gap decreased from 1.89 to 1.54 eV with the increase of substrate temperature from 303 to 523 K respectively.     

Superconductivity in single crystals of the nonperovskite-like cuprate Ba2Cu3O6−x

Spontaneous crystallization from a solution in a melt at a pressure of (0.8–1)×10⁻³ Pa was used to obtain single crystals of a new nonperovskite-like superconducting phase Ba₂Cu₃O_6−x space group P _ccm, a=13.065, b=20.654, and c=11.431 Å). The superconducting properties of the crystals were investigated by modulated microwave absorption. The superconducting transition temperatures were 5 K (sample No. 1), 7 K and 13 K (sample No. 2). The superconductivity in the Ba₂Cu₃O_6−x crystals is attributed to the presence of CuO₂ chains of edge-sharing copper-oxygen squares. Nonperovskite-like Ba₂Cu₃O_6−x crystals are a new class of one-dimensional (1D) superconductors. Pis’ma Zh. Tekh. Fiz. 23, 27–34 (December 26, 1997)     

Characterization of CuAlO2 films prepared by dc reactive magnetron sputtering

Thin films of copper aluminum oxide (CuAlO₂) were prepared on glass substrates by dc magnetron sputtering at a substrate temperature of 523 K under various oxygen partial pressures in the range 1 × 10⁻⁴–3 × 10⁻³ mbar. The dependence of cathode potential on the oxygen partial pressure was explained in terms of oxidation of the sputtering target. The influence of oxygen partial pressure on the structural, electrical and optical properties was systematically studied. p-Type CuAlO₂ films with polycrystalline nature, electrical resistivity of 3.1 Ω cm, Hall mobility of 13.1 cm² V⁻¹ s⁻¹ and optical band gap of 3.54 eV were obtained at an oxygen partial pressure of 6 × 10⁻⁴ mbar.     

In situ grown superconducting YBCO films on buffered silicon substrates for device applications

Thin films of YBa₂Cu₃O_7?δ (YBCO) have been grownin situ on silicon single-crystal (100) substrate by using SrTiO₃ as a buffer layer. The deposition has been carried out by on-axis rf magnetron sputtering method. The deposition condition have been optimized by studying the plasma characteristics and correlating them with the superconducting performance of the film. Films deposited at substrate temperature in the range of 680–700°C from stoichiometric YBCO targets in an argon + oxygen mixture (3∶1) are superconducting and showc-axis epitaxy. Compositional confirmation has been carried out using Rutherford backscattering. Scanning tunneling microscopy of the films reveal formation of well-defined layered structure with some defects in the initial stages ofin situ growth of the films. Films grown on SrTiO₃ substrates have excellent crystalline quality (XRD), transition temperatureT _c0=81 K and the critical current densityJ _c >2×10⁵ A/cm² for unpatterned films at 77 K. On silicon substrates using buffer layers thein situ deposited YBCO films shows a higher transition width andT _c0 is also slightly less (71 K).     

Preparation of epitaxial YBa2Cu3O7−x films by magnetron sputtering

Thin films of highT _c superconductor YBa₂Cu₃O_7−x were obtained by magnetron sputtering. MgO, YSZ, YSH and Al₂O₃ single crystals were used as substrates. Epitaxial films with tetragonal structure havingT _c 55–60 K grow at substrate temperaturesT _s between 930 K and 980 K. Orientation of the films in thisT _s range was (100) and (001) for (100) MgO substrate, (111) and (001) for (1012) Al₂O₃ and (111) YSH and (113) or (103) on (110) YSZ and (111) YSH. Single crystalline films with orthorhombic structure and (001) orientation were grown on all the substrates whenT _s exceeded 980 K. They haveT _c>80 K.     

Magnetic properties,microstructures and domain structures of arc-plasma sprayed Nd-Fe-B permanent magnet

Thin Nd-Fe-B films prepared by arc-plasma spraying at different substrate temperatures were investigated for their magnetic and structural properties. The isotropic magnets with the best magnetic properties (_M H _c=1.2 MA m^–1, _o M _r=0.6 T, (BH)_max=64 kJ m^–3), were obtained after plasma spraying the Nd-Fe-B powders on water-cooled copper substrates and subsequently annealing the films for 0.5 h at 750 °C. The optimum magnetic properties of the anisotropic Nd-Fe-B films, i.e. _M H _c=1.2 MA^–1, _o M _r=0.9 T and (BH)_max=180 kJ m^–3, were obtained in films sprayed on to heated to 600 °C substrates. The magnetic properties of the sprayed films were strongly influenced by the microstructure. The domain structure of these films is also presented.     

Effect of Substrate Temperature on the Properties of Nano-ZnO: In Transparent Conductive Films

High quality transparent conductive In-doped nano-ZnO thin films with In content of 2 at% were prepared by RF magnetron sputtering. The effect of substrate temperature on the structure, electrical and optical properties of nano-ZnO thin films was investigated by XRD, Hall measurement and optical transmittance spectroscopy. It shows that all the films are polycrystalline with hexagonal wurtzite structure and c-axis is perpendicular to the substrate. The grain size of the films changed from 22.4 to 28.7 nm with different substrate temperatures. The lowest resistivity of the films obtained is 3.18×10⁻³ Ω⋅cm as the growth temperature is 100 °C. The transmittance of all the films is about 85% in the visible region, and the optical band gap is in the range of 3.40∼3.45 eV.     

Organic superconductors with an incommensurate anion structure

Abstract

Superconducting incommensurate organic composite crystals based on the methylenedithio-tetraselenafulvalene (MDT-TSF) series donors, where the energy band filling deviates from the usual 3/4-filled, are reviewed. The incommensurate anion potential reconstructs the Fermi surface for both (MDT-TSF)(AuI₂)_0.436 and (MDT-ST)(I₃)_0.417 neither by the fundamental anion periodicity q nor by 2q, but by 3q, where MDT-ST is 5H-2-(1,3-dithiol-2-ylidene)-1,3-diselena-4,6-dithiapentalene, and q is the reciprocal lattice vector of the anion lattice. The selection rule of the reconstructing vectors is associated with the magnitude of the incommensurate potential. The considerably large interlayer transfer integral and three-dimensional superconducting properties are due to the direct donor–donor interactions coming from the characteristic corrugated conducting sheet structure. The materials with high superconducting transition temperature, T_c, have large ratios of the observed cyclotron masses to the bare ones, which indicates that the strength of the many-body effect is the major determinant of T_c. (MDT-TS)(AuI₂)_0.441 shows a metal–insulator transition at T_MI=50 K, where MDT-TS is 5H-2-(1,3-diselenol-2-ylidene)-1,3,4,6-tetrathiapentalene, and the insulating phase is an antiferromagnet with a high Néel temperature (T_N=50 K) and a high spin–flop field (B_sf=6.9 T). There is a possibility that this material is an incommensurate Mott insulator. Hydrostatic pressure suppresses the insulating state and induces superconductivity at T_c=3.2 K above 1.05 GPa, where T_c rises to the maximum, T_c^max=4.9 K at 1.27 GPa. This compound shows a usual temperature–pressure phase diagram, in which the superconducting phase borders on the antiferromagnetic insulating phase, despite the unusual band filling.     

Influence of sputtering power on the physical properties of magnetron sputtered molybdenum oxide films

Thin films of molybdenum oxide were formed on glass and silicon substrates by sputtering of molybdenum target under various sputtering powers in the range 2.3–6.8 W/cm², at a constant oxygen partial pressure of 2 × 10⁻⁴ mbar and substrate temperature 523 K employing DC magnetron sputtering technique. The effect of sputtering power on the core level binding energies, chemical binding configurations, crystallographic structure, surface morphology and electrical and optical properties was systematically studied. X-ray photoelectron spectroscopic studies revealed that the films formed at sputtering powers less than 5.7 W/cm² were mixed oxidation states of Mo⁵⁺ and Mo⁶⁺. The films formed at 5.7 W/cm² contained the oxidation state Mo⁶⁺ of MoO₃. Fourier transform infrared spectra contained the characteristic optical vibrations. The presence of a sharp absorption band at 1,000 cm⁻¹ in the case of the films formed at 5.7 W/cm² was also conformed the existence of α-phase MoO₃. X-ray diffraction studies also confirmed that the films formed at sputtering powers less than 5.7 W/cm² showed the mixed phase of α-and β-phase of MoO₃ where as at sputtering power of 5.7 W/cm² showed single phase α-MoO₃. The electrical conductivity of the films increased from 8 × 10⁻⁶ to 1.2 × 10⁻⁴ Ω⁻¹ cm⁻¹, the optical band gap decreased from 3.28 to 3.12 eV and the refractive index decreased from 2.12 to 1.94 with the increase of sputtering power from 2.3 to 6.8 W/cm², respectively.     

Superconducting characteristics and epitaxial-growth analyses of YBa2Cu3O7−x thin films by direct-current magnetron sputtering

Using direct-current magnetron sputtering deposition, we have successfully prepared highquality epitaxial YBa₂Cu₃O_7–x thin films, on (1 0 0) and (1 1 0) ZrO₂, SrTiO₃ and LaAlO₃ substrates. The films reached zero resistance at about 90 K and had a critical current density, J _c (at 77 K, H=O), above 10⁶ Acm^–2. Electrical measurements showed that the films had a small microwave surface resistance. The epitaxial structure of the films was studied by X-ray diffraction (XRD), Rutherford backscattering (RBS) and channeling spectroscopy, X-ray double-crystalline diffraction and transmission electron microscopy (TEM). It was found that the c-axis of the film grown on the (1 0 0) substrates under optimum deposition conditions was perpendicular to the substrate surface. But on the (1 1 0) substrates, epitaxial growth was along the (1 1 0) or (1 0 3) direction. The experimental results indicate that the films had excellent superconducting properties and complete epitaxial structure.     

Reactive deposition of Y1Ba2Cu3O7 −x superconductor films by pulsed laser ablation from an unreacted mixture of Y2O3, BaCO3 and CuO

Superconducting thin films of Y₁Ba₂Cu₃ O_{7 −x} have been deposited on (100) Y-ZrO₂ substrates by pulsed excimer laser ablation from anunreacted mixture of Y₂O₃, BaCO₃ and CuO. The films deposited at substrate temperature of 680°C and oxygen partial pressure of 200 mtorr were found to be superconducting with zero resistive transition temperature of 89 K and critical current density of over 3 × 10⁵ A/cm² at 77 K. These results are compared with those obtained by laser ablation from a sintered superconducting pellet.     

Effect of Firing Temperature on the Structure and Properties of YBa2Cu3O7−x Films by TFA-MOD Method

YBa₂Cu₃O_7−x (YBCO) films were fabricated on LaAlO₃ (LAO) substrate under various firing temperatures (760–870 °C) in the crystallization process by metalorganic deposition (MOD) method using trifluoroacetates. The effect of firing temperature on the structure and properties of YBCO films was systematically investigated. According to the XRD and SEM images, the films fired at low temperature (760–800 °C) showed poor electrical performance due to rough surfaces and impurity phases. However, the films fired at 850 °C showed the highest critical temperature of 90 K and the highest J _c of 3.1 MA/cm² which attribute to the formation of a purer YBCO phase, fewer pores, and stronger biaxial texture.     

Effect of post-annealing on thin YBCO films deposited from a nanocrystalline target

Pulsed laser deposition is used to ablate thin superconducting YBCO films on SrTiO ₃ substrates. The most important parameters of thin superconducting films are high critical current density, ability to stand magnetic fields and smoothness of surfaces. Smoothness is important in fabrication of layered structures and for research of basic properties of thin superconducting structures. The target sintered from YBCO nanopowder is a promising material for making films which meet most of the requirements above. Investigations by AFM show that our target has grains about one order of magnitude smaller than usual grain size of commercial targets. At optimal deposition parameters, the oxygen pressure of 0.4 torr in the chamber and the substrate temperature 725°C, films with T _c = 90 K, J _c =8 × 10⁶ A/cm ² (77 K) and RMS surface roughness = 1.5 nm are obtained. Thermal annealing of the deposited films for 18 h at 900°C further increases the value of J _c .     

Single cerium zirconate buffer layer on biaxially textured metal substrates for high performance coated conductors

Textured cerium zirconate (Ce _x Zr_1−x O₂) films were deposited on biaxially textured Ni-5at.%W substrate by direct-current (dc) reactive magnetron sputtering for low cost production of high performance YBa₂Cu₃O_7−δ (YBCO) coated conductors. Film composition was controlled by modulating dc power applied to the Ce metal target. X-ray diffraction analysis shows that all the samples exhibit epitaxial growth, with c-axis perpendicular to the substrate surface. The YBCO film deposited directly on the Ce_0.32Zr_0.68O₂ layer for optimized lattice matching shows a transition temperature T _c and critical current density J _c (75.5 K, self field) of 90.4 K and 1.3 MA/cm². The in-field dependence of J _c is similar to the standard CeO₂/YSZ/CeO₂ buffered samples. These results demonstrate that a single Ce _x Zr_1−x O₂ buffer layer, instead of CeO₂/YSZ/CeO₂ multi-buffer layers for the fabrication of YBCO coated conductors, provides advantages such as simplified architecture and potentially reduced cost due to the reduced fabrication steps.