The As-prepared surfaces of C-axis-oriented Nd1Ba2Cu3Oy thin films characterized using scanning probe microscopes

Recently, superconducting Nd₁Ba₂Cu₃O_y (Ndl23) thin films with high superconducting transition temperature (T _c) have been successfully fabricated at our institute employing the standard laser ablation method. In this paper, we report the results of surface characterization of the Nd123 thin films using an ultrahigh vacuum scanning tunneling microscope/spectroscopy (UHV-STM/STS) and an atomic force microscope (AFM) system operated in air. Clear spiral pattern is observed on the surfaces of Nd123 thin films by STM and AFM, suggesting that films are formed by two-dimensional island growth mode. Contour plots of the spirals show that the step heights of the spirals are not always the integer or half-integer number of thec-axis parameter of the structure. This implies that the surface natural termination layer of the films may not be unique. This result is supported byI-V STS measurements. The surface morphology of the Nd123 thin films is compared with that of thec-axis-oriented Y₁Ba₂Cu₃S_y thin films. Surface atomic images of the as-prepared Nd123 thin films are obtained employing both STM and AFM. STS measurements show that most of the surfaces are semiconductive. The results of STS measurements together with the fact that we are able to see the surface atomic images using scanning probe microscopes suggest that exposure to air does not cause serious degradation to the as-prepared surfaces of Nd123 thin films.     

Cryogenic STM/STS observation on oxide superconductors

The topographic and electronic properties of the surfaces of (001) and (110) oriented YBa₂Cu₃O_y, epitaxial films have been probed by atomic resolution STM/STS at 4.2 K. The STM image on the (001) surface clearly revealed the atomic corrugation of the tetragonal lattice with an average spacing of 0.4 nm. while on the (110) surface the orthorhombic atomic lattice, corresponding to the Cu atoms of both CuO₂ and CuO chain planes, was observed. The STS result on the (001) surface indicated the semiconducting nature of the terminating layer. As the tunneling tip came closer to the surface, however, the shape of the tunneling spectrum became more metallic and showed a superconducting energy gap, which seems to arise from the underlying superconducting layer. On the other hand, the tunneling spectra on the (110) surface indicated superconducting gap structures, independent of the tip-sample distance.     

Low Temperature Scanning Tunneling Spectroscopy Studies of High J c NdBa2Cu3O7 − δ Single Crystals

We report low temperature scanning tunneling spectroscopy (STS) studies on NdBa₂Cu₃O_{7 ? δ} (Nd123) single crystals. Two characteristic spectra with a nearly ohmic background spectrum and a V-shaped background are observed on the cleaved surfaces. The former spectum shows an inhomogeneous distribution of a superconducting energy gap (2Δ) for STS differential conductance map. The latter shows a homogeneous distribution. It is probable that those differences are attributed to a tunneling current from different surface layers. The temperature dependence of tunneling conductance spectrum with a V-shaped background reveals that the superconducting gap disappears around T _c, and no pseudogap behavior exists above T _c.     

Preparation and properties of Tl2Ba2CaCu2O8 thin films

Anex situ process has been developed to produce thin superconducting Tl₂Ba₂CaCu₂O₈ films. The properties of films grown on different substrates using different annealing regimes were studied. Critical temperatures of 103–107 K were measured on films prepared in a broad range of annealing temperatures on SrTiO₃, LaAlO₃, and Y-ZrO₂ substrates. A critical current density,J _c, of 2×10⁶ A/cm² at 77 K was measured on LaAlO₃. Film morphology was studied by SEM, AFM, and STM.     

Surface morphology of high-temperature superconductor thin films using scanning tunnelling microscopy

The surface morphology of laser-deposited superconducting YBa₂Cu₃O_7?x thin films has been studied using scanning tunnelling microscopy (STM). Very high resolution of the surface morphology has been obtained showing well-textured surfaces with very distinct growth patterns. The thin films produced byin situ laser deposition are highly oriented with typicalJ _c values > 1× 10⁶A cm^?2 at 77 K. The morphology of these surfaces as revealed by STM is a terraced, layer-like structure with a discrete rise of each terrace level approximately equal to thec-axis lattice spacing. These terraces are stacked upon each other in an ordered fashion. These terraces can also be viewed as a series of chip-like morphologies which increase in size at the lower levels. The surface structure (amount of texturing and size of terraces near the surface) shows a small but observable dependence upon the deposition conditions, with lower deposition rates producing larger grain sizes. We have also studied the chemical etching of these surfaces and the resultant morphologies have been followed using atomic force microscopy. Upon chemical etching the individual grains are revealed and due to the epitaxial growth of these films, most likely represent mutually aligned but separate grains. These etching studies provide valuable information about substructures. A model for film growth based upon nucleation and growth will be described.     

Low Temperature Scanning Tunneling Spectroscopy Studies of High Jc NdBa2Cu3O7 ? δ Single Crystals

We report low temperature scanning tunneling spectroscopy (STS) studies on NdBa₂Cu₃O_{7 –} (Nd123) single crystals. Two characteristic spectra with a nearly ohmic background spectrum and a V-shaped background are observed on the cleaved surfaces. The former spectum shows an inhomogeneous distribution of a superconducting energy gap (2) for STS differential conductance map. The latter shows a homogeneous distribution. It is probable that those differences are attributed to a tunneling current from different surface layers. The temperature dependence of tunneling conductance spectrum with a V-shaped background reveals that the superconducting gap disappears around T _c, and no pseudogap behavior exists above T _c.     

Investigation of structural,optical and micro-mechanical properties of (NdyTi1 − y)Ox thin films deposited by magnetron sputtering

TiO₂ and (Nd_yTi_1 − y)O_x thin films were deposited by reactive magnetron sputtering process from mosaic Ti–Nd targets and characterised by X-ray diffraction (XRD), Raman optical spectroscopy and nanoindentation technique. XRD measurements revealed that as-prepared titanium dioxide and TiO₂ thin films with 4 and 7 at.% of Nd had nanocrystalline rutile structure, while coatings with larger amount of Nd were amorphous. Raman spectroscopy investigations showed that the increase of the neodymium concentration caused amorphisation of the coatings and hindered their crystal growth. All as-prepared coatings were transparent in the visible wavelength range with a transmittance of approximately 80%. The refractive index and extinction coefficient of the thin films gradually decreased with the increase of the neodymium concentration. Micro-mechanical properties, i.e. hardness and elastic modulus, were determined using traditional load-controlled nanoindentation testing and continuous stiffness measurements. The highest hardness and elastic modulus values were obtained for thin films with 7 at.% of Nd and were approximately 14.8 GPa and 166.3 GPa, respectively.     

Epitaxial growth of anatase TiO2 thin films on LaAlO3(100) prepared using pulsed laser deposition

Titanium dioxide thin films were grown on a lattice-matched LaAlO₃(100) surfaces using pulsed laser deposition (PLD) in oxygen atmosphere. The films were characterized using X-ray diffraction (XRD), reflection high-energy electron diffraction (RHEED) and atomic force microscopy (AFM). The crystal structure of all the films was anatase. Preferred oriented films with a c-axis normal to the substrate surface were obtained. RHEED analysis also revealed that the films had the preferential in-plane orientation, demonstrating that anatase films were epitaxially grown on the substrate. The flatness of the films depended on their growth conditions and thickness.     

Preparation and properties of Tl2Ba2CaCu2O8 thin films

Anex situ process has been developed to produce thin superconducting Tl₂Ba₂CaCu₂O₈ films. The properties of films grown on different substrates using different annealing regimes were studied. Critical temperatures of 103–107 K were measured on films prepared in a broad range of annealing temperatures on SrTiO₃, LaAlO₃, and Y-ZrO₂ substrates. A critical current density,J _c, of 2×10⁶ A/cm² at 77 K was measured on LaAlO₃. Film morphology was studied by SEM, AFM, and STM.     

Investigations on TlBa2Ca2Cu3Ox superconducting thin films formation on LaAlO3 substrate

Investigations on pure superconducting phase TlBa₂Ca₂Cu₃O_x (Tl-1223) thin films formation, of about 100-125 nm in thickness, on (001) LaAlO₃ single crystal substrate, were made using radio-frequency sputtering deposition of Ba₂Ca₂Cu₃O_x precursor films and ex-situ thallination in sealed quartz tube. The precursor films were thallinated under different conditions of partial oxygen pressure, temperature, time and y thallium source content using unreacted pellets of composition Tl_yBa₂Ca₂Cu₃O_x. In all cases, strongly c-oriented multiphase films were obtained. A correlation between the Tl-1223 phase purity and the precursor film conditions of thallination is established. Temperature and time of thallination as well as the thallium source content and the partial pressure of oxygen play a key role in the quality of the obtained film. The films' onset temperature of the superconducting transition ranges between 90 and 103 K. It is shown that the best samples can be obtained from a dense precursor film and relatively medium thallination time.     

Analysis of indentation size effect (ISE) behavior in low-load Vickers microhardness testing of (Sm123)1−x(Nd123)x superconductor system

Indentation size effect (ISE) for (Sm123)_1?x(Nd123)_x superconducting samples which were fabricated by the solid state reaction technique for values of x = 0.00, 0.05, 0.10, 0.20, and 0.30 was investigated by analyzing the theoretical models. When the experimental data of a number of single crystals which have the different crystal structure and different chemical bonding inside the polycrystallined samples were analyzed with the ISE models, the sample encountering with resistance and elastic deformation was observed as well as plastic deformation. The microhardness values on different surfaces of materials were calculated by using Meyer Law, proportional specimen resistance model, modified proportional specimen resistance model, elastic/plastic deformation model and the Hays–Kendall (HK) approach. The results showed that the HK approach was determined as the most successful model. Furthermore, X-ray powder diffraction and scanning electron microscope measurements were analyzed for superconducting properties of (Sm123)_1?x(Nd123)_x superconductor system. The results showed that microhardness values at the minimum load and averaged plateau region of load increased with increase of Nd123 concentration. Nd123 content can be used as to be estimated the microhardness value of (Sm123)_1?x(Nd123)_x superconducting sample in the range of 0.878–2.717 GPa. The control of the microhardness value by using Nd123 content in (Sm123)_1?x(Nd123)_x superconducting structure can be useful in technological applications in superconductivity industry.     

Tl2Ba2CaCu2O8 thin films on 2 in. LaAlO3(0 0 1) substrates

High quality Tl₂Ba₂CaCu₂O₈ (Tl-2212) superconducting thin films are prepared on both sides of 2 in. LaAlO₃(0 0 1) substrates by off-axis magnetron sputtering and post-annealing process. XRD measurements show that these films possess pure Tl-2212 phase with C-axis perpendicular to the substrate surface. The thickness unhomogeneity of the whole film on the 2 in. wafer is less than 5%. The superconducting transition temperatures T_cs of the films are around 105 K. At zero applied magnetic field, the critical current densities J_cs of the films on both sides of the wafer were measured to be above 2 × 10⁶ A/cm² at 77 K. The microwave surface resistance R_s of film was as low as 350 μΩ at 10 GHz and 77 K. In order to test the suitability of Tl-2212 thin films for passive microwave devices, 3-pole bandpass filters have been fabricated from double-sided Tl-2212 films on LaAlO₃ substrates.     

Structure and Superconducting Properties of Cd0.8Ba2(Y0.7Ca0.4)Cu3.5Oy

A new Cd-containing superconductor with nominal composition ofCd_0.8Ba₂(Y_0.7Ca_0.4)Cu_3.5O _y was synthesized and investigated. The obtained Cd and Ca-doped 123 phase exhibits an orthorhombic (T _c=80 K) or tetragonal (T _c=65 K) modification depending on the reaction atmosphere. It was shown that the combined Cd and Ca substitution facilitates the 123 phase formation. The results of the EDX analysis, as well as the comparison of the obtained lattice parameters with those of undoped, Cd-doped, and Ca-doped 123 have shown that both Cd and Ca enter the 123 phase and form a new Cd–Ba–Y–Ca–Cu–O superconducting compound.     

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 .     

Characterization of size-quantized PbTe thin films synthesized by an electrochemical co-deposition method

Size-quantized thin films of PbTe were electrodeposited on Au (1 1 1) substrates using a practical electrochemical method, based on the simultaneous underpotential deposition of Pb and Te from the same solution containing ethylenediamine tetraacetic acid, Pb²⁺, and TeO₃²⁻ at a constant potential. These thin films were characterized by X-ray diffraction (XRD), scanning tunneling microscopy (STM), atomic force microscopy (AFM), energy dispersive spectroscopy (EDS), and reflection absorption-FTIR (RA-FTIR). AFM, STM, and XRD results indicate that the growth of PbTe thin films follows the nucleation and two dimensional growth mechanism, resulting in high crystalline films of PbTe (2 0 0) in cubic structure, which was grown at a kinetically preferred orientation on Au (1 1 1). The EDS analyses of the films reveal that Pb and Te are present in an atomic ratio of approximately 1:1. The quantum-confined effect of the PbTe thin films are confirmed by the RA-FTIR measurements.     

Superconductivity and scanning tunneling microscopy (STM) / spectroscopy (STS) of transition metal oxide artificial lattices

High T_c superconducting artificial lattices and superlattices have been constructed by a laser molecular beam epitaxy. Layer-by-layer growth method controlled by RHEED and STM is a promising method for the construction of these artificial lattices. Formation and properties of superconducting artificial lattices and super-conducting / ferromagnetic superlattices are presented as the typical examples. In order to investigate the electronic state of carrier doped strongly correlated electronic system, STS measurements have been performed on La_2–xSr_xCuO₄, La_2–xSr_xNiO₄, and La_1-xSr_xMnO₃ thin films. Based on the similarities and the differences between the STS spectra of the three types of the films, electronic states of the strongly correlated system are discussed.     

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.     

Broadband Microwave Measurements of Overdoped Y0.9Ca0.1Ba2Cu3O7−δ Films Using Corbino Geometry

The surface impedance of Y_0.9Ca_0.1Ba₂Cu₃O_7?δ thin films was measured using the Corbino spectroscopy method. This special geometry, in which the sample dimensions are well defined by a ring pattern, is ideal for broadband high frequency reflection measurements. Using the complex reflected signal, S ₁₁, measured by a vector network analyzer, one can find the surface impedance of the thin film, from which the complex conductivity can be deduced. In the current work we present the three-standard approach for calibration of the Corbino method and demonstrate the benefits of this approach in measuring superconducting Y_0.9Ca_0.1Ba₂Cu₃O_7?δ thin films up to 20 GHz and down to 6 K. For the data analysis the well-known generalized two-fluid model was implemented, taking into account a film thickness which is much smaller than the normal state skin depth and superconducting penetration depth.     

Piezo- and electrooptics phenomena in high temperature superconducting films

Optically-induced linear electrooptics and elastooptics effects were discovered in high temperature superconducting Hg_0.85Pb_0.18Ba_0.13CuO_4+δ (Hg-1201) (T_c=112 K) single crystalline films deposited on the LiNbO₃ surface. Investigations were done by picosecond fast-resolved set-up. The set-up allowed to perform simultaneous measurements of birefirngence in regime of external fields with precision up to the 10⁻⁷. It was shown that below the superconducting critical temperature both piezooptic and linear electrooptics coefficients are substantially changed and show tremendous sensitivity to the appearance of superconductivity.     

YBCO-Buffered NdBCO Film with Higher Thermal Stability in Seeding REBCO Growth and Recycling Failed Bulk YBCO Superconductors

In this work, we report a strengthened superheating effect caused by a buffering YBa₂Cu₃O _y (YBCO or Y123) layer in the Nd_1+x Ba_2?x Cu₃O_7?y (NdBCO or Nd123) thin film with MgO substrate (i.e., NdBCO/YBCO/MgO thin film). In the cold-seeding melt-textured (MT) growth, the NdBCO/YBCO/MgO film presented an even higher superheating level, about 20 °C higher than that of nonbuffered NdBCO film (i.e., NdBCO/MgO film). Pole figure (X-ray Φ-scan) measurement reveals that the NdBCO/YBCO/MgO film has better in-plane alignment than the NdBCO/MgO film, which may be the main origin of the enhanced thermal stability. Using this NdBCO/YBCO/MgO film as the seed and under a maximum processing temperature (T _max) up to 1120 °C, we succeeded in growing various RE_1+x Ba_2?x Cu₃O_7?y (REBCO, RE=Gd, Sm, Nd, RE refers to rare elements) bulk superconductors and recycling the failed REBCO (RE=Y) bulks in a simple and feasible process.