Microstructure and Magnetic Properties of Sn<Subscript>1 − <Emphasis Type="Italic">x</Emphasis></Subscript>Ni<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript>O<Subscript>2</Subscript> Thin Films Prepared by Flash Evaporation Technique

An effort was made to develop semiconductor oxide-based room temperature dilute magnetic semiconductor (DMS) thin films based on wide band gap and transparent host lattice with transition metal substitution. The Sn\(_{\mathrm {1}-x}\)Ni\(_{x}\textit {O}_{\mathrm {2}}\) (\(x\,= \mathrm {0.00, 0.03, 0.05, 0.07, 0.10, and \,0.15}\)) thin film samples were prepared on glass substrates by flash evaporation technique. All the samples were shown single phase crystalline rutile structure of host SnO\(_{\mathrm {2}}\) with dominant (110) orientation. The Ni substitution promotes reduction of average crystallite size in SnO\(_{\mathrm {2}}\) as evidenced from the reduction of crystallite size from 40 (SnO\(_{\mathrm {2}}\)) to 20 nm (Sn\(_{\mathrm {0.85}}\)Ni\(_{\mathrm {0.15}}\textit {O}_{\mathrm {2}}\)). In the energy dispersive spectra as well as X-ray photoelectron spectra of all the samples show, the chemical compositions are close to stoichiometric with noticeable oxygen deficiency. The crystalline films were formed by coalescence of oval-shaped polycrystalline particles of 100 nm size as evidenced from the electron micrographs. The energy band gap of DMS films decreases from 4 (SnO\(_{\mathrm {2}}\)) to 3.8 eV (x \(=\) 0.05) with increase of Ni content. The magnetic hysteresis loops of all the samples at room temperature show soft ferromagnetic nature except for SnO\(_{\mathrm {2}}\) film. The SnO\(_{\mathrm {2}}\) films show diamagnetic nature and it converts into ferromagnetic upon substitution of 3 % Sn\(^{\mathrm {4+}}\) by Ni\(^{\mathrm {2+}}\). The robust intrinsic ferromagnetism (saturation magnetization, 21 emu/cm\(^{\mathrm {3}}\)). Further increase of Ni content weakens ferromagnetic strength due to Ni-O antiferromagnetic interactions among the nearest neighbour Ni ions via O\(^{\mathrm {2-}}\) ions. The observed magnetic properties were best described by bound magnetic polarons model.     

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.     

Certification of YBa<Subscript>2</Subscript>Cu<Subscript>3</Subscript>O<Subscript>7−<Emphasis Type="Italic">x</Emphasis></Subscript> Single Crystals

A method for evaluation of the critical temperature T _c and the width of the superconducting transition ΔT _c in HTSC single crystals has been developed. By this method, the first derivative of the temperature dependence of the resistivity, \(\frac{\partial \rho (T)}{\partial T}\), is constructed. A technique for synthesis of YBa₂Cu₃O_7?x single crystals with highly reproducible physical-mechanical properties has been described. A standard sample with T _c=94 K and ΔT _c=0.25 K has been synthesized and certified.     

Sintering mechanisms in YBa<Subscript>2</Subscript>Cu<Subscript>3</Subscript>O<Subscript>7−<Emphasis Type="Italic">x</Emphasis></Subscript> superconducting ceramics

The densification of ceramic compacts of YBa₂Cu₃O_7−x (123) was studied with a vertical dilatometer. The runs effected under isothermal conditions (ISO) covered the 920–970^∘C range and were performed under static air atmosphere. Also, controlled heating rate (CHR) runs, from about 800 to 1050^∘C, were conducted at 5^∘C/min under either flowing oxygen or static air. The ISO data could be satisfactorily fitted by the solution-precipitation (SP) model giving an activation enthalpy of 221 kJ/mol. Furthermore, the CHR data for 920–970^∘C was also fitted with the same model giving 207 kJ/mol as the activation energy. From analysis of CHR data, the initial stage sintering is driven by solid state sintering between 827–894^∘C (823–908^∘C in O₂). Then, in the interval 902–920^∘C (914–934^∘C in O₂) the intermediate stage driven by grain growth (GG), competes with the rearrangement process associated to the presence of a liquid phase. This last process applied because the next sintering stage in the range 922–970^∘C (938–990^∘C in O₂ flow) could be fitted by the SP model with an activation enthalpy of 207 kJ/mol (229 kJ/mol in O₂). In the range 972–995^∘C (990–1014^∘C in O₂), the solid state (GG) intermediate stage mechanism and/or viscous flow competes with the SP process.     

Enhanced Superconductivity in Double-Doping Cu<Subscript>0.15</Subscript>TaSe<Subscript>2−<Emphasis Type="Italic">x</Emphasis></Subscript><Emphasis Type="Italic">S</Emphasis><Subscript><Emphasis Type="Italic">x</Emphasis></Subscript>

Superconducting Cu _x TaSe₂(x=0.05, 0.15) and Cu_0.15TaSe_2?x S _x (x=0, 0.5, 1, 1.5) single crystals have been systematically fabricated by a chemical vapor transport method. It is found that the double doping in TaSe₂, i.e., the simultaneous intercalation of Cu and substitution of Se by S, can substantially enhance the superconducting transition temperature. Transport property measurements give evidence of the coexistence and competition of charge density wave state and superconductivity in Cu _x TaSe₂ which provide meaningful information to understand the complex electronic states in this system. The parallel shift and the fan-shape broadening behaviors are observed in the superconducting transition curves under magnetic fields of Cu_0.15TaSeS and TaSeS, respectively, indicating an increase of coherence length and suppression of superconducting fluctuation induced by copper intercalation.     

Photoluminescence Properties of the Zn<Subscript>1−<Emphasis Type="Italic">x</Emphasis></Subscript>Y<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript>O Tubes Prepared by Polycarbonate Templates

We have prepared Zn_1−x Y _x O (x=0 and 0.01) tubes to study its structural and photoluminescent properties. A pore wetting process of porous polycarbonate templates with the liquid precursor and following thermal treatment were utilized for preparing the Zn_1−x Y _x O tube structure. Using the polycarbonate template with pore size of about 2 μm diameter, the Zn_1−x Y _x O tubes were obtained. Photoluminescence (PL) spectroscopy was used to measure optical emissions from 350 to 650 nm with a He-Cd laser. The results of the PL spectra show that the Zn_1−x Y _x O tubes have evident emission peaks at the UV (about 380 nm) and visible (around 500 to 650 nm) region. The emission peak at the UV region was slightly shifted to higher wavelengths with increasing Y content. Meanwhile, the green and yellow emission peaks intensity increases as Y content increases. These results are explained by the structure tuning and oxygen deficiency with the introduction of Y.     

Synthesis and Characterization of Ni<Subscript>1−<Emphasis Type="Italic">x</Emphasis></Subscript>Cu<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript>Bi<Subscript>3</Subscript> Superconductor

In this paper, we characterized the microstructure and superconducting properties of Cu-doped NiBi₃ samples. The polycrystalline Ni_1?x Cu _x Bi₃ (0 ≤ x ≤ 0.10) samples were prepared using a solid-state reaction method. The crystal structure and unit cell parameters were determined by Rietveld refinement of powder X-ray diffraction. The data showed that the main phase present corresponded to NiBi₃ without dependence on the Cu concentration, but with small quantities of Ni and Bi. The SEM and AFM measurements revealed that the main phase was inhomogeneous at microscopic level, with Bi richer regions in comparison to other regions. However, Raman spectroscopy results did not show significant changes in the spectra with Cu doping and in different regions of the samples. Another finding was that regardless of Cu doping, the superconducting transition temperature was 4.05–4.06 K.     

Fabrication and Analysis of Tri-layer YBa<Subscript>2</Subscript>Cu<Subscript>3</Subscript><Emphasis Type="Italic">O</Emphasis><Subscript>7−<Emphasis Type="Italic">δ</Emphasis></Subscript> Thick Films by Low-Fluorine MOD Method

Improving the thickness of superconducting layer in coated conductors is an effective way to enhance its critical current. In this work, tri-layer YBCO/YBCO/YDyBCO films were successfully deposited on buffered Hastelloy substrate using the multi-coating lowfluorine metal-organic decomposition (LF-MOD) method and the thickness of the films can be up to 2.4 μ m. The effects of high-temperature annealing time on microstructures and superconducting properties of the films were systematically studied. Energy dispersive X-ray spectroscopy (EDS) results reveal that there remains a large amount of F element in the upper layer of the film when the annealing time is too short. With increasing the annealing time, the fluoride-containing precursor converts to YBCO grains completely. But the coarsening of grains appeared, and the critical current density (J _c) of the film dropped slightly when the annealing time is too long. The cross-sectional scanning electron microscope (SEM) image and EDS plane analysis were applied to investigate the microstructure and element distribution of the final triple-layer YBCO films, respectively. The critical current of the final YBCO superconducting film could reach 316 A (77 k, self-field) for 1.2-cm-wide tapes with the optimal annealing conditions.     

Properties of YBaCuFe<Subscript>1 − <Emphasis Type="Italic">x</Emphasis></Subscript>Ni<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript>O<Subscript>5</Subscript> (0 < <Emphasis Type="Italic">x</Emphasis> ≤ 0.3) solid solutions

YBaCuFe_{1 – x}Ni_xO₅ solid solutions are shown to exist for x 0.3. Data are presented on the lattice parameters, thermal stability, thermal expansion, electrical conductivity, thermoelectric power, magnetic susceptibility, and dielectric properties of the solid solutions. Ni substitution for Fe notably increases the electrical conductivity of the solid solutions, reduces their thermoelectric power and thermal expansion, and shifts the antiferromagnetic—paramagnetic phase transition and dielectric anomalies in YBaCuFe_{1 – x}Ni_xO₅ to lower temperatures.Translated from Neorganicheskie Materialy, Vol. 40, No. 12, 2004, pp. 1515–1519.Original Russian Text Copyright © 2004 by Chizhova, Klyndyuk, Bashkirov, Petrov, Makhnach.     

Electrical properties of YBa<Subscript>2</Subscript>Cu<Subscript>3</Subscript>O<Subscript>7−<Emphasis Type="Italic">x</Emphasis></Subscript> films of various thicknesses

We have studied the electrical properties of high-T_c superconductor YBa₂Cu₃O_7?x films obtained by the ion-plasma deposition technique on sapphire substrates. Dependences of the surface resistance and the critical current density on the film thickness are determined.     

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.     

Effect of Ba/Y Molar Ratio on Superconducting Properties of BaTiO<Subscript>3</Subscript>-Doped YBa<Subscript>2</Subscript>Cu<Subscript>3</Subscript><Emphasis Type="Italic">O</Emphasis><Subscript>7−<Emphasis Type="Italic">δ</Emphasis></Subscript> Films

YBa₂Cu₃ O _7?δ (YBCO) films with BaTiO₃ (BTO) nanostructures were prepared by using the precursor solutions with different cationic molar ratios of Y:Ba:Cu = 1.0:1.6–2.0:3.0 in the TFA-MOD process. These YBCO films were deposited on (00 l)-oriented LaAlO₃ single-crystal substrates using a spin coater. The high superconducting critical current density (J _C) (77 K, self-filed) of more than 10 MA/cm² for the final BTO-doped YBCO film was obtained. Moreover, the effect of different Ba/Y molar ratios in the precursor solution on superconducting properties of BTO-doped YBCO films was investigated. Compared with the BTO-doped YBCO film deposited by using the precursor solutions with Ba/Y molar ratio of 2.0, an enhancement of J _C in a magnetic field for the film from the solution with Ba/Y molar ratio of 1.9 was achieved. For Ba/Y molar ratios of 1.6 and 1.7, a reduction of J _C in a magnetic field occurred. The J _C enhancement may be mainly ascribed to the enhanced flux pinning by the Y₂Cu₂ O ₅ nanostructures with the optimal number dispersing in YBCO matrix.     

Magnetic Properties and Superconductivity in GdFeAsO<Subscript>1−<Emphasis Type="Italic">x</Emphasis></Subscript>F<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript>

Abstract A series of GdFeAsO_1−x F _x (x=0,0.1, 0.2, and 0.25) samples have been synthesized with conventional solid-state method. The phase purity is significantly improved by using Fe₂O₃ as the source of oxygen, compared to those prepared using Gd₂O₃ as the precursor. The lattice parameters are found to shrink with increasing fluorine doping level. The F-doped samples show a superconducting transition with T _c increasing with doping level, reaching T _c=40.1 K at x=0.25. A pronounced Curie–Weiss-like paramagnetic background, which is usually attributed to the impurity phases, is found to be independent of the fluorine doping level and proven to come from the Gd³⁺ in the GdFeAsO_1−x F _x compound with the effective magnetic moment of Gd³⁺ being μ _eff=7.83±0.05 μ_B. The extrapolated slope of dH_c2/dT|_T=Tc{dH}_{\mathrm{c2}}/dT|_{T=T_{\mathrm{c}}} in this system is about −4.5 T/K.     

Superconducting and Magnetic Properties of Zn-doped YBa<Subscript>2</Subscript>Cu<Subscript>3</Subscript>O<Subscript>7−<Emphasis Type="Italic">δ</Emphasis></Subscript>

The superconducting properties and AC/DC magnetic properties of YBa₂Cu_3−x Zn _x O_7−δ , (x=0.0, 0.01, 0.03, 0.05, 0.10 and 0.15) compounds were investigated. Samples were synthesized through solid-state reaction route. X-ray diffraction data confirms the single-phase orthorhombic/tetragonal crystallization for the studied samples. Thermo-Gravimetric Analysis (TGA) was done for pure and Zn-doped YBa₂Cu₃O_7−δ (YBCO) samples. Results reveal that at higher dopant levels the doped samples are more oxygen-deficient than the undoped ones. The superconducting properties of YBa₂Cu_3−x Zn _x O_7−δ system always enhance with addition of oxygen to Cu–O chains, which causes enhancement of superconducting carrier density together with orthorhombic structure. Zn substitution causes an overall reduction of superconducting condensation energy with systematic degradation of superconducting properties like T _c and J _c. This occurs via induced non-homogeneity of hole carrier density created by extended nature of perturbation on electronic structure in CuO₂ planes and its weak-link type behavior. AC susceptibility measurement reveals that Zn doping reduces the inter-granular couplings. Scanning Electron Microscope (SEM) images indicate that increment of average grain size with increasing of Zn concentration.     

Influence of Oxygen on the Tribomechanical Properties of Single Crystals of YBa<Subscript>2</Subscript>Cu<Subscript>3</Subscript>O<Subscript>7−<Emphasis Type="Italic">δ</Emphasis></Subscript>

This paper reports a study on the mechanical and tribological properties of ab- and a (b) c?planes of YBa₂Cu₃O_7?δ single crystals. The single crystals were grown using a CuO-BaO self-flux method. The oxygenation effect on the mechanical and tribological properties of ab- and a (b) c?planes is reported. For the ab- plane, the hardness and elastic modulus were around 6 and 50 GPa, respectively. In this case, significant differences were not observed among the hardness and elastic modulus at different oxygenation states. However, the hardness and elastic modulus for as-grown and oxygenated YBa₂Cu₃O_7?δ single crystals were different from that of the a (b) c?plane, and were observed to be slightly higher for the as-grown than for the oxygenated samples. For as-grown and oxygenated samples, we observed hardness values around 4.7 and 2.0 GPa, respectively. Regarding the elastic modulus, the values were 75 and 40 GPa, respectively. The indentation fracture toughness values on the ab- plane for the as-grown and oxygenated YBa₂Cu₃O_7?δ single crystal were 3.7 ± 1.2 and 2.9 ± 1.2 MPa m^1/2, respectively. For the ab- plane, the scratch resistance of the as-grown sample was higher than that of the oxygenated sample and the scratches under load were deeper for the oxygenated sample. As regards the a (b) c?plane, the scar features were seemingly constant through all the scratch lengths and the scratches under load were deeper and larger for the oxygenated than that for the as-grown sample.     

Preparation and Properties of Mn<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript>Hg<Subscript>1 − <Emphasis Type="Italic">x</Emphasis></Subscript>Te

Mn _x Hg_{1 ? x}Te (x = 0.05, 0.12) single crystals were grown by solid-state recrystallization, and their axial and radial homogeneity was assessed by optical, electrical, and electron-microscopic measurements. The crystals are p-type, with a hole concentration of (4.3–5.3) × 10²² m^?3 and Hall mobility in the range (410–570) × 10^?4 m²/(V s).     

AC Susceptibility and Superconducting Properties of Graphene Added YBa<Subscript>2</Subscript>Cu<Subscript>3</Subscript>O<Subscript>7−<Emphasis Type="Italic">d</Emphasis></Subscript>

The effect of graphene (G) addition on YBa₂Cu₃O_7?δ(G)_x (x =?0 ? 0.03 wt%) has been studied using the X-ray diffraction method, scanning electron microscopy, electrical resistance versus temperature, transport critical current density J_c, and AC susceptibility measurements. XRD patterns showed single-phase YBa₂Cu₃O_7?δ (YBCO) for all samples. SEM micrographs showed filling of the voids between YBa₂Cu₃O_7?δ grains as graphene was added. The temperature-dependent electrical resistance curves showed metallic normal state behavior and onset transition temperature T_conset between 90 and 92 K for all samples. AC susceptibility measurement showed transition temperature \(T_{\mathrm {c} \chi ^{\prime }}\) between 90 and 93 K. \(T_{\mathrm {c} \chi ^{\prime }}\) was maintained or improved slightly as graphene was added. The x =?0.001 wt% showed the highest J_c, i.e., 2750 A cm^?2 at 77 K and 5570 mA cm^?2 at 30 K which was 13 and 40 times higher than that of the non-added YBCO, respectively. The peak temperature T_p of the imaginary part of the susceptibility χ^″ was around 78–82 K for all samples indicating grain coupling was not weakened as graphene was added.     

Microhardness of the YbAg<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript>In<Subscript>1 − <Emphasis Type="Italic">x</Emphasis></Subscript>Cu<Subscript>4</Subscript> alloy system

We report Vickers microhardness measurements on flux grown single crystals of the YbAg_xIn_{1 − x}Cu₄ alloy system. Although sample dependent, the microhardness exhibits a clear concentration dependence: in general, it decreases with x. The lattice parameter as a function of x exhibits a similar behavior. For x < 0.5, where the lattice parameter is almost constant, the microhardness exhibits a weak enhancement. Similar concentration dependence of the lattice parameter, resistivity and microhardness allows us to conclude that the microhardness reflects the evolution of the YbAg_xIn_{1 − x}Cu₄ alloy system towards more metallic character with increasing x.     

Properties of amorphous Si<Subscript>1 − <Emphasis Type="Italic">x</Emphasis></Subscript>Ge<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript>:H (<Emphasis Type="Italic">x</Emphasis> = 0−1) films

Plasma deposition has been used to grow Si_1?x Ge _x :H(x= 0 ? 1) films, undoped and doped with PH₃ or B₂H₆, for p-i-n solar cells and other optoelectronic applications. The optical, electrical, and photoelectric properties of the films have been studied at constant hydrogenation and doping levels. The films deposited under appropriate conditions are amorphous, and three-layer solar cells fabricated from such films offer an efficiency of 9.5% at an illumination of 100 mW/cm². The photoresponse of the a-Si_{1 ? x} Ge _x :H films strongly depends on Ge content. The hydrogen concentration in the films was controlled by varying the gas phase composition and was determined from the IR absorption in the films.     

Negative temperature coefficient thermistor based on BaFe<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript>Sn<Subscript>1−<Emphasis Type="Italic">x</Emphasis></Subscript>O<Subscript>3−ε</Subscript> solid solutions

A negative temperature coefficient (NTC) thermistors based on BaFe _x Sn_1−x O_3−ε were fabricated by conventional solid-state reaction method. The microstructure and electrical properties of the NTC thermistors were characterized by X-ray diffraction (XRD), electric (R(T)), and impedance measurements. The XRD analysis shows that the BaFe _x Sn_1−x O_3−ε still remains cubic perovskite structure and the crystal growth orientation changes at higher Fe content. Similarly, the electric measurements indicates that all the samples show typical NTCR behavior; with increasing Fe content, the room temperature resistivity, activation energy, and thermistor constant decrease, are in the range of 2.52–217 KΩ cm, 0.343–0.43 eV, and 3900–4896 K, respectively. The impedance spectroscopy confirms that the observed ac resistance, consisting of the grain bulks, grain boundaries, and electrode–ceramic interface, mainly attributes to the grain boundaries and grain bulks; with the rise in temperature the grain boundary resistance shows more rapid change than the grain resistance; moreover, the Fe concentration can greatly affect the grain and grain boundary resistance.