Transport and Cu K-XANES Studies of (Hg,Cr)Sr2(Ca,Y)Cu2O6 + δ

The nominal (Hg_0.7Cr_0.3)Sr₂(Ca_0.7Y_0.3)Cu₂O_{6 +} , referred to as (Hg,Cr)-1212, were successfully synthesized at high temperature in partial vacuum. The samples were subsequently annealed in Ar or O₂ annealed at 300°C under ambient pressure. No T _c was observed in any of these samples down to 12 K which is in contrast to high pressure synthesized Y-free (Hg,Cr)-1212 phase where the latter exhibits a superconductivity at 80 K. The divalent state of Cu, as shown by XANES in the as-prepared (Hg,Cr)-1212, is not affected either by Ar or O₂ annealing. Depletion of holes due to trivalent Y substitution at the Ca-site, and a relatively higher 'a' lattice parameter (3.851 Å) are the apparent reasons for the non-superconducting nature of the samples.     

Structural stability of ZnFe2O4 nanoparticles under different annealing conditions

We study the structural stability of surfactant coated ZnFe₂O₄ (ZF) nanoparticles of average particle size 10 nm annealed under different environments. The X-ray diffraction studies in oleic acid coated ZF (OC-ZF) show distinctly different phase transitions under different annealing conditions. The OC-ZF is reduced to α-Fe/ZnO phase under vacuum while it forms FeO/ZnO under argon whereas the ZnFe₂O₄ phase remains stable under air annealing. The simultaneous thermo gravimetric analysis (TGA), differential scanning calorimetry (DSC) coupled mass spectra (MS) in OC-ZF under argon atmosphere suggests that the residual carbon removes oxygen from the lattice to reduce the ZnFe₂O₄ phase into FeO/ZnO during argon annealing. Apart from CO and CO₂ gas evolution at high temperature under argon annealing, creation of oxygen vacancies due to the random removal of oxygen under vacuum annealing, leads to direct interaction between Fe–Fe and the formation of metal Fe. It appears that the residual carbon aids the reduction of ZF and the formation of α-Fe/ZnO during vacuum annealing. After annealing at 1000 °C in vacuum, the magnetization is increased abruptly from 13.8 to 106.5 emu g⁻¹. In sharp contrast, the air and argon annealed samples show a diminished magnetization of 1 emu g⁻¹. The field cooled (FC) and zero FC magnetization of vacuum and argon annealed samples exhibit superparamagnetic and spin-glass type behavior respectively. Our results offer possibilities to switch a magnetically inactive material to an active one.     

Growth and vacuum post-annealing effect on the properties of the new absorber CuSbS2 thin films

Post-growth treatments in vacuum atmosphere were performed on CuSbS₂ films prepared by the single-source thermal evaporation method on glass substrates. The films were annealed in vacuum atmosphere for 2 h in temperature range 130-200 °C. The effect of this thermal treatment on the structural, optical and electrical properties of the films was studied. X-ray diffraction (XRD) patterns indicated that the films exhibited an amorphous structure for annealing temperature below 200 °C and a polycrystalline structure with CuSbS₂ principal phase. For the films annealed at temperatures below 200 °C one direct optical transition in range 1.8-2 eV was found. For the films annealed at 200 °C, two optical direct transitions emerged at 1.3 and 1.79 eV corresponding to the CuSbS₂ and Sb₂S₃ values respectively. The electrical measurements showed a conversion from low resistivities (3.10^− 2-9.10^− 2) Ω cm for the samples annealed at temperatures below 200 °C to relatively high resistivities (2 Ω cm) for the samples annealed at 200 °C. In all cases the samples exhibited p-Ztype conductivity.     

Microstructure and electrical properties of Al2O3-ZrO2 composite films for gate dielectric applications

Al₂O₃-ZrO₂ composite films were fabricated on Si by ultrahigh vacuum electron-beam coevaporation. The crystallization temperature, surface morphology, structural characteristics and electrical properties of the annealed films are investigated. Our results indicate that the amorphous and mixed structure is maintained up to an annealing temperature of 900 °C, which is much higher than that of pure ZrO₂ film, and the interfacial oxide layer thickness does not increase after annealing at 900 °C. However, a portion of the Al₂O₃-ZrO₂ film becomes polycrystalline after 1000 °C annealing and interfacial broadening is observed. Possible explanations are given to explain our observations. A dielectric constant of 20.1 is calculated from the 900 °C-annealed ZrO₂-Al₂O₃ film based on high-frequency capacitance-voltage measurements. This dielectric characteristic shows an equivalent oxide thickness (EOT) as low as 1.94 nm. An extremely low leakage current density of ∼2×10⁻⁷ A/cm² at a gate voltage of 1 V and low interface state density are also observed in the dielectric film.     

Role of oxygen in enhancing N-type conductivity of CuInS2 thin films

Post-growth treatments in air atmosphere were performed on CuInS₂ films prepared by the single-source thermal evaporation method. Their effect on the structural, optical and electrical properties of the films was studied by means of X-ray diffraction (XRD), scanning electron microscopy (SEM), optical reflection and transmission and resistance measurements. The films were annealed from 100 to 350 °C in air. The stability of the observed N-type conductivity after annealing depends strongly on the annealing temperature. Indeed it is shown that for annealing temperatures above 200 °C the N-type conductivity is stable. The resistance of the N-CuInS₂ thin films correlates well with the corresponding annealing temperature. The samples after annealing have direct bandgap energies of 1.45-1.50 eV.     

Observation of weakly adsorbed oxygen on Y5Ba6Cu11Oy

We observed, for the first time, adsorption of weakly bonded oxygen at low temperature (<-250°C) by a Y₅Ba₆Cu₁₁O _y sample, using thermogravimetric analysis. The resulting oxygen enriched phase in the surface layers may be attributed to the observation of a superconductivity-like transition at above 200 K.     

Effect of annealing on the characteristics of Au layers grown on the high-temperature deposited Ni50Fe50 layers

80 nm-thick Ni₅₀Fe₅₀ layers were sputter-deposited on glass substrates at 400 °C and then Au layers were sputter-deposited on the Ni₅₀Fe₅₀ layers. The Au/Ni₅₀Fe₅₀ bilayer films were annealed in a vacuum of 5×10⁻⁴ Pa from 250 to 450 °C for 30 min or 90 min. The characteristics of the Au layers were studied by Auger electron spectroscopy, field emission scanning electron microscopy, X-ray diffraction and a four-point probe technique. When the annealing temperature reaches 450 °C, Fe and Ni atoms diffuse markedly into the Au layer and the Fe content is more than the Ni content. When the annealing temperature is lower than 450 °C, the grain size of the Au layers does not change markedly with annealing temperature. However, as the annealing temperature reaches 450 °C, the annealing promotes the grain growth of the Au layer. As the annealing temperature exceeds 300 °C, the resistivity of the bilayer films increases with increasing annealing temperature. The diffusion of Fe and Ni atoms into the Au layer results in an increase in the resistivity of the annealed bilayer film. Large numbers of Fe and Ni atoms diffusing into the Au layer of the annealed Au/Ni₅₀Fe₅₀ bilayer film lead to a significant decrease in the lattice constant of the Au layer.     

Electrical properties of non c-axis oriented SrBi2(Ta0.95V0.05)2O9 thin films

Pulsed laser deposition technique was used to grow off c-axis oriented SrBi₂(Ta_0.95V_0.05)₂O₉ (SBTV) ferroelectric thin films. X-ray diffraction studies revealed the c-axis suppression in the films grown at lower substrate temperature (350°C) followed by annealing at higher temperatures (650°C). In-plane lattice parameters of the films were decreased with increase in annealing temperature. SBTV films annealed at 750°C exhibited enhanced ferroelectric properties with remanent polarization (2P _r) of 31.5 C/cm² and coercive field (E _c) of 157 kV/cm. The dielectric permmitivity of the films increased with increase in annealing temperature and it was attributed to the grain size dependence. The films annealed at 750°C showed maximum value of dielectric permittivity 172 with a tangential loss of 0.1, at 100 kHz. Higher value of dissipation factor at lower annealing temperature is explained in terms of space charge accumulation at grain boundaries. The leakage current densities of the films follow ohmic behavior at low field regime and space charge limited current dominates at higher fields.     

Metastable states of the 2223 phase in the Bi(Pb)SrCaCuO system

By the magnetically modulated microwave absorption method (MAMMA) we observed the modifications induced by different calcination temperatures (between 830°C and 870°C) on the 2223 phase formed in a system sintered at (855±5)°C with the starting composition Bi_1.7Pb_0.3Sr₂Ca₂Cu₃O _y . The presence of the 2223 phase in almost distinct states (consequently, multiple 2223 phases) in the same sample was observed. As the calcination temperature was increased up to 850°C, the highest temperature state of the 2223 phase intensified. Higher calcination temperatures resulted in the enhancement of other lower-temperature states. The homogeneity of the 2223 phase was greatly improved by annealing the samples at, 800°C for 5 min in a flowing nitrogen atmosphere. We labeled as metastable the lower-temperature states having excess oxygen, which, by easily losing the supplementary oxygen under the above annealing procedure, were shifted to higher temperatures.     

Electrical and magnetic properties of Ni0.8Zn0.2Fe2O4/silica composite prepared by sol-gel method

Ultrafine Ni_0.8Zn_0.2Fe₂O₄ particles dispersed in silica (SiO₂) matrix are produced by sol-gel method. The powders were subjected to X-ray diffraction to confirm the formation of crystalline phases. The physical properties such as bulk density, true density, % of porosity and % of linear shrinkage were studied. The magnetic permeability as the function of frequency from 1 kHz to 13 MHz and temperatures from room temperature to 300°C were studied for samples sintered at temperature 1250°C. The AC electrical resistivity as the function of frequency and DC electrical resistivity as the function of temperature were studied. The AC-resistivity of the order of 10⁵ cm and DC-resistivity 10⁸ cm were obtained at room temperature. Microstructural features of sintered samples show the presence of ferrite grains of 1–2 m size.     

Si nanocrystals in SiO2 films analyzed by small angle X-ray scattering

Amorphous SiO/SiO₂ multilayers were studied using grazing-incidence small-angle X-ray scattering (GISAXS). Such SiO/SiO₂ superlattices were prepared by alternately magnetron sputtering of 3 nm thin films of SiO and 3 nm of SiO₂ (10 layers each) on Si (100) substrate. Rotation of the Si substrate during evaporation ensures the homogeneity of the films over the whole substrate. After evaporation the samples were annealed at 1050 °C for 2 h in vacuum or in air. The analysis of the 2D GISAXS pattern has shown that Si nanocrystals are formed in the annealed samples. Using a Guinier approximation, the inter-nanocrystal distance (10.5 nm) and radius of gyration (2.3 nm) have been obtained for the samples annealed in vacuum. Samples annealed in air have shown similar peak values which were however, much wider distributed.     

Interfacial reactions for the non-stoichiometric TiB x /(100)Si system

In order to evaluate the interfacial reactions in the TiB _x /(100)Si system and the thermal stability of non-stoichiometric TiB _x films (0 B/Ti 2.5), TiB _x /Si samples prepared by a co-evaporation process were annealed in vacuum at temperatures between 300 and 1000°C. The solid phase reactions were investigated by means of sheet resistance, X-ray diffraction, transmission electron microscopy, X-ray photo-electron spectroscopy, and stress measurement. For TiB _x samples with a ratio of B/Ti 2.0, an apparent structural change is not observed even after annealing at 1000°C for 1 h. For samples with a ratio of B/Ti < 2.0, however, there are two competitive solid phase reactions: the formation of a titanium silicide layer at the interface and the formation of a stoichiometric TiB₂ layer at the surface, indicating the salicide process. The sheet resistance and the film stress in the Ti/Si and TiB _x /Si systems are well explained by the solid phase reactions.     

Study on microstructure and magnetic domain structure in sputtered (Ni66Fe22Co12) x C1−x nanocomposite films

Composition and annealing temperature dependence of microstructure and magnetic domain structure in sputtered (Ni₆₆Fe₂₂Co₁₂) _x C_1–x nanocomposite films with x=10–75 at % were studied by X-ray diffraction and magnetic force microscopy (MFM). Films with x20 at % showed amorphous structures, and no domain structure could be found due to the disappearance of magnetocrystalline anisotropy. For the films with x=30–55 at %, face-centered cubic (fcc) NiFeCo nanocrystals encapsulated in graphite-like carbon could be found in the samples annealed beyond 400 °C, and stripe domains with typical dimension of 120–150 nm were observed. For the films with x62 at %, the as-deposited films went through a meta-stable stage at which a rhombohedral Ni₃C phase and fcc NiFeCo co-existed after annealing to a temperature between about 300–400 °C (dependent on composition). Upon further annealing to a sufficiently high temperature between about 350–500 °C, the carbide phase decomposed into fcc NiFeCo and graphite. While short-range domain structures were observed in the samples before the formation of carbide phase, long-range domain structure with dispersed domains in the meta-stable stage were observed. After the decomposition of carbide, large domains with typical size of 500–700 nm were observed due to the formation of large grain aggregators.     

Preparation, dielectric and ferroelectric properties of Pb5Ge3O11 and Pb5Ge2.85Si0.15O11 thin films fabricated by sol-gel process

Lead germanate-silicate (Pb₅Ge_2.85Si_0.15O₁₁) ferroelectric thin films were successfully fabricated on Pt/Ti/SiO₂/(100)Si substrates by the sol-gel process. The thin films were fabricated by multi-coating at preheating temperatures of 350 and 450 °C. After annealing the thin films at 600 °C, the films exhibited c-axis preferred orientation. The degree of c-axis preferred orientation of the thin films preheated at 350 °C was higher than that of films preheated at 450 °C. Grain growth was influenced by the annealing time. The thin films exhibited a well-saturated ferroelectric P-E hysteresis loop when preheated at 350 °C and annealed at 600 °C for 1.5 h. The values of the remanent polarization (Pr) and the coercive field (Ec) were approximately 2.1 μC/cm² and 100 kV/cm, respectively.     

Anisotropy in the resistive superconducting transition under magnetic fields in single crystal Pb2Sr2Ho0.5Ca0.5Cu3O8

Anisotropie properties of the single crystal Pb₂Sr₂Ho_0.5Ca_0.5Cu₃O₈ have been investigated by measuring the electrical resistivity in theab-plane _ab (H, ,T), which depends on the angle between theab-plane and the magnetic-field direction, in various constant fieldsH perpendicular to the current direction. All the angle-dependent values of _ab (H, ,T) at a constant temperature are scaled to be on one curve as a function of reduced field. The anisotropic parameter (m _c ^* /m _ab ^* )^1/2 is estimated as 12–13, which is larger than that of YBa₂Cu₃O₇ and much smaller than that of Bi₂Sr₂CaCu₂O₈. It has been concluded that the anisotropy does not always depend on the thickness of the blocking layer but seems to depend on the overlap of the electronic wave functions along thec-axis. Anisotropy in the pinning potential has also been discussed from the resistive tail in the temperature dependence of _ab (H,,T).     

Growth and characterization of Bi2Sr2Ca1Cu2O8+x single crystals

High-quality single crystals are well suited to the investigation of some intrinsic material properties. A modified Bridgman method using a sharp temperature gradient (300°C/cm) was used to grow Bi₂Sr₂Ca₁Cu₂O_8+x single crystals. Although the samples were contained in alumina ampoules, no aluminium contamination of the samples was detected. Blade-shaped crystals up to 7–8 mm length and 3–4 mm width could be grown by this method, although extraction from the matrix was difficult. Electron diffraction patterns of the [001] zone axis revealed a high degree of crystallinity. The narrowness of the superconducting transition temperature, as determined by ac susceptibility, also suggests the existence of well-formed crystalline domains. In order to determine the relative orientation of the crystalline domains, electron channeling patterns were recorded from several consecutive growth steps from a fracture surface. The poor contrast of these and Kikuchi patterns suggests the presence of a stacking structure. The results showed a [100] growth direction and (001) cleavage plane. Reversible oxygen loss at the peritectic decomposition temperature of 863°C was observed. Knoop indentation measurements showed that the crystals were quite soft, having a microhardness of 0.44 GPa.     

BPSCCO Superconductor with Addition of Ag2O Synthesized Under Electrical Field

Ag₂O-doped (1.2% wt.) nitrate freeze-dried powders (Bi : Pb : Sr : Ca : Cu = 1.7 : 0.3 : 2 : 2.5 : 3.5) were processed under an external electrical field and 17.5 MPa pressure at 800°C, for 4 min in vacuum. Final heat treatments (HT) were applied at 835–850°C for 70 h. in air (Bi, Pb)₂Sr₂CaCu₂O _x (2212-phase) was formed by electrical field processing in just 4 min. Electrical field application enhanced (Bi, Pb)₂Sr₂Ca₂Cu₃O _y (2223-phase) formation during final HT. Ag₂O additions to field sintered BSCCO ceramics increased the amount of 2223-phase and the zero resistance critical temperature (T _e(R=0)) by 4 k.     

Analyzing residual stress in bilayer chalcogenide Ge2Se3/SnTe films

Chalcogenide thin film stacks of polycrystalline SnTe and amorphous Ge₂Se₃ are analyzed for residual stress using X-ray diffraction. The as-deposited film stacks are annealed at different temperatures and the thermal dependence of stress is investigated. Stress evaluations are performed by employing the sin²ψ technique using a 2D area detector system. As-deposited samples are found to be compressively stressed and exhibit increasingly tensile thermal stress with increasing annealing temperature. Onset of crystallization of the bottom Ge₂Se₃ layer is indicated by a sharp drop in the stress level in the 270 °C-360 °C temperature range, due to volume shrinkage associated with the crystallization. Diffraction patterns of samples annealed at different temperatures indicate compositional changes that are attributed to inter-diffusion of ions between the two layers. The XRD profiles of samples annealed at 360 °C and 450 °C indicate the formation of a Ge₂Se₃-SnTe solid solution. It is suggested that both, residual stress and temperature dependent compositional changes affect the measured d spacings.     

Electrical Activity of Native Defects in n-Type ZnSe Crystals

The transport properties of n-type ZnSe crystals annealed in liquid Zn at temperatures from 600 to 950°C are studied in the range 55–500 K. As the annealing temperature increases to above 650°C, the concentration of shallow donors rises sharply, their ionization energy decreases from 28 to 9 meV, and the compensation ratio drops from 0.91 to 0.35. The electrical conductivity of the crystals annealed at low temperatures is determined by shallow donors such as Al_Zn, Ga_Zn, and In_Zn. At annealing temperatures above 800°C, the concentration of zinc vacancies, compensating the shallow donors, decreases sharply, whereas the concentration of selenium vacancies, which act as shallow donors and determine the electrical conductivity of the crystals, rises markedly. Reducing the annealing temperature to below 650°C drastically decreases the conductivity and electron concentration of the samples and leads to anomalously low carrier mobilities. The observed anomalies in the transport properties of illuminated n-type ZnSe crystals are interpreted in terms of a random impurity potential.