Analysis of Cu and O in high-Tc superconductors by 7–9 MeV protons

The use of proton-induced γ-ray emission for the simultaneous analysis of Cu and O in high-T_c superconductors is demonstrated. Utilizing 7–9 MeV protons, the ratio of O relative to Cu can be determined reliably to a few percent accuracy in homogeneous bulk samples and films thicker than 130 μm using standard bulk samples of O and Cu. Results of the present method are compared with those of the analysis of YBa₂Cu₃O_7xdone by the Rutherford scattering of particles and the non-Rutherford scattering through the ¹⁶O(p,p₀)¹⁶O reaction.     

Investigation of films of YBa2Cu3O7 using Rutherford backscattering spectrometry

Rutherford backscattering spectrometry (RBS) has been applied to films of the high-temperature superconductor YBa₂Cu₃O₇. The films were prepared by rf and dc sputtering and silk-screen printing onto substrates of alumina, sapphire and magnesia. Some of the samples were exposed to various heat treatments in order to promote the superconducting phase. A 2 MeV beam of He⁺ particles from the 3 MV Dynamitron accelerator at Birmingham University's School of Physics and Space Research was employed for the RBS measurements. The composition and the depth profile of the elements in the films were determined by simulating the observed RBS spectra with a simulation software package. The simulations show that the heat treatment causes marked interdiffusion of the film and substrate. The experimental results and the computer simulations shown in this paper illustrate the advantages of using RBS to characterise films of the new superconducting materials.     

2 MeV Si ion implantation damage in relaxed Si1−xGex

The damage produced by implanting, at room temperature, 3 μm thick relaxed Si_1−xGe_x layers with 2 MeV Si⁺ ions has been measured as a function of Ge content (x = 0.04, 0.13, 0.24 or 0.36) and Si dose in the dose range 10¹⁰–10¹⁵ cm⁻². The accumulation of damage with increasing dose has been studied as a function of Ge content by Rutherford Backscattering Spectrometry, Optical Reflectivity Depth Profiling and Transmission Electron Microscopy and an increased damage efficiency in Si_1−xGe_x with increasing x is observed. The characteristics of implantation-induced defects have been investigated by Electron Paramagnetic Resonance. The results are discussed in the context of a model of the damage process in SiGe.     

A comparative EPR study of ion implantation induced damage in Si, Si1−xGex (x ≠ 0) and SiC

Electron Paramagnetic Resonance (EPR) measurements have been made to investigate the build up of damage in silicon in relaxed crystalline Si_1−xGe_x (x = 0.04, 0.13, 0.24, 0.36) and in 6H-SiC as a result of increasing the ion dose from low levels (10¹² cm⁻²) up to values (10¹⁵ cm⁻²) sufficient to produce an amorphous layer. Si, Si_1−xGe_x (x ≠ 0) and SiC were implanted at room temperature with 1.5 MeV Si, 2 MeV Si and 0.2 MeV Ge ions respectively. A comparison is made between the ways in which the type and population of paramagnetic defects depend on ion dose for each material.     

Magnetic ordering in superconducting YBa2(Cu1−xFex)3Oy oxide

Magnetic susceptibility measurement and the zero-field muon-spin-relaxation experiment have been made for the YBa₂(Cu_1−xFe_x)₃O_y system. The susceptibility has been measured in the field strong enough for the magnetic flux to penetrate the superconductor and the resultant temperature dependence has demonstrated the field cooled effect and a cusp at low temperatures below T_c. The cusp has been observed when the high field has been applied. The dynamical depolarization rate of the muon obtained by the muon-spin-relaxation experiment has shown the maximum at the same temperature as the cusp. The results suggest that the spin glass freezing of localized magnetic moment takes place at the temperature of the cusp, which is consistent with the previous Mössbauer effect experiments. The magnetic phase diagram for the system has been obtained.     

Micro-PIXE and channeling PIXE analysis of Ag-doped YBa2Cu3O7−δ thin films

Nuclear Microscopy, utilizing a 2 MeV He⁺ beam for channeling Rutherford Backscattering (RBS) and PIXE analysis, was used to characterise Ag-doped YBa₂Cu₃O_7−δ thin films and measure the lateral distribution of the Ag. The samples were prepared by in situ two-beam pulsed laser deposition in order to investigate the effects of such dopings on critical current densities [1 and 2]. Films deposited at temperatures above 650°C form needle-like surface structures with a length of up to 100 μm; these tend to align with in-plane a–b axis. Results for a sample prepared at a substrate temperature of 730°C and a maximum Ag concentration of 5 at.% are discussed. The needle-like structures were found to be rich in Ag and Cu, and the YBa₂Cu₃O_7−δ film contained 0.02 at.% Ag. Broad beam PIXE-channeling results indicate that 19% of the Ag is substitutional.     

Density measurement of amorphous SixGe1 − x alloys

The atomic density of amorphous Si_xGe_{1 − x} alloys (x = 1, 0.85, 0.67, 0.50, 0.20 and 0) has been measured. Mono-crystalline Si_xGe_1−x layers Were implanted with 1.50–2.75 MeV Si²⁺ and Ge²⁺ ions to produce the amorphous material. Using surface profilometry and RBS/channeling, it was found that amorphous alloys are less dense than the crystalline alloys, and that Vegard's law underestimates the a-Si_xGe_1−x density.     

Thermodynamic studies on Cs4U5O17(s) and Cs2U2O7(s) by emf and calorimetric measurements

The oxygen potentials over the phase field: Cs₄U₅O₁₇(s)+Cs₂U₂O₇(s)+Cs₂U₄O₁₂(s) was determined by measuring the emf values between 1048 and 1206 K using a solid oxide electrolyte galvanic cell. The oxygen potential existing over the phase field for a given temperature can be represented by: Δμ(O₂) (kJ/mol) (±0.5)=−272.0+0.207T (K). The differential thermal analysis showed that Cs₄U₅O₁₇(s) is stable in air up to 1273 K. The molar Gibbs energy formation of Cs₄U₅O₁₇(s) was calculated from the above oxygen potentials and can be given by, Δ_fG⁰ (kJ/mol)±6=−7729+1.681T (K). The enthalpy measurements on Cs₄U₅O₁₇(s) and Cs₂U₂O₇(s) were carried out from 368.3 to 905 K and 430 to 852 K respectively, using a high temperature Calvet calorimeter. The enthalpy increments, (H⁰_T−H⁰₂₉₈), in J/mol for Cs₄U₅O₁₇(s) and Cs₂U₂O₇(s) can be represented by, H⁰_T−H⁰_298.15 (Cs₄U₅O₁₇) kJ/mol±0.9=−188.221+0.518T (K)+0.433×10⁻³T² (K)−2.052×10⁻⁵T³ (K) (368 to 905 K) and H⁰_T−H⁰_298.15 (Cs₂U₂O₇) kJ/mol±0.5=−164.210+0.390T (K)+0.104×10⁻⁴T² (K)+0.140×10⁵(1/T (K)) (411 to 860 K). The thermal properties of Cs₄U₅O₁₇(s) and Cs₂U₂O₇(s) were derived from the experimental values. The enthalpy of formation of (Cs₄U₅O₁₇, s) at 298.15 K was calculated by the second law method and is: Δ_fH⁰_298.15=−7645.0±4.2 kJ/mol.     

Chemical thermodynamic representation of AmO2−x

The AmO_2−x solid solution data set for the dependence of the oxygen potential on the composition, x, and temperature was retrieved from the literature and represented by a thermodynamic model. The data set was analysed by least-squares using equations derived from the classical thermodynamic theory for the solid solution of a solute in a solvent. Two representations of the AmO_2−x data were used, namely the Am_5/4O₂–AmO₂ and AmO_3/2–AmO₂ solid solution. No significant difference was found between the two, and the Am_5/4O₂–AmO₂ solution was preferred on the basis of the phase diagram. From the results the Gibbs energy of formation of Am_5/4O₂ has been derived.     

Sputtering yield of Ti1−xBx films by 2 keV deuterium bombardment

We deposited titanium borides (Ti_1−xB_x; 0.40 < x < 0.77) by the co-sputter coating method and measured their sputtering yield by 2 keV deuterium ion bombardment as a function of their chemical composition at room temperature. The total sputtering yield is found to increase with increase of the boron content in Ti_1−xB_x. The total sputtering yield of stoichiometric TiB₂ is estimated to be 2.8 × 10⁻², about the same as those reported previously. Concerning the partial sputtering yield, that of the titanium does not depend on the chemical composition, but that of the boron increases with increase of the boron content. These experimental results could be explained by assuming that the partial sputtering yield is proportional to the spatial concentration of each atom in the Ti_1−xB_x matrix.     

Thermal stability and brazing characteristics of Zr0.7−xMxBe0.3 (M=Ti or Nb) ternary amorphous filler metals

The effects of Ti or Nb substitution on the thermal stability and brazing characteristics of Zr_0.7−xM_xBe_0.3 (M=Ti or Nb) ternary amorphous alloys were investigated in order to improve properties of Zr–Be binary amorphous alloy as a new filler metal for joining zirconium alloy. The Zr_0.7−xM_xBe_0.3 (M=Ti or Nb; 0x0.1) ternary amorphous alloys were produced by melt-spinning method. In the selected compositional range, the thermal stability of Zr_0.7−xTi_xBe_0.3 and Zr_0.7−xNb_xBe_0.3 amorphous alloys are improved by the substitution of titanium or niobium for zirconium. As the Ti and Nb content increases, the crystallization temperatures increase from 610°C to 717°C and 610°C to 678°C, respectively. These amorphous alloys were put into practical use in joining bearing pads on zircaloy cladding sheath. Using Zr–Ti–Be amorphous alloys as filler metals, smooth interface and spherical primary particles (proeutectic phase) appear in the brazed layer, which is the similar microstructure of using Zr_0.7Be_0.3 binary amorphous alloys. In the case of Zr–Nb–Be amorphous alloys, Ni-precipitated Zr phase that may cause some degradation in ductility and corrosion-resistance is formed at both sides of the brazed layer.     

Ion beam synthesis and recrystallization of amorphous SiGe/SiC structures

Si_1−xGe_x amorphous layers implanted with different doses of carbon (between 5 × 10¹⁵ and 2 × 10¹⁷ cm⁻² and annealed at 700°C and 900°C have been analyzed by Raman and Infrared spectroscopies, electron microscopy and Auger electron spectroscopy. The obtained data show the synthesis of amorphous SiC by implanting at the highest doses. In these cases, recrystallization only occurs at the highest annealing temperature (900°C). The structure of the synthesized SiC strongly depends on the implantation dose, in addition to the anneal temperature. For the highest dose (2 × 10¹⁷ cm⁻²), crystalline β-SiC is formed. Finally, a strong migration of Ge towards the Si substrate is observed from the region where SiC precipitation occurs.     

Diffusion and strain relaxation in Si/Si1−xGex/Si structures studied with Rutherford backscattering spectrometry

The thermal stability of strained Si/Si_1−xGe_x/Si structures grown by molecular beam epitaxy was investigated by resistive heating and in situ Rutherford backscattering spectrometry. Ge profiles obtained from a 50 nm Si_1−xGe_x layer on a Si(100) substrate capped with 50 nm Si were evaluated for different Ge concentrations after sequential heating periods at a particular temperature between 850 and 1010° C. The diffusion coefficients, calculated from the increase in signal in the tail of the Ge profile, proved to be comparable to the value for Ge in bulk Si. A more pronounced decrease of the signal at the center of the Ge profile indicated a faster diffusion within the SiGe layer which was confirmed by analysis of the FWHM of the Ge profile. Ion channeling measurements were used to characterize tetragonal strain in the buried SiGe layers. Angular scans through the 111 direction were interpreted with Monte Carlo channeling calculations and used to study strain relaxation in dislocation-free and partially relaxed layers.     

Characterization of Si/GexSi1 − x heterojunction bipolar transistors formed by Ge ion implantation in Si

Epitaxial Si/Ge_xSi_{1 − x} heterojunctions were formed by high dose Ge ion implantation in Si followed by rapid thermal annealing at 1000°C for 10 s. This technique was adopted to fabricate Si/Ge_xSi_{1 − x} heterojunction n-p-n bipolar transistors (HBT) using a self-aligned, double polycrystalline silicon process commonly used for fast Si bipolar transistors. The devices are characterized by a 60 nm wide neutral base with a Ge concentration peak of ≈ 7 at.% at the base-collector junction. Good static and dynamic electrical characteristics are demonstrated and discussed.     

Electrical and optical properties of Co ion implanted a-Si1 − xCx:H alloys

Low resistivity a-Si_1 − xC_x:H alloy films have been formed by high dose Co⁺ ion implantation. The influence of the carbon content of the films on the resistivity has been studied and the lowest values, of the order of 10 Ω/Sq, have been observed for the carbon free films. Even lower resistivities, a further reduction of up to 50%, have resulted from annealing at temperatures up to 500°C. Changes in the optical and structural properties of the implanted a-Si_1 − xC_x:H films have been studied by means of IR and Raman spectroscopy. Results show that the implantation produces considerable structural and chemical modifications. The formation of, and the transition to, a possible CoSi₂ phase has been observed by examining the IR and Raman spectra as a function of implant dose.     

Radiation damage effects in CMR manganite materials

Polycrystalline La_0.5Pb_0.5Mn_1−xCr_xO₃ (x = 0.075 and 0.15) samples have been irradiated with 50 MeV Li³⁺ ions with different fluences and the effects on the transport properties have been studied by means of the temperature and magnetic field dependent resistivity measurements. Due to Li³⁺ ion irradiation, the resistivity increases and the metal–insulator transition temperature (T_mi) decreases. At low temperatures (below T_mi), a dominant contribution of the electron–magnon scattering process is observed for all the irradiated and unirradiated samples. The low temperature resistivity behavior as well as the magnetoresistance is modified due to irradiation. The changes in the magnetotransport properties due to irradiation have been compared with the changes caused due to Mn site substitution.     

Thermodynamic stability of Na2ZrO3 using the solid electrolyte galvanic cell technique

The sodium potential in the test electrode (a) Pt,O₂,Na₂ZrO₃,ZrO₂ was measured by using the emf technique employing Na-β^″-alumina as the solid electrolyte in conjunction with (b) Pt,O₂,Al₂O₃,NaAl₁₁O₁₇, (c) Pt,O₂,Na₂MoO₄,Na₂Mo₂O₇ and (d) Pt,Na₂CO₃,CO₂,O₂ as the reference electrodes over the ranges 880–1045, 700–800 and 850–940 K, respectively. The emf results between electrodes (b) and (c) were utilized for internal consistency checks. From the results on cells formed between (a) and (b) and those on (a) and (c), the standard Gibbs energy of formation, Δ_fG^o (kJ/mol) of Na₂ZrO₃ was determined to be −1699.4+0.3652T (K) valid over the temperature range 700–1045 K. The break in the emf data at 1045 K was corroborated by independent TG/DTA measurements carried out on Na₂ZrO₃ which exhibited an endotherm at 1055 K indicative of a phase transition in Na₂ZrO₃.     

Li4SiO4 pebbles reduction in He + 0.1% H2 purge gas and effects on tritium release properties

Lithium orthosilicate reduction was examined by Temperature Programmed Reaction (TPR) and Temperature Programmed Desorption (TPD) methods performed in He (or Ar) + H₂ purge gas flowing through pebble bed specimens. The parameters governing the kinetics and the steady-state of the reduction process to Li₄SiO_4−x were determined at 800°C. The level x of the O-vacancy concentration at steady-state (of the order of 1.5×10⁻³ mole fraction) was found to be compatible with the impurities content in the specimens. Pebble pre-annealing treatments were found to affect the microstructure and the reduction mechanism. Post-irradiation tritium release by TPD tests were performed on both stoichiometric and reduced pebbles with similar results. Tritium release properties of this breeder system seem to be independent from the material reduction state (x).     

Phase transitions in U3O8−z: I, heat capacity measurements

The heat capacity of U₃O_8−z with various O/U ratios was measured in the range from 250 to 750 K, and λ-type heat capacity anomalies were found in each sample. The transition temperatures were 487 and 573 K for UO_2.663, 490 and 576 K for UO_2.656 and 508, 562 and 618 K for UO_2.640. The entropy changes of the transitions were 0.44 and 0.39 J K⁻¹mol⁻¹ for UO_2.663, 0.58 and 0.47 J K⁻¹mol⁻¹ for UO_2.656 and 0.62, 0.51 and 0.25 J K⁻¹mol⁻¹ for UO_2.640, increasing as O/U decreases. The enthalpy change due to the transition varied linearly with the transition temperature except for UO_2.640, showing the presence of the same mechanism of phase transition among the samples with various O/U ratios. The mechanism of the phase transition was discussed on the assumption that the transition is originated from the order-disorder rearrangement of U⁵⁺ and U⁶⁺ with a consequent displacement of atoms, similarly to the case of U₄O_9−y.     

Interesting aspects of the analysis of resistivity in Li irradiated Bi-2212

Differently heat treated and 55 MeV Li³⁺ beam irradiated Bi₂Sr₂Ca₁Cu₂O_8+δ (Bi-2212) high temperature superconductors have been studied from the analysis of resistivity in the normal state as well as near the superconducting transition. For all the unirradiated and irradiated samples the so-called linear temperature dependence of the normal state resistivity, in a wide temperature range, can well be understood within the variable range hopping (VRH) conduction scenario. Near and above the bulk superconducting transition, the fluctuation enhanced conductivity (paraconductivity) analysis shows a noteworthy modification of the conduction process due to radiation induced defects.