Synthesis and characterization of the Aurivillius phases Bi2 − xPbxSr1 − xNdxNb2O9

The n = 2 Aurivillius phase Bi_{2 − x}Pb_xSr_{1 − x}Nd₂O₉ was successfully synthesized as a ceramic material over the whole range of simultaneous, charge compensated substitution x = 0–1.0. Structural investigations were performed by Rietveld refinement applying different space groups Fmmm and A2₁am, and additionally by X-ray absorption spectroscopy (EXAFS) on the Nd L_III-edge, confirming the accommodation of Nd on the atomic sites of Sr, which implies the substitution of Bi³⁺ by the isoelectronic Pb²⁺. The ferroelectric transition temperature T_c = 270 °C of the substituted powders with x = 0.4 and 1.0 is distinctly reduced compared to the unsubstituted sample with T_c = 450 °C. In temperature resolved powder X-ray diffraction patterns no structural phase transition could be detected.     

Silver ionic conductivity enhancement by network former mixed in oxide-based glasses

Glasses in the binary system xAg₂P₂O₆ − (1 − x)Ag₂Te₂O₅ have been prepared for 0 x 1. For each composition only one glass transition temperature is observed in the temperature range of 180–220 °C. All glasses appear homogeneous considering their optical and electrical properties. Nevertheless, in SEM observations, some glass compositions appear to be heterogeneous after decoration following short nitric acid etching. For each composition, conductivity data obtained in the temperature range of 25–200 °C using impedance techniques obey an Arrhenius relationship with a composition independent pre-exponential term. Variation of the conductivity activation energy with x induces correlative variations of isothermal conductivity curves leading to an increase of the ionic conductivity of about one order of magnitude compared with linearity at 25 °C. This behaviour is discussed with respect to the thermodynamic properties of the glassy solutions.     

Measurement of the acoustic properties of a nerve-muscle preparation as a function of physiologic state

Nerve-muscle preparations of Sprague Dawley rats were exposed to low dosage ultrasound. The objectives were to measure the velocity of propagation and attenuation of ultrasonic energy in both the relaxed and contracted states. A tension-measuring system and associated ultrasonic instrumentation were designed to measure the tension developed in stimulated muscle and its corresponding acoustic parameters, ie the attenuation coefficient, (db cm^-1) and the velocity of propagation, c (ms^-1). Each test was performed at ultrasonic frequencies 3.1, 5.35, and 7.68 MHz and with the preparation maintained at 23 ± 0.5° C. Attenuation of ultrasonic energy was observed to increase by 10 ± 0.5% in the active state from its value in the relaxed state. The relation between the attenuation and the acoustic frequency was found to be approximately linear over the frequency range tested. The velocity of propagation in the active state did not change appreciably from its value in the relaxed state and was observed to be independent of the acoustic frequency in the range used.     

Concerning infrared-stimulated luminescence from K-feldspars: evidence from heating before stimulating

Repeated heating and stimulation by infrared of feldspar samples causes a reduction in the luminescence signal. Two feldspars were investigated, one microcline and one orthoclase. Empirically the fraction of luminescence signal f(n) remaining after the nth cycle of heating and stimulation is given by f(n)=1−a ln(n) for laboratory dosed samples of both microcline and orthoclase feldspars, for heating temperatures of 150°C, 180°C and 220°C, for heating durations per cycle ranging from 20 s to 2400 s and with the study covering 10 cycles of heating and stimulation. Logarithmic decay of luminescence with time has been explained previously, in other contexts, as due either to quantum tunnelling or to a continuous distribution of states being involved but it is shown that these explanations do not fit the present data. The measured data on f(n) were corrected for the loss of luminescence due to infrared stimulation to ensure that this did not account for the differences between the data and the expectations from models; the functional form f(n)=1−a ln(n) remains valid, although with changed values of a. Numerical simulations of systems involving a limited number of trap depths, from 21 down to 3, were investigated and those with 5 or more trap depths were found to be capable of resembling the data. The simulations could not define a unique pattern of trap depths to match the data, but of the patterns investigated the data were best reproduced by a distribution of at least 5 traps in the energy range from 1.18–1.66 eV. These conclusions augment, and are consistent with, existing information on luminescence mechanisms in potassium-feldspars.     

Magnetic properties of Sm–Co–B-based nanocomposite magnets

The magnetic properties of nanocomposite melt-spun magnets with composition Sm_16−xCo_68+xB₁₆ (x=0–10, 2 at% interval) and Sm₈Co_92−yB_y (y=10–18, 2 at% interval) have been studied systematically. Several ribbons were fabricated with a wheel speed of 50 m/s, followed by annealing in the temperature range of 700–800°C for 2.5–40 min. XRD results and magnetization versus temperature curves showed that almost all of the samples were composed of the tetragonal Sm₂Co₁₄B and rhombohedral SmCo₁₂B₆ phases which are not magnetically hard at room temperature. However, a relatively high coercivity in the range of 3.5–5.5 kOe has been obtained in these samples. The highest coercivity of 5.5 kOe and a very promising β value of −0.28%/°C were obtained in Sm₈Co₇₄B₁₈ ribbons annealed at 750°C for 5 min. The high coercivities are attributed to the small grain size of the 2 : 14 : 1 phase, in which the large surface areas enhance its effective anisotropy, and make it uniaxial type.     

Effects of substitution of Ti for Fe in BiFeO3 films prepared by sol–gel process

Ti substituted BiFe_1−xTi_xO_3+δ films have been prepared on indium–tin oxide (ITO)/glass substrates by the sol–gel process. The films with x=0.00–0.20 were prepared at an annealing temperature of 600 °C. X-ray diffraction patterns indicate that all films adopt R3m structure and the films with x=0 and 0.10 show pure perovskite phase. Cross-section scanning shows the thickness of the films is about 300 nm. Through 0.05 Ti substitution, the 2P_r increases to 8.30 μC/cm² from 2.12 μC/cm² of the un-substituted BiFeO₃ film and show enhanced ferroelectricity at room temperature. The 2P_r values are 2.63 and 0.44 μC/cm² for the films with x=0.01 and 0.2, respectively. Moreover, the films with x=0.05 and 0.10 show enhanced dielectric property since the permittivity increases near 150 at the same measuring frequency. Through the substitution of Ti, the leakage conduction is reduced for the films with x=0.05–0.20.     

Accurate measurement of the refractive index of CO2, N2, He, O2, and air at 10.57 μ and T = 23 °C

The refractive index of carbon-dioxide, nitrogen, helium, oxygen and air have been measured at 23 °C temperature by means of a tunable CO₂ laser at 10.57 μm and of a differential interferometric technique. As the gas refractive index depends on the pressure P as n = 1 + _PP, the pressure coefficients _P has been measured with 5e–3 accuracy.     

Density, ultrasonic velocity, surface tension, excess volume and viscosity of quaternary fluid solutions

Density, ultrasonic velocity, surface tension, excess volume and viscosity of quaternary non-electrolyte solution n-pentane+tolune+n-heptane+cyclohexane has been experimentally determined at 25 °C over a wide range of composition. Assuming a quaternary fluid solution to be made of six binaries, a statistical approach of Prigogine–Flory–Patterson (PFP) theory has been extended to develop the expressions for dynamic viscosity, surface tension excess volume and ultrasonic velocity of quaternary fluid system. A reasonable agreement has been achieved between theory and experiment. An attempt has also bee made to explain the nature of molecular interactions involved in the light of excess thermodynamic functions whose sign and magnitude depend upon the chain length and size of the component fluids and also studied the role of order breakers (toluene and cyclohexane) on these properties.     

超声衰减和速度谱测量亚微米乳液的粒径

研究了超声衰减谱法和相速度测量高浓度多分散脂肪两相乳浊液的粒径分布问题.在理论分析基础上,实验测量了多个浓度(2%～20%)脂肪乳试样在2～13 MHz频带下超声衰减和相速度谱,结合反演算法由实验数据计算出乳浊液颗粒的粒径分布,并讨论了相速度法的意义和特点.将原始浓度(20%)下测得粒径分布与消光法在稀释条件下相同试样测量结果作对比,二者比较吻合,表明超声谱法可在无稀释的高浓度条件下作乳浊液粒径分布的表征.     

Structural and optical properties of thermally evaporated Bi2Te3 films

Bi₂Te₃ films were prepared by thermal evaporation technique. X-ray diffraction analysis for as-deposited and annealed films in vacuum at 150 °C were polycrystalline with rhombohedral structure. The crystallite size is found to increase as the film thickness increases and has values in the range 67–162 nm. The optical constants (the refractive index, n, and absorption index, k) were determined using transmittance and reflectance data in the spectral range 2.5–10 μm for Bi₂Te₃ films with different thicknesses (25–99.5 nm). Both n and k are independent on the film thickness in the investigated range. It was also found that Bi₂Te₃ is a high refractive index material (n has values of 4.7–8.8 in the wavelength range 2.5–10 μm). The allowed optical transitions were found to be direct optical transitions with energy gap  eV. The optical conductivities σ₁ = ƒ(hν) and σ₂ = f(hν) show distinct peaks at about 0.13 and 0.3 eV, respectively. These two peaks can be attributed to optical interband transitions.     

Oxygen tracer diffusion in La1 − xSrxCoO3

Tracer diffusion of ¹⁸O in dense, polycrystalline La_1−xSr_xCoO₃ for x = 0.1 has been measured in the temperature range 400 to 600 °C and at 500 °C for x = 0.2 at an oxygen partial pressure of 1 × 10⁵ Pa. Depth profiles were obtained by secondary ion mass spectrometry. The diffusion coefficient for La_0.9Sr_0.1CoO₃ is given by D = (17–247) exp[(−232 ± 8 kJ/mole)/RT] cm²/s. This value is several orders of magnitude lower than D extrapolated from the results for x = 0.2 measured in the 700–900 °C temperature range. One possible explanation for the discrepancy is that the two measurements reflect different diffusion paths. As expected, La_0.8Sr_0.2CoO₃ exhibits a higher diffusivity at 500 °C than does La_0.9Sr_0.1CoO₃.     

Oxygen nonstoichiometry and phase transitions of the neodymium-rich Nd1+xBa2−xCu3Oz solid solution

On the basis of chemical, thermal analysis and Cu K-edge X-ray absorption measurements, oxygen content in the Nd_1+xBa_2−xCu₃O_z solid solution was determined between 1000°C in air and 400°C in oxygen for x=0.05–0.9 compositions. It has been observed that the oxygen nonstoichiometry Δz of the Nd_1+xBa_2−xCu₃O_7+x/2−Δz solid solution decreases 2–2.5 times for a large substitution (Δz≈0.3–0.33 for x=0.9), despite of the acclaimed higher total oxygen content. The difference in nonstoichiometry is explained by a higher average value of the copper oxidation state (ACV), which is vital for the solid solution with large x even at elevated temperatures (ACV≈2–2.05 for x>0.3 at 1000°C, PO₂=0.21 atm). On the contrary, the ACV after complete oxygenation is almost constant (about 2.25–2.3) for the whole series. The x-dependence of the oxygen content is not monotonous and structural phase transitions can be observed at x=0.3 and x=0.6, as confirmed by the X-ray diffraction and the Raman scattering spectroscopy. The first well-known transition is connected with the oxygen disorder due to the Nd substitution for Ba at random Ba-sites. In the present work, it is proved by the apical oxygen mode broadening in Raman spectra. Ordering of the Nd and Ba atoms with a subsequent orthorhombic distortion of the lattice may occur even at 1000°C in air due to the second transformation at x≈0.6. The invariable orthorhombicity of the Nd-rich solid solution with x>0.6 is not caused by the oxygen absorption as in the x=0.05 case. Existence of high- and low-temperature orthorhombic modifications of this solid solution has been observed for the first time. Finally, a tentative 3D (z–x–T) diagram is suggested for the Nd_1+xBa_2−xCu₃O_z solid solution up to 1000°C in air, including the new x=0.6–0.9 region.     

A new surface phase in liquid normal-alkanes

A new surface phase is found in liquid normal-alkanes. X-ray and surface tension measurements show the formation of a crystalline monolayer on the surface of the liquid at temperatures up to 3°C above the bulk solidification temperature, T_f. The molecules in the monolayer are hexagonally packed and oriented normal to the surface. A single solid monolayer persists down to T_f, thus exhibiting a very limited partial wetting. The new surface phase is obtained only for chain lengths 14<n50. Its vanishing for n14 is interpreted as a possible transition from surface freezing to surface melting behaviour. The measurements are satisfactory accounted for within a simple theory based on surface energy cosiderations.     

Enhanced magnetic properties of Nd–Fe–B thin films crystallized by heat treatment

Nd₂Fe₁₄B Φ phase crystallites were formed in Nd_16.7Fe_65.5B_17.8 thin films prepared by RF sputtering with subsequent heat treatment. The 2 μm-thick films were deposited onto 0.1 mm Mo sheets at an average substrate temperature (T_s) of 365°C. The enhanced magnetic properties of the magnetically anisotropic thin films were investigated using different heating rates (h_r) of 10°C, 20°C, 50°C and 100°C/min in an annealing experiment. Transformation from the amorphous phase to the crystalline phase is clearly manifested by the formation of fine crystallites embedded as a columnar matrix of Nd₂Fe₁₄B phase. High-resolution scanning electron microscope data of the cross-section of the annealed films show columnar stacking of Nd₂Fe₁₄B crystallites with sizes <500 nm. Transmission electron microscope observations revealed that the microstructure of these films having out-of-plane magnetization consists of uniformly distributed Φ phase with grain size around 400 nm together with small Nd rich particles. This grain size of Φ phase is comparable to the single domain particle diameter of Nd₂Fe₁₄B. Significant change in _iH_c, 4πM_r and 4πM_s with h_r was confirmed. Annealing conditions with a heating rate of 50°C/min to an annealing temperature (T_a) of 650°C for 30 min was consequently found to give optimum properties for the NdFeB thin films. The resulting magnetic properties, considered to be the effect of varying h_r were _iH_c= 1307–1357 kA/m, 4πM_r=0.78–1.06 T and 4πM_s=0.81–1.07 T.     

Thermal expansion of solid CH4 and CD4

The linear expansion coefficients of solid light methane CH₄ and deuteromethane CD₄ have been denned in the temperature range 10°–24°K and 6°–58°K, respectively. The question about the nature of rotational motion of molecules in CH₄ and CD₄ crystals and about the existence of low temperature phase transition in solid methane is discussed.     

Oxygen nonstoichiometry and electrical conductivity of the solid solutions La2−xSrxNiOy (0≤x≤0.5)

Oxygen nonstoichiometry and electrical resistance of a series La_2−xSr_xNiO_y solid solutions, where x=0.0, 0.2 and 0.5 in argon flows at oxygen partial pressures 1.5, 10.2, 49.2, 100 and 286 Pa within the temperature range of 20–1050°C were studied. Nickelate oxygen desorption/sorption spectra when heating–cooling at constant rate demonstrated strong dependence of cation composition of the samples. Unlike La_1.5Sr_0.5NiO_y compounds those of La₂NiO_y and La_1.8Sr_0.2NiO_y have weakly bonded oxygen, capable to exchange reversibly with the gas phase at the temperatures higher than 250°C. The equilibrium values of oxygen nonstoichiometry and specific resistance for the these nickelates were determined at 300–1050°C and p_O2=1.5–286 Pa as a functions of temperature versus oxygen partial pressure. All nickelate studied appear to be p-type conductors with metal electric conductivity at equilibrium states.     

Entropy of planar random surfaces on the lattice

We study planar random surfaces on a hypercubic lattice in two and three dimensions by Monte Carlo techniques. Our data are consistent with the formula n₀(A;C) A^b₀A, where n₀(A;C) is the number of planar random surfaces with area A and boundary C. We find b₀ = −1.4 ± 0.2, = 5.31 ± 0.03 (for d = 2) and b₀ = −1.5 ± 0.2, = 7.13 ± 0.05 (for d = 3). The values of b₀ disagree with those obtained from the Polyakov string model.     

On the dielectric loss and thermal bleaching of calcite irradiated by X-rays

The changes produced by X-ray irradiation in the dielectric and optical properties of calcite crystals are reported. At ordinary temperatures, the dielectric constant as well as the dielectric loss of the uncoloured crystal remains practically unchanged in the frequency region of 10 kc/s-15 Mc/s. It has been found that the temperature variation of its dielectric loss can be represented by an equation tan where A and B are constants; this is attributed to the movement of vacancies in the crystal.

On irradiation by X-rays, calcite exhibits pronounced optical absorption in the ultraviolet region beyond 400 mμ; the dielectric loss of calcite also increases considerably on colouration. The thermoluminescence shows a very strong glow peak at 85°C with minor ones at higher temperatures. During thermal bleaching, the dielectric loss of the coloured crystal shows a prominent maximum in the temperature range 70–120°C and beyond 230°C, it varies in the same way as in the case of the uncoloured crystal. The correspondence between the change in dielectric loss and the first glow peak is possibly due to thermal release of trapped electrons. The optical absorption disappears when the crystal is heated to 350°C and on cooling to room temperature, its dielectric loss returns to its original value before colouration.     

Excess molar heat capacity of isobutyric acid–water binary liquid mixtures near and far away from the critical temperature

The heat capacity of the liquid–liquid mixture isobutyric acid–water has been measured for the first time near and far away from its critical point using an adiabatic calorimeter. The measurements were performed at atmospheric pressure, in the one phase region as a function of three temperatures: (1) T − T_C = 0.055 °C, (2) T − T_C = 3.055 °C, (3) T − T_C = 8.055 °C and of the composition X in acid (IA). The heat capacity C_p decreases rapidly when X increases at the used temperatures. Near the critical composition, C_p is not affected by the correlation of the concentration fluctuations.

The molar excess heat capacity of the system under investigation was analysed along the phase diagram and considered as a structural transformation effect.     

Trajectory-property relationships in MOD-derived YBCO films

A study of the physical and chemical changes during processing in MOD-derived YBCO films was performed. Fully processed films were 70–85% of theoretical density. The sintering rate increased substantially in the compositional range F/Ba = 1.8–1.5. The activation energy for sintering decreased above a P(H₂O) dependent threshold temperature. XRD indicated this temperature/composition threshold also corresponded to YBCO nucleation, suggesting ex situ YBCO forms in contact with a melt. The ramp rate and P(H₂O) were used to control F/Ba trajectories, which were correlated to performance. The nucleation of YBCO was strongly dependent on processing conditions. Nucleation temperature was varied by at least 60 °C in the study. The optimal YBCO nucleation temperature in the 300–800 nm films was around 725 °C. a-axis grains dominated the microstructures of films where YBCO nucleated at <700 °C. Large second phases, but no a-axis grains, were found when the nucleation temperature was >750 °C.