Formation and characterization of oxynitride glasses in the Si-Ca-Al-O-N and Si-Ca-Al,B-O-N systems

Oxynitride compositions in the Si-Ca-Al-O-N and Si-Ca-Al, B-O-N systems were melted and furnace-cooled in BN crucibles at temperatures from 1650 to 1850° C under dry nitrogen atmosphereS. Glass formation, phase stability and crystallization were studied by characterizing the cooled melts by X-ray diffraction, DTA, and electron microscopy. Oxynitride batches with nitrogen content up to 11 at % formed glasses in the Si-Ca-Al-O-N system. Glasses in the Si-Ca-Al, B-O-N system could be formed only when the B₂O₃ content of the batch was less than 3 wt %. Oxynitride glasses in these boron-containing systems were characteristically inhomogeneous, difficult to process, and prone to crystallization. In both the systems, glasses exhibited glass transitions beginning at 1000° C and crystallization at 1300 to 1500° C. Nitrogen-containing crystalline phases were identified in devitrified glasses via microstructural and micro-mechanical analyses.     

Synthesis of a nanophase,whisker-reinforced,ceramic/metal composite by electrochemical infiltration

A novel, nanophase metal-matrix composite sheet material has been synthesized. Nickel was infiltrated by electrodeposition into a wool-like mat of SiC whiskers that had been grown by chemical vapour deposition. Infiltration of nickel by d.c. plating, pulse plating, and the effects of a tin-palladium surface treatment of the SiC whiskers were evaluated. Pulse plating combined with the Sn-Pd treatment were effective in minimizing porosity. Compared to values for the unreinforced electrodeposited nickel, the hardness could be almost quadrupled and the wear rate decreased to approximately one sixth in a composite with 30 vol % whiskers.     

Mechanical and Corrosion Characteristics of Zr + 2.5% Nb Zirconium Reactor Alloy

The results of structural and phase hardening of pipes made of Zr + 2.5% Nb alloy show that ultrahigh-frequency thermal treatment of pipes (fast heating to the temperature of existence of the -phase followed by sharp cooling and annealing in the high-temperature range of the -phase) destroys the texture and forms a fine-grained structure (the grain diameter is about 1 m) with numerous transitional twins and a high density of precipitations of the secondary -niobium phase ( 10¹⁶cm^–3). In this state, the alloy is rather strong and plastic (at room temperature, _u 650 MPa, _0.2 550 MPa, and 20% both in the longitudinal and transverse directions). The efficiency of hardening by ultrahigh-frequency thermal treatment is not reduced with increase in the temperature of testing up to 500°C. Corrosion tests of channel pipes made of Zr + 2.5% Nb alloy subjected to ultrahigh-frequency thermal treatment in water containing various amounts of oxygen (from 0.1–0.3 to 600 mg/kg) at temperatures of 285–350°C for 700–6600 h under static conditions and in reactor water of the Ignalina Nuclear Power Plant for 5000 h under dynamic conditions showed that the corrosion resistance of this alloy is on a par with the corrosion resistance of the material of assembly channels of high-power channel reactors subjected to a standard treatment.     

Self-assembled germanium islands grown on (0 0 1) silicon substrates by low-pressure chemical vapor deposition

The time evolution of self-assembled Ge islands, during low-pressure chemical vapor deposition (LPCVD) of Ge on Si at 650 °C using high growth rates, has been investigated by atomic force microscopy, transmission electron microscopy, and Rutherford backscattering spectrometry. We have found three different island structures. The smallest islands are lens-shaped and characterized by a rather narrow size distribution, 4 nm high and 20 nm wide. Next to form are a distinct population of larger multifaceted dome-shaped islands, up to 25 nm high and 80–150 nm wide. Finally, the largest islands that form are square-based truncated pyramids with a very narrow size distribution, 50 nm high and 250 nm wide. The pyramidal islands normally seen in the intermediate size range (150 nm) are not observed. The small lens-shaped islands appear to be defect free, while some of the multifaceted islands as well as all the large truncated pyramids contain misfit dislocations. The existence of multifaceted islands, in the size range where pyramids have previously been reported and of truncated pyramids in the size range where multifaceted dome-shaped islands have previously been reported, is attributed to the high growth rate used. Furthermore, under the growth conditions used, the truncated-pyramid-shaped islands are characterized by a very narrow size distribution.     

The structure of a cast dental Ni-Cr-Be alloy

The structure of a typical dental Ni-Cr-Be alloy with 1.8 wt% Be has been investigated by SEM and TEM as well as by quantitative X-ray microanalyses in both instruments. Due to its low atomic weight the atomic fraction of Be is as high as 0.10. During solidification beryllium segregates substantially, and a large volume fraction of the casting is made up of a eutectic with coarse ( 1 µm diameter) alternating rods of fcc Ni-Cr and NiBe with a CsCl-type structure (ordered bcc). Smaller ( 0.1 µm diameter) rods of NiBe are precipitated in matrix in the solid state. Microanalyses of the NiBe rods show that they have a low chromium content ( 1.5 wt%). The cube boundary planes of the ordered b cc and fcc structures have a slight difference in orientation of about 7° which is most probably due to a small coherency misfit of the two types of lattices. The 100 directions in cube boundary plane of the fcc structure are nearly parallel to the 110 directions of the ordered bcc cube boundary plane. Sometimes another and more complex relationship between the two lattices occurs. The alloy contains 3.9 wt% Al which gives rise to numerous small ( 10 nm), spherical, ordered particles of Ni₃Al both in matrix as well as in the fcc eutectic rods.     

Directional dependence of c-plane slip in single crystals of mercuric iodide

An experimental study of plastic deformation in thin single crystals of mercuric iodide (Hgl₂) subjected to (0 0 1) [1 0 0] and (0 0 1) [1 1 0] shear loadings has established a directional dependence to the phenomenon of (0 0 1) orc-plane slip in Hgl₂. The average stressess _c for the onset of yielding were 12.6 psi (86.9 kPa) for (0 0 1) [1 0 0] shear and 16.5 psi (113.8 kPa) for (0 0 1) [1 1 0] shear; the average values of the deformation parameters ₀, interpreted as a bulk yield stress, were 24.7 psi (170.3 kPa) for (0 0 1) [1 0 0] shear and 37.7 psi (259.9 kPa) for (0 0 1) [1 1 0] shear. These values are in agreement with the theoretical relationss _c()=s _c(0)/cos ands ₀()=s ₀(0)/cos, where is the smallest angle between 1 0 0 crystallographic axis and the direction of shear stress applied in the (0 0 1) plane.     

Structure and Magnetism of the Composite Crystal Ca0.824CuO2

We have studied the magnetic state from a viewpoint of crystallographic features of the 1-D chain compound Ca_0.824CuO₂. A possible spin-hole arrangement in the magnetically coexisting state was determined by analyzing the local structural distortion in the CuO₂ chain by means of a modulated-crystal-structure analysis. The essential periodic sequence expected is (: up- and down-spin, : hole), which can be regarded as a kind of spin-1/2 ferromagnetic-antiferromagnetic alternating Heisenberg chain.     

Single-crystal growth and characterization of Cu2O and CuO

We have prepared a large number of crystals of cuprous oxide (Cu2O) by various procedures. Photoluminescence spectra of these crystals were studied to examine the concentration of defects, especially copper vacancy VCu to seek favourable conditions for growing Cu2O crystal. High-quality single crystals of Cu2O were prepared by the floating-zone melting method in air. Several synthetic crystals (specimens FA, FZ and GZ) and also a natural crystal were studied by X-ray analysis, inductively coupled plasma spectroscopy analysis, optical absorption, photoluminescence, photoconductivity and cyclotron resonance absorption, photoluminescence, photoconductivity and cyclotron resonance absorption to characterize their optical and electrical qualities. The best values of mobility and scattering time of photocarriers at T = 4.2 K are estimated to be h1.8 × 105 cm2 V–1 s–1 and h60 ps for positive holes, and 1.3 × 105 cm2 V–1 s–1 and 70 ps for electrons in Cu2O. Further, we report preliminary experimental results on transport property of crystals also of cupric oxide (CuO) purified by the floating-zone melting method.     

Complexities in STEM analyses of polymer blend thin films

Polystyrene (PS)-polyether sulphone (PES) polymer blend thin films were prepared for examination in a scanning transmission electron microscope. The microstructures observed in 75 wt % PS-25 wt % PES films consisted of spherical inclusions, ranging from 0.2 to 1.2m in diameter. X-ray spectrometric analysis in the microscope revealed that the inclusions were PES-rich, while the matrix contained only PS. Attention in this paper is paid to the contrast in the annular dark-field detector (ADF) images from these thin films. This image contrast has a complicated dependence on both the angular range subtended by the dark-field detector and mass-thickness variations within the films. On microscopes with appropriate lens controls which permit the acceptance angle of the ADF detector to be varied, it becomes possible actually to reverse the contrast between the two phases.     

Electrical transport properties of low-stage AsF5-intercalated graphite

The in-plane resistivity of stage 1 and stage 2 AsF₅-graphite intercalation compounds was measured using a contactless r.f. eddy current technique from 1.6 to 290 K. The magnetoresistance of a stage 1 compound was similarly measured from 4.2 K to 290 K. The low temperature stage 2 resistivity data show a well-defined intermediate T ² region in addition to the usual T high temperature region, in qualitative agreement with the Kukkonen theory and indicative of a small, elongated cylindrical Fermi surface. Stage 2 resistivity data also show, for the first time in a graphite-acceptor compound, an apparent low temperature phase transition at 21 K. Magnetoresistance data were used to determine a stage 1 carrier concentration of 9×10²⁰ holes cm^–3. Resistive anomalies were observed at 200 K and 220 K for stage 1 and stage 2 compounds, respectively.     

Sintering and crystallization of mullite powder prepared by sol-gel processing

Mullite powder with the stoichiometric composition (3Al₂O₃.2SiO₂) was synthesized by a sol-gel process, followed by hypercritical drying with CO₂. Within the limits of detection by X-ray diffraction, the powder was amorphous. Crystallization of the powder commenced at 1200 °C and was completed after 1 h at 1350 °C. In situ X-ray analysis showed no intermediate crystalline phases prior to the onset of mullite crystallization and the pattern of the fully crystallized powder was almost identical to that of stoichiometric mullite. The synthesized powder was compacted and sintered to nearly theoretical density below 1250 °C. The microstructure of the sintered sample consisted of nearly equiaxial grains with an average size of 0.2 m. The effect of heating rate (1–15 °C min^–1) on the sintering of the compacted powder was investigated. The sintering rate increased with increasing heating rate, and the maximum in the sintering curve shifted to higher temperatures. The sintering kinetics below 1150 °C can be described by available models for viscous sintering.     

Creep-sintering of polycrystalline ceramic particulate composites

The sintering of particulate composites consisting of a polycrystalline zinc oxide matrix with 10 vol % zirconia inclusions of two different sizes (3 and 14 m) was investigated at a constant heating rate of 4 °C min^–1 under an applied stress of 300 kPa. The presence of the inclusions produced a decrease in both the creep rate and the densification rate but the ratio of the densification to creep rate remained constant during the experiment. The ratio of the densification rate to creep rate for the composites was 1.5 times greater than that of the unreinforced matrix regardless of inclusion size. The creep viscosity of the composites was higher than that of the unreinforced matrix and increased slightly with decreasing inclusion size.     

Mechanical properties of alkaline earth-doped lanthanum gallate

Lanthanum gallate doped with alkaline earths was prepared from combustion-synthesized powders. Mechanical properties of the doped gallates were evaluated as a function of composition and temperature. The indentation fracture toughness of Sr-substituted gallates was significantly better than the Ca- and Ba-substituted materials, but the toughness of all the doped gallates was significantly lower than yttria-stabilized zirconia, a typical electrolyte material. Small improvements in room temperature toughness and strength were measured in (La_0.9Sr_0.1)_xGa_0.8Mg_0.2O_3–, (LSGM-1020) samples with significant A-site cation non-stoichiometry (x = 0.9). The flexural strength of stoichiometric LSGM-1020 decreased from 150 MPa at room temperature, to 100 MPa at higher temperatures (600–1000°C). The notched-beam fracture toughness of LSGM-1020 decreased from 2.0–2.2 MPam at room temperature, to 1.0 MPam at 600°C. The decrease in mechanical properties over this temperature range was correlated to changes in crystal structure that have been identified by neutron diffraction. These crystallographic changes were also accompanied by significant changes in the thermal expansion behavior and elastic modulus. For off-stoichiometric LSGM-1020 with A/B cation stoichiometry of 0.90, strength and toughness also decreased with temperature, but the retained toughness (1.5 MPam) at elevated temperatures was higher than the toughness of the stoichiometric LSGM material.     

Measurement of temperature in a non-steady-state gas flow

A method is described for measuring the temperature of a non-steady-state gas flow with a thermocouple which is an inertial component of the first order.Notation T*_f non-steady-state gas flow temperature - T_t thermosensor temperature - thermal inertia factor of thermosensor - time - C total heat capacity of thermosensor sensitive element - S total heat-exchange surface between sensitive element and flow - heat-liberation coefficient - temperature distribution nonuniformity coefficient in sensitive element - Re, Nu, Pr, Bi, Pd hydromechanical and thermophysical similarity numbers - P^* total flow pressure - P static flow pressure - T^* total flow temperature - d_t sensitive element diameter - w gas flow velocity - flow density - flow viscosity - _f flow thermal conductivity - k gas adiabatic constant - R universal gas constant - M Mach number - T thermodynamic flow temperature - _o, _o and values at T=288°K - A, m, n, p, r coefficients - _c heat-liberation coefficient due to colvection - _r heat-liberation coefficient due to radiation - _b emissivity of sensitive element material - Stefan-Boltzmann constant - T_e temperature of walls of environment - _c, _r, _tc thermosensor thermal inertia factors due to convective, radiant, and conductive heat exchange - L length of sensitive element within flow - a thermal diffusivity of sensitive element material - _t thermal conductivity of sensitive element material Translated from Inzhenerno-Fizicheskii Zhurnal, Vol. 47, No. 1, pp. 59–64, July, 1984.     

Coupling of order parameter collective modes to spin density in3He-B

We derive a general expression for the dynamic spin susceptibility of³He-B which is valid for all magnetic fields. The coupling of real and imaginary modes by particle-hole asymmetry is taken into account. Then we calculate the contribution of the mode at frequency =2 – 1/4 ( is the effective Larmor frequency) to the transverse susceptibility. The spectral weight of this mode in magnetic resonance absorption is proportional to (/)^1/2 (–)², where and are particle-hole asymmetry parameters. From the experimental coupling strength of the real squashing mode to sound we estimate (–)²10^–4. The dynamic susceptibility satisfies the sum rules of Leggett. Finally we point out the difficulties in calculating the transverse NMR frequency of³He-B. These difficulties arise from theS _z =0 Cooper pairs and from the coupling ofJ _z =±1 modes forJ=1 andJ=2.     

Oriented mosaic model analysis of anisotropic thermoelectric properties of heterogeneous materials

Thermoelectric properties of heterogeneous materials are discussed in terms of a randomly oriented rectangular plate-like mosaic of anisotropic crystalline grains embedded in a homogeneous host material. Anisotropies in effective thermoelectric parameters and the values of thermoelectric parameters can be related to the mean orientation of the plate-like grains which, in turn, can be related to the orientation factor of Lotgering. They are also functions of various parameters such as dimension ratios , and of electrical resistivities, thermal conductivities, and the Seebeck coefficient, respectively, of grains to those of host medium. Use of f-dependent anisotropies in conjunction with relative magnitudes of electrical and thermal conductivities as well as of the Seebeck coefficient, allows , and to be estimated, which characterize the intergranular medium.     

Phonon anomalies in La2CuO4 + δ

The phonon dispersion of oxygen doped La₂CuO_{4 +} has been investigated by inelastic neutron scattering on a large single crystal with 0.02 (T_c = 31 K). Most of the phonons were found to be very similar to those of La_1.9Sr_0.1CuO₄. However, in measurements of a phonon branch which exhibits a pronounced anomaly in (La, Sr)₂CuO₄ a two-peak structure was observed: one series of peaks corresponds to the phonon frequencies of undoped La₂CuO₄, the other one to that of La_2–xSr_xCuO₄ with x 0.1. This finding is presumably associated with a phase separation into domains with low and high , respectively.     

The effect of silica characterization on the microstructure of BaFe12O19 ferrites

The anisotropically formed BaFe₁₂O₁₉ ferrites were prepared from the hot-rolled mill scale and silica was added to the ferrite during fine milling in the range 0.15 to 0.50 wt%. These ferrites were sintered at 1220° C for 2 h. The grain growth of the ferrites is dominantly influenced by the sizes of the silica added. Coarse-grain ( 1m) silica tends to promote discontinuous grain growth, which increases drastically with slightly increasing amounts of silica added, while fine-grain ( 0.013m) silica tends to retain fine grain microstructures with the same increasing amount of silica. The average grain size of the ferrite without silica addition was 8 to 10m. The size was increased to as large as 30m on addition of 0.15% coarse-grain silica and the microstructure was full of extremely large grains on the addition of 0.50% coarse-grain silica.     

Anisotropic spin diffusion and multiple spin echoes in3He-4He solutions

We propose a ₁-t₁-₂ pulse-NMR experiment to detect the spin-diffusion anisotropy, =D-D, in degenerate spin-polarized³He-⁴He mixtures, where D and dare the transverse and longitudinal spin diffusion coefficients. In such an experiment the nonlinearity of the dynamics produces multiple spin echoes (MSE). At the ³He concentration x₃ 4% the spinrotation parameter vanishes (M 0), so that the nonlinearity of the equations of motion is entirely due to the anisotropy. In this situation, detection of MSE amounts to observation of D. For slight anisotropy, i.e. D/D 0.25, we use a perturbation scheme similiar to that developed by Einzel et al. (in that case, for small M and small demagnetizing field) to calculate the second and third echo heights. For larger anisotropy we numerically calculate the echo heights. We find that for D/D = 0.5 the heights are 2 % of the first echo, and should be detectable. The (₁, ₂) tip-angle dependence of the D echoes is different from that of the M and demagnetization echoes, and furthermore, they occur at right angles to these echoes (in spin space). Thus, even when small spin-rotation and demagnetization effects are present, the ₁-t₁-₂ experiment provides a sensitive means of detecting the anisotropy.     

CO/pH2: A Molecular Thermometer

We utilize reversible temperature dependent changes in the IR absorption spectrum of CO molecules isolated in solid parahydrogen (pH₂) to probe bulk temperature changes during rapid vapor deposition. The intensity of a well resolved feature near 2135 cm^–1 increases monotonically with temperature over the 2 to 5 K range. The thermally populated initial state of this transition lies 12 K above the CO/pH₂ ground state. During the deposition of 100 ppm CO/pH₂ samples, we detect temperature gradients 10 K/cm in 0.1 cm-thick samples subjected to heat loads 10 mW/cm². The resulting estimated thermal conductivity (TC) is 3(±2) mW/cm-K, averaged over the 2 to 5 K region. This value is 1000 times lower than the TC of single crystal solid pH₂, and 10 times lower than previously measured for pH₂ solids doped with 100 ppm concentrations of heavy impurities [Manzhelii, Gorodilov, and Krivchikov, Low Temp. Phys. 22, 131 (1996)]. We attribute this abnormally low TC to the known mixed fcc/hcp structure of the rapid vapor deposited solids.