The effect of Ag additions on the microstructure of aluminium–lithium alloys

Minor quantities of Ag have been added to Al–Li–Cu–Mg–Zr alloys. Their microstructure has been studied by means of optical metallography, transmission electron microscopy and X-ray diffraction. In the high Li, low Cu : Mg ratio alloys the main phases found were , , S and T₁, while fewer T₂ and Al₇Cu₂Fe precipitates were also observed. The addition of up to 0.5 wt% Ag diminishes the and T₁ precipitates size. This is attributed to a small increase of Li solubility in the matrix. In the low Li, high Cu : Mg ratio alloy the addition of 0.2 wt % Ag resulted in the precipitation of phase simultaneously with , , S and T₁ phases. Due to the low Li concentration an unusual growth of the / precipitates at the expense of the precipitates was also observed.     

Coherent Brillouin Spectroscopy in Solid Parahydrogen

We applied coherent Brillouin spectroscopy to solid parahydrogen, and measured the Brillouin spectra of longitudinal acoustic modes at 5.6K. It was found that the linewidth of these spectra is 1.5MHz. From the observed Brillouin shift and the crystal orientation, the elastic stiffness was determined as C ₁₁=0.355±0.016GPa and C ₃₃=0.432±0.022GPa.     

Agglomeration problems in the formation of FeSi2 from Fe-Si thin-film couples

The agglomeration process that occurs during annealing of thin Fe films (<200 nm) on Si substrates has been studied. Agglomeration occurred on uncapped films prior to silicide formation. Capping layers of SiO₂, or more appropriately Si-SiO₂, have been used to minimize agglomeration effects. Continuous thin films of -FeSi₂ have been grown on 11 1 and 100 oriented substrates. Preferred growth of (202) and (220) suicide planes on 111 Si has been obtained, while preferential growth was not observed on 100 Si.     

The formation of single-phase Si-Al-O-N ceramics

Si-Al-O-N ceramics have been prepared by hot-pressing mixtures of Si₃N₄, AIN and SiO₂ (with an addition of 1% MgO) having varying ratios of AIN/SiO₂. Microstructural analysis by transmission electron microscopy and Auger electron spectroscopy has demonstrated the progressive increase in grain-boundary silicate glass in pressings prepared from compositions with excess SiO₂ to compositions given by the formula Si_6–zAl_zO_zN_8–z. This formula represents the simple substitution of Al for Si atoms and O for N atoms in the hexagonalSi₃N₄ crystal. Microstructures for this balanced composition are essentially single phase, consiting of non-faceted, sub-micron, grains with a grain-boundary segregate layer of glass-forming silicate composition, containing impurity and additive metal ions, which may be detected only by Auger spectroscopy. This microstructure is in contrast with unbalanced compositions which contain faceted grains joined by a glassy silicate phase which is easily detected by electron microscopy. Final microstructural analysis combined with observations of density and phase content with progress of hot-pressing has confirmed the important role of liquid silicate formation and a solution-reprecipitation mechanism for densification. The presence of a 1% MgO additive is shown to accelerate this process, forming a low melting point silicate by reaction with SiO₂, assisting the early solution of AIN and the reprecipitation of substituted crystals.     

The relative stability ofβ andβ″-phases in Na2O-Al2O3 beta alumina

To reveal the relative stability of and -phases in beta alumina, effects of Na₂0 content and calcination and annealing history on the relative content of and -phases have been studied for compositions ranging from Na₂O-5Al₂O₃ to Na₂O-9.5Al₂O₃. The relative stability appears to be dependent on the calcination or annealing history, except holding time such as annealing or re-annealing time, but independent of the Na₂O content and the holding time. From these results it can be demonstrated that the relative stability of and -phases is sensitive to the heat treatment path, except the holding time. The two stage model on the /. polytypic transition in silicon carbide has been quoted to explain the heat treatment pathdependent characteristics.     

Mullite formation from non-crystalline precursors

X-ray diffraction, differential thermal analysis, and²⁹Si and²⁷Al MAS NMR spectroscopy were used to characterize the formation of mullite from non-crystalline precursors. The precursors were produced by the sol-gel route from organic starting compounds (SGM), and by coprecipitation of inorganic starting materials (CM). There is NMR evidence that both types of mullite precursor consist of Si-O and Al-O tetrahedra, and of Al-O octahedra. Furthermore, fivefold-coordinated Al-O polyhedra, or alternatively strongly distorted Al-O tetrahedra, do occur in the precursors. SGM and CM precursors transform to mullite in multi-step reactions with intermediate formation of-Al₂O₃, and a non-crystalline nearly pure SiO₂ phase. The-Al₂O₃ compound has a highly distorted spinel structure, and may contain some minor amount of Si. The diffusion-controlled decomposition of the precursors to-Al₂O₃ + SiO₂ at low temperature (1000°C) suggests that the precursors are diphasic, consisting of nanometre-sized, long-range-disordered Al₂O₃- and SiO₂-rich domains. The reaction of-Al₂O₃ + SiO₂ above about 1000°C initially produces Al₂O₃-rich mullite. This is explained by a possible nucleation of mullite on the surfaces of-Al₂O₃ crystallites. The gradual transformation of the unstable, low-temperature (1000 to 1400°C) Al₂O₃-rich mullites to the stable high-temperature ( 1400°C) 3/2-type mullites (3Al₂O₃ · 2SiO₂) is essentially controlled by the annealing temperatures, whereas annealing times play a minor role.     

Phase Transformations and Melt Structure of Calcium Metasilicate

The phase transition, melting, crystallization, and vitrification of calcium metasilicate were studied by high-temperature Raman scattering spectroscopy. The results demonstrate that, in the course of melting, the [Si₃O₉] metasilicate rings, which form the structural basis of the phase, transform mainly into [SiO₃] anions. The structural similarity or dissimilarity of the CaO · SiO₂ melt to crystalline phases is shown to have a crucial effect on its crystallization/vitrification behavior.     

Low temperature iron thin film-silicon reactions

Low temperature reactions between Fe thin films and Si substrates have been studied. Iron films were deposited by electron beam evaporation onto 111 orientated Si substrates. An SiO₂ capping layer was used to protect the Fe from oxidation during subsequent annealing. Samples were annealed at temperatures as high as 650 °C, for up to several hours. It has been shown that FeSi is the initial suicide to form, with 300 °C being the lowest formation temperature. Fe₃Si forms after most of the Fe has been consumed, and forms as a separate phase from -Fe and not through a disorder-order transformation. Microstructural evidence for nucleation controlled formation of -FeSi₂ from FeSi has also been given.     

Theoretical fundamentals of the method for thermal diffusivity measurements from auto-oscillation parameters in a system with a thermal feedback

Theoretical fundamentals of the method to determine thermal diffusivity from auto-oscillation parameters in a control system, CS, with thermal feedback through the test specimen, are developed. The equation of a CS with a flat specimen and proportional controller (nonlinear boundary value problem of nonstationary heat conduction) is considered. Periodic solutions of the boundary value problem, which is linearized in the vicinity of the stationary solution, are analyzed. It is proved that, with a certain value of CS gain factor, excitation of auto-oscillations occurs. Their frequency _c is related to the thermal diffusivity as = C_c, where C is constant. By nonlinear analysis, it is revealed that the auto-oscillation excitation mode is soft and the frequency depends on the gain factor to a very weak degree. Formulas for calculation of the thermal diffusivity and the specimen temperature field are obtained.Nomenclature A Generalized gain factor - A _c Critical value of A - a Thermal diffusivity - b ₂, c₂ Lyapunov coefficients - K Controller gain - k Wavenumber - q Heat flux - R Heater resistance - S Heater surface area - T(x, t) Difference between specimen and thermostat temperatures - t Real time - u ₀ Reference voltage - u ₁,u₂ Voltage - x Coordinate - x ₀ Thermocouple coordinate - Thermo emf factor - Specimen thickness - Relative deflection of A from A _c - Thermocouple normalized coordinate - Thermal conductivity - v Temperature wave phase delay through the whole specimen - Auto-oscillation amplitude - Heaviside step function - Normalized time - ¢ Spatial part of phase - Frequency     

Phase relationship between β′- and O′-sialon at 1623 K

-sialon whiskers and co-products of synthesis, such as -sialon powders and O-sialon powders, were annealed at 1623 K for 8 h in a closed graphite reaction tube under 1 atm nitrogen. Phase stabilities, Si/Al ratios, and crystallographic features were investigated. The O-sialon phase, which formed in the early stage of synthesis when oxygen partial pressure was relatively high, became less stable in the present annealing condition and decomposed. The majority of released aluminium and possibly oxygen from the decomposed O-powder was incorporated into -sialon whiskers with little change in its lattice parameters, when the -sialon whiskers were included in annealing. The aluminium contents were always lower in the -whiskers than in the powders even after increasing its aluminium content during 8 h annealing. The lattice parameters of both -whiskers and powders increased with increasing aluminium content and became closer after annealing. The lattice parameters of -whiskers remained the same before and after annealing despite the increased aluminium content, while the lattice parameters of -powders decreased despite its aluminium content remaining unchanged. The lattice parameters of O-sialon increased with increasing aluminium content, and the increase in thea direction is the largest when compared with other parameters.     

Microstructure of laser melted/rapidly solidified γ/Cr3Si metal silicide “in situ” composites

In order to improve the ductility of Cr₃Si metal silicide alloys, rapidly solidified /Cr₃Si metal silicide in situ composites were fabricated by laser melting/rapid solidification technology using Cr-Si-Ni alloy powders. Microstructure of the /Cr₃Si in situ composites was characterized by OM, SEM, XRD and EDS. The effect of Ni content in the alloy powder on microstructure and hardness of the /Cr₃Si composites was investigated. The /Cr₃Si metal silicide in situ composites have high hardness and rapidly solidified fine microstructure consisting of primary Cr₃Si dendrites and the interdendritic /Cr₃Si eutectics. The volume fraction of the Cr₃Si primary dendrites in the laser melted/rapidly solidified /Cr₃Si metal silicide in situ composites decreases with the increasing nickel content. Because of the presence of the ductile nickel-base solid solution and the rapidly solidified fine microstructure, the /Cr₃Si metal silicide in situ composites are expected to have adequate combination of strength and toughness. The results demonstrate that laser melting/rapid solidification for /Cr₃Si metal silicide in situ composites is a promising toughening method for improving the ductility of Cr₃Si metal silicide alloys.     

The viscosity and some related properties of liquid3He at the melting curve between 1 and 100 mK

The viscosity of liquid ³ He has been measured along the melting curve from 1 to 100 mK by means of a vibrating wire viscometer. In the normal Fermiliquid region we find 1/T² = 1.17–3.10T, where is in P and T in K. At the transition temperature T _A = 2.6 mK a rapid decrease occurs in _n , the viscosity of the normal component. Within 0.3 mK below T _A , _n decreases to about 25% of _A, but then becomes essentially constant. In the B phase _n first decreases to 20% of _A and then seems to increase below 1.4 mK. Data on _n , the density of the normal component, are also presented in the A and B phases. The results show that viscous flow is accompanied by a flow of zero dissipation, thus proving superfluidity in the A and B phases. The viscosity data at magnetic fields up to 0.9T have been related to theoretical calculations of the energy gap of superfluid ³ He near T _A . The splitting of the A transition and the suppression of the B phase in an external field were also measured.     

Stability of metastable phases and microstructures in the ageing process of Al–Mg–Si ternary alloys

Precipitation behaviour of Al–Mg–Si alloys, with balanced (Mg/Si=2), excess silicon (Mg/Si<2) and excess magnesium (Mg/Si>2) compositions, were studied by differential scanning calorimetry (DSC), transmission electron microscopy (TEM), and Vickers hardness tests. Four significant exothermic peaks were observed in DSC curves which were attributed to metastable clusters, , and stable phases. The peaks corresponding to and were formed closely in the DSC curves but showed different behaviour in isothermal annealing. The additional peak verifying the precipitation of phases, which has recently been proposed by some workers, was not detected. Transmission electron microscope observations and Vickers microhardness tests showed that precipitates played a major role in improving the hardness, but not precipitates. © 1998 Chapman & Hall     

Fabrication and mechanical properties of α-Al2O3/β-Al2O3/Al/Si composites by liquid displacement reaction

Al₂O₃/metal composites were fabricated by heating three kinds of commercial mullite refractories in contact with Al, and their mechanical properties were investigated. Aluminum reacted with the mullite and SiO₂-glass constituting the mullite refractories and changed them into -Al₂O₃ and Si. Simultaneously, -Al₂O₃ was formed by the reactions among -Al₂O₃ and sodium and potassium oxides in the glassy phase. Also, Al penetrated into the -Al₂O₃/-Al₂O₃/Si composite by partly dissolving Si. Finally, the mullite refractories were changed into -Al₂O₃/-Al₂O₃/Al/Si composites. The phase contents, microstructures and mechanical properties of the resulting composites varied with the composition of the refractories. The content of -Al₂O₃ in the composite was lowest at the lowest Na₂O and K₂O contents in the refractories. Silicon in the composite had its highest content at the highest SiO₂ content. The composite fabricated from SiO₂/Al₂O₃ (in mol) (SAR)=1.85 consisted of 2–5 m Al₂O₃ grains embedded in metal, but that from SAR=1.05 showed a complicated microstructure with small and large grains. The bending strength of the composites fabricated from the refractories of SAR=1.85, 1.24, and 1.05 were 327, 405 and 421 MPa, respectively. Also, the corresponding fracture toughness values were 5.2, 6.1, and 5.5 MPam , respectively.     

On the microscopic interaction in the Chevrel compounds Cu2Mo6S8 and Mo6Se8

The available data on the superconducting properties of Cu₂Mo₆S₈ and Mo₆Se₈ are used to gain some insight into their microscopic parameters ² F() and *, the electron-photon spectral density and Coulomb pseudopotential, respectively. While thermodynamic data play a prominent role in the analysis, use is also made of information on the generalized phonon frequency distributionG() and, for the case of Cu₂Mo₆S₈, on the second derivative of current-voltage tunneling data. The parameters obtained are tested against upper critical magnetic field data. The work suggests that the electron mass enhancement parameter may be of order 2 with * unusually large.     

Magnetic properties of highly dilutedPdFex andPtFex-alloys. Part II. Susceptibility at micro- and milli-kelvin temperatures

We have measured the 16 Hz susceptibility of the giant magnetic moments induced by Fe impurities in highly dilutedPdFe_x andPtFe_x samples with 2.5 ppm x 75 ppm in a wide temperature range, 30 K T 300 mK, and at static magnetic fields 0,01 mT B 25 mT. We find spin glass freezing at Tf(X)/X0,19mK/ppm Fe forPdFe_x and the larger value 0.26 mK/ppm Fe forPtFe_x. This is the first observation of spin glass freezing inPtFe_x. In the low-temperature range T 0.5T_f(x), the susceptibilities follow — ₀ T with small zero-temperature ₀ values forPdFe_X and vanishing ₀ values forPtFe_x. In the paramagnetic high-temperature range, we find (T — )^it-1 at T 10 mK independent of x forPdFe_x, and at T 2Tf(x) dependent of x forPtFe_x with vanishing values for both systems. The data compare well to the predictions of the Thouless-Anderson-Palmer TAP approach of the Sherrington-Kirkpatrick SK model for spin glasses.     

Synthesis, crystal structure and X-ray powder diffraction data of the phosphor matrix 4SrO·7Al2O3

The white phosphor matrix 4SrO·7Al₂O₃ has been synthesized by firing the appropriate mixture of SrCO₃, Al(OH)₃ and H₃BO₃ in the molar ratios 1:3.5:0.135 at 1300°C for 4–7 h. The crystal structure of 4SrO·7Al₂O₃ has been determined as a orthorhombic Pmma space group with a=24.7451(2)Å, b=8.4735(6)Å, c=4.8808(1)Å, V=1023.41(3)ų, Z=2, and D=3.66 g cm^–3 by the Rietveld analysis. The refinement figures of merit are R_p=8.26, R_wp=11.60, R_bragg=4.44 and s=2.61 for 844 reflections with 2<119.94°. And the corresponding X-ray powder diffraction data are presented for search/match analysis.     

Temperature dependence of electrical resistivity of deformed and undeformed V-rich V3Si single crystals

The electrical resistivity (T) of V-rich V₃Si single crystals (T _c-11.4 K) was measured from 4.2 to 300 K along the directions of [1 0 0] and [1 1 1] before and after plastic deformation at 1573 K. Anisotropy of (T) was observed although V₃Si has the cubic A15 structure. Plastic deformation does not affect the normal-state (T) behaviour but changes the normal-superconducting transition width T_c. At low temperatures (T _c<T 40 K), (T) varies approximately as T ⁿ where n-2.5 and this behaviour does not contradict the (0)- phase-diagram plot proposed by Gurvitch, where is the electron-phonon coupling constant and (0) is the residual resistivity.     

First viscosity of dilute3He-4He mixtures below 0.6 K

Starting with the Boltzmann transport equation, the first viscosity of dilute³He-⁴He mixtures for various³He concentrations x is evaluated up to around T 0.6 K by including the contribution from three-phonon processes (3PP) in the anomalous elementary excitation spectrum of liquid⁴He. Due to 3PP, the characteristic time for³He viscosity at high temperatures, i.e., T2T_F where T_F is the³He Fermi temperature, is evaluated as 5 × 10^–12/xT, which is smaller than the value estimated by Rosenbaum et al. This is interpolated with in the degenerate (quantum) region, TT_F. The obtained viscosities are in better agreement with experimental results than those of Baym and Saam, whose theory does not include 3PP. However, at very low concentrations there exists a discrepancy between the present theory and experiments, so that an alternate treatment should be considered.     

Incommensurate modulated structure in the cubic-tetragonal transition of V-Ru alloys studied by high resolution electron microscopy

The cubic-tetragonal transition of V-Ru alloys near 50 at % has been investigated by high resolution transmission electron microscopy. In the cubic to tetragonal transition process of thin foil specimens, we found an incommensurate modulated structure showing satellite spots near 1/4 0 1 1 positions in the electron diffraction patterns. This incommensurate structure is composed of many domains of the commensurate modulated structure with a pseudotetragonal cell of A=B=2(a ² + c ²)^1/2 and C=c, where a and c (1.07a) are the lattice constants of the tetragonally distorted CsCl-type structure. The modulation is interpreted in terms of the combination of dual elastic shear distortion waves nearly parallel to the 0 1 1 directions with the approximate wavelength of 22a. We propose a model for the incommensurate modulated structure.