The constitution of the Ni-Al-Ru system

The constitution of the Ni-Al-Ru system has been investigated in the range 0 to 50 at% Al. Isothermal sections at 1523 and 1273 K have been determined using microstructural observations, electron probe microanalysis and X-ray diffraction. The phases present were: nickel-based solid solution (); (based on Ni₃Al); solid solutions based on NiAl and RuAl, respectively (designated ₁ and ₂), and ruthenium-based solid solution (Ru). The maximum solubility of Ru in was 5 at%. ₁, and ₂ show extensive range of solubilities, namely up to 20at% Ru in ₁ and up to 25 to 35 at% Ni in ₂. Three-phase equilibrium between , ₂ and (Ru) existed at 1523 and 1273 K. Also at 1523 K, three-phase equilibria existed between , and ₁ and ,₁ and ₂, while at 1273 K, the equilibria were between , ₁,₂ and , , ₂ indicating the occurrence of a reaction +₁, +₂ at a temperature between 1523 and 1273 K. Liquidus features have been deduced from data on as-solidified structures. Lattice parameter data and hardnesses are also reported.     

Distribution of α-AlFeSi and β-AlFeSi particles in surface layer of AA6063 alloy billets after heat treatment

We developed the EPMA mapping method of small -AlFeSi(Al_8.3Fe₂Si) and -AlFeSi(Al_8.9Fe₂Si₂) particles in the billets of Al-Mg-Si alloys such as AA6063 alloys. To discriminate between -AlFeSi and -AlFeSi particles we used the relative X-ray intensities of Fe/Si ratio, the I _Fe/I _Si ratio, instead of the Fe/Si mass ratio. To obtain the I _Fe/I _Si ratio, we used a Monte Carlo method. In this study, using this method the mapping of -AlFeSi and -AlFeSi particles in the surface layer of AA6063 billets after the heat treatment (for 2 h at 580°C) was done. Namely, the distribution of -AlFeSi and -AlFeSi particles of zones from the billet surface to a depth of 800 m was measured. Results showed the zone from the surface to a depth of 200 m was occupied mainly by -AlFeSi particles and the zone from a depth of 200 m toward the center was occupied mainly by -AlFeSi particles. From these results, it was found that if we remove zones from the surface to a depth of 200 m, we can remove the majority of the -AlFeSi particles, and thus improve the quality of anodizing performance of Al-Mg-Si alloys extrusions.     

Sinterability of β-SiAlON powder prepared by carbothermal reduction and simultaneous nitridation of ultrafine powder in the Al2O3-SiO2 system

Three types of -SiAlON (Si_{6 – z} Al _z O _z N_{8 – z} ) powder were prepared by the carbothermal reduction and simultaneous nitridation of ultrafine powders in the Al₂O₃-SiO₂ system. The ultrafine starting oxide powders, prepared using the vapour-phase reaction technique, were mixed with carbon powder and heated at 1400 °C for 1 h under flowing nitrogen to form -SiAlON and followed by heating at 570 °C for 1 h in air to remove residual carbon. The resulting powders contained only -SiAlON with z values of 1.63, 2.05, and 2.99. The relative density (bulk density/true density) of -SiAlON compacts pressureless sintered at 1800 °C for 1 h under flowing nitrogen increased with z and reached 89.9% at z = 2.99. When the -SiAlON compact with z = 2.99 was hot pressed at 1800 °C for 1 h under flowing nitrogen, a maximum relative density of 93.6% was achieved. Although this hot pressed compact contained a small amount of 15R-SiAlON in addition to -SiAlON, it possessed a small average grain size (typically 0.5 m diameter) and high Vickers hardness (19.2 GPa).     

A new parameter for describing the structure bifurcation in two-phase alloys containing coherent particles

The so-called bifurcation diagrams for precipitate particles in nickel-based alloys were obtained by calculating the energy state for a pair of particles on the basis of the bifurcation theory. Based on the bifurcation diagrams, we have proposed a new parameter for describing the two-phase structure containing coherent particles. The parameter is defined as the mean particle radius at the intersection of the energy ridge and the line ofR=–0.5 orR=0.5 in the bifurcation diagram (R(r –r )/(r +r ), wherer andr are the radii of and ), and is symbolized by¯r ^* _±0.5. Because the energy state of the paired and is maximum at¯r ^* _±0.5 whenR=±0.5,¯r ^* _±0.5 is just like the watershed and hence we have termed it structureshed. This parameter successfully describes the effects of elastic energy as well as surface energy on the microstructural changes during coarsening of precipitate particles.     

Structure of martensite formed in Cu-Al-Fe single crystals duringin situ HVEM pseudoelastic tensile experiment

Single crystals of the CuAlFe alloy, containing 14.5 wt% Al and 2.2 wt% Fe were subjected toin situ tensile experiment using straining attachment in a 1 MV electron microscope. Loadelongation curves were obtained for three foil plane/tensile direction orientations: (001) [0 1 0], (0 0 1) [1 1 0] and (1 1 0) [¯1 1 2]. Each crystal was subjected to two cycles of pseudoelastic deformation up to maximum 2% strain, showing almost complete shape recovery. Structure observations and electron diffraction pattern indicated that during deformation of samples of (0 0 1) [1 1 0] and (1 1 0) [1 1 2] orientations, formation of ₁ martensite was observed and only at later stages narrow needles of ₁ nucleate in front of ₁. During pseudoelastic deformation in the (0 0 1) [1 0 0] direction, martensite forms as a mixture of narrow plates possessing either 2H or 18R structures. The following crystallographic relationship between the parent phase and both types of martensite was observed: [1 00] ₁ [101] ₁ and (0 0 1) ₁ (0 1 0)₁;(0 0 1) ₁ (0 1 0) ₁ and [1 1 0] ₁ [0 0 1] ₁. From the character of sidebands reflections presence of 1 0 1 1 0¯1 static displacement waves was inferred.     

Interface characterization of a β-SiC whisker-Al composite

The nature of the interface, the orientation relationship of -SiC whisker (-SiC_w)-Al combination, and the misfit dislocation structures at the -SiC_w-Al interfaces in a -SiC_w-Al composite have been observed by a high-resolution transmission electron microscopy (HRTEM). It was shown that quite a good bonding between the whisker and the aluminium was achieved due largely to the lattice match between SiC and aluminium at the interfaces. The orientation relationship between the whisker and the aluminium was {002}_SiC{111}_Al; 110_SiC110_Al. The interface was clean, faceted and semicoherent. The misfit dislocation cores were located in the whisker side away from the -SiC_w-Al interfaces.     

Distribution of electron concentrations in a discharge with nonlinear sources for the appearance and disappearance of particles

We have derived an approximate solution for the one-dimensional steady equation of electron balanceD _a² n+n+n ²=0, in which the coefficients and may vary as to sign. The nonlinear term was approximated by two segments of straight lines by the method of least squares, as a result of which the original equation was reduced to a system of two linear differential equations whose solution is presented in analytical form. We have obtained numerical data for the determination of the electron concentration profile in the range –8R²n₀/D_a20 for a plane, cylindrical, and spherical configuration of the discharge zones.Translated from Inzhenerno-Fizicheskii Zhurnal, Vol. 59, No. 2, pp. 225–229, August, 1990.     

Method for heat transfer calculation using isothermal coordinates

Equations for steady-state heat transfer are considered in curvilinear coordinates. The equations are shown to be simplest when one of the families of coordinates are isotherms. Conditions are obtained for which these coordinate systems and some exact solutions of the heat conduction equations must satisfy.Notation a ₁, a₂, ..., a_n coefficients determining the temperature dependence of thermal conductivity (see formula (8)) - f() function of the -coordinate (see formula (4)) - H ₁,H ₂,H ₃ coefficients of the first differential form (Lamé coefficients) (see formula (2)) - n number of a term of the series in formula (8) - q heat flux - Q power of volume heat release - x, y, z Cartesian coordinates - , , general curvilinear orthogonal coordinates - ₁, ₂ coordinates of the boundary surfaces on which the temperatures are prescribed - x ₀₁ thermal conductivity att=0 - () function of the -coordinate (see formula (4)) - () -function determining temperature distribution in the case of constant heat flux along the coordinate lines Scientific-Research and Design-Technological Institute of Machine Manufacture, Scientific-Production Subbranch Novator, Kramatorsk, Ukraine. Translated from Inzhenerno-Fizicheskii Zhurnal, Vol. 68, No. 4, pp. 651–659, July–August, 1995.     

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.     

o′-β′ sialon ceramics

Powders of Si₃N₄, Al₂O₃ and SiO₂ were mixed with Y₂O₃ as sintering aid and hot-pressed to form o- sialon. During sintering, the o phase preferentially precipitated in the temperature region of 1550 to 1600 °C, and the phase precipitated at temperatures of 1700 °C and above. The resultant microstructure consisted of dual phases of o and . The mechanical properties of o- sialon were improved with increasing amount of the phase. When SiO₂ required for the formation of the o phase was all included in the grain boundary phase, o- sialon exhibited a three-point bending strength as much as 1400 MPa. The oxidation resistance of o- sialon is expected to improve due to the presence of the o phase, but actually was not so good due to the presence of the grain-boundary glassy phase and impurities.     

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.     

Phase decomposition of liquid-quenched β-type Ti-Cr alloys

Phase decomposition behaviour of liquid-quenched (bcc) type Ti-Cr alloys was investigated by means of transmission electron microscopy and hardness measurements. It was found that decomposition of to ₁ (Ti-rich, bcc) + ₂ (Ti-lean, bcc) takes place in the intermediate composition range of the Ti-Cr system. This experimental result proves the theoretical prediction made by Menon and Aaronson, but the observed ₁ + ₂ two-phase field expands towards higher temperatures than the predicted binodal line. The coherent ₁ + ₂ two-phase state exhibits the so-called 100 modulated structure and it was concluded that the formation of such a structure is a result of spinodal decomposition of the -phase. We obtained time-temperature-transformation (TTT) diagrams of -type Ti-30, 40 and 50 at % Cr alloys. A typical sequence of structural change is coherent ₁ + ₂ incoherent ₁ + ₂ incoherent ₁ + ₂ + grain boundary precipitates stable state of + TiCr₂ or + TiCr₂. Not all the states in the above sequence appear, depending on alloy composition, liquid-quenching rate and ageing temperature.     

Crystallization of some spodumene-lithium zinc orthosilicate glasses

By using thermal analysis, X-ray diffraction, polarizing and electron microscopy the effect of compositional variation, thermal treatment and nucleation catalysts TiO₂ and ZrO₂ on the nature, type and stability fields of the crystallizing phases, as well as the resulting microstructures, is described for some stoichiometric glass compositions within the system LiAlSi₂O₆-Li₂ZnSiO₄. Intense uniform volume crystallization was achieved. Transparent glass-ceramics with ultrafine microstructures could also be obtained at temperatures near 700 °C. Crystallization begins with the formation of a proto - and/or _II-Li₂ZnSiO₄ followed by, or concomitant with, -eucryptite ss. The proto -phase was formed over a narrow temperature range and rapidly transformed into its _II-modification which, although showing a wider stability range, ultimately transformed into the stable _o-modification. The metastable -eucryptite ss starts its transformation into -spodumene around 800 °C. By prolonged heating at temperatures as high as 1000–1040 °C, -spodumene and _o-Li₂ZnSiO₄ were the main stable end products. TiO₂ and ZrO₂ have contrasting effects on the stability of the LiZn orthosilicates and -eucryptite ss -spodumene transformations. The former exhibits a catalytic effect and the latter showed a retarding effect on these processes.     

Phase transformation and densification during pressureless sintering of Si3N4 with MgO and Y3Al5O12 additives

The - transformation of Si₃N₄ during liquid-phase sintering appears to be controlled by the growth of the -Si₃N₄ grains in the direction perpendicular to thec-axis in the case of MgO additive. The diffusion through the liquid is the rate-controlling step in the case of the Y₄Al₅O₁₂ additive. The density of the sintered body at the solid skeleton stage was influenced by the change in the - transformation rate and/or by a change of the transformation mechanism. The indirect proportionality between the -phase content in the starting powder and the density at the solid skeleton stage was found. The microstructure of the sintered body is influenced by both the -phase content in the starting powder and the chemical composition of the additive. Fine, uniform microstructure with a high aspect ratio of -grains is obtained, when the -phase content in the starting powder is as small as possible and when the - transformation is controlled by grain growth.     

Nucleation and growth of β′magnesium sialons and their composition limits

Previous reports on the solubility of magnesium in -sialons have been conflicting. The present work shows conclusively that crystalline magnesium sialons with the silicon nitride structure do exist. They are formed by crystallization of magnesium sialon glasses at low temperatures. -magnesium sialon crystals nucleate on -sialon nuclei which are themselves formed by precipitation from Mg-Si-Al-O-N liquids at high temperatures. The current results suggest that -magnesium sialons exist only over a limited composition range within the 3M/4X plane of the Mg-Si-Al-O-N system, which is indicative of some form of ordering within the structure. Although the compositions investigated in the present study are unstable with respect to forsterite above about 1000° C, the possibility of producing -magnesium sialons which are stable at much higher temperatures cannot be fully discounted at present.     

Carbothermal production of β′-sialon from alumina,silica and carbon mixture

Mixtures of pure nanometer-sized amorphous silica and -alumina with the atomic ratio SiAl=1 were reduced by a stoichiometric amount of carbon between 1100 and 1450 °C in flowing nitrogen in order to produce -sialon powder. Using aqueous suspensions of starting materials, compacts with different microstructures were prepared for reaction. Silica reduction to SiO occurred at a temperature as low as 1300 °C and part of it was removed with flowing nitrogen. Carbothermal reaction involving nitrogen stated at 1350 °C and Si₂N₂O was found as an intermediate together with SiC, resulting in -sialon formation. Loss of silica from the system led to AlN formation. Decomposition of -sialon into sialon polytypoids (15R, 12H) was observed as a result of sialon and AlN reaction at 1450 °C. The reaction rate of sialon formation was slowed down compared to the carbothermal reduction of kaolin because of the lack of impurities. The microstructure of the reacted pellets influenced the reaction products, and the narrow pore size distribution as well as good homogeneity enhanced -sialon formation.On leave, from Silesian Technical University, Krasiskiego 8, 40-019 Katowice, Poland.     

EPMA mapping of small particles of α-AlFeSi and β-AlFeSi in AA6063 alloy billets

It is well known that the spatial distribution and the spatial density of the particles o-AlFeSi and -AlFeSi in the billets of Al-Mg-Si alloys, such as AA6063 alloys affect the quality of anodizing performance of their extrusions. For this reason it is very important to control the spatial distribution and the spatial density of both AlFeSi particles at extrusion plants. The X-ray diffraction method (XRD) has been used for discrimination between -AlFeSi and -ALFeSi particles. However it is not an appropriate method for determining the spatial distributions of particles in the alloys. As an alternative method an electron probe microanalyzer (EPMA) has been used for determining the spatial distributions of each element in the microstructures. However, unfortunately it is difficult to discriminate between the particles composed of the same elements like -AlFeSi and -AlFeSi particles. Thus, we tried to develop a convenient method to discriminate between -AlFeSi and -AlFeSi particles in the microstructure of AA6063 alloys and developed the EPMA mapping of -AlFeSi and -AlFeSi particles. First, in order to discriminate between the two particles, we tried to use the relative X-ray intensity ratio, the I _Fe/I _Si ratio instead of the Fe/Si mass ratio. Then, we calculated the value of the I _Fe/I _Si ratio from -AlFeSi and -AlFeSi by using Monte Carlo calculations and obtained the critical value of the I _Fe/I _Si ratio, to distinguish between -AlFeSi and -AlFeSi. After that, using the discrimination value, we developed the EPMA mapping program (EPMA method) to observe the distributions of -AlFeSi and -AlFeSi, and to calculate the areas (%) of -AlFeSi and -AlFeSi. Finally, we checked the correlation between the EPMA and the XRD methods. Consequently, the two methods were in good agreement. Today, this EPMA method instead of the XRD method is successfully used in the quality control of 6063 aluminum alloy billets after heat treatment at our aluminum extrusion works.     

Effect of grain size distribution on the strength of porous Si3N4 ceramics composed of elongated β-Si3N4 grains

The grain size distributions (diameter and aspect ratio) of porous Si₃N₄ ceramics composed of elongated -Si₃N₄ grains were evaluated statistically, and their effect on the pore size distribution and the flexural strength of the porous Si₃N₄ was investigated. Porous Si₃N₄ ceramics having porosities of 27 to 43% and median pore diameters of 0.56 to 0.96 m were used as specimens. The grain diameter distribution was well correlated to the pore size distribution of the porous Si₃N₄ ceramics. We concluded that the strength of the porous Si₃N₄ ceramics increased with increasing grain length of -Si₃N₄ as well as with decreasing porosity.     

The redistribution of alloying elements by rapid-heating solution treatment of an (α +β) titanium alloy

Thin-foil X-ray energy-dispersive chemical analysis of an (+) titanium alloy has been used to establish the compositional profiles which develop between the and phases as a result of heating into the field at a rate of 100 K sec^–1. The results show that phase transforms to via a diffusional mechanism as it is progressively enriched in-stabilizing solutes. Complete diffusional transformation of to occurs 160 K above the transus but the phase remains chemically inhomogeneous. On subsequent quenching at a rate of 400 K sec^–1, phase containing less than approximately 10wt% Mo equivalent of -stabilizing solutes transforms to martensite. The proposed transformation mechanisms are consistent with the results of resistivity measurements made during the heating and cooling cycles.     

Variation of aluminium concentration in β′-sialon grains formed during liquid-phase sintering of Si3N4-Al2O3-Nd2O3

The aluminium concentration in -sialon grains of the 74Si₃N₄ ()-6Al₂O₃-20Nd₂O₃ (wt%) specimen has been determined. As the - transformation proceeded, the average aluminium concentration in -sialon grains decreased. For individual grains, the aluminium concentration at the centre was higher than that at the edge. The observed variation of aluminium concentration has been explained in terms of the compositional change of the liquid matrix during sintering.