Microstructural and mechanical study of AL2O3/Er3Al5O12 eutectic rods grown by the laser floating zone method

Eutectic rods of Al2O3–Er3Al5O12 were grown by directional solidification using the laser-heated floating zone method at rates in the range 25–1500 mm/h. Their microstructure and mechanical properties (hardness, toughness and strength) were investigated as a function of the growth rate. A homogeneous and interpenetrated microstructure was found in most cases, and interphase spacing decreased with growth rate following the Hunt–Jackson law. Hardness increased slightly as the interphase spacing decreased while toughness was low and independent of the microstructure. The rods presented very high bending strength as a result of the homogeneous microstructure, and their strength increased rapidly as the interphase spacing decreased, reaching a maximum of 2.7 GPa for the rods grown at 750 mm/h. The bending strength remained constant up to 1300 K and decreased above this temperature. The relationship between the microstructure and the mechanical properties was established from the analysis of the microstructure and of the fracture mechanisms

On the structure of the floating zone in melting

Floating zone melting is used in crystal growth and purification of high melting materials. The use of a reduced gravity environment will remove the constraint imposed on the length of the zone by the hydrostatic pressure. The equilibrium of the fioatmg zone may involve, (1)Hydrostatic forces, when the zone rotates as a whole. (2)Convective driving forces, when the zone is stationary but fluid property gradients appear.(3) Hydrodynamic forces, when some parts of the zone are set into motion with respect to others. The last effects are considered in this paper. The flow pattern of a floating zone held between two discs in relative motion is complicated, and thence the solution of the problem is difficult even assuming a constant property-newtonian liquid Nevertheless, when a small parameter appears m the problem, the complete flow field can be split into zones where simple solutions are found. To illustrate this approach, the spin up from rest of an initially cylindrical floating zone is considered with detail. Here the small parameter is the time elapsed from the impulsive starting of motion. Since the problem which has been considered, as well as some others which can be tackled by use of similar methods, concern the viscous layer close to either plate, they can be simulated experimentally in the ground laboratory with short floating zones. Procedures to produce these zones are indicated.

Impulsive motions of the floating zone

A set of problems concerning the behaviour of a suddenly disturbed ideal floating zone is considered. Mathematical techniques of asymptotic expansions arc used to solve these problems. It is seen that many already available solutions, most of them concerning liquids enclosed in cavities, will be regarded as starting approximations which are valid except in the proximity of the free surface which laterally bounds the floating zone. In particular, the problem of the linear spin-up of an initially cylindrical floating zone is considered in some detail. The presence of a recircuiating fluid pattern near the free surface is detected. This configuration is attributed to the interplay between Coriolis forces and the azimuthal component of the viscous forces.

Floating zone stability

The present state of de preparation of an experiment on floating liquid zones to be performed in the first Spacelab flight is presented. In this experiment,a liquid bridge is to be placed between two parallel coaxial disks (in the Fluid Physics Module)and subjected to very precise disturbances in order to check the theoretical predictions about its stability limits and behavior under mechanical inputs: stretching of the zone, filling or removing the liquid,axial vibration, rotation, disalignment, etc. Several aspects of the research are introduced:1) Relevance of the study. 2) Theoretical predictions of the liquid behavior regarding the floating-zone stability limits and the expected response to vibrational and rotational disturbances. 3) Ground support experiments using the Plateau technique or the small scale simulation. 4) Instrumental aspects of the experimentation: the Fluid Physics Module utilization and post-flight data analysis.5)Research program for future flights.

Mechanical properties up to 1900 K of Al2O3/Er3Al5O12/ZrO2 eutectic ceramics grown by the laser floating zone method

Directionally solidified Al2O3–Er3Al5O12–ZrO2 eutectic rods were processed using the laser floating zone method at growth rates of 25, 350and 750 mm/h to obtain microstructures with different domain size. The mechanical properties were investigated as a function of the processing rate. The hardness, 15.6 GPa, and the fracture toughness, 4 MPa m1/2, obtained from Vickers indentation at room temperature were practically independent of the size of the eutectic phases. However, the flexural strength increased as the domain size decreased, reaching outstanding strength values close to 3 GPa in the samples grown at 750 mm/h. A high retention of the flexural strength was observed up to 1500 K in the materials processed at 25 and 350 mm/h, while superplastic behaviour was observed at 1700 K in the eutectic rods solidified at the highest rate of 750 mm/h

Hydrostatic instabilities in floating zone cristal growth process

If only Fluid Mechanics aspects are considered, the configuration appearing in the floating zone technique for crystal growth can be modelled as a mass of liquid spanning between two solid rods. Besides, if now the influence of temperature gradients and heat flow are not considered, the simplest fluid model consists of an isothermal liquid mass of constant properties (density and surface tension) held by capillary forces between two solid disks placed a distance L apart: the so called liquid bridge. As it is well known, if both supporting disks were parallel, coaxial and of the same diameter, 2R, the volume of liquid, V, were equal to that of a cylinder of the same L and R (V=KR~L) and no body forces were acting on the liquid column, the fluid configuration (under these conditions of cylindrical shape) will become unstable when the distance between the disks equals the length of the circumference of the supporting disks (L=2KR, the so-called Rayleigh stability limit). One should be aware that the Rayleigh stability limit can be dramatically modified when the geometry differs from the above described cylinder (due to having non-coaxial disks, different diameter disks, liquid volume different from the cylindrical one, etc) or when other external effects like accelerations either axial or lateral are considered. In this paper the stability limits of liquid bridges considering different types of perturbations are reviewed.

Superplastic deformation of directionally solidified nanofibrillar Al2O3-Y3Al5O12-ZrO2 eutectics

Nanofibrillar Al2O3–Y3Al5O12–ZrO2 eutectic rods were manufactured by directional solidification from the melt at high growth rates in an inert atmosphere using the laser-heated floating zone method. Under conditions of cooperative growth, the ternary eutectic presented a homogeneous microstructure, formed by bundles of single-crystal c-oriented Al2O3 and Y3Al5O12 (YAG) whiskers of ≈100 nm in width with smaller Y2O3-doped ZrO2 (YSZ) whiskers between them. Owing to the anisotropic fibrillar microstructure, Al2O3–YAG–YSZ ternary eutectics present high strength and toughness at ambient temperature while they exhibit superplastic behavior at 1600 K and above. Careful examination of the deformed samples by transmission electron microscopy did not show any evidence of dislocation activity and superplastic deformation was attributed to mass-transport by diffusion within the nanometric domains. This combination of high strength and toughness at ambient temperature together with the ability to support large deformations without failure above 1600 K is unique and shows a large potential to develop new structural materials for very high temperature structural applications.

Estabilidad de puentes líquidos bajo el efecto de una rotación no axilsimétrica

El estudio de la influencia de perturbaciones de distinta naturaleza en configuraciones de puentes líquidos apoyados en dos discos coaxiales en rotación encuentra una importante motivación en el uso de dicha configuración en la fabricación de cristales semiconductores ultra-puros por la denominada técnica de zona flotante, en la que la rotación de los discos se utiliza para alcanzar temperaturas uniformes. El presente estudio muestra los resultados obtenidos mediante la aplicación de un método numérico en el análisis de la estabilidad de puentes líquidos en isorrotación sometidos al efecto de una fuerza axial uniforme (gravedad axial) y una excentricidad entre el eje de giro y el eje de los discos. Se analiza el efecto de la aplicación de estos factores tanto de forma conjunta como por separado. Aunque existen numerosos estudios previos sobre puentes líquidos sometidos a diversos efectos, el análisis del efecto combinado de la rotación con excentricidad y gravedad axial no ha sido realizado con anterioridad. Este estudio permite además entender los resultados del experimento a bordo de la misión TEXUS-23, en el que un puente líquido sujeto entre dos discos circulares y coaxiales es sometido al efecto de una rotación creciente en torno a un eje desplazado respecto al eje de los discos. Aunque en el experimento no se impone una fuerza axial controlada, la desestabilización y rotura del puente se produce de forma notablemente asimétrica, lo que no puede ser explicado con los estudios precedentes y sugiere una posible presencia de una aceleración axial residual. Se ha desarrollado por tanto un método de análisis de imágenes que permite comparar las formas obtenidas en el experimento con las calculadas numéricamente. En este estudio se muestran los detalles del procesado realizado en las imágenes de la misión TEXUS-23, y los resultados de su comparación con el análisis numérico, que permiten determinar el valor de la gravedad axial que mejor reproduce los resultados del experimento. Estos resultados ponen de manifiesto la importancia del conocimiento y la modelización de efectos cuya presencia (intencionada o no) afectan de forma visible a la estabilidad y la morfología de los puentes líquidos. ABSTRACT The study of the influence of various disturbances in configurations consisting of a liquid bridge supported by two co-axial disks in rotation has an important motivation in the use of this configuration in the fabrication of ultrapure semiconductor crystals via the so-called floating zone technique, in which the rotation of the disks is used to achieve a uniform temperature field. The present study shows the results obtained through the application of a numerical method in the analysis of the stability of liquid bridges in isorotation under the effect of a uniform axial force field (axial gravity) and an offset between the rotation axis and the axis of the supporting disks (eccentricity). The analysis studies the effect of both the combined and separate application of these factors. Although there are numerous studies on liquid bridges subject to various effects, the analysis of the combined effect of rotation with eccentricity and axial gravity has not been done before. Furthermore, this study allows us to understand the results from the experiment aboard the TEXUS-23 mission, in which a liquid bridge supported between two circular-shaped, co-axial disks is subject to the effect of an increasing rotation around an axis with an offset with respect to the axis of the disks. Although the experiment conditions do not include a controlled axial force field, the instability and breakage of the bridge occurs with a marked asymmetry, which cannot be explained by previous studies and suggests the possible presence of a residual axial gravity. Therefore, an image analysis method has been developed which allows to compare the shapes obtained in the experiment with those calculated with the numerical method. This study shows the details of the processing performed on the images from the TEXUS-23 mission and the results from their comparison with the numerical analysis, which allow to determine the axial gravity value which best recovers the experimental results. These results highlight the importance of the understanding and modelling of effects which, when present (intentionally or not), noticeably affect the stability and shape of the liquid bridges.