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Robinson, M. B.

Publications and source records attributed to Robinson, M. B..

50 records · Page 3

Microstructures of niobium-germanium alloys processed in inert gas in the 100 meter drop tube

The 100 meter drop tube at NASA's Marshall Space Flight Center has been used for a series of experiments with niobium-germanium alloys. These experiments were conducted with electromagnetic levitation melting in a 200 torr helium environment. Liquid alloys experienced large degrees of undercooling prior to solidification in the drop tube. Several interesting metastable structures were observed. However, the recalescence event prevented extended solid solubility of germanium in the A-15 beta phase. Liquids of eutectic composition were found to undercool in the presence of solid alpha and solid Nb5Ge3.

Bayuzick, R. J.↗

Solidification of Nb-Ge alloys in long drop tubes

The 30-m and 100 m-long drop tubes at the Marshall Space Flight Center have been used to obtain large undercooling in Nb-Ge alloys. Electron beam melting has been used to obtain drops approximately 2.5 mm in diam. In the 30-m tube, many specimens fell the length of the tube without solidifying, and were ultimately liquid-quenched in oil. The amount of undercooling prior to the quench was usually around 0.13 T(m). In the 100-m tube, freezing generally initiated during free fall, and the maximum undercooling was around 0.22 T(m). Microstructures were characterized by a combination of X-ray diffraction, optical microscopy, and scanning electron microscopy with energy dispersive analysis by X-rays. A variety of interesting microstructures was observed.

Bayuzick, R. J.↗

High-temperature containerless calorimeter

A high-temperature (greater than 1500 K) containerless calorimeter is described and its usefulness demonstrated. The calorimeter uses the technique of omnidirectional electron bombardment of pendant drops to achieve an isothermal test environment. The small heat input into the sample (i.e., 15-50 W) can be controlled and measured. The apparatus can be used to determine the total hemispherical emissivity, specific heat, heat of fusion, surface tension, and equilibrium melting temperature of small molten drops in the temperature range of 1500 to 3500 K. The total hemispherical emissivity and specific heat of pure niobium and two alloys of niobium-germanium have been measured in the temperature range of 1700 to 2400 K. As reported in the literature, the total hemispherical emissivity varied as a function of temperature. However, specific heat values for both the pure metal and alloys seem to be independent of temperature. Specific heat for the liquid alloy phase was also measured and compared to the solid phase.

Robinson, M. B.↗

Undercooling of niobium-germanium alloys in a 100 meter drop tube

The undercoolings of pure Nb and Nb-Ge alloys are examined using the 100-m drop tube of the Marshall Space Flight Center. The temperatures of the samples prior to release were measured, and IR detectors were utilized to monitor recalescence from solidification. It is observed that the Nb and Nb-Ge samples undercooled to the homogeneous nucleation limit. The data reveal that all the samples displayed a dendritic primary phase, except for alloys nucleating in the beta-phase field, which had a cellular phase. The composition of these phases are studied using EDXA; it is detected that the composition of the phases corresponds to the Jorda (1978) phase diagram.

Hofmeister, W. H.↗

Microgravity containerless processing in long drop tubes

Extensive experience in utilizing long drop tubes for studying effects of microgravity on the solidification of alloys was obtained. While some modifications are necessary to improve versatility, the facility proved to be most useful. Both an electron beam furnace and an electromagnetic levitation furnace can be used. The electron beam furnace is used with vacuum environments (0.00001 torr), whereas the levitation furnace is presently used only in inert gas environments (above 100 torr). Experiments are best applied to refractory alloys because of the sensitivity of the detectors now being used to observe solidification. Processing of lower melting point metals and alloys simply cannot be recorded. On the other hand, expected improvements in detector sensitivity will allow experimentation with relatively low melting alloys. In such cases, solidification will occur in flight only if higher inert gas pressure is used (100 to 760 torr) to increase heat loss by convection. Under these conditions microgravity conditions no longer apply. However, as shown by results to date, it is not microgravity as such that is important in drop tube solidification. Instead it is the containerless nature of the process that is significant, leading to large degrees of undercooling before solidification and therefore to unique alloys.

Bayuzick, R. J.↗

A review of long drop tubes as a supplement/alternative to space experiments

A description of the 100-m drop tube at the Marshall Space Flight Center is presented, along with some undercooling observations and a discussion of some microstructural properties of deeply undercooled Nb-Ge alloys. The facility comprises two turbopumps which can evacuate the tube to 0.00001 torr, and three IR detectors at 15, 80, and 103-m levels which are sensitive to light in the range of 9660-2635 K (wavelength range of 0.2 to 1.1 microns), though recalescence events were detected at 1700 K. Finally, hypercooling regimes and maximum possible undercooling in vacuum are defined for several materials, including Al, Cu, Ni, Fe, Pt, and Nb.

Bayuzick, R. J.↗

Method and apparatus for supercooling and solidifying substances

An enclosure provides a containerless environment in which a sample specimen is positioned. The specimen is heated in the containerless environment, and the specimen melt is dropped through the tube in which it cools by radiation. The tube is alternatively backfilled with an inert gas whereby the specimen melt cools by both radiation and convection during its free fall. During the free fall, the sample is in a containerless, low-gravity environment which enhances supercooling in the sample and prevents sedimentation and thermal convection influences. The sample continues to supercool until nucleation occurs which is detected by silicon photovoltaic detectors. The sample solidifies after nucleation and becomes completely solid before entering the detachable catcher. The amount of supercooling of the specimen can be measured by knowing the cooling ratio and determining the time for nucleation to occur.

Lacy, L. L.↗

Containerless undercooling and solidification of bulk metastable Nb3Ge alloys

Experiments using containerless undercooling and low-gravity solidification of Nb(1-x)Ge(x) alloys for x=0.13-0.27 have been carried out in a 32-m drop-tube apparatus to study the feasibility of forming metastable Nb3Ge in bulk form. It is found that bulk samples (2-3 mm diam) of Nb-Ge alloys with 18-22% Ge can be undercooled by large amounts (300-500 K) and solidified in a containerless environment. Subsequent quenching of the solidified samples in oil helps preserve the metastable A-15 phase by removing the latent heat of fusion and quickly cooling the samples to a stable temperature below 1000 C. Even at an undercooling of less than 100 K, the superconducting transition temperature of the material is enhanced over the cast material by about 1 K.

Lacy, L. L.↗

Solidification studies of Nb-Ge alloys at large degrees of supercooling

A 32 meter evacuated drop tube has been used to investigate the solidification of Nb-Ge alloys after deep undercooling. Samples have been supercooled as much as 500 K below the liquidus by using free-fall conditions to eliminate crucible induced nucleation. Final microstructures are dependent on the quenching rates at the bottom of the drop tube with a striking extension of the beta phase solubility limit at the higher quenching rates.

Lacy, L. L.↗

Undercooling measurement in a low-gravity containerless environment

A technique is described for measuring the amount of undercooling for samples processed in a low-gravity containerless environment. The time of undercooling is determined by measuring the time of cooling before nucleation and recalescence by two infrared detectors. Once the cooling curve for each drop is calculated, the amount of undercooling can then be found. The technique is demonstrated by measuring the amount of undercooling for drops of pure niobium and select compositions of the niobium-germanium alloy system while free falling in a 32 n evacuated drop tube. The total hemispherical emissivities and specific heats for these materials were measured using a high-temperature containerless calorimeter. An overview of the effect of undercooling on drops of niobium and niobium-germanium is given.

Robinson, M. B.↗

Containerless undercooling and solidification in drop tubes

A containerless low-gravity environment, produced within a 32 m drop tube apparatus, has been used to undercool and solidify metals, alloys or glasses by eliminating crucible induced nucleation processes. Niobium droplets with diameters in the range of 2 to 5 mm have been undercooled by 525 K which corresponds to the maximum undercooling reported by Turnbull and others on fine dispersions of low melting point metals. Solidification at large undercooling resulted in single crystalline spheres with the formation of interdendritic shrinkage channels on the sample surface rather than interior shrinkage cavities. The grain refinement as observed for Ni samples undercooled and solidified in fused silica crucibles does not occur in free-falling drops of Nb. A calculated solidification speed of undercooled Nb is compared to Ni. A solidification speed of 320 m/s is found for the Nb drops. This solidification speed is greater than or comparable to the solidification speeds calculated in splat cooled samples. Thus, a drop tube apparatus can be useful in the preparation and study of high temperature metastable compounds or alloys in bulk form.

Lacy, L. L.↗

Containerless materials processing in the laboratory

Drop tube makes possible preparation of exotic materials. The 100 foot tube is oriented precisely vertical to prevent free-falling drop from hitting tube walls. Inert-gas supply, evacuation pumps, viewing ports, and flexibility in choice of melt technique allow precise control and monitoring of solidification.

Lacy, L. L.↗

Containerless high-temperature calorimeter

Samples are heated by electron bombardment in high-temperature calorimeter that operates from 1,000 to 3,600 C yet consumes less that 100 watts at temperatures less than 2,500 C. Contamination of samples is kept to minimum by suspending them from wire in vacuum chamber. Various sample slopes such as wires, dishs, spheres, rods, or irregular bodies can be accommodated and only about 100 nq of samples are needed for accurate measurements.

Lacy, L. L.↗

Radiative and gas cooling of falling molten drops

The supercooling rate and solidification time for molten drops of niobium, copper, and lead are calculated. Calculations for both radiation and helium gas cooling are presented in order to estimate the influence that the presence of helium gas would have upon the cooling rate of falling drops in the Marshall Space Flight Center space processing drop tube.

Robinson, M. B.↗