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Rathz, T. J.

Publications and source records attributed to Rathz, T. J..

35 records · Page 2

High Undercooling of Ni59Nb41 Alloy in a Containerless Electrostatic Levitation Facility

Utilizing the containerless electrostatic levitation facility at NASA/MSFC, we were able to undercool the Ni59Nb41 (atomic) alloy by 210 K which was 160 degrees farther than the results of previous flight experiments. Undercoolings were clustered around 200 K during the repeated melting-freezing cycles on a single sample. Prior to this work, a metastable liquid separation had been presumed to limit the undercooling of this alloy. However, microstructural observations have revealed that undercooling was limited by crystal nucleation.

Robinson, M. B.

Containerless, Low-Gravity Undercooling of Ti-Ce Alloys in the MSFC Drop Tube

Previous tests of the classical nucleation theory as applied to liquid-liquid gap miscibility systems found a discrepancy between experiment and theory in the ability to undercool one of the liquids before the L1-L2 separation occurs. To model the initial separation process in a two-phase liquid mixture, different theoretical approaches, such as free-energy gradient and density gradient theories, have been put forth. If there is a large enough interaction between the critical liquid and the crucible, both models predict a wetting temperature (T(sub w)) above which the minority liquid perfectly wets and layers the crucible interface, but only on one side of the immiscibility dome. Materials with compositions on the other side of the dome will have simple surface adsorption by the minority liquid before bulk separation occurs when the coexistence (i.e., binoidal) line in reached. If the interaction between the critical liquid and the crucible were to decrease, T(sub w) would increase, eventually approaching the critical consolute temperature (T(sub cc)). If this situation occurs, then there could be large regions of the miscibility gap where non-perfect wetting conditions prevail resulting in droplets of L1 liquid at the surface having a non-zero contact angle. The resulting bulk structure will then depend on what happens on the surface and the subsequent processing conditions. In the past several decades, many experiments in space have been performed on liquid metal binary immiscible systems for the purpose of determining the effects that different crucibles may have on the wetting and separation process of the liquids. Potard performed experiments that showed different crucible materials could cause the majority phase to preferentially wet the container and thus produce a dispersed microstructure of the minority phase. Several other studies have been performed on immiscibles in a semi-container environment using an emulsion technique. Only one previous study was performed using completely containerless processing of immiscible metals and the results of that investigation are similar to some of the emulsion studies. In all the studies, surface wetting was attributed as the cause for the similar microstructures or the asymmetry in the ability to undercool the liquid below the binoidal on one side of the immiscibility dome. By removing the container completely from the separation process, it was proposed that the loss of the crucible/liquid interaction would produce a large shift in T(sub w) and thus change the wetting characteristics at the surface. By investigating various compositions across the miscibility gap, a change in the type and amount of liquid wetting at the surface of a containerless droplet should change the surface nucleating behavior of the droplet - whether it be the liquid-liquid wetting or the liquid-to-solid transition. Undercooling of the liquid into the metastable region should produce significant differences in the separation process and the microstructure upon solidification. In this study, we attempt to measure these transitions by monitoring the temperature of the sample by optical pyrometry. Microstructural analysis will be made to correlate with the degree of undercooling and the separation mechanisms involved.

Robinson, M. B.

Direct Determination of the Metastable Liquid Miscibility Gap in Undercooled Cu-Co Alloys

Bulk Cu-Co alloys at compositions ranging from 10 to 80 wt pct Co were highly undercooled using a melt fluxing technique. The metastable liquid separation boundary has been directly determined from the measured temperature-time profiles. It was found that the critical point of the miscibility gap is slightly shifted towards the Co side and about 90 K below the liquidus. A droplet-shaped microstructure was observed for all solidified specimens (Cu- 10 to 80 wt pct Co), when the melts were undercooled into the metastable miscibility boundary.

Li, D.

Metastable Demixing of Supercooled Cu-Co and Cu-Fe Alloys in an Oxide Flux

A systematic study on the liquid separation in supercooled Cu-Co and Cu-Fe alloys was performed using a melt fluxing which permits high supercooling to be achieved. Moreover, this method renders it possible to directly measure binodal temperatures and establish metastable liquid miscibility gap (LMG). All phase-separated samples at compositions ranging from 10 to 80 wt pct Co or to 83 wt pct Fe were found to exhibit droplet-shaped morphologies, in spite of various droplet distributions. Uniformly dispersed microstructures were obtained as the minority component was less than 20 vol.%; while beyond this percentage, serious coarsening was brought about. Calculations of the miscibility gap in the Cu-Co system and Stokes movement velocity of Co and Fe droplets in Cu matrix were made to analyze the experimental results.

Li, D.

Liquidus Temperatures and Solidification Behavior in the Copper-Niobium System

The copper-niobium phase diagram has been under active debate; thus, a corroboratory experimental study is needed. In this investigation, the melts of Cu-Nb alloys at compositions ranging from 5 lo 86 wt% Nb were processed in different environments and solidified at relatively low rates of 50-75 C/s to determine liquidus temperatures and to study solidification behavior. For all samples processed under very clean conditions, only Nb dendrites in a Cu matrix were observed; while in the presents of oxygen impurities, the alloys containing 5-35 wt% Nb exhibited microstructure of Nb-rich spheroids and Nb dendrites in the Cu matrix. The results obtained from clean conditions are in fair agreement with the Cu-Nb phase diagram having an S-shaped, near-horizontal appearances of the liquidus. The formation of Nb-rich droplets at slow cooling rates is discussed in terms of a stable liquid miscibility gap induced by oxygen.

Li, D.

Liquidus Temperatures and Solidification Behavior in the Copper-Niobium System

The copper-niobium phase diagram has been under active debate; thus, a corroboratory experimental study is needed. In this investigation, the melts of Cu-Nb alloys at compositions ranging from 5 to 86 wt pct Nb were processed in different environments and solidified at relatively low cooling rates of 50 to 75 C/s to determine liquidus temperatures and to study solidification behavior. For all samples processed under very clean conditions, only Nb dendrites in a Cu matrix were observed; while in the presence of oxygen impurities the alloys containing 5 to 35 wt pct Nb exhibited microstructure of Nb-rich spheroids and Nb dendrites in the Cu matrix. The results obtained from clean conditions are in fair agreement with the Cu-Nb phase diagram having an S-shaped, near-horizontal appearance of the liquidus. The formation of Nb- rich droplets at slow cooling rates is discussed in terms of a stable liquid miscibility gap induced by oxygen.

Li, D.

On the Cu-Nb Phase Diagram and Solidified Microstructures

Container and containerless processing was employed to determine liquidus temperatures and to examine microstructural development in the Cu-Nb system. The Cu-Nb phase diagram of an S-shaped, near-horizontal liquidus, has been confirmed by both the temperature-time profiles and resultant microstructures with only Nb dendrites in a Cu matrix, which were obtained from crucible experiments under clean conditions. However, the microstructural pathways of Cu-Nb alloys are particularly sensitive to processing variables. By the addition of oxygen impurities or rapid solidification, droplet-shaped morphology was observed for some compositions, implying occurrence of a liquid-phase separation. The effects of impurities and cooling rates are analyzed in connection with a stable and metastable liquid miscibility gap, respectively.

Li, D.

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.

Tolerance requirements to prevent fluid leakage in the crucible/plunger MEA experiment MPS 770030

Molten Al-In leaked unexpectedly out of the crucible of a proposed MEA materials processing in space experiment. The molten metals use a spring loaded plunger to eliminate most free surfaces. The critical criteria necessary to initiate flow and the rate of fluid flow into the crucible/plunger annulus is calculated. Experimental in situ X-radiographs are interpreted according to the calculations. A note on possible effects of capillary flow if wetting occurs between crucible/plunger and liquids is included.

Rathz, T. J.

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.

Susceptibility measurements on the superconducting properties of Nb-Ge alloys

A susceptibility apparatus to measure superconducting properties of samples made in the MSFC Drop Tube was used to measure the transition temperature (Tc) and susceptibilities of Nb and Nb Ge Alloys prepared in bulk spherical (2-4 mm diameter) form using a 32 m drop tube in which containerless low gravity solidification could take place. Results indicate that a drop tube processing environment was beneficial for increasing the Tc of the superconducting phase of the material over that of arc melted material. The increase in Tc is found to be related to the amount of solidification of the total sample that took place before reaching the bottom of the drop tube. In phase and quadrature phase measurements of the specimen's susceptibility indicated that some improvement in homogeneity takes place in drop tube processing. These phase measurements also indicated little or no shielding of a lower Tc phase by a higher Tc filamentary structure.

Rathz, T. J.

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.

Interactive data-processing system for metallurgy

Equipment indicates that system can rapidly and accurately process metallurgical and materials-processing data for wide range of applications. Advantages include increase in contract between areas on image, ability to analyze images via operator-written programs, and space available for storing images.

Rathz, T. J.

The application of digital techniques to the analysis of metallurgical experiments

The application of a specific digital computer system (known as the Image Data Processing System) to the analysis of three NASA-sponsored metallurgical experiments is discussed in some detail. The basic hardware and software components of the Image Data Processing System are presented. Many figures are presented in the discussion of each experimental analysis in an attempt to show the accuracy and speed that the Image Data Processing System affords in analyzing photographic images dealing with metallurgy, and in particular with material processing.

Rathz, T. J.