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Undercooling studies on Nb-Pt and Nb-Si alloys using the 105 meter drop tube

Niobium-platinum samples of compositions ranging from 16 to 32 at. pct have been undercooled to as much as 540 K in the low gravity, containerless environment of a 105 meter drop tube. Undercooling was terminated in the Nb-Pt samples by the nucleation and growth of the Nb3Pt phase. In the 16-18 at. pct Pt samples, this resulted in samples which are completely Nb3Pt, in contrast to both the equilibrium phase diagram and the nonundercooled samples which formed with Nb dendrites and interdendritic Nb3Pt. Undercoolings for the Nb-Si samples were up to 670 K, which corresponds to 27 percent of the liquidus temperature or 80 percent of the estimated hypercooling limit. In the Nb-Si system, a coupled zone was identified as well as a metastable extension of the solubility limit of Si in Nb due to deep undercooling.

Robinson, M. B.↗

Containerless processing and rapid solidification of Nb-Si alloys of hypereutectic composition

A combination of bulk undercooling in an electromagnetic levitation apparatus and splat quenching between two copper plates is used to process Nb-Si alloys in order to maximize rapid solidification conditions and minimize the effects of recalescence, with emphasis on the solidification of characteristics of alloys in the 21 to 27 at. pct Si range of composition. SEM and TEM as well as X-ray diffraction are used to characterize the microstructures of the processed samples. In the range of compositions studied, the splat-quenched drops always formed the tetragonal Nb3Si phase directly from the liquid. Drops solidified in the coil were characterized by the presence of the primary intermetallic Nb5Si3 and the absence of both peritectic Nb3Si and the equilibrium eutectic. In these cases, a metastable alpha-Nb + beta-Nb5Si3 eutectic formed. The results are discussed in terms of possible metastable configurations of the Nb-Si phase diagram as well as concepts of nucleation and growth kinetics applied to the Nb3Si and Nb5Si3 intermetallics.

Hofmeister, W. H.↗

Containerless processing and rapid solidification of Nb-Si alloys in the niobium-rich eutectic range

Containerless processing and rapid solidification techniques were used to process Nb-Si alloys in the Nb-rich eutectic range. Electromagnetically levitated drops were melted and subsequently splat-quenched from different temperatures. A variety of eutectic morphologies was obtained as a function of the degree of superheating or undercooling of the drops prior to splatting. Metallic glass was observed only in drops quenched from above the melting temperature. Microstructures of splats deeply undercooled prior to quenching were very fine and uniform. These results are discussed in terms of classic nucleation theory concepts and the expected heat evolution at different regions of the splat during the rapid quenching process. The locations of the coupled-zone boundaries for the alpha-Nb + Nb3Si eutectic are also suggested.

Hofmeister, W. H.↗

Supercooling effects in faceted eutectic Nb-Si alloys

The effect of melt supercooling on the microstructure of an Nb-58 at. pct Si alloy is investigated experimentally using an electromagnetic levitation apparatus. It is found that, starting with an alloy nominally of eutectic composition, nucleation of Nb5Si3 occurs in the supercooled liquid first. Upon further cooling, the remaining liquid continues to supercool until the second phase, NbSi2 is nucleated, which is commonly accompanied by rapid recalescence. The primary phase exibits a eutectoid-type decomposition. The observations are discussed with reference to the results of quantitative microstructural measurements, compositional and thermal analysis, and preliminary thermodynamic modeling of the phase diagram.

Gokhale, A. B.↗

Rapid solidification of Nb-base alloys

New Nb-base alloys are of interest for aerospace structural applications at high temperatures, viz, 800 to 1650 C. Fundamental information regarding the effects of rapid solidification in achieving greatly refined microstructures, extended solid solubility, suppression of embrittling equilibrium phases, and formation of new phases is desired in a number of Nb-X alloys. The microstructures and selected properties of Nb-Si and other Nb-base alloys are presented for materials both rapidly quenched from the equilibrium liquidus and rapidly solidified following deep supercooling. Electromagnetic levitation was used to achieve melting and supercooling in a containerless inert gas environment. A variety of solidification conditions were employed including splatting or drop casting of supercooled samples. The morphology and composition of phases formed are discussed in terms of both solidification history and bulk composition.

Gokhale, A. B.↗

Containerless processing using electromagnetic levitation

The theory and practice of containerless processing via electromagnetic (EM) levitation is reviewed briefly. The use of EM levitation for the processing of alloys is described with particular emphasis on the bulk melt supercooling phenomenon in a containerless environment. The various effects associated with rapid solidification via bulk melt supercooling are discussed with examples of Nb-Si alloys. It is suggested that a detailed analysis of such effects can be utilized to select the potentially most promising alloys for future space-based processing.

Gokhale, A. B.↗

Low-Loss Microstrip Transmission Line Fabricated with Improved Liftoff Process

The µ-Spec integrated spectrometer operating at ~500 GHz, employs thin film superconducting Nb microstrip transmission lines deposited directly on a thin (450 nm) single-crystal silicon dielectric. This single-crystal silicon layer is chosen as the dielectric layer due to its low intrinsic loss, with the goal of achieving both high- efficiency and precise phase control in a compact spectrometer architecture. To avoid roughening or etching through the thin single-crystal silicon dielectric a liftoff technique was developed for patterning these microstrip transmission lines and ground plane structures. This two- layer liftoff process was designed for use with sputter deposition and resulted in a US patent. Although this original technique provided precise control of linewidth, results of initial prototype spectrometer devices and separate diagnostic co-planer waveguide resonator devices showed that unexpected loss was being introduced due to the lift-off process. This extra loss was believed to be due to the “tails” (thin tapered regions) at the edge of the metal traces resulting from the sputtering process, as well as an amorphous oxide layer at the Nb-Si interface. We have since demonstrated an improved lift-off technique, which provides a clean metal-Si interface and removes the loss-inducing tails by a two-step selective etching method. This results in a decrease in microwave loss by more than an order of magnitude when measured in co-planar waveguide microwave resonator structures. We present these microwave test results and also SEM and TEM images of the microstrip interfaces and edge profiles before and after application of the improved process.

Hess, Larry A.↗