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At least 163 records · Page 9

Laboratory Reproduction and Failure Analysis of Cracked Orbiter Reaction Control System Niobium Thruster Injectors

A viewgraph presentation describing cracks and failure analysis of an orbiter reaction control system is shown. The topics include: 1) Endeavour STS-113 Landing; 2) RCS Thruster; 3) Thruster Cross-Section; 4) RCS Injector; 5) RCS Thruster, S/N 120l 6) Counterbore Cracks; 7) Relief Radius Cracks; 8) RCS Thruster Cracking History; 9) Thruster Manufacturing Timelines; 10) Laboratory Reproduction of Injector Cracking; 11) The Brownfield Specimen; 12) HF EtchantTests/Specimen Loading; 13) Specimen #3 HF + 600F; 14) Specimen #3 IG Fracture; 15) Specimen #5 HF + 600F; 16) Specimen #5 Popcorn ; 17) Specimen #5 Cleaned and Bent; 18) HF Exposure Test Matrix; 19) Krytox143AC Tests; 20) KrytoxTests/Specimen Loading; 21) Specimen #13 Krytox + 600F; and 22) KrytoxExposure Test Matrix.

Jacobs, Jeremy B.↗

Metallographic Preparation of Space Shuttle Reaction Control System Thruster Electron Beam Welds for Electron Backscatter Diffraction

A Space Shuttle Reaction Control System (RCS) thruster failed during a firing test at the NASA White Sands Test Facility (WSTF), Las Cruces, New Mexico. The firing test was being conducted to investigate a previous electrical malfunction. A number of cracks were found associated with the fuel closure plate/injector assembly (Fig 1). The firing test failure generated a flight constraint to the launch of STS-133. A team comprised of several NASA centers and other research institutes was assembled to investigate and determine the root cause of the failure. The JSC Materials Evaluation Laboratory was asked to compare and characterize the outboard circumferential electron beam (EB) weld between the fuel closure plate (Titanium 6Al-4V) and the injector (Niobium C-103 alloy) of four different RCS thrusters, including the failed RCS thruster. Several metallographic challenges in grinding/polishing, and particularly in etching were encountered because of the differences in hardness, ductility, and chemical resistance between the two alloys and the bimetallic weld. Segments from each thruster were sectioned from the outboard weld. The segments were hot-compression mounted using a conductive, carbon-filled epoxy. A grinding/polishing procedure for titanium alloys was used [1]. This procedure worked well on the titanium; but a thin, disturbed layer was visible on the niobium surface by means of polarized light. Once polished, each sample was micrographed using bright field, differential interference contrast optical microscopy, and scanning electron microscopy (SEM) using a backscatter electron (BSE) detector. No typical weld anomalies were observed in any of the cross sections. However, areas of large atomic contrast were clearly visible in the weld nugget, particularly along fusion line interfaces between the titanium and the niobium. This prompted the need to better understand the chemistry and microstructure of the weld (Fig 2). Energy Dispersive X-Ray Spectroscopy (EDS) was used to confirm the chemical composition of the variations in contrast in these areas. Niobium alloys generally require exposure to more aggressive chemical reagents than titanium alloys for etching because of niobium s chemical resistance; therefore, the titanium portion of the sample was etched first. A five second immersion in Kroll s reagent revealed a general microstructure on the titanium portion of the sample; however, the titanium heat affected zone closest to the weld, was over-etched due to higher concentrations of refined grains and an increase in eta-phase. The Kroll s etchant also revealed some microstructure in the weld nugget itself; the niobium portion of the sample remained unetched.

Martinez, James↗

The design and evaluation of superconducting connectors

The development of a superconducting connector for superconducting circuits on space flights is described. It is proposed that such connectors be used between the superconducting readout loop and the SQUID magnetometer in the Gravity Probe B experiment. Two types of connectors were developed. One type employs gold plated niobium wires making pressure connections to gold plated niobium pads. Lead-plated beryllium-copper spring contacts can replace the niobium wires. The other type is a rigid solder or weld connection between the niobium wires and the niobium pads. A description of the methods used to produce these connectors is given and their performance analyzed.

Payne, J. E.↗

Nb-1Zr L-PBF In-situ Alloying and Elevated Temperature Mechanical Performance

Nb-1Zr is a readily-fabricable, dispersion-strengthened niobium alloy with improved elevated temperature properties compared to commercially pure niobium. This moderate strength niobium alloy is desirable in thermal management systems for fission power and propulsion applications; however, pre-alloyed spherical feedstock is generally unavailable. Laser powder bed fusion (L-PBF) in-situ alloying of a Nb-1Zr chemistry was performed using a pure niobium feedstock coated with 1 wt% of zirconium-based ceramic compound nano-powders. The additively manufactured material was mechanically tested at elevated temperatures in a controlled environment in the as-built condition. For comparison, traditionally manufactured wrought feedstock was also tested under identical conditions. Examination of the materials’ microstructure and elevated temperature mechanical response aimed to determine the Zr-compound nano-powder addition with the best performance, and the overall feasibility of the in-situ alloying approach.

Niobium-based alloys↗

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.↗

Advanced liquid rockets

A program to substitute iridium coated rhenium for silicide coated niobium in thrust chamber fabrications is reviewed. The life limiting phenomena in each of these material systems is also reviewed. Coating cracking and spalling is not a problem with iridium-coated rhenium as in silicide-coated niobium. Use of the new material system enables an 800 K increase in thruster operating temperature from around 1700 K for niobium to 2500 K for rhenium. Specific impulse iridium-coated rhenium rockets is nominally 20 seconds higher than comparable niobium rockets in the 22 N class and nominally 10 seconds higher in the 440 N class.

Schneider, Steven J.↗

Ac losses in type 2 superconductors

Electrical, and calorimetric measurements on alternating current loss in niobium zirconium, niobium titanium, and niobium stannide superconductors

Di Salvo, F.↗

Low-gravity processing of superconducting compounds

Low gravity conditions can be sustained on earth for several seconds in an evacuated drop tube. Because radiation cooling is most effective at high temperatures, the refractive metals and alloys are prime candidates for free fall solidification. The results of initial experiments on droplet formation, droplet release, critical size and evaporation losses are given. The time required for free fall solidification of different size droplets is calculated. The materials studied were copper, niobium and vanadium, and a niobium-tin alloys. Improvements in purity, composition, homogeneity and stoichiometry are expected during free fall solidification of niobium based alloys which should become evident in an increase in the superconducting transition temperature.

Otto, G. H.↗

Phase transitions in the ordered compound TiAl and in alloys having it as a base

The combined effect of alloying and heat treatment on the order-disorder transition in TiAl of stoichiometric composition was investigated. It is concluded from the data obtained that the TiAl 1 to TiAl 2 transition is a phase transition of the second kind. A phase transition was observed in TiAl of equiatomic composition in the 450-550 C temperature range. The introduction of niobium into the ordered compound TiAl of stoichiometric composition, instead of titanium or aluminum atoms, leads to partial softening. In this case, the effect of niobium atoms on softening of the alloys was greater when the niobium was introduced in place of aluminum atoms.

Zelenkov, I. A.↗

Low-Loss NbTiN Films for THz SIS Mixer Tuning Circuits

Recent results at 1 THz using normal-metal tuning circuits have shown that SIS mixers can work well up to twice the gap frequency of the junction material (niobium). However, the performance at 1 THz is limited by the substantial loss in the normal metal films. For better performance superconducting films with a higher gap frequency than niobium and with low RF loss are needed. Niobium nitride has long been considered a good candidate material, but typical NbN films suffer from high RF loss. To circumvent this problem we are currently investigating the RF loss in NbTiN films, a 15 K Tc compound superconductor, by incorporating them into quasi-optical slot antenna SIS devices.

Kooi, J. W.↗

Coating Thermoelectric Devices To Suppress Sublimation

A technique for suppressing sublimation of key elements from skutterudite compounds in advanced thermoelectric devices has been demonstrated. The essence of the technique is to cover what would otherwise be the exposed skutterudite surface of such a device with a thin, continuous film of a chemically and physically compatible metal. Although similar to other sublimation-suppression techniques, this technique has been specifically tailored for application to skutterudite antimonides. The primary cause of deterioration of most thermoelectric materials is thermal decomposition or sublimation - one or more elements sublime from the hot side of a thermoelectric couple, changing the stoichiometry of the device. Examples of elements that sublime from their respective thermoelectric materials are Ge from SiGe, Te from Pb/Te, and now Sb from skutterudite antimonides. The skutterudite antimonides of primary interest are CoSb3 [electron-donor (n) type] and CeFe(3-x)Co(x)Sb12 [electron-acceptor (p) type]. When these compounds are subjected to typical operating conditions [temperature of 700 C and pressure <10(exp -5) torr (0.0013 Pa)], Sb sublimes from their surfaces, with the result that Sb depletion layers form and advance toward their interiors. As the depletion layer advances in a given device, the change in stoichiometry diminishes the thermal-to-electric conversion efficiency of the device. The problem, then, is to prevent sublimation, or at least reduce it to an acceptably low level. In preparation for an experiment on suppression of sublimation, a specimen of CoSb3 was tightly wrapped in a foil of niobium, which was selected for its chemical stability. In the experiment, the wrapped specimen was heated to a temperature of 700 C in a vacuum of residual pressure <10(exp -5) torr (0.0013 Pa), then cooled and sectioned. Examination of the sectioned specimen revealed that no depletion layer had formed, indicating the niobium foil prevented sublimation of antimony at 700 C. This was a considerable improvement, considering that uncoated CoSb3 had been found to decompose to form the lowest antimonide at the surface at only 600 C. Evidently, because the mean free path of Sb at the given temperature and pressure was of the order of tens of centimeters, any barrier closer than tens of centimeters (as was the niobium foil) would have suppressed transport of Sb vapor, thereby suppressing sublimation of Sb

Sakamoto, Jeffrey↗

The Impact of Standard Semiconductor Fabrication Processes on Polycrystalline Nb Thin Film Surfaces

Polycrystalline superconducting Nb thin films are extensively used for submillimeter and millimeter transmission line applications and, less commonly, used in microwave kinetic inductance detector (MKID) applications. The microwave and mm-wave loss in these films is impacted, in part, by the presence of surface nitrides and oxides. In this study, glancing incidence x-ray diffraction was used to identify the presence of niobium nitride and niobium monoxide surface layers on Nb thin films which had been exposed to chemicals used in standard photolithographic processing. A method of mitigating the presence of ordered niobium monoxide surface layers is presented. Furthermore, we discuss the possibility of using glancing incidence x-ray diffraction as a non-destructive diagnostic tool for evaluating the quality of Nb thin films used in MKIDs and transmission lines. For a given fabrication process, we have both the x-ray diffraction data of the surface chemistry and a measure of the mm-wave and microwave loss, the latter being made in superconducting resonators.

superconducting films↗

The Impact of Standard Semiconductor Fabrication Processes on Polycrystalline Nb Thin Film Surfaces

Polycrystalline Nb thin films are extensively used for microwave kinetic inductance detectors (MKIDs) and superconducting transmission line applications. The microwave and mm-wave loss in these films is impacted, in part, by the presence of surface nitrides and oxides. In this study, glancing incidence x-ray diffraction was used to identify the presence of niobium nitride and niobium monoxide surface layers on Nb thin films which had been exposed to chemicals used in standard photolithographic processing. A method of mitigating the presence of ordered niobium monoxide surface layers is presented. Furthermore, we discuss the possibility of using glancing incidence x-ray diffraction as a non-destructive diagnostic tool for evaluating the quality of Nb thin films used in MKIDs and transmission lines. For a given fabrication process, we have both the X-ray diffraction data of the surface chemistry and a measure of the mm-wave and microwave loss, the latter being made in superconducting resonators.

superconducting films↗

The Impact of Standard Semiconductor Fabrication Processes on Polycrystalline Nb Thin Film Surfaces

Polycrystalline Nb thin films are extensively used for microwave kinetic inductance detectors (MKIDs) and superconducting transmission line applications. The microwave and mm-wave loss in these films is impacted, in part, by the presence of surface nitrides and oxides. In this study, glancing incidence x-ray diffraction was used to identify the presence of niobium nitride and niobium monoxide surface layers on Nb thin films which had been exposed to chemicals used in standard photolithographic processing. A method of mitigating the presence of ordered niobium monoxide surface layers is presented. Furthermore, we discuss the possibility of using glancing incidence x-ray diffraction as a non-destructive diagnostic tool for evaluating the quality of Nb thin films used in MKIDs and transmission lines. For a given fabrication process, we have both the X-ray diffraction data of the surface chemistry and a measure of the mm-wave and microwave loss, the latter being made in superconducting resonators.

superconducting films↗