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NASA NTRS1999

Macrosegregation of GeSi Alloys Grown in a Static Magnetic Field

Axial and radial macrosegregation profiles have been determined for GeSi alloy crystals grown by the vertical Bridgman technique. An axial 5 Tesla magnetic field was applied to several samples during growth to decrease the melt velocities by means of the Lorentz force. Compositions were measured with either energy dispersive X-ray spectroscopy (EDS) on a scanning electron microscope (SEM) or by wavelength dispersive X-ray spectroscopy (WDS) on a microprobe. The crystals were processed in graphite, hot-pressed boron nitride (BN), and pyrolytic boron nitride (PBN) ampoules, which produced various solid-liquid interface shapes during solidification. Those samples grown in a graphite ampoule exhibited radial profiles consistent with a highly concave interface and axial profiles indicative of complete mixing in the melt. The samples grown in BN and PBN ampoules had less radial variation. Axial macrosegregation profiles of these samples fell between the predictions for a completely mixed melt and one where solute transport is dominated by diffusion. Possible explanations for the apparent insufficiency of the magnetic field to achieve diffusion controlled growth conditions are discussed.

Ritter, T. M.↗

NASA NTRS1987

Superplastic forming/weld-brazing of Ti-6Al-4V panels for enhanced structural efficiency

An account is given of the results obtained by NASA-sponsored studies which exploit the processing advantages of superplastic forming (SPF) and joining by weld-brazing (WB) for the fabrication of Ti-alloy skin-stiffened structural components. The buckling strengths of panels with stiffeners having the geometry of a conventional hat shape are compared with those of panels having advanced-geometry stiffereners. Both single- and multiple-stiffened panels have been evaluated at room temperature; the SPF/WB panels with advanced-geometry stiffeners developed up to 60-percent higher buckling strength than panels with conventional-geometry stiffeners. Selective stiffener reinforcement with a boron-reinforced Al-matrix MMC was also evaluated.

Royster, Dick M.↗

NASA NTRS2003

Reduction of Defects in Germanium-Silicon

Crystals grown without contact with a container have far superior quality to otherwise similar crystals grown in direct contact with a container. In addition to float-zone processing, detached- Bridgman growth is a promising tool to improve crystal quality, without the limitations of float zoning or the defects introduced by normal Bridgman growth. Goals of this project include the development of the detached Bridgman process to be reproducible and well understood and to quantitatively compare the defect and impurity levels in crystals grown by these three methods. Germanium (Ge) and germanium-silicon (Ge-Si) alloys are being used. At MSFC, we are responsible for the detached Bridgman experiments intended to differentiate among proposed mechanisms of detachment, and to confirm or refine our understanding of detachment. Because the contact angle is critical to determining the conditions for detachment, the sessile drop method was used to measure the contact angles as a function of temperature and composition for a large number of substrates made of potential ampoule materials. Growth experiments have used pyrolytic boron nitride (pBN) and fused silica ampoules with the majority of the detached results occurring predictably in the pBN. Etch pit density (EPD) measurements of normal and detached Bridgman-grown Ge samples show a two order of magnitude improvement in the detached-grown samples. The nature and extent of detachment is determined by using profilometry in conjunction with optical and electron microscopy. The stability of detachment has been analyzed, and an empirical model for the conditions necessary to achieve sufficient stability to maintain detached growth for extended periods has been developed. We have investigated the effects on detachment of ampoule material, pressure difference above and below the melt, and Si concentration; samples that are nearly completely detached can be grown repeatedly in pBN. Current work is concentrated on developing a method to make in situ pressure measurements in the growth ampoules.

Source record↗

NASA NTRS1973

Development of ductile high-strength chromium alloys, phase 2

Strength and ductility were evaluated for chromium alloys dispersion hardened with the putative TaC, TaB, CbC, and CbB compounds. TaC and TaB proved to be the most potent strengtheners, but when combined, their effect far outweighed that produced individually. Tests at 1422 K (2100 F) on an alloy containing these two compounds at the combined level of 0.5 m/o revealed a 495 MN/sq m (70 ksi) tensile strength for wrought material, and a 100 hour rupture strength of 208 MN/sq m (30 ksi) when solution annealed and aged to maximize creep resistance. These levels of high temperature strength greatly exceed that reported for any other chromium-base alloy. The ductile-to-brittle transition temperature (DBTT) of the two phase strengthened alloy occurred at approximately 588 K (600 F) when heat treated to optimize creep strength and was not improved by fabrication to produce a wrought and recovered microstructure. The lowest DBTT measured on any of the alloys investigated was 422 K (300 F). Strengthening phases actually formed in Cr-Ta-B and Cr-Cb-B compositions are probable M2CrB2 (M=Ta or Cb) compounds of tetragonal crystal structure. The likely habit relationship between these compounds and chromium is postulated. Cube habit coherency was identified for TaC precipitation in chromium by electron microscopy. In another study, the maximum solubility of carbon in chromium was indicated to lie between 3/4 and 1 a/o and that of boron to be 1/2 a/o.

Filippi, A. M.↗

NASA NTRS1987

Materials for Advanced Turbine Engines (MATE). Project 4: Erosion resistant compressor airfoil coating

The ability of coatings to provide at least a 2X improvement in particulate erosion resistance for steel, nickel and titanium compressor airfoils was identified and demonstrated. Coating materials evaluated included plasma sprayed cobalt tungsten carbide, nickel carbide and diffusion applied chromium plus boron. Several processing parameters for plasma spray processing and diffusion coating were evaluated to identify coating systems having the most potential for providing airfoil erosion resistance. Based on laboratory results and analytical evaluations, selected coating systems were applied to gas turbine blades and evaluated for surface finish, burner rig erosion resistance and effect on high cycle fatigue strength. Based on these tests, the following coatings were recommended for engine testing: Gator-Gard plasma spray 88WC-12Co on titanium alloy airfoils, plasma spray 83WC-17Co on steel and nickel alloy airfoils, and Cr+B on nickel alloy airfoils.

Rashid, J. M.↗

NASA NTRS2002

Detached Bridgman Growth of Germanium and Germanium-Silicon Alloy Crystals

Earth based experiments on the science of detached crystal growth are being conducted on germanium and germanium-silicon alloys (2 at% Si average composition) in preparation for a series of experiments aboard the International Space Station (ISS). The purpose of the microgravity experiments includes differentiating among proposed mechanisms contributing to detachment, and confirming or refining our understanding of the detachment mechanism. Because large contact angle are critical to detachment, sessile drop measurements were used to determine the contact angles as a function of temperature and composition for a large number of substrates made of potential ampoule materials. Growth experiments have used pyrolytic boron nitride (pBN) and fused silica ampoules with the majority of the detached results occurring predictably in the pBN. The contact angles were 173 deg (Ge) and 165 deg (GeSi) for pBN. For fused silica, the contact angle decreases from 150 deg to an equilibrium value of 117 deg (Ge) or from 129 deg to an equilibrium value of 100 deg (GeSi) over the duration of the experiment. The nature and extent of detachment is determined by using profilometry in conjunction with optical and electron microscopy. The stability of detachment has been analyzed, and an empirical model for the conditions necessary to achieve sufficient stability to maintain detached growth for extended periods has been developed. Results in this presentation will show that we have established the effects on detachment of ampoule material, pressure difference above and below the melt, and silicon concentration; samples that are nearly completely detached can be grown repeatedly in pBN.

Szofran, F. R.↗

NASA NTRS1978

Trends and techniques for space base electronics

A system was developed for depositing aluminum and aluminum alloys by the D.C. sputtering technique. This system which was designed for a high level of cleanliness and ion monitoring the deposition parameters during film preparation is ready for studying the deposition and annealing parameters upon double level metal preparation. The finite element method was studied for use in the computer modeling of two dimensional MOS transistor structures. An algorithm was developed for implementing a computer study which is based upon the finite difference method. The program was modified and used to calculate redistribution data for boron and phosphorous which had been predeposited by ion implantation with range and straggle conditions typical of those used at MSFC. Data were generated for 111 oriented SOS films with redistribution in N2, dry O2 and steam ambients. Data are given showing both two dimensional effects and the evolution of the junction depth, sheet resistance and integrated dose with redistribution time.

Gassaway, J. D.↗

NASA NTRS2001

Detached Bridgman Growth of Germanium and Germanium-Silicon Alloy Crystals

Earth based experiments on the science of detached crystal growth are being conducted on germanium and germanium-silicon alloys (2at% Si average composition) in preparation for a series of experiments aboard the International Space Station (ISS) to differentiate among proposed mechanisms contributing to detachment. Sessile drop measurements were first carried out for a large number of substrates made of potential ampoule materials to determine the contact angles and the surface tension as a function of temperature and composition. The process atmosphere and duration of the experiment (for some cases) were also found to have significant influence on the wetting angle. Growth experiments have used pyrolytic boron nitride (pBN) and fused silica ampoules with the majority of the detached results occurring predictably in the pBN. The contact angles were 173 deg (Ge) and 165 deg (GeSi) for pBN. For fused silica, the contact angle decreases to an equilibrium value with duration of measurement ranging from 150 to 117 deg (Ge), 129 to 100 deg (GeSi). Forming gas (Ar + 2% H2) and vacuum have been used in the growth ampoules. With gas in the ampoule, a variation of the temperature profile during growth has been used to control the pressure difference between the top of the melt and the volume below the melt caused by detachment of the growing crystal. The stability of detachment has been modeled and substantial insight has been gained into the reasons that detachment has most often been observed in reduced gravity but nonetheless has occurred randomly even there. An empirical model for the conditions necessary to achieve sufficient stability to maintain detached growth for extended periods has been developed and will be presented. Methods for determining the nature and extent of detachment include profilometry and optical and electron microscopy. This surface study is the subject of another presentation at this Congress. Results in this presentation will show that we have established the effects of different ampoule materials, temperature profiles, pressure differences, and silicon concentrations and that samples that are nearly completely detached can be grown repeatedly.

Szofran, F. R.↗

NASA NTRS1988

Tribological properties of alumina-boria-silicate fabric from 25 to 850 C

Demanding tribological properties are required of the materials used for the sliding seal between the sidewalls and the lower wall of the variable area hypersonic engine. Temperatures range from room temperature and below to operating temperatures of 1000 C in an environment of air, hydrogen, and water vapor. Candidate sealing materials for this application are an alumina-boria-silicate, ceramic, fabric rope sliding against the engine walls which may be made from copper- or nickel-based alloys. Using a pin-on-disk tribometer, the friction and wear properties of some of these potential materials and possible lubrication methods are evaluated. The ceramic fabric rope displayed unacceptably high friction coefficients (0.6 to 1.3) and, thus, requires lubrication. Sputtered thin films of gold, silver, and CaF2 reduced the friction by a factor of two. Sprayed coatings of boride nitride did not effectively lubricate the fabric. Static heat treatment tests at 950 C indicate that the fabric is chemically attacked by large quantities of silver, CaF2, and boron nitride. Sputtered films or powder impregnation of the fabric with gold may provide adequate lubrication up to 1000 C without showing any chemical attack.

Dellacorte, Christopher↗

NASA NTRS1989

Tribological properties of alumina-boria-silicate fabric from 25 C to 850 C

Dellacorte, Christopher↗

NASA NTRS1983

The effects of Cr, Al, Ti, Mo, W, Ta, and Cb on the cyclic oxidation behavior of cast Ni-base superalloys at 1100 and 1150 C

Fifty Ni-base superalloys with concentrations of Cr, Al, Ti, Mo, W, Ta, and Cb systematically varied between two nonzero levels, were tested for cyclic oxidation resistance at 1100 and 1150 C. Oxidation resistance was interpreted in terms of the rate of specific weight change and the types of oxides formed. It is found that the resistance of the alloys to cyclic oxidation is largely determined by Al content, with a sharp increase in the oxidation resistance observed in the Al concentration range 5-8 at. pct. The effects of the other elements studied were small compared with that of aluminum. Best oxidation resistance characteristics were predicted for high Al (13 at. pct), low Cr (10 at. pct), low Ti (2 at. pct), low Cb (1 at. pct), and high Mo, W, and Ta (3 at. pct each). The effects of the refractory metals, however, are somewhat ambiguous and should be investigated further. Higher boron contents, which were unintentionally varied, were clearly detrimental even for the most resistant compositions.

Barrett, C. A.↗

NASA NTRS1989

Multiple doping of silicon-germanium alloys for thermoelectric applications

It is shown that heavy doping of n-type Si/Ge alloys with phosphorus and arsenic (V-V doping interaction) by diffusion leads to a significant enhancement of their carrier concentration and possible improvement of the thermoelectric figure of merit. High carrier concentrations were achieved by arsenic doping alone, but for a same doping level higher carrier mobilities and lower resistivities are obtained through phosphorus doping. By combining the two dopants with the proper diffusion treatments, it was possible to optimize the different properties, obtaining high carrier concentration, good carrier mobility and low electrical resistivity. Similar experiments, using the III-V doping interaction, were conducted on boron-doped p-type samples and showed the possibility of overcompensating the samples by diffusing arsenic, in order to get n-type behavior.

Fleurial, Jean-Pierre↗

NASA NTRS1973

Tensile fracture of unidirectional B-Al composite.

Fracture studies on unidirectional boron filament/aluminum matrix composite under axial tension were conducted using scanning electron microscopy, microradiography, and an acoustic emission technique. The combination of these analysis techniques has allowed the description and microstructural characterization of a new noncumulative fracture mode which involves filament break propagation. This fracture mode was found to severely limit the tensile strength of the composite, since the initiation of break propagation leads immediately to catastrophic failure at filament stress levels above a critical value. This critical filament stress was found to be 170,000 psi, and it appeared to be independent of filament diameter, number of filament layers, and the type of matrix alloy.

Steele, J. H.↗

NASA NTRS1971

Fundamental Mechanisms of Tensile Fracture in Aluminum Sheet Unidirectionally Reinforced with Boron Filament

Results are presented from an experimental research effort to gain a more complete understanding of the physics of tensile fracture in unidirectionally reinforced B-Al composite sheet. By varying the degree of filament degradation resulting from fabrication, composite specimens were produced which failed in tension by the cumulative mode, the noncumulative mode, or by any desired combination of the two modes. Radiographic and acoustic emission techniques were combined to identify and physically describe a previously unrecognized fundamental fracture mechanism which was responsible for the noncumulative mode. The tensile strength of the composite was found to be severely limited by the noncumulative mechanism which involved the initiation and sustenance of a chain reaction of filament fractures at a relatively low stress level followed by ductile fracture of the matrix. The minimum average filament stress required for initiation of the fracture mechanism was shown to be approximately 170 ksi, and appeared to be independent of filament diameter, number of filament layers, and the identity of the matrix alloy.

Herring, H. W.↗

NASA NTRS1983

Refractory materials for high-temperature thermoelectric energy conversion

Theoretical work of two decades ago adequately explained the transport behavior and effectively guided the development of thermoelectric materials of high conversion efficiencies of conventional semiconductors (e.g., SiGe alloys). The more significant contributions involved the estimation of optimum doping concentrations, the reduction of thermal conductivity by solid solution doping and the development of a variety of materials with ZT approx. 1 in the temperature range 300 K to 1200 K. ZT approx. 1 is not a theoretical limitation although, experimentally, values in excess of one were not achieved. Work has continued with emphasis on higher temperature energy conversion. A number of promising materials have been discovered in which it appears that ZT 1 is realizable. These materials are divided into two classes: (1) the rare-earth chalcogenides which behave as itinerant highly-degenerate n-type semiconductors at room-temperature, and (2) the boron-rich borides, which exhibit p-type small-polaronic hopping conductivity.

Wood, C.↗

NASA NTRS1984

Refractory materials for high-temperature thermoelectric energy conversion

Theoretical work of two decades ago adequately explained the transport behavior and effectively guided the development of thermoelectric materials of high conversion efficiencies of conventional semiconductors (e.g., SiGe alloys). The more significant contributions involved the estimaiation of optimum doping concentrations, the reduction of thermal conductivity by solid solution doping and the development of a variety of materials with ZT approx. 1 in the temperature range 300 K to 1200 K. ZT approx. 1 is not a theoretical limitation although, experimentally, values in excess of one were not achieved. Work has continued with emphasis on higher temperature energy conversion. A number of promising materials have been discovered in which it appears that ZT 1 is realizable. These materials are divided into two classes: (1) the rare-earth chalcogenides which behave as itinerant highly-degenerate n-type semiconductors at room-temperature, and (2) the boron-rich borides, which exhibit p-type small-polaronic hopping conductivity.

Wood, C.↗

NASA NTRS2009

Improved Blackbody Temperature Sensors for a Vacuum Furnace

Some improvements have been made in the design and fabrication of blackbody sensors (BBSs) used to measure the temperature of a heater core in a vacuum furnace. Each BBS consists of a ring of thermally conductive, high-melting-temperature material with two tantalum-sheathed thermocouples attached at diametrically opposite points. The name "blackbody sensor" reflects the basic principle of operation. Heat is transferred between the ring and the furnace heater core primarily by blackbody radiation, heat is conducted through the ring to the thermocouples, and the temperature of the ring (and, hence, the temperature of the heater core) is measured by use of the thermocouples. Two main requirements have guided the development of these BBSs: (1) The rings should have as high an emissivity as possible in order to maximize the heat-transfer rate and thereby maximize temperature-monitoring performance and (2) the thermocouples must be joined to the rings in such a way as to ensure long-term, reliable intimate thermal contact. The problem of fabricating a BBS to satisfy these requirements is complicated by an application-specific prohibition against overheating and thereby damaging nearby instrumentation leads through the use of conventional furnace brazing or any other technique that involves heating the entire BBS and its surroundings. The problem is further complicated by another application-specific prohibition against damaging the thin tantalum thermocouple sheaths through the use of conventional welding to join the thermocouples to the ring. The first BBS rings were made of graphite. The tantalum-sheathed thermocouples were attached to the graphite rings by use of high-temperature graphite cements. The ring/thermocouple bonds thus formed were found to be weak and unreliable, and so graphite rings and graphite cements were abandoned. Now, each BBS ring is made from one of two materials: either tantalum or a molybdenum/titanium/zirconium alloy. The tantalum-sheathed thermocouples are bonded to the ring by laser brazing. The primary advantage of laser brazing over furnace brazing is that in laser brazing, it is possible to form a brazed connection locally, without heating nearby parts to the flow temperature of the brazing material. Hence, it is possible to comply with the prohibition against overheating nearby instrumentation leads. Also, in laser brazing, unlike in furnace brazing, it is possible to exert control over the thermal energy to such a high degree that it becomes possible to braze the thermocouples to the ring without burning through the thin tantalum sheaths on the thermocouples. The brazing material used in the laser brazing process is a titanium-boron paste. This brazing material can withstand use at temperatures up to about 1,400 C. In thermal-cycling tests performed thus far, no debonding between the rings and thermocouples has been observed. Emissivity coatings about 0.001 in. (.0.025 mm) thick applied to the interior surfaces of the rings have been found to improve the performance of the BBS sensors by raising the apparent emissivities of the rings. In thermal-cycling tests, the coatings were found to adhere well to the rings.

Farmer, Jeff↗

NASA NTRSDate not supplied

Metallic Environmentally Resistant Coating Rapid Innovation Initiative

Lightweight alloys such as aluminum (Al) and titanium (Ti) are often specified for space systems to minimize mass while maintaining structural integrity [1,2]. Such alloys however, have poor tribological response (high friction and wear), especially in extreme space environments, which becomes worse with the additional presence of lunar regolith. This leads to short lifetimes and premature failures that will ultimately limit long term operations on the lunar surface [2]. This project is addressing this technology gap by developing advanced wear- and radiation-resistant coatings for lightweight parts to extend the life-time and sustainability of both lunar and Martian assets. Ceramics were considered for their high wear resistance, but were rejected because of their low fracture toughness, which would be especially problematic for structural components. The novel and existing coating technologies and deposition methods are being tested in this project. The coating materials are Boron Nitride-Aluminum (BN-Al), Nickle Titanium (NiTi), Aluminum Oxide (AlO3), Ti64 with hBN at 2 and 10 vol percent (Ti-2vol%hBN and Ti-10vol%hBN), and the deposition techniques are high pressure cold-spray (CS) and ambient and vacuum plasma-spray (APS and VPS) [3,4,5]. BN-Al, NiTi, Ti-2vol%hBN, and Ti-10vol%hBN were applied with all three deposition techniques, and AlO3 was applied only using the APS deposition technique. A tungstenite (WS2) film was applied to the NiTi VPS coating. The coating and deposition technique configurations are being tested against several key end-use performance parameters. The parameters include the capabilities of the coatings under wear environments such as regolith simulant, thermal cycling from high (120°C) to cryogenic (-173°C), high vacuum (~10-7 torr), and pre- and post-exposure to ionizing particle radiation. Wear tests include pin on disk, three-body abrasion, and surface erosion by high velocity regolith impacts. The initial down selection is being performed using on virgin and environmental exposure samples using pin on disk and three body abrasion wear tests. From preliminary assessment of this testing, a few configurations were eliminated. Ti-10vol%hBN could not be applied using CS application and NiTi could not be applied using APS or CS application so these configurations did not get tested. Early pin on disk wear tests showed poor wear performance of BN-Al so this coating was eliminated early in the testing process. AlO3 on Al substrate did not survive thermal cycling, but wear testing is continuing for AlO3 on Ti substrate. A more detailed analysis is being con-ducted to further reduce the number of configuration for phase II and III. Phase II testing will include conventionally and additively manufactured substrates with surface erosion testing. In phase III, the coatings will be applied to three mechanism types: channel and slot, ball and socket, and a hinge joint. Each will demonstrate a different type of wear incidence. The mechanisms and their base materials are of direct interest to the end users and infusion points: the Human Landing System (HLS) and the Lunar Surface Innovation Initiative (sustained lunar surface operations). The technology development project is based out of Marshall Space Flight Center, has partnered with Florida International University (Miami, FL) and Plasma Processes (Huntsville, Al), and is supported by a group of NASA mentors from different centers.

dust mitigation↗