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At least 127 records · Page 7

Containerless high temperature property measurements by atomic fluorescence

The use of laser induced fluorescence (LIF) techniques for containerless study of high temperature processes and material properties is studied. Gas jet and electromagnetic levitation and electromagnetic and laser heating techniques are used with LIF in Earth-based containerless high temperature experiments. The work to date includes development of an apparatus and its use in studies of chemical reactions on Al2O3, molybdenum, and tungsten specimens, novel methods for noncontact specimen temperature measurement, and levitation jet properties. Brief summaries of these studies are given. The apparatus is described and detailed results for the current reporting period are presented.

Source record↗

Containerless high temperature property measurements by atomic fluorescence

Laser induced fluorescence (LIF) techniques for containerless study of high temperature processes and material properties was studied. Gas jet and electromagnetic levitation and electromagnetic and laser heating techniques are used with LIF in earth-based containerless high temperature experiments. Included are the development of an apparatus and its use in the studies of (1) chemical reactions on Al2O3, molybdenum, tungsten and LaB6 specimens, (2) methods for noncontact specimen temperature measurement, (3) levitation jet properties and (4) radiative lifetime and collisional energy transfer rates for electronically excited atoms.

Schiffman, R. A.↗

Method for fabricating semiconductor devices

A process for fabricating gold/gallium arsenide structures, in situ, on molecular beam epitaxially grown gallium arsenide. The resulting interface proves to be Ohmic, an unexpected result which is interpreted in terms of increased electrode interdiffusion. More importantly, the present invention surprisingly permits the fabrication of Ohmic contacts in a III-V semiconductor material at room temperature. Although it may be desireable to heat the Ohmic contact to a temperature of, for example, 200 degrees Centigrade if one wishes to further decrease the resistance of the contact, such low temperature annealing is much less likely to have any deleterious affect on the underlying substrate. The use of the term in situ herein, contemplates continuously maintaining an ultra-high vacuum, that is a vacuum which is at least 10.sup.-8 Torr, until after the metallization has been completed. An alternative embodiment of the present invention comprising an additional step, namely the termination of the gallium arsenide by a two monolayer thickness of epitaxial aluminum arsenide as a diffusion barrier, enables the recovery of Schottky barrier behavior, namely a rectified I-V characteristic. The present invention provides a significant breakthrough in the fabrication of III-V semiconductor devices wherein excellent Ohmic contact and Schottky barrier interfaces to such devices can be achieved simply and inexpensively and without requiring the high temperature processing of the prior art and also without requiring the use of exotic high temperature refractory materials as substitutes for those preferred contact metals such as gold, aluminum and the like.

Kaiser, William J.↗

An investigation of some mechanical and thermal properties of lunar simulant materials heated at 2.45 GHz

Lunar simulant material was fabricated to simulate Apollo 11, Apollo 15, and Apollo 16 soils. The approximate compositions which these soils simulate are given. Samples of each soil simulate were fabricated into right circular cylinders, placed into a microwave reaction cavity, and heated using 2.45 GHz radiation to a particular processing temperature at which it was held for a prescribed length of time. Examples are given of two microwave heating programs for these simulant samples. Upon completion of thermal processing, each sample had its top and bottom surfaces polished. A technique was employed which looks at hardness data to determine the fracture toughness of a material and then relates this to thermal shock resistance. Some advantages of this technique are its low cost for analysis and thermal shock resistance as a function of initial sample orientation in the microwave field can be determined. Samples were prepared for testing and results are expected. At the same time, other samples are currently being investigated using scanning electron microscopy to determine their microstructures.

Meek, T. T.↗

Initial Measurement of the Vapor Pressures of Simple Refractory Materials: Cu and Fe

It has become increasingly clear over the past decade that high temperature processes played important roles in the Primitive Solar Nebula. Unfortunately, basic data, such as the vapor pressures of iron or SiO have not been measured over the appropriate temperature range (near T approximately equal to 2000K), but must be extrapolated from lower temperature measurements often made more than 50 years ago. The extrapolation of the available data to higher temperatures can be quite complex and can depend on other factors such as the oxygen fugacity or the presence of hydrogen gas. Moreover, modern technology has made possible more accurate measurements of such quantities over a wider temperature range. We recently acquired a commercial Thermo-Cahn Thermogravimetric system capable of vacuum operation to 1700 C and measurement of mass change with microgram accuracy in a 100g sample or smaller. In this paper, we will report our progress in learning to make vapor pressure measurements using this system.

Nuth, Joseph A., III↗

Apparatus and Method for Compensating for Process, Voltage, and Temperature Variation of the Time Delay of a Digital Delay Line

A process, voltage, and temperature (PVT) compensation circuit and a method of continuously generating a delay measure are provided. The compensation circuit includes two delay lines, each delay line providing a delay output. The two delay lines may each include a number of delay elements, which in turn may include one or more current-starved inverters. The number of delay lines may differ between the two delay lines. The delay outputs are provided to a combining circuit that determines an offset pulse based on the two delay outputs and then averages the voltage of the offset pulse to determine a delay measure. The delay measure may be one or more currents or voltages indicating an amount of PVT compensation to apply to input or output signals of an application circuit, such as a memory-bus driver, dynamic random access memory (DRAM), a synchronous DRAM, a processor or other clocked circuit.

Seefeldt, James↗

Effects of Melt Processing on Evolution of Structure in PEEK

We report on the effects of melt processing temperature on structure formation in Poly(ether-ether-ketone), PEEK. Real time Small Angle X-ray Scattering, SAXS, and thermal analysis are used to follow the melting behavior after various stages of processing. Assignment of peaks to structural entities within the material, the relative perfection of the crystals, and the possibility of their reorganization, are all influenced by the melt processing history. With the advent of high intensity synchrotron sources of X-radiation, polymer scientists gain a research tool which, when used along with thermal analysis, provides additional structural information about the crystals during growth and subsequent melting. PEEK is an engineering thermoplastic polymer with a very high glass transition temperature (145 C) and crystal melting point (337 C). PEEK has been the subject of recent studies by X-ray scattering in which melt and cold crystallization were followed in real-time. X-ray scattering and thermal studies have been used to address the formation of dual endothermic response which has been variously ascribed to lamellar insertion, dual crystal populations, or melting followed by re-crystallization. Another important issue is whether all of the amorphous phase is located in interlamellar regions, or alternatively whether some is located in "pockets" away from the crystalline lamellar stacks. The interpretation of scattering from lamellar stacks varies depending upon whether such amorphous pockets are formed. Some groups believe all of the amorphous phase is interlamellar. This leads to selection of a smaller thickness for the crystals. Other groups suggest that most amorphous phase is not interlamellar, and this leads to the suggestion that the crystal thickness is larger than the amorphous layer within the stacks. To investigate these ideas, we used SAXS and Differential Scanning Calorimetry to compare results of single and dual stage melt crystallization of PEEK using a treatment scheme involving annealing/crystallization at T(sub a1) followed by annealing at T(sub a2) where either T(sub a1) < T(sub a2) or T(sub a1) > T(sub a2). We proposed a model to explain multiple melting endotherms in PPS, treated according to one or two-stage melt or cold crystallization. Key features of this model are that multiple endotherms: (1) are due to reorganization/recrystallization after cold crystallization; and, (2) are dominated by crystal morphology after melt crystallization at high T. In other words, multiple distinct crystal populations are formed by the latter treatment, leading to observation of multiple melting. PEEK 45OG pellets (ICI Americas) were the starting material for this study. Films were compression molded at 400 C, then quenched to ice water. Samples were heated to 375 C in a Mettler FP80 hot stage and held for three min. to erase crystal seeds before cooling them to T(sub a1) = 280 C . Samples were held at T(sub a2) for a period of time, then immediately heated to 360 C. In the second treatment samples were held at T(sub a1) = 31 C for different crystallization times t(sub c) then cooled to 295 C and held 15 min. In situ (SAXS) experiments were performed at the Brookhaven National Synchrotron Light Source with the sample located inside the Mettler hot stage. The system was equipped with a two-dimensional position sensitive detector. The sample to detector distance was 172.7 cm and the X-ray wavelength was 1.54 Angstroms. SAXS data were taken continuously during the isothermal periods and during the heating to 360 C at 5 C/min. Each SAXS scan was collected for 30 sec. Since the samples were isotropic, circular integration was used to increase the signal to noise ratio. After dual stage melt crystallization with T(sub a1) < T(sub a2) the lower melting endotherm arises from holding at T(sub a1). During cooling a broad distribution of crystals forms, and the low-melting tail is perfected during T(sub al). Heating to T(sub a2) melts these imperfect crystals and allows others with greater average long spacing to form in their place. After dual stage crystallization with T(sub a1) > T(sub a2), the amount of space remaining for additional growth at T(sub a2) depends upon the holding time at T(sub a1). The long period of crystals formed at T(sub a2) is smaller than that formed at T(sub a1) due to growth in a now-restricted geometry. Perfection of crystals is seen as an increase of the intensity of the population scattering at higher s, while the intensity of the population scattering at lower s stays constant. During heating from below to above the minor endotherm, we see rapid decrease of the intensity of the X-ray scattering corresponding to the population of crystals scattering in the shoulder. Another important observation is that after the sample is annealed at 295 C, the shoulder intensity is restored once again. The population scattering at higher s remains longer before it disappears in the sample treated to the second stage of melt crystallization, compared to the sample crystallized with a single stage. This could be interpreted as an effect of continued perfection of the less perfect population, which is also reflected in the increased melting temperature of the smaller endotherm as the holding time at 295 C increases. In the corresponding DSC scans we see a shift in the area and the peak temperature of the lower melting endotherm with an increase of the annealing time.

Georgiev, Georgi↗

High-strength silicon carbides by hot isostatic pressing

Silicon carbide has strong potential for heat engine hardware and other high-temperature applications because of its low density, good strength, high oxidation resistance, and good high-temperature creep resistance. Hot isostatic pressing (HIP) was used for producing alpha and beta silicon carbide (SiC) bodies with near-theoretical density, ultrafine grain size, and high strength at processing temperatures of 1900 to 2000 C. The HIPed materials exhibited ultrafine grain size. Furthermore, no phase transformation from beta to alpha was observed in HIPed beta-SiC. Both materials exhibited very high average flexural strength. It was also shown that alpha-SiC bodies without any sintering aids, when HIPed to high final density, can exhibit very high strength. Fracture toughness K (sub C) values were determined to be 3.6 to 4.0 MPa m (sup 1/2) for HIPed alpha-SiC and 3.7 to 4.1 MPa m (sup 1/2) for HIPed beta-SiC. In the HIPed specimens strength-controlling flaws were typically surface related. In spite of improvements in material properties such as strength and fracture toughness by elimination of the larger strength-limiting flaws and by grain size refinement, HIPing has no effect on the Weibull modulus.

Dutta, Sunil↗

High-strength silicon carbides by hot isostatic pressing

Silicon carbide has strong potential for heat engine hardware and other high-temperature applications because of its low density, good strength, high oxidation resistance, and good high-temperature creep resistance. Hot isostatic pressing (HIP) was used for producing alpha and beta silicon carbide (SiC) bodies with near-theoretical density, ultrafine grain size, and high strength at processing temperatures of 1900 to 2000 C. The HIPed materials exhibited ultrafine grain size. Furthermore, no phase transformation from beta to alpha was observed in HIPed beta-SiC. Both materials exhibited very high average flexural strength. It was also shown that alpha-SiC bodies without any sintering aids, when HIPed to high final density, can exhibit very high strength. Fracture toughness K (sub C) values were determined to be 3.6 to 4.0 MPa m (sup 1/2) for HIPed alpha-SiC and 3.7 to 4.1 MPa m (sup 1/2) for HIPed beta-SiC. In the HIPed specimens strength-controlling flaws were typically surface related. In spite of improvements in material properties such as strength and fracture toughness by elimination of the larger strength-limiting flaws and by grain size refinement, HIPing has no effect on the Weibull modulus.

Dutta, Sunil↗

Effusion Cell Measurements of the Vapor Pressure of Cobalt at Temperatures up to 2000K; Comparisons with Iron and Nickel

It has become increasingly clear over the past decade that high temperature processes played important roles in the Primitive Solar Nebula. Unfortunately, basic data, such as the vapor pressures of Fe, Ni, Co or SiO have not been measured over the appropriate temperature range (near T approx. 2000K), but must be extrapolated from lower temperature measurements often made more than 50 years ago. The extrapolation of the available data to higher temperatures can be quite complex (e.g., see [1] for SiO vapor pressures) and can depend on other factors such as the oxygen fugacity or the presence of hydrogen gas not accounted for in the original measurements. Moreover, modern technology has made possible more accurate measurements of such quantities over a wider temperature range. We have acquired a commercial Thermo-Cahn Thermogravimetric system capable of vacuum operation to 1700C and measurement of a 10g change in sample mass using up to a 100g sample, with microgram accuracy. With this new system we have initiated a series of basic vapor pressure measurements on simple metals such as Fe[2] and Ni[3] with the intention to extend such measurements to more complex systems once we gain sufficient experience.

Nuth, J. A.↗

Vacuum Sintering of Highland Simulant CSM-LHT-1G

Sintering of lunar regolith is a process of interest to consolidate the ubiquitous granular material in durable structures on the lunar surface such as platforms, landing/launch pads, roads, and foundations for long-term robotic and human activities. Many publications do not report quantitative assessment of the effects of processing conditions on the strength properties of the sintered products. The work presented is an investigation into such effects on a carefully selected simulant, CSM-LHT-1G prepared for high temperature processing to eliminate undesired components that would not be present from lunar materials. Careful experiments under vacuum were conducted to identify the relevant factors that dominate the properties and the quality of the sintered product. CSM-LHT-1G simulant is a variant of the CSM-LHT-1 lunar highland simulant produced by Colorado School of Mines. The original mineralogical composition of CSM-LHT-1 (70 wt.% Greenspar, 30 wt.% Merriam Crater basalt) was modified to obtain a 30 wt.% glass content with the addition of NU-LHT-5M glass balanced with pyroxene (augite) to yield CSM-LHT-1G.

Vacuum Sintering↗

Finned Carbon-Carbon Heat Pipe with Potassium Working Fluid

This elemental space radiator heat pipe is designed to operate in the 700 to 875 K temperature range. It consists of a C-C (carbon-carbon) shell made from poly-acrylonitride fibers that are woven in an angle interlock pattern and densified with pitch at high process temperature with integrally woven fins. The fins are 2.5 cm long and 1 mm thick, and provide an extended radiating surface at the colder condenser section of the heat pipe. The weave pattern features a continuous fiber bath from the inner tube surface to the outside edges of the fins to maximize the thermal conductance, and to thus minimize the temperature drop at the condenser end. The heat pipe and radiator element together are less than one-third the mass of conventional heat pipes of the same heat rejection surface area. To prevent the molten potassium working fluid from eroding the C C heat pipe wall, the shell is lined with a thin-walled, metallic tube liner (Nb-1 wt.% Zr), which is an integral part of a hermetic metal subassembly which is furnace-brazed to the inner surface of the C-C tube. The hermetic metal liner subassembly includes end caps and fill tubes fabricated from the same Nb-1Zr alloy. A combination of laser and electron beam methods is used to weld the end caps and fill tubes. A tungsten/inert gas weld seals the fill tubes after cleaning and charging the heat pipes with potassium. The external section of this liner, which was formed by a "Uniscan" rolling process, transitions to a larger wall thickness. This section, which protrudes beyond the C-C shell, constitutes the "evaporator" part of the heat pipe, while the section inside the shell constitutes the condenser of the heat pipe (see figure).

Juhasz, Albert J.↗

Indigenous lunar construction materials

The utilization of local resources for the construction and operation of a lunar base can significantly reduce the cost of transporting materials and supplies from Earth. The feasibility of processing lunar regolith to form construction materials and structural components is investigated. A preliminary review of potential processing methods such as sintering, hot-pressing, liquification, and cast basalt techniques, was completed. The processing method proposed is a variation on the cast basalt technique. It involves liquification of the regolith at 1200-1300 C, casting the liquid into a form, and controlled cooling. While the process temperature is higher than that for sintering or hot-pressing (1000-1100 C), this method is expected to yield a true engineering material with low variability in properties, high strength, and the potential to form large structural components. A scenario for this processing method was integrated with a design for a representative lunar base structure and potential construction techniques. The lunar shelter design is for a modular, segmented, pressurized, hemispherical dome which could serve as habitation and laboratory space. Based on this design, estimates of requirements for power, processing equipment, and construction equipment were made. This proposed combination of material processing method, structural design, and support requirements will help to establish the feasibility of lunar base construction using indigenous materials. Future work will refine the steps of the processing method. Specific areas where more information is needed are: furnace characteristics in vacuum; heat transfer during liquification; viscosity, pouring and forming behavior of molten regolith; design of high temperature forms; heat transfer during cooling; recrystallization of basalt; and refinement of estimates of elastic moduli, compressive and tensile strength, thermal expansion coefficient, thermal conductivity, and heat capacity. The preliminary design of the lunar shelter showed us that joining is a critical technology needed for building a structure from large segments. The problem of joining is important to the design of any structure that is not completely prefabricated. It is especially important when the structure is subjected to tensile loading by an internal pressure. For a lunar shelter constructed from large segments the joints between these large segments must be strong, and they must permit automated construction. With a cast basalt building material which is brittle, there is the additional problem of connecting the joint with the material and avoiding stress concentration that would cause failure. Thus, a well-defined project which we intend to pursue during this coming year is the design of joints for cast basalt structural elements.

Rogers, Wayne P.↗

Comparison of AMZIRC and GRCop-84

The mechanical properties of two copper alloys with high thermal conductivity, GRCop-84 and AMZIRC, were compared. These are competing alloys in high temperature, high heat flux applications such as rocket nozzles. The GRCop-84 data presented was taken from previous work. The results of new tensile, creep, and compression tests on AMZIRC are presented. Tests were done on as-received hard drawn material, and on material that had been subjected to a heat treatment designed to simulate a brazing operation at 935 C. As-received AMZIRC was found to have excellent properties at temperatures below 550 C, with room temperature yield and ultimate tensile strengths of about 500 MPa, and ductile failures. By comparison, GRCop-84 s room temperature tensile yield and ultimate strengths are about 200 and 380 MPa respectively. However, the simulated brazing heat treatment substantially decreased the mechanical properties of AMZIRC; and the strength of as-received AMZIRC dropped precipitously as test temperatures exceeded 500 C. The properties of GRCop-84 were not significantly affected by the 935 C heat treatment. As a result, there appear to be advantages to GRCop- 84 over AMZIRC if use or processing temperatures of greater than 500 C are expected. Tensile creep tests were done at 500 and 650 C. At these temperatures, the creep properties of GRCop-84 were superior to AMZIRC s. At equivalent rupture life and stress, GRCop-84 was found to have a 150 C temperature advantage over AMZIRC; for equivalent rupture life and temperature GRCop-84 was two times stronger.

de Groh, Henry C. III↗

Approaches to New Endcaps for Improved Oxidation Resistance

Norbornenyl-end capped PMR polyimide resins are widely used as polymer matrix composite materials for aircraft engine applications, since they combine ease of processing with good oxidative stability up to 300 C. PMR resins are prepared by a two-step approach involving the initial formation of oligomeric pre-polymers capped at both ends by a latent reactive end cap. The end cap undergoes cross-linking during higher temperature processing, producing the desired low density, high specific strength materials, for PMR- 15. The end cap facilitates processing by controlling the molecular weight of the oligomer and allowing flow before it cross-links. However, after cross-linking, this very end cap accounts for much of the weight loss in the polymer on aging in air at elevated temperatures. Understanding this degradation provides clues for designing new end caps to slow down degradation, and prolong the lifetime of the material.

Meador, Mary Ann B.↗

Fiber-Optic Temperature Sensor Using a Thin-Film Fabry-Perot Interferometer

A fiber-optic temperature sensor was developed that is rugged, compact, stable, and can be inexpensively fabricated. This thin-film interferometric temperature sensor was shown to be capable of providing a +/- 2 C accuracy over the range of -55 to 275 C, throughout a 5000 hr operating life. A temperature-sensitive thin-film Fabry-Perot interferometer can be deposited directly onto the end of a multimode optical fiber. This batch-fabricatable sensor can be manufactured at a much lower cost than can a presently available sensor, which requires the mechanical attachment of a Fabry-Perot interferometer to a fiber. The principal disadvantage of the thin-film sensor is its inherent instability, due to the low processing temperatures that must be used to prevent degradation of the optical fiber's buffer coating. The design of the stable thin-film temperature sensor considered the potential sources of both short and long term drifts. The temperature- sensitive Fabry-Perot interferometer was a silicon film with a thickness of approx. 2 microns. A laser-annealing process was developed which crystallized the silicon film without damaging the optical fiber. The silicon film was encapsulated with a thin layer of Si3N4 over coated with aluminum. Crystallization of the silicon and its encapsulation with a highly stable, impermeable thin-film structure were essential steps in producing a sensor with the required long-term stability.

Beheim, Glenn↗

Brillouin Asymmetric Spatial Heterodyne Oceanographic Lidar Receiver for Profiling Temperature, Salinity, and Sound Velocity

No sensor today is capable of remotely sensing temperature and salinity at depth in oceanic waters, yet the physics to do so exists. Blue-green light (450-550 nm) can penetrate 10’s of meters into the water and interacts with water by the Brillouin scatter process. Temperature and salinity can be determined by analyzing the spectrum of Brillouin scatter. A host of scientific and operational drivers exist for such a sensor, from improved hurricane and red tide forecasting to studies of ocean fronts, eddies, and freshwater lenses. A low flying airborne light detection and ranging (lidar) instrument concept that exploits this physics is presented, along with simulation tools that potential data users can use to model its measurement performance, determine suitability for their application, and assess its implications.

John Anthony Smith↗