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NASA NTRS1991

Uniform-Dead-Weight Brazing

Method of deadweight loading for vacuum-furnace brazing improves quality of joint, increases yield, and reduces costs. In improved method, plates weighted with heavy stainless-steel blocks. Blocks act independently and are immune to distortion. Besides being uniformly distributed, force applied to plates larger and repeatable from one brazing operation to next. Larger blocks used on edges of plates, where more thermal mass needed to reduce differences between temperatures of interior and edge as temperature of furnace varied.

Gaw, William D.↗

NASA NTRS1990

Multiple sensor multifrequency eddy current monitor for solidification and growth

A compact cylindrical multisensor eddy current measuring system with integral furnace was develop to monitor II-VI crystal growth to provide interfacial information, solutal segregation, and conductivities of the growth materials. The use of an array of sensors surrounding the furnace element allows one to monitor the volume of interest. Coupling these data with inverse multifrequency analysis allows radial conductivity profiles to be generated at each sensor position. These outputs were incorporated to control the processes within the melt volume. The standard eddy current system functions with materials whose electric conductivities are as low as 2E2 Mhos/m. A need was seen to extend the measurement range to poorly conducting media so the unit was modified to allow measurement of materials conductivities 4 order of magnitude lower and bulk dielectric properties. Typically these included submicron thick films and semiinsulating GaAs. This system was used to monitor complex heat transfer in grey bodies as well as semiconductor and metallic solidification.

Wallace, John↗

NASA NTRS1991

Optimal design of solidification processes

An optimal design algorithm is presented for the analysis of general solidification processes, and is demonstrated for the growth of GaAs crystals in a Bridgman furnace. The system is optimal in the sense that the prespecified temperature distribution in the solidifying materials is obtained to maximize product quality. The optimization uses traditional numerical programming techniques which require the evaluation of cost and constraint functions and their sensitivities. The finite element method is incorporated to analyze the crystal solidification problem, evaluate the cost and constraint functions, and compute the sensitivities. These techniques are demonstrated in the crystal growth application by determining an optimal furnace wall temperature distribution to obtain the desired temperature profile in the crystal, and hence to maximize the crystal's quality. Several numerical optimization algorithms are studied to determine the proper convergence criteria, effective 1-D search strategies, appropriate forms of the cost and constraint functions, etc. In particular, we incorporate the conjugate gradient and quasi-Newton methods for unconstrained problems. The efficiency and effectiveness of each algorithm is presented in the example problem.

Dantzig, Jonathan A.↗

NASA NTRS1992

Pyrolytic boron nitride coatings on ceramic yarns and fabrication of insulations

Pyrolytic boron nitride (PBN) was deposited on Nicalon NL 202 silicon carbide yarns at 1000 to 1200 C with the goal of improving the resistance of the Nicalon to deterioration in an aerodynamic environment at temperatures up to 1000 C. For continuous coating, the yarns were fed through the deposition chamber of a pilot plant sized CVD furnace at a rate of about 2 feet per minute. PBN coatings were obtained by reacting boron trichloride and ammonia gases inside the deposition chamber. Most of the PBN coatings were made at around 1080 C to minimize thermal degradation of the Nicalon. Pressures were typically below 0.1 Torr. The coated yarns were characterized by weight per unit length, tensile strength and modulus, scanning electron microscopy, and scanning Auger microscopy. The PBN coated Nicalon was woven into cloth, but was not entirely satisfactory as a high temperature sizing. Several 13 in. square pieces of Nicalon cloth were coated with PBN in a batch process in a factory sized deposition furnace. Samples of cloth made from the PBN coated Nicalon were sewn into thermal insulation panels, whose performance is being compared with that of panels made using uncoated Nicalon.

Moore, Arthur W.↗

NASA NTRS1991

Analysis, design, and experimental results for lightweight space heat receiver canisters, phase 1

Critical technology experiments have been performed on thermal energy storage modules in support of the Brayton Advanced Heat Receiver program. The modules are wedge-shaped canisters designed to minimize the mechanical stresses that occur during the phase change of the lithium fluoride phase change material. Nickel foam inserts were used in some of the canisters to provide thermal conductivity enhancement and to distribute the void volume. Two canisters, one with a nickel foam insert, and one without, were thermally cycled in various orientations in a fluidized bed furnace. The only measurable impact of the nickel foam was seen when the back and short sides of the canister were insulated to simulate operation in the advanced receiver design. In tests with insulation, the furnace to back side delta T was larger in the canister with the nickel foam insert, probably due to the radiant absorptivity of the nickel. However, the differences in the temperature profiles of the two canisters were small, and in many cases the profiles matched fairly well. Computed Tomography (CT) was successfully used to nondestructively demarcate void locations in the canisters. Finally, canister dimensional stability, which was measured throughout the thermal cycling test program with an inspection fixture was satisfactory with a maximum change of 0.635 mm (0.025 in.).

Schneider, Michael G.↗

NASA NTRS1991

Technology for increased human productivity and safety on orbit

Technologies are addressed that can facilitate the efficient performance of station operations on the Space Station Freedom (SSF) and thereby optimize the utilization of SSF for scientific research. The dedication of SSF capabilities to scientific study and to the payload-user community is a key goal of the program. Robotics applications are discussed in terms of automating the processing of experiment materials on-orbit by transferring ampules to a furnace system or by handling plant-tissue cultures. Noncontact temperature measurement and medical support technology are considered important technologies for maximizing time for scientific purposes. Detailed examinations are conducted of other technologies including advanced data systems and furnace designs. The addition of the listed technologies can provide an environment in which scientific research is more efficient and accurate.

Ambrus, Judith↗

NASA NTRS1991

Zeolite crystal growth in space

The growth of large, uniform zeolite crystals in high yield in space can have a major impact on the chemical process industry. Large zeolite crystals will be used to improve basic understanding of adsorption and catalytic mechanisms, and to make zeolite membranes. To grow large zeolites in microgravity, it is necessary to control the nucleation event and fluid motion, and to enhance nutrient transfer. Data is presented that suggests nucleation can be controlled using chemical compounds (e.g., Triethanolamine, for zeolite A), while not adversely effecting growth rate. A three-zone furnace has been designed to perform multiple syntheses concurrently. The operating range of the furnace is 295 K to 473 K. Teflon-lined autoclaves (10 ml liquid volume) have been designed to minimize contamination, reduce wall nucleation, and control mixing of pre-gel solutions on orbit. Zeolite synthesis experiments will be performed on USML-1 in 1992.

Sacco, Albert, Jr.↗

NASA NTRS1992

Microwave processing of materials in microgravity

The Jet Propulsion Laboratory is investigating the use of microwave energy as a controlled heating and positioning source for the processing of materials in the microgravity environment of space. Ground-based studies of the positioning capabilities of microwave forces are presented. The ability to quickly and efficiently control the heating of a variety of materials is demonstrated, and the heating of several representative materials is presented. A compact cold-wall microwave furnace compatible with future flight experiments in a shuttle mid-deck cannister is evaluated. The development of a hybrid containerless processing facility that will serve both as an acoustic positioning chamber and a microwave-heating cavity is also proposed. The design characteristics of a cold-wall furnace and hybrid heater/positioner are reviewed.

Barmatz, M.↗

NASA NTRS1991

Analysis of advanced optical glass and systems

Optical lens systems performance utilizing optical materials comprising reluctant glass forming compositions was studied. Such special glasses are being explored by NASA/Marshall Space Flight Center (MSFC) researchers utilizing techniques such as containerless processing in space on the MSFC Acoustic Levitation Furnace and on the High Temperature Acoustic Levitation Furnace in the conceptual design phase for the United States Microgravity Laboratory (USML) series of shuttle flights. The application of high refractive index and low dispersive power glasses in optical lens design was investigated. The potential benefits and the impacts to the optical lens design performance were evaluated. The results of the studies revealed that the use of these extraordinary glasses can result in significant optical performance improvements. Recommendations of proposed optical properties for potential new glasses were also made. Applications of these new glasses are discussed, including the impact of high refractive index and low dispersive power, improvements of the system performance by using glasses which are located outside of traditional glass map, and considerations in establishing glass properties beyond conventional glass map limits.

Johnson, R. Barry↗

NASA NTRS1992

Investigation of microgravity effects on solidification phenomena of selected materials

A Get Away Special (GAS) experiment payload to investigate microgravity effects on solidification phenomena of selected experimental samples has been designed for flight. It is intended that the first flight of the assembly will (1) study the p-n junction characteristics for advancing semiconductor device applications, (2) study the effects of gravity-driven convection on the growth of HgCd crystals, (3) compare the textures of the sample which crystallizes in microgravity with those found in chondrite meteorites, and (4) modify glass optical characteristics through divalent oxygen exchange. The space flight experiment consists of many small furnaces. While the experiment payload is in the low gravity environment of orbital flight, the payload controller will sequentially activate the furnaces to heat samples to their melt state and then allow cooling to resolidification in a controlled fashion. The materials processed in the microgravity environment of space will be compared to the same materials processed on earth in a one-gravity environment. This paper discusses the design of all subassemblies (furnance, electronics, and power systems) in the experiment. A complete description of the experimental materials is also presented.

Maag, Carl R.↗

NASA NTRS1992

Development of a material processing plant for lunar soil

Currently there is considerable interest in developing in-situ materials processing plants for both the Moon and Mars. Two of the most important aspects of developing such a materials processing plant is the overall system design and the integration of the different technologies into a reliable, lightweight, and cost-effective unit. The concept of an autonomous materials processing plant that is capable of producing useful substances from lunar regolith was developed. In order for such a materials processing plant to be considered as a viable option, it must be totally self-contained, able to operate autonomously, cost effective, light weight, and fault tolerant. In order to assess the impact of different technologies on the overall systems design and integration, a one-half scale model was constructed that is capable of scooping up (or digging) lunar soil, transferring the soil to a solar furnace, heating the soil in the furnace to liberate the gasses, and transferring the spent soil to a 'tile' processing center. All aspects of the control system are handled by a 386 class PC via D/A, A/D, and DSP (Digital Signal Processor) control cards.

Goettsch, Ulix↗

NASA NTRS1991

Void control in the crystallization of lithium fluoride

The effect of tungsten-coated graphite fibers on the radiant heat transfer characteristics of salt-fiber composites was studied by measuring the onset of melting as a function of applied furnace power. As the fiber concentration was increased from 0 to 5.40 percent fiber by weight, the furnace temperature required to melt the lithium fluoride also increased. Upon cooling, each of the crystalline salt-fiber composites were cut open with a diamond saw to expose the void. Optical photographs of the voids revealed a trend in void location and size, with the largest void, and the least change in the outer dimension of the boule upon cooling, occurring in the sample with the most fiber.

Jaworske, Donald A.↗

NASA NTRS1993

Planar imaging of OH density distributions in a supersonic combustion tunnel

Images of absolute OH number density were obtained using planar laser-induced fluorescence (PLIF) in a supersonic H2-air combustion tunnel. A tunable KrF excimer laser was used to excite the Q2(11) ro-vibronic line. Calibration of the PLIF images was obtained by referencing the signal measured in the flame to that obtained by the excitation of OH produced by thermal dissociation of H2O in an atmospheric furnace. Measurement errors due to uncertainty in internal furnace atmospheric conditions and image temperature correction are estimated.

Quagliaroli, T. M.↗

NASA NTRS1992

Facility for continuous CVD coating of ceramic fibers

An inductively heated CVD furnace of pilot-plant scale, whose hot zone is 150 mm in diameter x 300 mm in length, has been adapted for continuous coating of ceramic yarns. Coatings at very low pressures are possible in this facility due to the fact that the entire apparatus, including yarn feeding and collecting equipment, is under vacuum. SiC yarn has been coated with 0.1-0.2 microns of BN at yarn speeds of 60 cm/min; a 500-m spool; was coated in about 14 hrs. Coating capacity was tripled by adding pulleys to allow three yarn passes through the furnace.

Moore, Arthur W.↗

NASA NTRS1994

Hydraulically Driven Grips For Hot Tensile Specimens

Pair of grips for tensile and compressive test specimens operate at temperatures up to 1,500 degrees F. Grips include wedges holding specimen inside furnace, where heated to uniform temperature. Hydraulic pistons drive wedges, causing them to exert clamping force. Hydraulic pistons and hydraulic fluid remain outside furnace, at room temperature. Cooling water flows through parts of grips to reduce heat transferred to external components. Advantages over older devices for gripping specimens in high-temperature tests; no need to drill holes in specimens, maintains constant gripping force on specimens, and heated to same temperature as that of specimen without risk of heating hydraulic fluid and acuator components.

Bird, R. Keith↗

NASA NTRS1994

Sensor Detects Semiconductor Escaping From Ampoule

Electrical resistance and temperature change upon exposure to semiconductors. Sensor detects breakage of ampoule containing molten semiconductor. Chemical reaction between hot semiconductor material and wire causes step increase in electrical resistance and temperature of wire. Step increase in temperature and resistance of sensor indicates presence of hot GaAs. Sensor used to shut down furnace automatically if ampoule breaks and prevents further release of molton semiconductor, which could quickly breach surrounding thin wall of cartridge, damage furnace, and/or release toxic vapors into surrounding area.

Watring, Dale A.↗

NASA NTRS1993

Solidification of eutectic system alloys in space (M-19)

It is well known that in the liquid state eutectic alloys are theoretically homogeneous under 1 g conditions. However, the homogeneous solidified structure of this alloy is not obtained because thermal convection and non-equilibrium solidification occur. The present investigators have clarified the solidification mechanisms of the eutectic system alloys under 1 g conditions by using the in situ observation method; in particular, the primary crystals of the eutectic system alloys never nucleated in the liquid, but instead did so on the mold wall, and the crystals separated from the mold wall by fluid motion caused by thermal convection. They also found that the equiaxed eutectic grains (eutectic cells) are formed on the primary crystals. In this case, the leading phase of the eutectic must agree with the phase of the primary crystals. In space, no thermal convection occurs so that primary crystals should not move from the mold wall and should not appear inside the solidified structure. Therefore no equiaxed eutectic grains will be formed under microgravity conditions. Past space experiments concerning eutectic alloys were classified into two types of experiments: one with respect to the solidification mechanisms of the eutectic alloys and the other to the unidirectional solidification of this alloy. The former type of experiment has the problem that the solidified structures between microgravity and 1 g conditions show little difference. This is why the flight samples were prepared by the ordinary cast techniques on Earth. Therefore it is impossible to ascertain whether or not the nucleation and growth of primary crystals in the melt occur and if primary crystals influence the formation of the equiaxed eutectic grains. In this experiment, hypo- and hyper-eutectic aluminum copper alloys which are near eutectic point are used. The chemical compositions of the samples are Al-32.4mass%Cu (Hypo-eutectic) and Al-33.5mass%Cu (hyper-eutectic). Long rods for the samples are cast by the Ohno Continuous Casting Process and they show the unidirectionally solidified structure. Each flight and ground sample was made of these same rods. The dimensions of all samples are 4.5 mm in diameter and 23.5 mm in length. Each sample is put in a graphite capsule and then vacuum sealed in a double silica ampoule. Then the ampoule is put in the tantalum cartridge and sealed by electron beam welding. For onbard experiments, a Continuous Heating Furnance (CHF) will be used for melting and solidifying samples under microgravity conditions. Six flight samples will be used. Four samples are hypo-eutectic and two are hyper-eutectic alloys. The surface of the two hypo-eutectic alloy samples are covered with aluminum oxide film to prevent Marangoni convection expected under microgravity conditions. Each sample will be heated to 700 C and held at that temperature for 5 min. After that the samples will be allowed to cool to 500 C in the furnace and they will be taken out of the furnace for He gas cooling. The heating and cooling diagrams for the flight experiments are shown. After collecting the flight samples, the solidified structures of the samples will be examined and the mechanisms of eutectic solidification under microgravity conditions will be determined. It is likely that successful flight experiment results will lead to production of high quality eutectic alloys and eutectic composite materials in space.

Ohno, Atsumi↗

NASA NTRS1993

Crystal growth of compound semiconductors in a low-gravity environment (InGaAs crystals) (M-22)

Compound semiconductor crystals, such as gallium arsenide and indium phosphide crystals, have many interesting properties that silicon crystals lack, and they are expected to be used as materials for optic and/or electro-optic integrated devices. Generally speaking, alloy semiconductors, which consist of more than three elements, demonstrate new functions. For example, values of important parameters, such as lattice constant and emission wavelength, can be chosen independently. However, as it is easy for macroscopic and/or microscopic fluctuations of composition to occur in alloy semiconductor crystals, it is difficult to obtain crystals having homogeneous properties. Macroscopic change of composition in a crystal is caused by the segregation phenomenon. This phenomenon is due to a continuous change in the concentration of constituent elements at the solid-liquid interfacing during solidification. On Earth, attempts were made to obtain a crystal with homogeneous composition by maintaining a constant melt composition near the solid-liquid interface, through suppression of the convection flow of the melt by applying a magnetic field. However, the attempt was not completely successful. Convective flow does not occur in microgravity because the gravity in space is from four to six orders of magnitude less than that on Earth. In such a case, mass transfer in the melt is dominated by the diffusion phenomenon. So, if crystal growth is carried out at a rate that is higher than the rate of mass transfer due to this phenomenon, it is expected that crystals having a homogeneous composition will be obtained. In addition, it is also possible that microscopic composition fluctuations (striation) may disappear because microscopic fluctuations diminish in the absence of convection. We are going to grow a bulk-indium gallium arsenide (InGaAs) crystal using the gradient heating furnace (GHF) in the first material processing test (FMPT). The structure of the sample is shown where InGaAs polycrystals in a crucible are doubly sealed in two quartz tubes for safety. The GHF consists of two zones, namely, high temperature and low temperature zones, which results in a large temperature gradient at the interface. Crystal growth is performed by moving the furnace (i.e. the temperature profile) from the left to right at a definite rate. Thus, we will grow crystals both on Earth and in space under the same conditions. As previously described, it is possible to obtain good quality crystals which are homogeneous in composition both macroscopically and microscopically due to the lack of convection in space. We are planning to study the effects of convection on crystal growth from a melt by comparing and characterizing the properties of crystals grown on Earth with those grown in space.

Tatsumi, Masami↗