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NASA NTRS1984

Studies on the Processing Methods for Extraterrestrial Materials

The literature was surveyed for high temperature mass spectrometric research on single oxides, complex oxides, and minerals in an effort to develop a means of separating elements and compounds from lunar and other extraterrestrial materials. A data acquisition system for determining vaporization rates as a function of time and temperature and software for the IEEE-488 Apple-ORTEC interface are discussed. Experimental design information from a 1000 C furnace were used with heat transfer calculations to develop the basic design for a 1600 C furnace. A controller was built for the higher temperature furnace and drawings are being made for the furnace.

Grimley, R. T.↗

NASA NTRS1987

Fiber glass pulling

Experiments were conducted to determine the viability of performing containerless glass fiber pulling in space. The optical transmission properties and glass-forming capabilities of the heavy metal fluorides are reviewed and the acoustic characteristics required for a molten glass levitation system are examined. The design limitations of, and necessary modifications to the acoustic levitation furnace used in the experiments are discussed in detail. Acoustic levitator force measurements were performed and a thermal map of the furnace was generated from thermocouple data. It was determined that the thermal capability of the furnace was inadequate to melt a glass sample in the center. The substitution of a 10 KW carbon monoxide laser for the original furnace heating elements resulted in improved melt heating.

Workman, Gary L.↗

NASA NTRS1987

Apparatus ad method for quiescent containerless processing of high temperature metals and alloys in low gravity

The electron bombardment furnace consists of two confinement grid sections which may be moved and separated from each other. Inside the bombardment furnace, a tungsten element is enclosed. The material specimen is located within the tungsten element and grounded by means of grounded support wires connected to the respective sections of the furnace. The material specimen is supported on the ground wires and heated by electron bombardment until melt occurs. The furnace sections are separated in opposite directions causing the ground wires to pull from the surfaces of the specimen, leaving the specimen freely suspended in the process chamber without the action of external forces. The specimen remains in its melt condition in the processing chamber where it can be undercooled without external forces acting on the specimen, which would cause dynamic nucleation.

Robinson, Michael B.↗

NASA NTRS1990

The NASA, Marshall Space Flight Center drop tube user's manual

A comprehensive description of the structural and instrumentation hardware and the experimental capabilities of the 105-meter Marshall Space Flight Center Drop Tube Facility is given. This document is to serve as a guide to the investigator who wishes to perform materials processing experiments in the Drop Tube. Particular attention is given to the Tube's hardware to which an investigator must interface to perform experiments. This hardware consists of the permanent structural hardware (with such items as vacuum flanges), and the experimental hardware (with the furnaces and the sample insertion devices). Two furnaces, an electron-beam and an electromagnetic levitator, are currently used to melt metallic samples in a process environment that can range from 10(exp -6) Torr to 1 atmosphere. Details of these furnaces, the processing environment gases/vacuum, the electrical power, and data acquisition capabilities are specified to allow an investigator to design his/her experiment to maximize successful results and to reduce experimental setup time on the Tube. Various devices used to catch samples while inflicting minimum damage and to enhance turnaround time between experiments are described. Enough information is provided to allow an investigator who wishes to build his/her own furnace or sample catch devices to easily interface it to the Tube. The experimental instrumentation and data acquisition systems used to perform pre-drop and in-flight measurements of the melting and solidification process are also detailed. Typical experimental results are presented as an indicator of the type of data that is provided by the Drop Tube Facility. A summary bibliography of past Drop Tube experiments is provided, and an appendix explaining the noncontact temperature determination of free-falling drops is provided. This document is to be revised occasionally as improvements to the Facility are made and as the summary bibliography grows.

Rathz, Thomas J.↗

NASA NTRS1989

Inverse heat transfer analysis of Bridgman crystal growth

The effects of asymmetry in furnace temperature profile and pulling velocity on the crystal interface shape are demonstrated while neglecting the latent heat of solidification. It is seen that the furnace temperature profile may be varied in order to influence the shape of the melt-crystal interface. An exact thermal analysis is then performed on the Bridgman technique by including the latent heat of solidification as a source term. The exact temperature field required for yielding a flat melt-crystal interface is obtained. The earlier observation regarding the influence of furnace temperature profile on the interface shape is confirmed and a criterion for achieving a flat interface is obtained. Various furnace temperature profiles are selected and their corresponding melt-crystal interface results are presented.

Taghavi, K.↗

NASA NTRS1990

Combined air and water pollution control system

A bioaquatic air pollution control system for controlling both water and atmospheric pollution is disclosed. The pollution control system includes an exhaust for directing polluted gases out of a furnace and a fluid circulating system which circulates fluid, such as waste water, from a source, past the furnace where the fluid flow entrains the pollutants from the furnace. The combined fluid and pollutants are then directed through a rock/plant/microbial filtering system. A suction pump pumps the treated waste water from the filter system past the exhaust to again entrain more pollutants from the furnace where they are combined with the fluid (waste water) and directed to the filter system.

Wolverton, Billy C.↗

NASA NTRS1992

An Automated Thermocouple Calibration System

An Automated Thermocouple Calibration System (ATCS) was developed for the unattended calibration of type K thermocouples. This system operates from room temperature to 650 C and has been used for calibration of thermocouples in an eight-zone furnace system which may employ as many as 60 thermocouples simultaneously. It is highly efficient, allowing for the calibration of large numbers of thermocouples in significantly less time than required for manual calibrations. The system consists of a personal computer, a data acquisition/control unit, and a laboratory calibration furnace. The calibration furnace is a microprocessor-controlled multipurpose temperature calibrator with an accuracy of +/- 0.7 C. The accuracy of the calibration furnace is traceable to the National Institute of Standards and Technology (NIST). The computer software is menu-based to give the user flexibility and ease of use. The user needs no programming experience to operate the systems. This system was specifically developed for use in the Microgravity Materials Science Laboratory (MMSL) at the NASA LeRC.

Bethea, Mark D.↗

NASA NTRS1992

Correction-free radiometry on specular spheres for containerless processing in microgravity

An analysis is presented that establishes how correction-free radiance measurements or pyrometry can be performed on targets in furnaces where there may be significant additional radiance from heated furnace walls or from reflecting surfaces close to the target. These configurations are common in microgravity and containerless processing applications where a specular target is radiantly heated in a hot-wall furnace, or inductively heated from the fields arising from nearby closely spaced electromagnetic coils. Proper design requires that the pyrometer does not view any images of the background features in the specular target so that stray radiation will not be reflected into the viewing optics of the pyrometer. To analyze the problem, conventional paraxial optics analysis is shown to be significantly in error. Instead a method of nonparaxial ray tracing, based on the derivatives of the ray paths, shows how the images must be located. This leads to analytical results that can be used to design such systems. The findings are applied to the furnace geometries that are presently being considered for flight in LEO.

Thomas, A. S. W.↗

NASA NTRS1993

Growth of binary organic NLO crystals: m.NA-p.NA and m.NA-CNA system

Experiments were carried out to grow 3.Nitroaniline (m.NA) crystals doped with 4.Nitroaniline (p.NA) and 2.chloro 4.Nitroaniline (CNA). The measured undercooling for m.NA, p.NA, and CNA were 0.21 tm K, 0.23 tm K, and 0.35 tm K respectively, where tm represents the melting temperature of the pure component. Because of the crystals' large heat of fusion and large undercooling, it was not possible to grow good quality crystals with low thermal gradients. In the conventional two-zone Bridgman furnace we had to raise the temperature of the hot zone above the decomposition temperature of CNA, p.NA, and m.NA to achieve the desired thermal gradient. To avoid decomposition, we used an unconventional Bridgman furnace. Two immiscible liquids, silicone oil and ethylene glycol, were used to build a special two-zone Bridgman furnace. A temperature gradient of 18 K/cm was achieved without exceeding the decomposition temperature of the crystal. The binary crystals, m.NA-p.NA and m.NA-CNA, were grown in centimeter size in this furnace. X-ray and optical characterization showed good optical quality.

Singh, N. B.↗

NASA NTRS1997

Crystal Growth Control

We present an innovative design of a vertical transparent multizone furnace which can operate in the temperature range of 25 C to 750 C and deliver thermal gradients of 2 C/cm to 45 C/cm for the commercial applications to crystal growth. The operation of the eight zone furnace is based on a self-tuning temperature control system with a DC power supply for optimal thermal stability. We show that the desired thermal profile over the entire length of the furnace consists of a functional combination of the fundamental thermal profiles for each individual zone obtained by setting the set-point temperature for that zone. The self-tuning system accounts for the zone to zone thermal interactions. The control system operates such that the thermal profile is maintained under thermal load, thus boundary conditions on crystal growth ampoules can be predetermined prior to crystal growth. Temperature profiles for the growth of crystals via directional solidification, vapor transport techniques, and multiple gradient applications are shown to be easily implemented. The unique feature of its transparency and ease of programming thermal profiles make the furnace useful for scientific and commercial applications for the determination of process parameters to optimize crystal growth conditions.

Duval, Walter M. B.↗

NASA NTRS1998

An Assessment of the Axial and Radial Dilation of a DPIMS Tantalum Cartridge for Space Shuttle Flight Experiments

Ground-based heat treatment tests are planned on an argon gas-filled tantalum cartridge developed as pan of a Diffusion Processes in Molten Semiconductors (DPIMS) experiment conducted on NASA's Space Shuttle. The possibility that the cartridge may creep during testing and touch the furnace walls is of real concern in this program. The present paper discusses the results of calculations performed to evaluate this possibility. Deformation mechanism maps were constructed using literature data in order to identify the creep mechanism dominant under the appropriate stresses and temperatures corresponding to the test conditions. These results showed that power-law creep was dominant when the grain size of the material exceeded 55 gm but Coble creep was the important mechanism below this value of grain size. Finite element analysis was used to analyze the heat treatment tWs assuming a furnace run away condition (which is a worst case scenario) using the appropriate creep parameters corresponding to grain sizes of 1 and 100 gm. Calculations were also conducted to simulate the effect of an initial 3 tilt of the cartridge assembly, the maximum possible tilt angle. The von Mises stress and su-ain distributions were calculated assuming that the cartridge was fixed at one end as it was heated from ambient temperature to 1823 K in 1.42 h, maintained at 1823 K for 9.5 h and then further heated to an over temperature condition of 2028 K in 0.3 h. The inelastic axial and radial displacements of the cartridge walls were evaluated by resolving the von Mises strain along the corresponding directions. These calculations reveal that the maximum axial and radial displacements are expected to be about 2.9 and 0.25 mm, respectively, for both fine and coarse-grained materials at 2028 K. It was determined that these displacements occur during heat-up to temperature and creep of the cartridge is likely to be relatively insignificant irrespective of grain size. Furthermore, with a 3' tilt of the cartridge, the deflection is increased by only 0.39 gm which is negligible. Since the gap between the furnace heating elements and the cartridge is about 7.5 mm and less than the maximum radial dilation of 0.25 mm at 2028 K, it is concluded that the cartridge is unlikely to touch the furnace walls during the experiments.

Raj, S.V.↗

NASA NTRS1998

Numerical Modeling of Physical Vapor Transport in Contactless Crystal Growth Geometry

Growth from the vapor under conditions of limited contact with the walls of the growth ampoule is beneficial for the quality of the growing crystal due to reduced stress and contamination which may be caused by interactions with the growth container. The technique may be of a particular interest for studies on crystal growth under microgravity conditions: elimination of some factors affecting the crystal quality may make interpretation of space-conducted processes more conclusive and meaningful. For that reason, and as a part of our continuing studies on 'contactless' growth technique, we have developed a computational model of crystal growth process in such system. The theoretical model was built, and simulations were performed using the commercial computational fluid dynamics code, (CFD) ACE. The code uses an implicit finite volume formulation with a gray discrete ordinate method radiation model which accounts for the diffuse absorption and reflection of radiation throughout the furnace. The three-dimensional model computes the heat transfer through the crystal, quartz, and gas both inside and outside the ampoule, and mass transport from the source to the crystal and the sink. The heat transport mechanisms by conduction, natural convection, and radiation, and mass transport by diffusion and convection are modeled simultaneously and include the heat of the phase transition at the solid-vapor interfaces. As the thermal boundary condition, temperature profile along the walls of the furnace is used. For different thermal profiles and furnace and ampoule dimensions, the crystal growth rate and development of the crystal-vapor and source-vapor interfaces (change of the interface shape and location with time) are obtained. Super/under-saturation in the ampoule is determined and critical factors determining the 'contactless' growth conditions are identified and discussed. The relative importance of the ampoule dimensions and geometry, the furnace dimensions and its temperature, and the properties of the grown material are analyzed. The results of the simulations are compared with related experimental results on growth of CdTe, CdZnTe, ZnTe, PbTe, and PbSnTe crystals by this technique.

Palosz, W.↗

NASA NTRS1999

Project Description and Publications List for UAH CMMR

This research combines a state of the art X-ray Transmission Microscope, XTM, with a specially designed x-ray transparent horizontal Bridgman furnace to image (with resolutions up to 3 micrometers) the solidification of metal alloys in real-time. The objective is to obtain real-time dynamic data to provide direct measure of the solute profile in the liquid, phase coalescence and growth in the liquid, and the detailed interface morphology (e,g., dendrites and cells) during solidification. We are also enhancing the XTM data with precise solid-liquid interfacial temperature and the thermal gradient measurement techniques, and working on the application of this technology to the study of the fundamentals of solidification in microgravity. Over the last several years we have successfully imaged in real-time: interfacial-morphologies, phase growth, coalescence, incorporation of phases into the growing interface, and the solute boundary layer in the liquid at the solid-liquid interface. We have also measured true local growth rates and can evaluate segregation structures in the solid. Interfacial undercoolings are being measured either with a special Seebeck furnace or with micro-thermocouple arrays we are developing. These later techniques are presently being incorporated with the XTM furnace. This last year emphasized the investigation of the solute layer in the melt during solidification. Methods were developed to quantify the solute concentrations using x-ray absorption and to compare to predictions from simulations. In addition, work is being completed on a brass-board portable XTM that incorporates a vertical Bridgman furnace.

Kaukler, William F.↗

NASA NTRS2000

Regolith Evolved Gas Analyzer

The Regolith Evolved Gas Analyzer (REGA) is a high-temperature furnace and mass spectrometer instrument for determining the mineralogical composition and reactivity of soil samples. REGA provides key mineralogical and reactivity data that is needed to understand the soil chemistry of an asteroid, which then aids in determining in-situ which materials should be selected for return to earth. REGA is capable of conducting a number of direct soil measurements that are unique to this instrument. These experimental measurements include: (1) Mass spectrum analysis of evolved gases from soil samples as they are heated from ambient temperature to 900 C; and (2) Identification of liberated chemicals, e.g., water, oxygen, sulfur, chlorine, and fluorine. REGA would be placed on the surface of a near earth asteroid. It is an autonomous instrument that is controlled from earth but does the analysis of regolith materials automatically. The REGA instrument consists of four primary components: (1) a flight-proven mass spectrometer, (2) a high-temperature furnace, (3) a soil handling system, and (4) a microcontroller. An external arm containing a scoop or drill gathers regolith samples. A sample is placed in the inlet orifice where the finest-grained particles are sifted into a metering volume and subsequently moved into a crucible. A movable arm then places the crucible in the furnace. The furnace is closed, thereby sealing the inner volume to collect the evolved gases for analysis. Owing to the very low g forces on an asteroid compared to Mars or the moon, the sample must be moved from inlet to crucible by mechanical means rather than by gravity. As the soil sample is heated through a programmed pattern, the gases evolved at each temperature are passed through a transfer tube to the mass spectrometer for analysis and identification. Return data from the instrument will lead to new insights and discoveries including: (1) Identification of the molecular masses of all of the gases liberated from heated soil samples; (2) Identification of the asteroid soil mineralogy to aid in the selection process for returned samples; (3) Existence of oxygen in the asteroid soil and the potential for in-situ resource utilization (ISRU); and (4) Existence of water and other volatiles in the asteroid soil. Additional information is contained in the original extended abstract.

Hoffman, John H.↗

NASA NTRS2001

Growth of Solid Solution Single Crystals

The solidification of a solid solution semiconductor, having a wide separation between liquidus and solidus has been extensively studied in ground based, high magnetic field and Spacelab experiments. Two alloys of mercury cadmium telluride have been studied; with 80.0 mole percent of HgTe and 84.8 mole percent of HgTe respectively, the remainder being cadmium telluride. Such alloys are extremely difficult to grow by directional solidification on earth due to high solutal and thermal density differences that give rise to fluid flow and consequent loss of interface shape and composition. Diffusion controlled growth is therefore impossible to achieve in conventional directional solidification. The ground based experiments consisted of growing crystals in several different configurations of heat pipe furnaces, NASA's Advanced Automated Directional Solidification Furnace (AADSF), and a similar furnace incorporated in a superconducting magnet capable of operating at up to 5T. The first microgravity experiment took place during the flight of STS-62 in March 1994, with the AADSF installed on the second United States Microgravity Payload (USMP-2). The alloy was solidified at 3/4 inch per day over a 9 day period, and for the first time a detailed evaluation was performed correlating composition variations to measured residual acceleration. The second flight experiment took place in the fourth United States Microgravity Payload Mission (USMP-4) in November 1997. Due to contamination of the furnace system, analysis shows that the conditions prevailing during the experiment were quite different from the requirements requested prior to the mission. The results indicate that the sample did accomplish the desired objectives.

Lehoczky, Sandor L.↗

NASA NTRS2002

QMI: Rising to the Space Station Design Challenge

The Quench Module Insert (QMI) materials processing furnace is being designed to operate for 8000 hours over four years on the International Space Station (ISS) as part of the first Materials Science Research Rack (MSRR-1) of the Materials Science Research Facility (MSRF). The Bridgman-type furnace is being built for the directional solidification processing of metals and alloys in the microgravity environment of space. Most notably it will be used for processing aluminum and related alloys. Designing for the space station environment presents intriguing design challenges in the form of a ten-year life requirement coupled with both limited opportunities for maintenance and resource constraints in the form of limited power and space. The long life requirement has driven the design of several features in the furnace, including the design of the heater core, the selection and placement of the thermocouples, overall performance monitoring, and the design of the chill block. The power and space limitations have been addressed through a compact furnace design using efficient vacuum insulation. Details on these design features, as well as development test performance results to date, are presented.

Carswell, W. E.↗

NASA NTRS1981

Pressure Controller

EPIC is Electronic Pressure Indicating Controller produced by North American Manufacturing Company. It is a high-sensitivity device for improving combustion efficiency in industrial furnaces that interprets a signal from a pressure transducer on a furnace and regulates furnace pressure accordingly. A controller can provide savings of from five to 25 percent of an industrial user's annual furnace fuel bill.

Source record↗

NASA NTRS1987

Reactor for producing large particles of materials from gases

A method and apparatus is disclosed for producing large particles of material from gas, or gases, containing the material (e.g., silicon from silane) in a free-space reactor comprised of a tube (20) and controlled furnace (25). A hot gas is introduced in the center of the reactant gas through a nozzle (23) to heat a quantity of the reactant gas, or gases, to produce a controlled concentration of seed particles (24) which are entrained in the flow of reactant gas, or gases. The temperature profile (FIG. 4) of the furnace is controlled for such a slow, controlled rate of reaction that virtually all of the material released condenses on seed particles and new particles are not nucleated in the furnace. A separate reactor comprised of a tube (33) and furnace (30) may be used to form a seed aerosol which, after passing through a cooling section (34) is introduced in the main reactor tube (34) which includes a mixer (36) to mix the seed aerosol in a controlled concentration with the reactant gas or gases.

Flagan, Richard C.↗