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All sourcesNASA NTRSDOE OSTI
NASA NTRS1999

Thermophysical Property Measurements of Molten Semiconductors in 1-g and Reduced-g Condition

Understanding and controlling the formation kinetics of varieties of crystal imperfections such as point defects, non uniform distribution of doping atoms, and impurity atoms in growing crystals are very important. Theoretical (numerical) modeling of the crystal growth process is an essential step to achieving these objectives. In order to obtain reliable modeling results, input parameters, i.e. various thermophysical parameters, must be accurate. The importance of accurate thermophysical properties of semiconductors in crystal growth cannot be overly emphasized. The total hemispherical emissivity, for instance, has a dramatic impact on the thermal environment. It determines the radiative emission from the surface of the melt which determines to a large extent the profile of the solidified crystal. In order to understand the convection and the turbulence in a melt, viscosity becomes an important parameter. The liquid surface tension determines the shape of the liquid-atmosphere interface near the solid-liquid-atmosphere triple point. Currently used values for these parameters are rather inaccurate, and this program intends to provide more reliable measurements of these thermophysical properties. Thus, the objective of this program is in the accurate measurements of various thermophysical properties which can be reliably used in the modeling of various crystal growth processes. In this program, thermophysical properties of molten semiconductors, such as Si, Ge, Si-Ge, and InSb will be measured as a function of temperature using the High Temperature Electrostatic Levitator at JPL. Each material will be doped by different kinds of impurities at various doping levels. Thermophysical properties which will be measured include: density, thermal expansion coefficient, surface tension, viscosity, specific heat, hemispherical total emissivity, and perhaps electrical and thermal conductivities. Many molten semiconductors are chemically reactive with crucibles. As a result, these dispersed impurities in the melts tend to substantially modify the properties of pure semiconductors. Sample levitation done in a vacuum clearly helps maintain the sample purity. However, in the 1-g environment, all gravity caused effects such as convection, sedimentation and buoyancy are still present in the sample. In addition, large forces needed to levitate a sample in the presence of the gravity can cause additional flows in the melt. The use of the High Temperature Electrostatic Levitator (HTESL) for the present research is a recent development and little is known about the flows induced by the electrostatic forces. In this ground base program, we will define the limits of HTESL technology as various thermophysical properties of molten semiconductors are measured.

Rhim, Won-Kyu↗
NASA NTRS2000

Rotating Molten Metallic Drops and Related Phenomena: A New Approach to the Surface Tension Measurement

Molten aluminum and tin drops were levitated in a high vacuum by controlled electric fields, and they were systematically rotated by applying by a rotating magnetic field. When the evolution of the drop shape was measured as a function of rotation frequency, it agreed quantitatively well with the Brown and Scriven's theoretical prediction. The normalized rotation frequencies at the bifurcation point agreed with the predicted value 0.559, within 2%. An anomalous phenomenon which totally deviated from the prediction was observed in rotating molten tin drops when they were kept in a high rotation rate for several hours. No anomaly was observed in aluminum drops when they underwent similar condition. It was speculated that under the strong centrifugal force in the drop the tin isotopes must be separating. Since Al-27 is essentially the only naturally abundant isotope in the aluminum drops, the same anomaly is not expected. Based on the shape deformation of a rotating drop, an alternate approach to the surface tension measurement was verified. This new surface tension measurement technique was applied to a glassforming alloy, Zr(41.2)Ti(13.8)Cu(12.5)Ni(10.0)Be(22.5) in its highly viscous states. Also demonstrated in the paper was a use of a molten aluminum drop to verify the Busse's prediction of the influence of the drop rotation on the drop oscillation frequency.

Rhim, Won-Kyu↗
NASA NTRS2002

Structural Fluctuations and Thermophysical Properties of Molten II-VI Compounds

The objectives of the project are to conduct ground-based experimental and theoretical research on the structural fluctuations and thermophysical properties of molten II-VI compounds to enhance the basic understanding of the existing flight experiments in microgravity materials science programs as well as to study the fundamental heterophase fluctuation phenomena in these melts by: 1) conducting neutron scattering analysis and measuring quantitatively the relevant thermophysical properties of the II-VI melts (such as viscosity, electrical conductivity, thermal diffusivity and density) as well as the relaxation characteristics of these properties to advance the understanding of the structural properties and the relaxation phenomena in these melts and 2) performing theoretical analyses on the melt systems to interpret the experimental results. All the facilities required for the experimental measurements have been procured, installed and tested. Thermal diffusivity of molten tellurium has been measured by a laser flash method in the temperature range of 500 C to 900 C. The measured diffusivity as a function of temperature agrees fairly well with published data. However, a relaxation phenomenon, which shows a slow drift of the measured thermal conductivity toward the equilibrium value after cooling of the melt, was observed for the first time. An apparatus based on the transient torque induced by a rotating magnetic field has been developed to determine the viscosity and electrical conductivity of semiconducting liquids. Viscosity measurements on molten tellurium showed a similar relaxation behavior to the measured diffusivity. The density and volume expansion coefficients for pure Te and HgTe melts were measured as a function of temperature using a pycnometric method. A density maximum was found for both melts but no relaxation behavior was observed. Neutron scattering experiments were performed on the HgTe and HgZnTe melts and the results on pair distribution showed better resolution than previously reported. A simple kinetic theory, which contains the formation reactions of Te polymerization that increases the molecular weight, was proposed to interpret the relaxation behavior of HgZnTe viscosity data.

Su, Ching-Hua↗
NASA NTRS1981

Continuous replenishment of molten semiconductor in a Czochralski-process, single-crystal-growing furnace

A replenishment crucible is mounted adjacent the usual drawing crucible, from which a monocrystalline boule is drawn according to the Czochralski method. A siphon tube for molten semiconductor transfer extends from the replenishment crucible to the drawing crucible. Each crucible is enclosed within its own hermetic shell and is provided with its own heater. The siphon tube is initially filled with molten semiconductor by raising the inert atmospheric pressure in the shell surrounding the replenishment crucible above that surrounding the drawing crucible. Thereafter, adjustment of the level of molten semiconductor in the drawing crucible may be achieved by adjusting the level in either crucible, since the siphon tube will establish the same level in both crucibles. For continuous processing, solid semiconductor may be added to and melted in the replenishment crucible during the process of drawing crystals from the drawing crucible. A constant liquid level of melted semiconductor is maintained in the system by an optical monitoring device and any of several electromechanical controls of the rate of replenishment or crucible height.

Fiegl, George↗
NASA NTRS2009

Production of Oxygen from Lunar Regolith by Molten Oxide Electrolysis

This paper describes the use of the molten oxide electrolysis (MOE) process for the extraction of oxygen for life support and propellant, and silicon and metallic elements for use in fabrication on the Moon. The Moon is rich in mineral resources, but it is almost devoid of chemical reducing agents, therefore, molten oxide electrolysis is ideal for extraction, since the electron is the only practical reducing agent. MOE has several advantages over other extraction methods. First, electrolytic processing offers uncommon versatility in its insensitivity to feedstock composition. Secondly, oxide melts boast the twin key attributes of highest solubilizing capacity for regolith and lowest volatility of any candidate electrolytes. The former is critical in ensuring high productivity since cell current is limited by reactant solubility, while the latter simplifies cell design by obviating the need for a gas-tight reactor to contain evaporation losses as would be the case with a gas or liquid phase fluoride reagent operating at such high temperatures. Alternatively, MOE requires no import of consumable reagents (e.g. fluorine and carbon) as other processes do, and does not rely on interfacing multiple processes to obtain refined products. Electrolytic processing has the advantage of selectivity of reaction in the presence of a multi-component feed. Products from lunar regolith can be extracted in sequence according to the stabilities of their oxides as expressed by the values of the free energy of oxide formation (e.g. chromium, manganese, Fe, Si, Ti, Al, magnesium, and calcium). Previous work has demonstrated the viability of producing Fe and oxygen from oxide mixtures similar in composition to lunar regolith by molten oxide electrolysis (electrowinning), also called magma electrolysis having shown electrolytic extraction of Si from regolith simulant. This paper describes recent advances in demonstrating the MOE process by a joint project with participation by NASA KSC and MSFC, and Ohio State University and MIT. Progress in measuring cell efficiency for oxygen production, development of non reacting electrodes, and cell feeding and withdrawal will be discussed.

Curreri, Peter A.↗
NASA NTRS2009

Ceramics for Molten Materials Transfer

The paper reviews the main issues associated with molten materials transfer and handling on the lunar surface during the operation of a hig h temperature electrowinning cell used to produce oxygen, with molten iron and silicon as byproducts. A combination of existing technolog ies and purposely designed technologies show promise for lunar exploi tation. An important limitation that requires extensive investigation is the performance of refractory currently used for the purpose of m olten metal containment and transfer in the lunar environment associa ted with electrolytic cells. The principles of a laboratory scale uni t at a scale equivalent to the production of 1 metric ton of oxygen p er year are introduced. This implies a mass of molten materials to be transferred consistent with the equivalent of 1kg regolithlhr proces sed.

Standish, Evan↗
NASA NTRS2010

Direct Electrolysis of Molten Lunar Regolith for the Production of Oxygen and Metals on the Moon

When considering the construction of a lunar base, the high cost ($ 100,000 a kilogram) of transporting materials to the surface of the moon is a significant barrier. Therefore in-situ resource utilization will be a key component of any lunar mission. Oxygen gas is a key resource, abundant on earth and absent on the moon. If oxygen could be produced on the moon, this provides a dual benefit. Not only does it no longer need to be transported to the surface for breathing purposes; it can also be used as a fuel oxidizer to support transportation of crew and other materials more cheaply between the surface of the moon, and lower earth orbit (approximately $20,000/kg). To this end a stable, robust (lightly manned) system is required to produce oxygen from lunar resources. Herein, we investigate the feasibility of producing oxygen, which makes up almost half of the weight of the moon by direct electrolysis of the molten lunar regolith thus achieving the generation of usable oxygen gas while producing primarily iron and silicon at the cathode from the tightly bound oxides. The silicate mixture (with compositions and mechanical properties corresponding to that of lunar regolith) is melted at temperatures near 1600 C. With an inert anode and suitable cathode, direct electrolysis (no supporting electrolyte) of the molten silicate is carried out, resulting in production of molten metallic products at the cathode and oxygen gas at the anode. The effect of anode material, sweep rate, and electrolyte composition on the electrochemical behavior was investigated and implications for scale-up are considered. The activity and stability of the candidate anode materials as well as the effect of the electrolyte composition were determined. Additionally, ex-situ capture and analysis of the anode gas to calculate the current efficiency under different voltages, currents and melt chemistries was carried out.

Sirk, Aislinn H. C.↗
NASA NTRS2008

Advances in Molten Oxide Electrolysis for the Production of Oxygen and Metals from Lunar Regolith

As part of an In-Situ Resource Utilization infrastructure to sustain long term-human presence on the lunar surface, the production of oxygen and metals by electrolysis of lunar regolith has been the subject of major scrutiny. There is a reasonably large body of literature characterizing the candidate solvent electrolytes, including ionic liquids, molten salts, fluxed oxides, and pure molten regolith itself. In the light of this information and in consideration of available electrolytic technologies, the authors have determined that direct molten oxide electrolysis at temperatures of approx 1600 C is the most promising avenue for further development. Results from ongoing studies as well as those of previous workers will be presented. Topics include materials selection and testing, electrode stability, gas capture and analysis, and cell operation during feeding and tapping.

Sadoway, Donald R.↗
NASA NTRS2019

Thermochemistry of Protective Coatings and Molten Silicate Debris

The durability of gas-turbine engine components can be significantly affected by the ingestion of siliceous particles, which can melt at high temperature and corrode protective coatings that are essential for long life requirements. The silicate debris consists mainly of CaO-MgO-Al2O3-SiO2 (CMAS) and is usually ingested by aircraft engines during and after take-off, sticking to their hot surfaces and resulting in the formation of calcium rare-earth silicate oxyapatites. The thermochemistry of coatings and their reaction products with molten silicate debris are crucial to understand in order to improve the durability of gas-turbine engines. Here we discuss results of high temperature drop solution calorimetry, drop-and-catch calorimetry (DnC) and differential thermal analysis (DTA) techniques for the thermodynamic properties of both thermal barrier coatings (TBCs) and environmental barrier coatings (EBCs) and their reaction with CMAS compositions. The enthalpies of solution of Y2Si2O7, Yb2Si2O7, 31YSZ, and 16RESZ based coatings and the oxyapatite are moderately positive. However, oxyapatite formation is only favorable over coating dissolution in terms of enthalpy for 7YSZ. The enthalpies of mixing between the coatings and the molten silicate are less exothermic for Yb2Si2O7 and CaYb4Si3O13 than for 7YSZ, indicating lower energetic stability of the latter against molten silicate corrosion. We also report for the first time the calorimetric measurements of the enthalpies of formation of rare-earth silicate based EBC coatings and oxyapatites (rare-earth, RE = Y, Yb, Gd, Dy, Er, Nd and Sm).

Costa, Gustavo↗
NASA NTRSDate not supplied

Molten Salt Lattice Confinement Fusion (LCF) Fast Fission Reactor for Lunar and Planetary Surface Power

Molten salt fission reactors (MSR) have been suggested for lunar and planetary surface power systems. They have the advantage of operating at high temperature, for efficient thermal-electrical conversion, low pressure, long-lived with high nuclear fuel burnup. MSR are often designed to breed fissile 233U from natural 232Th by neutron capture and  decay via: 232Th(n,)233Th(,)233Pa(,)233U Unfortunately, this process requires 233Pa isotope separation and segregation to decay to 233U. This requirement prevents additional neutron capture that interferes with 233U breeding. Instead, Wooley’s sub-critical, fast fission, molten salt reactor would use externally generated tokamak fusion neutrons1,2 to fission all actinides.We propose a simpler fusion-fast-fission sub-critical reactor that generates fast neutrons in situ from lattice confinement fusion (LCF) to fission fertile and fissile actinides. This hybrid reactor doesn't require enriched 235U fissile pins to initiate fis-sion reactions, nor 233Pa separation and segregation during operation. Like Wooley’s, this hybrid reactor “burns” natural uranium (238U) or thorium (232Th) which avoids uranium enrichment and additional fissile material launch safety and security costs. The LCF neutron source is initiated by bremsstrahlung photoneutrons (Fig. 1)3 or isotopic neutron sources in electron-screened lattices (Fig. 2)4,5. Alternatively, the electrolytic Pd-deuterium co-deposition6protocol fast fissions7 both 232Th and 238U. However, an aqueous electrolyte-based system, without pressurization similar to conventional pressurized water fission reactors, is incapable of high temperatures due to the boiling point of the electrolyte slightly over 100 C. Molten salts can be used instead as was demonstrated at the University of Hawaii8 using a variety of Ni and Pd cathodes in lithiated, hydrided and deuterated salts. These salts have melting points often exceeding 500C making them suitable to efficiently produce electrical power9 through either Advanced Stirling Genera-tors (< 100 kWe) or closed-Brayton Cycle (> 100 kWe). This hybrid reactor could power a wide range of lunar or Martian applications from unmanned in-struments, to charging vehicles and entire facilities such as human habitats or in situ resource utilization. The power conversion cycles are Carnot Cycle limited, but generally 30% efficient at best. However, waste heat on the moon or Mars is important to surviving either two-week lunar nights or Martian nights as well as providing process heat for mineral extraction and “living off the land”

Lawrence Forsley↗
NASA NTRS2023

Galvanic Protected Anode Materials for Molten Regolith Electrolysis

This effort aimed to explore the use of refractory alloys as long-lifetime electrode materials for use in a molten regolith electrolysis (MRE) reactor, a technology that can produce oxygen (O2) from regolith. To find a material capable of withstanding the high temperatures and corrosive nature of molten regolith, first-principles thermodynamic calculations were performed on platinum group metals in the presence of iron (Fe) and silicon (Si) to determine favorable compositions for resisting unwanted secondary phases that could form on the surface of the material. As a result of these first-principles calculations, the kinetic properties of elements such as aluminum (Al), Fe, and Si can be more easily derived, which would provide insight into the longevity of such a material when used in an MRE reactor. The effort funded by this CIF project mapped the entire phase diagram of platinum group metals, which is beneficial not only to MRE where high temperatures and molten material are present, but also aerospace applications like turbine materials, terrestrial metal processing techniques, and energy storage applications. This project narrowed a broad spectrum of refractory metals down to a small list of alloys that would be able to survive not only the high temperatures of an MRE reactor, but also the thermodynamic forces that would cause inferior alloys to form secondary phases, which would ultimately consume the electrodes of the reactor. This research needs to be followed up with experimental demonstrations of these alloys in an MRE environment.

Kevin Grossman↗
NASA NTRS2025

Thermochemical Stability of Ca2Yb8(SiO4)6O2 Apatite in Presence of Molten Calcium-Magnesium-AluminoSilicate (CMAS)

Thermochemical stability of ytterbium silicon oxyapatite Ca 2 Yb 8 (SiO 4 ) 6 O 2 (CYbS) in the presence of molten calcium-magnesium aluminosilicate (CMAS) has been investigated at elevated temperatures. CYbS apatite powder was synthesized from the constituent oxides via solid state reaction method. Hot pressed apatite substrates were exposed to molten CMAS at 1200, 1300, and 1400 °C for 1, 10, and 50 h. Development of phases in the interaction region of the heat-treated specimens was monitored using scanning electron microscopy, transmission electron microscopy, high angle annular dark field imaging, selected area electron diffraction and energy dispersive X-ray spectroscopy. Monoclinic cyclosilicate Ca 3 Yb 2 (Si 3 O 9 ) 2 formed from interaction of CYbS apatite with CaO in the CMAS melt at the apatite-CMAS reaction front and continued to nucleate and grow within the residual CMAS in diffusion couples annealed for 1-50 h at 1200 °C and those heat treated at 1300 °C for 1 h. Residual CMAS was Ca-depleted when cyclosilicate was present. Dendritic wollastonite CaSiO 3 was observed within the residual CMAS in couples annealed at 1200 and 1300 °C. Ingress of molten CMAS, because of its exponential decrease in viscosity, occurred through open pores and along the grain boundaries of the apatite substrates without any detectable chemical reaction at 1300 and 1400 °C. Results of this study indicate that Ca 2 Yb 8 (SiO 4 ) 6 O 2 apatite has the potential to mitigate the CMAS corrosion up to about 1200 °C but not at higher temperatures.

X-ray diffraction↗
NASA NTRS2026

Thermochemical Stability of Ca2Yb8(SiO4)6O2 Apatite in Presence of Molten Calcium-Magnesium-Aluminosilicate (CMAS)

Thermochemical stability of ytterbium silicon oxyapatite Ca 2 Yb 8 (SiO 4 ) 6 O 2 (CYbS) in the presence of molten calcium-magnesium aluminosilicate (CMAS) has been investigated at elevated temperatures for consideration as a thermal and environmental barrier coating (T/EBC) material. CYbS apatite powder was synthesized from the constituent oxides via a solid-state reaction method. Hot-pressed apatite substrates were exposed to molten CMAS at 1200, 1300, and 1400 °C for 1, 10, and 50 h. Development of phases in the interaction region of the heat-treated specimens was monitored using scanning electron microscopy, transmission electron microscopy, high-angle annular dark-field imaging, selected area electron diffraction, and energy dispersive x-ray spectroscopy. Monoclinic cyclosilicate Ca 3 Yb 2 (Si 3 O 9 ) 2 formed from interaction of CYbS apatite with CaO in the CMAS melt at the apatite-CMAS reaction front and continued to nucleate and grow within the residual CMAS in diffusion couples annealed for 1 to 50 h at 1200 °C as well as in those heat treated at 1300 °C for 1 h. Residual CMAS was depleted of Ca when cyclosilicate was present. Dendritic wollastonite (CaSiO3) was observed within the residual CMAS in couples annealed at 1200 and 1300 °C. Ingress of molten CMAS, because of its exponential decrease in viscosity, occurred through open pores and along the grain boundaries of the apatite substrates without any detectable chemical reaction at 1300 and 1400 °C. Results of this study indicate that Ca 2 Yb 8 (SiO 4 ) 6 O 2 apatite has the potential to mitigate the CMAS corrosion up to about 1200 °C but not at higher temperatures.

Narottam P Bansal↗
NASA NTRS2023

Long Life Molten Salt Battery for NASA Venus Application

A development program is being conducted at Advanced Thermal Batteries (ATB) to create a low discharge rate, long life, molten salt battery for a NASA Venus surface probe. Battery goals are 60 days continuous operation at +25V +0/-6 volts and -25V +6/-0 Volts under severe environments of 465°C, 92 atm pressure, and corrosive sulfur dioxide in a super critical carbon dioxide atmosphere. Conveniently, molten salt thermal battery electrochemistry starts to operate efficiently at 330°C. However, a major barrier to direct application of existing thermal battery technology is the high self-discharge rate, resulting in lifetimes in only minutes, not days. The best performance to date, which meets the required voltage regulation, has been a lithium silicon (LiSi) alloy anode discharging through all three voltage plateau versus an iron monosulfide (FeS) cathode. In order to perform reproducibly, additional engineering controls within the battery design are required to limit cell–to–cell parasitic discharge mechanisms. Results of these trials have improved the efficiency and manufacturability of the design.

Thermal Battery↗
NASA NTRS1975

Stress corrosion cracking of Ti-8Al-1 Mo-1V in molten salts

The stress corrosion cracking (SCC) behavior of Ti-8Al-1 Mo-1V has been studied in several molten salt environments. Extensive data are reported for the alloy in highly pure LiCl-KCl. The influence of the metallurgical heat treatment and texture, and the mechanical microstructure show similarities with aqueous solutions at lower temperature. The fracture path and cracking modes are also similar to that found in other environments. The influence of H2O and H(-) in molten LiCl-KCl lead to the conclusion that hydrogen does not play a major role in crack extension in this environment.

Smyrl, W. H.↗
NASA NTRS1976

Does Mercury have a molten core

The question of whether or not Mercury could contain a molten metallic core is investigated by studying the possible thermal evolution of a metallic core in that planet. The calculations involve the solution of the equation of heat conduction for a spherically symmetric body with internal heat sources, modifications to take account of the latent heat of fusion as well as the redistribution of radioactive heat sources as a consequence of melting, the terrestrial Fe/U ratio, and a Th/U ratio of 3.7. The temperature profile predicted by the calculations for a period of 4.6 billion years indicates that the inner 1400 km of the core would now be solid while the outer 500 km would be molten. It is emphasized that this result is a direct consequence of a discontinuity in melting temperatures at the core-mantle boundary and that although a dynamo is possible, it would have to be driven mechanically rather than by thermal convection.

Fricker, P. E.↗
NASA NTRS1977

Thermal energy storage heat exchanger: Molten salt heat exchanger design for utility power plants

The use of thermal energy storage (TES) in the latent heat of molten salts as a means of conserving fossil fuels and lowering the cost of electric power was evaluated. Public utility systems provided electric power on demand. This demand is generally maximum during late weekday afternoons, with considerably lower overnight and weekend loads. Typically, the average demand is only 60% to 80% of peak load. As peak load increases, the present practice is to purchase power from other grid facilities or to bring older less efficient fossil-fuel plants on line which increase the cost of electric power. The widespread use of oil-fired boilers, gas turbine and diesel equipment to meet peaking loads depletes our oil-based energy resources. Heat exchangers utilizing molten salts can be used to level the energy consumption curve. The study begins with a demand analysis and the consideration of several existing modern fossil-fuel and nuclear power plants for use as models. Salts are evaluated for thermodynamic, economic, corrosive, and safety characteristics. Heat exchanger concepts are explored and heat exchanger designs are conceived. Finally, the economics of TES conversions in existing plants and new construction is analyzed. The study concluded that TES is feasible in electric power generation. Substantial data are presented for TES design, and reference material for further investigation of techniques is included.

Ferarra, A.↗