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All sourcesNASA NTRSDOE OSTI
NASA NTRS2026

Prototype Demonstration of Solar-Carbothermal System to Extract Oxygen From Regolith

The Carbothermal Reduction Demonstration (CaRD) project was an effort to develop a prototype system to demonstrate the extraction of oxygen from simulated lunar regolith using concentrated solar energy and a carbothermal reaction. The prototype consisted of a deployable solar concentrator capable of tracking the sun, carbothermal reactor, fluid system, gas analysis, and a solar concentrator control system consisting of avionics and software. These subsystems were developed by multiple NASA centers and a private industry partner, Sierra Space. The various teams worked together to define requirements and interfaces to successfully assemble the complex system and demonstrate an integrated solar carbothermal process. The solar concentrator developed at Glenn Research Center (GRC) was designed to be stowed for a launch environment then deployed on the lunar surface. It utilized a crossed dragone configuration of composite mirrors to direct horizontal sunlight onto a target 90° from the incoming sunlight. The key performance parameters for the solar concentrator were efficiency and power density. The carbothermal reactor was developed by Sierra Space through a separate project called the Carbothermal Oxygen Production Reactor (COPR) where it successfully demonstrated a fully automated process in a thermal vacuum environment [1]. The fluid system needed for the carbothermal reaction was also developed by Sierra Space and successfully demonstrated in the same thermal vacuum test. The gas analysis system was developed at Kennedy Space Center (KSC) and was required to determine the amount of oxygen extracted during each test. The gas analysis system was based on the Mass Spectrometer Observing Lunar Operations (MSOLO) instrument. Avionics and software for the CaRD prototype were also developed at KSC and based on experience with MSOLO avionics and software. The control system was designed to stow, deploy, track the sun, and perform beam alignment of the concentrated light. The prototype subsystems were integrated and tested at Johnson Space Center’s (JSC) Energy Systems Test Area. A heliostat was used to direct sunlight toward the prototype in a way that is representative of the sunlight conditions at the south pole of the Moon. When concentrated sunlight was focused on simulated lunar regolith within the reactor, the gas analysis team confirmed the presence of carbon monoxide gas, which confirmed that a solar carbothermal reaction took place. The key performance parameter for the integrated prototype was grams of oxygen extracted per kilowatt hour of energy arriving at the concentrator primary mirror. The prototype design successfully demonstrated end-to-end capability and further steps to achieve a flight capable system have been defined. With lunar data, engineers would be able to design a scaled-up system capable of extracting oxygen from regolith at useful quantities for crew life support and rocket propellant. On the long term, this method of In-Situ Resource Utilization could be used to drastically reduce the cost and risk of a sustained human presence on the Moon by reducing the amount of oxygen that would have to be delivered.

Koorosh R Araghi↗
NASA NTRS2026

Prototype Demonstration of Solar Carbothermal System to Extract Oxygen from Regolith

The Carbothermal Reduction Demonstration (CaRD) project was an effort to develop a prototype system to demonstrate the extraction of oxygen from simulated lunar regolith using concentrated solar energy and a carbothermal reaction. The prototype consisted of a deployable solar concentrator capable of tracking the sun, carbothermal reactor, fluid system, gas analysis, and a solar concentrator control system consisting of avionics and software. These subsystems were developed by multiple NASA centers and a private industry partner, Sierra Space. The various teams worked together to define requirements and interfaces to successfully assemble the complex system and demonstrate an integrated solar carbothermal process. The solar concentrator developed at Glenn Research Center (GRC) was designed to be stowed for a launch environment then deployed on the lunar surface. It utilized a crossed dragone configuration of composite mirrors to direct horizontal sunlight onto a target 90° from the incoming sunlight. The key performance parameters for the solar concentrator were efficiency and power density. The carbothermal reactor was developed by Sierra Space through a separate project called the Carbothermal Oxygen Production Reactor (COPR) where it successfully demonstrated a fully automated process in a thermal vacuum environment. The fluid system needed for the carbothermal reaction was also developed by Sierra Space and successfully demonstrated in the same thermal vacuum test. The gas analysis system was developed at Kennedy Space Center (KSC) and was required to determine the amount of oxygen extracted during each test. The gas analysis system was based on the Mass Spectrometer Observing Lunar Operations (MSOLO) instrument. Avionics and software for the CaRD prototype were also developed at KSC and based on experience with MSOLO avionics and software. The control system was designed to stow, deploy, track the sun, and perform beam alignment of the concentrated light. The prototype subsystems were integrated and tested at Johnson Space Center’s (JSC) Energy Systems Test Area. A heliostat was used to direct sunlight toward the prototype in a way that is representative of the sunlight conditions at the south pole of the Moon. When concentrated sunlight was focused on simulated lunar regolith within the reactor, the gas analysis team confirmed the presence of carbon monoxide gas, which confirmed that a solar carbothermal reaction took place. The key performance parameter for the integrated prototype was grams of oxygen extracted per kilowatt hour of energy arriving at the concentrator primary mirror. The prototype design successfully demonstrated end-to-end capability and further steps to achieve a flight capable system have been defined. With lunar data, engineers would be able to design a scaled-up system capable of extracting oxygen from regolith at useful quantities for crew life support and rocket propellant. On the long term, this method of In-Situ Resource Utilization could be used to drastically reduce the cost and risk of a sustained human presence on the Moon by reducing the amount of oxygen that would have to be delivered.

Aaron Paz↗
NASA NTRS2026

Prototype Demonstration of an Integrated Solar Concentrator System and Carbothermal Reactor Using Solar Energy to Extract Oxygen from Regolith

The Carbothermal Reduction Demonstration (CaRD) project was an effort to develop a prototype system to demonstrate the extraction of oxygen from simulated lunar regolith using concentrated solar energy and a carbothermal reaction. The prototype consisted of a deployable solar concentrator capable of tracking the sun, carbothermal reactor, fluid system, gas analysis, and a solar concentrator control system consisting of avionics and software. These subsystems were developed by multiple NASA centers and a private industry partner, Sierra Space. The various teams worked together to define requirements and interfaces to successfully assemble the complex system and demonstrate an integrated solar carbothermal process. The solar concentrator developed at Glenn Research Center (GRC) was designed to be stowed for a launch environment then deployed on the lunar surface. It utilized a crossed dragone configuration of composite mirrors to direct horizontal sunlight onto a target 90° from the incoming sunlight. The key performance parameters for the solar concentrator were efficiency and power density. The carbothermal reactor was developed by Sierra Space through a separate project called the Carbothermal Oxygen Production Reactor (COPR) where it successfully demonstrated a fully automated process in a thermal vacuum environment. The fluid system needed for the carbothermal reaction was also developed by Sierra Space and successfully demonstrated in the same thermal vacuum test. The gas analysis system was developed at Kennedy Space Center (KSC) and was required to determine the amount of oxygen extracted during each test. The gas analysis system was based on the Mass Spectrometer Observing Lunar Operations (MSOLO) instrument. Avionics and software for the CaRD prototype were also developed at KSC and based on experience with MSOLO avionics and software. The control system was designed to stow, deploy, track the sun, and perform beam alignment of the concentrated light. The prototype subsystems were integrated and tested at Johnson Space Center’s (JSC) Energy Systems Test Area. A heliostat was used to direct sunlight toward the prototype in a way that is representative of the sunlight conditions at the south pole of the Moon. When concentrated sunlight was focused on simulated lunar regolith within the reactor, the gas analysis team confirmed the presence of carbon monoxide gas, which confirmed that a solar carbothermal reaction took place. The key performance parameter for the integrated prototype was grams of oxygen extracted per kilowatt hour of energy arriving at the concentrator primary mirror. The prototype design successfully demonstrated end-to-end capability and further steps to achieve a flight capable system have been defined. With lunar data, engineers would be able to design a scaled-up system capable of extracting oxygen from regolith at useful quantities for crew life support and rocket propellant. On the long term, this method of In-Situ Resource Utilization could be used to drastically reduce the cost and risk of a sustained human presence on the Moon by reducing the amount of oxygen that would have to be delivered.

Oxygen from Regolith↗
NASA NTRS1990

Production of oxygen from lunar ilmenite

The following subjects are addressed: (1) the mechanism and kinetics of carbothermal reduction of simulated lunar ilmenite using carbon and, particularly, CO as reducing agents; (2) the determination of the rate-limiting steps; (3) the investigation of the effect of impurities, particularly magnesium; (4) the search for catalysts suitable for enhancement of the rate-limiting step; (5) the comparison of the kinetics of carbothermal reduction with those of hydrogen reduction; (6) the study of the combined use of CO and hydrogen as products of gasification of carbonaceous solids; (7) the development of reduction methods based on the use of waste carbonaceous compounds for the process; (8) the development of a carbothermal reaction path that utilizes gasification of carbonaceous solids to reducing gaseous species (hydrocarbons and carbon monoxide) to facilitate the reduction reaction kinetics and make the process more flexible in using various forms of carbonaceous feeds; (9) the development of advanced gas separation techniques, including the use of high-temperature ceramic membranes; (10) the development of an optimum process flow sheet for carbothermal reduction, and comparison of this process with the hydrogen reduction scheme, as well as a general comparison with other leading oxygen production schemes; and (11) the use of new and advanced material processing and separation techniques.

Zhao, Y.↗
NASA NTRSDate not supplied

Carbothermal Reduction Demonstration (CaRD) Gas Analysis Subsystem Development

The Carbothermal Reduction Demonstration (CaRD) project is currently developing a subscale system to demonstrate the operation and performance of the carbothermal reduction process and quantify the production of molar equivalent oxygen (carbon monoxide (CO) and carbon dioxide (CO2)). Traditionally, gas chromatography (GC) systems are utilized to qualify gases due to their ability to separate the volatile compounds within the gas mixture, followed by quantification of the isolated component of interest. Despite these capabilities, GCs require consumables for their operational mobile phase and consequently are not often considered a flight-forward option. An alternative analytical technique known as mass spectrometry measures the presentence of gas phase molecules based on their mass-to-charge ratio. Residual gas analyzers (RGAs) which utilize mass spectrometry are not traditionally used to quantify analytes, but proper design and calibrations can result in a flight-forward analytical instrument capable of direct quantification of volatile gases of interest. Kennedy Space Center's role for the project is to design a gas analyzer system to detect and quantify the CO and CO2 gas produced during the carbothermal reaction utilizing a commercial version of the Mass Spectrometer Observing Lunar Operations (MSolo) instrument. MSolo is a modified commercial off-the-shelf mass spectrometer which consists of quadrupole mass filter and space rated electronics. MSolo is currently a TRL 6 technology and manifested on the PRIME-1 and VIPER missions. This paper describes leveraging MSolo based instrumentation to develop a gas analysis system for the work outlined in the 2023 International Conference on Environmental Systems (ICES) paper number 313. The design and testing of the brassboard phase of the project will be described along with the current work underway which will cover the design and preliminary test results of the prototype phase.

Ryan Patrick Gott↗
NASA NTRS2024

Carbothermal Reduction Demonstration (CaRD) Gas Analysis Subsystem Development

The Carbothermal Reduction Demonstration (CaRD) project is currently developing a subscale system to demonstrate the operation and performance of the carbothermal reduction process and quantify the production of molar equivalent oxygen via carbon monoxide (CO) and carbon dioxide (CO2). Traditionally, gas chromatography (GC) systems are utilized to quantify gases due to their ability to separate volatile compounds within the gas mixture, followed by detection of the isolated component of interest. Despite their capabilities, GCs require carrier gas consumables for their operational mobile phase and consequently are not often considered a flight-forward option. An alternative analytical technique known as mass spectrometry measures the presence of gas phase molecules without the need of carrier gas. Residual gas analyzers (RGAs), which are smaller and rugged mass spectrometers, are not traditionally used to quantify analytes as they serve more as a monitoring tool. However, proper application and calibration can result in a flight-forward analytical instrument capable of direct quantification of volatile compounds of interest. Kennedy Space Center's role for the JSC led CaRD project is to design a gas analyzer system to detect and quantify the CO and CO2 gases produced during the carbothermal reaction utilizing a commercial version of the Mass Spectrometer observing lunar operations (MSolo) instrument. MSolo is a modified commercial off-the-shelf RGA, which consists of quadrupole mass filter and space rated electronics. MSolo is currently a TRL 6 technology and manifested on the PRIME-1 and VIPER missions. This paper describes leveraging MSolo based instrumentation to develop a gas analysis system for the work outlined in the 2023 International Conference on Environmental Systems (ICES) paper number 313.

Ryan P Gott↗
DOE OSTI2024

On the product phases and the reaction kinetics of carbothermic reduction of UO 2 +C at relatively low temperatures

The synthesis of UC using carbothermic reduction of UO 2 and C mixtures has been well studied at high temperatures. However, the product phase behavior of carbothermic reduction at low temperatures (≤1773 K) is not well studied. Such a study is important as low temperatures permit single phase UC synthesis without forming secondary higher carbides, and it further supports the knowledge base of the process that needs to be used for transuranic elements such as plutonium that have high vapor pressures at elevated temperatures. Therefore, a low temperature carbothermic reduction of two different C/UO 2 molar ratios under inert and reducing environments have been studied here. Two different sample holding crucibles, alumina (Al 2 O 3 ) and graphite, were also used here to differentiate the hypostoichiometric (UC 1-a ) and oxygen dissolved (UC 1-x O x ) uranium monocarbide phases adding more details on the two systems. Also, the reaction kinetics involved in the formation of UC via the carbothermic reduction of UO 2 +C using product phases instead of evolved gases such as carbon monoxide is reported here. Under inert atmospheres but with significant oxygen partial pressures, the low temperature carbothermic reduction of UO 2 +C produced up to 90 wt.% UC 1-x O x type oxycarbides as was confirmed by Xray powder diffraction. Reducing Ar-4%H 2 environments at these temperatures were not successful in synthesizing UC as it reduces the amount of C required for the carbothermic reduction, leaving UC phase at a non-equilibrium state. Inert atmospheres with low or negligible oxygen partial pressures on the other hand produced near stoichiometric UC at high phase purity, especially at 1673 – 1773 K temperature range. An activation energy of 377±75 kJmol -1 was also calculated using product phase concentrations of the carbothermic reduction of UO 2 +C under these inert Ar (g) atmospheres.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Boron carbide amorphous solid with tunable band gap

Boron carbide B x C (x = 1/6 – 10) powders were synthesized through a microwave-assisted carbothermic reduction reaction as a potential clean energy material. Their crystallographic structures and optical properties were characterized. X-ray diffraction and electron diffraction indicated that the synthesized B x C powders were amorphous. Electron energy-loss spectroscopy demonstrated that the composition of boron and carbon was in amorphous materials, and their chemical bonding were disclosed from Raman scattering spectroscopy. Here, UV-vis absorption spectroscopy indicated that the bandgap of the bulks varied from 2.30 eV to 3.90 eV, tuned by the boron/carbon element ratio.

36 MATERIALS SCIENCE↗
NASA NTRSDate not supplied

Carbothermal Reduction Demonstration: Laser Driven Reaction in a Thermal-Vacuum Environment and Project Status

Introduction: Lunar regolith is approximately 45% oxygen by mass. The majority of the oxygen is bound in silicate minerals. The carbothermal reduction process has been proven to be effective at removing oxygen from lunar regolith simulants [1]. The Carbothermal Reduction Demonstration (CaRD) project aims to increase the Technology Readiness Level (TRL) of a combined solar concentrator and carbothermal reduction systemin order to demonstrate this technology on the lunar surface. The CaRD project is divided into two design cycles, a brass board and prototype. The status of both design cycles will be discussed, as well as concepts for how this technology can be applied to the Artemis program in the future. Brassboard Vacuum Test: For the brassboard demonstration, a 2 kW Nd-YAG laser was used to heat lunar regolith simulant within a carbothermal reactor developed by Sierra Space. The reactor was placed inside of a 15 ft thermal vacuum chamber at the Johnson Space Center. The resulting reaction products were analyzed using both a gas chromotograph and mass spectrometer provided by Kennedy Space Center. Thermal data was also collected. Prototype Design: For the prototype, the CaRD team will perform another thermal vacuum test at JSC using the same interfaces and assets developed for the brassboard but will test a new carbothermal reactor design that Sierra Space is developing through the Carbothermal Oxygen Production Reactor (COPR) Tipping Point project that will include a means to autonomously move regolith in and out of the reactor. In addition, a deployable solar concentrator is being developed by Glenn Research Center using mirrors produced by Carbon Mirror Applications. The solar concentrator will be used to deliver solar energy into a carbothermal reactor to melt regolith and extract oxygen. Avionics and software for the concentrator are being developed by Kennedy Space Center. Future Concepts: An ongoing task within the CaRD project is to update models that can be used to determine the mass, power, and size of In-Situ Resource Utilization concepts at various scales. These models can now be used to analyze alternatives for future applications based on the latest available data.

A J Paz↗
DOE OSTI2020

Synthesis and flash sintering of (Hf 1-x Zr x )B 2 solid solution powders

(Hf 1-x Zr x )B 2 solid solution powders were synthesized by two methods. First, solution-based processing of HfCl 4 , ZrCl 4 , sucrose, and H 3 BO 3 was conducted followed by heat treatment in Argon to carry out the carbothermal reduction (CTR) reaction to form the diboride powders. Alternatively, in the so-called borohydride reduction (BHR) method, HfCl 4 , ZrCl 4 and NaBH 4 were mixed in an Argon glove box followed by heat treatment in Argon at 700-1500°C. The synthesized powders were characterized by XRD, SEM, TEM, EDS, and TGA, and the influence of different parameters such as starting composition, heat treatment temperature and time on products characteristics were revealed. Both CTR and BHR solid solution powders were then consolidated within ~5 min in a homemade flash sintering (FS) setup. Here, the composition, microstructure, hardness, and thermal-oxidation properties of flash sintered ceramics were characterized, and the implication of this study and directions for future research were discussed.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Synthesis and Flash Sintering of (Hf1-xZrx)B2 Solid Solution Fine Powders

Fine powders of (Hf1-xZrx)B2 solid solution were synthesized by two methods. In the first one, solution-based processing of HfCl4, ZrCl4, sucrose and H3BO3 was carried out followed by heat treatment (e.g., at 1500 °C for 1 h) in Argon to achieve the carbothermal reduction (CTR) reaction to form the boride solid solution. In the second one, called boron hydride reduction (BHR) method, HfCl4, ZrCl4 and NaBH4 were directly mixed in a glove box followed by heat treatment in Argon at elevated temperatures from 700 to 1500 °C. In addition, the powders synthesized via both methods were flash sintered without sample preheating in a homemade setup. The synthesized powders as well as the flash sintered bulk ceramics were characterized using different techniques including XRD, SEM, EDS, TEM, TGA-DSC, and Vickers hardness test to reveal the inter-relationships between starting materials composition, processing conditions, and the resulting materials microstructure and physical/chemical properties.

Belisario, Jose↗
DOE OSTI2022

High-entropy boride–carbide ceramics by sequential boro/carbothermal synthesis

We report a dual-phase high-entropy boride/carbide ceramic with fine grain size was synthesized by a sequential boro/carbothermal process. In the first step, a Hf-Nb-Ta-Ti-Zr-containing carbide was synthesized by carbothermal reduction of oxides followed by reaction of the carbide with B4C and ZrH2 to convert part of the carbide to boride. The resulting composition was ~29 vol% high-entropy boride with an average grain size of ~1.1 µm. Solid solution formation occurred at the densification temperature of 1900°C resulting in a relative density higher than 99%. The Vickers’ hardness was 26.5 ± 1.4 GPa. This is the first report of synthesizing dual-phase boride-carbide high-entropy ceramics from carbothermally synthesized, high-entropy carbide powders.

36 MATERIALS SCIENCE↗
NASA NTRS1992

Reduction of iron-bearing lunar minerals for the production of oxygen

The kinetics and mechanism of the reduction of simulants of the iron-bearing lunar minerals olivine ((Fe,Mg)2SiO4), pyroxene ((Fe,Mg,Ca)SiO3), and ilmenite (FeTiO3) are investigated, extending previous work with ilmenite. Fayalite is reduced by H2 at 1070 K to 1480 K. A layer of mixed silica glass and iron forms around an unreacted core. Reaction kinetics are influenced by permeation of hydrogen through this layer and a reaction step involving dissociated hydrogen. Reaction mechanisms are independent of Mg content. Augite, hypersthene, and hedenbergite are reduced in H2 at the same temperatures. The products are iron metal and lower iron silicates mixed throughout the mineral. Activation energy rises with calcium content. Ilmenite and fayalite are reduced with carbon deposited on partially reduced minerals via the CO disproportionation reaction. Reduction with carbon is rapid, showing the carbothermal reduction of lunar minerals is possible.

Massieon, Charles↗
NASA NTRS1992

The onsite manufacture of propellant oxygen from lunar resources

The Aerojet carbothermal process for the manufacture of oxygen from lunar materials has three essential steps: the reduction of silicate with methane to form carbon monoxide and hydrogen; the reduction of carbon monoxide with hydrogen to form methane and water; and the electrolysis of water to form hydrogen and oxygen. The reactions and the overall process are shown. It is shown with laboratory experimentation that the carbothermal process is feasible. Natural silicates can be reduced with carbon or methane. The important products are carbon monoxide, metal, and slag. The carbon monoxide can be completely reduced to form methane and water. The water can be electrolyzed to produce hydrogen and oxygen. A preliminary engineering study shows that the operation of plants using this process for the manufacture of propellant oxygen has a large economic advantage when the cost of the plant and its operation is compared to the cost of delivering oxygen from Earth.

Rosenberg, Sanders D.↗
NASA NTRSDate not supplied

Carbothermal Reduction Demonstration (CaRD)

Introduction: Lunar regolith is approximately 45% oxygen by mass. The majority of the oxygen is bound in silicate minerals. The carbothermal reduction process has been proven to be effective at removing oxygen from lunar regolith simulants. The Carbothermal Reduction Demonstration (CaRD) project aims to increase the Technology Readiness Level (TRL) of a combined solar concentrator and carbothermal reduction systemin order to demonstrate this technology on the lunar surface. The CaRD project is divided into two design cycles, a brass board and prototype. The status of both design cycles will be discussed, as well as concepts for how this technology can be applied to the Artemis program in the future. Brassboard Vacuum Test: For the brassboard demonstration, a 2 kW Nd-YAG laser was used to heat lunar regolith simulant within a carbothermal reactor developed by Sierra Space. The reactor was placed inside of a 15 ft thermal vacuum chamber at the Johnson Space Center. The resulting reaction products were analyzed using both a gas chromotograph and mass spectrometer provided by Kennedy Space Center. Thermal data was also collected. Prototype Design: For the prototype, the CaRD team will perform another thermal vacuum test at JSC using the same interfaces and assets developed for the brassboard but will test a new carbothermal reactor design that Sierra Space is developing through the Carbothermal Oxygen Production Reactor (COPR) Tipping Point project that will include a means to autonomously move regolith in and out of the reactor. In addition, a deployable solar concentrator is being developed by Glenn Research Center using mirrors produced by Carbon Mirror Applications. The solar concentrator will be used to deliver solar energy into a carbothermal reactor to melt regolith and extract oxygen. Avionics and software for the concentrator are being developed by Kennedy Space Center. Future Concepts: An ongoing task within the CaRD project is to update models that can be used to determine the mass, power, and size of In-Situ Resource Utilization concepts at various scales. These models can now be used to analyze alternatives for future applications based on the latest available data.

Aaron Paz↗
NASA NTRS1989

Production of oxygen from lunar ilmenite

The overall objective of this project was to develop a novel carbothermal reduction process for production of oxygen from lunar ilmenite. The specific objective was to use a reaction sequence in which a wide variety of carbonaceous compounds (including carbonaceous wastes) can be used as reducing agents. During the first phase, two reactor systems were designed, constructed, and operated to study the reaction fundamental important in this process. One system is a small fluidized bed, and the other is a thermo-gravimetric reactor system. Preliminary experiments on synthetic ilmenite are conducted to study the effect of carbon type, carbon loading, temperature, and gas flow rate. Results indicate that a reaction path based on carbon gasification can be used to promote the overall kinetics. A unique temperature and concentration-programmed reaction procedure was being developed for rapid parametric study of the process.

Shadman, F.↗
DOE OSTI2023

Crystallographic Study of Product Phases of Carbothermic Reduction and Nitridation of Hafnium Dioxide

Details of the carbothermic reduction/nitridation to synthesize hafnium nitride (HfN) and hafnium carbide (HfC) are scarce in the literature. Therefore, this current study was carried out to evaluate two pathways for synthesizing these two refractory materials: direct nitridation and carbothermic reduction/nitridation. Two mixtures of hafnium dioxide and carbon with C/HfO 2 molar ratios of 2.15 and 3.1 were nitridized directly using flowing nitrogen gas at elevated temperatures (1300–1700 °C). The 3.1 C/HfO 2 molar ratio mixture was also carbothermically reduced under flowing argon gas to synthesize HfC, which was converted into HfN by introducing a nitridation step under both N 2(g ) and N 2(g) -10% H 2(g) . X-ray diffraction results showed the formation of HfN at 1300 and 1400 °C and HfC 1–y N y at ≥1400 °C under direct nitridation of samples using a C/HfO 2 molar ratio of 2.15. These phase analysis data together with lower lattice strain and greater crystallite sizes of HfC 1–y N y that formed at higher temperatures suggested that the HfC 1–y N y phase is preferred over HfN at those temperatures. Carbothermic reduction of 3.1 C/HfO 2 molar ratio samples under an inert atmosphere produced single-phased HfC with no significant levels of dissolved oxygen. In conclusion, carbothermic reduction nitridation made two phases of different carbon levels (HfC 1–y N y and HfC 1–y 'N y ', where y' < y), while direct nitridation produced a single HfC 1–y N y phase under both N 2 and N 2 -10% H 2 cover gas environments.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗