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High-burnup Experiments in Reactivity Initiated Accidents (HERA)

High-burnup Experiments in Reactivity-initiated Accidents (HERA) is a joint experimental program (JEEP) operating within the United States (U.S.) Nuclear Energy Agency’s (NEA’s) framework for irradiation experiments (FIDES). HERA is dedicated to the understanding of light water reactor (LWR) fuel performance at high burnup under reactivity-initiated accidents (RIA). In-pile RIA experiments have been performed on high-burnup fuels (e.g., above 60 gigawatt days per metric ton of uranium [GWd/MTU]) in the CABRI reactor at the Cadarache site in southern France, and the Nuclear Safety Research Reactor (NSRR) in Japan. However, most of these experiments have taken place with heavily corroded Zircaloy claddings with pulse widths that are narrower (e.g., 5 ms – 30 ms full-width-half-max [FWHM]) than what would be likely in a commercial LWR (e.g., 30 ms – 80 ms FWHM). A few tests were performed in the CABRI facility with FWHM up to 76 ms, though only one “blistered” rod experienced cladding failure. Heavy waterside corrosion and narrow pulse widths are both known to increase the vulnerability of LWR fuel to pellet cladding mechanical interaction (PCMI). The HERA proposal is designed to: (1) quantify the impact of pulse width on fuel performance, offering new insight into the applicability of existing data; (2) generate new data on high burnup fuel under pulse conditions prototypic of LWRs; (3) quantify the additional margin provided by modern cladding alloys to PCMI failure limits; and (4) offer improved data for modelers using specially designed tests that eliminate key uncertainties in high-burnup fuel tests.

(HERA)↗

SAM Two-Phase Flow Model Development and Applications for Operational Transients in Advanced Reactors

As advanced nuclear technologies continue to develop, the need for the flexible operation and generation of these advanced reactors becomes necessary to maximize economic potential. As large-scale experiments are not always feasible, modeling and simulations of advanced reactors play a crucial role in design optimization and analysis. The SAM (System Analysis Module) code developed at Argonne National Laboratory is a state-of-the-art system-level thermal-hydraulic code aimed at simulating advanced reactor systems. Recent code developments have implemented two-phase flow modeling using the homogeneous equilibrium model, and a new steam generator component has been developed to utilize the two-phase flow implementation. In addition to verification tests, a load-following simulation was performed to model a realistic load-following transient in a proposed integrated system consisting of a conceptual advanced reactor known as the Advanced Burner Test Reactor (ABTR) and thermal energy storage (TES) tanks. The integrated system model uses two large TES tanks designed for sodium and a model helical coil steam generator to simulate the operational load-following transient. The flow rates of the feedwater and secondary loops are regulated to meet a prescribed steam generator load consistent with the electricity demand over a 24-h period. In conclusion, the results found the ABTR system was able to maintain stable reactor conditions and primary- and secondary-side characteristics over the course of the load-following transient.

Advanced Burner Test Reactor (ABTR)↗

Development of Temperature Compensation Tools for SPNDs Operating in High Temperature Environments

Two rhodium-based self-powered neutron detectors (Rh-SPNDs) were irradiated at the Massachusetts Institute of Technology Reactor as a follow-on experiment to the heated irradiation previously conducted at the Neutron Radiography facility at Idaho National Laboratory. The experiment was conducted over the temperature ranges of 600-850°C to further examine the effects of temperature on the Rh-SPNDs. Four tests of varying temperature and power were performed. The tests identified two types of temperature effects consistent with historical evaluations. One effect is a prompt proportionality to temperature at steady-state reactor power due to the decrease in Rh-SPND insulation resistance. The other effect is a delayed effect generated from displacement currents generated by changing the space charge within the insulator as a function of temperature. The result of this experiment demonstrates a characterizable responses to temperature that is feasible for developing a temperature compensation tool for SPND operating in high temperatures. The characteristics identified in this experiment will be integrated within the delayed-response compensation techniques for FY23 evaluation.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Inorganic Alterations in Unconventional Shale Reservoirs: Importance of Additive and Base Fluid Chemistry

The effective development of unconventional petroleum systems requires the use of significant water resources. In an effort to reduce the consumption of freshwater resources for hydraulic fracturing, highly saline produced waters are increasingly recycled for use as a base fluid. However, there are significant knowledge gaps regarding potential water–rock interactions resulting from the introduction of produced waters and associated additives into shale reservoirs such as formation and deposition of mineral scale, which can negatively affect hydrocarbon production through wellbore restriction and damage to hydraulically generated fractures. To assess the impacts of field stimulation practices in the subsurface, a series of laboratory experiments were completed using (a) three distinct sedimentary rock formations of the Midland Basin (Texas, USA) and (b) additives with two different base fluids: municipal fresh water and clean brine. The experimental approach used relevant injection sequences and mixing ratios in specialized reactors for 3 weeks. Static pressurized experiments and nonpressurized time-resolved experiments were undertaken. The resulting solids and liquids were analyzed by using a variety of laboratory- and synchrotron-based techniques. The use of an acid spearhead (15% HCl) resulted in texturing of both clay-rich and calcareous shales, which can temporarily enhance porosity but subsequently result in mineral scale deposition. The primary matrix scale was Fe(III)-bearing phases, which occurred in all experiments regardless of base fluid chemistry. Additionally, strontium sulfate (SrSO 4 ) precipitated on shale surfaces when clean brines were used. It was concluded that clean brine was the main source of Sr 2+ species, while persulfate breaker degradation and oxidation of pyrite were the sources of SO 4 2– . Sulfate scaling was more pronounced in clay-rich shales, suggesting that Sr sorption is important for promoting celestite formation. This work demonstrates that mineral scale deposition is a complex phenomenon, whereby the type and proportions of various mineral phases are determined from reservoir alteration processes and coprecipitation of constituents from injection fluids. In conclusion, the experimental results shown here should be considered when evaluating different base fluids and additives in order to mitigate mineral precipitation in unconventional shale reservoirs, which could result in reservoir degradation.

Jew, Adam D. [SLAC National Accelerator Laboratory↗

DESIGN AND PROTOYPING OF A FISSILE-BEARING CHLORIDE SALT IRRADIATION EXPERIMENT

Limited data exists on the properties of irradiated fueled chloride-based salts for use in advanced nuclear reactors. The design and prototyping of a salt irradiation experiment is underway. Mechanical design will integrate the experiment into existing assemblies in TRIGA type cores. Neutronics modeling demonstrated how targeted power densities can be reached and provide insight on radionuclide source term generation within the experiment. Thermal-hydraulic and computational fluid dynamics (CFD) analysis indicated that temperature ranges in the salt can satisfy both safety and programmatic requirements. Initial prototyping tests provided confidence in the ability to extract the salt post-irradiation, and in the heater performance. Future planned prototyping will provide an integral assessment of the proposed design prior to insertion in the reactor.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

AFRRI TRIGA Reactor Neutron and Gamma Dose Characterization Preliminary Results

Integral Experiment Request (IER) 484 is part of a series of dose characterization and nuclear accident dosimeter (NAD) exercises performed under the Department of Energy (DOE) Nuclear Criticality Safety Program (NCSP). The Armed Forces Radiobilogy Research Institute (AFRRI) 1.1 MW Training, Research, Isotopes, General Atomics (TRIGA) Mark-F reactor is the third facility to undergo a dose study to establish reference dose values. A preliminary measurement was performed earlier this year, where a variety of foils were irradiated and activation gamma rays were measured using a high-purity germanium (HPGe) detector. The data was taken and analyzed to calculate the neutron spectrum in the irradiation facility. This paper will present preliminary results of the neutron dose measured. The characterization of the AFRRI dose field is planned in August.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Building Interfaces with Echo Using R

The following report details the functionality that was developed to directly query the MongoDB and read in echo records from within R, and the ability to create a cinema database directly from echo records. Both of these efforts used the data collected under the MINOS project for development. The nuclear facility under consideration is the High-Flux Isotope Reactor (HFIR) and co-located Radiochemical Engineering Development Center (REDC) at Oak Ridge National Laboratory in Oak Ridge, TN. HFIR is an 85 MW research reactor and is used primarily for production of a medical radioisotopes, material irradiation experiments, neutron activation, and neutron scattering. Targets for the reactor are fabricated and processed and dissolved at REDC, in addition to other glove-box and hot-cell type activities. An overhead view of the facility is provided. The rest of the report is organized as follows: Section 2 describes how to query the MongoDB and load in echo records from within R, with background information on the database type, MongoDB, and the file format of echo records, hdf5, as well as lessons learned during the development phase. Section 3 details the functionality and usage of creating a cinema database directly from echo records within R. A series of appendixes display all the R code (Section 5), some example scripts where the code is used (Section 6), and useful links for further exploration (Section 7).

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

HALEU Experiments [Slides]

The DNCSH, through the HALEU Availability Program, needs publicly available benchmarks supporting Advanced Reactor Fuel Cycle and Transportation. LANL is uniquely positioned to support this goal, with its past experiments at TA-18, planned experiments at NCERC, experiment design capability, and ties to industry. The Deimos experiment will be executed soon and serve as a premier benchmark for the program. LANL expects to submit proposals to the call when issued (soon). Additional experiments supporting DNCSH have already been designed

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

Immersive Scientific Visualization of Molten-Salt Reactor Waste Characteristics Using Virtual Reality

Immersive visualization is changing how we explore, communicate, and understand complex scientific systems. In nuclear energy, an area in which data are often multidimensional, time-dependent, and difficult to interpret, virtual reality (VR) represents a powerful and intuitive informational medium. This work introduces a VR-based platform that visualizes the post-shutdown behavior and waste management lifecycle of molten-salt reactors (MSRs), a next-generation reactor type with unique operational and safety characteristics. The platform, built in Unity, is streamed on the Meta Quest 3 headset. It transforms high-fidelity simulation data into an interactive, immersive experience. Users can explore time-dependent reactor characteristics such as nuclide decay, which is a key factor for evaluating reactor waste strategies. The datasets were generated using the MOOSE (Multiphysics Object-Oriented Simulation Environment) framework and then processed through ParaView scripting for smooth integration into Unity. From a visualization standpoint, the platform emphasizes spatial storytelling, temporal exploration, and user-centered interaction. Users can navigate 3D reactor geometries, slice through volumetric data, and manipulate time to observe how physical phenomena evolve. Real-scale rendering and embodied interaction make the experience feel tangible. The interface is designed to be accessible, even to those without nuclear or simulation expertise. This lowers the barrier for stakeholders, policymakers, and the general public, while still supporting expert analysis and collaborative decision-making. This work shows how immersive visualization can function as both a scientific tool and a communication interface. By integrating simulation, processing, and visualization into a cohesive workflow, we offer a scalable framework for immersive scientific storytelling. The modular design supports future extensions to other reactor types and lifecycle stages, from shutdown to long-term storage, making the platform adaptable for both research and outreach.

99 - GENERAL AND MISCELLANEOUS↗

Pronghorn: A Multidimensional Coarse Mesh Application for Advanced Reactor Thermal-Hydraulics

This paper presents an overview of Pronghorn, a multiscale thermal-hydraulic (T/H) application developed by Idaho National Laboratory and the University of California, Berkeley. Pronghorn, built on the open-source finite element Multiphysics Object-Oriented Simulation Environment (MOOSE), leverages state-of-the-art physical models, numerical methods, and nonlinear solvers to deliver fast-running advanced reactor T/H simulation capabilities within a modern software engineering environment. This work summarizes the physical models, multiphysics and multiscale coupling, and numerical discretization in Pronghorn with emphasis on our initial target application to pebble bed reactors (PBRs). A diverse set of applications are shown to depressurized natural circulation in the SANA experiments, forced convection in the Pebble Bed Modular Reactor, three-dimensional (3-D)/one-dimensional coupling of Pronghorn and RELAP-7 systems T/H for loop analysis in the High Temperature Reactor Power Module, and forced convection in the Mark-1 Pebble Bed Fluoride-Salt-Cooled High-Temperature Reactor. A multiphysics coupling of Pronghorn, RELAP-7, and Griffin deterministic neutronics for a gas-cooled PBR demonstrates the capability of the MOOSE framework for reactor design calculations. These applications highlight the verification and validation underlying Pronghorn’s software development while emphasizing features that improve upon capabilities offered by legacy tools in areas such as 3-D unstructured meshing, physics modeling, and multiphysics coupling.

97 MATHEMATICS AND COMPUTING↗

FY22 Status Report on the ART-GCR CMVB and CNWG International Collaborations

This work presents the numerical model for the high temperature test reactor (HTTR) loss of forced cooling (LOFC) experiment with the INL codes Griffin, BISON, and RELAP-7, based on the Multiphysics Object-Oriented Simulation Environment (MOOSE) framework. Promising results were obtained, with the overall behavior of the reactor successfully captured. Changes in the heat transfer coupling, as compared to the fiscal year (FY)-21 model, enabled drastic improvement of the steady-state solution, both in terms of computational time and global energy discrepancies. The former was reduced by a factor of roughly 60, whereas the latter decreased from 11% to less than 2%. Furthermore, the discrepancy in the steady-state multiplication factor was improved from +2,300 and +2,900 pcm (for the 30 and 9 MW cases) to -700 and +1,200 pcm, respectively, and now falls well within the large measurement uncertainties stemming from graphite impurities. Validation of the Monte Carlo model used to generate cross sections was also performed against available measurements. Though significant, the discrepancies remain acceptable overall in light of the large uncertainty. Numerous improvements are still needed to better compare with the experiment involving the 9 MW case and to instill greater confidence in the model’s ability to accurately predict the 30 MW behavior. Specifically, the power levels predicted by the 9 MW transient simulation following re-criticality remain low, pointing to an underestimation of the passive cooling of the core. A key aspect of future work will be to better understand the flow pattern during the LOFC event, particularly to determine if natural or forced convection is occurring inside the reactor pressure vessel (RPV). More generally, additional validation data would be immensely useful for further enhancing the numerical model and better matching the experiments. In addition, a more sophisticated thermal-hydraulics model that simulates all the channels as a single system model should be considered to take into account the rest of the primary loop. Finally, even if the results are in better agreement with the experiments, sensitivity analysis and uncertainty quantification will be necessary to evaluate the model uncertainty.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

The Physical and Engineering Limits of Coupled In situ TEM Experiments

Almost all future energy systems (advanced nuclear reactors, fusion energy system, concentrating solar-thermal power (CSP), and wind technologies) are limited by degradation of key material systems exposed to multiple environmental stressors. The degradation during exposure to high temperatures, radiation, mechanical loading, and chemical attack is often dictated by mechanisms active at the microstructural level. The nature of these mechanisms and the associated variations between sequential and concurrent interplay can be explored if the transmission electron microscope (TEM) is utilized as a toolbox for exploration [1]. One such tool developed at Sandia National Laboratories to couple several of these environments is the In situ Ion Irradiation TEM (I3TEM) [2]. Several studies over the last decade utilizing this tool have shown that the scientific intuition developed over decades of sequential experiments is not always a good indicator of concurrent mechanisms or failure routes. This presentation will highlight the recent and planned additions into the I3TEM facility of a Waviks gas injection system and Raman system, respectively, as can be seen in Fig. 1, permitting environmental degradation from gas species leaked into the pole piece region during quantitative mechanical loading (indentation, monotonic loading, high temperature creep, irradiation induced creep, and high-cycle fatigue); multi-beam ion irradiation (energies ranging from 1 keV to 48 MeV and species from H to Au); laser exposure (20 W and 1064 nm), or various combinations thereof that are already possible [3]. This addition permits the facility to explore both sequential or concurrently the four axes of stressors: thermal, mechanical, radiation, and chemical. This information can be directly coupled to modeling, expediting the refinement and validation of both atomistic and mesoscale models.

degradation↗

HDG-1 Experiment Irradiation Monitoring Data Qualification Final Report

SUMMARY The U.S. Department of Energy (DOE) Advanced Reactor Technologies (ART) Graphite Research and Development (GRD) Program is conducting a series of six experiments to quantify the effects of irradiation on nuclear-grade graphite. This report documents the qualification of irradiation monitoring data for the fifth experiment, High Dose Graphite-1 (HDG-1). Qualified monitoring data are required by the ART program to support the design and licensing of the first high-temperature reactor (HTR) nuclear plant. Data are classified as Qualified if they meet the usage requirements described in the experiment planning and quality assurance (QA) documents, Failed if they do not meet those requirements and provide no usable information, or Trend if they do not fully meet all requirements but still provide useful information subject to an assessment of how any deficiencies may affect a particular use of the data. HDG-1 irradiation began with Advanced Test Reactor (ATR) Cycle 168B on August 24, 2020, and concluded after Cycle 173C on January 27, 2025. The HDG-1 capsule was removed from the reactor core twice—during core internal change (CIC) Cycle 170A and powered axial locator mechanism (PALM) Cycle 172A—to prevent overheating of the graphite specimens during high-power PALM cycles. The capsule was therefore irradiated during a total of seven normal ATR cycles: 168B, 169A, 171A, 171B, 173A, 173B, and 173C. Irradiation monitoring data evaluated in this report include thermocouple (TC) temperature, gas flow rate, gas moisture, gas pressure, specimen load, and graphite stack displacement. Temperature. A total of 14,508,065 TC temperature records were captured. Of these, 13,901,785 (95.8%) are Qualified and 606,280 (4.2%) are Failed. The principal source of failed temperature data was the instrument failure of TC-9 (Zone 2) on June 24, 2024, and TC-10 (Zone 1) on July 5, 2024, near the end of Cycle 173A, which resulted in 595,554 Failed readings. An additional 379 missing values and 10,347 slightly negative values from TC-13 during ATR outages are also Failed. Neither TC-9 nor TC-10 was used as a temperature-control TC, and their failures did not compromise capsule condition monitoring. Correlation analysis of all 13 TCs found no evidence of virtual junction formation. Control chart analysis revealed clear downward drift of approximately 80°C for TC-6 (Zone 3) relative to other stable TCs, and possible downward drift of approximately 60°C for TC-13 relative to the Zone 5 control TC (TC-1), though TC-13 remained consistent with the Zone 2 control TC (TC-12). Gas flow. A total of 20,088,090 gas flow rate records were captured. Of these, 19,941,463 (99.3%) are Qualified and 146,627 (0.7%) are Failed due to missing values. All argon, helium, and total gas flow data were within expected ranges throughout the irradiation. Gas moisture. A total of 1,116,005 outlet gas moisture values were captured. Of these, 1,101,421 (98.7%) are Qualified and 14,584 (1.3%) are Failed, comprising 14,556 out-of-range values and 28 missing values. The out-of-range moisture values exceeded 22,000 ppmv for approximately 1 week at the beginning of Cycle 173A, when accumulated moisture evaporated after the capsule was retrieved from water storage during PALM Cycle 172A and reinserted into the east flux trap. Moisture levels returned to below 25 ppmv for the remaining three cycles, and the transient high-moisture event did not affect the integrity of specimen irradiation. Gas pressure. A total of 7,812,035 gas pressure values were captured. Of these, 6,642,048 (85.0%) are Qualified and 1,169,987 (15.0%) outlet pressure values are Failed, comprising 718,537 zero outlet pressure values due to sensor failure from Cycle 168B through Cycle 171B, 54,550 missing values, and 396,900 too-low outlet pressure values, ranging from 1.1 to 1.6 psia after sensor replacement during Cycle 173A. Load. A total of 6,696,030 load values were captured. Of these, 6,694,580 (99.98%) are Qualified and 1,450 (0.02%) are Failed due to missing values. Applied loads to the six specimen stacks were stable throughout the irradiation. Stack displacement. A total of 6,696,030 displacement values were captured. Of these, 5,713,297 (85.32%) are Qualified and 3,781 (0.06%) are Failed due to missing values. Stack displacement increased consistently throughout the irradiation, reaching approximately 3.08 in. for Channels 5 and 6 by the end of irradiation. 978,952 (14.62%) substantially elevated displacements observed for Channel 6 beginning in Cycle 171A and for Channel 5 beginning in Cycle 173A are assigned Trend status. Raising pressure. A total of 1,115,999 raising pressure values were captured. Of these, 1,115,430 (99.95%) are Qualified and 569 (0.05%) are Failed due to missing values. Ram pressure. A total of 6,696,030 ram pressure values were captured. Of these, 6,692,249 (99.95%) are Qualified and 3,484 (0.05%) are Failed due to missing values. Stack raising was perf

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Multiphysics Simulation of KRUSTY Warm Critical Experiments Using MOOSE Tools

A series of critical experiments were performed during the Kilopower Reactor Using Stirling TechnologY (KRUSTY) project, producing valuable and unique data for the validation of corresponding microreactor models. In this paper, the development of a high-fidelity multiphysics model of the KRUSTY microreactor within the MOOSE ecosystem is presented, with a focus on the microreactor configuration during the warm critical experiments. The model was established by coupling a deterministic neutronics model using the Griffin code, with a BISON thermomechanical model. The multiphysics model successfully simulated the KRUSTY 15 ¢ and 30 ¢ warm critical reactivity insertion experiments in satisfactory agreement with the experimental measurement data. In conclusion, the modeling results demonstrated the performance of MOOSE-based multiphysics tools in microreactor simulations, and spotlighted the useful applications of these tools in supporting microreactor design, qualification, and licensing activities.

KRUSTY↗

MHD stability of negative triangularity DIII-D plasmas

Abstract Negative triangularity (NT) experiments in DIII-D point to an emergent reactor scenario free of sawteeth, endowed with benign, nondisruptive n = 2 tearing modes, which experience q min ⩾ 1 similar to the positive triangularity hybrid scenario. Plasmas exhibiting this behavior attain β N > 3 , high enough to reconsider long held views of NT stability. Ideal MHD and tearing stability analysis of well-diagnosed equilibrium reconstructions of experimental hybrid-like plasmas predict that among shape parameters, MHD stability limits are only sensitive to average triangularity. Operation is predicted to be possible at β N relevant to upcoming tokamaks and commercial NT reactors.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Monolithic ATF MiniFuel Sample Capsules Ready for HFIR Insertion

Several advanced nuclear fuel concepts are being considered throughout the nuclear industry. Implementation of these concepts could increase accident tolerance or enhance performance beyond the capabilities of the UO₂-based nuclear fuel currently in use. Qualification and deployment of any new fuel requires rigorous irradiation testing to demonstrate performance under representative normal and off-normal operating conditions. The traditional approach for qualifying new fuels requires exhaustive execution of many integral fuel tests. However, due to the long timeframe for executing these integral tests and the limited number of available materials test reactors, this approach is becoming impractical. To accelerate fuel qualification, Oak Ridge National Laboratory developed the MiniFuel irradiation vehicle for use in conducting accelerated separate effects irradiation testing of a wide range of nuclear fuel materials in the High Flux Isotope Reactor (HFIR). The first MiniFuel irradiations performed in the facility tested sol gel–derived uranium nitride kernels and tristructural isotropic (TRISO)-coated particle fuels. This report describes the preparation and assembly of the first set of monolithic MiniFuel irradiations conducted to support accident-tolerant fuel (ATF) development and accelerated fuel qualification. Two irradiation targets containing a variety of UO₂ and U₃Si₂ disk fuel specimens were fabricated and assembled for irradiation to burnups of 8-10 and 28-40 MWd/kg U. The target irradiation temperature is 450-550°C. Irradiation of U₃Si₂ will provide new data regarding the irradiation performance of a candidate ATF to complement current ATF-1 integral experiments being performed in the Advanced Test Reactor. UO₂ samples were included as a reference so that the results from the MiniFuel experiments can be compared with the extensive UO₂ fuel performance database. The monolithic MiniFuel capsules were successfully assembled, welded, and tested per HFIR requirements and are ready for insertion into the reactor. Pictures of the assembly process are included in this report. The experiment is planned for insertion into the HFIR during cycle 487 in April 2020.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Metal nitride materials for solar-thermal ammonia production [Slides]

Solar Thermal Ammonia Production has the potential to synthesize ammonia in a green, renewable process that can greatly reduce the carbon footprint left by the conventional Haber-Bosch reaction. Co 3 Mo 3 N has been identified as a potential candidate for ammonia production. It is synthesized via oxide precursor synthesis followed by nitridation under 10% H 2 /N 2 . The synthesis method can be extended to other candidate nitrides. The Co 3 Mo 3 N → Co 6 Mo 6 N reduction is demonstrated on TGA with rapid kinetics. The formation of NH 3 is qualitatively observed, but not quantitatively determined. The material retains crystal structure, but no secondary phases are observed in XRD. Partial re-nitridation back to CMN331 of ~35% of max nitridation is observed. Reaction parameters in TGA differ from experimental conditions in the literature. Experiments at Georgia Tech better mimic re-nitridation conditions with more sensitive, quantitative analytical techniques (GC-MS). The ASU NH 3 synthesis/re-nitridation reactor is under development and will permit experiments (reduction/re-nitridation) under precisely controlled T, pH 2 .

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗