Search NASA⌕ Search

SEARCH · Search NASA

Results for “Thermogravimetric analysis”

Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 145 records · Page 8

Supercritical, liquid, and gas CO 2 reactive transport and carbonate formation in portland cement mortar

In this paper, we investigate carbonate formation and reactive transport rate in variably saturated portland cement mortars when high concentrations of gas, liquid, or supercritical CO 2 flow through their pore network. Xray computed tomography completed during CO 2 flow is used to quantify the microstructural evolution as the mortar carbonates. After in situ tests, higher resolution scans, thermogravimetric analysis, and desorption isotherm analysis are performed to further quantify microstructural changes. We found that at dry conditions supercritical CO 2 moves more rapidly through the pore space and precipitates more carbonates than liquid or gas CO 2 . However, at 50% degree of saturation (DOS) the CO 2 state did not affect the rate of transport in that each specimen exposed to a different CO 2 state carbonated within the first hour of CO 2 exposure. When the pore space is at 50 or 100% DOS, supercritical CO 2 did not react with hydration products more rapidly nor did it result in more carbonate formation during exposure compared to gas or liquid CO 2 . The amount of Ca(OH) 2 that contributes to CaCO 3 formation is correlated to the DOS. For the mortar composition analyzed, Ca(OH) 2 contributes to approximately 40% of the carbonates formed in the 50% DOS specimens and 15% in the 100% DOS specimens. In other words, as the amount of moisture in the pore space increases, phases other than Ca(OH) 2 contribute to more than 50% of the total CaCO 3 formed.

42 ENGINEERING↗

Impacts of engine lubrication oil-derived ash on soot oxidative reactivity on a catalytic gasoline particulate filter

Characterizing soot oxidation kinetics is crucial for understanding how gasoline particulate filters (GPFs) perform both in terms of filtration efficiency and pressure drop. The most common method for measuring soot oxidative reactivity is thermogravimetric analysis (TGA). Because TGA is an offline method, it may inaccurately predict how soot oxidizes on a GPF, especially if a catalytic washcoat is present that may enhance oxidation rates through surface interactions as the soot loads on the filter. In this work, a novel in-situ soot oxidative reactivity measurement method was developed. The method involved loading a catalytic GPF under high temperature conditions conducive to soot oxidation and measuring the filtration efficiency of 100 nm particles. A correlation was made between filtration efficiency and loaded soot mass on the filter to allow calculation of the soot oxidation rate. The method was evaluated in experiments using a 2.0 L gasoline direct injection (GDI) engine with three oils of varying additive packages, including an oil with a high zinc dialkyldithiophosphate (ZDDP) concentration, a non-additive, pure poly-alpha olefin (PAO) oil, and an oil with a high concentration of calcium sulfonate. Calculated specific soot oxidation rates ranged from ~0.06–0.6 min –1 and showed strong dependence on GPF inlet gas temperature and lubrication oil additive type. The results clearly demonstrated a catalytic effect of calcium-containing ash particles. Reactivity of soot produced by the engine running with the high calcium containing lubrication oil was increased. Similarly, the results indicated that the catalytic washcoat on the filter increased soot oxidation rates on-filter, especially at low soot loading. Conversely, the ZDDP oil additive exhibited a reactivity inhibiting effect, resulting in lower soot oxidation rates. Finally, this work represents the first known in-situ soot oxidative reactivity measurements on a GPF and elucidates the effect of lubrication oil additives and catalytic washcoat on oxidation rate.

42 ENGINEERING↗

Spark plasma sintering (SPS) densified U 3 Si 2 pellets: Microstructure control and enhanced mechanical and oxidation properties

Dense U 3 Si 2 pellets with controlled grain structure and enhanced thermal-mechanical and oxidation properties are synthesized with spark plasma sintering (SPS). Microstructure and phase composition of the SPS densified pellets are characterized systematically using SEM, EDS, and XRD. Thermal-mechanical properties and oxidation behavior of the sintered silicide fuel pellets are analyzed by laser flash, indentation, and dynamic thermogravimetric analysis. Dense U 3 Si 2 pellets are consolidated by combining high energy ball milling and rapid sintering by SPS, and the microstructure structures are controlled from micron-sized (~5.7 μm grain size) for conventional silicide to a nanocrystalline matrix with an average grain size of ~280 nm. A dominant phase of distorted U 3 Si 2 was identified with lattice expansion due to residual thermal stress upon SPS consolidation and rapid cooling processes. Both micron-sized and nano-sized pellets show exceptional thermal transport properties, consistent with monolithic silicides reported in literature. The SPS-densified pellets possess simultaneously high hardness and fracture toughness. The SPS-densified silicide pellets also demonstrate exceptional oxidation performance with extended onset oxidation temperature above 500 °C and reduced oxidation kinetics, particularly for nano-sized pellets. A strong strain effect was proposed in which compressive stress in nano-sized pellets enhances the oxidation resistance of silicide fuels, as evidenced by the degradation of oxidation performance upon strain relaxation by isothermal annealing. The correlation among the sintering process – microstructure control – physical properties and fuel behavior is established. A new concept of strain engineering is proposed further properties optimization, enabling the development of potential oxidation and corrosion-resistant silicides with extended performance, the key technological challenge of U 3 Si 2 as the leading concept of accident tolerant fuels.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

High hardness and oxidation-resistant Cr-containing medium entropy ZrTaW diboride

This study reports the successful synthesis of a Cr-containing (Zr 0.30 Ta 0.34 Cr 0.06 W 0.30 )B 2 medium-entropy boride (MEB) via an in-situ reactive borothermal reduction route from oxide precursors. High-energy ball milling was employed to homogenize the precursor mixture prior to reactive densification. X-ray diffraction confirmed the formation of a predominantly AlB₂-type hexagonal diboride structure together with a secondary (W X , M 1-X )B monoboride phase. Microstructural characterization revealed compositional heterogeneity and localized W-rich regions associated with the secondary phase. The synthesized medium-entropy boride exhibited enhanced mechanical properties, which are attributed to lattice distortion and solid-solution strengthening effects. Thermogravimetric analysis revealed complex multistage oxidation behavior, and the oxidation resistance was compared with conventional ultra-high-temperature diborides. The results demonstrate the strong relationship between oxide-derived processing, compositional complexity, phase evolution, and oxidation behavior, highlighting the potential of medium-entropy borides for high-temperature structural applications

36 MATERIALS SCIENCE↗

Supported molybdenum oxides for the aldol condensation reaction of acetaldehyde

The (retro-)aldol condensation reaction is an important chemical transformation in the upgrading of biomass-derived compounds into fuels and valuable specialty chemicals. In this study, we found that supported molybdenum oxide (MoO x ) catalysts were active and selective for the aldol condensation of acetaldehyde to crotonaldehyde under steady-state reactor conditions. Through a combination of transmission electron microscopy (TEM), ultraviolet–visible (UV–VIS) diffuse reflectance spectroscopy, Fourier transform infrared (FTIR) spectroscopy of adsorbed pyridine, and steady-state reactor testing, we determined that highly dispersed MoO x has a strong interaction with a γ-Al 2 O 3 support resulting in optimal catalyst performance at low weight loadings. In contrast, MoO x particles supported on SiO 2 have a weaker interaction with the support, resulting in a monotonic relationship between Mo loading and aldol condensation activity. The Lewis acid site density and strength are important parameters for predicting aldol condensation activity across all samples. The concentration of weak acid sites had a poor correlation with aldol condensation activity, most likely because these sites are too weak to activate acetaldehyde for the reaction. Medium and strong acid sites both had good correlations to aldol condensation activity. Results from X-ray absorption near edge structure (XANES) and acetaldehyde temperature programmed desorption (TPD) indicated that partially reduced MoO x was more active for aldol condensation, but pretreatment in reducing or oxidizing environments had no significant effect on steady-state catalytic activity. Finally, characterization of spent catalyst samples through temperature programmed oxidation (TPO) and thermogravimetric analysis (TGA) revealed that catalysts with high densities of strong acid sites tended to form more carbonaceous deposits on the surface over the course of the reaction.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Recycled polyethylene and crumb rubber composites modified asphalt with improved aging resistance and thermal stability

Crumb rubbers (CR) and recycled Polyethylene (PE) are commonly used as modifiers to improve the asphalt properties. However, the addition of these modifiers individually may result in phase separation of PE and inadequate degradation of CR, which may not simultaneously satisfy the rheological and aging resistance of the binder blends. In this study, a type of CR/PE composites manufactured through melt extrusion procedures was adopted for the improvement of the modified binder blends. The modified binder blends after short-term (RTFO) and long-term (PAV) aging were collected for dynamic shear rheometer and bending beam rheometer tests. FTIR tests were also used to quantify the aging resistance, while differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) were applied to evaluate the thermal behaviors of the binder blends. Optical microscopy tests were used to explore the modification mechanism and visualize the microstructures of original and PAV aged binder blends. Test results showed that CR/PE composites could significantly improve the aging resistance of the binder blends. The dispersed PE particles still interacted with each other and meanwhile worked with the diffused rubbery phase, which could form a similar TPEs network. The oxidation and high-temperature aging of such binder blends would strengthen the network that resisted the aging severity of the binder blends. Furthermore, it was also revealed that CR/PE modified asphalt could sustain more heat before a rapid degradation and the well-dispersed PE particles could interact with the diffused CR particles to form a network to resist aging.

02 PETROLEUM↗

Carbon sequestration into lime-stabilized soils: Engineering and mineralogical characterization

Stabilizing weak clayey soils with lime is an effective method for improving the mechanical properties of soil. However, lime production is an energy-intensive process producing significant CO 2 emissions in lime-stabilized soils, which can be counteracted through accelerated carbonation that enhances its engineering performance. The present study evaluates accelerated carbonation of lime-treated soils by adding gaseous (CO 2 -rich gas), liquid (water-CO 2 mixture), and solid (sodium bicarbonate) CO 2 sources. Results indicated that samples carbonated with gaseous CO 2 exhibited 100% lime carbonation, while samples treated with solid and aqueous sources of CO 2 had a mean lime carbonation of 60% and 40%, respectively. Further, all lime-treated-carbonated samples exhibited a mean 50% increase in unconfined compressive strength compared to the untreated samples after a 7-day curing period. Durability evaluation through cyclic wetting and drying indicated that the carbonated samples had higher durability than the untreated samples. X-ray computed tomography showed that adding solid and liquid sources of CO 2 facilitated the flocculation of montmorillonite, reducing the porosity. However, a higher dosage of solid CO 2 induced clay dispersion, increasing the porosity. X-ray diffraction and thermogravimetric analysis verified CO 2 sequestration through the formation of calcite, a thermodynamically stable polymorph of calcium carbonate.

58 GEOSCIENCES↗

A novel solid oxide electrolytic cell with reduced endothermic load for CO 2 electrolysis using (La 0.80 Sr 0.20 ) 0.95 MnO 3-δ cathode

CO 2 conversion to CO via solid oxide electrolysis provides a potentially efficient method for converting CO 2 into an industrially relevant product. A solid oxide electrolysis cell with (La 0.80 Sr 0.20 ) 0.95 MnO 3-δ (LSM) as the CO 2 reduction cathode, yttrium stabilized zirconia (YSZ) as electrolyte, and nickel as the H 2 oxidation anode was operated 800 °C and 850 °C. Thermogravimetric analysis of the LSM material showed no catalyst oxidation at operating temperatures allowing for CO 2 electrolysis without reducing safe gas. In addition, no cathode material mass gain was observed in the presence of CO suggesting little to no carbon deposition occurred above 750 °C. The formation rates of CO for the cell reached 1.15 mL∙min-1∙ cm -2 for an applied current of 150 mA∙cm -2 achieving a faradaic efficiency of 100 %. Furthermore, the cell displayed good stability in the short-term CO 2 electrolysis test with a nominal voltage drop of 4 mV h -1 for 10 h at 850°C. This study shows the feasibility of operating a solid oxide CO 2 electrolysis cell for CO production with H 2 at the anode to reduce endothermic process load.

(La0.80Sr0.20)0.95MnO3-δ↗

Effect of metal-free mesoporous silica incorporated ZSM-5 composite on thermo-catalytic pyrolysis of polypropylene

Although different zeolites impregnated with transition metals have been used in catalytic deconstruction of waste plastics to other products, the influence of hierarchical structures on conversion and product selectivity in plastic upcycling has not been thoroughly investigated. This research explores a transition metal free zeolite-based hierarchical composite, synthesized by incorporating SBA-15 in ZSM-5 framework, for efficient thermos-catalytic upcycling of polypropylene (PP). Thermogravimetric analysis reveals that ZSM-5@SBA-15 can break down PP at a significantly lower temperature, 240 °C, compared to that of pristine PP using ZSM-5 or SBA-15. In addition, pyrolysis of PP at 400 °C using ZSM-5@SBA-15 composite outperforms ZSM-5 or SBA-15 used separately and yields 90 % conversion with 70 % selectivity to propene. The presence of mesopores in the catalyst appears to reduce the diffusion resistance of intermediate products for successive scission, thereby reducing the activation energy of reaction and improving catalytic activity. In conclusion, the hierarchical composite ZSM-5@SBA-15 has significant potential for upcycling of PP into valuable monomers and lighter olefins, with lower energy demands, enhancing the economic feasibility of the process.

ZSM-5@SBA-15↗

Enhanced grindability of bastnaesite ore by ex-situ CO 2 treatment under the partial pressure of 0-100 psi

High grinding energy consumption has long constrained the sustainable development of mineral processing. This study introduces an innovative technology that employs ex-situ CO 2 treatment to enhance the grindability of bastnaesite ore. The grinding aid effect was evaluated under CO 2 partial pressures ranging from 0 psi to 100 psi using particle size distribution and the Bond work index (BWI), while the underlying mechanism was elucidated with various characterization techniques including inductively coupled plasma (ICP), scanning electron microscopy (SEM), thermogravimetric analysis (TGA), and Brunauer-Emmett-Teller (BET). The optimal grinding aid effect was achieved at 100 psi partial pressure, 50% slurry concentration, and 3 h reaction duration. Correspondingly, the P80 of the grinding product decreased from 81.76 μm to 72.73 μm and the BWI of bastnaesite ore decreased from 6.96 kW·h/t to 6.30 kW·h/t, a reduction of 9.48%. The grinding aid effect primarily resulted from the transformation of sparingly soluble carbonates like calcite and dolomite into more soluble bicarbonates, which created substantial cracks and pores, thereby reducing the ore's hardness and improving its grindability. By significantly saving grinding energy consumption while delivering environmental benefits, this technology exhibits great promise for further optimization and widespread adoption.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Adsorptive denitrogenation of model aviation fuel using mesoporous silica in a packed bed adsorption system

This study aims to understand the effects of system process parameters such as flow rate, adsorbent particle size, and use of recycled adsorbent on denitrogenation performance of a model fuel using mesoporous silica gel. The goal is to reduce the nitrogen content of the model fuel from 1500 parts per million to single-digit ppm to meet ASTM specifications for drop-in fuels. This work was done with the intent of applying adsorptive denitrogenation to sustainable aviation fuel (SAF) product fractions produced via hydrothermal liquefaction (HTL). The adsorption performance of the silica is evaluated via packed column breakthrough data, with data generated from collecting from the column outlet and quantifying nitrogen content via gas chromatography. Select experiments use a significantly larger (2.5x column diameter and length) column to demonstrate linear scalability of the process. Thermogravimetric analysis data is collected to evaluate the effects of thermal calcination as a sorbent regeneration method. Effects of a more complex feed are also investigated using a known reference fuel with additional added nitrogen containing compounds. The results presented in this work successfully demonstrate up to 99.8 % removal of NCCs from a model fuel fraction at an original NCC concentration of approximately 1500 ppm to single-digit parts per million after treatment. We also examine calcination of sorbent materials to remove the adsorbed species to enable sorbent reuse and minimize waste generation and show that the calcined material can be reused up to 5 cycles with reduced adsorption capacity. Overall, this work indicates that adsorptive denitrogenation using silica gel is a viable solution to enable the integration of HTL-derived aviation fuels into existing fuel infrastructure.

Adsorption techniques↗

Conversion kinetics during melting of simulated nuclear waste glass feeds measured by dissolution of silica

In this work, we experimentally investigated the batch-to-glass conversion kinetics of two low-activity and two high-level nuclear waste melter feeds that represent widely different behavior during melting; tests comprised thermogravimetric analysis, the feed expansion test, evolved gas analysis, and x-ray diffraction. Our study indicates that the conversion processes, which include gas-evolving reactions, dissolution of crystalline phases, and primary foam expansion and collapse, are interconnected and influenced by the feed’s thermal history. The fraction of dissolved silica was adopted as a measure of the extent of conversion inside the cold cap—the floating layer of feed material on the top surface of the melt in an electric melter. The interface between the cold cap and the free-flowing melt below was associated with a constant fraction of dissolved silica. The estimated viscosity of glass-forming melt at this interface lies within a narrow range for the feeds studied.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

U 3 Si 2 and UO 2 composites densified by spark plasma sintering for accident-tolerant fuels

This work reports the synthesis and characterization of the U 3 Si 2 and UO 2 composites sintered by spark plasma sintering (SPS) with controlled microstructures for accident-tolerant fuel application. The U 3 Si 2 and UO 2 composites with different silicide and oxide ratios were synthesized by SPS at temperatures from 1000 to 1300 °C for 5 minutes. The microstructure and phase composition of the SPS densified composite fuels were characterized with scanning electron microscopy, X-ray diffraction (XRD), and energy dispersed spectroscopy (EDS). A systematic study of the thermal and mechanical properties was conducted using microhardness testing and laser flash apparatus, along with oxidation resistance measurements using thermogravimetric analysis (TGA). The results show that the synthesis of composite fuels can be achieved with a 90% theoretical density (TD) at 1000 °C and over 95% TD when sintered at 1300 °C. XRD and EDS results confirmed that the dominant phases in the composites are U 3 Si 2 and UO 2 . Improved physical density generally leads to improved hardness, fracture toughness, thermal diffusivity, and onset temperature during the oxidation process. U 3 Si 2 was found to play a dominant role in determining the mechanical and oxidation properties of the composite fuels, whereas UO 2 had a more important impact on controlling the thermal diffusivity of the composites. The composite with 50 wt% UO 2 sintered at 1300 °C displayed the onset oxidation temperature of 500 °C by dynamic oxidation testing using TGA at a ramp degree of 10 °C/min. The composite also achieved a high fracture toughness of ~3.5 MPa m ½ . Finally, these results highlight the potential of composite fuel forms densified by SPS with simultaneously enhanced fissile element density, fracture toughness, thermal transport properties, and oxidation resistance.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Steam oxidation of chromium corrosion barrier coatings for sic-based accident tolerant fuel cladding

SiC-based materials are currently being considered for accident tolerant fuel (ATF) cladding, however, there are concerns regarding hydrothermal corrosion rates and hermeticity. These issues may be addressed with the utilization of a Cr corrosion barrier coating (CBC) but the interaction of Cr with SiC under loss of coolant accident (LOCA) conditions needs to be investigated. In the present work, Cr coatings were deposited onto chemically vapor deposited (CVD) SiC with either high power impulse magnetron sputtering (HiPIMS), cathodic arc (CA), or a combination of both. Annealing and steam thermogravimetric analysis (TGA) was used to study reaction product formation with and without oxidation. Additionally, after 1200 °C annealing, formation of a Cr x C y carbide layer at the ambient interface and a Cr x Si y C z silicide layer at the SiC interface was observed. After 1200 °C TGA exposure, similar carbide and silicide layers were observed but with a Cr 2 O 3 outer reaction layer and a Si and O rich interfacial layer forming between the carbide and silicide layers. Initial mass gain of the coatings during the 1200 °C TGA exposure was parabolic and were similar to reported rates of chromia formation. Mass gain behavior and observed transitions in chromia microstructure indicate that metallic Cr may be consumed within the first ~1 h at 1200 °C and that subsequent chromia formation occurs at the expense of the underlying Cr carbide layer. Overall, the results show no detrimental impact of Cr coatings on the steam oxidation resistance of SiC up to 4 h at 1200 °C.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Effect of Added Gadolinium Oxide on the Thermal Air Oxidation of Uranium Dioxide

To develop a more reliable and stable UO2-based nuclear fuel, the Pacific Northwest National Laboratory (PNNL) investigated modifying fuel with several soluble lanthanides and zirconium. This article provides the results of these studies investigating gadolinium doping at levels up to 10 mass%. The authors characterized and compared commercially- and PNNL-prepared gadolinium-doped UO2 to determine the oxygen-to-metal ratio, elemental distribution, chemical composition, physical appearance, lattice parameters, and grain structure using atomic force microscopy, scanning electron microscopy coupled with energy dispersive spectroscopy, and X-ray diffractometry. After confirming PNNL-prepared UO2 and (Gd,U)O2 were similar to commercially prepared UO2 and (Gd,U)O2, we measured the thermal behavior of these gadolinium-doped UO2 materials to air oxidation using differential scanning calorimetry and thermogravimetric analysis. Addition of gadolinium stabilized the first oxidation product U4¬O9/U3O7 and slowed the subsequent oxidation to U3O8. Comparison of our measured two-step oxidation of UO2 to U3O8 at 325°C to common gas/solid kinetic reaction models found that each oxidation step is best described as a convolution of kinetic behaviors; the gadolinium insertion into the UO2 lattice enforces a significant alteration in mechanism and oxidation rate. Noticeable changes in mechanism become apparent between 1% and 3% gadolinium content.

Uranium Dioxide, Gadolinium Oxide, Thermal Air Oxi↗

Air oxidation of yttrium hydride as a high temperature moderator for thermal neutron spectrum fission reactors

Yttrium hydride (YH x ) is an attractive moderator material for thermal neutron spectrum fission reactors requiring a small reactor core volume and has been selected as the neutron moderator for the Transformational Challenge Reactor (TCR), an advanced gas-cooled microreactor. Before YH x can be used in this application, it is important to understand the material response to off-normal conditions. In the present study, 550–650 °C isothermal dry air oxidation was performed to simulate a depressurized loss of force circulation (DLOFC) event. The oxidation was performed using thermogravimetric analysis (TGA) on bulk crack-free YHx coupons. Oxidation studies were also performed on Y coupons to elucidate the impact of H on oxidation. Both the chemistry and distribution of processing impurities were found to strongly affect oxidization behavior on a batch-to-batch basis. Regardless of batch, YHx oxidized at a significantly lower rate than Y at all temperatures, and the lower rate was directly correlated with increased hydride content. Metallic Y exhibited complex exponential kinetics, whereas YH x also exhibited complex kinetics but gained considerably less mass. According to literature reports on protonic and native-ion conductivities of Y 2 O 3 and mass spectrometry analysis of gaseous reaction products formed during the oxidation of YH x , a mechanism for the reduced oxidation rate of yttrium hydride is suggested.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Investigation of UO 2 doped with Fe 2 O 3 sintered under a reducing atmosphere

Nuclear fuel produced with trace amounts of transition metal additives is of potential interest for introducing intentional signatures for accelerating nuclear forensics. In this work, we investigate the effects on microstructure, grain size, crystal structure, and stoichiometry when trace amounts of Fe in the form of Fe 2 O 3 are added to UO 2 . Sintering of compacts with different concentrations, from 250 to 3000 ppmw, was performed under a reducing atmosphere at 1773 K. The persistence of the taggant during the fuel fabrication process as well as its impact on grain size, crystal lattice, and first-neighbor chemistry was evaluated using inductively coupled plasma–optical emission spectroscopy, powder X-ray diffraction (pXRD), Raman spectroscopy, scanning electron microscopy–backscatter electron spectroscopy, energy dispersive spectroscopy, and thermogravimetric analysis. We observed that a negligible amount of Fe was lost during sintering. Our results indicate that the feedstock, Fe 2 O 3 transforms into Fe and FeO under the test sintering conditions. For all compositions, metallic Fe precipitate was found in grain boundaries as a secondary phase. In conclusion, the potential incorporation of ionic Fe into the UO 2 unit cell was determined by pXRD and Raman spectra.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Physicochemical evolution of uranium nitride kernel microstructure with varying carbon distribution for advanced TRISO fuel forms

Uranium nitride (UN) has emerged as a fuel candidate for advanced nuclear reactor concepts due to its superior uranium density, thermal conductivity, and high melting temperature. However, the fabrication route for converting UO 2 to UN is complex and difficult to standardize. Although the chemistry of this conversion process is well-studied, more insight into the physicochemical dynamics of this conversion using advanced characterization techniques can help further our understanding of this material system. This work leveraged thermogravimetric analysis (TGA), X-ray diffraction (XRD), and nondestructive 3D X-ray computed tomography (XCT) to characterize dynamic microstructural changes in the UO 2 → UCO → UN fabrication pathway for two kernels with a varying carbon distribution in the starting composition. TGA and XRD were used to quantify changes in the mass, density, and chemical composition of the two kernels, while three-dimensional image processing and segmentation of XCT data were used to quantify the volume, surface area, and spatial distribution of features within each kernel for multiple steps along the fabrication pathway. The analysis indicates distinct differences between the two kernels that are correlated to downstream conversion efficiency. In conclusion, this work is among the first to perform 3D quantification of physicochemical evolution during UN conversion, providing quantitative correlation between processing, properties, and expected fuel performance.

Nuclear fuel↗