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Du Frane, Wyatt L.

Publications and source records attributed to Du Frane, Wyatt L..

13 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Advanced Fabrication Techniques of Metal Hydrides for Science and Technology Applications (Abbreviated Final Report)

Lithium Hydride (LiH) atomic properties make it an excellent candidate for thermal energy storage, hydrogen storage, and nuclear reactor technology. High Energy Density (HED) experiments on LiH at the National Ignition Facility (NIF) can also provide critical Equation of State (EOS) and Hugoniot data. Density requirements for LiH vary per application and therefore physical and structural requirements for LiH are non-uniform. Historical production of LiH relies on casting processesthat are limited by density and grain-size control, which leads to unfavorable machinable characteristics. LiH manufacturing is further hindered due to its chemical reactivity and propensity to readily react with moisture. This work aimed at exploring advanced fabrication techniques for LiH such as 1) uniaxial powder pressing methods and 2) laser powder bed fusion (L-PBF) additive manufacturing. Uniaxial powder compaction offers advantageous tailorable mechanical and physical properties via density control, and L-PBF can produce net-shaped complex parts with unique microstructure. Uniaxial pressing proved successful in readily producing LiH with density control.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Advanced Fabrication Techniques of Metal Hydrides for Science and Technology Applications (Full Technical Report)

Lithium Hydride (LiH) atomic properties make it an excellent candidate for thermal energy storage, hydrogen storage, and nuclear reactor technology. High Energy Density (HED) experiments on LiH at the National Ignition Facility (NIF) can also provide critical Equation of State (EOS) and Hugoniot data. Density requirements for LiH vary per application and therefore physical and structural requirements for LiH are non-uniform. Historical production of LiH relies on casting processes that are limited by density and grain-size control, which leads to unfavorable machinable characteristics. LiH manufacturing is further hindered due to its chemical reactivity and propensity to readily react with moisture. This work aimed at exploring advanced fabrication techniques for LiH such as 1) uniaxial powder pressing methods and 2) laser powder bed fusion (L-PBF) additive manufacturing. Uniaxial powder compaction offers advantageous tailorable mechanical and physical properties via density control, and L-PBF can produce net-shaped complex parts with unique microstructure. Uniaxial pressing proved successful in readily producing LiH with density control.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Investigation of B 4 C for inhibiting crystallization in silica at high temperatures

Amorphous silica has numerous high temperature applications due to its inherent thermal shock resistance and low coefficient of thermal expansion (CTE). However, at the high temperatures required for processing (>1200 °C), the metastable β-cristobalite phase preferentially forms and is accompanied by a volume change, and potential cracking, upon conversion to the low temperature α-cristobalite phase. The CTE of the final crystalline phase is an order of magnitude higher than its amorphous counterpart. Here experimental results demonstrate that small additions of B 4 C (3.5 wt%) effectively inhibit silica crystallization in powder and sintered gel-cast forms up to 22h at temperatures as high as 1500°C as confirmed via x-ray diffraction. Further, the oxidation of B 4 C to B 2 O 3 and its subsequent melt and evaporation disrupts the nucleation and growth of the cristobalite phase. The mechanism for crystallization inhibition is further explored through optical microscopy to probe changes in surface morphology.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Processing and characterization of the homologous Zr x Ta 2 O 2x+5 series

In this study, Zr x Ta 2 O 2x+5 (ZTOx) was systematically studied to determine ideal solid-state synthesis and pressureless sintering conditions. For Zr 6 Ta 2 O 17 (ZTO6) and other compositions with values of x in ZTOx the optimal synthesis temperature of 1100 °C with 1 h dwell time was optimal. XRD phase analysis of the homologous series indicated that for ZTOx, x = 5, 6, 7, and 8 were within the phase stability field while x = 4 and x = 9 were outside the phase stability field. Unit cell lattice parameters changed anisotropically with Zr:Ta ratio with an overall <0.1% change in unit cell volume across the solid solution. Some Raman modes red shifted while others blue shifted, indicating competing tensile and compressive strains. Sintering of ZTOx required a progressively higher temperature as Zr-content increased despite the same starting powder grain sizes and synthesis temperature. Higher Vickers hardness for Zr-rich (12.7–12.8 GPa) than Ta-rich Zr x Ta 2 O 2x+5 (11.6–11.7 GPa) disappeared when accounting for different sintering temperatures. Indentation toughness was similar for all compositions (1.2–1.4 MPa m 1/2 ). Properties of Zr x Ta 2 O 2x+5 series indicate tunability of Zr:Ta composition ratio while maintaining the structure and room temperature mechanical properties comparable to Hf 6 Ta 2 O 17 and 8 mol% yttria stabilized zirconia ceramics.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Three-dimensional printing of ceramic materials

An ink, and products formed from the ink, formulated at least in part from ceramic particles. The ink is formulated so that it can be used in additive manufacturing processes to form three-dimensional printed bodies. The three-dimensional printed bodies can have graded density and can be infiltrated by an infiltration material.

Chandrasekaran, Swetha↗
DOE OSTI2023

Thermostructural evolution of boron carbide characterized using in-situ x-ray diffraction

Boron carbide, with a nominal stoichiometry of B 4 C, is a highly desired ceramic candidate for armor applications due to its high hardness derived from the complex crystal structure. However, stress-induced local amorphization can lead to failure and is a known challenge for this material which must be addressed for applications in ballistic environments. Understanding boron carbide's atomic structural behavior and bonding environment is critical in determining effective strategies to mitigate these issues. Here, in this work, the thermo-structural behavior of B 4 C has been studied in detail using a conical nozzle levitator system coupled with in-situ synchrotron X-ray diffraction. Lattice expansion and the resulting thermal expansion coefficients (CTEs) were determined from 25-2100 °C. Rietveld refinements showed anisotropic atomic displacement for each of the 4 unique sites as a function of temperature. An exceptionally large z-axis displacement for the boron chain center is linked to bond weakness and may be linked to faster expansion of the α 33 relative to α 11 CTEs. Thermally induced lattice changes can inform the use of boron carbide at elevated temperatures as well as help develop strategies for mitigating structural failure for armor applications.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Synthesis, sintering, and grain growth kinetics of Hf 6 Ta 2 O 17

Here Aasystematic study of the solid-state synthesis, pressureless sintering, and grain growth kinetics of Hf 6 Ta 2 O 17 is presented. The ideal conditions for solids-state synthesis of Hf 6 Ta 2 O 17 powder with minimal particle necking was 1250 °C for 2 h in air. The resultant powder has an average particle size of 210 ± 70 nm. The combined synthesis and ball-milling procedure produces highly sinterable Hf 6 Ta 2 O 17 powder, achieving > 97 % of theoretical density after pressureless sintering at 1600 °C for 2 h in air. The grain growth mechanism was sensitive to processing conditions, appearing to be primarily driven by surface diffusion below 1600 °C and grain boundary diffusion above 1650 °C. The respective activation energies for grain growth were found to be Q S = 659 ± 79 kJ mol -1 and Q GB = 478 ± 63 kJ mol -1 .

36 MATERIALS SCIENCE↗
DOE OSTI2023

Densification and microstructure features of lithium hydride fabrication

The manufacturing of lithium hydride (LiH) utilizing uniaxial pressing, which offers fabrication with tailorable properties via microstructure control, can lead to the expansion in application of LiH while bypassing the challenges presented by historical casting manufacturing techniques. Through control of consolidation conditions such as pressure, temperature, dwell time and powder load, the presented work highlights the densification of LiH, with an emphasis on quantifying oxygen content, for applications requiring a specific density range necessary for optimized material performance. Karl Fischer Titration and X-ray Diffraction proved useful in determining oxygen and phase content while Computed Tomography and Scanning Electron Microscopy provided structural analysis. The temperature dependent densification of LiH fit with an Arrhenius term resulted in an activation energy of 21.2 kJ/mol. Images of fractured surfaces of LiH pressed at 500 °C revealed drastic grain coarsening, aided by the presence of oxygen impurities.

36 MATERIALS SCIENCE↗
DOE OSTI2023

$In-situ$ synchrotron x-ray diffraction and thermal expansion of TiB2 up to ~3050 °C

There is an increasing interest in understanding the performance and properties of ultra-high temperature ceramics due to their high melting points (<3000 °C) that make them promising for extreme environment applications. In-situ high temperature X-ray diffraction experiments were performed on TiB 2 beads up to ~3050 °C. For these experiments, TiB 2 powders were fabricated into spherical beads via gel casting methods and densified in a high temperature graphite furnace. These sample beads were then levitated in a conical nozzle levitator with reducing atmosphere (3% H 2 -Ar) while being heated using a 400 W CO 2 laser. During levitation a collimated synchrotron X-ray source was used to perform in-situ, temperature-dependent structural characterizations. The anisotropic coefficients of thermal expansion of TiB 2 were characterized as a function of temperature up to ~3050 °C. Elucidation of these properties are critical for the advancement of TiB 2 ceramics and other transition metal di-borides for use in high temperature applications such as hypersonic platforms, nuclear reactors, and atmospheric re-entry.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Moisture ingress in commercial steel drums: Water content determination, diffusion modelling and predicted permeation rates

Commercial steel drums underpin the global economy, playing a pivotal role in the storage and transportation of critical materials. Transported and stored materials, such as food, chemical and nuclear waste, can be sensitive to ambient conditions, particularly moisture that can enhance negative effects such as corrosion and material degradation. Although international standards and regulations are in place for the qualification of steel drums, there are no current testing requirements, established limits or boundaries for the permeation of moisture into the drums during transportation or storage. This work aims to provide insights into the moisture ingress over time into properly sealed steel drums and provides estimated moisture ingress rates over time through extrapolation. Water vapour transmission rate (WVTR) measurements through the gasket material at 10–40°C were 0.11–2.1 g/m 2 /day resulting in a permeation activation energy of 30.2 kJ/mol. Water sorption measurements and Karl Fischer titration (KFT) on ethylene propylene diene monomer (EPDM) gasket material revealed a decrease in equilibrium moisture saturation with increasing temperature. KFT measurements also revealed the presence of moisture within the adhesive and drum wall after exposure to ambient conditions. KFT and Fourier transform infrared spectroscopy (FTIR) show that moisture will desorb from the EPDM and drum wall after exposure to desiccating conditions, although a minimal amount of moisture will remain present. When sealed to the manufacturer's recommendations, the steel drums are effective in minimizing moisture ingress. In conclusion, in sealed empty drums, moisture ingress rates for 19-L drums were 0.4–1.5 mg/day at 25°C 15% relative humidity (RH) and increased to 7.1–8.8 mg/day at 40°C 90% RH, and moisture ingress rates for 210-L drums were 2.5 and 3.5 mg/day at field deployment conditions of 15.5°C 51.5% RH and 23°C 40% RH, respectively.

42 ENGINEERING↗
DOE OSTI2021

Synthesis of nanograined zirconium diboride microsphere powder feedstock via emulsification of suspensions

Ceramic nanograined materials have desirable characteristics compared to their macroparticle counterparts but are rarely used in industrial applications due to issues with poor handleability and health hazards. Due to interparticle forces that become more dominant as the particle size decreases, it is difficult to use nanomaterials to fill dies, spread on surfaces, or flow through hoppers found in various manufacturing processes. In this work, we report a scalable gelcasting solution and unique emulsification process to create microspheres composed of nanoscale powders to enhance the flowability and handleability of nanomaterials. The gelcasting solution and emulsification process can be used with any nanoparticle composition that can be suspended in a liquid phase. This paper reports the effects of various parameters on zirconium diboride microsphere formation, such as surfactant content and mixing conditions. The microspheres maintain the nano-scale characteristics of the powder but improve its flowability by using cross-linked polyvinyl alcohol to combine irregularly shaped zirconium diboride nanoparticles with a particle diameter of 60 nm into larger spherical particles with a d 50 ~25 μm. This hierarchical feedstock engineering design combine the positive characteristics of materials across both length scales and improve the flowability of the feedstock from a Hausner Ratio of 1.56 to 1.19. The materials produced using this technique can be used in thermal plasma spray, die filling for hot pressing or spark plasma sintering, and binder jet printing applications.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Electrical Properties of Carbon Dioxide Hydrate: Implications for Monitoring CO 2 in the Gas Hydrate Stability Zone

CO 2 and CH 4 clathrate hydrates are of keen interest for energy and carbon cycle considerations. While both typically form on Earth as cubic structure I (sI), we find that pure CO 2 hydrate exhibits over an order of magnitude higher electrical conductivity ( σ ) than pure CH 4 hydrate at geologically relevant temperatures. In this study, the conductivity was obtained from frequency-dependent impedance ( Z ) measurements made on polycrystalline CO 2 hydrate (CO 2 ·6.0 ± 0.2H 2 O by methods here) with 25% gas-filled porosity, compared with CH 4 hydrate (CH 4 ·5.9H 2 O) formed and measured in the same apparatus and exhibiting closely matching grain characteristics. The conductivity of CO 2 hydrate is 6.5 × 10 –4 S/m at 273K with an activation energy ( E a ) of 46.5 kJ/mol at 260–281 K, compared with ~5 × 10 –5 S/m and 34.8 kJ/m for CH 4 hydrate. Equivalent circuit modeling indicates that different pathways govern conduction in CO 2 versus CH 4 hydrate. Results show promise for use of electromagnetic methods in monitoring CO 2 hydrate formation in certain natural settings or in CO 2 /CH 4 exchange efforts.

58 GEOSCIENCES↗