Bead Fabrication for Extreme Environment Analysis Development

Project Overview

High temperature materials testing is a challenge due to the difficulty of collecting quality data that is able to uncover fundamental properties of the systems of interest. This is especially important when tailoring materials and designs for new systems which are subjected to hypersonic speeds creating environments that can affect or even degrade the most robust materials, leading to a reduction in system performance or even failure. In order to advance research and developments in this field, a better understanding of these materials and their behavior at high temperature is necessary. The work undertaken by this project team presents an in-depth materials study of ultra-high temperature ceramics (such as Ti, Zr, Nb, Hf, Ta carbides, borides, and nitrides) along with other relevant ceramics, composites, and even metals for high temperature applications using in-situ and ex-situ characterization techniques that track the thermochemical and thermophysical properties of these compounds on multiple length scales.

Major advancements that were enabled by this project are shown through novel fabrication techniques, a deep dive in atomic scale characterization of materials at extreme temperatures, and development of bulk testing through a standardization study. Spherical beads (~3 mm) were fabricated through a material and shape agnostic technique developed here at Lawrence Livermore National Laboratory (LLNL). These developed fabrication techniques allowed high temperature synchrotron X-ray diffraction experiments to be carried out on 44 different compositions of materials which otherwise could not have been tested in the presented levitation method. These fabricated beads were heated during levitation using a conical nozzle levitator system equipped with CO2 lasers at Argonne National Laboratory to collect high temperature data through a container less method across the relevant operating temperatures and up to ~3050°C. The materials were characterized using high temperature in-situ X-ray diffraction for crystallographic evaluation at the atomic scale, ceramic test parts were studied to observe microstructural effects using X-ray CT along with microscopy methods, and bulk testing using an oxyacetylene torch paired with ex-situ evaluation was used for standardization of this new LLNL capability. The techniques utilized through this study are relevant to a variety of materials which have high temperature applications and allowed this project team to be the first to observe these high temperature properties with a high level of fidelity. Through this work a repository of fundamental data on the chemical behavior of ultra-high temperature ceramic materials, composites, and metals at extreme temperatures was collected which can be used to inform accurate modeling and simulations. This data will serve as a baseline for researchers worldwide striving to advance materials and presents the versatility of the method as a rapid screening capability to test tailored materials with relevance to DOE and DOD applications.

Mission Impact

This project has developed science and technology tools and capabilities to meet future national security challenges through the in-depth study of ceramics, composite materials, and even metals at extreme temperatures on multiple length scales presented by this work. The data that has been gathered through this project will provide a basis for researchers at the lab and beyond performing materials calculations and modeling and will guide materials selection for several different high temperature applications. The project team was able to form new collaborations within the laboratory, across DOD institutions, and academia leading to more opportunities for follow on work due to a diverse team. Strong academic collaborations made through this project have opened doors to further educational development of staff members at LLNL through the University of California distance learning program. In addition, presentation of results both internally and externally have led to new research directions within the realm of materials forensics focused on ceramics through the expertise built in this project. 

Publications, Presentations, and Patents

Charalambous, Qirong Yang, Jesus Rivera, Isabel R. Cystal, Leila Yici Sun, Fox thorpe, William Rosenberg, Scott McCormack, Gabriella C. S. King, James T. Cahil, Wyaltt L DuFrane, Joshua D. Kuntz, Elizabeth Sobalvarro Converse. "Thermostructural evolution of boron carbide characterized using in-situ x-ray diffraction." Acta Materialia. Volume 265, 15 February 2024, 119597. https://doi.org/10.1016/j.actamat.2023.119597

Converse, E.S., F. Thorpe, J. Rivera, H. Charalambous, G. King, J.T. Cahill, W.L. Du Frane, J.D. Kuntz, S.J. McCormack. "In-situ synchrotron x-ray diffraction and thermal expansion of TiB2 up to ∼3050 °C." Journal of the European Ceramic Society 43(8) (2023) 3005-301 https://doi.org/10.1016/j.jeurceramsoc.2023.01.050

E.Converse,F.Thorpe, J. Rivera, H. Charalambous, Q.R. Yang, S. Chandrasekaran, A. Wat, G. King, J. Cahill, S.J. McCormack,  W. Du Frane, J. Kuntz, "Ultra high temperature evaluation of metal diborides MB2 (M = Ta, Ti, Hf, Zr, Nb)" (Presentation, Conference Talk at CMS Conference, St Augustine, Florida, January 2023). 

Sobalvarro Converse, E.M.; Thorpe, F.; Rivera, J.; Charalambous, H.; Yang, Q. R.; Chandrasekaran, S.; Wat, A.; King, G.; Cahill, J.; McCormack, S.J.; Du Frane, W.; Kuntz, J.,  "Ultra high temperature evaluation of metal diborides MB2 (M = Ta, Ti, Hf, Zr, Nb)" (Presentation, Conference Talk at STOHT Conference, Tempe, Arizona, August 2022). 

Sobalvarro Converse, E.M.; Thorpe, F.; Rivera, J.; Charalambous, H.; Yang, Q. R.; Chandrasekaran, S.; Wat, A.; King, G.; Cahill, J.; McCormack, S.J.; Du Frane, W.; Kuntz, J., "From the atomic scale to the bulk: Ultra high temperature evaluation of metal diborides MB2 (M = Ta, Ti, Hf, Zr, Nb)" (Presentation, Conference Talk at Ultra-High Temperature Ceramics: Materials For Extreme Environment Applications V, Snowbird, Utah, July 2022). 

F. Thorpe, S.J. McCormack, E. M. Converse Sobalvarro, G. King, W. Du Frane, J. Kuntz,"Environmental Conical Nozzle Levitator Equipped with Dual Lasers"(Poster Presentation, Ultra-High Temperature Ceramics: Materials For Extreme Environment Applications V, Snowbird, Utah, July 2022). 

S.J. McCormack, F. Thorpe, E.M. Converse Sobalvarro, G. King, W. Du Frane, J. Kuntz,"In-situ high temperature spatially resolved X-ray diffraction of TiB2 up to ~3250 ˚C" (Presentation, Conference Talk at Ultra-High Temperature Ceramics: Materials For Extreme Environment Applications V, Snowbird, Utah, July 2022). 

S.J. McCormack, S. Ness, F. Thorpe, E.M. Converse Sobalvarro, G. King, J. Cahill, "High temperature thermochemical and thermophysical properties of ZrB2 up to 3400 ˚C" (Presentation, Invited Talk at 46th International Conference and Expo on Advanced Ceramics and Composites (ICACC 2022), Virtual, January 2022).