Phase transformations in oxides above 2000°C: experimental technique development
Abstract
The oxidation of boride and carbide-based ultra-high-temperature ceramics is the primary limiting factor for their use as aerodynamic surfaces. Understanding the behaviour of the oxides that can result from oxidation of metal borides and carbides at very high temperatures is essential to optimise and tailor the performance of these materials; yet experimental thermodynamic and structural data for refractory oxides above 2000°C are mostly absent. The following techniques that can be applied to fill this gap are discussed: (i) commercial ultra-high-temperature differential thermal analysis for investigation of phase transformations and melting in inert environments to 2500°C, (ii) a combination of laser heating with a splittable nozzle aerodynamic levitator for splat quenching and drop calorimetry from temperatures limited only by sample evaporation, (iii) synchrotron X-ray and neutron diffraction on laser-heated aerodynamically levitated oxide samples for in situ observation of phase transformations in variable atmospheres, refinement of high-temperature structures and thermal expansion. Recent experimental findings include anomalous thermal expansion of the defect fluorite phase of YSZ, thermodynamics of pyrochlore–fluorite transformation from high-temperature structure refinements, and measurement of thermal expansion to the melting temperatures and fusion enthalpies of Zr, Hf, La, Yb and Lu oxides. These methods provide temperatures, enthalpies and volume change formore »
- Authors:
-
[1];
[1];
[1];
[1];
[1];
[2];
[2];
[3];
[4];
[4];
[1]
- Univ. of California, Davis, CA (United States)
- Argonne National Lab. (ANL), Lemont, IL (United States)
- Argonne National Lab. (ANL), Lemont, IL (United States); Materials Development Inc., Arlington Heights, IL (United States)
- Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)
- Publication Date:
- Research Org.:
- Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Argonne National Lab. (ANL), Argonne, IL (United States)
- Sponsoring Org.:
- National Science Foundation (NSF); USDOE Office of Science (SC), Basic Energy Sciences (BES)
- OSTI Identifier:
- 1492158
- Alternate Identifier(s):
- OSTI ID: 1496229; OSTI ID: 1630528
- Grant/Contract Number:
- AC05-00OR22725; AC02-06CH11357
- Resource Type:
- Accepted Manuscript
- Journal Name:
- Advances in Applied Ceramics
- Additional Journal Information:
- Journal Volume: 117; Journal Issue: sup1; Journal ID: ISSN 1743-6753
- Publisher:
- Taylor & Francis
- Country of Publication:
- United States
- Language:
- English
- Subject:
- 36 MATERIALS SCIENCE; thermal analysis; X-ray diffraction; oxides; phase diagrams; calorimetry; neutron diffraction; thermal expansion
Citation Formats
Ushakov, Sergey V., Maram, Pardha S., Kapush, Denys, Pavlik, III, Alfred J., Fyhrie, Matthew, Gallington, Leighanne C., Benmore, Chris J., Weber, Richard, Neuefeind, Joerg C., McMurray, Jake W., and Navrotsky, Alexandra. Phase transformations in oxides above 2000°C: experimental technique development. United States: N. p., 2018.
Web. doi:10.1080/17436753.2018.1516267.
Ushakov, Sergey V., Maram, Pardha S., Kapush, Denys, Pavlik, III, Alfred J., Fyhrie, Matthew, Gallington, Leighanne C., Benmore, Chris J., Weber, Richard, Neuefeind, Joerg C., McMurray, Jake W., & Navrotsky, Alexandra. Phase transformations in oxides above 2000°C: experimental technique development. United States. https://doi.org/10.1080/17436753.2018.1516267
Ushakov, Sergey V., Maram, Pardha S., Kapush, Denys, Pavlik, III, Alfred J., Fyhrie, Matthew, Gallington, Leighanne C., Benmore, Chris J., Weber, Richard, Neuefeind, Joerg C., McMurray, Jake W., and Navrotsky, Alexandra. Mon .
"Phase transformations in oxides above 2000°C: experimental technique development". United States. https://doi.org/10.1080/17436753.2018.1516267. https://www.osti.gov/servlets/purl/1492158.
@article{osti_1492158,
title = {Phase transformations in oxides above 2000°C: experimental technique development},
author = {Ushakov, Sergey V. and Maram, Pardha S. and Kapush, Denys and Pavlik, III, Alfred J. and Fyhrie, Matthew and Gallington, Leighanne C. and Benmore, Chris J. and Weber, Richard and Neuefeind, Joerg C. and McMurray, Jake W. and Navrotsky, Alexandra},
abstractNote = {The oxidation of boride and carbide-based ultra-high-temperature ceramics is the primary limiting factor for their use as aerodynamic surfaces. Understanding the behaviour of the oxides that can result from oxidation of metal borides and carbides at very high temperatures is essential to optimise and tailor the performance of these materials; yet experimental thermodynamic and structural data for refractory oxides above 2000°C are mostly absent. The following techniques that can be applied to fill this gap are discussed: (i) commercial ultra-high-temperature differential thermal analysis for investigation of phase transformations and melting in inert environments to 2500°C, (ii) a combination of laser heating with a splittable nozzle aerodynamic levitator for splat quenching and drop calorimetry from temperatures limited only by sample evaporation, (iii) synchrotron X-ray and neutron diffraction on laser-heated aerodynamically levitated oxide samples for in situ observation of phase transformations in variable atmospheres, refinement of high-temperature structures and thermal expansion. Recent experimental findings include anomalous thermal expansion of the defect fluorite phase of YSZ, thermodynamics of pyrochlore–fluorite transformation from high-temperature structure refinements, and measurement of thermal expansion to the melting temperatures and fusion enthalpies of Zr, Hf, La, Yb and Lu oxides. These methods provide temperatures, enthalpies and volume change for phase transformations above 2000°C, which are required for thermodynamic assessments and calculation of phase diagrams of multicomponent systems.},
doi = {10.1080/17436753.2018.1516267},
journal = {Advances in Applied Ceramics},
number = sup1,
volume = 117,
place = {United States},
year = {Mon Nov 19 00:00:00 EST 2018},
month = {Mon Nov 19 00:00:00 EST 2018}
}
Free Publicly Available Full Text
Publisher's Version of Record
Other availability
Search WorldCat to find libraries that may hold this journal
Cited by: 9 works
Citation information provided by
Web of Science
Web of Science
Figures / Tables:
Figure 1: DTA of melting and crystallisation of Y2O3 and instrument schematics. Experiments performed in Ar flow at 10°C/min heating and cooling rates on 87.34 mg Y2O3, laser melted and sealed in W crucible. No corrections or baseline subtractions applied. Cooling and heating segments were recorded with different sensors –more »
All figures and tables
(5 total)
Save to My Library
You must Sign In or Create an Account in order to save documents to your library.
Works referenced in this record:
Thermal Property Measurements at Very High Temperatures
journal, June 1960
- Rasor, N. S.; McClelland, J. D.
- Review of Scientific Instruments, Vol. 31, Issue 6
New techniques for high-temperature melting measurements in volatile refractory materials via laser surface heating
journal, November 2008
- Manara, D.; Sheindlin, M.; Heinz, W.
- Review of Scientific Instruments, Vol. 79, Issue 11
Drop-and-catch (DnC) calorimetry using aerodynamic levitation and laser heating
journal, October 2016
- Ushakov, Sergey V.; Shvarev, Alexey; Alexeev, Timur
- Journal of the American Ceramic Society, Vol. 100, Issue 2
Aerodynamic levitation technique for containerless high temperature studies on liquid and solid samples
journal, December 1976
- Winborne, David A.; Nordine, Paul C.; Rosner, Daniel E.
- Metallurgical Transactions B, Vol. 7, Issue 4
The Visibility of Radiation in the Red End of the Visible Spectrum
journal, September 1915
- Hyde, Edward P.; Forsythe, W. E.
- The Astrophysical Journal, Vol. 42
DTA method applikation to the highest refractory oxide systems investigation
journal, September 1985
- Shevthenko, A. V.; Lopato, L. M.
- Thermochimica Acta, Vol. 93
Aerodynamic levitation of laser‐heated solids in gas jets
journal, September 1982
- Nordine, Paul C.; Atkins, Robert M.
- Review of Scientific Instruments, Vol. 53, Issue 9
Experimental Approaches to the Thermodynamics of Ceramics Above 1500°C
journal, March 2012
- Ushakov, Sergey V.; Navrotsky, Alexandra
- Journal of the American Ceramic Society, Vol. 95, Issue 5
Solid-liquid phase equilibria of Fe-Cr-Al alloys and spinels
journal, August 2017
- McMurray, J. W.; Hu, R.; Ushakov, S. V.
- Journal of Nuclear Materials, Vol. 492
Principles of the optical differential thermal analysis (ODTA)
journal, October 1988
- Caslavsky, J. L.
- Thermochimica Acta, Vol. 134
Melting temperatures of refractory oxides: Part I
journal, January 1982
- Hlavac, J.
- Pure and Applied Chemistry, Vol. 54, Issue 3
A levitation instrument for containerless study of molten materials
journal, December 2012
- Nordine, Paul C.; Merkley, Dennis; Sickel, Jeffrey
- Review of Scientific Instruments, Vol. 83, Issue 12
A combined experimental and theoretical study of enthalpy of phase transition and fusion of yttria above 2000 °C using “drop-n-catch” calorimetry and first-principles calculation
journal, February 2017
- Kapush, D.; Ushakov, S. V.; Navrotsky, A.
- Acta Materialia, Vol. 124
Thermophysical properties of 22 pure metals in the solid and liquid state – The pulse-heating data collection
journal, January 2011
- Hüpf, T.; Cagran, C.; Pottlacher, G.
- EPJ Web of Conferences, Vol. 15
In Situ Diffraction from Levitated Solids Under Extreme Conditions—Structure and Thermal Expansion in the Eu 2 O 3 –ZrO 2 System
journal, December 2014
- Maram, Pardha S.; Ushakov, Sergey V.; Weber, Richard J. K.
- Journal of the American Ceramic Society, Vol. 98, Issue 4
Aerodynamic levitation, supercooled liquids and glass formation
journal, May 2017
- Benmore, C. J.; Weber, J. K. R.
- Advances in Physics: X, Vol. 2, Issue 3
GSAS-II : the genesis of a modern open-source all purpose crystallography software package
journal, March 2013
- Toby, Brian H.; Von Dreele, Robert B.
- Journal of Applied Crystallography, Vol. 46, Issue 2
CALPHAD, first and second generation – Birth of the materials genome
journal, January 2014
- Kaufman, Larry; Ågren, John
- Scripta Materialia, Vol. 70
Material design and development: From classical thermodynamics to CALPHAD and ICME approaches
journal, September 2015
- Luo, Alan A.
- Calphad, Vol. 50
Aerodynamic levitation and laser heating:: Applications at synchrotron and neutron sources
journal, May 2011
- Hennet, L.; Cristiglio, V.; Kozaily, J.
- The European Physical Journal Special Topics, Vol. 196, Issue 1
Structure and Thermal Expansion of YSZ and La 2 Zr 2 O 7 Above 1500°C from Neutron Diffraction on Levitated Samples
journal, July 2015
- Ushakov, Sergey V.; Navrotsky, Alexandra; Weber, Richard J. K.
- Journal of the American Ceramic Society, Vol. 98, Issue 10
Direct measurements of fusion and phase transition enthalpies in lanthanum oxide
journal, February 2011
- Ushakov, Sergey V.; Navrotsky, Alexandra
- Journal of Materials Research, Vol. 26, Issue 7
On the thermodynamic modeling of the Zr–O system
journal, September 2004
- Wang, Chong; Zinkevich, Matvei; Aldinger, Fritz
- Calphad, Vol. 28, Issue 3
Direct observation of the liquid miscibility gap in the zirconia–silica system
journal, November 2015
- Telle, Rainer; Greffrath, Fabian; Prieler, Robert
- Journal of the European Ceramic Society, Vol. 35, Issue 14
The Melting-Point of Tungsten
journal, August 1915
- Langmuir, Irving
- Physical Review, Vol. 6, Issue 2
Levitation apparatus for structural studies of high temperature liquids using synchrotron radiation
journal, September 1997
- Krishnan, Shankar; Felten, John J.; Rix, James E.
- Review of Scientific Instruments, Vol. 68, Issue 9
Particle surface temperature measurements with multicolor band pyrometry
journal, January 2009
- Lu, Hong; Ip, Leong-Teng; Mackrory, Andrew
- AIChE Journal, Vol. 55, Issue 1
Laser Melting of Zirconium Carbide: Determination of Phase Transitions in Refractory Ceramic Systems: Laser Melting of Zirconium Carbide
journal, April 2011
- Jackson, Heather F.; Jayaseelan, Daniel D.; Manara, Dario
- Journal of the American Ceramic Society, Vol. 94, Issue 10
Structure and thermal expansion of Lu2O3 and Yb2O3 up to the melting points
journal, November 2017
- Pavlik, Alfred; Ushakov, Sergey V.; Navrotsky, Alexandra
- Journal of Nuclear Materials, Vol. 495
The Spectropyrometer—a Practical Multi-wavelength Pyrometer
conference, January 2003
- Felice, Ralph A.
- TEMPERATURE: Its Measurement and Control in Science and Industry; Volume VII; Eighth Temperature Symposium, AIP Conference Proceedings
Probing disorder in pyrochlore oxides using in situ synchrotron diffraction from levitated solids–A thermodynamic perspective
journal, July 2018
- Maram, Pardha S.; Ushakov, Sergey V.; Weber, Richard J. K.
- Scientific Reports, Vol. 8, Issue 1
Thermochemistry of lanthanum zirconate pyrochlore
journal, November 2009
- Radha, A. V.; Ushakov, Sergey V.; Navrotsky, Alexandra
- Journal of Materials Research, Vol. 24, Issue 11
Properties of high-temperature melts using levitation
journal, January 2000
- Nordine, Paul C.; Weber, J. K. Richard; Abadie, Johan G.
- Pure and Applied Chemistry, Vol. 72, Issue 11
Direct Measurement of Fusion Enthalpy of LaAlO 3 and Comparison of Energetics of Melt, Glass, and Amorphous Thin Films
journal, January 2014
- Ushakov, Sergey V.; Navrotsky, Alexandra
- Journal of the American Ceramic Society, Vol. 97, Issue 5
The melting-point of tungsten
journal, October 1915
- Langmuir, Irving
- Journal of the Franklin Institute, Vol. 180, Issue 4
Theory and practice of radiation thermometry
journal, July 1991
- Garimella, Suresh V.
- Experimental Thermal and Fluid Science, Vol. 4, Issue 4
Figures / Tables found in this record:
Figures/Tables have been extracted from DOE-funded journal article accepted manuscripts.