High temperature X-ray studies of mayenite synthesized using the citrate sol-gel method

Sabina N. Ude; Claudia J. Rawn; Roberta A. Peascoe; Melanie J. Kirkham; Gregory L. Jones; E. Andrew Payzant

doi:10.1016/j.ceramint.2013.06.112

High temperature X-ray studies of mayenite synthesized using the citrate sol-gel method

Sabina N. Ude, Claudia J. Rawn, Roberta A. Peascoe, Melanie J. Kirkham, Gregory L. Jones, E. Andrew Payzant

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27 Scopus citations

Abstract

Room temperature and high temperature x-ray powder diffraction and differential thermal analysis/thermo-gravimetric analysis (DTA/TGA) have been used to characterize the phase evolution of bulk mayenite (Ca ₁₂Al₁₄O₃₃) prepared using the citrate sol-gel method. These studies have shown that single phase mayenite forms at 900 C in air after approximately three hours. High temperature x-ray powder diffraction data show that when firing in air at temperatures 600 C and below only amorphous content is observed; above 600 C CaCO₃ is the first phase to crystallize. For samples quenched at 800 C and evaluated using room temperature x-ray powder diffraction mayenite, CaAl₂O₄, and CaCO ₃ were present. High temperature x-ray diffraction data collected while firing in 4% H₂/96% N₂ reveals that CaCO₃ does not form and Ca₁₂Al₁₄O₃₃ starts to form around 850 C. DTA/TGA data collected either in a nitrogen environment or air on samples synthesized using the citrate gel method support the complete decomposition of metastable phases and the formation of mayenite at 900 C, although the phase evolution is different depending on the environment.

Original language	English
Pages (from-to)	1117-1123
Number of pages	7
Journal	Ceramics International
Volume	40
Issue number	1 PART A
DOIs	https://doi.org/10.1016/j.ceramint.2013.06.112
State	Published - Jan 2014

Funding

SNU was partly supported by Pipeline Engineering Diversity Program under DOE grant DE-FG02-05ER25717 , and partly sponsored by the Center for Materials Processing (CMP) at the University of Tennessee. X-ray powder diffraction data were collected at the High Temperature Materials Laboratory at Oak Ridge National Laboratory, which is sponsored by the US Department of Energy, Office of Energy Efficiency and Renewable Energy, Vehicle Technologies Program. A portion of this research was conducted at the Center for Nanophase Materials Sciences, sponsored at Oak Ridge National Laboratory by the Scientific User Facilities Division, Office of Basic Energy Sciences, US Department of Energy. The authors would like to thank Austin Albert for his help with the BET data collection and analysis.

Funders	Funder number
Scientific User Facilities Division
U.S. Department of Energy	DE-FG02-05ER25717
Office of Energy Efficiency and Renewable Energy
Basic Energy Sciences
Oak Ridge National Laboratory
University of Tennessee

Keywords

A. Citrate sol-gel
B. High temperature X-ray
B. Scanning electron microscopy
C. Thermal expansion

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10.1016/j.ceramint.2013.06.112

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title = "High temperature X-ray studies of mayenite synthesized using the citrate sol-gel method",

abstract = "Room temperature and high temperature x-ray powder diffraction and differential thermal analysis/thermo-gravimetric analysis (DTA/TGA) have been used to characterize the phase evolution of bulk mayenite (Ca 12Al14O33) prepared using the citrate sol-gel method. These studies have shown that single phase mayenite forms at 900 C in air after approximately three hours. High temperature x-ray powder diffraction data show that when firing in air at temperatures 600 C and below only amorphous content is observed; above 600 C CaCO3 is the first phase to crystallize. For samples quenched at 800 C and evaluated using room temperature x-ray powder diffraction mayenite, CaAl2O4, and CaCO 3 were present. High temperature x-ray diffraction data collected while firing in 4% H2/96% N2 reveals that CaCO3 does not form and Ca12Al14O33 starts to form around 850 C. DTA/TGA data collected either in a nitrogen environment or air on samples synthesized using the citrate gel method support the complete decomposition of metastable phases and the formation of mayenite at 900 C, although the phase evolution is different depending on the environment.",

keywords = "A. Citrate sol-gel, B. High temperature X-ray, B. Scanning electron microscopy, C. Thermal expansion",

author = "Ude, {Sabina N.} and Rawn, {Claudia J.} and Peascoe, {Roberta A.} and Kirkham, {Melanie J.} and Jones, {Gregory L.} and {Andrew Payzant}, E.",

year = "2014",

month = jan,

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language = "English",

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AU - Rawn, Claudia J.

AU - Peascoe, Roberta A.

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AU - Jones, Gregory L.

AU - Andrew Payzant, E.

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N2 - Room temperature and high temperature x-ray powder diffraction and differential thermal analysis/thermo-gravimetric analysis (DTA/TGA) have been used to characterize the phase evolution of bulk mayenite (Ca 12Al14O33) prepared using the citrate sol-gel method. These studies have shown that single phase mayenite forms at 900 C in air after approximately three hours. High temperature x-ray powder diffraction data show that when firing in air at temperatures 600 C and below only amorphous content is observed; above 600 C CaCO3 is the first phase to crystallize. For samples quenched at 800 C and evaluated using room temperature x-ray powder diffraction mayenite, CaAl2O4, and CaCO 3 were present. High temperature x-ray diffraction data collected while firing in 4% H2/96% N2 reveals that CaCO3 does not form and Ca12Al14O33 starts to form around 850 C. DTA/TGA data collected either in a nitrogen environment or air on samples synthesized using the citrate gel method support the complete decomposition of metastable phases and the formation of mayenite at 900 C, although the phase evolution is different depending on the environment.

AB - Room temperature and high temperature x-ray powder diffraction and differential thermal analysis/thermo-gravimetric analysis (DTA/TGA) have been used to characterize the phase evolution of bulk mayenite (Ca 12Al14O33) prepared using the citrate sol-gel method. These studies have shown that single phase mayenite forms at 900 C in air after approximately three hours. High temperature x-ray powder diffraction data show that when firing in air at temperatures 600 C and below only amorphous content is observed; above 600 C CaCO3 is the first phase to crystallize. For samples quenched at 800 C and evaluated using room temperature x-ray powder diffraction mayenite, CaAl2O4, and CaCO 3 were present. High temperature x-ray diffraction data collected while firing in 4% H2/96% N2 reveals that CaCO3 does not form and Ca12Al14O33 starts to form around 850 C. DTA/TGA data collected either in a nitrogen environment or air on samples synthesized using the citrate gel method support the complete decomposition of metastable phases and the formation of mayenite at 900 C, although the phase evolution is different depending on the environment.

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JO - Ceramics International

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ER -

High temperature X-ray studies of mayenite synthesized using the citrate sol-gel method

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