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Title: Facile emulsion mediated synthesis of phase-pure diopside nanoparticles

Abstract

Diopside is a common natural pyroxene that is rarely found in a pure state, since magnesium is often partially substituted by iron, and other elements (sodium and aluminum) are often present. This pyroxene, along with feldspars and olivines, is common in concrete. As the prospective license renewal of light water reactors to 80 years of operation has raised concerns on the effects of radiation in the concrete biological shield surrounding the reactors, mineral nanoparticles can be valuable to perform amorphization studies to inform predictive models of mechanical properties of irradiated concrete. The synthesis of diopside nanoparticles was achieved in this study using a reverse-micelle sol-gel method employing TEOS, calcium chloride and Mg(MeO) 2 in a methanol/toluene solution. Tert-butylamine and water were used as hydrolysis agents, and dodecylamine as a surfactant. The resulting amorphous precursor was centrifuged to remove organics and fired at 800 °C. Additional reaction with hydrogen peroxide was used to remove amine remnants. TEM and SEM examinations revealed a product comprised of 50–100 nm diameter nanoparticles. XRD indicated phase pure diopside and BET indicated a surface area of 63.5 m 2/g before peroxide treatment, which at a bulk density of 3.4 g/cm 3 is equivalent to particles withmore » diameter of 28 nm.« less

Authors:
ORCiD logo [1]; ORCiD logo [2]; ORCiD logo [1]; ORCiD logo [3]; ORCiD logo [1]
  1. Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Fusion and Materials for Nuclear Systems Division
  2. Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Chemical Sciences Division
  3. Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Center for Nanophase Materials Science (CNMS)
Publication Date:
Research Org.:
Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)
Sponsoring Org.:
USDOE Office of Nuclear Energy (NE); USDOE Office of Science (SC), Basic Energy Sciences (BES) (SC-22). Chemical Sciences, Geosciences & Biosciences Division
OSTI Identifier:
1468047
Grant/Contract Number:  
AC05-00OR22725
Resource Type:
Accepted Manuscript
Journal Name:
Scientific Reports
Additional Journal Information:
Journal Volume: 8; Journal Issue: 1; Journal ID: ISSN 2045-2322
Publisher:
Nature Publishing Group
Country of Publication:
United States
Language:
English
Subject:
36 MATERIALS SCIENCE; 37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY

Citation Formats

Tajuelo Rodriguez, Elena, Anovitz, Lawrence M., Clement, Caleb D., Rondinone, Adam J., and Cheshire, Michael C. Facile emulsion mediated synthesis of phase-pure diopside nanoparticles. United States: N. p., 2018. Web. doi:10.1038/s41598-018-21485-9.
Tajuelo Rodriguez, Elena, Anovitz, Lawrence M., Clement, Caleb D., Rondinone, Adam J., & Cheshire, Michael C. Facile emulsion mediated synthesis of phase-pure diopside nanoparticles. United States. doi:10.1038/s41598-018-21485-9.
Tajuelo Rodriguez, Elena, Anovitz, Lawrence M., Clement, Caleb D., Rondinone, Adam J., and Cheshire, Michael C. Thu . "Facile emulsion mediated synthesis of phase-pure diopside nanoparticles". United States. doi:10.1038/s41598-018-21485-9. https://www.osti.gov/servlets/purl/1468047.
@article{osti_1468047,
title = {Facile emulsion mediated synthesis of phase-pure diopside nanoparticles},
author = {Tajuelo Rodriguez, Elena and Anovitz, Lawrence M. and Clement, Caleb D. and Rondinone, Adam J. and Cheshire, Michael C.},
abstractNote = {Diopside is a common natural pyroxene that is rarely found in a pure state, since magnesium is often partially substituted by iron, and other elements (sodium and aluminum) are often present. This pyroxene, along with feldspars and olivines, is common in concrete. As the prospective license renewal of light water reactors to 80 years of operation has raised concerns on the effects of radiation in the concrete biological shield surrounding the reactors, mineral nanoparticles can be valuable to perform amorphization studies to inform predictive models of mechanical properties of irradiated concrete. The synthesis of diopside nanoparticles was achieved in this study using a reverse-micelle sol-gel method employing TEOS, calcium chloride and Mg(MeO)2 in a methanol/toluene solution. Tert-butylamine and water were used as hydrolysis agents, and dodecylamine as a surfactant. The resulting amorphous precursor was centrifuged to remove organics and fired at 800 °C. Additional reaction with hydrogen peroxide was used to remove amine remnants. TEM and SEM examinations revealed a product comprised of 50–100 nm diameter nanoparticles. XRD indicated phase pure diopside and BET indicated a surface area of 63.5 m2/g before peroxide treatment, which at a bulk density of 3.4 g/cm3 is equivalent to particles with diameter of 28 nm.},
doi = {10.1038/s41598-018-21485-9},
journal = {Scientific Reports},
number = 1,
volume = 8,
place = {United States},
year = {2018},
month = {2}
}

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