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Title: Thermally-Induced morphological evolution of spherical silica nanoparticles using in-operando X-ray scattering measurements

Abstract

The assembly and morphology of pores determine thermodynamic, flow and reactive properties of confined fluids. Yet, there is a limited understanding of how pore architectures dynamically develop in engineered and natural materials. To develop a calibrated understanding of fluid properties in confinement, the synthesis of architected materials has been proposed. The design of geo-architected materials has to be informed by the dynamic evolution of the morphology in response to thermal or chemical events. Here, we probe thermally induced morphological evolution of spherical silica nanoparticles 220 ± 30 nm in diameter using in-operando Ultra-Small and Small Angle X-Ray Scattering measurements. The calcination experiments demonstrated that at temperatures up to 600 °C the pore radii remained in the range of 2.15 nm–2.35 nm and the particle diameters in the range of 220 ± 30 nm. Sintering these calcined silica nanoparticles to temperatures up to 1050 °C reduced the pore size from 2.2 ± 0.1 nm to ~1.8–0.2 nm. These changes corresponded to the formation of siloxane (Si-O-Si) bridges resulting from dehydroxylation. The characteristic pore radius of sintered particles was also confirmed by N2 adsorption measurements. These studies represent the use of non-invasive dynamic characterization methods such as X-ray scattering to elucidate thermallymore » induced morphological evolution in architected siliceous materials.« less

Authors:
ORCiD logo [1];  [2];  [2]; ORCiD logo [1];  [3];  [2]; ORCiD logo [1]
  1. Cornell Univ., Ithaca, NY (United States)
  2. Univ. of Utah, Salt Lake City, UT (United States)
  3. Argonne National Lab. (ANL), Argonne, IL (United States)
Publication Date:
Research Org.:
Energy Frontier Research Centers (EFRC) (United States). Multi-Scale Fluid-Solid Interactions in Architected and Natural Materials (MUSE); Univ. of Utah, Salt Lake City, UT (United States); Argonne National Laboratory (ANL), Argonne, IL (United States)
Sponsoring Org.:
USDOE Office of Science (SC), Basic Energy Sciences (BES)
OSTI Identifier:
1596100
Alternate Identifier(s):
OSTI ID: 1580177; OSTI ID: 1615468
Grant/Contract Number:  
SC0019285; AC02-06CH11357
Resource Type:
Accepted Manuscript
Journal Name:
Colloids and Surfaces. A, Physicochemical and Engineering Aspects
Additional Journal Information:
Journal Volume: 586; Journal Issue: C; Journal ID: ISSN 0927-7757
Publisher:
Elsevier
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY; SiO2 nanoparticles; Sintering; X-ray scattering; sintering

Citation Formats

Asgar, Hassnain, Semeykina, Viktoriya, Hunt, Mikaila, Mohammed, Sohaib, Kuzmenko, Ivan, Zharov, Ilya, and Gadikota, Greeshma. Thermally-Induced morphological evolution of spherical silica nanoparticles using in-operando X-ray scattering measurements. United States: N. p., 2019. Web. doi:10.1016/j.colsurfa.2019.124260.
Asgar, Hassnain, Semeykina, Viktoriya, Hunt, Mikaila, Mohammed, Sohaib, Kuzmenko, Ivan, Zharov, Ilya, & Gadikota, Greeshma. Thermally-Induced morphological evolution of spherical silica nanoparticles using in-operando X-ray scattering measurements. United States. https://doi.org/10.1016/j.colsurfa.2019.124260
Asgar, Hassnain, Semeykina, Viktoriya, Hunt, Mikaila, Mohammed, Sohaib, Kuzmenko, Ivan, Zharov, Ilya, and Gadikota, Greeshma. Sat . "Thermally-Induced morphological evolution of spherical silica nanoparticles using in-operando X-ray scattering measurements". United States. https://doi.org/10.1016/j.colsurfa.2019.124260. https://www.osti.gov/servlets/purl/1596100.
@article{osti_1596100,
title = {Thermally-Induced morphological evolution of spherical silica nanoparticles using in-operando X-ray scattering measurements},
author = {Asgar, Hassnain and Semeykina, Viktoriya and Hunt, Mikaila and Mohammed, Sohaib and Kuzmenko, Ivan and Zharov, Ilya and Gadikota, Greeshma},
abstractNote = {The assembly and morphology of pores determine thermodynamic, flow and reactive properties of confined fluids. Yet, there is a limited understanding of how pore architectures dynamically develop in engineered and natural materials. To develop a calibrated understanding of fluid properties in confinement, the synthesis of architected materials has been proposed. The design of geo-architected materials has to be informed by the dynamic evolution of the morphology in response to thermal or chemical events. Here, we probe thermally induced morphological evolution of spherical silica nanoparticles 220 ± 30 nm in diameter using in-operando Ultra-Small and Small Angle X-Ray Scattering measurements. The calcination experiments demonstrated that at temperatures up to 600 °C the pore radii remained in the range of 2.15 nm–2.35 nm and the particle diameters in the range of 220 ± 30 nm. Sintering these calcined silica nanoparticles to temperatures up to 1050 °C reduced the pore size from 2.2 ± 0.1 nm to ~1.8–0.2 nm. These changes corresponded to the formation of siloxane (Si-O-Si) bridges resulting from dehydroxylation. The characteristic pore radius of sintered particles was also confirmed by N2 adsorption measurements. These studies represent the use of non-invasive dynamic characterization methods such as X-ray scattering to elucidate thermally induced morphological evolution in architected siliceous materials.},
doi = {10.1016/j.colsurfa.2019.124260},
journal = {Colloids and Surfaces. A, Physicochemical and Engineering Aspects},
number = C,
volume = 586,
place = {United States},
year = {Sat Nov 23 00:00:00 EST 2019},
month = {Sat Nov 23 00:00:00 EST 2019}
}

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