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

Asgar, Hassnain; Semeykina, Viktoriya; Hunt, Mikaila; Mohammed, Sohaib; Kuzmenko, Ivan; Zharov, Ilya; Gadikota, Greeshma

doi:10.1016/j.colsurfa.2019.124260

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

Journal Article · Sat Nov 23 00:00:00 EST 2019 · Colloids and Surfaces. A, Physicochemical and Engineering Aspects

DOI:https://doi.org/10.1016/j.colsurfa.2019.124260· OSTI ID:1596100

^[1]; Semeykina, Viktoriya ^[2]; Hunt, Mikaila ^[2];

^[1]; Kuzmenko, Ivan ^[3]; Zharov, Ilya ^[2];

^[1]

Cornell Univ., Ithaca, NY (United States)
Univ. of Utah, Salt Lake City, UT (United States)
Argonne National Lab. (ANL), Argonne, IL (United States)

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.

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Research Organization:: 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 Organization:: USDOE Office of Science (SC), Basic Energy Sciences (BES)

Grant/Contract Number:: SC0019285; AC02-06CH11357

OSTI ID:: 1596100

Alternate ID(s):: OSTI ID: 1580177; OSTI ID: 1615468

Journal Information:: Colloids and Surfaces. A, Physicochemical and Engineering Aspects, Vol. 586, Issue C; ISSN 0927-7757

Publisher:: ElsevierCopyright Statement

Country of Publication:: United States

Language:: English

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Cited by: 7 works

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