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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 Lab. (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. https://doi.org/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 = {2019},
month = {11}
}

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Works referenced in this record:

Tuneable graphene nanopores for single biomolecule detection
journal, January 2016

  • Al-Dirini, Feras; Mohammed, Mahmood A.; Hossain, Md Sharafat
  • Nanoscale, Vol. 8, Issue 19
  • DOI: 10.1039/C5NR05274B

Controlling particle size in the Stöber process and incorporation of calcium
journal, May 2016

  • Greasley, Sarah L.; Page, Samuel J.; Sirovica, Slobodan
  • Journal of Colloid and Interface Science, Vol. 469
  • DOI: 10.1016/j.jcis.2016.01.065

Porous Carbon Nanotube Membranes for Separation of H 2 /CH 4 and CO 2 /CH 4 Mixtures
journal, December 2012

  • Bucior, Benjamin J.; Chen, De-Li; Liu, Jinchen
  • The Journal of Physical Chemistry C, Vol. 116, Issue 49
  • DOI: 10.1021/jp3098022

A critical review of water uptake by shales
journal, August 2016


A review on capillary condensation in nanoporous media: Implications for hydrocarbon recovery from tight reservoirs
journal, November 2016


A review of phase behavior simulation of hydrocarbons in confined space: Implications for shale oil and shale gas
journal, August 2019


Critical Knowledge Gaps in Mass Transport through Single-Digit Nanopores: A Review and Perspective
journal, May 2019

  • Faucher, Samuel; Aluru, Narayana; Bazant, Martin Z.
  • The Journal of Physical Chemistry C, Vol. 123, Issue 35
  • DOI: 10.1021/acs.jpcc.9b02178

Water transport control in carbon nanotube arrays
journal, January 2014

  • Fasano, Matteo; Chiavazzo, Eliodoro; Asinari, Pietro
  • Nanoscale Research Letters, Vol. 9, Issue 1
  • DOI: 10.1186/1556-276X-9-559

An Experimental Study on the Influence of Sub-Core Scale Heterogeneities on CO2 Distribution in Reservoir Rocks
journal, June 2009


Chemical reaction kinetics leading to the first Stober silica nanoparticles – NMR and SAXS investigation
journal, January 2003


Structurally bound water and surface characterization of amorphous silica
journal, January 1989


Accurate Amorphous Silica Surface Models from First-Principles Thermodynamics of Surface Dehydroxylation
journal, April 2014

  • Ewing, Christopher S.; Bhavsar, Saurabh; Veser, Götz
  • Langmuir, Vol. 30, Issue 18
  • DOI: 10.1021/la500422p

Synthesis and characterization of spherical silica nanoparticles by modified Stöber process assisted by organic ligand
journal, September 2013

  • Gholami, Tahereh; Salavati-Niasari, Masoud; Bazarganipour, Mehdi
  • Superlattices and Microstructures, Vol. 61
  • DOI: 10.1016/j.spmi.2013.06.004

Hybrid silica bearing different organosilanes produced by the modified Stöber method
journal, November 2016


Tailless X‐Ray Single‐Crystal Reflection Curves Obtained by Multiple Reflection
journal, November 1965

  • Bonse, U.; Hart, M.
  • Applied Physics Letters, Vol. 7, Issue 9
  • DOI: 10.1063/1.1754396

Capillary trapping for geologic carbon dioxide storage – From pore scale physics to field scale implications
journal, September 2015

  • Krevor, Samuel; Blunt, Martin J.; Benson, Sally M.
  • International Journal of Greenhouse Gas Control, Vol. 40
  • DOI: 10.1016/j.ijggc.2015.04.006

Applying Mesoporous Silica SBA-15 in Electrochemical Detection of DNA Hybridization
journal, April 2016

  • Josypčuk, Oksana; Fojta, Miroslav; Daňhel, Aleš
  • Electroanalysis, Vol. 28, Issue 8
  • DOI: 10.1002/elan.201501137

Polydispersity during the Formation and Growth of the Stöber Silica Particles from Small-Angle X-Ray Scattering Measurements
journal, September 2000

  • Boukari, Hacène; Long, G. G.; Harris, M. T.
  • Journal of Colloid and Interface Science, Vol. 229, Issue 1
  • DOI: 10.1006/jcis.2000.7007

Small molecule electro-optical binding assay using nanopores
journal, April 2019

  • Cai, Shenglin; Sze, Jasmine Y. Y.; Ivanov, Aleksandar P.
  • Nature Communications, Vol. 10, Issue 1
  • DOI: 10.1038/s41467-019-09476-4

Fluid structure and transport properties of water inside carbon nanotubes
journal, December 2005

  • Liu, Yingchun; Wang, Qi; Wu, Tao
  • The Journal of Chemical Physics, Vol. 123, Issue 23
  • DOI: 10.1063/1.2131070

Revising the synthesis of Stöber silica nanoparticles: A multivariate assessment study on the effects of reaction parameters on the particle size
journal, September 2019

  • Fernandes, Rafael S.; Raimundo, Ivo M.; Pimentel, M. Fernanda
  • Colloids and Surfaces A: Physicochemical and Engineering Aspects, Vol. 577
  • DOI: 10.1016/j.colsurfa.2019.05.053

Ultra-small-angle X-ray scattering at the Advanced Photon Source
journal, April 2009

  • Ilavsky, Jan; Jemian, Pete R.; Allen, Andrew J.
  • Journal of Applied Crystallography, Vol. 42, Issue 3
  • DOI: 10.1107/S0021889809008802

Irena : tool suite for modeling and analysis of small-angle scattering
journal, February 2009


Asphaltene-Derived Activated Carbon and Carbon Nanotube Membranes for CO 2 Separation
journal, October 2018


Synthesis of nanometric silica particles via a modified Stöber synthesis route
journal, February 2018

  • Meier, Manuel; Ungerer, Julian; Klinge, Mira
  • Colloids and Surfaces A: Physicochemical and Engineering Aspects, Vol. 538
  • DOI: 10.1016/j.colsurfa.2017.11.047

Preparation of monodisperse silica particles: Control of size and mass fraction
journal, August 1988

  • Bogush, G. H.; Tracy, M. A.; Zukoski, C. F.
  • Journal of Non-Crystalline Solids, Vol. 104, Issue 1, p. 95-106
  • DOI: 10.1016/0022-3093(88)90187-1

Bubble Point Measurements of Hydrocarbon Mixtures in Mesoporous Media
journal, February 2017


Molecular dynamics simulation of oil detachment from calcite surface in aqueous surfactant solution
journal, September 2016


Confinement Effects on Carbon Dioxide Methanation: A Novel Mechanism for Abiotic Methane Formation
journal, August 2017


Experimental and Molecular Modeling Study of Bubble Points of Hydrocarbon Mixtures in Nanoporous Media
journal, February 2017


Spark plasma sintering of silica glass: experimental study on the temperature distribution and the influence of the heating rate on bubble formation
journal, June 2016

  • Barazani, Bruno; Torikai, Delson
  • Glass Technology: European Journal of Glass Science and Technology Part A, Vol. 57, Issue 3
  • DOI: 10.13036/17533546.57.3.022

Confinement-induced modulation of elastic properties of nano-confined fluids in slit pore
journal, March 2019


Unraveling the Mystery of Stöber Silica’s Microporosity
journal, August 2016


Applications of an amorphous silicon-based area detector for high-resolution, high-sensitivity and fast time-resolved pair distribution function measurements
journal, May 2007

  • Chupas, Peter J.; Chapman, Karena W.; Lee, Peter L.
  • Journal of Applied Crystallography, Vol. 40, Issue 3
  • DOI: 10.1107/S0021889807007856

Process Modeling of CO 2 Injection into Natural Gas Reservoirs for Carbon Sequestration and Enhanced Gas Recovery
journal, March 2001

  • Oldenburg, C. M.; Pruess, K.; Benson, S. M.
  • Energy & Fuels, Vol. 15, Issue 2
  • DOI: 10.1021/ef000247h

Phase behavior and flow in shale nanopores from molecular simulations
journal, December 2016


Influence of reaction conditions on sol-precipitation process producing silicon oxide particles
journal, January 2002


Janus Polymer/Carbon Nanotube Hybrid Membranes for Oil/Water Separation
journal, September 2014

  • Gu, Jincui; Xiao, Peng; Chen, Jing
  • ACS Applied Materials & Interfaces, Vol. 6, Issue 18
  • DOI: 10.1021/am504326m

Nika : software for two-dimensional data reduction
journal, March 2012


Study of short range structure of amorphous Silica from PDF using Ag radiation in laboratory XRD system, RAMAN and NEXAFS
journal, May 2018


A review of reverse osmosis membrane materials for desalination—Development to date and future potential
journal, March 2011


Single step synthesis of 5–30nm monodisperse silica nanoparticles: Important experimental parameters and modeling
journal, January 2012

  • Fouilloux, Sarah; Daillant, Jean; Thill, Antoine
  • Colloids and Surfaces A: Physicochemical and Engineering Aspects, Vol. 393
  • DOI: 10.1016/j.colsurfa.2011.11.009

Preparation of spherical silica particles by St?ber process with high concentration of tetra-ethyl-orthosilicate
journal, January 2010

  • Wang, Xiao-Dong; Shen, Zheng-Xiang; Sang, Tian
  • Journal of Colloid and Interface Science, Vol. 341, Issue 1
  • DOI: 10.1016/j.jcis.2009.09.018

Investigation of nanopore confinement on fluid flow in tight reservoirs
journal, February 2017


Residual trapping of carbon dioxide during geological storage—Insight gained through a pore-network modeling approach
journal, July 2018


Surface-Modified Silica Colloidal Crystals: Nanoporous Films and Membranes with Controlled Ionic and Molecular Transport
journal, December 2013

  • Zharov, Ilya; Khabibullin, Amir
  • Accounts of Chemical Research, Vol. 47, Issue 2
  • DOI: 10.1021/ar400157w

Small-Angle Scattering from Polymeric Mass Fractals of Arbitrary Mass-Fractal Dimension
journal, April 1996


Autogenic analyte translocation in nanopores
journal, June 2019


Microtomography and Pore-Scale Modeling of Two-Phase Fluid Distribution
journal, August 2010

  • Silin, Dmitriy; Tomutsa, Liviu; Benson, Sally M.
  • Transport in Porous Media, Vol. 86, Issue 2
  • DOI: 10.1007/s11242-010-9636-2

Size control of monodisperse nonporous silica particles by seed particle growth
journal, June 2011


Smart Control of Monodisperse Stöber Silica Particles:  Effect of Reactant Addition Rate on Growth Process
journal, February 2005

  • Nozawa, K.; Gailhanou, H.; Raison, L.
  • Langmuir, Vol. 21, Issue 4
  • DOI: 10.1021/la048569r

Simulation of chemical reaction equilibria and kinetics in heterogeneous carbon micropores
journal, August 2002


Development of combined microstructure and structure characterization facility for in situ and operando studies at the Advanced Photon Source
journal, June 2018

  • Ilavsky, Jan; Zhang, Fan; Andrews, Ross N.
  • Journal of Applied Crystallography, Vol. 51, Issue 3
  • DOI: 10.1107/S160057671800643X

Pore-scale Considerations on Ostwald Ripening in Rocks
journal, July 2017


Tailoring the size and microporosity of Stöber silica particles
journal, March 2018


Transport Properties and Distribution of Water Molecules Confined in Hydrophobic Nanopores and Nanoslits
journal, August 2004

  • Liu, Yingchun; Wang, Qi; Lu, Linghong
  • Langmuir, Vol. 20, Issue 16
  • DOI: 10.1021/la036325l

Chemo-morphological coupling during serpentine heat treatment for carbon mineralization
journal, September 2018


A new method for in situ structural investigations of nano-sized amorphous and crystalline materials using mixed-flow reactors
journal, August 2019

  • Hoeher, Alexandria; Mergelsberg, Sebastian; Borkiewicz, Olaf J.
  • Acta Crystallographica Section A Foundations and Advances, Vol. 75, Issue 5
  • DOI: 10.1107/S2053273319008623

Current understanding of shale wettability: A review on contact angle measurements
journal, June 2018


Local electrical potential detection of DNA by nanowire–nanopore sensors
journal, December 2011


Approximations Leading to a Unified Exponential/Power-Law Approach to Small-Angle Scattering
journal, December 1995


The surface chemistry of amorphous silica. Zhuravlev model
journal, November 2000


Capillary filling of confined water in nanopores: Coupling the increased viscosity and slippage
journal, August 2018


Free-Standing Silica Colloidal Nanoporous Membranes
journal, March 2009

  • Bohaty, Andrew K.; Smith, Joanna J.; Zharov, Ilya
  • Langmuir, Vol. 25, Issue 5
  • DOI: 10.1021/la801922a

Ordered porous materials for emerging applications
journal, June 2002


Silver behenate and silver stearate powders for calibration of SAS instruments
journal, March 2012


Nanofiltration membranes review: Recent advances and future prospects
journal, January 2015


Molecular dynamics investigation of substrate wettability alteration and oil transport in a calcite nanopore
journal, March 2019


Small Angle X-ray Scattering for Nanoparticle Research
journal, April 2016


Ultra-Small-Angle X-ray Scattering Instrument at the Advanced Photon Source: History, Recent Development, and Current Status
journal, October 2012

  • Ilavsky, J.; Zhang, F.; Allen, A. J.
  • Metallurgical and Materials Transactions A, Vol. 44, Issue 1
  • DOI: 10.1007/s11661-012-1431-y

Silica, carbon and boron nitride monoliths with hierarchical porosity prepared by spark plasma sintering process
journal, April 2008


SAXS exploration of the synthesis of ultra monodisperse silica nanoparticles and quantitative nucleation growth modeling
journal, June 2010

  • Fouilloux, Sarah; Désert, Anthony; Taché, Olivier
  • Journal of Colloid and Interface Science, Vol. 346, Issue 1
  • DOI: 10.1016/j.jcis.2010.02.052

Relative permeability and trapping of CO 2 and water in sandstone rocks at reservoir conditions : MULTIPHASE FLOW OF CO
journal, February 2012

  • Krevor, Samuel C. M.; Pini, Ronny; Zuo, Lin
  • Water Resources Research, Vol. 48, Issue 2
  • DOI: 10.1029/2011WR010859

Surface characterization of amorphous silica—a review of work from the former USSR
journal, July 1993


Thermodynamics, structure, and dynamics of water confined between hydrophobic plates
journal, November 2005


Sol–Gel Synthesis and Characterization of Microporous Silica Membranes I: SAXS Study on the Growth of Polymeric Structures
journal, March 1996

  • Nair, Balagopal N.; Elferink, Wilma J.; Keizer, Klaas
  • Journal of Colloid and Interface Science, Vol. 178, Issue 2
  • DOI: 10.1006/jcis.1996.0152

Preparation of Dense and Porous Silicon Oxycarbide Submicrometer-Sized Spheres Using a Modified Stöber Process
journal, July 2011


Synthesis and characterization of spherical silica nanoparticles by modified Stöber process assisted by slow-hydrolysis catalyst
journal, January 2018


Understanding Stöber Silica’s Pore Characteristics Measured by Gas Adsorption
journal, January 2015

  • Li, Shanshan; Wan, Quan; Qin, Zonghua
  • Langmuir, Vol. 31, Issue 2
  • DOI: 10.1021/la5042103

Effect of confinement on chemical reaction equilibria: The reactions 2NO⇔(NO)2 and N2+3H2⇔2NH3 in carbon micropores
journal, January 2001

  • Turner, C. Heath; Johnson, J. Karl; Gubbins, Keith E.
  • The Journal of Chemical Physics, Vol. 114, Issue 4
  • DOI: 10.1063/1.1328756

Enhanced charge transport in nano-confined ionic liquids
journal, January 2012

  • Iacob, C.; Sangoro, J. R.; Kipnusu, W. K.
  • Soft Matter, Vol. 8, Issue 2
  • DOI: 10.1039/C1SM06581E

Analysis of textural properties of CaO-based CO2 sorbents by ex situ USAXS
journal, January 2019


Experimental investigation of confinement effect on phase behavior of hexane, heptane and octane using lab-on-a-chip technology
journal, September 2016


Recent Advances in Polymeric Solvent-Resistant Nanofiltration Membranes
journal, July 2014

  • Cheng, Xi Quan; Zhang, Yong Ling; Wang, Zhen Xing
  • Advances in Polymer Technology, Vol. 33, Issue S1
  • DOI: 10.1002/adv.21455

Size, volume fraction, and nucleation of Stober silica nanoparticles
journal, October 2003


Reactive geochemical transport simulation to study mineral trapping for CO 2 disposal in deep arenaceous formations : TRANSPORT SIMULATION FOR CO
journal, February 2003

  • Xu, Tianfu; Apps, John A.; Pruess, Karsten
  • Journal of Geophysical Research: Solid Earth, Vol. 108, Issue B2
  • DOI: 10.1029/2002JB001979

Carbon Dioxide Capture and Storage: An Overview With Emphasis on Capture and Storage in Deep Geological Formations
journal, October 2006


Measurements of hydrocarbon bubble points in synthesized mesoporous siliceous monoliths
journal, February 2018


A Novel Highly Sensitive Humidity Sensor Based on ZnO/SBA-15 Hybrid Nanocomposite
journal, August 2015

  • Tomer, Vijay K.; Duhan, Surender; Malik, Ritu
  • Journal of the American Ceramic Society, Vol. 98, Issue 12
  • DOI: 10.1111/jace.13836