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Quantification of initial steps of nucleation and growth of silica nanoparticles: An in-situ SAXS and DLS study

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Title: Quantification of initial steps of nucleation and growth of silica nanoparticles: An in-situ SAXS and DLS study
Authors: Tobler, Dominique J.1 tobler@see.leeds.ac.uk, Shaw, Sam1, Benning, Liane G.1
Source: Geochimica et Cosmochimica Acta. Sep2009, Vol. 73 Issue 18, p5377-5393. 17p.
Subjects: Nucleation, Silica, Nanoparticles, Quantitative chemical analysis, Polymerization, pH effect, Chemical kinetics, Light scattering, Small-angle X-ray scattering
Abstract: Abstract: The initial steps of silica polymerization and silica nanoparticle formation have been studied in-situ and in real-time. The experiments were carried out in near neutral pH (7–8) solutions with initial silica concentrations of 640 and 1600ppm ([SiO2]) and ionic strengths (IS) of 0.02, 0.05, 0.11 and 0.22M. The polymerization reactions were induced by neutralizing a high pH silica solution (from pH 12 to 7) and monitored by the time-dependent depletion in monosilicic acid concentration over time. The accompanied nucleation and growth of silica nanoparticles (i.e., change in particle size over time) was followed in-situ using time-resolved synchrotron-based Small Angle X-ray Scattering (SAXS) and conventional Dynamic Light Scattering (DLS) combined with scanning and (cryo)-transmission electron microscopy (SEM/cryo-TEM). The critical nucleus diameter was quantified (1.4–2nm) and results from SAXS and DLS showed that over 3h the particle diameter increased to a final size of ∼8nm. SEM and TEM photomicrographs verified the SAXS and DLS data and confirmed the spherical and hydrous structure of the forming silica nanoparticles. Furthermore, fractal analysis (i.e., fractal dimension, D m ∼2.2) indicated that the formed particles consisted of open, polymeric, low-density structures. For the nucleation and growth of silica nanoparticles a 3-stage growth process is proposed: (1) homogeneous and instantaneous nucleation of silica nanoparticles, (2) 3-D, surface-controlled particle growth following 1st order reaction kinetics and (3) Ostwald ripening and particle aggregation. [Copyright &y& Elsevier]
Copyright of Geochimica et Cosmochimica Acta is the property of Pergamon Press - An Imprint of Elsevier Science and its content may not be copied or emailed to multiple sites without the copyright holder's express written permission. Additionally, content may not be used with any artificial intelligence tools or machine learning technologies. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract. (Copyright applies to all Abstracts.)
Database: Engineering Source
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Header DbId: egs
DbLabel: Engineering Source
An: 43618456
AccessLevel: 6
PubType: Academic Journal
PubTypeId: academicJournal
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  Data: Quantification of initial steps of nucleation and growth of silica nanoparticles: An in-situ SAXS and DLS study
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  Data: <searchLink fieldCode="AR" term="%22Tobler%2C+Dominique+J%2E%22">Tobler, Dominique J.</searchLink><relatesTo>1</relatesTo><i> tobler@see.leeds.ac.uk</i><br /><searchLink fieldCode="AR" term="%22Shaw%2C+Sam%22">Shaw, Sam</searchLink><relatesTo>1</relatesTo><br /><searchLink fieldCode="AR" term="%22Benning%2C+Liane+G%2E%22">Benning, Liane G.</searchLink><relatesTo>1</relatesTo>
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  Data: <searchLink fieldCode="JN" term="%22Geochimica+et+Cosmochimica+Acta%22">Geochimica et Cosmochimica Acta</searchLink>. Sep2009, Vol. 73 Issue 18, p5377-5393. 17p.
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  Data: <searchLink fieldCode="DE" term="%22Nucleation%22">Nucleation</searchLink><br /><searchLink fieldCode="DE" term="%22Silica%22">Silica</searchLink><br /><searchLink fieldCode="DE" term="%22Nanoparticles%22">Nanoparticles</searchLink><br /><searchLink fieldCode="DE" term="%22Quantitative+chemical+analysis%22">Quantitative chemical analysis</searchLink><br /><searchLink fieldCode="DE" term="%22Polymerization%22">Polymerization</searchLink><br /><searchLink fieldCode="DE" term="%22pH+effect%22">pH effect</searchLink><br /><searchLink fieldCode="DE" term="%22Chemical+kinetics%22">Chemical kinetics</searchLink><br /><searchLink fieldCode="DE" term="%22Light+scattering%22">Light scattering</searchLink><br /><searchLink fieldCode="DE" term="%22Small-angle+X-ray+scattering%22">Small-angle X-ray scattering</searchLink>
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  Label: Abstract
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  Data: Abstract: The initial steps of silica polymerization and silica nanoparticle formation have been studied in-situ and in real-time. The experiments were carried out in near neutral pH (7–8) solutions with initial silica concentrations of 640 and 1600ppm ([SiO2]) and ionic strengths (IS) of 0.02, 0.05, 0.11 and 0.22M. The polymerization reactions were induced by neutralizing a high pH silica solution (from pH 12 to 7) and monitored by the time-dependent depletion in monosilicic acid concentration over time. The accompanied nucleation and growth of silica nanoparticles (i.e., change in particle size over time) was followed in-situ using time-resolved synchrotron-based Small Angle X-ray Scattering (SAXS) and conventional Dynamic Light Scattering (DLS) combined with scanning and (cryo)-transmission electron microscopy (SEM/cryo-TEM). The critical nucleus diameter was quantified (1.4–2nm) and results from SAXS and DLS showed that over 3h the particle diameter increased to a final size of ∼8nm. SEM and TEM photomicrographs verified the SAXS and DLS data and confirmed the spherical and hydrous structure of the forming silica nanoparticles. Furthermore, fractal analysis (i.e., fractal dimension, D m ∼2.2) indicated that the formed particles consisted of open, polymeric, low-density structures. For the nucleation and growth of silica nanoparticles a 3-stage growth process is proposed: (1) homogeneous and instantaneous nucleation of silica nanoparticles, (2) 3-D, surface-controlled particle growth following 1st order reaction kinetics and (3) Ostwald ripening and particle aggregation. [Copyright &y& Elsevier]
– Name: AbstractSuppliedCopyright
  Label:
  Group: Ab
  Data: <i>Copyright of Geochimica et Cosmochimica Acta is the property of Pergamon Press - An Imprint of Elsevier Science and its content may not be copied or emailed to multiple sites without the copyright holder's express written permission. Additionally, content may not be used with any artificial intelligence tools or machine learning technologies. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract.</i> (Copyright applies to all Abstracts.)
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        Value: 10.1016/j.gca.2009.06.002
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        Text: English
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      – SubjectFull: Nucleation
        Type: general
      – SubjectFull: Silica
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      – SubjectFull: Nanoparticles
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      – SubjectFull: Quantitative chemical analysis
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      – SubjectFull: Polymerization
        Type: general
      – SubjectFull: pH effect
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      – SubjectFull: Chemical kinetics
        Type: general
      – SubjectFull: Light scattering
        Type: general
      – SubjectFull: Small-angle X-ray scattering
        Type: general
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      – TitleFull: Quantification of initial steps of nucleation and growth of silica nanoparticles: An in-situ SAXS and DLS study
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            NameFull: Tobler, Dominique J.
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            NameFull: Shaw, Sam
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            NameFull: Benning, Liane G.
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              M: 09
              Text: Sep2009
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