Porosity of silica Stöber particles determined by spin-echo small angle neutron scattering

S. R. Parnell; A. L. Washington; A. J. Parnell; A. Walsh; R. M. Dalgliesh; F. Li; W. A. Hamilton; S. Prevost; J. P.A. Fairclough; R. Pynn

doi:10.1039/c5sm02772a

Porosity of silica Stöber particles determined by spin-echo small angle neutron scattering

S. R. Parnell, A. L. Washington, A. J. Parnell, A. Walsh, R. M. Dalgliesh, F. Li, W. A. Hamilton, S. Prevost, J. P.A. Fairclough, R. Pynn

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37 Scopus citations

Abstract

Stöber silica particles are used in a diverse range of applications. Despite their widespread industrial and scientific uses, information on the internal structure of the particles is non-trivial to obtain and is not often reported. In this work we have used spin-echo small angle neutron scattering (SESANS) in conjunction with ultra small angle X-ray scattering (USAXS) and pycnometry to study an aqueous dispersion of Stöber particles. Our results are in agreement with models which propose that Stöber particles have a porous core, with a significant fraction of the pores inaccessible to solvent. For samples prepared from the same master sample in a range of H₂O-D₂O ratio solutions we were able to model the SESANS results for the solution series assuming monodisperse, smooth surfaced spheres of radius 83 nm with an internal open pore volume fraction of 32% and a closed pore fraction of 10%. Our results are consistent with USAXS measurements. The protocol developed and discussed here shows that the SESANS technique is a powerful way to investigate particles much larger than those studied using conventional small angle scattering methods.

Original language	English
Pages (from-to)	4709-4714
Number of pages	6
Journal	Soft Matter
Volume	12
Issue number	21
DOIs	https://doi.org/10.1039/c5sm02772a
State	Published - 2016
Externally published	Yes

Funding

Construction of LENS was supported by the National Science Foundation grants DMR-0220560 and DMR-0320627, the 21st Century Science and Technology fund of Indiana, Indiana University, and the Department of Defence. One of us, Steven Parnell acknowledges funding from Oak Ridge National Laboratory. We thank the ISIS facility (STFC) in the UK for the award of beam time.

Funders	Funder number
National Science Foundation	DMR-0220560, DMR-0320627
U.S. Department of Defense
Directorate for Mathematical and Physical Sciences	0320627, 0220560
Oak Ridge National Laboratory
Indiana University
Science and Technology Facilities Council

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title = "Porosity of silica St{\"o}ber particles determined by spin-echo small angle neutron scattering",

abstract = "St{\"o}ber silica particles are used in a diverse range of applications. Despite their widespread industrial and scientific uses, information on the internal structure of the particles is non-trivial to obtain and is not often reported. In this work we have used spin-echo small angle neutron scattering (SESANS) in conjunction with ultra small angle X-ray scattering (USAXS) and pycnometry to study an aqueous dispersion of St{\"o}ber particles. Our results are in agreement with models which propose that St{\"o}ber particles have a porous core, with a significant fraction of the pores inaccessible to solvent. For samples prepared from the same master sample in a range of H2O-D2O ratio solutions we were able to model the SESANS results for the solution series assuming monodisperse, smooth surfaced spheres of radius 83 nm with an internal open pore volume fraction of 32% and a closed pore fraction of 10%. Our results are consistent with USAXS measurements. The protocol developed and discussed here shows that the SESANS technique is a powerful way to investigate particles much larger than those studied using conventional small angle scattering methods.",

author = "Parnell, {S. R.} and Washington, {A. L.} and Parnell, {A. J.} and A. Walsh and Dalgliesh, {R. M.} and F. Li and Hamilton, {W. A.} and S. Prevost and Fairclough, {J. P.A.} and R. Pynn",

note = "Publisher Copyright: {\textcopyright} 2016 The Royal Society of Chemistry.",

year = "2016",

doi = "10.1039/c5sm02772a",

language = "English",

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T1 - Porosity of silica Stöber particles determined by spin-echo small angle neutron scattering

AU - Parnell, S. R.

AU - Washington, A. L.

AU - Parnell, A. J.

AU - Walsh, A.

AU - Dalgliesh, R. M.

AU - Li, F.

AU - Hamilton, W. A.

AU - Prevost, S.

AU - Fairclough, J. P.A.

AU - Pynn, R.

PY - 2016

Y1 - 2016

N2 - Stöber silica particles are used in a diverse range of applications. Despite their widespread industrial and scientific uses, information on the internal structure of the particles is non-trivial to obtain and is not often reported. In this work we have used spin-echo small angle neutron scattering (SESANS) in conjunction with ultra small angle X-ray scattering (USAXS) and pycnometry to study an aqueous dispersion of Stöber particles. Our results are in agreement with models which propose that Stöber particles have a porous core, with a significant fraction of the pores inaccessible to solvent. For samples prepared from the same master sample in a range of H2O-D2O ratio solutions we were able to model the SESANS results for the solution series assuming monodisperse, smooth surfaced spheres of radius 83 nm with an internal open pore volume fraction of 32% and a closed pore fraction of 10%. Our results are consistent with USAXS measurements. The protocol developed and discussed here shows that the SESANS technique is a powerful way to investigate particles much larger than those studied using conventional small angle scattering methods.

AB - Stöber silica particles are used in a diverse range of applications. Despite their widespread industrial and scientific uses, information on the internal structure of the particles is non-trivial to obtain and is not often reported. In this work we have used spin-echo small angle neutron scattering (SESANS) in conjunction with ultra small angle X-ray scattering (USAXS) and pycnometry to study an aqueous dispersion of Stöber particles. Our results are in agreement with models which propose that Stöber particles have a porous core, with a significant fraction of the pores inaccessible to solvent. For samples prepared from the same master sample in a range of H2O-D2O ratio solutions we were able to model the SESANS results for the solution series assuming monodisperse, smooth surfaced spheres of radius 83 nm with an internal open pore volume fraction of 32% and a closed pore fraction of 10%. Our results are consistent with USAXS measurements. The protocol developed and discussed here shows that the SESANS technique is a powerful way to investigate particles much larger than those studied using conventional small angle scattering methods.

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JO - Soft Matter

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ER -

Porosity of silica Stöber particles determined by spin-echo small angle neutron scattering

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