Mesoporous Silica Formation Mechanisms Probed Using Combined Spin-Echo Modulated Small-Angle Neutron Scattering (SEMSANS) and Small-Angle Neutron Scattering (SANS)

Julien Schmitt; Jan Joost Zeeuw; Jan Joost Zeeuw; Jeroen Plomp; Wim G. Bouwman; Adam L. Washington; Robert M. Dalgliesh; Chris P. Duif; Michel A. Thijs; Fankang Li; Roger Pynn; Roger Pynn; Steven R. Parnell; Karen J. Edler

doi:10.1021/acsami.0c03287

Mesoporous Silica Formation Mechanisms Probed Using Combined Spin-Echo Modulated Small-Angle Neutron Scattering (SEMSANS) and Small-Angle Neutron Scattering (SANS)

Julien Schmitt, Jan Joost Zeeuw, Jan Joost Zeeuw, Jeroen Plomp, Wim G. Bouwman, Adam L. Washington, Robert M. Dalgliesh, Chris P. Duif, Michel A. Thijs, Fankang Li, Roger Pynn, Roger Pynn, Steven R. Parnell, Karen J. Edler

Neutron Optics & Polarization

Research output: Contribution to journal › Article › peer-review

19 Scopus citations

Abstract

The initial formation stages of surfactant-templated silica thin films which grow at the air-water interface were studied using combined spin-echo modulated small-angle neutron scattering (SEMSANS) and small-angle neutron scattering (SANS). The films are formed from either a cationic surfactant or nonionic surfactant (C16EO8) in a dilute acidic solution by the addition of tetramethoxysilane. Previous work has suggested a two stage formation mechanism with mesostructured particle formation in the bulk solution driving film formation at the solution surface. From the SEMSANS data, it is possible to pinpoint accurately the time associated with the formation of large particles in solution that go on to form the film and to show their emergence is concomitant with the appearance of Bragg peaks in the SANS pattern, associated with the two-dimensional hexagonal order. The combination of SANS and SEMSANS allows a complete depiction of the steps of the synthesis that occur in the subphase.

Original language	English
Pages (from-to)	28461-28473
Number of pages	13
Journal	ACS Applied Materials and Interfaces
Volume	12
Issue number	25
DOIs	https://doi.org/10.1021/acsami.0c03287
State	Published - Jun 24 2020

Funding

Experiments at the ISIS Pulsed Neutron and Muon Source were supported by a beamtime allocation for Larmor from the Science and Technology Facilities Council under proposal number RB1710181. Jan S. Pedersen is warmly thanked for designing the homemade Fortran software used to fit the SANS data. Part of this research was funded by a NWO groot (Grant LARMOR 721.012.102). F. Li would like to acknowledge the support from Oak Ridge National Laboratory, managed by UT-Battelle, LLC, for the U. S. Department of Energy. R. Pynn acknowledges partial support from the US Department of Commerce through cooperative agreement number 70NANB15H259. The authors warmly thank Ernst van der Wal for the design of the front cover associated to this article

Funders	Funder number
ISIS
U.S. Department of Energy
U.S. Department of Commerce	70NANB15H259
Oak Ridge National Laboratory
Science and Technology Facilities Council	RB1710181
Nederlandse Organisatie voor Wetenschappelijk Onderzoek	LARMOR 721.012.102

Keywords

kinetics
mesophase
mesoporous silica
micelles
particles
silica films
small-angle neutron scattering (SANS)
spin-echo modulated small-angle neutron scattering (SEMSANS)

Access to Document

10.1021/acsami.0c03287

Cite this

Schmitt, J., Zeeuw, J. J., Zeeuw, J. J., Plomp, J., Bouwman, W. G., Washington, A. L., Dalgliesh, R. M., Duif, C. P., Thijs, M. A., Li, F., Pynn, R., Pynn, R., Parnell, S. R., & Edler, K. J. (2020). Mesoporous Silica Formation Mechanisms Probed Using Combined Spin-Echo Modulated Small-Angle Neutron Scattering (SEMSANS) and Small-Angle Neutron Scattering (SANS). ACS Applied Materials and Interfaces, 12(25), 28461-28473. https://doi.org/10.1021/acsami.0c03287

@article{f177064e92624187b2ccdc52de6b4300,

title = "Mesoporous Silica Formation Mechanisms Probed Using Combined Spin-Echo Modulated Small-Angle Neutron Scattering (SEMSANS) and Small-Angle Neutron Scattering (SANS)",

abstract = "The initial formation stages of surfactant-templated silica thin films which grow at the air-water interface were studied using combined spin-echo modulated small-angle neutron scattering (SEMSANS) and small-angle neutron scattering (SANS). The films are formed from either a cationic surfactant or nonionic surfactant (C16EO8) in a dilute acidic solution by the addition of tetramethoxysilane. Previous work has suggested a two stage formation mechanism with mesostructured particle formation in the bulk solution driving film formation at the solution surface. From the SEMSANS data, it is possible to pinpoint accurately the time associated with the formation of large particles in solution that go on to form the film and to show their emergence is concomitant with the appearance of Bragg peaks in the SANS pattern, associated with the two-dimensional hexagonal order. The combination of SANS and SEMSANS allows a complete depiction of the steps of the synthesis that occur in the subphase.",

keywords = "kinetics, mesophase, mesoporous silica, micelles, particles, silica films, small-angle neutron scattering (SANS), spin-echo modulated small-angle neutron scattering (SEMSANS)",

author = "Julien Schmitt and Zeeuw, {Jan Joost} and Zeeuw, {Jan Joost} and Jeroen Plomp and Bouwman, {Wim G.} and Washington, {Adam L.} and Dalgliesh, {Robert M.} and Duif, {Chris P.} and Thijs, {Michel A.} and Fankang Li and Roger Pynn and Roger Pynn and Parnell, {Steven R.} and Edler, {Karen J.}",

note = "Publisher Copyright: {\textcopyright} 2020 American Chemical Society.",

year = "2020",

month = jun,

day = "24",

doi = "10.1021/acsami.0c03287",

language = "English",

volume = "12",

pages = "28461--28473",

journal = "ACS Applied Materials and Interfaces",

issn = "1944-8244",

publisher = "American Chemical Society",

number = "25",

}

Schmitt, J, Zeeuw, JJ, Zeeuw, JJ, Plomp, J, Bouwman, WG, Washington, AL, Dalgliesh, RM, Duif, CP, Thijs, MA, Li, F, Pynn, R, Pynn, R, Parnell, SR & Edler, KJ 2020, 'Mesoporous Silica Formation Mechanisms Probed Using Combined Spin-Echo Modulated Small-Angle Neutron Scattering (SEMSANS) and Small-Angle Neutron Scattering (SANS)', ACS Applied Materials and Interfaces, vol. 12, no. 25, pp. 28461-28473. https://doi.org/10.1021/acsami.0c03287

Mesoporous Silica Formation Mechanisms Probed Using Combined Spin-Echo Modulated Small-Angle Neutron Scattering (SEMSANS) and Small-Angle Neutron Scattering (SANS). / Schmitt, Julien; Zeeuw, Jan Joost; Zeeuw, Jan Joost et al.
In: ACS Applied Materials and Interfaces, Vol. 12, No. 25, 24.06.2020, p. 28461-28473.

Research output: Contribution to journal › Article › peer-review

TY - JOUR

T1 - Mesoporous Silica Formation Mechanisms Probed Using Combined Spin-Echo Modulated Small-Angle Neutron Scattering (SEMSANS) and Small-Angle Neutron Scattering (SANS)

AU - Schmitt, Julien

AU - Zeeuw, Jan Joost

AU - Plomp, Jeroen

AU - Bouwman, Wim G.

AU - Washington, Adam L.

AU - Dalgliesh, Robert M.

AU - Duif, Chris P.

AU - Thijs, Michel A.

AU - Li, Fankang

AU - Pynn, Roger

AU - Parnell, Steven R.

AU - Edler, Karen J.

PY - 2020/6/24

Y1 - 2020/6/24

N2 - The initial formation stages of surfactant-templated silica thin films which grow at the air-water interface were studied using combined spin-echo modulated small-angle neutron scattering (SEMSANS) and small-angle neutron scattering (SANS). The films are formed from either a cationic surfactant or nonionic surfactant (C16EO8) in a dilute acidic solution by the addition of tetramethoxysilane. Previous work has suggested a two stage formation mechanism with mesostructured particle formation in the bulk solution driving film formation at the solution surface. From the SEMSANS data, it is possible to pinpoint accurately the time associated with the formation of large particles in solution that go on to form the film and to show their emergence is concomitant with the appearance of Bragg peaks in the SANS pattern, associated with the two-dimensional hexagonal order. The combination of SANS and SEMSANS allows a complete depiction of the steps of the synthesis that occur in the subphase.

AB - The initial formation stages of surfactant-templated silica thin films which grow at the air-water interface were studied using combined spin-echo modulated small-angle neutron scattering (SEMSANS) and small-angle neutron scattering (SANS). The films are formed from either a cationic surfactant or nonionic surfactant (C16EO8) in a dilute acidic solution by the addition of tetramethoxysilane. Previous work has suggested a two stage formation mechanism with mesostructured particle formation in the bulk solution driving film formation at the solution surface. From the SEMSANS data, it is possible to pinpoint accurately the time associated with the formation of large particles in solution that go on to form the film and to show their emergence is concomitant with the appearance of Bragg peaks in the SANS pattern, associated with the two-dimensional hexagonal order. The combination of SANS and SEMSANS allows a complete depiction of the steps of the synthesis that occur in the subphase.

KW - kinetics

KW - mesophase

KW - mesoporous silica

KW - micelles

KW - particles

KW - silica films

KW - small-angle neutron scattering (SANS)

KW - spin-echo modulated small-angle neutron scattering (SEMSANS)

UR - http://www.scopus.com/inward/record.url?scp=85087110467&partnerID=8YFLogxK

U2 - 10.1021/acsami.0c03287

DO - 10.1021/acsami.0c03287

M3 - Article

C2 - 32330001

AN - SCOPUS:85087110467

SN - 1944-8244

VL - 12

SP - 28461

EP - 28473

JO - ACS Applied Materials and Interfaces

JF - ACS Applied Materials and Interfaces

IS - 25

ER -

Mesoporous Silica Formation Mechanisms Probed Using Combined Spin-Echo Modulated Small-Angle Neutron Scattering (SEMSANS) and Small-Angle Neutron Scattering (SANS)

Abstract

Funding

Keywords

Access to Document

Other files and links

Fingerprint

Cite this