Controlled synthesis of SPION@SiO2 nanoparticles using design of experiments

Clarissa L.G. Harman; Niamh Mac Fhionnlaoich; Aaron M. King; Joseph R.H. Manning; Wu Lin; Peter Scholes; Stefan Guldin; Gemma Louise Davies

doi:10.1039/d2ma00369d

Controlled synthesis of SPION@SiO₂ nanoparticles using design of experiments

Clarissa L.G. Harman, Niamh Mac Fhionnlaoich, Aaron M. King, Joseph R.H. Manning, Wu Lin, Peter Scholes, Stefan Guldin^*, Gemma Louise Davies^*

^*Corresponding author for this work

Chemistry

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

3 Citations (Scopus)

15 Downloads (Pure)

Abstract

The synthesis of single-core superparamagnetic iron oxide nanoparticles (SPIONs) coated with a silica shell of controlled thickness remains a challenge, due to the dependence on a multitude of experimental variables. Herein, we utilise design of experiment (DoE) to study the formation of SPION@SiO₂ nanoparticles (NPs) via reverse microemulsion. Using a 3³ full factorial design, the influence of reactant concentration of tetraethyl orthosilicate (TEOS) and ammonium hydroxide (NH₄OH), as well as the number of fractionated additions of TEOS on the silica shell was investigated with the aim of minimising polydispersity and increasing the population of SPION@SiO₂ NPs formed. This investigation facilitated a reproducible and controlled approach for the high yield synthesis of SPION@SiO₂ NPs with uniform silica shell thickness. Application of a multiple linear regression analysis established a relationship between the applied experimental variables and the resulting silica shell thickness. These experimental variables were similarly found to dictate the monodispersity of the SPION@SiO₂ NPs formed. The overall population of single-core@shell particles was dependent on the interaction between the number of moles of TEOS and NH₄OH, with no influence from the number of fractionated additions of TEOS. This work demonstrates the complexity of the preparative method and produces an accessible and flexible synthetic model to achieve monodisperse SPION@SiO₂ NPs with controllable shell thickness.

Original language	English
Pages (from-to)	6007-6018
Number of pages	12
Journal	Materials Advances
Volume	3
Issue number	14
Early online date	31 May 2022
DOIs	https://doi.org/10.1039/d2ma00369d
Publication status	Published - 21 Jul 2022

Bibliographical note

Funding Information:
The authors acknowledge financial support from the Engineering and Physical Sciences Research Council through the Centre for Doctoral Training in Advanced Therapeutics and Nanomedicines (EP/L01646X, supporting CLGH). For the purpose of open access, the authors have applied a Creative Commons Attribution (CC BY) licence to any Author Accepted Manuscript version arising. Thanks to Dr Steve York and Dr Yisong Han, at the University of Warwick's Research Technology Platform, for electron microscopy imaging.

Publisher Copyright:
© 2022 RSC.

ASJC Scopus subject areas

Chemistry (miscellaneous)
General Materials Science

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Cite this

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title = "Controlled synthesis of SPION@SiO2 nanoparticles using design of experiments",

abstract = "The synthesis of single-core superparamagnetic iron oxide nanoparticles (SPIONs) coated with a silica shell of controlled thickness remains a challenge, due to the dependence on a multitude of experimental variables. Herein, we utilise design of experiment (DoE) to study the formation of SPION@SiO2 nanoparticles (NPs) via reverse microemulsion. Using a 33 full factorial design, the influence of reactant concentration of tetraethyl orthosilicate (TEOS) and ammonium hydroxide (NH4OH), as well as the number of fractionated additions of TEOS on the silica shell was investigated with the aim of minimising polydispersity and increasing the population of SPION@SiO2 NPs formed. This investigation facilitated a reproducible and controlled approach for the high yield synthesis of SPION@SiO2 NPs with uniform silica shell thickness. Application of a multiple linear regression analysis established a relationship between the applied experimental variables and the resulting silica shell thickness. These experimental variables were similarly found to dictate the monodispersity of the SPION@SiO2 NPs formed. The overall population of single-core@shell particles was dependent on the interaction between the number of moles of TEOS and NH4OH, with no influence from the number of fractionated additions of TEOS. This work demonstrates the complexity of the preparative method and produces an accessible and flexible synthetic model to achieve monodisperse SPION@SiO2 NPs with controllable shell thickness.",

author = "Harman, {Clarissa L.G.} and {Mac Fhionnlaoich}, Niamh and King, {Aaron M.} and Manning, {Joseph R.H.} and Wu Lin and Peter Scholes and Stefan Guldin and Davies, {Gemma Louise}",

note = "Funding Information: The authors acknowledge financial support from the Engineering and Physical Sciences Research Council through the Centre for Doctoral Training in Advanced Therapeutics and Nanomedicines (EP/L01646X, supporting CLGH). For the purpose of open access, the authors have applied a Creative Commons Attribution (CC BY) licence to any Author Accepted Manuscript version arising. Thanks to Dr Steve York and Dr Yisong Han, at the University of Warwick's Research Technology Platform, for electron microscopy imaging. Publisher Copyright: {\textcopyright} 2022 RSC.",

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AU - Harman, Clarissa L.G.

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AU - King, Aaron M.

AU - Manning, Joseph R.H.

AU - Lin, Wu

AU - Scholes, Peter

AU - Guldin, Stefan

AU - Davies, Gemma Louise

N1 - Funding Information: The authors acknowledge financial support from the Engineering and Physical Sciences Research Council through the Centre for Doctoral Training in Advanced Therapeutics and Nanomedicines (EP/L01646X, supporting CLGH). For the purpose of open access, the authors have applied a Creative Commons Attribution (CC BY) licence to any Author Accepted Manuscript version arising. Thanks to Dr Steve York and Dr Yisong Han, at the University of Warwick's Research Technology Platform, for electron microscopy imaging. Publisher Copyright: © 2022 RSC.

PY - 2022/7/21

Y1 - 2022/7/21

N2 - The synthesis of single-core superparamagnetic iron oxide nanoparticles (SPIONs) coated with a silica shell of controlled thickness remains a challenge, due to the dependence on a multitude of experimental variables. Herein, we utilise design of experiment (DoE) to study the formation of SPION@SiO2 nanoparticles (NPs) via reverse microemulsion. Using a 33 full factorial design, the influence of reactant concentration of tetraethyl orthosilicate (TEOS) and ammonium hydroxide (NH4OH), as well as the number of fractionated additions of TEOS on the silica shell was investigated with the aim of minimising polydispersity and increasing the population of SPION@SiO2 NPs formed. This investigation facilitated a reproducible and controlled approach for the high yield synthesis of SPION@SiO2 NPs with uniform silica shell thickness. Application of a multiple linear regression analysis established a relationship between the applied experimental variables and the resulting silica shell thickness. These experimental variables were similarly found to dictate the monodispersity of the SPION@SiO2 NPs formed. The overall population of single-core@shell particles was dependent on the interaction between the number of moles of TEOS and NH4OH, with no influence from the number of fractionated additions of TEOS. This work demonstrates the complexity of the preparative method and produces an accessible and flexible synthetic model to achieve monodisperse SPION@SiO2 NPs with controllable shell thickness.

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