In Situ Sol–Gel Synthesis of Unique Silica Structures Using Airborne Assembly: Implications for In-Air Reactive Manufacturing

Connor R. Barker; Francesca Lewns; Gowsihan Poologasundarampillai; Andrew D. Ward

doi:10.1021/acsanm.2c02683

In Situ Sol–Gel Synthesis of Unique Silica Structures Using Airborne Assembly: Implications for In-Air Reactive Manufacturing

Connor R. Barker, Francesca Lewns, Gowsihan Poologasundarampillai^*, Andrew D. Ward^*

^*Corresponding author for this work

Dentistry

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

12 Downloads (Pure)

Abstract

Optical trapping enables the real-time manipulation and observation of morphological evolution of individual particles during reaction chemistry. Here, optical trapping was used in combination with Raman spectroscopy to conduct airborne assembly and kinetic experiments. Micro-droplets of alkoxysilane were levitated in air prior to undergoing either acid- or base-catalyzed sol–gel reaction chemistry to form silica particles. The evolution of the reaction was monitored in real-time; Raman and Mie spectroscopies confirmed the in situ formation of silica particles from alkoxysilane droplets as the product of successive hydrolysis and condensation reactions, with faster reaction kinetics in acid catalysis. Hydrolysis and condensation were accompanied by a reduction in droplet volume and silica formation. Two airborne particles undergoing solidification could be assembled into unique 3D structures such as dumb-bell shapes by manipulating a controlled collision. Our results provide a pipeline combining spectroscopy with optical microscopy and nanoscale FIB–SEM imaging to enable chemical and structural insights, with the opportunity to apply this methodology to probe structure formation during reactive inkjet printing.

Original language	English
Pages (from-to)	11699–11706
Number of pages	8
Journal	ACS Applied Nano Materials
Volume	5
Issue number	8
Early online date	17 Aug 2022
DOIs	https://doi.org/10.1021/acsanm.2c02683
Publication status	Published - 26 Aug 2022

Bibliographical note

Acknowledgments:
This study was made possible thanks to funding from the Medical Research Council (grant number MR/N013913/1), the Engineering and Physical Sciences Research Council (grant number EP/M023877/1), and the Science and Technology Facilities Council─Central Laser Facility─for access to equipment funded under app. no.: 16130023. We would like to thank Royal Holloway, University of London, and STFC for funding Connor Barker’s PhD studies. We would like to thank Dr Ali Gholinia for his help with performing the FIB–SEM imaging and Professor Yasuaki Tokudome for his informative comments and suggestions on the discussion. Raw data requests to the authors for analysis are encouraged.

Access to Document

10.1021/acsanm.2c02683Licence: Creative Commons: Attribution (CC BY)

BarkerC2022InsituFinal published version, 5.51 MBLicence: Creative Commons: Attribution (CC BY)

https://pubs.acs.org/doi/full/10.1021/acsanm.2c02683Licence: Creative Commons: Attribution (CC BY)

Cite this

@article{1a8b7625d86a49048e8e572560df503f,

title = "In Situ Sol–Gel Synthesis of Unique Silica Structures Using Airborne Assembly: Implications for In-Air Reactive Manufacturing",

abstract = "Optical trapping enables the real-time manipulation and observation of morphological evolution of individual particles during reaction chemistry. Here, optical trapping was used in combination with Raman spectroscopy to conduct airborne assembly and kinetic experiments. Micro-droplets of alkoxysilane were levitated in air prior to undergoing either acid- or base-catalyzed sol–gel reaction chemistry to form silica particles. The evolution of the reaction was monitored in real-time; Raman and Mie spectroscopies confirmed the in situ formation of silica particles from alkoxysilane droplets as the product of successive hydrolysis and condensation reactions, with faster reaction kinetics in acid catalysis. Hydrolysis and condensation were accompanied by a reduction in droplet volume and silica formation. Two airborne particles undergoing solidification could be assembled into unique 3D structures such as dumb-bell shapes by manipulating a controlled collision. Our results provide a pipeline combining spectroscopy with optical microscopy and nanoscale FIB–SEM imaging to enable chemical and structural insights, with the opportunity to apply this methodology to probe structure formation during reactive inkjet printing.",

author = "Barker, {Connor R.} and Francesca Lewns and Gowsihan Poologasundarampillai and Ward, {Andrew D.}",

note = "Acknowledgments: This study was made possible thanks to funding from the Medical Research Council (grant number MR/N013913/1), the Engineering and Physical Sciences Research Council (grant number EP/M023877/1), and the Science and Technology Facilities Council─Central Laser Facility─for access to equipment funded under app. no.: 16130023. We would like to thank Royal Holloway, University of London, and STFC for funding Connor Barker{\textquoteright}s PhD studies. We would like to thank Dr Ali Gholinia for his help with performing the FIB–SEM imaging and Professor Yasuaki Tokudome for his informative comments and suggestions on the discussion. Raw data requests to the authors for analysis are encouraged.",

year = "2022",

month = aug,

day = "26",

doi = "10.1021/acsanm.2c02683",

language = "English",

volume = "5",

pages = "11699–11706",

journal = "ACS Applied Nano Materials",

number = "8",

}

TY - JOUR

T1 - In Situ Sol–Gel Synthesis of Unique Silica Structures Using Airborne Assembly

T2 - Implications for In-Air Reactive Manufacturing

AU - Barker, Connor R.

AU - Lewns, Francesca

AU - Poologasundarampillai, Gowsihan

AU - Ward, Andrew D.

N1 - Acknowledgments: This study was made possible thanks to funding from the Medical Research Council (grant number MR/N013913/1), the Engineering and Physical Sciences Research Council (grant number EP/M023877/1), and the Science and Technology Facilities Council─Central Laser Facility─for access to equipment funded under app. no.: 16130023. We would like to thank Royal Holloway, University of London, and STFC for funding Connor Barker’s PhD studies. We would like to thank Dr Ali Gholinia for his help with performing the FIB–SEM imaging and Professor Yasuaki Tokudome for his informative comments and suggestions on the discussion. Raw data requests to the authors for analysis are encouraged.

PY - 2022/8/26

Y1 - 2022/8/26

N2 - Optical trapping enables the real-time manipulation and observation of morphological evolution of individual particles during reaction chemistry. Here, optical trapping was used in combination with Raman spectroscopy to conduct airborne assembly and kinetic experiments. Micro-droplets of alkoxysilane were levitated in air prior to undergoing either acid- or base-catalyzed sol–gel reaction chemistry to form silica particles. The evolution of the reaction was monitored in real-time; Raman and Mie spectroscopies confirmed the in situ formation of silica particles from alkoxysilane droplets as the product of successive hydrolysis and condensation reactions, with faster reaction kinetics in acid catalysis. Hydrolysis and condensation were accompanied by a reduction in droplet volume and silica formation. Two airborne particles undergoing solidification could be assembled into unique 3D structures such as dumb-bell shapes by manipulating a controlled collision. Our results provide a pipeline combining spectroscopy with optical microscopy and nanoscale FIB–SEM imaging to enable chemical and structural insights, with the opportunity to apply this methodology to probe structure formation during reactive inkjet printing.

AB - Optical trapping enables the real-time manipulation and observation of morphological evolution of individual particles during reaction chemistry. Here, optical trapping was used in combination with Raman spectroscopy to conduct airborne assembly and kinetic experiments. Micro-droplets of alkoxysilane were levitated in air prior to undergoing either acid- or base-catalyzed sol–gel reaction chemistry to form silica particles. The evolution of the reaction was monitored in real-time; Raman and Mie spectroscopies confirmed the in situ formation of silica particles from alkoxysilane droplets as the product of successive hydrolysis and condensation reactions, with faster reaction kinetics in acid catalysis. Hydrolysis and condensation were accompanied by a reduction in droplet volume and silica formation. Two airborne particles undergoing solidification could be assembled into unique 3D structures such as dumb-bell shapes by manipulating a controlled collision. Our results provide a pipeline combining spectroscopy with optical microscopy and nanoscale FIB–SEM imaging to enable chemical and structural insights, with the opportunity to apply this methodology to probe structure formation during reactive inkjet printing.

U2 - 10.1021/acsanm.2c02683

DO - 10.1021/acsanm.2c02683

M3 - Article

VL - 5

SP - 11699

EP - 11706

JO - ACS Applied Nano Materials

JF - ACS Applied Nano Materials

IS - 8

ER -

In Situ Sol–Gel Synthesis of Unique Silica Structures Using Airborne Assembly: Implications for In-Air Reactive Manufacturing

Abstract

Bibliographical note

Access to Document

Fingerprint

Cite this