Synthesis of Porous Hollow Organosilica Particles with Tunable Shell Thickness

Porous hollow silica particles possess promising applications in many fields, ranging from drug delivery to catalysis. From the synthesis perspective, the most challenging parameters are the monodispersity of the size distribution and the thickness and porosity of the shell of the particles. This pa...

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Main Authors: Mohammed A. Al-Khafaji, Anikó Gaál, Bálint Jezsó, Judith Mihály, Dorota Bartczak, Heidi Goenaga-Infante, Zoltán Varga
Format: Article
Language:English
Published: MDPI AG 2022-04-01
Series:Nanomaterials
Subjects:
Online Access:https://www.mdpi.com/2079-4991/12/7/1172
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author Mohammed A. Al-Khafaji
Anikó Gaál
Bálint Jezsó
Judith Mihály
Dorota Bartczak
Heidi Goenaga-Infante
Zoltán Varga
author_facet Mohammed A. Al-Khafaji
Anikó Gaál
Bálint Jezsó
Judith Mihály
Dorota Bartczak
Heidi Goenaga-Infante
Zoltán Varga
author_sort Mohammed A. Al-Khafaji
collection DOAJ
description Porous hollow silica particles possess promising applications in many fields, ranging from drug delivery to catalysis. From the synthesis perspective, the most challenging parameters are the monodispersity of the size distribution and the thickness and porosity of the shell of the particles. This paper demonstrates a facile two-pot approach to prepare monodisperse porous-hollow silica particles with uniform spherical shape and well-tuned shell thickness. In this method, a series of porous-hollow inorganic and organic-inorganic core-shell silica particles were synthesized via hydrolysis and condensation of 1,2-bis(triethoxysilyl) ethane (BTEE) and tetraethyl orthosilicate (TEOS) in the presence of hexadecyltrimethylammonium bromide (CTAB) as a structure-directing agent on solid silica spheres as core templates. Finally, the core templates were removed via hydrothermal treatment under alkaline conditions. Transmission electron microscopy (TEM) was used to characterize the particles′ morphology and size distribution, while the changes in the chemical composition during synthesis were followed by Fourier-transform infrared spectroscopy. Single-particle inductively coupled plasma mass spectrometry (spICP-MS) was applied to assess the monodispersity of the hollow particles prepared with different reaction parameters. We found that the presence of BTEE is key to obtaining a well-defined shell structure, and the increase in the concentration of the precursor and the surfactant increases the thickness of the shell. TEM and spICP-MS measurements revealed that fused particles are also formed under suboptimal reaction parameters, causing the broadening of the size distribution, which can be preceded by using appropriate concentrations of BTEE, CTAB, and ammonia.
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spelling doaj.art-b61cd48df59148548710806b9d0533802023-11-30T23:45:31ZengMDPI AGNanomaterials2079-49912022-04-01127117210.3390/nano12071172Synthesis of Porous Hollow Organosilica Particles with Tunable Shell ThicknessMohammed A. Al-Khafaji0Anikó Gaál1Bálint Jezsó2Judith Mihály3Dorota Bartczak4Heidi Goenaga-Infante5Zoltán Varga6Institute of Materials and Environmental Chemistry, Research Centre for Natural Sciences, H-1117 Budapest, HungaryInstitute of Materials and Environmental Chemistry, Research Centre for Natural Sciences, H-1117 Budapest, HungaryInstitute of Materials and Environmental Chemistry, Research Centre for Natural Sciences, H-1117 Budapest, HungaryInstitute of Materials and Environmental Chemistry, Research Centre for Natural Sciences, H-1117 Budapest, HungaryNational Measurement Laboratory, LGC Limited, Teddington TW11 0LY, UKNational Measurement Laboratory, LGC Limited, Teddington TW11 0LY, UKInstitute of Materials and Environmental Chemistry, Research Centre for Natural Sciences, H-1117 Budapest, HungaryPorous hollow silica particles possess promising applications in many fields, ranging from drug delivery to catalysis. From the synthesis perspective, the most challenging parameters are the monodispersity of the size distribution and the thickness and porosity of the shell of the particles. This paper demonstrates a facile two-pot approach to prepare monodisperse porous-hollow silica particles with uniform spherical shape and well-tuned shell thickness. In this method, a series of porous-hollow inorganic and organic-inorganic core-shell silica particles were synthesized via hydrolysis and condensation of 1,2-bis(triethoxysilyl) ethane (BTEE) and tetraethyl orthosilicate (TEOS) in the presence of hexadecyltrimethylammonium bromide (CTAB) as a structure-directing agent on solid silica spheres as core templates. Finally, the core templates were removed via hydrothermal treatment under alkaline conditions. Transmission electron microscopy (TEM) was used to characterize the particles′ morphology and size distribution, while the changes in the chemical composition during synthesis were followed by Fourier-transform infrared spectroscopy. Single-particle inductively coupled plasma mass spectrometry (spICP-MS) was applied to assess the monodispersity of the hollow particles prepared with different reaction parameters. We found that the presence of BTEE is key to obtaining a well-defined shell structure, and the increase in the concentration of the precursor and the surfactant increases the thickness of the shell. TEM and spICP-MS measurements revealed that fused particles are also formed under suboptimal reaction parameters, causing the broadening of the size distribution, which can be preceded by using appropriate concentrations of BTEE, CTAB, and ammonia.https://www.mdpi.com/2079-4991/12/7/1172porous hollow silica particlesorganosilica1,2-bis(triethoxysilyl) ethanespICP-MS
spellingShingle Mohammed A. Al-Khafaji
Anikó Gaál
Bálint Jezsó
Judith Mihály
Dorota Bartczak
Heidi Goenaga-Infante
Zoltán Varga
Synthesis of Porous Hollow Organosilica Particles with Tunable Shell Thickness
Nanomaterials
porous hollow silica particles
organosilica
1,2-bis(triethoxysilyl) ethane
spICP-MS
title Synthesis of Porous Hollow Organosilica Particles with Tunable Shell Thickness
title_full Synthesis of Porous Hollow Organosilica Particles with Tunable Shell Thickness
title_fullStr Synthesis of Porous Hollow Organosilica Particles with Tunable Shell Thickness
title_full_unstemmed Synthesis of Porous Hollow Organosilica Particles with Tunable Shell Thickness
title_short Synthesis of Porous Hollow Organosilica Particles with Tunable Shell Thickness
title_sort synthesis of porous hollow organosilica particles with tunable shell thickness
topic porous hollow silica particles
organosilica
1,2-bis(triethoxysilyl) ethane
spICP-MS
url https://www.mdpi.com/2079-4991/12/7/1172
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