Synthesis and Characterization of Anatase TiO2 Nanorods: Insights from Nanorods’ Formation and Self-Assembly

Seyed Naveed Hosseini; Xiaodan Chen; Patrick J. Baesjou; Arnout Imhof; Alfons van Blaaderen

doi:10.3390/app12031614

Synthesis and Characterization of Anatase TiO₂ Nanorods: Insights from Nanorods’ Formation and Self-Assembly

Seyed Naveed Hosseini, Xiaodan Chen, Patrick J. Baesjou^*, Arnout Imhof, Alfons van Blaaderen

^*Corresponding author for this work

Sub Soft Condensed Matter

Utrecht University

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

Abstract

Highly crystalline, organic-solvent-dispersible titanium dioxide (TiO2) nanorods (NRs) present promising chemicophysical properties in many diverse applications. In this paper, based on a modified procedure from literature, TiO2 NRs were synthesized via a ligand-assisted nonhydrolytic sol-gel route using oleic acid as the solvent, reagent, and ligand and titanium (IV) isopropoxide as the titanium precursor. This procedure produced monodisperse TiO2 NRs, as well as some semispherical titania nanocrystals (NCs) that could be removed by size-selective precipitation. X-ray diffraction and selected area electron diffraction results showed that the nanorods were anatase, while the semipheres also contained the TiO2(B) phase. By taking samples during the particle growth, it was found that the average length of the initially grown NRs decreased during the synthesis. Possible reasons for this unusual growth path, partially based on high-resolution transmission electron microscopy (HRTEM) observations during the growth, were discussed. The dispersion of anatase TiO2 nanorods was capable of spontaneous formation of lyotropic liquid crystals on the TEM grid and in bulk. Considering high colloidal stability together with the large optical birefringence displayed by these high refractive index liquid crystalline domains, we believe these TiO2 NRs dispersions are promising candidates for application in transparent and switchable optics.

Original language	English
Article number	1614
Pages (from-to)	1-18
Journal	Applied Sciences (Switzerland)
Volume	12
Issue number	3
DOIs	https://doi.org/10.3390/app12031614
Publication status	Published - 1 Feb 2022

Bibliographical note

Funding Information:
Funding: This research was funded by the Dutch Technology Foundation STW (grant 14176), which is part of the Netherlands Organization for Scientific Research-Applied and Engineering Sciences (NWO-TTW) and partly funded by the Ministry of Economic Affairs.

Funding Information:
Acknowledgments: The authors acknowledge the Dutch Technology Foundation STW (grant 14176), which is part of the Netherlands Organization for Scientific Research-Applied and Engineering Sciences (NWO-TTW) and partly funded by the Ministry of Economic Affairs. X.C. acknowledges the European Research Council for their support via the ERC Consolidator Grant NANO-INSITU (grant 683076). The authors would like to thank Dennie Wezendonk for the X-ray measurements, Peter Helfferich for his help during POM measurements, Chris Schneijdenberg for technical assistance in electron microscopy analysis, Albert Grau-Carbonell for carrying out numerical calculations for van der Waals interaction potentials, and Dagney Mackaaij for her contributions on titania synthesis experiments.

Funding Information:
This research was funded by the Dutch Technology Foundation STW (grant 14176), which is part of the Netherlands Organization for Scientific Research- Applied and Engineering Sciences (NWO-TTW) and partly funded by the Ministry of Economic Affairs.

Publisher Copyright:
© 2022 by the authors. Licensee MDPI, Basel, Switzerland.

Funding

Funding: This research was funded by the Dutch Technology Foundation STW (grant 14176), which is part of the Netherlands Organization for Scientific Research-Applied and Engineering Sciences (NWO-TTW) and partly funded by the Ministry of Economic Affairs. Acknowledgments: The authors acknowledge the Dutch Technology Foundation STW (grant 14176), which is part of the Netherlands Organization for Scientific Research-Applied and Engineering Sciences (NWO-TTW) and partly funded by the Ministry of Economic Affairs. X.C. acknowledges the European Research Council for their support via the ERC Consolidator Grant NANO-INSITU (grant 683076). The authors would like to thank Dennie Wezendonk for the X-ray measurements, Peter Helfferich for his help during POM measurements, Chris Schneijdenberg for technical assistance in electron microscopy analysis, Albert Grau-Carbonell for carrying out numerical calculations for van der Waals interaction potentials, and Dagney Mackaaij for her contributions on titania synthesis experiments. This research was funded by the Dutch Technology Foundation STW (grant 14176), which is part of the Netherlands Organization for Scientific Research- Applied and Engineering Sciences (NWO-TTW) and partly funded by the Ministry of Economic Affairs.

Keywords

Inorganic liquid crystals
Nanorods
Self-assembly
Titanium dioxide

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Cite this

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title = "Synthesis and Characterization of Anatase TiO2 Nanorods: Insights from Nanorods{\textquoteright} Formation and Self-Assembly",

abstract = "Highly crystalline, organic-solvent-dispersible titanium dioxide (TiO2) nanorods (NRs) present promising chemicophysical properties in many diverse applications. In this paper, based on a modified procedure from literature, TiO2 NRs were synthesized via a ligand-assisted nonhydrolytic sol-gel route using oleic acid as the solvent, reagent, and ligand and titanium (IV) isopropoxide as the titanium precursor. This procedure produced monodisperse TiO2 NRs, as well as some semispherical titania nanocrystals (NCs) that could be removed by size-selective precipitation. X-ray diffraction and selected area electron diffraction results showed that the nanorods were anatase, while the semipheres also contained the TiO2(B) phase. By taking samples during the particle growth, it was found that the average length of the initially grown NRs decreased during the synthesis. Possible reasons for this unusual growth path, partially based on high-resolution transmission electron microscopy (HRTEM) observations during the growth, were discussed. The dispersion of anatase TiO2 nanorods was capable of spontaneous formation of lyotropic liquid crystals on the TEM grid and in bulk. Considering high colloidal stability together with the large optical birefringence displayed by these high refractive index liquid crystalline domains, we believe these TiO2 NRs dispersions are promising candidates for application in transparent and switchable optics.",

keywords = "Inorganic liquid crystals, Nanorods, Self-assembly, Titanium dioxide",

author = "Hosseini, {Seyed Naveed} and Xiaodan Chen and Baesjou, {Patrick J.} and Arnout Imhof and Blaaderen, {Alfons van}",

note = "Funding Information: Funding: This research was funded by the Dutch Technology Foundation STW (grant 14176), which is part of the Netherlands Organization for Scientific Research-Applied and Engineering Sciences (NWO-TTW) and partly funded by the Ministry of Economic Affairs. Funding Information: Acknowledgments: The authors acknowledge the Dutch Technology Foundation STW (grant 14176), which is part of the Netherlands Organization for Scientific Research-Applied and Engineering Sciences (NWO-TTW) and partly funded by the Ministry of Economic Affairs. X.C. acknowledges the European Research Council for their support via the ERC Consolidator Grant NANO-INSITU (grant 683076). The authors would like to thank Dennie Wezendonk for the X-ray measurements, Peter Helfferich for his help during POM measurements, Chris Schneijdenberg for technical assistance in electron microscopy analysis, Albert Grau-Carbonell for carrying out numerical calculations for van der Waals interaction potentials, and Dagney Mackaaij for her contributions on titania synthesis experiments. Funding Information: This research was funded by the Dutch Technology Foundation STW (grant 14176), which is part of the Netherlands Organization for Scientific Research- Applied and Engineering Sciences (NWO-TTW) and partly funded by the Ministry of Economic Affairs. Publisher Copyright: {\textcopyright} 2022 by the authors. Licensee MDPI, Basel, Switzerland.",

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AU - Hosseini, Seyed Naveed

AU - Chen, Xiaodan

AU - Baesjou, Patrick J.

AU - Imhof, Arnout

AU - Blaaderen, Alfons van

N1 - Funding Information: Funding: This research was funded by the Dutch Technology Foundation STW (grant 14176), which is part of the Netherlands Organization for Scientific Research-Applied and Engineering Sciences (NWO-TTW) and partly funded by the Ministry of Economic Affairs. Funding Information: Acknowledgments: The authors acknowledge the Dutch Technology Foundation STW (grant 14176), which is part of the Netherlands Organization for Scientific Research-Applied and Engineering Sciences (NWO-TTW) and partly funded by the Ministry of Economic Affairs. X.C. acknowledges the European Research Council for their support via the ERC Consolidator Grant NANO-INSITU (grant 683076). The authors would like to thank Dennie Wezendonk for the X-ray measurements, Peter Helfferich for his help during POM measurements, Chris Schneijdenberg for technical assistance in electron microscopy analysis, Albert Grau-Carbonell for carrying out numerical calculations for van der Waals interaction potentials, and Dagney Mackaaij for her contributions on titania synthesis experiments. Funding Information: This research was funded by the Dutch Technology Foundation STW (grant 14176), which is part of the Netherlands Organization for Scientific Research- Applied and Engineering Sciences (NWO-TTW) and partly funded by the Ministry of Economic Affairs. Publisher Copyright: © 2022 by the authors. Licensee MDPI, Basel, Switzerland.

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N2 - Highly crystalline, organic-solvent-dispersible titanium dioxide (TiO2) nanorods (NRs) present promising chemicophysical properties in many diverse applications. In this paper, based on a modified procedure from literature, TiO2 NRs were synthesized via a ligand-assisted nonhydrolytic sol-gel route using oleic acid as the solvent, reagent, and ligand and titanium (IV) isopropoxide as the titanium precursor. This procedure produced monodisperse TiO2 NRs, as well as some semispherical titania nanocrystals (NCs) that could be removed by size-selective precipitation. X-ray diffraction and selected area electron diffraction results showed that the nanorods were anatase, while the semipheres also contained the TiO2(B) phase. By taking samples during the particle growth, it was found that the average length of the initially grown NRs decreased during the synthesis. Possible reasons for this unusual growth path, partially based on high-resolution transmission electron microscopy (HRTEM) observations during the growth, were discussed. The dispersion of anatase TiO2 nanorods was capable of spontaneous formation of lyotropic liquid crystals on the TEM grid and in bulk. Considering high colloidal stability together with the large optical birefringence displayed by these high refractive index liquid crystalline domains, we believe these TiO2 NRs dispersions are promising candidates for application in transparent and switchable optics.

AB - Highly crystalline, organic-solvent-dispersible titanium dioxide (TiO2) nanorods (NRs) present promising chemicophysical properties in many diverse applications. In this paper, based on a modified procedure from literature, TiO2 NRs were synthesized via a ligand-assisted nonhydrolytic sol-gel route using oleic acid as the solvent, reagent, and ligand and titanium (IV) isopropoxide as the titanium precursor. This procedure produced monodisperse TiO2 NRs, as well as some semispherical titania nanocrystals (NCs) that could be removed by size-selective precipitation. X-ray diffraction and selected area electron diffraction results showed that the nanorods were anatase, while the semipheres also contained the TiO2(B) phase. By taking samples during the particle growth, it was found that the average length of the initially grown NRs decreased during the synthesis. Possible reasons for this unusual growth path, partially based on high-resolution transmission electron microscopy (HRTEM) observations during the growth, were discussed. The dispersion of anatase TiO2 nanorods was capable of spontaneous formation of lyotropic liquid crystals on the TEM grid and in bulk. Considering high colloidal stability together with the large optical birefringence displayed by these high refractive index liquid crystalline domains, we believe these TiO2 NRs dispersions are promising candidates for application in transparent and switchable optics.

KW - Inorganic liquid crystals

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KW - Self-assembly

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