Wet spinning imogolite nanotube fibres: an in situ process study
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Published version
Author(s)
Shaffer, Milo
Moore, Joe
Paineau, Erwan
Launois, Pascale
Type
Journal Article
Abstract
Imogolite nanotubes (INTs) form transparent aqueous nematic solutions, with strong birefringence and X-ray scattering
power. They provide an ideal model system for studying the assembly of one-dimensional nanomaterials into fibres, as well
as offering interesting properties in their own right. Here, in-situ polarised optical microscopy is used to study the wet
spinning of pure INTs into fibres, illustrating the influence of process variables during extrusion, coagulation, washing and
drying on both structure and mechanical properties. Tapered spinnerets were shown to be significantly more effective than
thin cylindrical channels for forming homogeneous fibres; a result related to simple capilliary rheology by fitting a shear
thinning flow model. The washing step has a strong influence of structure and properties, combining the removal of residual
counter-ions and structural relaxation to produce a less aligned, denser and more networked structure; the timescales and
scaling behviour of the processes are compared quantitatively. Both strength and stiffness are higher for INT fibres with a
higher packing fraction and lower degree of alignment, indicating the importance of forming a rigid jammed network to
transfer stress through these porous, rigid rod assemblies. The electrostatically-stabilised, rigid rod INT solutions were
successfully cross-linked using multivalent anions, providing robust gels, potentially useful in other contexts.
power. They provide an ideal model system for studying the assembly of one-dimensional nanomaterials into fibres, as well
as offering interesting properties in their own right. Here, in-situ polarised optical microscopy is used to study the wet
spinning of pure INTs into fibres, illustrating the influence of process variables during extrusion, coagulation, washing and
drying on both structure and mechanical properties. Tapered spinnerets were shown to be significantly more effective than
thin cylindrical channels for forming homogeneous fibres; a result related to simple capilliary rheology by fitting a shear
thinning flow model. The washing step has a strong influence of structure and properties, combining the removal of residual
counter-ions and structural relaxation to produce a less aligned, denser and more networked structure; the timescales and
scaling behviour of the processes are compared quantitatively. Both strength and stiffness are higher for INT fibres with a
higher packing fraction and lower degree of alignment, indicating the importance of forming a rigid jammed network to
transfer stress through these porous, rigid rod assemblies. The electrostatically-stabilised, rigid rod INT solutions were
successfully cross-linked using multivalent anions, providing robust gels, potentially useful in other contexts.
Date Issued
2023-06-21
Date Acceptance
2023-05-15
Citation
Nanoscale Advances, 2023, 5 (12), pp.3376-3385
ISSN
2516-0230
Publisher
The Royal Society of Chemistry
Start Page
3376
End Page
3385
Journal / Book Title
Nanoscale Advances
Volume
5
Issue
12
Copyright Statement
© 2023 The Author(s). Published by the Royal Society of Chemistry. This article is licensed under a Creative Commons Attribution 3.0 Unported Licence.
License URL
Identifier
https://pubs.rsc.org/en/content/articlelanding/2023/na/d3na00013c
Publication Status
Published
Date Publish Online
2023-05-31