Direct imaging of carbon nanotubes spontaneously filled with solvent

Green, Micah J.; Young, Colin C.; Parra-Vasquez, A. Nicholas G.; Majumder, Mainak; Juloori, Varun; Behabtu, Natnael; Pint, Cary L.; Schmidt, Judith; Kesselman, Ellina; Hauge, Robert H.; Cohen, Yachin; Talmon, Yeshayahu; Pasquali, Matteo

doi:10.1039/c0cc03915b

Cited by 14 publications

(19 citation statements)

References 30 publications

(43 reference statements)

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“…By adjusting the electron dose to the thickness of the vitrified acid cryo‐specimens (thicker areas require more etching), one can generate sufficient contrast to image carbon nanotubes and graphene in superacids (Davis et al ., ; Behabtu et al ., ; Parra‐Vasquez et al ., ; Green et al ., ; Behabtu, ) We have used irradiation contrast enhancement in the development of a method for measuring the length of individual CNTs (Bengio et al ., ).…”

Section: Methodsmentioning

confidence: 97%

“…Thus, the vitrified acid matrix is more optically dense than the CNTs or graphene embedded in it and appears darker than the dispersed objects. However, the relatively large thickness of the vitrified acid matrix in comparison to nanometre‐scale thickness of the embedded aggregates (especially SWNTs), together with the spontaneous filling of nanotubes by the acid (Green et al ., ), reduces the contrast dramatically. We have found that controlling the cryo‐specimen and imaging parameters, such as film thickness, electron exposure and underfocus, are critical for good contrast.…”

Section: Methodsmentioning

confidence: 99%

“…Spontaneous CNT filling with liquids (for example Gogotsi et al ., ; Bekou & Mattia, ) and with CSA in particular (Green et al ., ) was recently observed by cryo‐TEM and other techniques. Big diameter MWNTs all are readily discernible due to the thinness of the vitrified specimen (Fig.…”

Section: Methodsmentioning

confidence: 99%

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Cryogenic‐temperature electron microscopy direct imaging of carbon nanotubes and graphene solutions in superacids

Kleinerman

Parra-Vasquez

Green

et al. 2015

Journal of Microscopy

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Cryogenic electron microscopy (cryo-EM) is a powerful tool for imaging liquid and semiliquid systems. While cryogenic transmission electron microscopy (cryo-TEM) is a standard technique in many fields, cryogenic scanning electron microscopy (cryo-SEM) is still not that widely used and is far less developed. The vast majority of systems under investigation by cryo-EM involve either water or organic components. In this paper, we introduce the use of novel cryo-TEM and cryo-SEM specimen preparation and imaging methodologies, suitable for highly acidic and very reactive systems. Both preserve the native nanostructure in the system, while not harming the expensive equipment or the user. We present examples of direct imaging of single-walled, multiwalled carbon nanotubes and graphene, dissolved in chlorosulfonic acid and oleum. Moreover, we demonstrate the ability of these new cryo-TEM and cryo-SEM methodologies to follow phase transitions in carbon nanotube (CNT)/superacid systems, starting from dilute solutions up to the concentrated nematic liquid-crystalline CNT phases, used as the 'dope' for all-carbon-fibre spinning. Originally developed for direct imaging of CNTs and graphene dissolution and self-assembly in superacids, these methodologies can be implemented for a variety of highly acidic systems, paving a way for a new field of nonaqueous cryogenic electron microscopy.

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Section: Methodsmentioning

confidence: 97%

Section: Methodsmentioning

confidence: 99%

See 1 more Smart Citation

Cryogenic‐temperature electron microscopy direct imaging of carbon nanotubes and graphene solutions in superacids

Kleinerman

Parra-Vasquez

Green

et al. 2015

Journal of Microscopy

Self Cite

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“…23 A very recent experimental result showed a similar deformation of CNTs lled with chlorosulfonic acid by employing cryogenic transmission electron microscopy. 24 Our previous work has shown that a CNT lled with droplets could be continuously deformed by increasing the lling ratio. 22 The tube was observed to smoothly change from a circular shape to an elliptical shape when the capillary forces outweigh the elastic force.…”

Section: Introductionmentioning

confidence: 98%

“…21 Hence, the phenomenon of elasto-capillarity could not be ignored in liquid inltrated CNTs. The deformation of CNTs has been both theoretically 22 and experimentally 23,24 reported by several research groups. Rossi et al reported elastic deformation of CNTs induced by water condensation on the inner walls of the nanotubes.…”

Section: Introductionmentioning

confidence: 99%

The collapse of an elastic tube induced by encapsulated liquid droplets

Yang

Yuan

et al. 2013

Soft Matter

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Using molecular dynamic simulations, we studied the equilibrium structure of an elastic nanotube filled with separated liquid droplets. When the filling of liquid droplets exceeded a certain critical ratio, the circular carbon nanotube was observed to be deformed into an elliptical one, associated with the coalescence of liquid droplets. We have proposed a theoretical model to explain such an abrupt structural deformation. Based on the competition between capillary and elastic energy, our theoretical model explained the collapse of the elastic tube very well and gave consistent predictions with the simulation results. The theoretical model was quite general and can be extended to other similar soft matter systems although it was originally deduced from the liquid-filled carbon nanotube systems.

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Ultrastrong Hybrid Fibers with Tunable Macromolecular Interfaces of Graphene Oxide and Carbon Nanotube for Multifunctional Applications

et al. 2022

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Individual carbon nanotubes (CNT) and graphene have unique mechanical and electrical properties; however, the properties of their macroscopic assemblies have not met expectations because of limited physical dimensions, the limited degree of dispersion of the components, and various structural defects. Here, a state‐of‐the‐art assembly for a novel type of hybrid fiber possessing the properties required for a wide variety of multifunctional applications is presented. A simple and effective multidimensional nanostructure of CNT and graphene oxide (GO) assembled by solution processing improves the interfacial utilization of the components. Flexible GOs are effectively intercalated between nanotubes along the shape of CNTs, which reduces voids, enhances orientation, and maximizes the contact between elements. The microstructure is finely controlled by the elements content ratio and dimensions, and an optimal balance improves the mechanical properties. The hybrid fibers simultaneously exhibit exceptional strength (6.05 GPa), modulus (422 GPa), toughness (76.8 J g–1), electrical conductivity (8.43 MS m–1), and knot strength efficiency (92%). Furthermore, surface and electrochemical properties are significantly improved by tuning the GO content, further expanding the scope of applications. These hybrid fibers are expected to offer a strategy for overcoming the limitations of existing fibers in meeting the requirements for applications in the fiber industry.

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Direct imaging of carbon nanotubes spontaneously filled with solvent

Cited by 14 publications

References 30 publications

Cryogenic‐temperature electron microscopy direct imaging of carbon nanotubes and graphene solutions in superacids

Cryogenic‐temperature electron microscopy direct imaging of carbon nanotubes and graphene solutions in superacids

The collapse of an elastic tube induced by encapsulated liquid droplets

Ultrastrong Hybrid Fibers with Tunable Macromolecular Interfaces of Graphene Oxide and Carbon Nanotube for Multifunctional Applications

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