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In This Article

  • Summary
  • Abstract
  • Introduction
  • Protocol
  • Representative Results
  • Discussion
  • Disclosures
  • Acknowledgements
  • Materials
  • References
  • Reprints and Permissions

Summary

A method for the functionalization of carbon nanotubes with structure-tunable polymeric encapsulation layers and structural characterization using small-angle neutron scattering is presented.

Abstract

We demonstrate a protocol for single-walled carbon nanotube functionalization using thermo-sensitive PEO-PPO-PEO triblock copolymers in an aqueous solution. In a carbon nanotube/PEO105-PPO70-PEO105 (poloxamer 407) aqueous solution, the amphiphilic poloxamer 407 adsorbs onto the carbon nanotube surfaces and self-assembles into continuous layers, driven by intermolecular interactions between constituent molecules. The addition of 5-methylsalicylic acid changes the self-assembled structure from spherical-micellar to a cylindrical morphology. The fabricated poloxamer 407/carbon nanotube hybrid particles exhibit thermo-responsive structural features so that the density and thickness of poloxamer 407 layers are also reversibly controllable by varying temperature. The detailed structural properties of the poloxamer 407/carbon nanotube particles in suspension can be characterized by small-angle neutron scattering experiments and model fit analyses. The distinct curve shapes of the scattering intensities depending on temperature control or addition of aromatic additives are well described by a modified core-shell cylinder model consisting of a carbon nanotube core cylinder, a hydrophobic shell, and a hydrated polymer layer. This method can provide a simple but efficient way for the fabrication and in-situ characterization of carbon nanotube-based nano particles with a structure-tunable encapsulation.

Introduction

Carbon nanotubes (CNTs) are hollow cylindrical nanoparticles formed by rolling a micrometer-scale graphite sheet into a nanotube. Because of their extraordinary mechanical, thermal, and electrical properties, CNTs have been extensively investigated as a novel candidate for functional nanoparticles in therapeutic and bio-sensing applications as well as nano-fillers in self-assembled nanocomposite materials.1-3 However, their poor solubility and strong preference toward making bundles in commonly used organic and aqueous solvents hinder easy and environmentally-friendly processing as well as advances in biological applications. Therefore, a variety of functio....

Protocol

Note: This protocol requires special care in the handling of nanomaterials. As-purchased single-walled carbon nanotubes (SWNTs) exist in the form of fine powder and thus, they should be considered as nano-hazardous materials before dispersing them in aqueous solutions. Please use appropriate safety equipment described in the material safety data sheets (MSDS).

1. Preparation of Poloxamer 407/SWNT Aqueous Suspensions

Note: Proceed with all the sample preparation proced.......

Representative Results

Poloxamer 407-coated SWNT nanorod suspensions were fabricated using the sample preparation procedure (Figure 4), which can be divided into two important processes; the physical adsorption process of poloxamer 407 on SWNT surfaces using ultra-sonication, and the fractionation process of individually-stabilized SWNTs from bundled aggregates using centrifugation.

The SANS scattering intensities were obtained for th.......

Discussion

SANS and AFM measurements showed that SWNTs have been successfully de-bundled and individually dispersed in aqueous solution using a poloxamer 407 triblock copolymer. In this sample preparation method, ultra-sonication and centrifugation processes are the critical steps determining the characteristics of the final suspension. The strong interaction between the SWNTs, which forces uncoated SWNTs to bundle together in solution, must be overcome to stabilize the individual SWNTs with block copolymers. Providing a sufficient.......

Disclosures

The authors have nothing to disclose.

Acknowledgements

The Research at Oak Ridge National Laboratory's Spallation Neutron Source and Center for Nanophase Materials Sciences was sponsored by the Scientific User Facilities Division, Office of Basic Energy Sciences, U.S. Department of Energy. The author, Zhe Zhang, gratefully acknowledges the financial support from Jülich Center for Neutron Science, Research center Jülich.

....

Materials

NameCompanyCatalog NumberComments
HiPco Single-walled carbon nanotubesUnidymP2771
Pluronic F127BASF9003-11-6Mw = 12.6 kg/mol
5-methylsalicylic acidTCI AmericaC0410
Ultrasonic processorCole-ParmerML-04714-52
Sorvall 6 plus centrifugeThermo Scientific46910
Innova AFM Bruker
Si-waferSilicon Quest International150 mm in diameter  ; N type <1-1-1> cut ; 1-10 Ohm/cm ; Single-side polyshed (675 +- 25 um) ; Diced (12 mm x 12 mm)

References

  1. Kostarelos, K., Bianco, A., Prato, M. Promises, facts and challenges for carbon nanotubes in imaging and therapeutics. Nat Nanotechnol. 4 (10), 627-633 (2009).
  2. Baughman, R. H., Zakhidov, A. A., de Heer, W. A. Carbon nanotubes....

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Carbon NanotubesBlock CopolymersSmall angle Neutron ScatteringFunctionalizationThermo reversibleNanoparticlesStimuli responsiveSelf assemblyUltrasonicationCentrifugation5 methylsalicylic Acid

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