Name: functionalization of single-walled carbon nanotubes with thermo-reversible block copolymers and characterization by small-angle neutron scattering
Uploaded: 2016-06-01T13:00:00
Description: Watch this Scientific Journal Video about Functionalization of Single-walled Carbon Nanotubes with Thermo-reversible Block Copolymers and Characterization by Small-angle Neutron Scattering at JoVE.com

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 J&#252;lich Center for Neutron Science, Research center J&#252;lich.

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...

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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...

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 functionalization methods, such as ultra-sonication, chemical surface modification, and non-covalent functionalization by using surfactants and block copolymers,4-9 have been developed to modify the CNT surfaces and improve their dispersibility in a wide range of solvents. Non-covalent functionalization methods based on physical surface treatments, in particular, are considered to be a promising and robust strategy, because any surface-modification induced suppression in intrinsic CNT properties can be minimized.10 To date, there have been numerous efforts to improve the dispersion efficiency of non-covalent functionalization methods by employing various types of dispersive agents including basic surfactants (e.g., SDS, CTAB, NaDDBS),7,11 amphiphilic block copolymers,8 bio-materials (e.g., DNA),12,13 and synthetic functional polymers (e.g., conjugated polymer, aromatic polymer).14,15
PEO-PPO-PEO polymers, a kind of triblock copolymer consisting of two hydrophilic poly(ethylene oxide) (PEO) chains at both ends covalently bound to one hydrophobic poly(propylene oxide) (PPO) chain at the center, can extend the potential application of non-covalently functionalized CNTs in aqueous solution. These polymers provide the interface, which is friendly not only to the CNT surfaces but also to aqueous media and other polymer matrices and exhibits tremendous biocompatibility due to the minimal toxicity of the PEO chains. This facilitates easier processing in a wide range of dispersing environments as well as the utilization of polymer-coated CNTs in biomedical applications.12,16-17 Moreover, the rich thermodynamic phase behavior of these polymers based on their sensitive responses to external stimuli enables the fabrication of the smart block copolymer-CNT hybrid nanostructures in which intra- and inter-particle structures can be reversibly and precisely controlled.18-21 Here, we present a protocol for the fabrication of CNT-based hybrid nanoparticles with a tunable encapsulation layer of PEO105-PPO70-PEO105 (poloxamer 407). The resulting structure is characterized by small-angle neutron scattering (SANS). This work is expected to introduce the concept of smart functional building blocks and help non-specialists easily prepare block copolymer-functionalized CNT suspensions and use SANS for the detailed characterization at Oak Ridge National Laboratory.

<table border="0" cellpadding="0" cellspacing="0" width="634">
	<tbody>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">HiPco Single-walled carbon nanotubes</td>
			<td style="width:71px;">Unidym</td>
			<td style="width:119px;">P2771</td>
			<td style="width:228px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Pluronic F127</td>
			<td style="width:71px;">BASF</td>
			<td>9003-11-6</td>
			<td>Mw = 12.6 kg/mol</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">5-methylsalicylic acid</td>
			<td style="width:71px;">TCI America</td>
			<td>C0410</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Ultrasonic processor</td>
			<td style="width:71px;">Cole-Parmer</td>
			<td>ML-04714-52</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Sorvall 6 plus centrifuge</td>
			<td style="width:71px;">Thermo Scientific</td>
			<td align="right" style="width:119px;">46910</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Innova AFM&#160;</td>
			<td style="width:71px;">Bruker</td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="89">
			<td height="89" style="height:89px;width:216px;">Si-wafer</td>
			<td style="width:71px;">Silicon Quest International</td>
			<td style="width:119px;"></td>
			<td style="width:228px;">150 mm in diameter&#160; ; N type &#60;1-1-1&#62; cut ; 1-10 Ohm/cm ; Single-side polyshed (675 +- 25 um) ; Diced (12 mm x 12 mm)</td>
		</tr>
	</tbody>
</table>

functionalization of single-walled carbon nanotubes with thermo-reversible block copolymers and characterization by small-angle neutron scattering

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.

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...

Watch this Scientific Journal Video about Functionalization of Single-walled Carbon Nanotubes with Thermo-reversible Block Copolymers and Characterization by Small-angle Neutron Scattering at JoVE.com

Functionalization of Single-walled Carbon Nanotubes with Thermo-reversible Block Copolymers and Characterization by Small-angle Neutron Scattering

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

We demonstrate a protocol for single-walled carbon nanotube functionalization using thermo-sensitive PEO-PPO-PEO triblock copolymers in an aqueous ...

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