Name: grafting multiwalled carbon nanotubes with polystyrene to enable self-assembly and anisotropic patchiness
Uploaded: 2018-04-01T13:00:00
Description: Watch this Scientific Journal Video about Grafting Multiwalled Carbon Nanotubes with Polystyrene to Enable Self-Assembly and Anisotropic Patchiness at JoVE.com

We would like to acknowledge the FQ-PAIP and DGAPA-PAPIIT programs from National Autonomous University of Mexico (grant numbers 5000-9158, 5000-9156, IA205616 and IA205316) and the National Council for Science and Technology from Mexico -CONACYT- (grant number 251533).

Caution: Please consult all relevant material safety data sheets (MSDS) before use. Several of the chemicals used in this protocol are acutely toxic and carcinogenic. Carbon nanotube derivatives may have additional respiratory hazards compared to other traditional bulk carbon allotropes. It is suspected that carbon nanotubes in aerosol may affect lungs in a similar way than asbestos, though their carcinogenic properties have not been completely elucidated so far. Please use all appropriate safety practices when performin...

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In this method, there are some steps which result critical to guarantee a successful grafting process. First, the biphasic catalytically mediated oxidation reaction (Step 1.1) should be carried out with recently dispersed carbon nanotubes (Step 1.1.1.5). If dispersion results unviable according to the recommendations in the protocol, the use of an ultrasonic tip sonicator would be helpful if using the same indications (Step 1.1.1.6). Using shorter MWCNTs may also help in solving dispersion issues. Second, setting of the ...

Since the discovery of single-walled carbon nanotubes (SWCNTs),1,2 the scientific communities have applied their outstanding electrical, mechanical and thermal properties3 in a wide range of cutting-edge applications by modulating their surface properties via covalent4 and non-covalent5 strategies. Examples of those applications include their use as transducers in sensors,6,7 electrodes in solar cells,8 heterogeneous supports in catalysis,9 nanoreactors in synthesis,10 anti-fouling agents in protective films,11 fillers in composite materials,12etc. However, the possibility to modulate the surface properties of their more robust, yet industrially available multiwalled counterparts namely, MWCNTs, to control the directionality in their non-covalent interactions at the nanoscale, has remained a difficult task so far.13
Supramolecular self-assembly of molecular building blocks is one of the most versatile strategies to control the organization of matter at the nanoscale.14,15 In this sense, supramolecular interactions involve directional, short-range and mid-range non-covalent interactions such as H-bond, Van der Waals, dipole-dipole, ion-dipole, dipole-induced dipole, &#960;- &#960; stacking, cation-&#960;, anion-&#960;, coulombic, among others.16 Unfortunately, directionality in self-assembly for larger structures such as MWCNTs is not spontaneous and usually requires external motive forces (e.g. templates or energy dissipation systems).17 A recent report used non-covalent wrapping of nanotubes with tailored co-polymers to pursue the latter goal,18 but the use of covalent strategies to offer new alternatives to solve that problem have remained scarcely explored.
Chemical modification of carbon nanotubes can be selectively carried out to introduce different functional groups either to the termini or to the sidewalls of the same.19,20 One of the most useful approaches to tailor the surface properties in carbon nanostructures is polymer-grafting through standard polymerization routes. Typically, those approaches involve the preliminary introduction of polymerizable or initiator groups (acrylic, vinyl, etc.) on the nanostructure surface and their successive polymerization with a suitable monomer.21 In the case of MWCNTs, the covalent introduction of polymer chains on the sidewalls to control their patchiness in an anisotropic fashion has remained a challenge.
Here we will show how a series of straightforward chemical modification steps22,23 can be applied to insert PS chains on the sidewalls of MWCNTs in order to modify their surface patchiness and to promote their anisotropic self-assembly23 at the nanoscale. During the modification route, a first step allows for the selective hydroxylation of pristine MWCNTs at the sidewalls by following a biphasic catalytically mediated oxidation reaction to yield the hydroxylated counterparts namely, MWCNT-OH. A second step uses 3-(trimethoxysilyl)propyl methacrylate (TMSPMA) to introduce silylated methacrylic moieties to the previously created hydroxyl groups (MWCNT-O-TMSPMA). These inserts will provide surface reactive sites during a third step, when styrene monomer is polymerized from the methacrylic moieties thus yielding polymer chains grafted to the sidewalls of the nanotubes at the end (i.e. MWCNT-O-PS).

<table border="0" cellpadding="0" cellspacing="0" width="1573">
	<tbody>
		<tr height="21">
			<td height="21" style="height:21px;width:379px;">Tetrapropylammonium bromide, 99 % (TPABr)</td>
			<td style="width:181px;">Sigma-Aldrich</td>
			<td align="right" style="width:119px;">88104</td>
			<td style="width:895px;">Irritant, toxic</td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:379px;">Potassium permanganate, 99 % (KMnO4)</td>
			<td style="width:181px;">Sigma-Aldrich</td>
			<td align="right" style="width:119px;">223468</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:379px;">Acetic acid, 99.5 %</td>
			<td style="width:181px;">Sigma-Aldrich</td>
			<td align="right" style="width:119px;">45726</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:379px;">Pristine multiwalled carbon nanotubes, 99 % (MWCNTs)</td>
			<td style="width:181px;">Bayer Technology Services</td>
			<td style="width:119px;">Donated sample</td>
			<td>Harmful dusts. &#62;1 mm in length and 13&#8211;16 nm in outer diameter. Alternative supplier: Nanocyl, Catalog N. NC7000, website: http://www.nanocyl.com/</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:379px;">Sodium Chloride, 98 % (NaCl)</td>
			<td style="width:181px;">Sigma-Aldrich</td>
			<td style="width:119px;">S3014</td>
			<td>Technical grade can also be used</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:379px;">Ethanol, 99.8 % (EtOH)</td>
			<td style="width:181px;">Sigma-Aldrich</td>
			<td align="right" style="width:119px;">32221</td>
			<td>Technical grade can also be used</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:379px;">Methanol, 99.8 % (MeOH)</td>
			<td style="width:181px;">Sigma-Aldrich</td>
			<td align="right" style="width:119px;">322415</td>
			<td>Highly toxic. Technical grade can also be used</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:379px;">Hydroquinone, 99 %</td>
			<td style="width:181px;">Sigma-Aldrich</td>
			<td style="width:119px;">H9003</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:379px;">Toluene, 99.8 %</td>
			<td style="width:181px;">Sigma-Aldrich</td>
			<td align="right" style="width:119px;">244511</td>
			<td>Anhydrous</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:379px;">3-(Trimethoxysilyl)propyl methacrylate, 98 % (TMSPMA)</td>
			<td style="width:181px;">Sigma-Aldrich</td>
			<td align="right" style="width:119px;">440159</td>
			<td>Air sensitive, toxic</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:379px;">Azobisisobutyronitrile, 99 % (AIBN)</td>
			<td style="width:181px;">Sigma-Aldrich</td>
			<td align="right" style="width:119px;">755745</td>
			<td>Explosive</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:379px;">Styrene, 99 %</td>
			<td style="width:181px;">Sigma-Aldrich</td>
			<td style="width:119px;">S4972</td>
			<td>Purified using an alumina gel preparative column and stored at 4 &#176;C</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:379px;">Acetone, 99.5 %</td>
			<td style="width:181px;">Sigma-Aldrich</td>
			<td align="right" style="width:119px;">179124</td>
			<td>Technical grade can also be used</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:379px;">Tetrahydrofuran, 99.9 % (THF)</td>
			<td style="width:181px;">Sigma-Aldrich</td>
			<td align="right" style="width:119px;">494461</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:379px;">Dichloromethane, 99.5 %</td>
			<td style="width:181px;">Sigma-Aldrich</td>
			<td align="right" style="width:119px;">443484</td>
			<td>Highly toxic</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:379px;">Hydrochloric acid, 37 %</td>
			<td style="width:181px;">Sigma-Aldrich</td>
			<td align="right" style="width:119px;">435570</td>
			<td>Harmful fumes</td>
		</tr>
	</tbody>
</table>

grafting multiwalled carbon nanotubes with polystyrene to enable self-assembly and anisotropic patchiness

We demonstrate a straightforward protocol to graft pristine multiwalled carbon nanotubes (MWCNTs) with polystyrene (PS) chains at the sidewalls through a free-radical polymerization strategy to enable the modulation of the nanotube surface properties and produce supramolecular self-assembly of the nanostructures. First, a selective hydroxylation of the pristine nanotubes through a biphasic catalytically mediated oxidation reaction creates superficially distributed reactive sites at the sidewalls. The latter reactive sites are subsequently modified with methacrylic moieties using a silylated methacrylic precursor to create polymerizable sites. Those polymerizable groups can address further polymerization of styrene to produce a hybrid nanomaterial containing PS chains grafted to the nanotube sidewalls. The polymer-graft content, amount of silylated methacrylic moieties introduced and hydroxylation modification of the nanotubes are identified and quantified by Thermogravimetric Analysis (TGA). The presence of reactive functional groups hydroxyl and silylated methacrylate are confirmed by Fourier Transform Infrared Spectroscopy (FT-IR). Polystyrene-grafted carbon nanotube solutions in tetrahydrofuran (THF) provide wall-to-wall collinearly self-assembled nanotubes when cast samples are analyzed by transmission electron microscopy (TEM). Those self-assemblies are not obtained when suitable blanks are similarly cast from analogous solutions containing non-grafted counterparts. Therefore, this method enables the modification of the nanotube anisotropic patchiness at the sidewalls which results into spontaneous auto-organization at the nanoscale.

TGA data were collected from pristine nanotubes, hydroxylated nanotubes, nanotubes modified with silylated methacrylic moieties and polystyrene-grafted nanotubes (Figure 1). FT-IR results were collected from hydroxylated nanotubes and nanotubes modified with silylated methacrylic moieties (Figure 2). TEM images were collected from pristine nanotubes and polystyrene-grafted nanotubes (Figure 3). TGA d...

Watch this Scientific Journal Video about Grafting Multiwalled Carbon Nanotubes with Polystyrene to Enable Self-Assembly and Anisotropic Patchiness at JoVE.com

Grafting Multiwalled Carbon Nanotubes with Polystyrene to Enable Self-Assembly and Anisotropic Patchiness

A procedure for the synthesis of polystyrene-grafted multiwalled carbon nanotubes using successive chemical modification steps to selectively introduce the polymer chains to the sidewalls and their self-assembly via anisotropic patchiness is presented.

We demonstrate a straightforward protocol to graft pristine multiwalled carbon nanotubes (MWCNTs) with polystyrene (PS) chains at the sidewalls through a ...

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