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

Vi skulle vilja erkänna de FQ-PAIP och DGAPA-PAPIIT program från National Autonomous University of Mexico (grant nummer 5000-9158, 5000-9156, IA205616 och IA205316) och nationella rådet för vetenskap och teknik från Mexiko - CONACYT-(bevilja nummer 251533).

Varning: Läs alla relevanta säkerhetsdatablad (MSDS) före användning. Flera av de kemikalier som används i detta protokoll är akut giftigt och cancerframkallande. Carbon nanotube derivat kan ha ytterligare luftvägarna risker jämfört med andra traditionella bulk kol allotropes. Det misstänks att kolnanorör i aerosol kan påverka lungorna på ett liknande sätt än asbest, men deras cancerframkallande egenskaper inte har helt klarlagts hittills. Använd alla lämpliga säkerhetsrutiner när du utför den kemiska...

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I denna metod finns det vissa steg som leder kritiska att garantera en lyckad ympning process. Först, den bifasisk katalytiskt medierad oxidationsreaktionen (steg 1.1) utföras med nyligen spridda kolnanorör (steg 1.1.1.5). Om spridning leder olönsamma enligt rekommendationerna i protokollet, skulle användning av en ultraljud tips någon sonikator vara bra om använder samma indikationer (steg 1.1.1.6). Med kortare MWCNTs kan också hjälpa lösa dispersion problem. Andra är inställningen av dammsugarfilter systeme...

Sedan upptäckten av singel-walled kolnanorör (SWCNTs),1,2 forskarsamfund har tillämpat sina enastående elektriska, mekaniska och termiska egenskaper3 i ett brett utbud av banbrytande program genom att modulera deras ytegenskaper via kovalenta4 och icke-kovalenta5 strategier. Exempel på dessa program är deras användning som givare i sensorer,6,7 elektroder i solceller,8 heterogena stöder i katalys,9 nanoreactors i syntesen,10 antifouling agenter i skyddande filmar,11 fyllmedel i kompositmaterial,12etc. Dock har möjlighet att modulera en ytegenskaper av deras mer robust, men ändå industriellt tillgängliga multiwalled motsvarigheter nämligen MWCNTs, att styra riktningen i sin icke-kovalenta interaktioner på nanonivå, varit en svår uppgift hittills. 13
Supramolekylär självmontering av molekylära byggstenarna är en av de mest mångsidiga strategierna att styra organisationen av material på nanonivå. 14 , 15 i denna mening, Supramolekylära interaktioner involvera directional, korta avstånd och mid-range icke-kovalenta interaktioner såsom H-bond, Van der Waals, dipol-dipol, Jon-dipol, dipol-inducerad dipol, π-π stapling, katjon-π, anjon-π, coulombic, bland andra. 16 tyvärr riktverkan i självmontering för större strukturer såsom MWCNTs är inte spontan och kräver oftast yttre motiv styrkor (t.ex. mallar eller försvinnande energisystem). 17 en senaste rapport används icke-kovalenta inslagning av nanorör med skräddarsydda sampolymerer att fullfölja det sistnämnda målet,18 men användning av kovalent strategier för att erbjuda nya alternativ för att lösa detta problem har förblivit knappt utforskade.
Kemisk modifiering av kolnanorör kan utföras selektivt för att införa olika funktionella grupper antingen till termini eller till sidoväggarna av detsamma. 19 , 20 är en av de mest användbara metoderna att skräddarsy ytegenskaper i kol nanostrukturer polymer-ympning genom standard polymerisation vägar. Dessa metoder omfattar vanligtvis, preliminära införandet av polymerizable eller initieraren grupper (akryl, vinyl, osv.) på nanostruktur ytan och deras efterföljande polymerisation med en lämplig monomer. 21 när det gäller MWCNTs, kovalent införandet av polymern kedjar på sidoväggarna att styra deras flammighet i en Anisotrop mode har varit en utmaning.
Här visar vi hur en serie enkel kemisk modifiering steg22,23 kan tillämpas om du vill infoga PS kedjor på sidoväggarna av MWCNTs för att ändra deras yta flammighet och främja deras Anisotrop självmontering23 på nanonivå. Under sträckan ändring möjliggör ett första steg selektiv hydroxylering av orörda MWCNTs på sidoväggarna genom att följa en bifasisk katalytiskt medierad oxidationsreaktionen för att ge de hydroxylerade motsvarigheterna nämligen MWCNT-OH. Ett andra steg använder 3-(Trimetoxysilyl) propyl form (TMSPMA) att införa silylerad metakrylsyra beståndsdelarna till de tidigare skapade hydroxylgrupperna (MWCNT-O-TMSPMA). Dessa skär ger ytan reaktiva platser under ett tredje steg, när styren monomer är polymeriseras från de metakrylsyra beståndsdelarna således framställning av polymern kedjar ympade till sidoväggarna av nanorör i slutet (dvs 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

Vi visar ett enkelt protokoll för att ympa orörda multiwalled kolnanorör (MWCNTs) med polystyren (PS) kedjor på sidoväggarna genom en fria radikaler polymerisation strategi att aktivera moduleringen av nanotube ytegenskaper och producera supramolekylär självmontering av nanostrukturerna. Först skapar en selektiv hydroxylering av orörda nanorör genom en bifasisk katalytiskt medierad oxidationsreaktionen ytligt distribuerade reaktiva platser på sidoväggarna. De sistnämnda reaktiva platserna modifieras därefter med metakrylsyra beståndsdelarna med en silylerad metakrylsyra föregångare för att skapa polymerizable platser. Dessa polymerizable grupper kan hantera ytterligare polymerisation av styren att producera en hybrid nanomaterial som innehåller PS kedjor ympade till nanotube sidoväggarna. Polymer-graft innehåll, mängd silylerad metakrylsyra beståndsdelarna infördes och hydroxylering modifiering av nanorör identifieras och kvantifieras genom termogravimetrisk analys (TGA). Förekomsten av reaktiva funktionella grupper hydroxyl och silylerad bekräftas av Fourier Transform infraröd spektroskopi (FT-IR). Polystyren-ympade carbon nanotube lösningar i tetrahydrofuran (THF) ger heltäckande collinearly själv monterade nanorör när rösterna prover analyseras av transmissionselektronmikroskopi (TEM). Dessa self-assemblies uppnås inte när lämplig blanks gjuts likaså från liknande lösningar som innehåller icke-ympade motsvarigheter. Denna metod kan därför ändring av den nanotube Anisotrop flammighet på sidoväggarna som leder till spontana auto-organisation på nanonivå.

TGA data samlades in från orörda nanorör, hydroxylerade nanorör, nanorör modifierad med silylerad metakrylsyra beståndsdelarna och polystyren-ympade nanorör (figur 1). FT-IR resultaten samlades från hydroxylerade nanorör och nanorör modifierad med silylerad metakrylsyra beståndsdelarna (figur 2). TEM bilder samlades in från orörda nanorör och polystyren-ympade nanorör (figur 3). TGA dr...

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

Ett förfarande för syntesen av polystyren-ympade multiwalled kolnanorör med successiva kemisk modifiering kliver till selektivt presentera polymern kedjar till sidoväggarna och deras självmontering via Anisotrop flammighet är presenterade.

Ympning Multiwalled kolnanorör med polystyren för självmontering och Anisotrop flammighet

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

The overall goal of this procedure is to offer a straightforward strategy for grafting multiwalled carbon nanotubes by polystyrene chains, which mediates a pro-molecular self-assembly and anisotropic patchiness. This method can help to modulate the surface properties of multiwalled carbon nanotubes, so as to establish improved processing conditions of the same in the field of thermoplastic polymers. The grafting strategy offers a straightforward alternative in processing protocols for carbon nanotubes in order to compatibilize them with industrially relevant, yet challenging polymers, such as polystyrene.In general, the method starts with the traditional hydroxyl groups on the side walls of pristine carbon nanotubes followed by the coupling of silylated methacrylic moieties to the OH groups, and their sequential free radical polymerization with styrene on the inner atmosphere. To find the yield, nanotubes grafted with polystyrene chains. The main advantage of this technique is that it can be easily deployed to mole surface properties of carbon nanotubes.And consequently, promote their anisotropic self assembly, which in turn may facilitate their inclusion in a polymer matrix. This technique opens promising alternatives to improve the supply chain of nanostructure carbon nanotropes in industrial processes, thus allowing for the creation of electrical percolation networks in polymer composites, which could find direct applications in electromagnetic shielding systems, mechanically reinforced parts, and electrically conducting materials under attractive cost-benefit conditions. Dry to 5 grams of pristine multi-walled carbon nanotubes, by introducing them into a vacuum oven at 80 Celsius degrees and 200 millimeters of mercury for 12 hours.Pour the dried carbon nanotubes into a 100 milliliter round-bottom flask. Afterwards, transfer 50 milliliters of dichloromethane, 99 percent, into the flask, and set the mechanical stirring at 60 rpm. This will be the organic phase of a bi-faceted chotilitically mediated reaction.In order to prepare the aqueous phase, dissolve 0.6 grams of tetroaropyl ammonium bromide in five milliliters of distilled water. Add five milliliters of acetic acid and five milliliters of an aqueous solution, containing potassium permanganate, 0.16 molar. Pour the latter solution into the round-bottom flask, already containing the organic phase and agitate vigorously, for example, about 80 rpm at room temperature for 24 hours.After that time, transfer the reaction mixture into a separatory funnel. Then, agrigate around 0.25 milliliters of concentrated hydrochloric acid, 36 percent, and carefully agitate the system and purge. Then, discard the supernatant aqueous phase.Once the aqueous phase was retired, the organic phase can be filtered using a vacuum filtration system as it is further described. Set this topper on base firmly into the neck of the filtered flask. With the small-tip forceps, center out 47 millimeter diameter membrane filter on the support surface.Make sure to use a membrane with a pore size between 0.45 micrometers and 20 micrometers. Smaller pore sizes will easily block, while larger pore sizes will retain lower amounts of filtered nanotubes. Without disturbing the filter, center the flange of the holder on top of the assembly and lock the funnel and base together with a spring clamp.Connect the filtering flask to the vacuum source, pour the sample into the funnel, and apply vacuum to filter the sample. Once the filter solid looks to be dried, wash with methanol 95 percent for at least five times the volume of the filtered solution. Afterward, transfer the solute into a petri dish and let it dry under vacuum for 24 hours at 80 Celsius degrees, at 200 millimeters of mercury.In order to insert polymerizable methacrylic moieties into the hydroxilated carbon nanotube walls, disperse about 2.5 grams of the nanotubes and five grams of hydrochinoin 99 percent, using a 100 milliliters schlenk flask. Then, with the aid of a cannula, carefully add 50 milliliters of Toluene under nitrogen atmosphere, using a vacuum inner gas manifold. Later, put it under vigorous mechanical agitation.Then, incorporate five milliliters of 3-thremethyl silane propel methacrylate 98 percent, and take it to reflux at 100 Celsius degrees for 12 hours. Once the reaction is complete, wash the obtained product with methanol in excess, using the vacuum filtration system and dry it overnight under vacuum at 80 Celsius degrees and 200 millimeters of mercury and store until needed. In order to graft the methacrylic modified nanotubes with acetoground polystyrene chains, disperse about 2.5 grams of the modified carbon nanotubes and 75 milligrams of AIBN in 50 milliliters of toluene.Using a shlenk flask, improach the system with nitrogen atmosphere, using the vacuum inner gas manifold. Then, add freshly purified 7.5 milliliters of styrene monomer. AIBN will act as the initiator of the free-radical polymerization.Subsequently, set the heating system at 70 Celsius degrees and stir it for 12 hours, under nitrogen atmosphere and reflux. Afterwards, filter the reaction mixture using the vacuum filtration system. Wash it with acetone, and finally wash it again with DHF 99 percent for at least five times to remove unbound polystyrene.Dry the product under vacuum for 24 hours at 80 Celsius degrees and 200 millimeters of mercury. The solid will contain carbon nanotubes grafted with polystyrene chains. The polymer grafted carbon nanotubes were characterized by TM.Here are representative TM images for dropcast samples in which polystyrene wraps its carbon nanotubes appear as partially aligned and self-assembled by the side walls.Such behavior is absent when pristine nanotubes are analyzed in a similar form. The values curve of thermogramemetric analysis for polymer-modified carbon nanotubes showed that the first weight loss, due to the loss of polystyrene chains starts at 270 Celsius degrees. Then, a second moderated step, which starts around 400 Celsius degrees, is caused by the loss of the siliyated methracrylic moieties, where as the final remark weight loss starting at around 600 Celsius degrees, corresponds to the carbon nanotubes.Here we show our representative weight loss present-age curve of grafted carbon nanotubes with polyester range in comparison with pristine ones, which confirms that the most significant alteration in the samples weighed is comprised between 270 Celsius degrees and 775 Celsius degrees. From TGA, it is possible to affirm that after the hydroxilation step, carbon nanotube-side walls will typically contain hydroxyl moieties at two percent to five percent in weight. It is important to mention that after co-insulating material moieties to the OH groups, modified carbon nanotubes will typically contain between eight and ten percent weight for methracrylic in comparison with the nanotube content.Once accomplished, the free radical polymerization with styrene, it is typically expected a grafting degree of about 30 to 40 percent relative to the nanotube weight. So, a selective modification of the surface properties of the nanotubes is obtained by successive chemical modification in steps to insert reactive functional robselectively to the side walls. We expect that this strategy can be reapplied to other acrylic or vinyl derivative polymer types and new hybrid materials and composites could arise in the future.After watching this video, you should have a good understanding of the different steps needed to chemically modify carbon nanotubes with acetogram polyester range chains, which might play an important role in the surface properties of that kind of carbon nanotubes via super-molecular forces. This can result in the creation of self-assembly nanotubes through anisotropic nanoscale interactions, with potential applications in wide areas, such as material science and engineering, nanoscience and nanotechnology, or macromolecular chemistry. While attempting this procedure, it is important to be aware of the hazardous conditions of all reactants used in this technique, and ensure the use of suitable laboratory equipment.

Research

JoVE Journal

Chemistry

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