Name: synthesis and characterization of supramolecular colloids
Uploaded: 2016-04-22T14:00:00
Description: Watch this Scientific Journal Video about Synthesis and Characterization of Supramolecular Colloids at JoVE.com

Forfatterne erkender Holland Organisation for Videnskabelig forskning (NWO ECHO-STIP Grant 717.013.005, NWO VIDI Grant 723.014.006) til finansiel støtte.

1. Syntese af Core-shell Silica Partikler Bemærk: Silicapartikler syntetiseres ifølge den følgende procedure, som er baseret på den Stöber metoden 24,25. <ol><li> Syntese af fluorescerende silica frø <ol><li> Opløs 105 mg (0,27 mmol) af fluorescein-isothiocyanat i 5 ml ethanol. </li><li> Tilsættes 100 pi (3-aminopropyl) triethoxysilan (APTES, 0,43 mmol) til den foregående opløsning. </li><li> Sonikeres opløsningen under 5 min og lad d...

<ol>
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B. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Magnetic+assembly+of+colloidal+superstructures+with+multipole+symmetry.">Magnetic assembly of colloidal superstructures with multipole symmetry.</a> Nature. 457 (7232), 999-1002 (2009).</li><li>Vutukuri, H. R., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Colloidal+analogues+of+charged+and+uncharged+polymer+chains+with+tunable+stiffness.">Colloidal analogues of charged and uncharged polymer chains with tunable stiffness.</a> Angew. Chem. Int. Edit. 51 (45), 11249-11253 (2012).</li><li>De Greef, T. F. A., Meijer, E. 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Når cyclohexan, med et brydningsindeks på 1,426, anvendes som et opløsningsmiddel til at dispergere BTA-kolloider, van der Waals interaktioner er meget svage, eftersom brydningsindekserne af kolloider og opløsningsmiddel er næsten de samme. Bemærk, at koncentrationen af ​​funktionaliserede kolloider anvendes til de SLS eksperimenter i cyclohexan er meget højere sammenlignet med de nøgne silica kolloider i vand. Dette er nødvendigt for at opnå en tilstrækkelig stærk spredning på grund af den lave kontras...

Mesostructured kolloide materialer finder udbredt anvendelse inden for videnskab og teknologi, som modelsystemer for grundlæggende undersøgelser af atomare og molekylære materialer 1,2, som fotoniske materialer 3,4, som lægemiddelafgivelsessystemer 5,6, som belægninger 7 og i litografi til overfladen mønster 8,9. Da lyofobe kolloider er metastabile materialer, der i sidste ende aggregerer irreversibelt på grund af de allestedsnærværende van der Waals interaktioner, deres manipulation i specifikke mål strukturer er notorisk vanskeligt. Talrige strategier er blevet udviklet til at styre kolloid selvsamling herunder brug af tilsætningsstoffer til at tune de elektrostatiske 10,11 eller udtynding interaktioner 12,13 eller eksterne triggere såsom magnetiske 14 eller elektriske 15 felter. En sofistikeret alternativ strategi for at opnå kontrol over struktur, dynamik og mekanik disse systemer er deres funktionalisering with molekyler interagerer gennem specifikke og retningsbestemte kræfter. Supramolekylær kemi tilbyder en omfattende værktøjskasse af små molekyler udviser stedspecifikke, retningsbestemt og stærke alligevel reversible interaktioner, som kan moduleres i styrke ved solvent polaritet, temperatur og lys 16. Siden deres egenskaber er blevet undersøgt grundigt i bulk og i opløsning, disse molekyler er attraktive kandidater til at strukturere bløde materialer i eksotiske faser på en forudsigelig måde. På trods af den klart potentiale for en sådan en integreret tilgang til orkestrere kolloid samling via supramolekylær kemi, har disse discipliner sjældent grænseflader til skræddersy egenskaber mesostructured kolloide materialer 17,18. En solid platform af supramolekylære kolloider skal opfylde tre vigtigste krav. For det første bør kobling af den supramolekylære delen ske under milde-betingelser for at forhindre nedbrydning. For det andet, overflade kræfter separator;ons større end direkte kontakt bør være domineret af de tøjrede motiver, hvilket betyder, at ikke-coatede kolloider næsten udelukkende skal interagere via udelukket volumen interaktioner. Derfor bør de fysisk-kemiske egenskaber af kolloiderne skræddersys til at undertrykke andre interaktioner forbundet med kolloide systemer, såsom van der Waals eller elektrostatiske kræfter. For det tredje bør karakterisering give mulighed for en entydig tildeling af samlingen til tilstedeværelsen af ​​de supramolekylære dele. For at opfylde disse tre forudsætninger blev en robust to-trins syntese af supramolekylære kolloider udviklet (figur 1a). I et første skridt, hydrofobe NVOC-funktionaliserede silica partikler er forberedt til spredning i cyclohexan. Den NVOC-gruppen kan let spaltes, hvilket gav amin-funktionaliserede partikler. Den høje reaktivitet af aminer muliggør enkel post-funktionalisering med den ønskede supramolekylære del ved anvendelse af en bred vifte af milde reaktionsbetingelser. Heri vi PRepare supramolekylære kolloider ved funktionalisering af silicaperler med stearylalkohol og en benzen-1,3,5-tricarboxamide (BTA) derivat 20. Den stearylalkohol spiller flere vigtige roller: det gør kolloider organofile og den indfører kortrækkende steriske repulsioner som hjælper til at reducere uspecifik vekselvirkning mellem kolloider 21,22. van der Waals kræfter reduceres yderligere på grund af den tætte match mellem brydningsindekset af kolloider og 23 opløsningsmiddel. Light-og termoresponsiv kortrækkende attraktive overflade kræfter genereres ved inkorporering af o-nitrobenzyl beskyttet BTA 20. O nitrobenzyl del er en foto-spaltelige gruppe, der blokerer for dannelsen af hydrogenbindinger mellem tilstødende BTA, når de indgår på amider i discotics (figur 1b). Ved fotospaltning med UV-lys, BTA i opløsning er i stand til at genkende og interagere med identiske BTA molekyler gennem en 3 gange hydrogen bond array, med en bindingsstyrke, som er stærkt temperaturafhængig 17. Da van der Waals seværdigheder er minimale for stearyl- coatede silicapartikler i cyclohexan samt lys- og temperatur-uafhængig, skal den observerede stimuli-responsive kolloid samling være BTA-medieret. Denne detaljerede video viser, hvordan at syntetisere og karakterisere supramolekylære kolloider og hvordan man studerer deres selv-samling ved UV-bestråling ved konfokal mikroskopi. Hertil kommer, at en simpel billedanalyse protokol skelne kolloide slåbrokker fra grupperede kolloider og at bestemme mængden af ​​kolloider pr klynger er rapporteret. Alsidigheden af ​​den syntetiske strategi tillader let variere partikelstørrelse, overfladedækning samt den indførte bindingsenhed, der åbner nye muligheder for udvikling af en stor familie af kolloide byggesten til mesostructured avancerede materialer.

<table border="0" cellpadding="0" cellspacing="0" width="1805">
	<tbody>
		<tr height="21">
			<td height="21" style="height:21px;width:524px;">APTES</td>
			<td style="width:128px;">Sigma-Aldrich</td>
			<td style="width:119px;"></td>
			<td style="width:1035px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:524px;">FTIC</td>
			<td style="width:128px;">Sigma-Aldrich</td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:524px;">TEOS</td>
			<td style="width:128px;">Sigma-Aldrich</td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:524px;">LUDOX AS-40</td>
			<td style="width:128px;">Sigma-Aldrich</td>
			<td style="width:119px;"></td>
			<td>Silica particles of 13 nm in radius</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:524px;">MilliQ</td>
			<td style="width:128px;">---</td>
			<td style="width:119px;">---</td>
			<td style="width:1035px;">18.2 M&#937;&#183;cm at 25 &#176;C</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:524px;">Ethanol</td>
			<td style="width:128px;">SolvaChrom</td>
			<td style="width:119px;"></td>
			<td style="width:1035px;">---</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:524px;">Ammonia (25% in water)</td>
			<td style="width:128px;">Sigma-Aldrich</td>
			<td style="width:119px;"></td>
			<td style="width:1035px;">---</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:524px;">Chloroform</td>
			<td style="width:128px;">SolvaChrom</td>
			<td style="width:119px;"></td>
			<td style="width:1035px;">---</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:524px;">Cyclohexane</td>
			<td style="width:128px;">Sigma-Aldrich</td>
			<td style="width:119px;"></td>
			<td style="width:1035px;">---</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:524px;">Dimethylformamide (DMF)</td>
			<td style="width:128px;">Sigma-Aldrich</td>
			<td style="width:119px;"></td>
			<td style="width:1035px;">---</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:524px;">Stearyl alcohol</td>
			<td style="width:128px;">Sigma-Aldrich</td>
			<td style="width:119px;"></td>
			<td style="width:1035px;">---</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">N,N-Diisopropylethylamine (DIPEA)</td>
			<td style="width:128px;">Sigma-Aldrich</td>
			<td style="width:119px;"></td>
			<td style="width:1035px;">---</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Benzotriazol-1-yl-oxytripyrrolidinophosphonium hexafluorophosphate (PyBOP)</td>
			<td style="width:128px;">Sigma-Aldrich</td>
			<td style="width:119px;"></td>
			<td style="width:1035px;">---</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Succinimidyl 3-(2-pyridyldithio)propionate (SPDP)</td>
			<td style="width:128px;">Sigma-Aldrich</td>
			<td style="width:119px;"></td>
			<td style="width:1035px;">---</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Dithiothreitol (DTT)&#160;</td>
			<td style="width:128px;">Sigma-Aldrich</td>
			<td style="width:119px;"></td>
			<td style="width:1035px;">---</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:524px;">NVOC-C11-OH</td>
			<td style="width:128px;">Synthesized</td>
			<td style="width:119px;">---</td>
			<td style="width:1035px;">I. de Feijter, 2014 Responsive materials from adaptive supramolecular constructs, Doctoral thesis, Technical University of Eindhoven, The Netherlands</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:524px;">BTA</td>
			<td style="width:128px;">Synthesized</td>
			<td style="width:119px;">---</td>
			<td style="width:1035px;">I. de Feijter, 2014 Responsive materials from adaptive supramolecular constructs, Doctoral thesis, Technical University of Eindhoven, The Netherlands</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:524px;">Centrifuge</td>
			<td style="width:128px;">Thermo Scientific</td>
			<td style="width:119px;"></td>
			<td>Heraeus Megafuge 1.0</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:524px;">Ultrasound bath</td>
			<td style="width:128px;">VWR</td>
			<td style="width:119px;"></td>
			<td>Ultrasonic cleaner</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Peristaltic pumps</td>
			<td>Harvard Apparatus</td>
			<td></td>
			<td>PHD Ultra Syringe Pump</td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:524px;">UV-oven</td>
			<td style="width:128px;">Luzchem</td>
			<td style="width:119px;"></td>
			<td>LZC-a V UV reactor equipped with 8x8 UVA light bulbs (&#955;max=354 nm)</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:524px;">Stirrer-heating plate</td>
			<td style="width:128px;">Heidolph</td>
			<td style="width:119px;"></td>
			<td>MR-Hei Standard</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:524px;">Light Scattering</td>
			<td style="width:128px;">ALV</td>
			<td style="width:119px;"></td>
			<td>CGS-3 MD-4 compact goniometer system, equipped with a Multiple Tau digital real time correlator (ALV-7004) and a solid-state laser (&#955;=532 nm, 40 mW)</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">UV-Vis spectrophotometer</td>
			<td style="width:128px;">Thermo Scientific</td>
			<td style="width:119px;"></td>
			<td>NanoDrop 1000 Spectrophotometer</td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;">Confocal microscope</td>
			<td style="width:128px;">Nikon</td>
			<td style="width:119px;"></td>
			<td>Ti Eclipse with an argon laser with &#955;excitation=488 nm</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:524px;">Slide spacers</td>
			<td style="width:128px;">Sigma-Aldrich</td>
			<td style="width:119px;"></td>
			<td>Grace BioLabs Secure seal imaging spacer (1 well, diam. &#215; thickness 13 mm &#215; 0.12 mm)</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:524px;">Syringes</td>
			<td style="width:128px;">BD Plastipak</td>
			<td style="width:119px;"></td>
			<td>20 mL syringe</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:524px;">Plastic tubing</td>
			<td style="width:128px;">SCI</td>
			<td style="width:119px;">BB31695-PE/5</td>
			<td>Ethylene oxide gas sterilizable micro medical tubing</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:524px;">Pulsating vortex mixer</td>
			<td style="width:128px;">VWR</td>
			<td style="width:119px;"></td>
			<td>Electrical: 120V, 50/60Hz, 150W Speed Range: 500&#8211;3000 rpm</td>
		</tr>
	</tbody>
</table>

synthesis and characterization of supramolecular colloids

Control over colloidal assembly is of utmost importance for the development of functional colloidal materials with tailored structural and mechanical properties for applications in photonics, drug delivery and coating technology. Here we present a new family of colloidal building blocks, coined supramolecular colloids, whose self-assembly is controlled through surface-functionalization with a benzene-1,3,5-tricarboxamide (BTA) derived supramolecular moiety. Such BTAs interact via directional, strong, yet reversible hydrogen-bonds with other identical BTAs. Herein, a protocol is presented that describes how to couple these BTAs to colloids and how to quantify the number of coupling sites, which determines the multivalency of the supramolecular colloids. Light scattering measurements show that the refractive index of the colloids is almost matched with that of the solvent, which strongly reduces the van der Waals forces between the colloids. Before photo-activation, the colloids remain well dispersed, as the BTAs are equipped with a photo-labile group that blocks the formation of hydrogen-bonds. Controlled deprotection with UV-light activates the short-range hydrogen-bonds between the BTAs, which triggers the colloidal self-assembly. The evolution from the dispersed state to the clustered state is monitored by confocal microscopy. These results are further quantified by image analysis with simple routines using ImageJ and Matlab. This merger of supramolecular chemistry and colloidal science offers a direct route towards light- and thermo-responsive colloidal assembly encoded in the surface-grafted monolayer.

I betragtning af, at de to-trins procedure, der anvendes til at syntetisere de supramolekylære kolloider (figur 1a), kobler BTA- derivater (figur 1b) i et andet trin ved stuetemperatur og i mild-reaktionsbetingelser, er dens stabilitet sikres. <img alt="figur 1" src="/files/ftp_upload/53934/53934fig1.jpg" /> Figur 1. Scheme af syntesen af supramolekylære kolloider. A) K...

Watch this Scientific Journal Video about Synthesis and Characterization of Supramolecular Colloids at JoVE.com

Synthesis and Characterization of Supramolecular Colloids

A protocol for the synthesis and characterization of colloids coated with supramolecular moieties is described. These supramolecular colloids undergo self-assembly upon the activation of the hydrogen-bonds between the surface-anchored molecules by UV-light.

Syntese og karakterisering af supramolekylære Colloids

Control over colloidal assembly is of utmost importance for the development of functional colloidal materials with tailored structural and mechanical ...

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