Name: synthesis of ligand-free cds nanoparticles within a sulfur copolymer matrix
Uploaded: 2016-05-01T15:00:00
Description: Watch this Scientific Journal Video about Synthesis of Ligand-free CdS Nanoparticles within a Sulfur Copolymer Matrix at JoVE.com

The authors would like to acknowledge the State of Washington for supporting this research through the University of Washington Clean Energy Institute Exploratory Fellowship Program, and National Science Foundation (NSF) Sustainable Energy Pathway (SEP) Award CHE-1230615.

Caution: Cadmium precursors are highly toxic and must be handled with great care. Wear proper protective equipment, use appropriate engineering controls and consult relevant materials safety data sheets (MSDS). In addition, the formation of nanoparticles may present additional hazards. The reactions described herein are conducted with a standard vacuum gas manifold, in order to conduct the experiments within an inert atmosphere. All chemicals were purchased commercially and used as received. This protocol is based upon a previously developed...

<ol>
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We have developed a method to synthesize CdS nanoparticles within a sulfur copolymer matrix. This sulfur copolymer is composed of elemental sulfur and methylstyrene.5 An important feature of this method is that the copolymer can be used as both a high-temperature solvent and a sulfur source that reacts with a cadmium precursor to produce CdS nanoparticles in solution.5 The critical step in the procedure is the synthesis of the sulfur copolymer with a suitable ratio of methylstyrene and sulfur. The u...

Although proven useful for synthesis, conventional aliphatic ligands present a number of challenges for the implementation of nanoparticles in photonic and electrochemical devices. Aliphatic ligands are highly insulating, hydrophobic, and constitute a significant barrier to electrochemical surface reactions.1 Accordingly, several studies have developed ligand exchange and ligand stripping protocols that replace these aliphatic ligands with functional moieties or that strip away the ligands to reveal a bare nanoparticle surface.1-3 These reactions, however, pose several intrinsic problems. They significantly add to the complexity of the synthetic process, do not always go to completion, and can deteriorate the surface of the nanoparticles, which can in turn impose significant problems during device fabrication when using these techniques.4
We have developed a sulfur copolymer that can be used as both a high temperature solvent and sulfur source during the synthesis of CdS nanoparticles.5 This copolymer is based on a network copolymer developed by Chung et al. that uses elemental sulfur and 1,3-diisopropenylbenzene (DIB).6 In our case, a methylstyrene monomer is implemented instead of DIB. The methylstyrene monomer limits cross-linking reactions, which would otherwise produce a high molecular weight network copolymer.5,6 The presence of only one vinylic functional group on the methylstyrene monomer promotes the formation of oligomeric radicals once heated, which allows the sulfur copolymer to operate as a liquid solvent and sulfur source in parallel during the nanoparticle synthesis.5 Specifically, the sulfur polymer is produced by heating elemental sulfur to 150 &#176;C, which causes the S8 rings to transition into a linearly structured liquid sulfur diradical form. Next, methylstyrene is injected into the liquid sulfur in a 1:50 molar ratio of methylstyrene molecules to sulfur atoms.5 The methylstyrene double bond reacts with the sulfur chains to produce the copolymer, as presented in Figure 1.5 The sulfur copolymer is then cooled and the cadmium precursor is added. This mixture is then reheated to 200 &#176;C, during which, the sulfur copolymer melts and the nanoparticle nucleation and growth processes are initiated within the solution.5 A 20:1 molar ratio of sulfur to cadmium precursor is used, so that only some of the sulfur is consumed during the reaction.5 This copolymer stabilizes the nanoparticles by suspending them within a solid polymer matrix once the reaction has been terminated.5 The copolymer can be removed after the synthesis, resulting in the production of CdS nanoparticles that do not have organic coordinating ligands, as depicted in Figure 2.5
The synthetic method presented in this work is relatively simple in comparison with other methods presented in the literature.1-3,7 It is applicable for a diverse range of applications where traditional ligated nanoparticles have proven problematic or undesirable. This technique can open doors to higher throughput testing, where one batch of nanoparticles can be used to examine a complete spectrum of subsequent functionalizations without the need for complex and time consuming ligand stripping or exchange procedures.2,4,8,9 These unligated nanoparticles also offer opportunities to reduce the number of carbon defects commonly observed in printed nanoparticle devices, by eliminating the carbon source.10-16 This detailed protocol is intended to help others implement this new method and to help spur its active use in a variety of fields that will find it of particular significance.

<table>
	<tbody>
		<tr>
			<td>Sulfur (S8), 99.5%</td>
			<td>Sigma Aldrich</td>
			<td>84683</td>
			<td></td>
		</tr>
		<tr>
			<td>&#945;-methylstyrene, 99%</td>
			<td>Sigma Aldrich</td>
			<td>M80903</td>
			<td></td>
		</tr>
		<tr>
			<td>Cadmium acetylacetonate (Cd(acac)), 99.9%</td>
			<td>Sigma Aldrich</td>
			<td>517585</td>
			<td>Highly Toxic</td>
		</tr>
		<tr>
			<td>Chloroform (CHCl3), 99.5%</td>
			<td>Sigma Aldrich</td>
			<td>C2432</td>
			<td></td>
		</tr>
		<tr>
			<td>Hotplate / magnetic stirrer</td>
			<td>IKA RCT&#160;</td>
			<td>3810001</td>
			<td></td>
		</tr>
		<tr>
			<td>Temperature controller with probe and heating mantle</td>
			<td>Oakton Temp 9000</td>
			<td>WD-89800</td>
			<td></td>
		</tr>
		<tr>
			<td>Centrifuge</td>
			<td>Beckman Coulter Allegra X-22</td>
			<td>392186</td>
			<td></td>
		</tr>
		<tr>
			<td>Centrifuge Tubes</td>
			<td>Thermo Scientific</td>
			<td>3114</td>
			<td>Teflon for resistance to chlorinated solvents</td>
		</tr>
		<tr>
			<td>TEM with attached EDS detector</td>
			<td>FEI Tecnai G2 F-20 with EDAX detector</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>TEM Sample Grid</td>
			<td>Ted Pella</td>
			<td>1824</td>
			<td>Ultrathin carbon film substrate with holey carbon support films on a 400 mesh copper grid</td>
		</tr>
		<tr>
			<td>XRD</td>
			<td>Bruker F-8 Focus Diffractometer</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Molybdenum coated soda lime glass substrates</td>
			<td></td>
			<td></td>
			<td>750 nm thick sputtered molybdenum layer</td>
		</tr>
		<tr>
			<td>Quartz Fluorescence Cuvettes</td>
			<td>Sigma Aldrich</td>
			<td>Z803073</td>
			<td>10 mm by 10 mm, 4 polished sides with screw top</td>
		</tr>
		<tr>
			<td>UV-Vis-NIR</td>
			<td>Perkin Elmer Lambda 1050 Spectrometer</td>
			<td></td>
			<td>With 3D WB Detector Module</td>
		</tr>
		<tr>
			<td>PL</td>
			<td>Horiba FL3-21tau Fluorescence Spectrophotometer</td>
			<td></td>
			<td></td>
		</tr>
	</tbody>
</table>

synthesis of ligand-free cds nanoparticles within a sulfur copolymer matrix

Aliphatic ligands are typically used during the synthesis of nanoparticles to help mediate their growth in addition to operating as high-temperature solvents. These coordinating ligands help solubilize and stabilize the nanoparticles while in solution, and can influence the resulting size and reactivity of the nanoparticles during their formation. Despite the ubiquity of using ligands during synthesis, the presence of aliphatic ligands on the nanoparticle surface can result in a number of problems during the end use of the nanoparticles, necessitating further ligand stripping or ligand exchange procedures. We have developed a way to synthesize cadmium sulfide (CdS) nanoparticles using a unique sulfur copolymer. This sulfur copolymer is primarily composed of elemental sulfur, which is a cheap and abundant material. The sulfur copolymer has the advantages of operating both as a high temperature solvent and as a sulfur source, which can react with a cadmium precursor during nanoparticle synthesis, resulting in the generation of ligand free CdS. During the reaction, only some of the copolymer is consumed to produce CdS, while the rest remains in the polymeric state, thereby producing a nanocomposite material. Once the reaction is finished, the copolymer stabilizes the nanoparticles within a solid polymeric matrix. The copolymer can then be removed before the nanoparticles are used, which produces nanoparticles that do not have organic coordinating ligands. This nascent synthesis technique presents a method to produce metal-sulfide nanoparticles for a wide variety of applications where the presence of organic ligands is not desired.

The TEM image in Figure 3a shows small CdS nanoparticles (3-4 nm) that have nucleated within the sulfur copolymer before the sulfur copolymer has been completely removed. The image in Figure 3a was acquired by taking an aliquot of the nanoparticle solution immediately after the solution reached 200 &#176;C. Figure 3b shows larger nanoparticles (7-10 nm) that have grown in solution for 30 min before the sulfur copolymer has been completely removed. Figure 3c</stro...

Watch this Scientific Journal Video about Synthesis of Ligand-free CdS Nanoparticles within a Sulfur Copolymer Matrix at JoVE.com

Synthesis of Ligand-free CdS Nanoparticles within a Sulfur Copolymer Matrix

Herein we present a method to synthesize ligand-free cadmium sulfide (CdS) nanoparticles based on a unique sulfur copolymer. The sulfur copolymer operates as a high temperature solvent and a sulfur source during the nanoparticle synthesis and stabilizes the nanoparticles after the reaction.

Aliphatic ligands are typically used during the synthesis of nanoparticles to help mediate their growth in addition to operating as high-temperature ...

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