Name: photochemical oxidative growth of iridium oxide nanoparticles on cdse@cds nanorods
Uploaded: 2016-02-11T15:00:00
Description: Watch this Scientific Journal Video about Photochemical Oxidative Growth of Iridium Oxide Nanoparticles on CdSe@CdS Nanorods at JoVE.com

This research was supported by the I-CORE Program of the Planning and Budgeting Committee and The Israel Science Foundation (Grant No. 152/11). We thank the Schulich Faculty of Chemistry and the Technion - Israel Institute of Technology for the renovated laboratory and startup package. We also thank the Royal Society of Chemistry for permission in adapting materials from http://dx.doi.org/10.1039/C4TA06164K for use in this manuscript. Dr. Kalisman thanks the Schulich postdoctoral fellowship for their support. We thank Dr. Yaron Kauffmann for his assistance with HR-TEM and HAADF as well as Dr. Kamira Weinfeld for her assistance with XPS characterization.

1. Synthesis of Quantum Dots21
<ol>
	<li>Preparation of TOP:Se Precursor
	<ol>
		<li>Combine 58 mg of Se powder with 0.360 g of Tri-n-octylphosphine (TOP) in a vial with a septum.</li>
		<li>Sonicate the TOP:Se mixture until it is clear with no solids.</li>
	</ol>
	</li>
	<li>Synthesis of CdSe
	<ol>
		<li>Combine 3.0 g trioctylphosphine oxide (TOPO), 280 mg n-octadecylphosphonic acid (ODPA), and 60 mg CdO with a 3 mm x 8 mm cylindrical stir bar in a 25 ml 3-neck round bottom flask equipped with a thermocoupl...

<ol>
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The synthesis of CdSe seeds and CdSe@CdS seeded rods has been well studied21,24,25. Slight modifications to the amounts, temperatures, and times for steps of the synthesis of these substrate particles can be used to tune their length, diameter, and/or morphology. The synthetic protocol described herein yields highly photoluminescent seeded-rods of uniform dimensions.
The ligand exchange procedure allows for the use of seeded rods in polar environments, in this case water. At the fin...

Photocatalysis presents an attractive and promising solution for renewable energy generation and other environmental applications such as water treatment and air purification1-3. Overall water splitting, driven by solar energy, could be a source of clean and renewable hydrogen fuel; however, despite decades of research, systems that are sufficiently stable and efficient for practical use have not yet been realized.
Both photodeposition and semiconductor-mediated photocatalysis rely on the same mechanism of separating photo-generated electron-hole pairs and driving them to the surface where they can initiate redox reactions. The similarities between these two processes make photodeposition an attractive synthetic tool for the field of photocatalysis4-6. This method is expected to take photocatalyst production to new and unexplored frontiers. It might potentially offer pristine control over the spatial arrangement of the different components in a heterostructures, and advance the ability to construct sophisticated nanoparticle systems. Ultimately the method will bring us one step closer to realizing an efficient photocatalyst for direct solar-to-fuel energy conversion.
We investigated the growth of IrO2 as a co-catalyst, as it is known to be an efficient catalyst for water oxidation7-11. A tunable structure of quantum dot (CdSe) embedded in a rod (cadmium sulfide)12,13 was used as our photocatalyst substrate14,15. It is currently undetermined whether the oxidative pathway occurs via a mediated pathway, or by a direct hole attack. Here, our knowledge and control over the photogenerated holes in the semiconductor heterostructure can be harnessed for a mechanistic study of oxidation reactions. This is made possible by the substrate architecture, which facilitates localization of confined holes16,17 and formation of a distinct oxidation reaction site on the rod. The use of nanoscale materials with localized charge carrier can be exploited for mechanistic studies of redox reactions by simple examination of the products. In this way photodeposition can be used as a unique probe of both reduction and oxidation reaction pathways. This is one example of the new and exciting possibilities afforded by the combination of photodeposition and cutting edge colloidal synthesis18-20.
The quest to develop an efficient photocatalyst for water splitting and renewable energy conversion has become an important thrust within the materials community. This has spurred worldwide interest in CdS, which is known to be highly active for hydrogen production, though it is hampered by photochemical instability. Our work here treats the Achilles heel of the material. IrO2 decorated CdSe@CdS rods demonstrate remarkable photochemical stability under prolonged illumination in pure water.

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	<tbody>
		<tr height="21">
			<td height="21" style="height:21px;width:304px;">Sulfur (S)</td>
			<td style="width:79px;">Sigma</td>
			<td style="width:119px;">84683</td>
			<td style="width:321px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Selenium (Se)</td>
			<td>Sigma</td>
			<td>229865</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Cadmium Oxide (CdO)</td>
			<td>Sigma</td>
			<td>202894</td>
			<td>Highly Toxic</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">n-Octadecylphosphonic acid (ODPA)</td>
			<td>Sigma</td>
			<td>715166</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Propylphosphonic acid (PPA)</td>
			<td>Sigma</td>
			<td>305685</td>
			<td>Highly regulated in some countries and regions</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Butylphosphonic acid (BPA)</td>
			<td>Sigma</td>
			<td>737933</td>
			<td>Alternative to PPA</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Hexylphosphonic acid (HPA)</td>
			<td>Sigma</td>
			<td>750034</td>
			<td>Alternative to PPA</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Trioctylphosphonic oxide (TOPO)</td>
			<td>Sigma</td>
			<td>346187</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Tri-n-octylphosphine, 97% (TOP)</td>
			<td>Sigma</td>
			<td>718165</td>
			<td>Air sensitive</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Spectrochemical Stirbar</td>
			<td>Sigma</td>
			<td><a href="http://www.sigmaaldrich.com/catalog/product/sigma/z363545?lang=en&amp;region=US">Z363545</a></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Sodium Hydroxide</td>
			<td>Sigma</td>
			<td>S5881</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Methanol</td>
			<td>Sigma</td>
			<td>322415</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Toluene</td>
			<td>Sigma</td>
			<td>244511</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Hexane</td>
			<td>Sigma</td>
			<td>296090</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Octylamine</td>
			<td>Sigma</td>
			<td>74988</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Nonanoic Acid</td>
			<td>Sigma</td>
			<td>N5502</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Isopropanol</td>
			<td>Sigma</td>
			<td>278475</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Mercaptoundecanoic Acid (MUA)</td>
			<td>Sigma</td>
			<td>674427</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Tetramethylammonium Hydroxide (TMAH)</td>
			<td>Sigma</td>
			<td>T7505</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Apiezon H Grease (high temperature grease)</td>
			<td>Sigma</td>
			<td>Z273562</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Sodium Persulfate</td>
			<td>Sigma</td>
			<td>216232</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Sodium Nitrate</td>
			<td>Sigma</td>
			<td>229938</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Sodium Hexachloroiridate(III) hydrate</td>
			<td>Sigma</td>
			<td>288160</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Mounted 455nm LED</td>
			<td>Thorlabs</td>
			<td>M455L3</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Cuvette Holder</td>
			<td>Thorlabs</td>
			<td>CVH100</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">25mL 3-neck Round Bottom Flask</td>
			<td>Chemglass</td>
			<td>CG-1524-A-02</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Liebig Condensor</td>
			<td>Chemglass</td>
			<td>CG-1218-A-20</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">T-Joint Adapter</td>
			<td>Chemglass</td>
			<td>AF-0509-10</td>
			<td></td>
		</tr>
	</tbody>
</table>

photochemical oxidative growth of iridium oxide nanoparticles on cdse@cds nanorods

We demonstrate a procedure for the photochemical oxidative growth of iridium oxide catalysts on the surface of seeded cadmium selenide-cadmium sulfide (CdSe@CdS) nanorod photocatalysts. Seeded rods are grown using a colloidal hot-injection method and then moved to an aqueous medium by ligand exchange. CdSe@CdS nanorods, an iridium precursor and other salts are mixed and illuminated. The deposition process is initiated by absorption of photons by the semiconductor particle, which results with formation of charge carriers that are used to promote redox reactions. To insure photochemical oxidative growth we used an electron scavenger. The photogenerated holes oxidize the iridium precursor, apparently in a mediated oxidative pathway. This results in the growth of high quality crystalline iridium oxide particles, ranging from 0.5 nm to about 3 nm, along the surface of the rod. Iridium oxide grown on CdSe@CdS heterostructures was studied by a variety of characterization methods, in order to evaluate its characteristics and quality. We explored means for control over particle size, crystallinity, deposition location on the CdS rod, and composition. Illumination time and excitation wavelength were found to be key parameters for such control. The influence of different growth conditions and the characterization of these heterostructures are described alongside a detailed description of their synthesis. Of significance is the fact that the addition of iridium oxide afforded the rods astounding photochemical stability under prolonged illumination in pure water (alleviating the requirement for hole scavengers).

Transmission electron micrographs (TEM) were collected in order to see the distribution of iridium oxide on the seeded rods (Figure 1). TEM samples were prepared by pipetting a drop of dissolved particles onto a TEM grid. X-ray diffraction (XRD, Figure 2) and X-ray photoelectron spectra (XPS, Figure 3) were used to characterize the observed growth as a mix of crystalline IrO2 and Ir2O3. Preparation of XRD ...

Watch this Scientific Journal Video about Photochemical Oxidative Growth of Iridium Oxide Nanoparticles on CdSe@CdS Nanorods at JoVE.com

Photochemical Oxidative Growth of Iridium Oxide Nanoparticles on CdSe@CdS Nanorods

A protocol for the photochemical oxidative growth of small crystalline iridium oxide nanoparticles on the surface of CdSe@CdS seeded rod nanoparticles is presented.

We demonstrate a procedure for the photochemical oxidative growth of iridium oxide catalysts on the surface of seeded cadmium selenide-cadmium sulfide ...

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Molten-Salt Synthesis of Complex Metal Oxide Nanoparticles

The development of feasible synthesis methods is critical for the successful exploration of novel properties and potential applications of nanomaterials. ...

Growth of Gold Dendritic Nanoforests on Titanium Nitride-coated Silicon Substrates

In this study, a high-power impulse magnetron sputtering system is used to coat a flat and firm titanium nitride (TiN) film on silicon (Si) wafers, and a ...