Name: large area substrate-based nanofabrication of controllable and customizable gold nanoparticles via capped dewetting
Uploaded: 2019-02-26T14:30:00
Description: Watch this Scientific Journal Video about Large Area Substrate-Based Nanofabrication of Controllable and Customizable Gold Nanoparticles Via Capped Dewetting at JoVE.com

We acknowledge the support from the Microscopy Core Facility at Utah State University for the SEM result. We also acknowledge the National Science Foundation (Award #162344) for the DC Magnetron Sputtering System, the National Science Foundation (Award #133792) for the (Field Electron and Ion) FEI Quanta 650, and the Department of Energy, Nuclear Energy University Program for the FEI Nova Nanolab 600.

NOTE: The large-area fabrication of controllable and customizable gold nanoparticle films is achieved by following the detailed protocol. The protocol follows three major areas that are (1) substrate preparation, (2) dewetting and etching, and (3) characterization.
1. Substrate Preparation
<ol>
	<li>Clean the substrate (100 nm SiO2 on Si) using an acetone rinse followed by an isopropyl alcohol rinse and then dry using a stream of N2 gas.</li>
	<li>Load the substrate int...

<ol>
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The protocol is a feasible and easy process for a nano-manufacturing process for producing nanoparticles on a substrate over large areas with controllable characteristics. The dewetting phenomenon, which leads to the production of particles, is based on the tendency of the dewetted layer to achieve minimum surface energy. The control over the size and shape of the particles is targeted with the deposition of a second surface on the main layer to tune the surface energies, and the final equilibrium between the adhesion an...

Large-area nanoparticle film fabrication is critically important for the adoption of recent technological advances in solar energy conversion and high-density data storage with the use of plasmonic nanoparticles1,2,3,4,5. Interestingly, it is the magnetic properties of some of these plasmonic nanoparticles, which provide these nanoparticles with the ability to manipulate and control light at the nanoscale. This controllability of light provides the possibility to enhance light entrapment of the incident light at the nanoscale and increase the absorptivity of the surface. Based on these same properties and having the ability to have nanoparticles in either a magnetized and a non-magnetized state, scientists are also defining a new platform for high-density digital data storage. In each of these applications, it is critical that a large area and affordable nanofabrication technique is developed that allows for the control of nanoparticle size, spacing, and shape.
The available techniques to produce nanoparticles are mostly based on nanoscale lithography, which have significant scalability and cost issues. There have been multiple different studies that have attempted to address the scalability problem of these techniques, but to date, no process exists that provides the level of control needed for nanoparticle fabrication and is cost and time effective enough for adoption in industrial applications6,7,8,9,10,11. Some recent research efforts improved the controllability of pulsed laser induced dewetting (PLiD) and templated solid-state dewetting12,13,14, but they still have significant required lithography steps and thus the scalability problem.
In this manuscript, we present the protocol of a nanofabrication method that will address this scalability and cost issue that has plagued the adoption and use of nanoparticle films in widespread industrial applications. This processing method allows the control over the produced nanoparticle size and spacing by manipulating the surface energies which dictate the self-assembly of the nanoparticles formed. Here, we demonstrate the use of this technique using a thin gold film to produce gold nanoparticles, but we have recently published a slightly different version of this method using a nickel film and thus this technique can be used with any desired metal. The goal of this method is to produce nanoparticle films while minimizing the cost and complexity of the process and thus we have modified our previous approach, which used atomic layer deposition and nanosecond laser irradiation on a Ni-alumina system and replaced them with physical vapor deposition and a hot plate. The result of our work on a Ni-alumina system also showed an acceptable level of control on the morphology of the surface after the dewetting15.

<table>
	<tbody>
		<tr>
			<td>100 nm SiO2/Si Substrate</td>
			<td>University Wafer</td>
			<td>Thermal Oxide Wafer</td>
			<td></td>
		</tr>
		<tr>
			<td>Alumina Sputter Target (99.5%)</td>
			<td>Kurt J. Lesker</td>
			<td>Alumina Target</td>
			<td></td>
		</tr>
		<tr>
			<td>Gold Wire (99.99%)</td>
			<td>Kurt J. Lesker</td>
			<td>Gold Wire</td>
			<td></td>
		</tr>
		<tr>
			<td>H2O2</td>
			<td>Sigma-Aldrich</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Hot Plate</td>
			<td>Thermo Scientific</td>
			<td>Cimarec</td>
			<td></td>
		</tr>
		<tr>
			<td>NH4OH</td>
			<td>Sigma-Aldrich</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Scanning Electron Microscope</td>
			<td>FEI</td>
			<td>Quanta 650</td>
			<td></td>
		</tr>
		<tr>
			<td>Scanning Electron Microscope</td>
			<td>FEI</td>
			<td>Nova Nanolab 600</td>
			<td></td>
		</tr>
		<tr>
			<td>Sputter Deposition System</td>
			<td>AJA International</td>
			<td>Orion-5</td>
			<td></td>
		</tr>
		<tr>
			<td>Thermal Evaporator</td>
			<td>Edwards</td>
			<td>360</td>
			<td></td>
		</tr>
	</tbody>
</table>

large area substrate-based nanofabrication of controllable and customizable gold nanoparticles via capped dewetting

Recent scientific advances in the utilization of metallic nanoparticle for enhanced energy conversion efficiency, improved optical device performance, and high-density data storage have demonstrated the potential benefit of their use in industrial applications. These applications require precise control over nanoparticle size, spacing, and sometimes shape. These requirements have resulted in the use of time and cost intensive processing steps to produce nanoparticles, thus making the transition to industrial application unrealistic. This protocol will resolve this issue by providing a scalable and affordable method for the large-area production of nanoparticle films with improved nanoparticle control compared to the current techniques. In this article, the process will be demonstrated with gold, but other metals can also be used.

The protocol described here has been used for multiple metals and has shown the ability to produce nanoparticles on a substrate over large-area, with controllable size and spacing. Figure 1 shows the protocol with representative results showing the ability to control the fabricated nanoparticle size and spacing. When following this protocol, the result, which is the fabricated nanoparticle film with size and spacing distributions, will be dependent upon the c...

Watch this Scientific Journal Video about Large Area Substrate-Based Nanofabrication of Controllable and Customizable Gold Nanoparticles Via Capped Dewetting at JoVE.com

Large Area Substrate-Based Nanofabrication of Controllable and Customizable Gold Nanoparticles Via Capped Dewetting

This protocol details a novel nano-manufacturing technique that can be used to make controllable and customizable nanoparticle films over large areas based on the self-assembly of dewetting of capped metal films.

Recent scientific advances in the utilization of metallic nanoparticle for enhanced energy conversion efficiency, improved optical device performance, and ...

Our protocol provides a technique to customize nanoparticle distribution, fabricated on a substrate, with changing the dewetting dynamics, without changing the material thickness. Our technique is simple, yet still provides a range of particle sizes. Other techniques out there require extensive lithographic steps to provide the particle control.Our control of particle distribution provides a technique for nanoparticle fabrication that benefits research focused on solar energy conversion, creating photonic devices, and increasing density of data storage. Pay close attention to the deposition thicknesses at each step. Our technique is extremely sensitive to layer thicknesses.Seeing the experiment performed provides a level of detail that can't be conveyed in print. Seeing examples moving throughout the process is essential. First, clean a 100 nanometer silicon dioxide on silicon substrate, using an acetone rinse, followed by an isopropyl alcohol rinse.Dry the substrate using a stream of nitrogen gas. Load the substrate into a thermal evaporator system and evacuate the chamber to reach the desired pressure for the deposition of the metal film. Ensure that the chamber is evacuated to a pressure on the order of 10 to the minus six torr for the removal of air and water vapor in the chamber.Using the thermal evaporator system, deposit the gold film at the desired thickness, which is five nanometers in this experiment. At the second deposition stages, the argon pressure is one to five millitorr, and the range is given as different pressures are chosen to calibrate for the deposition rate. Our technique is extremely sensitive to film thicknesses, as shown in our results.It is critical to calibrate the deposition rates prior to depositing the films, to ensure appropriate thicknesses. Following deposition, vent the chamber and remove the substrate, with the deposited metal film, from the thermal evaporator system. Next, load the substrate, with a deposited metal film, into a direct current magnetron sputter deposition system and evacuate to reach the desired pressure for deposition of the capping film.To locate the sample in the system, put the sample in the load lock. And the device transfers the sample to the main deposition chamber to ensure a sufficient level of vacuum. Now, deposit the capping layer of the desired material and thickness, following a similar procedure and condition as the gold layer deposition.With variable thickness Illumina, in this case. Following deposition, vent the chamber and remove the prepared sample from the sputter deposition system. Place the five nanometer gold film, capped with Illumina, onto a pre-heated hot plate at 300 degrees Celsius, and allow the sample to dewet for one hour.Etch the Illumina, while leaving the gold and underlying substrate with an aqueous solution of ammonium hydroxide and hydrogen peroxide at 80 degrees Celsius for one hour. For characterization, prepare the sample to be vacuum-compatible by rinsing with acetone and isopropyl alcohol. Then, dry the sample using a stream of nitrogen gas.Image the nanoparticle films using scanning electron microscopy under high vacuum and at high magnification. Perform image analysis to obtain information on nanoparticle size and spacing distributions. The protocol described here has been used for multiple metals and has shown the ability to produce nanoparticles on a substrate over large area, with controllable size and spacing.Representative results are shown here, and highlight the ability to control the fabricated nanoparticle size and spacing. The size and spacing distributions of the fabricated nanoparticle film will be dependent upon the metal, the substrate, the capping layer material, the metal thickness, and the capping layer thickness. As an example, the five nanometer gold film on silicon dioxide, with aluminum oxide capping layer thickness of zero, five, 10, and 20 nanometers result in an average nanoparticle radii of 14.2, 18.4, 17.3, and 15.6 nanometers respectively.And an average nonoparticle spacing of 36.9, 56.9, 51.3, and 47.2 nanometers respectively. For the desired particle distribution, accurate control of the deposition layer thicknesses is critical. Depending on the application of your nanoparticle films, more characterization may be required.This would include application-based measurements, like light absorption and magnetic properties. Studies of nanoparticle films in application can be performed using this technique, to control their particle size and distribution. Appropriate personal protective equipments should be worn.Especially do not come into contact with the etchings. Avoid contact with the hot plate.

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