This work was supported by the Basic Science Research Program through the National Research Foundation of Korea (NRF), funded by the Ministry of Education, Science and Technology (NRF-2013R1A1A1010575), and by Nano R&#38;D program through the Korea Science and Engineering Foundation funded by the Ministry of Education, Science and Technology (NRF-2012M3A7B4049863).

1. Synthesis of Vertically Aligned Multi-walled Carbon Nanotubes (VAMWCNTs)
<ol>
	<li>Preparation of wafer and deposition of catalyst layers
	<ol>
		<li>Prepare a n-type (100) Si wafer.</li>
		<li>Deposit a 250-nm-thick SiO2 layer on the Si wafer by thermal oxidation or alternative methods such as sputtering. Inject 200 sccm of O2 for 3 hr 20 min at 1,000 &#176;C in a horizontal furnace.</li>
		<li>Use bulk Al2O3 (99.9%) as a multi-sputter (RF power: 1,000 W) source and depos...

<ol>
	<li>Zhou, X., Torabi, M., Lu, J., Shen, R. Q., Zhang, K. L. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Nanostructured+Energetic+Composites:+Synthesis,+Ignition/Combustion+Modeling,+and+Applications.">Nanostructured Energetic Composites: Synthesis, Ignition/Combustion Modeling, and Applications.</a> Acs Appl Mater Inter. 6, 3058-3074 (2014).</li><li>Zhang, K., Chou, S., Ang, S., Tang, X. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+MEMS-based+solid+propellant+microthruster+with+Au/Ti+igniter.">A MEMS-based solid propellant microthruster with Au/Ti igniter.</a> Sensors and Actuators A: Physical. 122, 113-123 (2005).</li><li>Zhang, W. C., 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=Significantly+Enhanced+Energy+Output+from+3D+Ordered+Macroporous+Structured+Fe2O3/Al+Nanothermite+Film.">Significantly Enhanced Energy Output from 3D Ordered Macroporous Structured Fe2O3/Al Nanothermite Film.</a> Acs Appl Mater Inter. 5, 239-242 (2013).</li><li>Choi, W., Abrahamson, J. T., Strano, J. M., Strano, M. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Carbon+nanotube-guided+thermopower+waves.">Carbon nanotube-guided thermopower waves.</a> Materials Today. 13, 22-33 (2010).</li><li>Choi, W., 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=Chemically+driven+carbon-nanotube-guided+thermopower+waves.">Chemically driven carbon-nanotube-guided thermopower waves.</a> Nat Mater. 9, 423-429 (2010).</li><li>Abrahamson, J. T., 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=Wavefront+Velocity+Oscillations+of+Carbon-Nanotube-Guided+Thermopower+Waves:+Nanoscale+Alternating+Current+Sources.">Wavefront Velocity Oscillations of Carbon-Nanotube-Guided Thermopower Waves: Nanoscale Alternating Current Sources.</a> Acs Nano. 5, 367-375 (2011).</li><li>Walia, S., 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=ZnO+based+thermopower+wave+sources.">ZnO based thermopower wave sources.</a> Chem Commun. 48, 7462-7464 (2012).</li><li>Walia, S., 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=Sb2Te3+and+Bi2Te3+based+thermopower+wave+sources.">Sb2Te3 and Bi2Te3 based thermopower wave sources.</a> Energ Environ Sci. 4, 3558-3564 (2011).</li><li>Hong, S., 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=Enhanced+Electrical+Potential+of+Thermoelectric+Power+Waves+by+Sb2Te3-Coated+Multiwalled+Carbon+Nanotube+Arrays.">Enhanced Electrical Potential of Thermoelectric Power Waves by Sb2Te3-Coated Multiwalled Carbon Nanotube Arrays.</a> J Phys Chem C. 117, 913-917 (2013).</li><li>Walia, S., 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=MnO2-Based+Thermopower+Wave+Sources+with+Exceptionally+Large+Output+Voltages.">MnO2-Based Thermopower Wave Sources with Exceptionally Large Output Voltages.</a> J Phys Chem C. 117, 9137-9142 (2013).</li><li>Aria, A. I., Gharib, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Dry+oxidation+and+vacuum+annealing+treatments+for+tuning+the+wetting+properties+of+carbon+nanotube+arrays.">Dry oxidation and vacuum annealing treatments for tuning the wetting properties of carbon nanotube arrays.</a> J Vis Exp. , (2013).</li><li>Zhao, Y., Tang, Y., Star, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Synthesis+and+functionalization+of+nitrogen-doped+carbon+nanotube+cups+with+gold+nanoparticles+as+cork+stoppers.">Synthesis and functionalization of nitrogen-doped carbon nanotube cups with gold nanoparticles as cork stoppers.</a> J Vis Exp. , e50383 (2013).</li><li>Copic, D., Park, S. J., Tawfick, S., De Volder, M., Hart, A. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Fabrication,+densification,+and+replica+molding+of+3D+carbon+nanotube+microstructures.">Fabrication, densification, and replica molding of 3D carbon nanotube microstructures.</a> J Vis Exp. , (2012).</li><li>Grimme, S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Do+Special+Noncovalent+&#960;&#8211;&#960;+Stacking+Interactions+Really+Exist.">Do Special Noncovalent &#960;&#8211;&#960; Stacking Interactions Really Exist.</a> Angewandte Chemie International Edition. 47, 3430-3434 (2008).</li><li>Yeo, T., 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=Effects+of+chemical+fuel+composition+on+energy+generation+from+thermopower+waves.">Effects of chemical fuel composition on energy generation from thermopower waves.</a> Nanotechnology. 25, (2014).</li><li>Hong, S., 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=Enhanced+Electrical+Potential+of+Thermoelectric+Power+Waves+by+Sb2Te3-Coated+Multiwalled+Carbon+Nanotube+Arrays.">Enhanced Electrical Potential of Thermoelectric Power Waves by Sb2Te3-Coated Multiwalled Carbon Nanotube Arrays.</a> The Journal of Physical Chemistry C. 117, 913-917 (2013).</li><li>Kim, P., Shi, L., Majumdar, A., McEuen, P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Thermal+transport+measurements+of+individual+multiwalled+nanotubes.">Thermal transport measurements of individual multiwalled nanotubes.</a> Physical review letters. 87, 215502 (2001).</li><li>Garner, W., Abernethy, C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Heats+of+combustion+and+formation+of+nitro-compounds.+Part+I.+Benzene,+toluene,+phenol+and+methylaniline+series.">Heats of combustion and formation of nitro-compounds. Part I. Benzene, toluene, phenol and methylaniline series.</a> Proceedings of the Royal Society of London. Series A. 99, 213-235 (1921).</li><li>Passingham, C., Hendra, P. J., Hodges, C., Willis, H. A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+Raman+spectra+of+some+aromatic+nitro+compounds.">The Raman spectra of some aromatic nitro compounds.</a> Spectrochimica Acta Part A: Molecular Spectroscopy. 47, 1235-1245 (1991).</li><li>Rinkenbach, W. H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+Heats+Of+Combustion+And+Formation+Of+Aromatic+Nitro+Compounds.">The Heats Of Combustion And Formation Of Aromatic Nitro Compounds.</a> Journal of the American Chemical Society. 52, 115-120 (1930).</li></ol>

The authors have nothing to disclose.

The protocols of thermopower wave experiments involve critical steps that enable ideal thermal wave propagation as well as electrical energy generation. First, the specific position of ignition and the corresponding reaction transfer are considerable factors in controlling energy conversion from thermopower waves. Ignition at one end of the hybrid composite launched guided combustion along the interfaces between the core materials and chemical fuels in one direction. However, ignition at any other position generated bi-d...

Chemical fuels have very high energy density and have been widely used as useful energy sources in a broad range of applications from microsystems to macrosystems.1 In particular, many researchers have endeavored to use chemical fuels as the energy source for next-generation micro/nanosystems-based technologies.2 However, owing to the difficulty in integrating energy conversion components in extremely small spaces in micro/nanodevices, there are fundamental limitations to the conversion of chemical fuels into electrical energy. Therefore, the combustion of chemical fuels has mainly been employed for the production of chemical or mechanical energy in micro/nanodevices such as nanothermites or microactuators.1,3
Thermopower waves&#8212;a newly developed energy conversion concept&#8212;have attracted considerable attention as a method for converting the chemical energy of a fuel directly to electrical energy without using any converting components.4,5 Thermopower waves can be generated using a hybrid composite of a chemical fuel and a micro/nanostructured material.5 When the chemical fuel at a certain position in a hybrid composite is ignited, chemical combustion occurs along the interface between the chemical fuel and micro/nanostructured material. Simultaneously, dynamic changes in thermal and chemical potentials across the core micro/nanostructured material result in concomitant electrical energy generation induced by charge transfer in the form of a high-output voltage pulse. It has been proven that diverse micro/nanostructured materials such as multi-walled carbon nanotubes (MWCNTs)4-6 and ZnO,7 Bi2Te3,8 Sb2Te3,9 and MnO210 micro/nanostructured materials allow hybrid composites to utilize thermopower waves and show chemical&#8211;thermal&#8211;electrical energy conversion. Specifically, core materials with a high Seebeck coefficient enable the generation of high output voltages solely from propagated combustion. However, other parameters pertaining to identical composites, such as the mixture of chemical fuels, mass ratio of fuel/core&#8211;materials, the manufacturing process, and ignition conditions critically affect the overall properties of thermopower waves.
Herein, we show how the manufacturing processes, formation of an aligned chemical fuel, and mass ratio of fuel/core materials affect thermopower wave performance. On the basis of a MWCNT array fabricated by thermal chemical vapor deposition (TCVD), we show how a hybrid composite of a chemical fuel and MWCNTs is prepared for thermopower wave energy generation. Design of the experimental setup that enables the evaluation of energy conversion is introduced along with corresponding experimental measurements for processes such as combustion propagation and direct electrical energy generation. Moreover, we demonstrate that polarity distribution&#8212;described by the dynamic output voltage and specific peak power&#8212;crucially determines the electrical energy conversion. This study will provide specific strategies to enhance energy generation, and will help in understanding the underlying physics of thermopower waves. Furthermore, the manufacturing process and experiments described here will help in extending research opportunities on thermopower waves, as well as on chemical&#8211;thermal&#8211;electrical energy conversion.

<table border="0" cellpadding="0" cellspacing="0">
	<tbody>
		<tr>
			<td>4&#8221; n-type silicon wafer</td>
			<td>Unisill</td>
			<td>4&#8221; Si-wafer</td>
			<td></td>
		</tr>
		<tr>
			<td>Al2O3</td>
			<td>TAEWON</td>
			<td>A-1008</td>
			<td>99.9999% Purity</td>
		</tr>
		<tr>
			<td>Fe</td>
			<td>Sigma Aldrich</td>
			<td>267945</td>
			<td>99.9999% Purity</td>
		</tr>
		<tr>
			<td>Ar</td>
			<td>Seoul specialty gas</td>
			<td>Ar(N60)</td>
			<td>99.9999% Purity</td>
		</tr>
		<tr>
			<td>C2H4</td>
			<td>Seoul specialty gas</td>
			<td>C2H4</td>
			<td>99.5% Purity</td>
		</tr>
		<tr>
			<td>H2</td>
			<td>Seoul specialty gas</td>
			<td align="left"><img src="file:///C:/Users/BENSAL~1/AppData/Local/Temp/msohtmlclip1/01/clip_image002.png" />
			<table cellpadding="0" cellspacing="0">
				<tbody>
					<tr>
						<td>H2(N60)</td>
					</tr>
				</tbody>
			</table>
			</td>
			<td>99.9999% Purity</td>
		</tr>
		<tr>
			<td>Silver paste</td>
			<td>Fujikura Kasei</td>
			<td>D-550</td>
			<td></td>
		</tr>
		<tr>
			<td>Picric acid</td>
			<td>Sigma Aldrich</td>
			<td>197378</td>
			<td>&#65310;98% Purity 
			Highly toxic</td>
		</tr>
		<tr>
			<td>Sodium azide</td>
			<td>Sigma Aldrich</td>
			<td>S2002</td>
			<td>&#65310;99.5% Purity</td>
		</tr>
		<tr>
			<td>Acetonitrile</td>
			<td>Sigma Aldrich</td>
			<td>271004</td>
			<td>99.8% Purity</td>
		</tr>
		<tr>
			<td>Power supply</td>
			<td>Mastech</td>
			<td>HY3010</td>
			<td></td>
		</tr>
		<tr>
			<td>TCVD</td>
			<td>Scientech</td>
			<td>TCVD</td>
			<td></td>
		</tr>
		<tr>
			<td>Oscilloscope</td>
			<td>Tektronix</td>
			<td>DPO2004B</td>
			<td></td>
		</tr>
		<tr>
			<td>High-speed microscopy system</td>
			<td>Phantom</td>
			<td>V7.3</td>
			<td></td>
		</tr>
	</tbody>
</table>

preparation and evaluation of hybrid composites of chemical fuel and multi-walled carbon nanotubes in the study of thermopower waves

When a chemical fuel at a certain position in a hybrid composite of the fuel and a micro/nanostructured material is ignited, chemical combustion occurs along the interface between the fuel and core materials. Simultaneously, dynamic changes in thermal and chemical potentials across the micro/nanostructured materials result in concomitant electrical energy generation induced by charge transfer in the form of a high-output voltage pulse. We demonstrate the entire procedure of a thermopower wave experiment, from synthesis to evaluation. Thermal chemical vapor deposition and the wet impregnation process are respectively employed for the synthesis of a multi-walled carbon nanotube array and a hybrid composite of picric acid/sodium azide/multi-walled carbon nanotubes. The prepared hybrid composites are used to fabricate a thermopower wave generator with connecting electrodes. The combustion of the hybrid composite is initiated by laser heating or Joule-heating, and the corresponding combustion propagation, direct electrical energy generation, and real-time temperature changes are measured using a high-speed microscopy system, an oscilloscope, and an optical pyrometer, respectively. Furthermore, the crucial strategies to be adopted in the synthesis of hybrid composite and initiation of their combustion that enhance the overall thermopower wave energy transfer are proposed.

The aligned MWCNT array, as a core nanostructured material for thermopower waves, was synthesized by TCVD,11-13 as shown in Figure 4A. The diameter of as-grown MWCNTs is 20&#8211;30 nm (Figure 4B). The aligned hybrid composite of the picric acid/sodium azide/MWCNTs is shown in Figure 5A. This composite was synthesized by the wet impregnation process,14 as described in the protocol section. In order to form an interface between the chemical fuel and ...

Watch this Scientific Journal Video about Preparation and Evaluation of Hybrid Composites of Chemical Fuel and Multi-walled Carbon Nanotubes in the Study of Thermopower Waves at JoVE.com

Preparation and Evaluation of Hybrid Composites of Chemical Fuel and Multi-walled Carbon Nanotubes in the Study of Thermopower Waves

A protocol for conducting thermopower wave experiments is presented. The synthesis of hybrid composites of a chemical fuel and micro/nanostructured material, manufacturing of a thermopower wave generator, and methods for measuring the corresponding physical phenomena are described.

When a chemical fuel at a certain position in a hybrid composite of the fuel and a micro/nanostructured material is ignited, chemical combustion occurs ...

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8.7K Görüntüleme.  Korea University. A protocol for conducting thermopower wave experiments is presented. The synthesis of hybrid composites of a chemical fuel and micro/nanostructured material, manufacturing of a thermopower wave generator, and methods for measuring the corresponding physical phenomena are described. 