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 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 ...

preparation-evaluation-hybrid-composites-chemical-fuel-multi-walled

Research

JoVE Journal

Engineering

8.7K ビュー.  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. 

ビデオ: 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.

synthesis of multi-walled carbon nanotubes modified with silver nanoparticles and evaluation of their antibacterial activities and cytotoxic properties

Synthesis of Multi-walled Carbon Nanotubes Modified with Silver Nanoparticles and Evaluation of Their Antibacterial Activities and Cytotoxic Properties

In this study, antimicrobial nanomaterials were synthesized by acidic oxidation of multiwalled carbon nanotubes and subsequent reductive deposition of silver nanoparticles. Antimicrobial activity and cytotoxicity tests were performed with the as-prepared...

simultaneous synthesis of single-walled carbon nanotubes and graphene in a magnetically-enhanced arc plasma

Simultaneous Synthesis of Single-walled Carbon Nanotubes and Graphene in a Magnetically-enhanced Arc Plasma

Anodic arc discharge is one of the most practical and efficient methods to synthesize various carbon nanostructures. To increase the arc controllability and flexibility, a non-uniform magnetic field was introduced to process the one-step synthesis of large-scale graphene flakes and high-purity single-walled carbon...

functionalization of single-walled carbon nanotubes with thermo-reversible block copolymers and characterization by small-angle neutron scattering

Functionalization of Single-walled Carbon Nanotubes with Thermo-reversible Block Copolymers and Characterization by Small-angle Neutron Scattering

A method for the functionalization of carbon nanotubes with structure-tunable polymeric encapsulation layers and structural characterization using small-angle neutron scattering is...

engineering molecular recognition with bio-mimetic polymers on single walled carbon nanotubes

Engineering Molecular Recognition with Bio-mimetic Polymers on Single Walled Carbon Nanotubes

We present a protocol for engineering the corona phase of near infrared fluorescent single walled carbon nanotubes (SWNTs) using amphiphilic polymers and DNA to develop sensors for molecular targets without known recognition...

facile preparation of internally self-assembled lipid particles stabilized by carbon nanotubes

Facile Preparation of Internally Self-assembled Lipid Particles Stabilized by Carbon Nanotubes

We report on a smart application of carbon nanotubes for kinetic stabilization of lipid particles that contain self-assembled nanostructures in their cores. The preparation of lipid particles requires rather low concentrations of carbon nanotubes permitting their use in biomedical applications such as drug...

localization and relative quantification of carbon nanotubes in cells with multispectral imaging flow cytometry

Localization and Relative Quantification of Carbon Nanotubes in Cells with Multispectral Imaging Flow Cytometry

In this study, the main purpose was to monitor the cellular uptake and eventual exocytosis of carbon nanotubes (CNTs). From this perspective, we proposed here a unique method using multispectral imaging flow cytometry allowing a quantification and localization of CNTs in a statistically relevant number of...

transport of surface-modified carbon nanotubes through a soil column

Transport of Surface-modified Carbon Nanotubes through a Soil Column

Surface properties of a nanoparticle are important for their interaction with the surrounding medium. Therefore the surface modification of carbon nanotubes can be critical for their transport and retention through porous media. Here, lab scale column experiments are used to understand the possible transport and retention of these nanoparticles.

membraneless hydrogen peroxide fuel cells as a promising clean energy source

Author Spotlight: Design and Evaluation of Au-Electroplated Carbon Fiber Cloth Electrodes for Hydrogen Peroxide Fuel Cells 

This protocol introduces the design and evaluation of innovative three-dimensional electrodes for hydrogen peroxide fuel cells, utilizing Au-electroplated carbon fiber cloth and Ni-foam electrodes. The research findings highlight hydrogen peroxide's potential as a promising candidate for sustainable energy...

Exploring Innovative 3D Electrodes for Hydrogen Peroxide Fuel Cells

https://cloudfront.jove.com/CDNSource/teasers/65920_b.jpg

grafting multiwalled carbon nanotubes with polystyrene to enable self-assembly and anisotropic patchiness

Grafting Multiwalled Carbon Nanotubes with Polystyrene to Enable Self-Assembly and Anisotropic Patchiness

A procedure for the synthesis of polystyrene-grafted multiwalled carbon nanotubes using successive chemical modification steps to selectively introduce the polymer chains to the sidewalls and their self-assembly via anisotropic patchiness is...

the effect of interfacial chemical bonding in tio2-sio2 composites on their photocatalytic nox abatement performance

The Effect of Interfacial Chemical Bonding in TiO2-SiO2 Composites on Their Photocatalytic NOx Abatement Performance

The focus of the present work is to establish means to generate and quantify levels of Ti-O-Si linkages and to correlate these with the photocatalytic properties of the supported...

The Effect of Interfacial Chemical Bonding in TiO2-SiO2 Composites on Their Photocatalytic NOx Abatement Performance

confocal time lapse imaging as an efficient method for the cytocompatibility evaluation of dental composites

Confocal Time Lapse Imaging as an Efficient Method for the Cytocompatibility Evaluation of Dental Composites

The most studied aspect of the biocompatibility of dental composites is their cytotoxicity 3D CLSM time lapse imaging combined with fluorescent signal quantification allows sensitive evaluation of the cell fate over time. Utilizing this method could be an efficient tool to assess the cytocompatibility of dental...

combining chemical cross-linking and mass spectrometry of intact protein complexes to study the architecture of multi-subunit protein assemblies

Combining Chemical Cross-linking and Mass Spectrometry of Intact Protein Complexes to Study the Architecture of Multi-subunit Protein Assemblies

The architecture of protein complexes is essential for their function. Combining various mass spectrometric techniques proved powerful to study their assembly. We provide protocols for chemical cross-linking and native mass spectrometry and show how these complementary techniques help to elucidate the architecture of multi-subunit protein...

improving the combustion performance of a hybrid rocket engine using a novel fuel grain with a nested helical structure

Improving the Combustion Performance of a Hybrid Rocket Engine using a Novel Fuel Grain with a Nested Helical Structure

A technique utilizing a solid fuel grain with a novel nested helical structure to improve the combustion performance of a hybrid rocket engine is...

preparation and characterization of c60/graphene hybrid nanostructures

Preparation and Characterization of C60/Graphene Hybrid Nanostructures

Here we present a protocol for the fabrication of C60/graphene hybrid nanostructures by physical thermal evaporation. Particularly, the proper manipulation of deposition and annealing conditions allow the control over the creation of 1D and quasi 1D C60 structures on rippled...

Preparation and Characterization of C60/Graphene Hybrid Nanostructures

a synthetic methodology for preparing impregnated and grafted amine-based silica composites for carbon capture

Author Spotlight: Standardizing the Development of Amine-Based Silica Composites as CO2 Adsorbents for Direct Air Capture 

This work aims to facilitate the development of standardized techniques for impregnating or grafting aminated compounds onto silica substrates, which are often broadly described in the literature. Specific amounts of solvent, substrate, amines, and the values of other important experimental parameters will be discussed in detail.

A Synthetic Methodology for Preparing Impregnated and Grafted Amine-Based Silica Composites for Carbon Capture

on the preparation and testing of fuel cell catalysts using the thin film rotating disk electrode method

On the Preparation and Testing of Fuel Cell Catalysts Using the Thin Film Rotating Disk Electrode Method

Preparing and testing Pt/C fuel cell catalysts is subject to continuous discussion in the scientific community with respect to reproducibility and best practice. With the presented work, we intend to present a step-by-step tutorial to make and test Pt/C catalysts, which can serve as benchmark for novel catalyst...

fabrication and design of wood-based high-performance composites

Fabrication and Design of Wood-Based High-Performance Composites

Delignified densified wood represents a new promising lightweight, high-performance and bio-based material with great potential to partially substitute natural fiber reinforced- or glass fiber reinforced composites in the future. We here present two versatile fabrication routes and demonstrate the possibility to create complex composite...

preparation of carbon nanosheets at room temperature

Preparation of Carbon Nanosheets at Room Temperature

We present the synthesis of an amphiphilic hexayne and its use in the preparation of carbon nanosheets at the air-water interface from a self-assembled monolayer of these reactive, carbon-rich molecular...

preparation, procedures and evaluation of platelet-rich plasma injection in the treatment of knee osteoarthritis

Preparation, Procedures and Evaluation of Platelet-Rich Plasma Injection in the Treatment of Knee Osteoarthritis

Knee osteoarthritis is frequently seen in the orthopedic department. We introduce in detail the entire knee osteoarthritis treatment process with platelet-rich plasma injection, including preparation, procedures, and...

Encapsulation and Permeability Characteristics of Plasma Polymerized Hollow Particles

In this protocol, core-shell nanostructures are synthesized by plasma enhanced chemical vapor deposition. We produce an amorphous barrier by plasma polymerization of isopropanol on various solid substrates, including silica and potassium chloride. This versatile technique is used to treat nanoparticles and nanopowders with sizes ranging from 37 nm to 1 micron, by depositing films whose thickness can be anywhere from 1 nm to upwards of 100 nm. Dissolution of the core allows us to study the rate of permeation through the film. In these experiments, we determine the diffusion coefficient of KCl through the barrier film by coating KCL nanocrystals and subsequently monitoring the ionic conductivity of the coated particles suspended in water. The primary interest in this process is the encapsulation and delayed release of solutes. The thickness of the shell is one of the independent variables by which we control the rate of release. It has a strong effect on the rate of release, which increases from a six-hour release (shell thickness is 20 nm) to a long-term release over 30 days (shell thickness is 95 nm). The release profile shows a characteristic behavior: a fast release (35% of the final materials) during the first five minutes after the beginning of the dissolution, and a slower release till all of the core materials come out.

We have used plasma enhanced chemical vapor deposition to deposit thin films ranging from a few nm to several 100 nm on nano-sized particles of various materials. We subsequently etch the core material to produce hollow nanoshells whose permeability is controlled by the thickness of the shell. We characterize the permeability of these coatings to small solutes and demonstrate that these barriers can provide sustained release of the core material over several days.

In this protocol, core-shell nanostructures are synthesized by plasma enhanced chemical vapor deposition. We produce an amorphous barrier by plasma ...

Probing and Mapping Electrode Surfaces in Solid Oxide Fuel Cells

Solid oxide fuel cells (SOFCs) are potentially the most efficient and cost-effective solution to utilization of a wide variety of fuels beyond hydrogen 1-7. The performance of SOFCs and the rates of many chemical and energy transformation processes in energy storage and conversion devices in general are limited primarily by charge and mass transfer along electrode surfaces and across interfaces. Unfortunately, the mechanistic understanding of these processes is still lacking, due largely to the difficulty of characterizing these processes under in situ conditions. This knowledge gap is a chief obstacle to SOFC commercialization. The development of tools for probing and mapping surface chemistries relevant to electrode reactions is vital to unraveling the mechanisms of surface processes and to achieving rational design of new electrode materials for more efficient energy storage and conversion2. Among the relatively few in situ surface analysis methods, Raman spectroscopy can be performed even with high temperatures and harsh atmospheres, making it ideal for characterizing chemical processes relevant to SOFC anode performance and degradation8-12. It can also be used alongside electrochemical measurements, potentially allowing direct correlation of electrochemistry to surface chemistry in an operating cell. Proper in situ Raman mapping measurements would be useful for pin-pointing important anode reaction mechanisms because of its sensitivity to the relevant species, including anode performance degradation through carbon deposition8, 10, 13, 14 ("coking") and sulfur poisoning11, 15 and the manner in which surface modifications stave off this degradation16. The current work demonstrates significant progress towards this capability. In addition, the family of scanning probe microscopy (SPM) techniques provides a special approach to interrogate the electrode surface with nanoscale resolution. Besides the surface topography that is routinely collected by AFM and STM, other properties such as local electronic states, ion diffusion coefficient and surface potential can also be investigated17-22. In this work, electrochemical measurements, Raman spectroscopy, and SPM were used in conjunction with a novel test electrode platform that consists of a Ni mesh electrode embedded in an yttria-stabilized zirconia (YSZ) electrolyte. Cell performance testing and impedance spectroscopy under fuel containing H2S was characterized, and Raman mapping was used to further elucidate the nature of sulfur poisoning. In situ Raman monitoring was used to investigate coking behavior. Finally, atomic force microscopy (AFM) and electrostatic force microscopy (EFM) were used to further visualize carbon deposition on the nanoscale. From this research, we desire to produce a more complete picture of the SOFC anode.

We present a unique platform for characterizing electrode surfaces in solid oxide fuel cells (SOFCs) that allows simultaneous performance of multiple characterization techniques (e.g. in situ Raman spectroscopy and scanning probe microscopy alongside electrochemical measurements). Complementary information from these analyses may help to advance toward a more profound understanding of electrode reaction and degradation mechanisms, providing insights into rational design of better materials for SOFCs.

Solid oxide fuel cells (SOFCs) are potentially the most efficient and cost-effective solution to utilization of a wide variety of fuels beyond hydrogen ...

Preparation and Reactivity of Gasless Nanostructured Energetic Materials

High-Energy Ball Milling (HEBM) is a ball milling process where a powder mixture placed in the ball mill is subjected to high-energy collisions from the balls. Among other applications, it is a versatile technique that allows for effective preparation of gasless reactive nanostructured materials with high energy density per volume (Ni+Al, Ta+C, Ti+C). The structural transformations of reactive media, which take place during HEBM, define the reaction mechanism in the produced energetic&#160;composites. Varying the processing conditions permits fine tuning of the milling-induced microstructures of the fabricated composite particles. In turn, the reactivity, i.e., self-ignition temperature, ignition delay time, as well as reaction kinetics, of high energy density materials depends on its microstructure. Analysis of the milling-induced microstructures suggests that the formation of fresh oxygen-free intimate high surface area contacts between the reagents is responsible for the enhancement of their reactivity. This manifests itself in a reduction of ignition temperature and delay time, an increased rate of chemical reaction, and an overall decrease of the effective activation energy of the reaction. The protocol provides a detailed description for the preparation of reactive nanocomposites with tailored microstructure using short-term HEBM method. It also describes a high-speed thermal imaging technique to determine the ignition/combustion characteristics of the energetic materials. The protocol can be adapted to preparation and characterization of a variety of nanostructured energetic composites.

This protocol describes the preparation of gasless nanostructured energetic materials (Ni+Al, Ta+C, Ti+C) using the short-term high-energy ball milling (HEBM) technique. It also describes a high-speed thermal imaging method to study the reactivity of mechanically fabricated nanocomposites. These protocols can be extended to other reactive nanostructured energetic materials.

High-Energy Ball Milling (HEBM) is a ball milling process where a powder mixture placed in the ball mill is subjected to high-energy collisions from the ...

Ultrasonic Welding of Thermoplastic Composite Coupons for Mechanical Characterization of Welded Joints through Single Lap Shear Testing

This paper presents a novel straightforward method for ultrasonic welding of thermoplastic-composite coupons in optimum processing conditions. The ultrasonic welding process described in this paper is based on three main pillars. Firstly, flat energy directors are used for preferential heat generation at the joining interface during the welding process. A flat energy director is a neat thermoplastic resin film that is placed between the parts to be joined prior to the welding process and heats up preferentially owing to its lower compressive stiffness relative to the composite substrates. Consequently, flat energy directors provide a simple solution that does not require molding of resin protrusions on the surfaces of the composite substrates, as opposed to ultrasonic welding of unreinforced plastics. Secondly, the process data provided by the ultrasonic welder is used to rapidly define the optimum welding parameters for any thermoplastic composite material combination. Thirdly, displacement control is used in the welding process to ensure consistent quality of the welded joints. According to this method, thermoplastic-composite flat coupons are individually welded in a single lap configuration. Mechanical testing of the welded coupons allows determining the apparent lap shear strength of the joints, which is one of the properties most commonly used to quantify the strength of thermoplastic composite welded joints.

A straightforward procedure for ultrasonic welding of thermoplastic composite coupons for basic mechanical testing is described. Key characteristics of this ultrasonic welding process are the use of flat energy directors for simplified process preparation and the use of process data for the fast definition of optimum processing conditions.

This paper presents a novel straightforward method for ultrasonic welding of thermoplastic-composite coupons in optimum processing conditions. The ...

Preparation and 3D Tracking of Catalytic Swimming Devices

We report a method to prepare catalytically active Janus colloids that "swim" in fluids and describe how to determine their 3D motion using fluorescence microscopy. One commonly deployed method for catalytically active colloids to produce enhanced motion is via an asymmetrical distribution of catalyst. Here this is achieved by spin coating a dispersed layer of fluorescent polymeric colloids onto a flat planar substrate, and then using directional platinum vapor deposition to half coat the exposed colloid surface, making a two faced "Janus" structure. The Janus colloids are then re-suspended from the planar substrate into an aqueous solution containing hydrogen peroxide. Hydrogen peroxide serves as a fuel for the platinum catalyst, which is decomposed into water and oxygen, but only on one side of the colloid. The asymmetry results in gradients that produce enhanced motion, or "swimming". A fluorescence microscope, together with a video camera is used to record the motion of individual colloids. The center of the fluorescent emission is found using image analysis to provide an x and y coordinate for each frame of the video. While keeping the microscope focal position fixed, the fluorescence emission from the colloid produces a characteristic concentric ring pattern which is subject to image analysis to determine the particles relative z position. In this way 3D trajectories for the swimming colloid are obtained, allowing swimming velocity to be accurately measured, and physical phenomena such as gravitaxis, which may bias the colloids motion to be detected.

A method to prepare catalytically active Janus colloids that can "swim" in fluids and determine their 3D trajectories is presented.

We report a method to prepare catalytically active Janus colloids that "swim" in fluids and describe how to determine their 3D motion using fluorescence ...

Combustion Characterization and Model Fuel Development for Micro-tubular Flame-assisted Fuel Cells

Combustion based power generation has been accomplished for many years through a number of heat engine systems. Recently, a move towards small scale power generation and micro combustion as well as development in fuel cell research has created new means of power generation that combine solid oxide fuel cells with open flames and combustion exhaust. Instead of relying upon the heat of combustion, these solid oxide fuel cell systems rely on reforming of the fuel via combustion to generate syngas for electrochemical power generation. Procedures were developed to assess the combustion by-products under a wide range of conditions. While theoretical and computational procedures have been developed for assessing fuel-rich combustion exhaust in these applications, experimental techniques have also emerged. The experimental procedures often rely upon a gas chromatograph or mass spectrometer analysis of the flame and exhaust to assess the combustion process as a fuel reformer and means of heat generation. The experimental techniques developed in these areas have been applied anew for the development of the micro-tubular flame-assisted fuel cell. The protocol discussed in this work builds on past techniques to specify a procedure for characterizing fuel-rich combustion exhaust and developing a model fuel-rich combustion exhaust for use in flame-assisted fuel cell testing. The development of the procedure and its applications and limitations are discussed.

A protocol for creating a model fuel-rich combustion exhaust is developed through combustion characterization and is applied for micro-tubular flame-assisted fuel cell testing and research.

Combustion based power generation has been accomplished for many years through a number of heat engine systems. Recently, a move towards small scale power ...

Two-way Valorization of Blast Furnace Slag: Synthesis of Precipitated Calcium Carbonate and Zeolitic Heavy Metal Adsorbent

The aim of this work is to present a zero-waste process for storing CO2 in a stable and benign mineral form while producing zeolitic minerals with sufficient heavy metal adsorption capacity. To this end, blast furnace slag, a residue from iron-making, is utilized as the starting material. Calcium is selectively extracted from the slag by leaching with acetic acid (2 M CH3COOH) as the extraction agent. The filtered leachate is subsequently physico-chemically purified and then carbonated to form precipitated calcium carbonate (PCC) of high purity (&lt;2 wt% non-calcium impurities, according to ICP-MS analysis). Sodium hydroxide is added to neutralize the regenerated acetate. The morphological properties of the resulting calcitic PCC are tuned for its potential application as a filler in papermaking. In parallel, the residual solids from the extraction stage are subjected to hydrothermal conversion in a caustic solution (2 M NaOH) that leads to the predominant formation of a particular zeolitic mineral phase (detected by XRD), namely analcime (NaAlSi2O6&#8729;H2O). Based on its ability to adsorb Ni2+, as reported from batch adsorption experiments and ICP-OES analysis, this product can potentially be used in wastewater treatment or for environmental remediation applications.

A protocol for the parallel production of precipitated calcium carbonate and zeolitic material from blast furnace slag via mineral carbonation and alkaline hydrothermal conversion, respectively, is presented. The performance of the zeolitic material towards nickel adsorption is tested.

The aim of this work is to present a zero-waste process for storing CO2 in a stable and benign mineral form while producing zeolitic minerals with ...

Production and Characterization of Vacuum Deposited Organic Light Emitting Diodes

A method for producing simple and efficient thermally-activated delayed fluorescence organic light-emitting diodes (OLEDs) based on guest-host or exciplex donor-acceptor emitters is presented. With a step-by-step procedure, readers will be able to repeat and produce OLED devices based on simple organic emitters. A patterning procedure allowing the creation of personalized indium tin oxide (ITO) shape is shown. This is followed by the evaporation of all layers, encapsulation and characterization of each individual device. The end goal is to present a procedure that will give the opportunity to repeat the information presented in cited publication but also using different compounds and structures in order to prepare efficient OLEDs.

A protocol for the production of simple structured organic light-emitting diodes (OLEDs) is presented.

A method for producing simple and efficient thermally-activated delayed fluorescence organic light-emitting diodes (OLEDs) based on guest-host or exciplex ...

Film Control to Study Contributions of Waves to Droplet Impact Dynamics on Thin Flowing Liquid Films

Droplet impact is a very common phenomenon in nature and attracts attention due to its aesthetic fascination and wide-ranging applications. Previous studies on flowing liquid films have neglected the contributions of spatial structures of waves to the impact outcome, while this has recently been shown to have a significant influence on the drop impact dynamics. In this report, we outline a step-by-step procedure to investigate the effect of periodic inlet forcing of a flowing liquid film leading to the production of spatiotemporally regular wave structures on drop impact dynamics. A function generator in connection with a solenoid valve is used to excite these spatiotemporally regular wave structures on the film surface while the impact dynamics of uniform-sized droplets are captured using a high-speed camera. Three distinct regions are then studied; viz. the capillary wave region preceding the large wave peak, the flat film region, and the wave hump region. The effects of important dimensionless quantities such as film Reynolds, drop Weber and Ohnesorge numbers parameterized by the film flow rate, drop speed, and drop size are also examined. Our results show interesting, hitherto undiscovered dynamics brought about by this application of film inlet forcing of the flowing film for both low and high inertia drops.

A protocol to study the contributions of waves to droplet impact dynamics on flowing liquid films is presented.

Droplet impact is a very common phenomenon in nature and attracts attention due to its aesthetic fascination and wide-ranging applications. Previous ...

Delignified densified wood is a new promising and sustainable material that possesses the potential to replace synthetic materials, such as glass fiber reinforced composites, due to its excellent mechanical properties. Delignified wood, however, is rather fragile in a wet state, which makes handling and shaping challenging. Here we present two fabrication processes, closed-mold densification and vacuum densification, to produce high-performance cellulose composites based on delignified wood, including an assessment of their advantages and limitations. Further, we suggest strategies for how the composites can be re-used or decomposed at the end-of-life cycle. Closed-mold densification has the advantage that no elaborate lab equipment is needed. Simple screw clamps or a press can be used for densification. We recommend this method for small parts with simple geometries and large radii of curvature. Vacuum densification in an open-mold process is suitable for larger objects and complex geometries, including small radii of curvature. Compared to the closed-mold process, the open-mold vacuum approach only needs the manufacture of a single mold cavity.

Delignified densified wood represents a new promising lightweight, high-performance and bio-based material with great potential to partially substitute natural fiber reinforced- or glass fiber reinforced composites in the future. We here present two versatile fabrication routes and demonstrate the possibility to create complex composite parts.

Delignified densified wood is a new promising and sustainable material that possesses the potential to replace synthetic materials, such as glass fiber ...