This material is based upon work supported by the Department of&#160;Energy, National Nuclear Security Administration,&#160;under Award Number DE-NA0002377. Funding from the Defense Threat Reduction Agency (DTRA), Grant Number HDTRA1-10-1-0119. Counter-WMD basic research program, Dr. Suhithi M. Peiris, program director is gratefully acknowledged. This work was also supported by the Ministry of Education and Science and Education of the Russian Federation in the framework of Increase Competitiveness Program of NUST &#8220;MISIS&#8221; grant No. K2-2014-001.

1. High-energy Ball Milling
<ol>
	<li>Prepare 35 g of the initial 1:1 molar ratio Ni+Al mixture. In this case, weigh 11.02 g of Al and 23.98 g of Ni powders.</li>
	<li>Use a steel milling jar for HEBM of this system. Ensure that the jar has a higher hardness than the powders to be added, otherwise the powders will damage the jar and contamination will arise. Note: Typical jar choices include steel, zirconium oxide, or tungsten carbide.</li>
	<li>Use a 5:1 ball:powder (charge ratio) for this system, i.e., 175 g...

<ol>
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V., 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=Tailored+Reactivity+of+Ni+AlNanocomposites:+Microstructural+Correlations.">Tailored Reactivity of Ni+AlNanocomposites: Microstructural Correlations.</a> The Journal of Physical Chemistry C. 116 (39), 21027-21038 (2012).</li><li>Qiu, X., Wang, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Bonding+Silicon+Wafers+with+Reactive+Multilayer+Foils.">Bonding Silicon Wafers with Reactive Multilayer Foils.</a> Sensors and Actuators A. 141 (2), 476-481 (2008).</li><li>Wang, J., 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=Joining+of+Stainless-Steel+Specimens+with+Nanostructured+Al/Ni+Foils.">Joining of Stainless-Steel Specimens with Nanostructured Al/Ni Foils.</a> Journal of Applied Physics. 95 (1), 248-256 (2004).</li><li>Rogachev, A. S., Mukasyan, A. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Combustion+of+Heterogeneous+Nanostructural+Systems+(Review).">Combustion of Heterogeneous Nanostructural Systems (Review).</a> Combustion, Explosion, and Shock Waves. (Engl. Transl). 46 (3), 243-266 (2010).</li><li>Granier, J. J., Pantoya, M. L. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Laser+Ignition+of+Nanocomposite+Thermites).">Laser Ignition of Nanocomposite Thermites).</a> Combustion and Flame. 138 (4), 373-383 (2004).</li><li>Bockmon, B. S., Pantoya, M. L., Son, S. F., Asay, B. W., Mang, J. 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A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Heat+of+Combustion+of+Tantalum&#8722;Tungsten+Oxide+Thermite+Composites.">Heat of Combustion of Tantalum&#8722;Tungsten Oxide Thermite Composites.</a> Combustion and Flame. 157 (12), 2326-2332 (2010).</li><li>Leventis, N., Chandrasekaran, N., Sadekar, A. G., Sotiriou-Leventis, C., Lu, H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=One-Pot+Synthesis+of+Interpenetrating+Inorganic/Organic+Networks+of+CuO/Resorcinol-Formaldehyde+Aerogels:+Nanostructured+Energetic+Materials.">One-Pot Synthesis of Interpenetrating Inorganic/Organic Networks of CuO/Resorcinol-Formaldehyde Aerogels: Nanostructured Energetic Materials.</a> Journal of the American Chemical Society. 131 (13), 4576-4577 (2009).</li><li>Zhang, K., Rossi, C., Ardila Rodriguez, G. 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The authors have nothing to disclose.

The protocol provides a detailed description for preparation of reactive energetic (Ti+C, Ta+C, Ni+Al) nanocomposites with tailored microstructure by using the short-term HEBM method. HEBM of gasless heterogeneous mixtures involve their processing in a high-speed planetary ball mill, where the particles of the mixture are subjected to mechanical impact with a force sufficient for breakdown of brittle components (e.g. graphite) and deformation of plastic components (e.g., Al, Ti, Ta, Ni). Brittle reactan...

Classical energetic materials, i.e., explosives, propellants and pyrotechnics are a class of material with a high amount of stored chemical energy that can be released during rapid exothermic reaction1-5. For example, explosives are usually generated by combining fuel and oxidizer groups into one molecule. The energy density of those materials is very high. For example, upon decomposition trinitrotoluene (TNT) releases 7.22 kJ/cm3 and forms 8.36 moles of gases per 100 g (Table 1) in a very short period of time. These materials are composed of micrometer-scale organic and inorganic species (fuels and oxidizers).
Thermite systems, where reactions take place between the inorganic compound, i.e., reducing metals (e.g., Al) and oxides (Fe2O3, CuO, Bi2O3), belong to another type of energetic materials. The energy density (15-21 kJ/cm3) of such systems exceeds that of TNT, however the amount of gas products (0.15-0.6 moles per 100 g) is typically much less than for explosives (Table 1). Also, the nano-thermites may show extremely high velocity of combustion wave propagation (&#62;1,000 m/sec)2-5.
It was recently shown6-12 that a number of gasless heterogeneous reactive systems (Ni+Al, Ti+C, Ti+B) that form intermetallic or refractory compounds could also be considered as energetic materials. The energy densities (kJ/cm3) of those systems are closer or higher than that of TNT (Table 1). At the same time, the absence of gas products during the reaction makes such materials excellent candidates for a variety of applications including synthesis of nanomaterials, reactive bonding of refractory and dissimilar parts, gasless micro power generators, etc.11-17. However, the relatively high ignition temperature of those systems (900-3,000 K, see Table 1) compared to thermites (~1,000 K) hinders their applications. The preparation of engineered nanostructured composites could significantly enhance the ignition and combustion characteristics of gasless heterogeneous systems12-14, 17.
Many methods have been developed to fabricate the engineered energetic nanocomposites, such as ultrasonic mixing18,19, self-assembly approaches5, sol-gel20-22, vapor deposition techniques16,17,23,24, as well as high-energy ball milling (HEBM)1,5. The disadvantage of ultrasonic mixing of nano-powder is that a thick (5-10 nm) oxide shell on metal nanoparticles reduces energy density and degrades the combustion performance of reactive mixtures. Also, the distribution of fuel and oxidizer is not uniform, and the interfacial contact between reactants is not intimate. Sol-gel and self-assembly strategies were developed for preparation of specific thermite nanocomposites. Despite being low-cost techniques, those strategies are not green from an environmental standpoint. Moreover, large amounts of impurities are introduced into prepared composites. Vapor deposition or magnetron sputtering is used to prepare reactive multi-layer foils and core-shell energetic materials. It provides a pore-free and well-defined geometry of composites that simplifies theoretical modeling and enhances accuracy. However, this technology is expensive and difficult to scale up. Furthermore, the prepared layered nanocomposites are unstable in certain conditions.
High-Energy Ball Milling (HEBM) is an environmentally friendly, easily scalable approach that allows effective fabrication of nanostructured energetic composites5,9-14. HEBM is inexpensive and can be used with various reactive material compositions (e.g., thermites, reactions that form intermetallics, carbides, borides, etc.).
The protocol provides a detailed description for preparation of reactive energetic (Ni+Al, Ti+C, Ta+C) nanocomposites with tailored microstructure by using the short-term HEBM method. It also describes a high-speed thermal imaging technique to determine the ignition/combustion characteristics of as-fabricated energetic materials. Finally it shows the analysis of the microstructure of the nanocomposites using Field Emission Scanning Electron Microscope (FESEM) Equipped by Focused Ion Beam (FIB). The protocol is an important guide for the preparation of different energetic nanomaterials (gasless and thermite systems) that could be used as either high energy density sources or for synthesis and processing of advanced nanomaterials by combustion-based approaches.

<table border="0" cellpadding="0" cellspacing="0">
	<tbody>
		<tr>
			<td>Titanium</td>
			<td>Alfa Aesar</td>
			<td>42624</td>
			<td>Particle size: -325 mesh</td>
			<td>Purity, 99.5%</td>
		</tr>
		<tr>
			<td>Graphite</td>
			<td>Alfa Aesar</td>
			<td>46304</td>
			<td>Particle size: 7-11 micron</td>
			<td>Purity, 99%</td>
		</tr>
		<tr>
			<td>Nickel</td>
			<td>Alfa Aesar</td>
			<td>10256</td>
			<td>Particle size: 3-7 micron</td>
			<td>Purity, 99.9%</td>
		</tr>
		<tr>
			<td>Aluminum</td>
			<td>Alfa Aesar</td>
			<td>11067</td>
			<td>Particle size: -325 mesh</td>
			<td>Purity, 99.5%</td>
		</tr>
		<tr>
			<td>Tantalum</td>
			<td>Materion advanced chemicals</td>
			<td>T-2017</td>
			<td>Particle size: 325 mesh</td>
			<td>Purity, 99.9%</td>
		</tr>
		<tr>
			<td>Carbon lampblack</td>
			<td>Fisher scientific</td>
			<td>C198-500</td>
			<td>Particle size: 0.1 micron</td>
			<td>Purity, 99.9%</td>
		</tr>
		<tr>
			<td>Tungsten wire</td>
			<td>Mcmaster Carr</td>
			<td>n/a</td>
			<td>0.032&#34; diameter</td>
			<td>n/a</td>
		</tr>
		<tr>
			<td>Planetary Ball Mill</td>
			<td>Retsch GmbH, Germany</td>
			<td>n/a</td>
			<td>n/a</td>
			<td>n/a</td>
		</tr>
		<tr>
			<td>Uniaxial press</td>
			<td>Carver Hydraulic</td>
			<td>n/a</td>
			<td>n/a</td>
			<td>n/a</td>
		</tr>
		<tr>
			<td>Sieve shaker</td>
			<td>Gilson performer</td>
			<td>n/a</td>
			<td>5mm diameter</td>
			<td>n/a</td>
		</tr>
		<tr>
			<td>Cylindrical stainless steel press die</td>
			<td>Action Machine</td>
			<td>n/a</td>
			<td>n/a</td>
			<td>n/a</td>
		</tr>
		<tr>
			<td>Stainless steel sieves</td>
			<td>Mcmaster Carr</td>
			<td>Type 304</td>
			<td>n/a</td>
			<td>n/a</td>
		</tr>
		<tr>
			<td>High-speed thermal camera (SC6000)</td>
			<td>FLIR</td>
			<td>n/a</td>
			<td>n/a</td>
			<td>n/a</td>
		</tr>
		<tr>
			<td>Helios NanoLab 600, Field Emission Scanning Electron Microscope (FESEM) Equipped by Focus Ion Beam (FIB)</td>
			<td>FEI</td>
			<td>n/a</td>
			<td>n/a</td>
			<td>n/a</td>
		</tr>
		<tr>
			<td>Cylindrical reactor with a vacuum pomp</td>
			<td>Action Machine</td>
			<td>n/a</td>
			<td>n/a</td>
			<td>n/a</td>
		</tr>
		<tr>
			<td>Autoslice and View (S&#38;V)</td>
			<td>FEI</td>
			<td>n/a</td>
			<td>n/a</td>
			<td>n/a</td>
		</tr>
		<tr>
			<td>Avizo Fire</td>
			<td>FEI</td>
			<td>n/a</td>
			<td>n/a</td>
			<td>n/a</td>
		</tr>
	</tbody>
</table>

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.

To prepare nanostructured energetic composites, a mixture of desired powdered components (typically micrometer-sized) is mechanically treated under preset milling conditions. Processing time (typically minutes) is accurately controlled to generate the compositionally homogenized nanocomposite particles but not permitting the self-sustaining chemical reaction to initiate during milling.
Figure 1 and Video 1 show that contact surface area between the reactants i...

Watch this Scientific Journal Video about Preparation and Reactivity of Gasless Nanostructured Energetic Materials at JoVE.com

Preparation and Reactivity of Gasless Nanostructured Energetic Materials

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 ...

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10.1K Views.  University of Notre Dame.  Questo protocollo descrive la preparazione di gasless nanostrutturati materiali energetici (Ni + Al, Ta + C, Ti + C) utilizzando la sfera ad alta energia a breve termine di fresatura (HEBM) tecnica. Viene inoltre descritto un metodo di imaging termico ad alta velocità per studiare la reattività di nanocompositi fabbricati meccanicamente. Questi protocolli possono essere estesi ad altri materiali energetici nanostrutturati reattiva. 