Detonation Synthesis Research Articles

Secondary-explosion modification study on gaseous detonation synthesis of Fe@C nanoparticles

To enhance the graphitization degree of Fe@C nanoparticles synthesized via gaseous detonation, this study employed ferrocene as the precursor and hydrogen–oxygen mixed gas as the explosion source to investigate the effects of secondary-explosion on the phase composition, morphology, and magnetic properties of carbon-encapsulated iron nanoparticles. The results show that after the secondary-explosion, the phase composition of Fe@C nanoparticles changes significantly, with partial oxidation of iron carbide/iron to FeO. The morphology remains largely unchanged, with particle sizes between 20–40 nm, but the crystallinity of both the metal core and carbon layer improves markedly, and lattice fringes become more distinct. The saturation magnetization(Ms) and residual magnetization(Mr) of Fe@C nanoparticles decrease by 56.7 % and 69 %, respectively, while the coercivity force shows little change.

Extrastrong aggregates of detonation nanodiamonds: structure and formation

Commercially available powders of detonation nanodiamond (DND) contain extrastrong 20–120 nm sized aggregates, in an amount sometimes up to 50% by mass sustainable to the conventional methods of deaggregation. It demonstrates the significant inhomogeneity structure of products of detonation synthesis and noticeably reduces the yield of 4.0 − 5.0 nm individual isolated particles obtained from DNDs. The presence of these aggregates is obviously related to the some essential features of detonation synthesis. This work presents the results of studying such extrastrong aggregates from DND powder. In order to determine the structure we applied the heat treatment of samples in vacuum and in air, and the subsequent study using Raman spectroscopy, X-ray diffraction, UV–vis spectroscopy, analysis of specific surface and dynamic light scattering (DLS). As a result, a structural model of extrastrong aggregates is proposed. It is shown that extrastrong aggregates consist notably of relatively large (∼8.0 nm) single crystalline diamond particles bonded by facets and covered by smaller 4.5 − 3.0 nm and less crystalline grains. Our results add the details for description of formation processes of diamond particles and aggregates in detonation synthesis from excessive carbon in the composition of explosives.

A New Method for Analysis of Martials Nano and Micro Electronics Technologies

This final qualifying work investigates prospective microelectronic and nano electronic materials. The purpose of the final qualifying mission is to evaluate potential manufacturing technologies and materials. In the first phase of the endeavor, potential materials for microelectronics and nanoelectronics were investigated. Graphene, fullerenes, fullerites, carbon nanotubes (CNT), nanofibers, ferrites, barium hexaferrite, nano powders, and epitaxial coatings are among these substances. An investigation into diverse methodologies pertaining to the production of auspicious materials was undertaken during the preliminary stage of the undertaking. Molecular beam epitaxy, pulsed laser deposition, spray deposition, physical vapor deposition (PVD), chemical solution deposition, gas-phase synthesis, electrospinning, chemosynthesis, detonation synthesis and electric explosion, chemical vapor deposition (CVD), spray deposition, physical vapor deposition (PVD), and the sol-gel method were among these processes.

Structure formation of ultradispersed diamond by detonation synthesis

In the present work, we report on structure formation of ultradispersed diamond through detonation synthesis. In particular, based on the present data, we can state that ultradispersed diamond of detonation (UDD) synthesis is characterized by a rail substructure formation, which is typical for diamonds of dynamic and static synthesis formed from graphite by the martensitic mechanism. The formation of UDD is characterized by a two-stage process: the first stage is the formation of graphite from detonation products, and the second stage is the transformation of graphite into diamond by the martensitic mechanism. A microlamellar substructure in the rails of diamonds formed from the original graphite is due to the presence of basic packing defects that is characteristic for covalent crystals with a wurtzite lattice deformed at high pressures and temperatures typical for lonsdaleite. The presence of lonsdaleite in UDD also indicates its formation in the process of synthesis of diamond from graphite through the martensitic transformation.

Nanometer battery materials from explosives

The growth of Li1+xMn2O4 via detonation reaction was investigated with respect to the presence of energetic precursors, such as the metallic nitrates and the degree of confinement of the explosive charge. The detonation products were characterized by scanning electron microscopy. Powder X-ray diffraction and transmission electron microscopy were used to characterize the products. Li1+xMn2O4 with 1 ∼ 2μm spherical morphology and more uniform secondary particles, but with smaller primary particles of diameters from 20 to 60 nm and a variety of morphologies were found. The oxides produced by this cheap method affirmed the validity of detonation synthesis of nano-size powders.

Air-thermal oxidation of diamond nanopowders obtained by the methods of mechanical grinding and detonation synthesis

In this work, using the methods of X-ray phase analysis, transmission electron microscopy, X-ray photoelectron spectroscopy and Raman spectroscopy, the features of the impact of annealing in air within the temperature range of t = 200÷÷550 °C on the morphology, elemental and phase composition, chemical state and structure of primary particles of nanopowders obtained by grinding natural diamond and the method of detonation synthesis are studied. It is shown that heat treatment in air at given values of temperature and heating time does not affect the elemental composition and atomic structure of primary particles of nanopowders obtained both by the methods of detonation synthesis (DND) and natural diamond grinding (PND). Using XPS, Raman spectroscopy, and transmission electron microscopy, it has been found that annealing in air within the temperature range of 400–550 °C results in the effective removal of amorphous and graphite-like carbon atoms in the sp2- and sp3-states from diamond nanopowders by oxidation with atmospheric oxygen. In the original DND nanopowder, containing about 33.2 % of non-diamond carbon atoms of the total number of carbon atoms, after annealing for 5 h at a temperature of 550 °C, the relative number of nondiamond carbon atoms in the sp2-state decreased to ~21.4 %. In this case, the increase in the relative number of carbon atoms in the sp3-state (in the lattice of the diamond core) and in the composition of oxygen-containing functional groups ranged from ~39.8 % to ~46.5 % and from ~27 % to ~32.1 %, respectively. In the PND nanopowder, which prior to annealing contains about 10.6 % of non-diamond carbon atoms in the sp2-state of the total number of carbon atoms, after annealing under the same conditions as the DND nanopowder, their relative number decreased to 7.1 %. The relative number of carbon atoms in the sp3-state increased from 72.9 % to 82.1 %, and the proportion of carbon atoms in the composition of oxygen-containing functional groups also slightly increased from 10.2 % to 10.8 %. It is demonstrated that the annealing of PND and DND nanopowders in air leads to a change in their color, they become lighter as a result of oxidation of non-diamond carbon by atmospheric oxygen. The maximum effect is observed at a temperature of 550 °C and an annealing time of 5 h. In this case, the weight loss of PND and DND nanopowders after annealing was 5.37 % and 21.09 %, respectively. The significant weight loss of DND nanopowder compared to PND is primarily caused by the high content of non-diamond carbon in the initial state and the high surface energy of primary particles due to their small size.

Detonation Synthesis as a Modern Eco-Friendly Method for Obtaining 2D Nanocarbons

Detonation Synthesis as a Modern Eco-Friendly Method for Obtaining 2D Nanocarbons

Detonation Synthesis Nanodiamond Soot as a Promising Filler for Polymer Composites

In this work, the results of a complex investigation of structure and properties of nanodiamond soot (NDS) of detonation synthesis are presented. Size distribution of NDS particles, dispersed in different liquid media, was investigated using dynamic light scattering and laser diffraction analysis methods. The results of the investigation, as well as the results of zeta-potential measurements, allowed us to characterize the agglomeration process of the NDS particles as independent of the medium, making NDS a good model filler for research of composite-modified nanosized particles. Additional data obtained using scanning electron microscopy, scanning tunneling microscopy, atomic force microscopy, X-ray diffraction, and Raman spectroscopy, demonstrated that in NDS the spherical nanodiamond (ND) particles with diameter ~5 nm are densely packed into strong-coupled aggregates with diameter ~300 nm, surrounded by graphite nanoribbons. X-ray diffraction analysis estimated the volume fraction of NDs in NDS as ~45 vol.%, simultaneously showing that the graphite is not defective, which was confirmed with the electron diffraction method. It was demonstrated that this structure of NDS allows to efficiently use NDS as a filler for polymer composites to increase polymer characteristics such as electrical conductivity or tribological characteristics, similarly to conventionally applied fillers such as carbon black.

Relating detonation parameters to the detonation synthesis of silicon carbide

Detonation synthesis of silicon carbide (SiC) nanoparticles from carbon liberated by negatively oxygen balanced explosives was evaluated in a 23 factorial design to determine the effects of three categorical experimental factors: (1) cyclotrimethylene-trinitramine (RDX)/2,4,6-trinitrotoluene (TNT) ratio, (2) silicon (Si) additive concentration, and (3) Si particle size. These factors were evaluated at low and high levels as they relate to the detonation performance of the explosive and the solid Si-containing phases produced. Detonation velocity and Chapman–Jouguet (C–J) detonation pressure, which were measured using rate stick plate dent tests, were evaluated. Solid detonation product mass, silicon carbide product concentration, and residual silicon concentration were evaluated using the x-ray diffraction analysis. The factors of Si concentration and the RDX:TNT ratio were shown to affect detonation performance in terms of detonation velocity and C–J pressure by up to 10% and 22%, respectively. Increased concentration of Si in the reactants improved the average SiC concentration in the detonation products from 1.9 to 2.8 wt. %. Similarly, increasing the ratio of RDX to TNT further oxidized detonation products and reduced the average residual Si remaining after detonation from 8.6 to 2.8 wt. %. A 70:30 mass ratio mixture of RDX to TNT loaded with 10 wt. % < 44 μm silicon powder produced an estimated 1.33 g of nanocrystalline cubic silicon carbide from a 150-g test charge. Using a lower concentration of added silicon with a finer particle size reduced SiC yield in the residue to 0.38 g yet improved the SiC to residual Si ratio to 1.64:1.

Experimental setup for elemental analysis using prompt gamma rays at research reactor IBR-2

The new experimental setup has been built at the 11b channel of the IBR-2 research reactor at FLNP, JINR, to study the elemental composition of samples by registration of prompt gamma emission during thermal neutron capture. The setup consists of a curved mirror neutron guide and a radiation-resistant HPGe high-purity germanium detector. The detector is surrounded by lead shielding to suppress the natural background gamma level. The sample is placed in a vacuum channel and surrounded by a LiF shield to suppress the gamma background generated by scattered neutrons. This work presents characteristics of the experimental setup. An example of hydrogen concentration determining in a diamond powder made by detonation synthesis is given and on its basis, the sensitivity of the setup is calculated being ∼4 μg.

Detonation synthesis of nanoscale silicon carbide from elemental silicon

Direct reaction of precursors with the products of detonation remains an underexplored area in the ever-growing body of detonation synthesis literature. This study demonstrated the synthesis of silicon carbide during detonation by reaction of elemental silicon with carbon products formed from detonation of RDX/TNT mixtures. Continuum scale simulation of the detonation showed that energy transfer by the detonation wave was completed within 2–9 μs depending on location of measurement within the detonating explosive charge. The simulated environment in the detonation product flow beyond the Chapman-Jouguet condition where pressure approaches 27 GPa and temperatures reach 3300 K was thermodynamically suitable for cubic silicon carbide formation. Carbon and added elemental silicon in the detonation products remained chemically reactive up to 500 ns after the detonation wave passage, which indicated that the carbon-containing products of detonation could participate in silicon carbide synthesis provided sufficient carbon-silicon interaction. Controlled detonation of an RDX/TNT charge loaded with 3.2 wt% elemental silicon conducted in argon environment lead to formation of ∼3.1 wt% β-SiC in the condensed detonation products. Other condensed detonation products included primarily amorphous silica and carbon in addition to residual silicon. These results show that the energized detonation products of conventional high explosives can be used as precursors in detonation synthesis of ceramic nanomaterials.

Application of ultrasounds to improve the dispersion of nanoparticulates in a Al-Si7Mg0.6 alloy reinforced with 0.5 wt. % of nanodiamonds

One of the most important technical barriers that hinders the development and implementation of nanoparticulate reinforced aluminium alloys is the difficulty to avoid the formation of clusters and to obtain their homogeneous distribution. The present work summarises the results obtained with the use of an ultrasound probe that was immersed into the melt alloy containing nanodiamond particulates just before the casting step. The microstructure and tensile properties of the obtained specimens are compared with nanoreinforced samples obtained with conventional stir cast process. The materials used in the study are the Al-Si7Mg0.6 casting alloy and nanodiamond particulates obtained by detonation synthesis. Samples containing up to 0.5 wt.% of nanodiamonds have been obtained. The use of the ultrasound probe results in the elimination of nanoparticulate clusters and provides an improvement of mechanical properties in comparison to properties measure with the unreinforced alloy and also with the conventionally stir cast composite.

Synthesis of turbostratic nanoscale graphene via chamber detonation of oxygen/acetylene mixtures

AbstractA study of the detonation synthesis method to make graphene and the properties of the resulting graphene is presented. The gaseous precursors are mixtures of oxygen and acetylene with oxygen/carbon molar ratios of O/C = 0.25 to 0.75. Chamber pressure and temperature data indicate pressures ≤ 300 psi and temperatures of 2550 ± 100K after initiation of the reaction mixture. The graphene material collected from the chamber after the detonation was characterized by Raman, XRD (X‐ray diffraction), BET, SEM (scanning electron microscopy), TEM (transmission electron microscopy), and so on. The material properties divide into two groups: low O/C (≤ 0.45) and high O/C (≥ 0.5). Low O/C graphene appears as a low density, aerosol gel with ∼8 weakly associated, disordered turbostratic layers with a lateral extent of 20 to 30 nm. High O/C graphene appears as a denser powder with ∼30 weakly associated turbostratic layers, with a lateral extent of 100 to 200 nm. We conclude, as we have previously, that the high detonation temperature during the reaction is the primary reason that graphene is formed rather than soot. Differentiation into two types of graphene products is hypothesized to be a result of aggregation kinetics to form a static gel that pre‐empts layering (stacking) when O/C is low.

Biodistribution of Detonation Synthesis Nanodiamonds in Mice after Intravenous Administration and Some Biochemical Changes in Blood Plasma.

Biodistribution of nanodiamonds in mice after intravenous administration, activities of AST and ALT, and the level of bilirubin in the blood plasma were studied in 2.5 h and 10, 35, and 97 days after injection of nanodiamonds. In 2.5 h after intravenous injection, nanodiamonds mainly accumulate in the lungs and liver. Then, redistribution of nanodiamonds from all organs to the liver was observed. Activities of AST and ALT and the level of bilirubin in the blood increased after 2.5 h and then decreased to the initial values.

Diaphite-structured nanodiamonds with six- and twelve-fold symmetries

Nanodiamonds (ND) with 1-5 nm dimensions found in meteorites or produced by chemical vapour deposition (CVD) and detonation synthesis are typically described in terms of an sp3-bonded carbon network. However, ultra-high-resolution transmission electron microscopy (uHRTEM) combined with density functional theory (DFT) modelling leads to a different structural interpretation. uHRTEM imaging and nanodiffraction studies of many NDs show six-fold symmetry features whose identity has long been controversial. We also observe diffraction patterns with twelve equally-spaced and symmetrically but unequally arranged reflections, indicating structures with crystallographically-forbidden ideal and distorted twelve-fold symmetry. Structural models based on our DFT calculations lead to an interpretation of these unusual features found throughout the meteoritic and CVD samples in terms of sp3 domains arranged around and coherently bonded to graphitic domains embedded within the diamond matrix. The bonding at the sp2-sp3 interface can explain the unusual features observed in electron energy-loss spectra (EELS) below the onset of the main diamond C1s core-loss edge leading to predictions of low-dimensional conductivity behaviour. The presence of sp2- as well as sp3-bonded regions allows us to interpret previously unexplained features of the Raman spectra and EELS data of ND materials.

Fabrication of Detonation Nanodiamonds Containing Silicon‐Vacancy Color Centers by High Temperature Annealing

Detonation nanodiamonds (DNDs) with sizes below 10 nm have attracted attention as single photon emitters with potential in many research fields from life sciences to quantum technologies. However, while nitrogen‐vacancy (NV) color centers are found in nanodiamonds directly after the detonation synthesis without the need for irradiation or annealing, silicon‐vacancy (SiV) color centers are not present in these pristine samples. Herein, SiV centers are created in DNDs by an annealing treatment up to 1100 °C in high vacuum. As silicon is not added, the precursor of the SiV centers must be pristine silicon impurities inside the nanodiamond lattice. A sharp emission line at the wavelength of 737 nm with a linewidth of 7.7 nm is observed in DNDs that are electron irradiated before annealing. This wavelength is consistent with the characteristic emission line of SiV centers and its linewidth is comparable with that in larger nanodiamonds created by chemical vapor deposition and subsequent milling. The average lifetime (0.4 ± 0.04 ns) of the fluorescence, which is in the range of reported lifetimes in nanodiamonds, also support that the observed emission peak are due to SiV centers in DNDs.

Submicrosecond Aggregation during Detonation Synthesis of Nanodiamond.

Detonation nanodiamond (DND) is known to form aggregates that significantly reduce their unique nanoscale properties and require postprocessing to separate. How and when DND aggregates is an important question that has not been answered experimentally and could provide the foundation for approaches to limit aggregation. To answer this question, time-resolved small-angle X-ray scattering was performed during the detonation of high-explosives that are expected to condense particulates in the diamond, graphite, and liquid regions of the carbon phase diagram. DND aggregation into low fractal dimension structures could be observed as early as 0.1 μs, along with a separate scattering population also observed from an explosive that produces primarily graphitic products. A counterexample is the case of a high-explosive that produces nano-onions, where no hierarchical scattering was observed for at least 10 μs behind the detonation front. These results suggest that DND aggregation occurs on time scales comparable to particle formation.

Synthesis of Oxide Ceramics in Detonating Atmosphere

A detonation process based on 2,4,6 trinitrotoluene (TNT), used as an energetic reagent, was successfully implemented in the synthesis of a series of metal oxide ceramics. TNT offers better physicochemical and mechanical properties than the energetic compounds traditionally used in such processes, thus offering safer handling and transport conditions. The experimental procedure, which consisted to of mixing the energetic molecule with a ceramic salt, was simple to perform. The detonation products were characterized by X-ray diffraction, scanning and transmission electron microscopies, energy dispersive X-ray spectroscopy and nitrogen physisorption. The as-synthesized ceramic powders (CeO2, HfO2, Nb2O5, and In2O3) were crystalline and made of nano-sized quasi-spherical particles. This investigation provides an enhanced detonation synthesis process for elaborating ceramics. The majority of the oxide materials mentioned in this study had never previously been prepared by the detonation process.

Several Aspects of Application of Nanodiamonds as Reinforcements for Metal Matrix Composites

After detonation synthesis, primary nanodiamond particles are around 4–6 nm in size. However, they join into agglomerates with larger parameters and weak bonds between particles. The introduction of agglomerates into a metal matrix can lead to the weakness of composites. This paper demonstrates the possibility of obtaining a non-agglomerated distribution of nanodiamonds inside a metal matrix. The fabrication method was based on mechanical alloying to create additional stresses and deformations by phase transformations during treatment in a planetary mill. According to the findings, the starting temperature of the reaction between the non-agglomerated nanodiamonds and aluminium matrix reduces to 450 °C. Furthermore, the paper shows that existing methods (annealing for the transformation of a diamond structure into graphitic material and cleaning from this graphitic material) cannot reduce the sizes of nanodiamonds in the agglomerated state. Agglomerated nanodiamonds transform into carbon onions (graphitic material) during annealing in a vacuum in the following way: the nanodiamonds located in the surface layers of the agglomerate are the first to undergo the complete transformation followed by the transformation of nanoparticles in its deeper layers. In the intermediate state, the agglomerate has a graphitic surface layer and a core from nanodiamonds: cleaning from graphite cannot reduce nanodiamond particle size.

Composition and Chemical State of Nanopowder Particles Obtained by Grinding Natural Diamond and by Detonation Synthesis

The initial composition and chemical state of primary particles of nanopowders obtained by grinding natural diamond and detonation synthesis have been investigated using X-ray photoelectron spectroscopy. It is shown that the primary particles of both nanopowders contain mainly carbon and oxygen atoms. Signals from nitrogen, sulfur, chlorine, and metal atoms do not exceed the noise level in the photoelectron spectrum. It has been found that in the primary particles of detonation synthesis nanopowder and nanopowder obtained by grinding natural diamond, the proportion of carbon atoms is ~ 46.5 and ~ 67.8% in the sp1-hybridization state, ~ 26.8 and ~ 17.4% in sp2 – hybridization, and ~ 26.7 and ~ 14.7%, respectively, in the composition of oxygen-containing functional groups.