Pushing the limits of energetic materials - the synthesis and characterization of dihydroxylammonium 5,5'-bistetrazole-1,1'-diolate

The safe preparation and characterization (XRD, NMR and vibrational spectroscopy, DSC, mass spectrometry, sensitivities) of a new explosive dihydroxylammonium 5,5'-bistetrazole-1,1'-diolate (TKX-50) that outperforms all other commonly used explosive materials is detailed. While much publicized high-performing explosives, such as octanitrocubane and CL-20, have been at the forefront of public awareness, this compound differs in that it is simple and cheap to prepare from commonly available chemicals. TKX-50 expands upon the newly exploited field of tetrazole oxide chemistry to produce a material that not only is easily prepared and exceedingly powerful, but also possesses the required thermal insensitivity, low toxicity, and safety of handling to replace the most commonly used military explosive, RDX (1,3,5-trinitro-1,3,5-triazacyclohexane). In addition, the crystal structures of the intermediates 5,5'-bistetrazole-1,1'-diol dihydrate, 5,5'-bistetrazole-1,1'-diol dimethanolate and dimethylammonium 5,5'-bistetrazole-1,1'-diolate were determined and presented

A Laboratory Preparation of High-Purity Calcium Cyanamide

Calcium cyanamide is an important fertilizer and a chemical precursor. However, its large scale synthesis is extremely energy intensive via the historical Frank–Caro synthesis of fixing atmospheric nitrogen with calcium carbide at an elevated temperature, and the product material contains a large number of impurities. In this work, we prepare calcium cyanamide in a purity higher than that achievable by the Frank–Caro route in a convenient laboratory metho

Detection of high-energy compounds using photoluminescent silicon nanocrystal paper based sensors

Luminescent silicon nanocrystals (Si-NCs) surface functionalized with dodecyl groups were exposed to solutions of nitroaromatic compounds including nitrobenzene, nitrotoluene, and dinitrotoluene. It was found that Si-NC luminescence was quenched upon exposure to nitroaromatics via an electron transfer mechanism as indicated by Stern-Volmer analysis. This quenching was exploited and a straightforward paper-based Si-NC sensor was developed. This paper motif was found to be sensitive to solution, vapor, and solid phase nitroaromatics, as well as solution borne RDX and PETN. \ua9 2014 The Royal Society of Chemistry.Peer reviewed: YesNRC publication: Ye

Synthesis and Energetic Characterization of Borane-Amines on High-Nitrogen Heterocycles

Borane-amines have garnered attention over the last several decades in a variety of applications, ranging from hydrogen storage materials to hypergolic fuel systems. An investigation into the synthesis of borane-amines with high-nitrogen content heterocycles was undertaken in this work. Borane-amines were formed by the reaction of BH3·Me2S in tetrahydrofuran (THF) with the requisite nitrogen-containing heterocycle and isolated by placing the crude reaction mixture in hexanes to precipitate the product. X-ray crystallography, thermogravimetric analysis (TGA), high resolution mass spectroscopy (HRMS), 1H NMR, 13C NMR, and 11B NMR were utilized for product characterization, while impact and friction sensitivity testing were conducted to identify sensitivity in the synthesized compounds. Most isolated borane-amines, except one, were found to decompose in the atmosphere and were more sensitive to mechanical stimuli than their starting materials; however, all synthesized compounds were found to be hypergolic in the presence of white fuming nitric acid (WFNA)