As part of a new materials effort, we are exploring the use of sol-gel chemistry to manufacture energetic materials. Traditional manufacturing of energetic materials involves processing of granular solids. One application is the production of detonators where powders of energetic material and a binder are typically mixed and compacted at high pressure to make pellets. Performance properties are strongly dependent on particle size distribution, surface area of its constituents, homogeneity of the mix, and void volume.The goal is to produce detonators with fast energy release rate that are insensitive to unintended initiation. In this paper, we report results of our early work in this field of research, including the preparation of detonators from xerogel molding powders and aerogels, comparing the material properties with present state-of-the-art technology.
Partielles Phasenverhalten von HMXaDMSO-Lo ÈsungenDas Phasendiagramm von HMXaDMSO und der Solvatkomplex HMX-(DMSO) 2 wurde untersucht mittels Sichtkontrolle, HPLC, DSC und optischer Mikroskopie. Die Sichtkontrolle zeigte, daû der solvatisierte Komplex einen inkongruenten Schmelzpunkt aufweist, d.h. der Schmelzpunkt des solvatisierten Kristalls erscheint innerhalb des Bereichs des Phasendiagramms, wo sich das HMX abscheidet. Wenn der solvatisierte Kristall aus der Lo Èsung entfernt und erhitzt wird, zerfa Èllt er in festes HMX und DMSO bei der peritektischen Temperatur ( $ 70 C). Unter Verwendung der HPLC wurde die A È nderung der Konzentration in der¯u Èssigen Phase als Funktion der Temperatur aufgezeichnet, um die Phasengrenze zwischen DMSO und Solvatkomplex basierend auf der Sichtkontrolle zu besta Ètigen. Mit einem Polarisationsmikroskop wurde die Abscheidung in den geimpften Lo Èsungen bei verschiedenen Konzentrationen ebenfalls untersucht, um diese Befunde zu besta Ètigen. Es ist mo Èglich, daû auch ein 1 : 1 Komplex existiert, aber es wurde keine Besta Ètigung fu Èr solch einen Komplex bei diesen Experimenten gefunden. Caracte Âristique de phase partielle de solutions HMXaDMSO Le diagramme de phase de HMXaDMSO et du complexe solvate  HMX-(DMSO) 2 a e Âte  e Âtudie  par observation visuelle, HPLC, DSC et microscopie optique. L'observation visuelle a montre  que le complexe solvate  posse Âdait un point de fusion incongru, c. a Á. d. le point de fusion du cristal solvate  apparaõ Ãt dans le domaine du diagramme de phase, la Á ou Á se produit la pre Âcipitation de HMX. Lorsque le cristal solvate  est retire  de la solution et chauffe Â, il se de Âcompose en HMX solide et DMSO a Á la tempe Ârature pe Âritectique ( % 70 C). L'utilisation de la HPLC a permis d'enregistrer la modi®cation de la concentration en phase liquide en fonction de la tempe Ârature pour con®rmer la limite de phase entre le DMSO et le complexe solvate  observe Âe visuellement. A l'aide d'une microscopie a Á lumie Áre polarise Âe, on a e Âgalement e Âtudie  la dissolution dans des solutions ensemence Âes pour diffe Ârentes concentrations a®n de con®rmer ces re Âsultats. Il est possible qu'il existe e Âgalement un complexe 1 : 1 mais ces expe Âriences n'ont pas permis de con®rmer l'existence d'un tel complexe. SummaryThe phase diagram of HMXaDMSO and the solvated complex HMXÁ(DMSO) 2 has been investigated by visual observation, high performance liquid chromatography (HPLC), differential scanning calorimetry (DSC), and optical microscopy. Visual observations showed the solved complex exhibited an incongruent melting point, i.e., the melting point of the solvated crystal occurs within the region of the phase diagram where HMX itself precipitates. If the solvated crystal is removed from solution and heated, it reverts to solid HMX and DMSO at the peritectic temperature ( $ 70 C). Using HPLC the change in concentration of the liquid phase was monitored as a function of temperature to con®rm the phase line of the DMSOasolvated complex bas...
The preparation of 3‐chloro‐5‐methoxypyridine N‐oxide and its nitration are reported. Mononitration yields 5‐chloro‐3‐methoxy‐2‐nitro‐pyridine N‐oxide while more drastic conditions give 3‐chloro‐5‐methoxy‐2,6‐dinitropyridine. Removal of various substituents by base hydrolysis is also discussed.
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