The initial interaction mechanism is very important for the design and safety of nano-scale composite energetic materials composed of ammonium dinitramide (ADN) and nitrocellulose (NC). The thermal behaviors of ADN, NC and an NC/ADN mixture under different conditions were studied by using differential scanning calorimetry (DSC) with sealed crucibles, an accelerating rate calorimeter (ARC), a self-developed gas pressure measurement instrument and a DSC-thermogravimetry (TG)—quadrupole mass spectroscopy (MS)—Fourier transform infrared spectroscopy (FTIR) combined technique. The results show that the exothermic peak temperature of the NC/ADN mixture shifted forward greatly in both open and closed circumstances compared to those of NC or ADN. After 585.5 min under quasi-adiabatic conditions, the NC/ADN mixture stepped into the self-heating stage at 106.4 °C, which was much less than the initial temperatures of NC or ADN. The significant reduction in net pressure increment of NC, ADN and the NC/ADN mixture under vacuum indicates that ADN initiated the interaction of NC with ADN. Compared to gas products of NC or ADN, two new kinds of oxidative gases O2 and HNO2 appeared for the NC/ADN mixture, while NH3 and aldehyde disappeared. The mixing of NC with ADN did not change the initial decomposition pathway of either, but NC made ADN more inclined to decompose into N2O, which resulted in the formation of oxidative gases O2 and HNO2. The thermal decomposition of ADN dominated the initial thermal decomposition stage of the NC/ADN mixture, followed by the oxidation of NC and the cation of ADN.
Nanoscale composite energetic materials (CEMs) based on oxidizer and fuel have potential advantages in energy adjustment and regulation through oxygen balance (OB) change. The micro- and nanosized fibers based on nano nitrocellulose (NC)-ammonium dinitramide (ADN) were prepared by the electrospinning technique, and the morphology, thermal stability, combustion behaviors, and mechanical sensitivity of the fibers were characterized by means of scanning electron microscope (SEM), transmission electron microscopy (TEM), differential scanning calorimetry (DSC), gas pressure measurement of thermostatic decomposition, laser ignition, and sensitivity tests. The results showed that the prepared fibers with fluffy 3D macrostructure were constructed by the overlap of micro/nanofibers with the energetic particles embedded in the NC matrix. The first exothermic peak temperature (Tp) of the samples containing ADN decreased by 10.1 °C at most compared to that of ADN, and the pressure rise time of all the samples containing ADN moved forward compared to that of the sample containing NC only. Furthermore, ADN can decrease the ignition delay time of NC-based fibers under atmosphere at room temperature from 33 ms to 9 ms and can enhance the burning intensity of NC-based fibers under normal pressure. In addition, compared to the single high explosive CL-20 or RDX, the mechanical sensitivities of the composite materials containing high explosive CL-20 or RDX were much decreased. The positive oxygen balance of ADN and the intensive interactions between ADN and NC can reduce the ignition delay time and promote the burning reaction intensity of NC-based composite fibers, while the mechanical sensitivities of composite fibers could be improved.
The fluffy fibers based on nitrocellulose (NC)/ammonium dinitramide (ADN) with high explosives have been fabricated by electrospinning technique. The morphology, thermal stability, combustion behaviors and mechanical sensitivity of NC/ADN-based composite fibers were characterized by means of scanning electron microscope (SEM), transmission electron microscopy (TEM), differentialscanning calorimetry (DSC), gas pressure measurement of thermostatic decomposition, laser ignition and sensitivity test, respectively. The results showed that the prepared fibers with fluffy 3D macrostructure were constructed by the overlap of mirco/nanofibers with the energetic particles imbedded in NC matrix. The addition of ADN can accelerate the thermal decomposition with the peak temperature (Tp) decrease by 10.1 oC and the pressure rise time moving forward. Furthermore, ADN can decrease the ignition delay time of NC-based fibers under atmosphere at room temperature from 33 ms to 9 ms, and enhance the burning strength of NC-based fibers under normal pressure. In addition, the impact sensitivities were reduced from 100–56% for NC-based fibers containing CL-20 and from 88–56% for NC-based fibers containing RDX; the friction sensitivities were reduced from 100–64% for NC-based fibers containing CL-20 and from 84–60% for NC-based fibers containing RDX, respectively.
Organoaluminum compounds have been employed as catalysts in many reactions. However, due to their high reactivity of the AlÀ C bond towards water or air, the accurate analysis and detection of organoaluminum compounds are still challenging. Here we demonstrate the possibility of rapidly and precisely detecting the purity and impurities of triethylaluminium (TEAL). An indirect GC-MS method via alcoholysis reaction using a designed alcoholysis reactor was adopted to detect and separate the main components and impurities of the synthesized TEAL. Previously, the nuclear magnetic resonance (NMR) and the inductively coupled plasma-mass spectrometer (ICP-MS) methods were also selected to detect the main compounds in the synthesized TEAL. The impurities in TEAL was identified as n-butyl aluminum, and the purity of synthesized TEAL is 97.47 % with high accuracy (ca. 99 %). This work suggests a new strategy to detect the purity and impurities of some kind of hazardous compounds.
The detection and separation of impurities are crucial for the quality control of triethylboron. While the purity of triethylboron is the key factor for ballistic performance, impact accuracy, and storage safety. This work will explore a modified gas chromatography‐mass spectrometer method to detect and separate the impurities in synthesized triethylboron. They are identified as CH3CH2OCH2CH3, (CH3CH2)3B, (CH3CH2O)3B, CH3CH2CH2CH2B(CH3CH2)2 and (CH3CH2)3O3B3. Further, optimized GC conditions are demonstrated to quantify the synthesized triethylboron accurately and determine its purity. The purity of triethylboron is 96.39 % via a normalization method with high accuracy (RSD=0.05 %). The optimized GC conditions were as follows: a hydrogen flame ionization detector, nitrogen as carrier gas whose pathway was installed with a water trap and an oxygen trap, an HP‐5 capillary column (30 m×0.32 mm×0.25 μm) with the column temperature of 60 °C, an inlet temperature of 120 °C, the detector temperature of 150 °C, and an injection volume of 0.6 μL. This work demonstrates a simple and precise method to analyze the synthesized triethylboron and its impurities.
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