An energetic co-crystal consisting of the most promising military explosive 2, 4,6,8,10,4,6,8,10, and the most well-known oxidant applied in propellants ammonium perchlorate has been prepared with a simple solvent evaporation method. Scanning electron microscopy revealed that the morphology of co-crystal differs greatly from each component. The X-ray diffraction spectrum, FTIR, Raman spectra, and differential scanning calorimetry characterisation further prove the formation of the co-crystal. The result of determination of hygroscopic rate indicated the hygroscopicity was effectively reduced. At last, the crystallisation mechanism has been discussed. Defence Science Journal, Vol. 67, No. 5, September 2017, pp. 510-517, DOI : 10.14429/dsj.67.10188 2017 STuDY OF AN ENERGETIC-OXIDANT CO-CRYSTAL: PREPARATION, CHARACTERISATION AND CRYSTALLISATION MECHANISM 511 to do differential scanning calorimetry (DSC) analysis. 2 mg -3 mg simple was weighed into alumina crucible each time. Test conditions were recorded with 20 mL/min nitrogen purge flow at 20 °C /min from 25 °C to 500 °C.
SEM StudiesAs shown in Fig. 1, AP crystals tend to be spherical with rounded edges and corners, which particle size is approximately 100 μm. Raw CL-20 particles are more like irregular polyhedron with uneven size. However, CL-20/AP co-crystal, presenting cubo octahedron, varies greatly from the morphology of each single component. stretching respectively. However, these two bands shifted to 3209.30 cm -1 and 3054.41 cm -1 in the co-crystal.
XRD CharacterisationThe XRD patterns of AP, CL-20 and co-crystal are presented in Fig. 5. The characteristic peaks of AP with 2θ-values of 19.52, 22.79, 24.00, and 24.75 are not present in the co-crystal pattern. In the case of CL-20, the characteristic peaks at 10.88°, 12.74°, 13.95°, 16.46°, 25.96° and 28.02° are not present in the co-crystal. However in the co-crystal, a new peak at about 12.06°, 13.67°, 27.49° and 41.75° formed after crystallisation. The result indicated that the pattern of the as prepared co-crystal differs enormously from each individual component. The appearance of the unique powder diffraction pattern is evidence for the formation of a new crystal.
FT-IR SpectraThe FT-IR spectra of AP, CL-20 and co-crystal are as shown in Fig. 4 and 3281.29 cm -1 , respectively. Similarly, some characteristic absorption peaks of CL-20 also shift after crystallisation. Those phenomena may be caused by the hydrogen bond interactions involved in co-crystal formation which changes the symmetry characteristic.
Raman SpectraThe Raman spectra of AP, CL-20 and co-crystal are presented in Fig. 5. Some characteristic peaks of AP and CL-20 are detected in the co-crystal from Micro-Raman spectroscopy (MRS). Similar to FTIR, some peak shift also take place for Raman spectra which can be attributed to intermolecular hydrogen-bonding. For example, AP has band at 3212.38 cm
Thermal PropertyAs shown in Fig. 6, CL-20/AP co-crystal presents a unique thermal property which is different from single componen...