Morphology-controlled
precipitation of three powerful organic high
energetic compounds (HECs) viz. cyclotrimethylenetrinitramine (RDX),
octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine (HMX), and 2-methyl-1,3,5-trinitrobenzene
(TNT) was achieved by two different processes, namely, drop-by-drop
(DBD) and drop-to-drop (DTD) solvent–antisolvent interaction
methods. Effect of different experimental parameters on the mean size
and morphology of the prepared submicron-sized particles of HECs was
investigated thoroughly. The DBD method favors the formation of nanosized
particles of RDX and TNT at lower concentrations (5 mM). However,
a significant increase in the mean particle size occurred at higher
concentrations (25 and 50 mM). Formation of facetted crystals of RDX,
HMX, and nanorods of TNT was observed at higher concentrations because
of the interaction of crystal facets with the antisolvent. Relatively,
smaller sized, spherical particles of RDX and HMX could be prepared
through the DTD method even at higher concentrations (25 mM). The
DTD method is a continuous process and hence is a facile method for
industrial applications. X-ray diffraction and Fourier transform infrared
spectroscopy studies revealed that RDX, HMX and TNT were precipitated
in their most stable polymorphic forms α, β, and monoclinic,
respectively. Differential scanning calorimetry showed that the thermal
response of the nano-HECs was similar to the respective raw-HECs.
A slight decrease in crystallinity and the melting point was observed
because of the decrease in the mean particle size.