Process analysis and mechanism investigation of low temperature synthesis of nanoscale calcium hexaboride powder.
The synthesis of nanoscale CaB6 powder via the low temperature chemical reaction of Calcium chloride (CaCl2) with Sodium Borohyride (NaBH4) in vacuum has been investigated in this study. The reaction temperature was determined by differential scanning calorimetry and thermogravimetric analysis (DSC and TG). Crystallization process was provided through studying the influence of heat preservation time on the crystal particles morphologies in vacuum. X-ray diffraction (XRD) was used to investigate the phase and structure of CaB6. The characterization for microstructure was performed by transmission electron microscopy (TEM) and high resolution transmission electron microscopy (HRTEM). The elemental analysis was conducted by X-ray photoelectron spectroscopy (XPS). It is concluded that CaB6 nanoparticles can be successfully prepared under low temperature at 500 degrees C. The results showed that in vacuum, 2 hours heat preservation time is enough for the reaction to complete at this temperature. The average size of crystal grains is 25.1 nm with high crystallinity and cubic shaped, which particles size is at the range of 20-100 nm. Longer heat preservation time more than 2 hours will make CaB6 particles connected together to form hard aggregations, that is the sintering process occurred under this temperature. However, the crystal grain size changed unobviously accompanying the holding time prolong due to the high chemical stability of CaB6. The atomic ratio of B to Ca is 5.37:1, less than but close to its stoichiometric ratio 6:1. The synthesis process and mechanism were investigated in this paper.
Lin
L
Zhang
Gang
G
Feng
Guanghui
G
Min