Heating behavior and crystal growth mechanism in microwave field

A simple microwave solid-state reactor was designed on the basis of a domestic microwave oven by using graphite powder as heating medium. The heating behavior of the reactor was studied by using an on-line computer to monitor the real-time temperature during irradiation. It was found that the temperature (T) was related to the time (t) and that microwave power depended on the duty cycle (x) of microwave irradiation. Two empirical equations were proposed and could be applied to the similar microwave solid-state reactors. Four inorganic layered materials, LiV(3)O(8), KNb(3)O(8), KTiNbO(5), and KSr(2)Nb(3)O(10), were successfully synthesized in the designed reactor at a suitable heating rate and temperature that were fully controlled by the empirical equations. Characterization results of X-ray diffraction (XRD), Fourier transform infrared (FTIR) and Raman spectroscopy, and scanning (SEM) and transmission (TEM) electron microscopy indicated that the phases of samples prepared by traditional and microwave methods were in good agreement; nevertheless, the heating nature and the morphologies of products were quite different. The samples synthesized in the microwave field had crystallographic defects and showed an incompactly stacking structure of nanosheets. Due to the rapid formation of crystallites and different extended growth rate along the crystal axis of the products in microwave field, the crystal growth mechanism of layered metal oxides was not according to that of the traditional method and is briefly discussed.