ABSTRACT
In this work, a reaction coupling self-propagating high-temperature synthesis (RC-SHS) method was developed for the in situ controlled synthesis of novel, high activity TiB2/(TiB2-TiN) hierarchical/heterostructured nanocomposites using TiO2, Mg, B2O3, KBH4 and NH4NO3 as raw materials. The as-synthesized samples were characterized using X-ray diffraction (XRD), scanning electron microscope (SEM), X-ray energy dispersive spectroscopy (EDX), transition electron microscopy (TEM), high-resolution TEM (HRTEM) and selected-area electron diffraction (SAED). The obtained TiB2/TiN hierarchical/heterostructured nanocomposites demonstrated an average particle size of 100-500 nm, and every particle surface was covered by many multibranched, tapered nanorods with diameters in the range of 10-40 nm and lengths of 50-200 nm. In addition, the tapered nanorod presents a rough surface with abundant exposed atoms. The internal and external components of the nanorods were TiB2 and TiN, respectively. Additionally, a thermogravimetric and differential scanning calorimetry analyzer (TG-DSC) comparison analysis indicated that the as-synthesized samples presented better chemical activity than that of commercial TiB2 powders. Finally, the possible chemical reactions as well as the proposed growth mechanism of the TiB2/(TiB2-TiN) hierarchical/heterostructured nanocomposites were further discussed.
ABSTRACT
Nanocrystalline niobium nitride (NbN0.9) was successfully synthesized at 600 degrees C through a solid-state reaction. The synthesis was carried out in an autoclave by using NbCl5 and NaN3 as the reactants. The X-ray powder diffraction pattern indicates the formation of cubic NbN0.9. Transmission electron microscopy images show that typical NbN0.9 crystallites are composed of uniform particles with an average size of about 30 nm and nanorod crystallites with a typical size of about 40 x 2500 nm. Magnetic measurements exhibited that a superconducting transition occurred at 15.4 K for the NbN0.9 product.
Subject(s)
Crystallization , Nanostructures/chemistry , Nanotechnology/methods , Niobium/chemistry , Nitrogen/chemistry , Hot Temperature , Microscopy, Electron, Transmission , Nanostructures/ultrastructure , Time Factors , X-Ray DiffractionABSTRACT
Titanium nitride hollow spheres were synthesized by the reaction of TiCl4 and NaNH2 at room temperature. X-ray powder diffraction (XRD) pattern could be indexed as cubic TiN with the lattice constants of a = 4.236 A. Transmission electron microscopy (TEM) images showed hollow spheres with diameter about 200 nm. A possible formation mechanism of TiN hollow spheres was discussed.
