Morphology evolution of ZrB2 nanoparticles synthesized by sol-gel method

Zirconium diboride (ZrB₂) nanoparticles were synthesized by sol-gel method using zirconium n-propoxide (Zr(OPr)₄), boric acid (H₃BO₃), sucrose (C₁₂H₂₂O₁₁), and acetic acid (AcOH). Clearly, it was a non-aqueous solution system at the very beginning of the reactions. Here, AcOH was used as both chemical modifier and solvent to control Zr(OPr)₄ hydrolysis. Actually, AcOH could dominate the hydrolysis by self-produced water of the chemical propulsion, rather than the help of outer water. C₁₂H₂₂O₁₁ was selected, since it can be completely decomposed to carbon. Thus, carbon might be accounted precisely for the carbothermal reduction reaction. Furthermore, we investigated the influence of the gelation temperature on the morphology of ZrB₂ particles. Increasing the gelation temperature, the particle shapes changed from sphere-like particles at 65 °C to a particle chain at 75 °C, and then form rod-like particles at 85 °C. An in-depth HRTEM observation revealed that the nanoparticles of ZrB₂ were gradually fused together to evolve into a particle chain, finally into a rod-like shape. These crystalline nature of ZrB₂ related to the gelation temperature obeyed the “oriented attachment mechanism” of crystallography.