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Synthesis and flash sintering of zirconium nitride powder
Authors:Suprabha Das  Diego Dubois  Md Shariful Islam Sozal  Yusuf Emirov  Borzooye Jafarizadeh  Chunlei Wang  Vadym Drozd  Andriy Durygin  Zhe Cheng
Affiliation:1. Department of Mechanical and Materials Engineering, Florida International University, Miami, Florida, USA;2. Department of Mechanical and Materials Engineering, Florida International University, Miami, Florida, USA

Center for the Study of Matter at Extreme Conditions (CeSMEC), Florida International University, Miami, Florida, USA;3. Nanotechnology Research and Education Center, University of South Florida, Tampa, Florida, USA;4. Center for the Study of Matter at Extreme Conditions (CeSMEC), Florida International University, Miami, Florida, USA

Abstract:Zirconium nitride (ZrN) is a transition metal nitride of great interest due to its excellent physical and chemical properties. This study aims to synthesize ZrN fine powders by a facile and low-cost urea route that avoids the use of any solvent. ZrCl4 and urea mixtures were heat-treated at up to 1600˚C in nitrogen gas. The products were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, energy-dispersive X-ray spectroscopy, and thermogravimetric analysis. The effects of different processing parameters such as metal to urea molar ratio, heat treatment temperature, and dwelling time on the product phase and stoichiometry were studied to understand the synthesis method. In addition, synthesized ZrN powder was consolidated into near fully dense single-phase bulk ceramic with a homemade flash sintering setup. A constant DC electrical field of ∼80 V/cm and pressure of ∼14 MPa at room temperature triggered flash sintering without pre-heating, and the entire process finished in 200 s. The composition, microstructure, density, hardness, and oxidation properties of the sintered pellet were also characterized.
Keywords:flash sintering  metal nitrides  soft urea method  ultra-high temperature ceramics  zirconium compounds
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