In this paper, an attractive and rapid ARS-1620 approach for synthesizing cubic δ-TaN nanoparticles is
developed. This approach includes the combustion of K2TaF7 + (5 + k)NaN3 + kNH4F exothermic mixture under nitrogen atmosphere and water purification of final products to produce cubic δ-TaN. The approach described in this study is simple and cost-effective for the large-scale production of δ-TaN. Methods For sample EX 527 supplier preparation, the following chemicals were used: K2TaF7 (prepared at the Graduate School of Green Energy Technology, Chungnam National University, Korea), NaN3 powder (99.0% purity; particle size < 50 μm; Daejung Chemical and Metals Co., Ltd., Shiheung City, South Korea). Chemical-grade ammonium halides (NH4F and NH4Cl) see more were purchased from Samchun Pure Chemical Co., Ltd., Pyeongtaek City, South Korea. All salts were handled in a glove box in dry argon atmosphere (99.99%; Messer, Northumberland, UK). To prepare the reaction mixture, controlled amounts of reactant powders, K2TaF7, NaN3, and NH4F, were weighed and thoroughly mixed in a glove box in argon atmosphere. About 60 to 80 g of the mixture was compacted by hand in a stainless steel cup (4.0 cm in diameter) and placed
in a high-pressure reaction vessel for combustion (Figure 1). A vacuum was applied to remove the air from the combustion vessel, which was then filled with nitrogen gas with a pressure of 2.0 MPa. The combustion process was initiated by a hot nickel-chromium filament system, and the reaction temperatures were measured using WR-20/WR-5 thermocouples inserted into the reaction pellet. After completion of the combustion process, the burned-down sample was cooled to room temperature and transferred to a 500-ml beaker for further purification. The sample was purified by washing with distilled water in order to remove the NaF and KF salts that formed during the reaction. The purified black powder was dried in air at 80°C to 90°C. Figure 1 Experimental setup for the synthesis cubic TaN nanoparticles. We used the simulation software
‘Thermo’ to predict adiabatic combustion temperature (T ad) and concentrations of equilibrium SPTLC1 phases in the combustion wave . Calculations of equilibrium characteristics were based on minimizing the thermodynamic potential of the system. The initial parameters (temperature and pressure) of the system were set as 25°C and 2.0 MPa, respectively. The crystal structure and morphology of the TaN nanoparticles were characterized X-ray diffraction (XRD) with Cu Kα radiation (D5000, Siemens AG, Munich, Germany), field-emission scanning electron microscopy (FESEM; JSM 6330F, JEOL Ltd., Akishima, Tokyo, Japan), and transmission electron microscopy (TEM; JEM 2010, JEOL Ltd.). The specific surface area of the nanoparticles was determined from the linear portion of the Brunauer, Emmett, and Teller plot.