ZrN nanoparticles were prepared by an exothermic reduction of ZrCl4 with NaN3 in the presence of NaCl flux in a nitrogen atmosphere. Using a solid-state combustion approach, we have demonstrated that the zirconium nitride nanoparticles synthesis process can be completed in only several minutes compared with a few hours for previous synthesis approaches. The chemistry of the combustion process is not complex and is based on a metathesis reaction between ZrCl4 and NaN3. Because of the low melting and boiling points of the raw materials it was possible to synthesize the ZrN phase at low combustion temperatures. It was shown that the combustion temperature and the size of the particles can be readily controlled by tuning the concentration of the NaCl flux. The results show that an increase in the NaCl concentration (from 2 to 13 M) results in a temperature decrease from 1280 to 750˚C. ZrN nanoparticles have a high surface area (50-70 m2/g), narrow pore size distribution, and nano-particle size between 10 and 30 nm. The activation energy, which can be extracted from the experimental combustion temperature data, is: E = 20 kcal/mol. The method reported here is self-sustaining, rapid, and can be scaled up for a large scale production of a transition metal nitride nanoparticle system (TiN, TaN, HfN, etc.) with suitable halide salts and alkali metal azide.
In this study, the heat flow of the plant scale aluminum extrusion process was investigated to establish optimum continuous heat treatment conditions. During the extrusion of 6061 aluminum alloy, processing parameters such as the extrusion pressure, speed and temperature histories of billets were logged as a function of time. The surface temperature of the billets increased at constant ram speed, while it decreased with decreases of the ram speed. In order to maintain the billet temperature within a solutionizing temperature range prior to the succeeding water quenching step, the ram speed or the temperature of the blower should be controlled. The temperature histories of the billets during the extrusion and hot air blowing processes were successfully simulated by using the velocity boundary model in ANSYS CFX. The methodology to design an optimum process by using a commercial simulation program is described in this study on the basis of the metallurgical validation results of the microstructural observation of the extrudates. The developed model allowed the advantages of taking into account the motion of the extrudate coupled with the temperature change based on empirical data. Calculations were made for the extrudate passing through the isothermal chamber maintained at appropriate temperature. It was confirmed that the continuous heat treatment system is beneficial to the productivity enhancement of the commercial aluminum extrusion industry.
The liquid-phase sintering method was used to prepare a glass lens forming core composed of SiC-Al2O3-Y2O3. Spark plasma sintering was used to obtain dense sintered bodies. The sintering characteristics of different SiC sources and compositions of additives were studied. Results revealed that, owing to its initial larger surface area, α-SiC offers sinterability that is superior to that of β-SiC. A maximum density of 3.32 g/cm3 (theoretical density [TD] of 99.7%) was obtained in α-SiC-10 wt% (6Al2O3-4Y2O3) sintered at 1850˚C without high-energy ball milling. The maximum hardness and compression stress of the sintered body reached 2870 Hv and 1110 MPa, respectively. The optimum ultra-precision machining parameters were a grinding speed of 1243 m/min, work spindle rotation rate of 100 rpm, feed rate of 0.5 mm/min, and depth of cut of 0.2 μm. The surface roughnesses of the thus prepared final products were Ra = 4.3 nm and Rt = 55.3 nm for the aspheric lens forming core and Ra = 4.4 nm and Rt = 41.9 for the spherical lens forming core. These values were found to be sufficiently low, and the cores showed good compatibility between SiC and the diamond-like carbon (DLC) coating material. Thus, these glass lens forming cores have great potential for application in the lens industry.